data_lumsdenite _audit_creation_method 'SHELXL-2016/6' _shelx_SHELXL_version_number '2016/6' _chemical_name_mineral 'lumsdenite' _chemical_compound_source 'Packrat mine, Colorado' _chemical_formula_sum 'As7 H90 Ca3.19 Mg2 Na0.81 O96 V12' _chemical_formula_weight 2957.53 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'As' 'As' 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ca' 'Ca' 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'V' 'V' 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mg' 'Mg' 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Na' 'Na' 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.3490(5) _cell_length_b 17.6263(9) _cell_length_c 23.2556(16) _cell_angle_alpha 82.208(6) _cell_angle_beta 88.351(6) _cell_angle_gamma 81.702(6) _cell_volume 4158.8(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _exptl_crystal_density_diffrn 2.362 _exptl_crystal_F_000 2923 _exptl_crystal_size_max 0.180 _exptl_crystal_size_mid 0.080 _exptl_crystal_size_min 0.030 _exptl_absorpt_coefficient_mu 4.408 _shelx_estimated_absorpt_T_min 0.504 _shelx_estimated_absorpt_T_max 0.879 _diffrn_measurement_device_type 'Rigaku R-axis RAPID II' _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details Higashi2001 _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_reflns_number 36970 _diffrn_reflns_av_unetI/netI 0.0945 _diffrn_reflns_av_R_equivalents 0.1003 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.042 _diffrn_reflns_theta_max 22.454 _diffrn_reflns_theta_full 22.454 _diffrn_measured_fraction_theta_max 0.986 _diffrn_measured_fraction_theta_full 0.986 _diffrn_reflns_Laue_measured_fraction_max 0.986 _diffrn_reflns_Laue_measured_fraction_full 0.986 _diffrn_reflns_point_group_measured_fraction_max 0.986 _diffrn_reflns_point_group_measured_fraction_full 0.986 _reflns_number_total 10623 _reflns_number_gt 7560 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2016/6 (Sheldrick, 2016)' _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0825P)^2^+6.1461P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens . _refine_ls_hydrogen_treatment undef _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 10623 _refine_ls_number_parameters 1091 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0870 _refine_ls_R_factor_gt 0.0585 _refine_ls_wR_factor_ref 0.1612 _refine_ls_wR_factor_gt 0.1434 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Na Na 0.2347(7) 0.5594(3) 0.9636(2) 0.093(3) Uani 0.81(3) 1 d . . P . . Ca Ca 0.2347(7) 0.5594(3) 0.9636(2) 0.093(3) Uani 0.19(3) 1 d . . P . . Ca1 Ca 0.3935(2) 0.19972(13) 0.02764(9) 0.0337(6) Uani 1 1 d . . . . . Ca2 Ca 0.5615(2) 0.05030(13) 0.79386(10) 0.0370(6) Uani 1 1 d . . . . . Ca3 Ca 1.3758(2) 0.10512(13) 0.46149(9) 0.0331(6) Uani 1 1 d . . . . . Mg1 Mg 0.3334(3) 0.45075(19) 0.42140(15) 0.0302(9) Uani 1 1 d . . . . . Mg2 Mg 0.2105(4) 0.6832(2) 0.66617(16) 0.0382(10) Uani 1 1 d . . . . . As1 As 0.05776(11) 0.20195(6) 0.74520(5) 0.0267(3) Uani 1 1 d . . . . . As2 As 0.27158(11) 0.48727(6) 0.68303(5) 0.0280(3) Uani 1 1 d . . . . . As3 As 0.21973(11) 0.37009(6) 0.92173(5) 0.0300(3) Uani 1 1 d . . . . . As4 As 0.15779(10) 0.06728(6) 0.98533(4) 0.0259(3) Uani 1 1 d . . . . . As5 As 1.14023(10) -0.13228(6) 0.80861(5) 0.0272(3) Uani 1 1 d . . . . . As6 As 1.18983(11) 0.98578(6) 0.58012(5) 0.0274(3) Uani 1 1 d . . . . . As7 As 0.25359(11) 0.30051(6) 0.51771(5) 0.0285(3) Uani 1 1 d . . . . . V1 V 0.01970(17) 0.39800(10) 0.71179(8) 0.0291(5) Uani 1 1 d . . . . . V2 V -0.00816(18) 0.33408(10) 0.83983(8) 0.0291(5) Uani 1 1 d . . . . . V3 V -0.04341(17) 0.14092(10) 0.88133(7) 0.0265(4) Uani 1 1 d . . . . . V4 V 0.94840(17) 0.03048(10) 0.78744(7) 0.0250(4) Uani 1 1 d . . . . . V5 V 0.97214(17) 0.10314(10) 0.63944(8) 0.0276(5) Uani 1 1 d . . . . . V6 V 0.00395(17) 0.27654(10) 0.60481(7) 0.0277(5) Uani 1 1 d . . . . . V7 V 0.29760(18) 0.35261(10) 0.78970(8) 0.0291(5) Uani 1 1 d . . . . . V8 V 0.22558(16) 0.01161(10) 0.86135(7) 0.0251(4) Uani 1 1 d . . . . . V9 V 0.27910(17) 0.14336(10) 0.60462(7) 0.0262(4) Uani 1 1 d . . . . . V10 V 0.32330(17) 0.31533(10) 0.64886(8) 0.0278(5) Uani 1 1 d . . . . . V11 V 0.26494(17) 0.19447(10) 0.89078(7) 0.0269(4) Uani 1 1 d . . . . . V12 V 1.24733(17) 0.99512(10) 0.71509(7) 0.0260(4) Uani 1 1 d . . . . . O1 O -0.0260(7) 0.2018(4) 0.6782(3) 0.0299(18) Uani 1 1 d . . . . . O2 O 0.9553(6) 0.1451(3) 0.7929(3) 0.0261(17) Uani 1 1 d . . . . . O3 O -0.0149(6) 0.2977(4) 0.7599(3) 0.0241(16) Uani 1 1 d . . . . . O4 O 0.3031(7) 0.5761(4) 0.6592(3) 0.0342(19) Uani 1 1 d . . . . . O5 O 0.3487(7) 0.4267(4) 0.6387(3) 0.0349(19) Uani 1 1 d . . . . . O6 O 0.3232(7) 0.4593(4) 0.7519(3) 0.0295(17) Uani 1 1 d . . . . . O7 O 0.1087(7) 0.4860(4) 0.6794(3) 0.0336(18) Uani 1 1 d . . . . . O8 O 0.2362(8) 0.4234(4) 0.9738(3) 0.041(2) Uani 1 1 d . . . . . O9 O 0.3000(7) 0.4034(4) 0.8616(3) 0.0320(18) Uani 1 1 d . . . . . O10 O 0.2805(7) 0.2768(4) 0.9435(3) 0.0341(18) Uani 1 1 d . . . . . O11 O 0.0580(7) 0.3734(4) 0.9074(3) 0.0341(19) Uani 1 1 d . . . . . O12 O 0.1544(7) 0.0430(4) 0.0558(3) 0.0296(17) Uani 1 1 d . . . . . O13 O 0.0069(6) 0.1031(4) 0.9614(3) 0.0315(18) Uani 1 1 d . . . . . O14 O 0.2216(6) 0.9942(4) 0.9485(3) 0.0256(16) Uani 1 1 d . . . . . O15 O 0.2495(7) 0.1414(4) 0.9712(3) 0.0307(17) Uani 1 1 d . . . . . O16 O 0.1397(7) 0.7736(4) 0.8240(3) 0.0360(19) Uani 1 1 d . . . . . O17 O 0.2075(6) 0.8993(4) 0.8646(3) 0.0289(17) Uani 1 1 d . . . . . O18 O 0.9884(7) 0.9159(4) 0.7956(3) 0.0324(18) Uani 1 1 d . . . . . O19 O 0.2329(7) 0.8857(4) 0.7477(3) 0.0341(18) Uani 1 1 d . . . . . O20 O 0.2077(7) 0.9234(4) 0.5321(3) 0.0360(19) Uani 1 1 d . . . . . O21 O 0.0332(7) 0.0210(4) 0.5916(3) 0.0339(18) Uani 1 1 d . . . . . O22 O 0.2549(7) 0.9407(4) 0.6436(3) 0.0322(18) Uani 1 1 d . . . . . O23 O 0.2714(7) 0.0603(4) 0.5538(3) 0.0294(17) Uani 1 1 d . . . . . O24 O 0.2831(7) 0.3413(4) 0.4508(3) 0.0372(19) Uani 1 1 d . . . . . O25 O 0.0956(7) 0.3200(4) 0.5346(3) 0.0364(19) Uani 1 1 d . . . . . O26 O 0.3428(7) 0.3379(4) 0.5637(3) 0.0302(18) Uani 1 1 d . . . . . O27 O 0.3003(7) 0.2032(4) 0.5246(3) 0.0290(17) Uani 1 1 d . . . . . O28 O -0.0112(7) 0.2362(4) 0.8793(3) 0.0353(19) Uani 1 1 d . . . . . O29 O 0.9606(7) 0.0453(4) 0.7069(3) 0.0339(18) Uani 1 1 d . . . . . O30 O 0.0259(7) 0.3541(4) 0.6466(3) 0.0343(18) Uani 1 1 d . . . . . O31 O -0.1238(7) 0.4457(4) 0.7112(3) 0.040(2) Uani 1 1 d . . . . . O32 O -0.1550(7) 0.3743(4) 0.8438(3) 0.0388(19) Uani 1 1 d . . . . . O33 O -0.1960(6) 0.1484(4) 0.8911(3) 0.0315(18) Uani 1 1 d . . . . . O34 O 0.7951(7) 0.0306(4) 0.7979(3) 0.0331(18) Uani 1 1 d . . . . . O35 O 0.8260(7) 0.1206(4) 0.6164(3) 0.041(2) Uani 1 1 d . . . . . O36 O -0.1407(7) 0.2982(4) 0.5806(3) 0.039(2) Uani 1 1 d . . . . . O37 O 0.0820(6) 0.4111(4) 0.7893(3) 0.0233(16) Uani 1 1 d . . . . . O38 O 0.0065(6) 0.0281(4) 0.8693(3) 0.0268(17) Uani 1 1 d . . . . . O39 O 0.0613(6) 0.1725(4) 0.5801(3) 0.0256(16) Uani 1 1 d . . . . . O40 O 0.2387(6) 0.3346(4) 0.7180(3) 0.0289(17) Uani 1 1 d . . . . . O41 O 0.2141(6) 0.2765(4) 0.8346(3) 0.0260(17) Uani 1 1 d . . . . . O42 O 0.1836(6) 0.1223(4) 0.8666(3) 0.0272(17) Uani 1 1 d . . . . . O43 O 0.1660(6) 0.0247(4) 0.7795(3) 0.0276(17) Uani 1 1 d . . . . . O44 O 0.1967(7) 0.0832(4) 0.6653(3) 0.0279(17) Uani 1 1 d . . . . . O45 O 0.2321(6) 0.2379(4) 0.6338(3) 0.0262(17) Uani 1 1 d . . . . . O46 O 0.4446(7) 0.3116(4) 0.7900(3) 0.0355(19) Uani 1 1 d . . . . . O47 O 0.4151(7) 0.1696(4) 0.8778(3) 0.0330(18) Uani 1 1 d . . . . . O48 O 0.3798(6) 0.0063(4) 0.8486(3) 0.0294(17) Uani 1 1 d . . . . . O49 O 0.3986(6) 0.9953(4) 0.7264(3) 0.0287(17) Uani 1 1 d . . . . . O50 O 0.4294(7) 0.1228(4) 0.6208(3) 0.0340(19) Uani 1 1 d . . . . . O51 O 0.4648(7) 0.2721(4) 0.6667(3) 0.0368(19) Uani 1 1 d . . . . . OW1 O 0.5737(7) 0.0439(4) 0.5310(3) 0.040(2) Uani 1 1 d . . . . . OW2 O 0.6422(7) 0.1777(4) 0.7867(4) 0.049(2) Uani 1 1 d . . . . . OW3 O 0.3902(8) 0.5592(5) 0.3895(4) 0.056(2) Uani 1 1 d . . . . . OW4 O 0.3258(8) 0.4854(4) 0.5076(3) 0.043(2) Uani 1 1 d . . . . . OW5 O 0.2400(10) 0.6713(5) 0.7557(3) 0.066(3) Uani 1 1 d . . . . . OW6 O 0.1265(8) 0.7975(4) 0.6680(3) 0.049(2) Uani 1 1 d . . . . . OW7 O 0.1755(8) 0.6976(4) 0.5778(3) 0.048(2) Uani 1 1 d . . . . . OW8 O 1.2780(9) 0.2168(4) 0.3956(3) 0.060(3) Uani 1 1 d . . . . . OW9 O 0.5120(7) 0.0728(4) 0.0314(4) 0.047(2) Uani 1 1 d . . . . . OW10 O 0.4627(8) 0.0774(5) 0.3680(3) 0.051(2) Uani 1 1 d . . . . . OW11 O 0.5436(7) 0.4123(4) 0.4378(3) 0.043(2) Uani 1 1 d . . . . . OW12 O 0.3951(7) 0.1498(4) 0.7533(3) 0.038(2) Uani 1 1 d . . . . . OW13 O 0.0264(9) 0.6443(5) 0.6807(5) 0.073(3) Uani 1 1 d . . . . . OW14 O 0.3413(11) 0.3234(5) 0.0622(4) 0.084(4) Uani 1 1 d . . . . . OW15 O 0.1372(8) 0.4976(5) 0.4139(4) 0.062(3) Uani 1 1 d . . . . . OW16 O 0.3726(9) 0.4137(5) 0.3382(4) 0.064(3) Uani 1 1 d . . . . . OW17 O 0.3958(7) 0.7219(4) 0.6543(3) 0.046(2) Uani 1 1 d . . . . . OW18 O 0.6152(7) 0.0384(4) 0.8984(3) 0.040(2) Uani 1 1 d . . . . . OW19 O 0.2417(7) 0.1579(4) 0.1018(3) 0.043(2) Uani 1 1 d . . . . . OW20 O 0.5681(7) 0.1834(4) 0.4488(3) 0.046(2) Uani 1 1 d . . . . . OW21 O 0.6245(8) 0.9110(5) 0.7970(4) 0.052(2) Uani 1 1 d . . . . . OW22 O 0.5371(8) 0.1915(5) 0.1123(3) 0.053(2) Uani 1 1 d . . . . . OW23 O 1.1808(8) 0.0667(5) 0.4197(3) 0.052(2) Uani 1 1 d . . . . . OW24 O 0.6390(8) 0.0526(5) 0.6927(3) 0.053(2) Uani 1 1 d . . . . . OW25 O 0.5823(8) 0.2301(6) 0.9767(4) 0.078(3) Uani 1 1 d . . . . . OW26 O 0.0065(18) 0.5744(15) 0.9335(9) 0.254(13) Uani 1 1 d . . . . . OW27 O 0.2991(14) 0.6819(8) 0.9093(7) 0.147(6) Uani 1 1 d . . . . . OW28 O 0.0930(15) 0.6751(7) 0.9958(6) 0.137(6) Uani 1 1 d . . . . . OW29 O 0.417(3) 0.5623(14) 0.0175(11) 0.284(13) Uani 1 1 d . . . . . OW30 O 0.845(2) 0.4793(9) 0.9379(6) 0.188(9) Uani 1 1 d . . . . . OW31 O 0.320(4) 0.5522(11) 0.8608(13) 0.39(2) Uani 1 1 d . . . . . OW32 O -0.3942(8) 0.2868(5) 0.5265(4) 0.056(2) Uani 1 1 d . . . . . OW33 O -0.0208(7) 0.1677(4) 0.4731(3) 0.0361(19) Uani 1 1 d . . . . . OW34 O 0.8239(7) 0.1801(4) 0.0260(3) 0.043(2) Uani 1 1 d . . . . . OW35 O -0.0695(8) 0.4239(4) 0.4622(3) 0.048(2) Uani 1 1 d . . . . . OW36 O 0.7015(8) 0.3282(5) 0.7059(4) 0.070(3) Uani 1 1 d . . . . . OW37 O 0.5913(8) 0.4700(5) 0.7530(4) 0.065(3) Uani 1 1 d . . . . . OW38 O 0.5963(9) 0.3499(7) 0.8877(4) 0.089(4) Uani 1 1 d . . . . . OW39 O 0.1299(10) 0.1275(6) 0.3021(4) 0.088(3) Uani 1 1 d . . . . . OW40 O 0.4762(12) 0.7958(7) 0.7474(6) 0.111(4) Uani 1 1 d . . . . . OW41 O 0.9149(12) 0.7241(7) 0.8561(8) 0.161(7) Uani 1 1 d . . . . . OW42 O 0.2296(15) 0.2849(11) 0.2673(6) 0.170(7) Uani 1 1 d . . . . . OW43 O 0.522(2) 0.6581(13) 0.8267(9) 0.238(10) Uani 1 1 d . . . . . OW44 O 0.727(2) 0.5454(9) 0.8289(8) 0.224(11) Uani 1 1 d . . . . . OW45 O 0.028(2) 0.5586(7) 0.8109(6) 0.180(9) Uani 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Na 0.162(7) 0.053(4) 0.074(4) -0.018(3) 0.006(4) -0.040(4) Ca 0.162(7) 0.053(4) 0.074(4) -0.018(3) 0.006(4) -0.040(4) Ca1 0.0394(14) 0.0312(14) 0.0313(13) -0.0025(11) -0.0023(11) -0.0096(11) Ca2 0.0330(13) 0.0375(15) 0.0381(14) 0.0070(11) -0.0001(11) -0.0085(11) Ca3 0.0407(14) 0.0289(13) 0.0301(13) -0.0033(10) 0.0055(10) -0.0083(11) Mg1 0.042(2) 0.021(2) 0.030(2) 0.0001(16) 0.0083(17) -0.0185(17) Mg2 0.052(2) 0.023(2) 0.041(2) -0.0065(17) 0.0062(19) -0.0102(18) As1 0.0346(6) 0.0205(6) 0.0257(6) -0.0009(5) 0.0008(5) -0.0087(5) As2 0.0362(7) 0.0186(6) 0.0299(7) -0.0006(5) 0.0025(5) -0.0096(5) As3 0.0405(7) 0.0219(6) 0.0288(7) -0.0035(5) 0.0001(5) -0.0084(5) As4 0.0308(6) 0.0220(6) 0.0255(6) -0.0005(5) 0.0011(5) -0.0086(5) As5 0.0335(7) 0.0195(6) 0.0292(6) -0.0011(5) 0.0027(5) -0.0083(5) As6 0.0354(7) 0.0233(6) 0.0258(6) -0.0043(5) 0.0028(5) -0.0119(5) As7 0.0387(7) 0.0218(6) 0.0261(6) -0.0003(5) 0.0022(5) -0.0109(5) V1 0.0336(11) 0.0198(10) 0.0344(11) -0.0004(8) -0.0013(9) -0.0079(8) V2 0.0365(11) 0.0219(10) 0.0291(11) -0.0031(8) 0.0040(8) -0.0063(9) V3 0.0327(11) 0.0201(10) 0.0266(10) -0.0008(8) 0.0030(8) -0.0067(8) V4 0.0277(10) 0.0214(10) 0.0267(10) -0.0004(8) 0.0001(8) -0.0091(8) V5 0.0329(11) 0.0251(11) 0.0266(10) -0.0030(8) 0.0016(8) -0.0114(8) V6 0.0334(11) 0.0231(10) 0.0267(11) -0.0005(8) 0.0008(8) -0.0073(8) V7 0.0362(11) 0.0233(11) 0.0274(11) 0.0006(8) 0.0025(8) -0.0074(9) V8 0.0270(10) 0.0226(10) 0.0272(10) -0.0033(8) 0.0011(8) -0.0090(8) V9 0.0325(11) 0.0194(10) 0.0279(11) -0.0006(8) -0.0002(8) -0.0101(8) V10 0.0360(11) 0.0201(10) 0.0289(11) -0.0024(8) 0.0004(8) -0.0100(8) V11 0.0340(11) 0.0206(10) 0.0267(10) -0.0014(8) 0.0012(8) -0.0081(8) V12 0.0316(10) 0.0221(10) 0.0256(10) -0.0015(8) 0.0008(8) -0.0099(8) O1 0.040(4) 0.023(4) 0.026(4) 0.001(3) 0.004(3) -0.009(3) O2 0.036(4) 0.013(4) 0.029(4) 0.006(3) 0.003(3) -0.010(3) O3 0.028(4) 0.021(4) 0.021(4) 0.002(3) 0.003(3) -0.002(3) O4 0.055(5) 0.010(4) 0.041(5) -0.006(3) 0.008(4) -0.016(3) O5 0.050(5) 0.020(4) 0.034(4) -0.001(3) 0.007(4) -0.005(4) O6 0.037(4) 0.024(4) 0.032(4) -0.007(3) 0.001(3) -0.018(3) O7 0.035(4) 0.028(4) 0.037(4) 0.005(3) 0.003(3) -0.007(3) O8 0.063(5) 0.024(4) 0.039(5) -0.011(4) -0.012(4) -0.003(4) O9 0.042(4) 0.025(4) 0.030(4) 0.003(3) 0.001(3) -0.012(3) O10 0.050(5) 0.022(4) 0.031(4) -0.003(3) -0.003(4) -0.006(4) O11 0.041(5) 0.033(4) 0.027(4) -0.004(3) 0.000(3) -0.003(4) O12 0.037(4) 0.028(4) 0.025(4) -0.002(3) 0.000(3) -0.011(3) O13 0.030(4) 0.032(4) 0.031(4) -0.004(3) -0.001(3) -0.002(3) O14 0.024(4) 0.024(4) 0.029(4) -0.004(3) 0.000(3) -0.006(3) O15 0.036(4) 0.029(4) 0.029(4) -0.001(3) 0.001(3) -0.014(3) O16 0.051(5) 0.019(4) 0.038(5) 0.001(3) 0.011(4) -0.012(4) O17 0.036(4) 0.019(4) 0.032(4) 0.005(3) 0.005(3) -0.012(3) O18 0.040(4) 0.020(4) 0.039(5) -0.002(3) 0.001(3) -0.010(3) O19 0.049(5) 0.020(4) 0.033(4) -0.001(3) 0.005(4) -0.009(4) O20 0.052(5) 0.030(4) 0.030(4) -0.016(3) 0.005(4) -0.011(4) O21 0.040(4) 0.033(4) 0.031(4) -0.010(3) 0.004(3) -0.010(4) O22 0.050(5) 0.020(4) 0.027(4) -0.005(3) 0.002(3) -0.006(3) O23 0.037(4) 0.017(4) 0.034(4) -0.002(3) 0.002(3) -0.009(3) O24 0.051(5) 0.032(4) 0.027(4) 0.001(3) 0.007(4) -0.005(4) O25 0.033(4) 0.032(4) 0.041(5) 0.005(4) 0.005(4) -0.006(4) O26 0.054(5) 0.018(4) 0.022(4) 0.005(3) 0.001(3) -0.021(3) O27 0.046(5) 0.014(4) 0.027(4) 0.000(3) 0.004(3) -0.007(3) O28 0.051(5) 0.025(4) 0.029(4) -0.001(3) 0.010(4) -0.007(4) O29 0.040(5) 0.028(4) 0.036(5) -0.007(3) 0.006(4) -0.011(4) O30 0.045(5) 0.025(4) 0.034(4) 0.001(3) -0.006(4) -0.012(4) O31 0.043(5) 0.028(4) 0.045(5) 0.002(4) 0.003(4) -0.002(4) O32 0.040(5) 0.035(5) 0.042(5) -0.006(4) 0.003(4) -0.005(4) O33 0.031(4) 0.030(4) 0.031(4) 0.002(3) 0.004(3) -0.002(3) O34 0.033(4) 0.028(4) 0.037(5) -0.002(3) 0.000(3) -0.003(3) O35 0.045(5) 0.041(5) 0.037(5) -0.005(4) -0.003(4) -0.005(4) O36 0.040(5) 0.041(5) 0.037(5) -0.006(4) -0.002(4) -0.003(4) O37 0.026(4) 0.024(4) 0.022(4) -0.002(3) 0.000(3) -0.011(3) O38 0.029(4) 0.027(4) 0.027(4) -0.010(3) 0.001(3) -0.006(3) O39 0.030(4) 0.018(4) 0.029(4) 0.000(3) 0.006(3) -0.010(3) O40 0.032(4) 0.020(4) 0.034(4) 0.003(3) 0.005(3) -0.009(3) O41 0.023(4) 0.023(4) 0.032(4) 0.001(3) -0.005(3) -0.006(3) O42 0.028(4) 0.024(4) 0.029(4) 0.000(3) -0.001(3) -0.003(3) O43 0.038(4) 0.013(4) 0.034(4) -0.002(3) -0.001(3) -0.011(3) O44 0.039(4) 0.022(4) 0.023(4) -0.005(3) 0.001(3) -0.002(3) O45 0.031(4) 0.018(4) 0.030(4) -0.004(3) 0.004(3) -0.006(3) O46 0.032(4) 0.027(4) 0.046(5) 0.001(4) 0.000(4) -0.007(3) O47 0.033(4) 0.027(4) 0.038(5) 0.000(3) 0.004(3) -0.005(3) O48 0.026(4) 0.034(4) 0.030(4) -0.006(3) 0.002(3) -0.009(3) O49 0.032(4) 0.024(4) 0.031(4) -0.001(3) -0.010(3) -0.010(3) O50 0.034(4) 0.037(5) 0.030(4) 0.000(4) 0.004(3) -0.004(4) O51 0.042(5) 0.027(4) 0.043(5) -0.005(4) 0.005(4) -0.012(4) OW1 0.046(5) 0.033(5) 0.042(5) -0.005(4) 0.008(4) -0.010(4) OW2 0.047(5) 0.029(5) 0.070(6) -0.002(4) -0.010(4) -0.006(4) OW3 0.065(6) 0.046(6) 0.059(6) -0.007(4) 0.001(5) -0.016(5) OW4 0.057(5) 0.037(5) 0.035(5) 0.001(4) 0.001(4) -0.009(4) OW5 0.114(8) 0.043(6) 0.035(5) -0.005(4) 0.005(5) 0.007(5) OW6 0.067(6) 0.025(5) 0.054(5) -0.003(4) 0.000(4) -0.002(4) OW7 0.057(5) 0.037(5) 0.049(5) -0.005(4) -0.013(4) -0.003(4) OW8 0.095(7) 0.035(5) 0.045(5) -0.005(4) -0.014(5) 0.004(5) OW9 0.044(5) 0.033(5) 0.064(6) -0.003(4) -0.012(4) -0.004(4) OW10 0.064(6) 0.045(5) 0.045(5) -0.013(4) 0.018(4) -0.012(4) OW11 0.043(5) 0.042(5) 0.047(5) -0.008(4) 0.003(4) -0.011(4) OW12 0.050(5) 0.032(5) 0.032(4) -0.002(4) -0.006(4) -0.003(4) OW13 0.071(7) 0.033(5) 0.116(9) -0.004(5) 0.013(6) -0.023(5) OW14 0.146(10) 0.044(6) 0.062(6) -0.020(5) -0.044(6) 0.006(6) OW15 0.066(6) 0.053(6) 0.062(6) 0.024(5) -0.023(5) -0.015(5) OW16 0.093(7) 0.045(6) 0.060(6) -0.009(5) 0.002(5) -0.028(5) OW17 0.046(5) 0.045(5) 0.049(5) -0.003(4) 0.001(4) -0.019(4) OW18 0.043(5) 0.038(5) 0.036(5) -0.001(4) -0.003(4) -0.004(4) OW19 0.043(5) 0.044(5) 0.043(5) -0.007(4) 0.007(4) -0.014(4) OW20 0.049(5) 0.041(5) 0.046(5) -0.001(4) 0.008(4) -0.007(4) OW21 0.053(5) 0.041(5) 0.061(6) -0.004(4) -0.005(4) -0.008(4) OW22 0.052(5) 0.057(6) 0.050(5) -0.011(4) -0.019(4) -0.001(4) OW23 0.055(5) 0.051(6) 0.056(6) -0.013(4) 0.001(4) -0.024(4) OW24 0.046(5) 0.067(6) 0.047(5) -0.004(4) -0.001(4) -0.017(4) OW25 0.046(6) 0.105(8) 0.074(7) 0.025(6) 0.007(5) -0.019(5) OW26 0.166(18) 0.38(3) 0.25(2) -0.20(2) -0.070(16) 0.025(19) OW27 0.142(13) 0.088(10) 0.211(17) -0.019(10) -0.051(12) -0.009(9) OW28 0.220(16) 0.092(9) 0.115(11) -0.034(8) 0.093(10) -0.078(10) OW29 0.29(3) 0.27(3) 0.31(3) -0.14(2) 0.12(2) -0.04(2) OW30 0.30(2) 0.127(13) 0.113(12) -0.042(10) -0.003(13) 0.070(14) OW31 0.75(7) 0.094(14) 0.37(4) -0.127(19) 0.07(4) -0.15(3) OW32 0.060(6) 0.059(6) 0.052(6) -0.014(5) 0.005(4) -0.013(5) OW33 0.043(5) 0.028(4) 0.040(5) -0.005(4) -0.004(4) -0.015(4) OW34 0.052(5) 0.037(5) 0.039(5) 0.000(4) 0.010(4) -0.010(4) OW35 0.050(5) 0.040(5) 0.050(5) 0.003(4) -0.008(4) 0.000(4) OW36 0.054(6) 0.056(6) 0.099(8) 0.007(5) -0.009(5) -0.021(5) OW37 0.056(6) 0.071(7) 0.067(6) 0.000(5) 0.008(5) -0.020(5) OW38 0.069(7) 0.124(10) 0.074(7) 0.032(7) -0.006(5) -0.053(6) OW39 0.099(8) 0.093(8) 0.077(8) -0.018(6) -0.032(6) -0.023(7) OW40 0.094(9) 0.096(9) 0.149(12) -0.038(8) -0.009(8) -0.012(7) OW41 0.109(10) 0.067(8) 0.32(2) -0.073(11) 0.140(12) -0.045(7) OW42 0.136(13) 0.28(2) 0.109(11) -0.018(12) 0.012(9) -0.098(13) OW43 0.28(3) 0.23(2) 0.189(19) -0.043(17) -0.026(18) 0.038(19) OW44 0.32(3) 0.128(13) 0.213(19) -0.058(13) -0.166(18) 0.068(15) OW45 0.37(3) 0.050(8) 0.118(11) -0.017(8) 0.096(14) -0.025(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Na OW29 2.31(3) 1_556 ? Na O8 2.374(9) . ? Na OW26 2.450(19) . ? Na OW30 2.453(18) 2_667 ? Na OW27 2.516(16) . ? Na OW28 2.521(14) . ? Na OW31 2.54(3) . ? Ca1 OW25 2.347(9) 1_554 ? Ca1 OW9 2.383(7) . ? Ca1 OW14 2.408(9) . ? Ca1 OW19 2.412(8) . ? Ca1 O15 2.434(7) 1_554 ? Ca1 O10 2.449(7) 1_554 ? Ca1 OW22 2.477(8) . ? Ca1 V11 3.503(3) 1_554 ? Ca2 OW12 2.388(7) . ? Ca2 O34 2.395(7) . ? Ca2 O48 2.403(7) . ? Ca2 OW21 2.440(8) 1_545 ? Ca2 OW24 2.459(8) . ? Ca2 OW18 2.484(7) . ? Ca2 OW2 2.490(8) . ? Ca2 O49 2.698(7) 1_545 ? Ca2 V12 4.076(3) 1_445 ? Ca2 V11 4.457(3) . ? Ca3 OW10 2.414(8) 1_655 ? Ca3 OW8 2.438(8) . ? Ca3 O27 2.447(7) 1_655 ? Ca3 O23 2.460(7) 1_655 ? Ca3 OW23 2.482(8) . ? Ca3 OW20 2.569(9) 1_655 ? Ca3 OW1 2.586(7) 2_756 ? Ca3 OW1 2.656(8) 1_655 ? Ca3 V9 3.572(3) 1_655 ? Ca3 Ca3 4.389(4) 2_856 ? Mg1 OW15 2.081(9) . ? Mg1 O24 2.091(8) . ? Mg1 OW3 2.113(9) . ? Mg1 OW16 2.136(9) . ? Mg1 OW4 2.169(8) . ? Mg1 OW11 2.211(8) . ? Mg2 O4 2.014(7) . ? Mg2 OW7 2.071(8) . ? Mg2 OW6 2.081(8) . ? Mg2 OW5 2.091(9) . ? Mg2 OW13 2.118(10) . ? Mg2 OW17 2.125(9) . ? As1 O1 1.805(7) . ? As1 O2 1.815(6) 1_455 ? As1 O3 1.818(6) . ? As1 V12 4.022(2) 1_445 ? As1 V11 4.036(2) . ? As1 V10 4.072(2) . ? As2 O4 1.664(7) . ? As2 O5 1.687(7) . ? As2 O6 1.689(7) . ? As2 O7 1.694(7) . ? As2 V10 3.204(2) . ? As3 O8 1.657(7) . ? As3 O9 1.686(7) . ? As3 O10 1.688(7) . ? As3 O11 1.707(7) . ? As3 V11 3.238(2) . ? As4 O12 1.638(7) 1_556 ? As4 O13 1.678(6) . ? As4 O14 1.689(6) 1_545 ? As4 O15 1.714(7) . ? As4 V11 3.214(2) . ? As5 O16 1.650(7) 1_645 ? As5 O17 1.688(7) 1_645 ? As5 O18 1.690(7) 1_545 ? As5 O19 1.707(7) 1_645 ? As5 V12 3.203(2) 1_545 ? As6 O20 1.660(6) 1_655 ? As6 O21 1.678(7) 1_665 ? As6 O22 1.687(7) 1_655 ? As6 O23 1.698(7) 1_665 ? As6 V12 3.242(2) . ? As7 O24 1.662(7) . ? As7 O25 1.668(7) . ? As7 O26 1.690(7) . ? As7 O27 1.700(6) . ? As7 V10 3.208(2) . ? V1 O31 1.596(7) . ? V1 O30 1.789(7) . ? V1 O7 1.970(7) . ? V1 O37 1.985(6) . ? V1 O3 2.033(7) . ? V1 O40 2.377(7) . ? V1 V2 3.058(3) . ? V1 V10 3.623(2) . ? V2 O32 1.587(7) . ? V2 O28 1.845(7) . ? V2 O11 1.979(7) . ? V2 O37 1.991(7) . ? V2 O3 2.053(6) . ? V2 O41 2.383(6) . ? V2 V11 3.584(2) . ? V3 O33 1.578(7) . ? V3 O28 1.754(7) . ? V3 O13 1.950(7) . ? V3 O38 2.035(7) . ? V3 O2 2.049(7) 1_455 ? V3 O42 2.346(7) . ? V3 V11 3.477(3) . ? V4 O34 1.598(7) . ? V4 O29 1.860(7) . ? V4 O18 1.987(7) 1_545 ? V4 O38 2.007(6) 1_655 ? V4 O2 2.053(6) . ? V4 O43 2.243(7) 1_655 ? V4 V12 3.495(2) 1_545 ? V5 O35 1.592(7) . ? V5 O29 1.761(7) . ? V5 O21 1.966(7) 1_655 ? V5 O39 2.012(7) 1_655 ? V5 O1 2.067(7) 1_655 ? V5 O44 2.382(7) 1_655 ? V5 V6 3.115(3) 1_655 ? V5 V12 3.556(2) 1_545 ? V6 O36 1.590(7) . ? V6 O30 1.824(7) . ? V6 O25 1.984(7) . ? V6 O39 2.000(6) . ? V6 O1 2.055(7) . ? V6 O45 2.449(7) . ? V6 V10 3.671(3) . ? V7 O46 1.587(7) . ? V7 O40 1.873(7) . ? V7 O41 1.881(7) . ? V7 O9 2.002(7) . ? V7 O6 2.016(7) . ? V7 O37 2.318(6) . ? V7 V10 3.423(2) . ? V7 V11 3.444(2) . ? V8 O48 1.607(7) . ? V8 O42 1.957(7) . ? V8 O43 1.991(7) . ? V8 O17 2.006(7) 1_545 ? V8 O14 2.009(7) 1_545 ? V8 O38 2.249(7) . ? V8 V12 3.451(2) 1_445 ? V8 V11 3.466(3) . ? V9 O50 1.589(7) . ? V9 O45 1.878(6) . ? V9 O44 1.905(7) . ? V9 O23 2.014(7) . ? V9 O27 2.033(7) . ? V9 O39 2.309(7) . ? V9 V10 3.425(2) . ? V9 V12 3.452(2) 1_445 ? V10 O51 1.589(7) . ? V10 O45 1.843(7) . ? V10 O40 1.857(7) . ? V10 O26 1.976(7) . ? V10 O5 2.000(7) . ? V10 O30 3.056(7) . ? V11 O47 1.584(7) . ? V11 O42 1.781(7) . ? V11 O41 1.839(6) . ? V11 O15 1.988(7) . ? V11 O10 2.048(7) . ? V11 O28 2.857(7) . ? V12 O49 1.595(7) 1_655 ? V12 O43 1.799(7) 1_665 ? V12 O44 1.827(6) 1_665 ? V12 O19 2.000(7) 1_655 ? V12 O22 2.025(7) 1_655 ? V12 O29 2.976(7) 1_565 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag OW29 Na O8 98.9(7) 1_556 . ? OW29 Na OW26 161.3(7) 1_556 . ? O8 Na OW26 88.0(7) . . ? OW29 Na OW30 79.0(8) 1_556 2_667 ? O8 Na OW30 73.3(4) . 2_667 ? OW26 Na OW30 86.5(8) . 2_667 ? OW29 Na OW27 83.1(8) 1_556 . ? O8 Na OW27 150.6(5) . . ? OW26 Na OW27 99.4(8) . . ? OW30 Na OW27 135.1(6) 2_667 . ? OW29 Na OW28 98.4(6) 1_556 . ? O8 Na OW28 137.4(4) . . ? OW26 Na OW28 65.7(6) . . ? OW30 Na OW28 72.3(4) 2_667 . ? OW27 Na OW28 70.1(5) . . ? OW29 Na OW31 104.8(11) 1_556 . ? O8 Na OW31 87.9(5) . . ? OW26 Na OW31 92.8(10) . . ? OW30 Na OW31 161.2(6) 2_667 . ? OW27 Na OW31 63.5(6) . . ? OW28 Na OW31 124.3(7) . . ? OW25 Ca1 OW9 80.9(3) 1_554 . ? OW25 Ca1 OW14 95.0(4) 1_554 . ? OW9 Ca1 OW14 152.7(3) . . ? OW25 Ca1 OW19 164.1(3) 1_554 . ? OW9 Ca1 OW19 92.2(3) . . ? OW14 Ca1 OW19 84.5(3) . . ? OW25 Ca1 O15 113.4(3) 1_554 1_554 ? OW9 Ca1 O15 80.1(3) . 1_554 ? OW14 Ca1 O15 125.4(3) . 1_554 ? OW19 Ca1 O15 79.1(3) . 1_554 ? OW25 Ca1 O10 83.8(3) 1_554 1_554 ? OW9 Ca1 O10 126.7(3) . 1_554 ? OW14 Ca1 O10 79.1(3) . 1_554 ? OW19 Ca1 O10 111.6(3) . 1_554 ? O15 Ca1 O10 60.3(2) 1_554 1_554 ? OW25 Ca1 OW22 82.2(3) 1_554 . ? OW9 Ca1 OW22 77.4(3) . . ? OW14 Ca1 OW22 75.3(3) . . ? OW19 Ca1 OW22 82.4(3) . . ? O15 Ca1 OW22 150.2(3) 1_554 . ? O10 Ca1 OW22 149.4(3) 1_554 . ? OW25 Ca1 V11 85.5(3) 1_554 1_554 ? OW9 Ca1 V11 93.0(2) . 1_554 ? OW14 Ca1 V11 113.7(2) . 1_554 ? OW19 Ca1 V11 109.3(2) . 1_554 ? O15 Ca1 V11 33.36(16) 1_554 1_554 ? O10 Ca1 V11 34.90(16) 1_554 1_554 ? OW22 Ca1 V11 165.4(2) . 1_554 ? OW12 Ca2 O34 136.7(3) . . ? OW12 Ca2 O48 82.1(3) . . ? O34 Ca2 O48 138.7(2) . . ? OW12 Ca2 OW21 139.2(3) . 1_545 ? O34 Ca2 OW21 75.0(3) . 1_545 ? O48 Ca2 OW21 80.7(3) . 1_545 ? OW12 Ca2 OW24 83.9(3) . . ? O34 Ca2 OW24 74.0(3) . . ? O48 Ca2 OW24 135.6(3) . . ? OW21 Ca2 OW24 83.2(3) 1_545 . ? OW12 Ca2 OW18 119.8(2) . . ? O34 Ca2 OW18 74.4(2) . . ? O48 Ca2 OW18 72.4(2) . . ? OW21 Ca2 OW18 89.3(3) 1_545 . ? OW24 Ca2 OW18 148.4(3) . . ? OW12 Ca2 OW2 70.7(3) . . ? O34 Ca2 OW2 70.5(2) . . ? O48 Ca2 OW2 129.2(3) . . ? OW21 Ca2 OW2 145.2(3) 1_545 . ? OW24 Ca2 OW2 84.0(3) . . ? OW18 Ca2 OW2 84.9(3) . . ? OW12 Ca2 O49 68.4(2) . 1_545 ? O34 Ca2 O49 130.5(2) . 1_545 ? O48 Ca2 O49 68.3(2) . 1_545 ? OW21 Ca2 O49 70.9(2) 1_545 1_545 ? OW24 Ca2 O49 67.4(2) . 1_545 ? OW18 Ca2 O49 138.2(3) . 1_545 ? OW2 Ca2 O49 131.7(2) . 1_545 ? OW12 Ca2 V12 59.74(19) . 1_445 ? O34 Ca2 V12 144.36(19) . 1_445 ? O48 Ca2 V12 58.15(17) . 1_445 ? OW21 Ca2 V12 79.8(2) 1_545 1_445 ? OW24 Ca2 V12 78.4(2) . 1_445 ? OW18 Ca2 V12 130.41(19) . 1_445 ? OW2 Ca2 V12 128.58(19) . 1_445 ? O49 Ca2 V12 13.92(14) 1_545 1_445 ? OW12 Ca2 V11 53.08(17) . . ? O34 Ca2 V11 130.81(19) . . ? O48 Ca2 V11 54.00(17) . . ? OW21 Ca2 V11 133.2(2) 1_545 . ? OW24 Ca2 V11 136.3(2) . . ? OW18 Ca2 V11 68.07(17) . . ? OW2 Ca2 V11 75.51(19) . . ? O49 Ca2 V11 98.70(15) 1_545 . ? V12 Ca2 V11 84.82(5) 1_445 . ? OW10 Ca3 OW8 76.9(3) 1_655 . ? OW10 Ca3 O27 147.5(3) 1_655 1_655 ? OW8 Ca3 O27 75.5(2) . 1_655 ? OW10 Ca3 O23 148.6(3) 1_655 1_655 ? OW8 Ca3 O23 122.5(3) . 1_655 ? O27 Ca3 O23 63.3(2) 1_655 1_655 ? OW10 Ca3 OW23 79.9(3) 1_655 . ? OW8 Ca3 OW23 73.4(3) . . ? O27 Ca3 OW23 108.0(3) 1_655 . ? O23 Ca3 OW23 82.7(3) 1_655 . ? OW10 Ca3 OW20 78.1(3) 1_655 1_655 ? OW8 Ca3 OW20 80.1(3) . 1_655 ? O27 Ca3 OW20 80.5(2) 1_655 1_655 ? O23 Ca3 OW20 126.4(3) 1_655 1_655 ? OW23 Ca3 OW20 148.8(3) . 1_655 ? OW10 Ca3 OW1 73.9(3) 1_655 2_756 ? OW8 Ca3 OW1 140.6(3) . 2_756 ? O27 Ca3 OW1 138.4(2) 1_655 2_756 ? O23 Ca3 OW1 76.5(2) 1_655 2_756 ? OW23 Ca3 OW1 75.8(3) . 2_756 ? OW20 Ca3 OW1 118.2(2) 1_655 2_756 ? OW10 Ca3 OW1 101.8(3) 1_655 1_655 ? OW8 Ca3 OW1 146.8(3) . 1_655 ? O27 Ca3 OW1 92.2(2) 1_655 1_655 ? O23 Ca3 OW1 75.5(2) 1_655 1_655 ? OW23 Ca3 OW1 139.6(3) . 1_655 ? OW20 Ca3 OW1 67.3(2) 1_655 1_655 ? OW1 Ca3 OW1 66.3(3) 2_756 1_655 ? OW10 Ca3 V9 174.4(2) 1_655 1_655 ? OW8 Ca3 V9 106.3(2) . 1_655 ? O27 Ca3 V9 33.28(15) 1_655 1_655 ? O23 Ca3 V9 32.92(16) 1_655 1_655 ? OW23 Ca3 V9 105.3(2) . 1_655 ? OW20 Ca3 V9 97.85(18) 1_655 1_655 ? OW1 Ca3 V9 105.10(17) 2_756 1_655 ? OW1 Ca3 V9 73.03(16) 1_655 1_655 ? OW10 Ca3 Ca3 87.7(2) 1_655 2_856 ? OW8 Ca3 Ca3 164.0(2) . 2_856 ? O27 Ca3 Ca3 117.60(18) 1_655 2_856 ? O23 Ca3 Ca3 73.25(16) 1_655 2_856 ? OW23 Ca3 Ca3 108.4(2) . 2_856 ? OW20 Ca3 Ca3 92.60(18) 1_655 2_856 ? OW1 Ca3 Ca3 33.64(17) 2_756 2_856 ? OW1 Ca3 Ca3 32.65(16) 1_655 2_856 ? V9 Ca3 Ca3 88.68(7) 1_655 2_856 ? OW15 Mg1 O24 90.9(3) . . ? OW15 Mg1 OW3 90.8(4) . . ? O24 Mg1 OW3 177.6(4) . . ? OW15 Mg1 OW16 101.4(4) . . ? O24 Mg1 OW16 88.1(3) . . ? OW3 Mg1 OW16 89.9(3) . . ? OW15 Mg1 OW4 87.2(3) . . ? O24 Mg1 OW4 93.7(3) . . ? OW3 Mg1 OW4 88.0(3) . . ? OW16 Mg1 OW4 171.2(4) . . ? OW15 Mg1 OW11 172.2(4) . . ? O24 Mg1 OW11 93.0(3) . . ? OW3 Mg1 OW11 85.5(3) . . ? OW16 Mg1 OW11 85.5(3) . . ? OW4 Mg1 OW11 85.8(3) . . ? O4 Mg2 OW7 88.6(3) . . ? O4 Mg2 OW6 174.9(4) . . ? OW7 Mg2 OW6 88.7(3) . . ? O4 Mg2 OW5 93.2(3) . . ? OW7 Mg2 OW5 178.0(4) . . ? OW6 Mg2 OW5 89.6(3) . . ? O4 Mg2 OW13 92.9(3) . . ? OW7 Mg2 OW13 88.7(4) . . ? OW6 Mg2 OW13 91.3(4) . . ? OW5 Mg2 OW13 90.3(4) . . ? O4 Mg2 OW17 87.2(3) . . ? OW7 Mg2 OW17 93.0(3) . . ? OW6 Mg2 OW17 88.6(3) . . ? OW5 Mg2 OW17 88.0(4) . . ? OW13 Mg2 OW17 178.3(4) . . ? O1 As1 O2 97.9(3) . 1_455 ? O1 As1 O3 97.5(3) . . ? O2 As1 O3 98.6(3) 1_455 . ? O1 As1 V12 85.6(2) . 1_445 ? O2 As1 V12 84.5(2) 1_455 1_445 ? O3 As1 V12 175.3(2) . 1_445 ? O1 As1 V11 176.4(2) . . ? O2 As1 V11 83.7(2) 1_455 . ? O3 As1 V11 85.5(2) . . ? V12 As1 V11 91.28(4) 1_445 . ? O1 As1 V10 87.2(2) . . ? O2 As1 V10 173.4(2) 1_455 . ? O3 As1 V10 85.0(2) . . ? V12 As1 V10 91.64(4) 1_445 . ? V11 As1 V10 91.06(4) . . ? O4 As2 O5 108.1(3) . . ? O4 As2 O6 110.9(3) . . ? O5 As2 O6 110.2(3) . . ? O4 As2 O7 108.8(3) . . ? O5 As2 O7 108.7(4) . . ? O6 As2 O7 110.2(3) . . ? O4 As2 V10 140.5(2) . . ? O5 As2 V10 32.6(2) . . ? O6 As2 V10 93.8(2) . . ? O7 As2 V10 89.6(2) . . ? O8 As3 O9 109.5(4) . . ? O8 As3 O10 110.1(3) . . ? O9 As3 O10 109.6(3) . . ? O8 As3 O11 109.7(4) . . ? O9 As3 O11 110.4(3) . . ? O10 As3 O11 107.5(4) . . ? O8 As3 V11 143.3(2) . . ? O9 As3 V11 92.7(2) . . ? O10 As3 V11 33.3(2) . . ? O11 As3 V11 88.0(2) . . ? O12 As4 O13 109.9(3) 1_556 . ? O12 As4 O14 113.7(3) 1_556 1_545 ? O13 As4 O14 109.9(3) . 1_545 ? O12 As4 O15 107.4(3) 1_556 . ? O13 As4 O15 106.3(3) . . ? O14 As4 O15 109.2(3) 1_545 . ? O12 As4 V11 139.5(3) 1_556 . ? O13 As4 V11 87.6(2) . . ? O14 As4 V11 92.2(2) 1_545 . ? O15 As4 V11 32.3(2) . . ? O16 As5 O17 108.6(3) 1_645 1_645 ? O16 As5 O18 111.9(4) 1_645 1_545 ? O17 As5 O18 110.4(3) 1_645 1_545 ? O16 As5 O19 109.1(3) 1_645 1_645 ? O17 As5 O19 108.9(3) 1_645 1_645 ? O18 As5 O19 107.8(3) 1_545 1_645 ? O16 As5 V12 142.1(2) 1_645 1_545 ? O17 As5 V12 92.8(2) 1_645 1_545 ? O18 As5 V12 87.9(2) 1_545 1_545 ? O19 As5 V12 33.0(2) 1_645 1_545 ? O20 As6 O21 113.0(4) 1_655 1_665 ? O20 As6 O22 108.5(3) 1_655 1_655 ? O21 As6 O22 108.8(3) 1_665 1_655 ? O20 As6 O23 107.4(3) 1_655 1_665 ? O21 As6 O23 108.8(3) 1_665 1_665 ? O22 As6 O23 110.3(3) 1_655 1_665 ? O20 As6 V12 140.7(2) 1_655 . ? O21 As6 V12 88.7(2) 1_665 . ? O22 As6 V12 32.2(2) 1_655 . ? O23 As6 V12 94.8(2) 1_665 . ? O24 As7 O25 110.6(3) . . ? O24 As7 O26 107.7(3) . . ? O25 As7 O26 109.2(4) . . ? O24 As7 O27 110.8(3) . . ? O25 As7 O27 110.1(3) . . ? O26 As7 O27 108.5(3) . . ? O24 As7 V10 138.9(3) . . ? O25 As7 V10 88.9(3) . . ? O26 As7 V10 31.5(2) . . ? O27 As7 V10 94.5(2) . . ? O31 V1 O30 103.3(4) . . ? O31 V1 O7 96.0(3) . . ? O30 V1 O7 96.0(3) . . ? O31 V1 O37 101.5(3) . . ? O30 V1 O37 154.4(3) . . ? O7 V1 O37 87.7(3) . . ? O31 V1 O3 99.8(3) . . ? O30 V1 O3 91.0(3) . . ? O7 V1 O3 160.7(3) . . ? O37 V1 O3 78.5(3) . . ? O31 V1 O40 175.0(3) . . ? O30 V1 O40 81.3(3) . . ? O7 V1 O40 81.4(3) . . ? O37 V1 O40 74.1(2) . . ? O3 V1 O40 82.0(2) . . ? O31 V1 V2 91.6(3) . . ? O30 V1 V2 132.6(2) . . ? O7 V1 V2 127.3(2) . . ? O37 V1 V2 39.79(19) . . ? O3 V1 V2 41.78(18) . . ? O40 V1 V2 86.58(17) . . ? O31 V1 V10 155.9(3) . . ? O30 V1 V10 57.4(2) . . ? O7 V1 V10 73.9(2) . . ? O37 V1 V10 99.96(19) . . ? O3 V1 V10 95.19(18) . . ? O40 V1 V10 27.14(16) . . ? V2 V1 V10 112.03(6) . . ? O32 V2 O28 103.6(4) . . ? O32 V2 O11 97.2(3) . . ? O28 V2 O11 93.3(3) . . ? O32 V2 O37 104.9(3) . . ? O28 V2 O37 151.2(3) . . ? O11 V2 O37 87.7(3) . . ? O32 V2 O3 98.7(3) . . ? O28 V2 O3 93.4(3) . . ? O11 V2 O3 160.8(3) . . ? O37 V2 O3 77.8(3) . . ? O32 V2 O41 178.5(3) . . ? O28 V2 O41 77.4(3) . . ? O11 V2 O41 81.6(3) . . ? O37 V2 O41 74.3(2) . . ? O3 V2 O41 82.3(2) . . ? O32 V2 V1 93.2(3) . . ? O28 V2 V1 134.0(2) . . ? O11 V2 V1 127.1(2) . . ? O37 V2 V1 39.65(18) . . ? O3 V2 V1 41.28(18) . . ? O41 V2 V1 86.82(16) . . ? O32 V2 V11 152.9(3) . . ? O28 V2 V11 52.3(2) . . ? O11 V2 V11 74.7(2) . . ? O37 V2 V11 100.70(19) . . ? O3 V2 V11 95.40(17) . . ? O41 V2 V11 27.57(16) . . ? V1 V2 V11 112.46(7) . . ? O33 V3 O28 103.3(4) . . ? O33 V3 O13 97.4(3) . . ? O28 V3 O13 98.3(3) . . ? O33 V3 O38 103.1(3) . . ? O28 V3 O38 153.0(3) . . ? O13 V3 O38 83.9(3) . . ? O33 V3 O2 97.0(3) . 1_455 ? O28 V3 O2 94.4(3) . 1_455 ? O13 V3 O2 158.1(3) . 1_455 ? O38 V3 O2 76.8(3) . 1_455 ? O33 V3 O42 176.8(3) . . ? O28 V3 O42 79.9(3) . . ? O13 V3 O42 82.2(3) . . ? O38 V3 O42 73.7(3) . . ? O2 V3 O42 82.5(2) 1_455 . ? O33 V3 V11 155.1(3) . . ? O28 V3 V11 54.9(2) . . ? O13 V3 V11 76.4(2) . . ? O38 V3 V11 100.19(19) . . ? O2 V3 V11 96.8(2) 1_455 . ? O42 V3 V11 27.89(17) . . ? O34 V4 O29 102.0(3) . . ? O34 V4 O18 94.1(3) . 1_545 ? O29 V4 O18 95.5(3) . 1_545 ? O34 V4 O38 100.2(3) . 1_655 ? O29 V4 O38 156.7(3) . 1_655 ? O18 V4 O38 89.7(3) 1_545 1_655 ? O34 V4 O2 98.4(3) . . ? O29 V4 O2 92.6(3) . . ? O18 V4 O2 163.4(3) 1_545 . ? O38 V4 O2 77.4(3) 1_655 . ? O34 V4 O43 175.6(3) . 1_655 ? O29 V4 O43 82.0(3) . 1_655 ? O18 V4 O43 83.6(3) 1_545 1_655 ? O38 V4 O43 76.1(3) 1_655 1_655 ? O2 V4 O43 83.2(2) . 1_655 ? O34 V4 V12 155.9(3) . 1_545 ? O29 V4 V12 58.4(2) . 1_545 ? O18 V4 V12 75.6(2) 1_545 1_545 ? O38 V4 V12 101.52(19) 1_655 1_545 ? O2 V4 V12 96.54(19) . 1_545 ? O43 V4 V12 26.66(17) 1_655 1_545 ? O35 V5 O29 104.1(4) . . ? O35 V5 O21 96.7(3) . 1_655 ? O29 V5 O21 98.9(3) . 1_655 ? O35 V5 O39 100.9(3) . 1_655 ? O29 V5 O39 153.9(3) . 1_655 ? O21 V5 O39 85.7(3) 1_655 1_655 ? O35 V5 O1 98.5(3) . 1_655 ? O29 V5 O1 92.4(3) . 1_655 ? O21 V5 O1 158.4(3) 1_655 1_655 ? O39 V5 O1 76.4(3) 1_655 1_655 ? O35 V5 O44 174.6(3) . 1_655 ? O29 V5 O44 81.3(3) . 1_655 ? O21 V5 O44 81.9(3) 1_655 1_655 ? O39 V5 O44 73.8(2) 1_655 1_655 ? O1 V5 O44 81.6(2) 1_655 1_655 ? O35 V5 V6 90.1(3) . 1_655 ? O29 V5 V6 132.9(2) . 1_655 ? O21 V5 V6 124.2(2) 1_655 1_655 ? O39 V5 V6 38.91(18) 1_655 1_655 ? O1 V5 V6 40.75(18) 1_655 1_655 ? O44 V5 V6 86.50(17) 1_655 1_655 ? O35 V5 V12 156.7(3) . 1_545 ? O29 V5 V12 56.6(2) . 1_545 ? O21 V5 V12 75.8(2) 1_655 1_545 ? O39 V5 V12 100.45(19) 1_655 1_545 ? O1 V5 V12 95.51(19) 1_655 1_545 ? O44 V5 V12 27.83(16) 1_655 1_545 ? V6 V5 V12 112.53(7) 1_655 1_545 ? O36 V6 O30 104.9(3) . . ? O36 V6 O25 97.4(3) . . ? O30 V6 O25 94.7(3) . . ? O36 V6 O39 102.9(3) . . ? O30 V6 O39 151.6(3) . . ? O25 V6 O39 86.9(3) . . ? O36 V6 O1 100.8(3) . . ? O30 V6 O1 92.6(3) . . ? O25 V6 O1 157.9(3) . . ? O39 V6 O1 76.9(3) . . ? O36 V6 O45 174.7(3) . . ? O30 V6 O45 79.6(3) . . ? O25 V6 O45 79.2(3) . . ? O39 V6 O45 72.9(2) . . ? O1 V6 O45 81.7(2) . . ? O36 V6 V5 92.8(3) . 1_455 ? O30 V6 V5 133.3(2) . 1_455 ? O25 V6 V5 125.9(2) . 1_455 ? O39 V6 V5 39.20(19) . 1_455 ? O1 V6 V5 41.05(19) . 1_455 ? O45 V6 V5 85.99(16) . 1_455 ? O36 V6 V10 155.8(3) . . ? O30 V6 V10 56.1(2) . . ? O25 V6 V10 71.8(2) . . ? O39 V6 V10 98.2(2) . . ? O1 V6 V10 95.4(2) . . ? O45 V6 V10 26.60(15) . . ? V5 V6 V10 111.15(6) 1_455 . ? O46 V7 O40 102.2(3) . . ? O46 V7 O41 101.6(3) . . ? O40 V7 O41 95.7(3) . . ? O46 V7 O9 98.9(3) . . ? O40 V7 O9 157.7(3) . . ? O41 V7 O9 87.1(3) . . ? O46 V7 O6 99.5(3) . . ? O40 V7 O6 87.8(3) . . ? O41 V7 O6 157.3(3) . . ? O9 V7 O6 81.5(3) . . ? O46 V7 O37 179.3(3) . . ? O40 V7 O37 77.6(3) . . ? O41 V7 O37 77.8(2) . . ? O9 V7 O37 81.4(3) . . ? O6 V7 O37 81.1(3) . . ? O46 V7 V10 80.9(3) . . ? O40 V7 V10 23.3(2) . . ? O41 V7 V10 109.5(2) . . ? O9 V7 V10 163.2(2) . . ? O6 V7 V10 81.91(19) . . ? O37 V7 V10 98.95(16) . . ? O46 V7 V11 81.5(3) . . ? O40 V7 V11 108.7(2) . . ? O41 V7 V11 21.96(19) . . ? O9 V7 V11 81.6(2) . . ? O6 V7 V11 163.0(2) . . ? O37 V7 V11 98.01(17) . . ? V10 V7 V11 114.86(7) . . ? O48 V8 O42 99.6(3) . . ? O48 V8 O43 98.0(3) . . ? O42 V8 O43 92.7(3) . . ? O48 V8 O17 99.0(3) . 1_545 ? O42 V8 O17 161.2(3) . 1_545 ? O43 V8 O17 87.0(3) . 1_545 ? O48 V8 O14 101.2(3) . 1_545 ? O42 V8 O14 87.4(3) . 1_545 ? O43 V8 O14 160.5(3) . 1_545 ? O17 V8 O14 86.7(3) 1_545 1_545 ? O48 V8 O38 173.3(3) . . ? O42 V8 O38 77.4(3) . . ? O43 V8 O38 76.3(3) . . ? O17 V8 O38 84.3(3) 1_545 . ? O14 V8 O38 84.7(2) 1_545 . ? O48 V8 V12 77.3(2) . 1_445 ? O42 V8 V12 106.0(2) . 1_445 ? O43 V8 V12 23.12(19) . 1_445 ? O17 V8 V12 80.4(2) 1_545 1_445 ? O14 V8 V12 166.6(2) 1_545 1_445 ? O38 V8 V12 97.70(17) . 1_445 ? O48 V8 V11 82.0(3) . . ? O42 V8 V11 20.92(19) . . ? O43 V8 V11 106.24(19) . . ? O17 V8 V11 166.5(2) 1_545 . ? O14 V8 V11 79.9(2) 1_545 . ? O38 V8 V11 96.11(18) . . ? V12 V8 V11 112.79(6) 1_445 . ? O50 V9 O45 102.2(3) . . ? O50 V9 O44 102.9(3) . . ? O45 V9 O44 95.5(3) . . ? O50 V9 O23 97.8(3) . . ? O45 V9 O23 158.0(3) . . ? O44 V9 O23 89.1(3) . . ? O50 V9 O27 98.0(3) . . ? O45 V9 O27 88.9(3) . . ? O44 V9 O27 157.2(3) . . ? O23 V9 O27 79.1(3) . . ? O50 V9 O39 179.3(3) . . ? O45 V9 O39 78.4(3) . . ? O44 V9 O39 77.5(3) . . ? O23 V9 O39 81.6(3) . . ? O27 V9 O39 81.5(3) . . ? O50 V9 V10 81.4(3) . . ? O45 V9 V10 22.8(2) . . ? O44 V9 V10 109.4(2) . . ? O23 V9 V10 161.2(2) . . ? O27 V9 V10 82.5(2) . . ? O39 V9 V10 99.10(17) . . ? O50 V9 V12 82.9(3) . 1_445 ? O45 V9 V12 108.4(2) . 1_445 ? O44 V9 V12 21.85(19) . 1_445 ? O23 V9 V12 83.15(19) . 1_445 ? O27 V9 V12 162.2(2) . 1_445 ? O39 V9 V12 97.38(17) . 1_445 ? V10 V9 V12 115.18(6) . 1_445 ? O50 V9 Ca3 86.6(3) . 1_455 ? O45 V9 Ca3 130.2(2) . 1_455 ? O44 V9 Ca3 130.7(2) . 1_455 ? O23 V9 Ca3 41.6(2) . 1_455 ? O27 V9 Ca3 41.35(18) . 1_455 ? O39 V9 Ca3 92.69(17) . 1_455 ? V10 V9 Ca3 119.87(7) . 1_455 ? V12 V9 Ca3 121.35(7) 1_445 1_455 ? O51 V10 O45 104.6(3) . . ? O51 V10 O40 105.6(3) . . ? O45 V10 O40 97.1(3) . . ? O51 V10 O26 101.5(3) . . ? O45 V10 O26 85.9(3) . . ? O40 V10 O26 151.0(3) . . ? O51 V10 O5 102.6(3) . . ? O45 V10 O5 150.6(3) . . ? O40 V10 O5 86.0(3) . . ? O26 V10 O5 78.0(3) . . ? O51 V10 O30 160.0(3) . . ? O45 V10 O30 63.5(2) . . ? O40 V10 O30 62.6(2) . . ? O26 V10 O30 93.9(2) . . ? O5 V10 O30 93.0(2) . . ? O47 V11 O42 105.3(3) . . ? O47 V11 O41 104.6(3) . . ? O42 V11 O41 100.3(3) . . ? O47 V11 O15 100.8(3) . . ? O42 V11 O15 88.0(3) . . ? O41 V11 O15 149.9(3) . . ? O47 V11 O10 99.2(3) . . ? O42 V11 O10 152.3(3) . . ? O41 V11 O10 85.5(3) . . ? O15 V11 O10 74.8(3) . . ? O47 V11 O28 163.5(3) . . ? O42 V11 O28 65.7(2) . . ? O41 V11 O28 65.4(2) . . ? O15 V11 O28 92.9(2) . . ? O10 V11 O28 93.2(2) . . ? O49 V12 O43 104.6(3) 1_655 1_665 ? O49 V12 O44 105.3(3) 1_655 1_665 ? O43 V12 O44 98.3(3) 1_665 1_665 ? O49 V12 O19 99.2(3) 1_655 1_655 ? O43 V12 O19 88.1(3) 1_665 1_655 ? O44 V12 O19 152.0(3) 1_665 1_655 ? O49 V12 O22 101.5(3) 1_655 1_655 ? O43 V12 O22 151.6(3) 1_665 1_655 ? O44 V12 O22 85.2(3) 1_665 1_655 ? O19 V12 O22 76.8(3) 1_655 1_655 ? O49 V12 O29 161.2(3) 1_655 1_565 ? O43 V12 O29 63.6(3) 1_665 1_565 ? O44 V12 O29 64.5(3) 1_665 1_565 ? O19 V12 O29 95.1(3) 1_655 1_565 ? O22 V12 O29 93.6(2) 1_655 1_565 ? As1 O1 V6 122.1(4) . . ? As1 O1 V5 123.0(3) . 1_455 ? V6 O1 V5 98.2(3) . 1_455 ? As1 O2 V3 122.5(4) 1_655 1_655 ? As1 O2 V4 122.4(3) 1_655 . ? V3 O2 V4 99.3(3) 1_655 . ? As1 O3 V1 124.3(3) . . ? As1 O3 V2 123.0(3) . . ? V1 O3 V2 96.9(3) . . ? As2 O4 Mg2 134.1(4) . . ? As2 O5 V10 120.4(4) . . ? As2 O6 V7 118.0(4) . . ? As2 O6 V10 59.25(19) . . ? V7 O6 V10 65.64(18) . . ? As2 O7 V1 124.4(4) . . ? As2 O7 V10 62.5(2) . . ? V1 O7 V10 74.5(2) . . ? As3 O8 Na 127.3(4) . . ? As3 O9 V7 119.9(4) . . ? As3 O9 V11 60.4(2) . . ? V7 O9 V11 66.28(19) . . ? As3 O10 V11 119.9(4) . . ? As3 O10 Ca1 138.2(4) . 1_556 ? V11 O10 Ca1 101.9(3) . 1_556 ? As3 O11 V2 124.1(4) . . ? As3 O11 V11 63.8(2) . . ? V2 O11 V11 73.4(2) . . ? As4 O13 V3 126.7(4) . . ? As4 O13 V11 64.3(2) . . ? V3 O13 V11 71.5(2) . . ? As4 O14 V8 119.4(3) 1_565 1_565 ? As4 O14 V11 60.5(2) 1_565 1_565 ? V8 O14 V11 67.69(18) 1_565 1_565 ? As4 O15 V11 120.3(4) . . ? As4 O15 Ca1 135.2(4) . 1_556 ? V11 O15 Ca1 104.3(3) . 1_556 ? As5 O17 V8 120.1(3) 1_465 1_565 ? As5 O17 V12 60.03(19) 1_465 1_455 ? V8 O17 V12 67.16(18) 1_565 1_455 ? As5 O18 V4 122.8(4) 1_565 1_565 ? As5 O18 V12 63.8(2) 1_565 . ? V4 O18 V12 71.7(2) 1_565 . ? As5 O19 V12 119.3(4) 1_465 1_455 ? As6 O21 V5 125.5(4) 1_445 1_455 ? As6 O21 V12 63.6(2) 1_445 1_445 ? V5 O21 V12 72.4(2) 1_455 1_445 ? As6 O22 V12 121.4(4) 1_455 1_455 ? As6 O23 V9 117.4(4) 1_445 . ? As6 O23 Ca3 136.8(4) 1_445 1_455 ? V9 O23 Ca3 105.5(3) . 1_455 ? As6 O23 V12 58.6(2) 1_445 1_445 ? V9 O23 V12 64.94(18) . 1_445 ? Ca3 O23 V12 157.0(3) 1_455 1_445 ? As7 O24 Mg1 130.2(4) . . ? As7 O25 V6 127.4(4) . . ? As7 O25 V10 63.4(2) . . ? V6 O25 V10 76.5(2) . . ? As7 O26 V10 121.9(4) . . ? As7 O27 V9 116.7(3) . . ? As7 O27 Ca3 137.7(3) . 1_455 ? V9 O27 Ca3 105.4(3) . 1_455 ? As7 O27 V10 58.61(19) . . ? V9 O27 V10 65.00(18) . . ? Ca3 O27 V10 155.2(3) 1_455 . ? V3 O28 V2 150.3(4) . . ? V3 O28 V11 94.9(3) . . ? V2 O28 V11 97.0(3) . . ? V5 O29 V4 152.9(4) . . ? V5 O29 V12 93.8(3) . 1_545 ? V4 O29 V12 89.5(3) . 1_545 ? V1 O30 V6 153.5(4) . . ? V1 O30 V10 93.1(3) . . ? V6 O30 V10 94.2(3) . . ? V4 O34 Ca2 167.2(4) . . ? V1 O37 V2 100.6(3) . . ? V1 O37 V7 103.3(3) . . ? V2 O37 V7 103.3(3) . . ? V4 O38 V3 101.3(3) 1_455 . ? V4 O38 V8 103.2(3) 1_455 . ? V3 O38 V8 104.8(3) . . ? V6 O39 V5 101.9(3) . 1_455 ? V6 O39 V9 104.8(3) . . ? V5 O39 V9 103.8(3) 1_455 . ? V10 O40 V7 133.1(4) . . ? V10 O40 V1 117.1(3) . . ? V7 O40 V1 104.8(3) . . ? V11 O41 V7 135.6(4) . . ? V11 O41 V2 115.6(3) . . ? V7 O41 V2 104.5(3) . . ? V11 O42 V8 136.0(4) . . ? V11 O42 V3 114.1(3) . . ? V8 O42 V3 103.9(3) . . ? V12 O43 V8 131.1(4) 1_445 . ? V12 O43 V4 119.3(3) 1_445 1_455 ? V8 O43 V4 103.9(3) . 1_455 ? V12 O44 V9 135.3(4) 1_445 . ? V12 O44 V5 114.7(3) 1_445 1_455 ? V9 O44 V5 104.6(3) . 1_455 ? V10 O45 V9 133.9(4) . . ? V10 O45 V6 116.9(3) . . ? V9 O45 V6 103.6(3) . . ? V7 O46 V10 72.8(3) . . ? V7 O46 V11 72.4(3) . . ? V10 O46 V11 109.0(2) . . ? V8 O48 Ca2 150.8(4) . . ? V8 O48 V12 75.9(2) . 1_445 ? Ca2 O48 V12 85.84(19) . 1_445 ? V8 O48 V11 71.9(2) . . ? Ca2 O48 V11 93.4(2) . . ? V12 O48 V11 108.84(18) 1_445 . ? V12 O49 Ca2 142.1(4) 1_455 1_565 ? V9 O50 V10 72.3(2) . . ? V9 O50 V12 71.3(2) . 1_445 ? V10 O50 V12 108.12(17) . 1_445 ? Ca3 OW1 Ca3 113.7(3) 2_756 1_455 ? Mg1 OW3 V10 148.1(3) . 2_666 ? Mg1 OW4 V10 118.2(3) . . ? Mg2 OW6 V12 135.8(3) . 1_455 ? Ca3 OW10 V12 146.4(3) 1_455 2_766 ? Ca2 OW12 V12 84.6(2) . 1_445 ? Ca2 OW12 V10 145.5(3) . . ? V12 OW12 V10 110.27(19) 1_445 . ? Ca2 OW12 V11 94.6(2) . . ? V12 OW12 V11 108.2(2) 1_445 . ? V10 OW12 V11 108.86(18) . . ? Ca1 OW25 V11 59.3(2) 1_556 . ? _refine_diff_density_max 1.187 _refine_diff_density_min -0.895 _refine_diff_density_rms 0.163 _shelx_res_file ; TITL TRPR2 trpr2.res created by SHELXL-2016/6 at 13:31:46 on 21-Jul-2018 CELL 0.71075 10.34900 17.62630 23.25560 82.20820 88.35070 81.70200 ZERR 2 0.00046 0.00092 0.00163 0.00580 0.00620 0.00580 LATT 1 SFAC AS CA O V MG NA H UNIT 14 6.38 192 24 4 1.62 180 L.S. 10 CONN 6 3.05 V10 CONN 6 3.05 V11 CONN 6 3.05 V12 omit 2 -3 2 omit 5 1 0 omit 8 3 3 omit 7 1 2 omit 4 9 22 omit -5 -10 16 omit -7 11 1 omit -2 12 19 EXYZ NA CA EADP NA CA FMAP 2 PLAN 30 HTAB BOND $H ACTA SIZE 0.180 0.080 0.030 WGHT 0.082500 6.146100 FVAR 0.16381 0.81206 NA 6 0.234685 0.559375 0.963623 21.00000 0.16213 0.05287 = 0.07446 -0.01760 0.00607 -0.03986 CA 2 0.234685 0.559375 0.963623 -21.00000 0.16213 0.05287 = 0.07446 -0.01760 0.00607 -0.03986 CA1 2 0.393511 0.199723 0.027641 11.00000 0.03943 0.03123 = 0.03134 -0.00255 -0.00228 -0.00955 CA2 2 0.561519 0.050298 0.793857 11.00000 0.03300 0.03752 = 0.03811 0.00700 -0.00007 -0.00854 CA3 2 1.375792 0.105121 0.461495 11.00000 0.04067 0.02887 = 0.03014 -0.00325 0.00552 -0.00826 MG1 5 0.333361 0.450749 0.421403 11.00000 0.04242 0.02086 = 0.02999 0.00008 0.00829 -0.01848 MG2 5 0.210498 0.683157 0.666169 11.00000 0.05186 0.02327 = 0.04111 -0.00655 0.00624 -0.01023 AS1 1 0.057757 0.201947 0.745201 11.00000 0.03460 0.02052 = 0.02568 -0.00090 0.00080 -0.00868 AS2 1 0.271583 0.487274 0.683030 11.00000 0.03619 0.01865 = 0.02986 -0.00063 0.00249 -0.00964 AS3 1 0.219732 0.370092 0.921731 11.00000 0.04050 0.02193 = 0.02877 -0.00348 0.00014 -0.00837 AS4 1 0.157788 0.067275 0.985326 11.00000 0.03081 0.02202 = 0.02547 -0.00055 0.00112 -0.00859 AS5 1 1.140233 -0.132282 0.808610 11.00000 0.03348 0.01947 = 0.02921 -0.00106 0.00268 -0.00825 AS6 1 1.189826 0.985778 0.580115 11.00000 0.03545 0.02334 = 0.02580 -0.00427 0.00277 -0.01186 AS7 1 0.253589 0.300506 0.517710 11.00000 0.03867 0.02181 = 0.02606 -0.00028 0.00218 -0.01087 V1 4 0.019702 0.397996 0.711792 11.00000 0.03356 0.01976 = 0.03445 -0.00041 -0.00133 -0.00792 V2 4 -0.008163 0.334077 0.839832 11.00000 0.03651 0.02190 = 0.02906 -0.00308 0.00398 -0.00625 V3 4 -0.043407 0.140916 0.881330 11.00000 0.03275 0.02006 = 0.02660 -0.00082 0.00298 -0.00671 V4 4 0.948396 0.030478 0.787439 11.00000 0.02766 0.02144 = 0.02675 -0.00044 0.00008 -0.00915 V5 4 0.972142 0.103143 0.639438 11.00000 0.03290 0.02506 = 0.02662 -0.00297 0.00156 -0.01137 V6 4 0.003947 0.276539 0.604813 11.00000 0.03343 0.02305 = 0.02666 -0.00054 0.00078 -0.00734 V7 4 0.297599 0.352609 0.789705 11.00000 0.03623 0.02334 = 0.02736 0.00061 0.00248 -0.00744 V8 4 0.225582 0.011608 0.861347 11.00000 0.02701 0.02256 = 0.02723 -0.00325 0.00107 -0.00899 V9 4 0.279100 0.143362 0.604620 11.00000 0.03245 0.01939 = 0.02792 -0.00056 -0.00022 -0.01010 V10 4 0.323305 0.315333 0.648860 11.00000 0.03596 0.02013 = 0.02892 -0.00244 0.00040 -0.01000 V11 4 0.264942 0.194469 0.890782 11.00000 0.03397 0.02059 = 0.02670 -0.00135 0.00120 -0.00815 V12 4 1.247325 0.995117 0.715086 11.00000 0.03155 0.02207 = 0.02557 -0.00154 0.00076 -0.00992 O1 3 -0.026029 0.201809 0.678202 11.00000 0.04013 0.02321 = 0.02631 0.00053 0.00446 -0.00921 O2 3 0.955330 0.145106 0.792865 11.00000 0.03608 0.01301 = 0.02867 0.00586 0.00306 -0.01021 O3 3 -0.014882 0.297664 0.759928 11.00000 0.02805 0.02079 = 0.02131 0.00211 0.00335 -0.00153 O4 3 0.303120 0.576149 0.659204 11.00000 0.05545 0.00998 = 0.04069 -0.00570 0.00833 -0.01591 O5 3 0.348735 0.426722 0.638669 11.00000 0.04952 0.01954 = 0.03438 -0.00130 0.00691 -0.00458 O6 3 0.323177 0.459345 0.751910 11.00000 0.03699 0.02412 = 0.03213 -0.00680 0.00140 -0.01765 O7 3 0.108654 0.486032 0.679358 11.00000 0.03453 0.02765 = 0.03676 0.00459 0.00329 -0.00723 O8 3 0.236210 0.423431 0.973781 11.00000 0.06268 0.02450 = 0.03870 -0.01057 -0.01232 -0.00289 O9 3 0.300047 0.403357 0.861577 11.00000 0.04156 0.02485 = 0.02985 0.00291 0.00134 -0.01250 O10 3 0.280494 0.276821 0.943477 11.00000 0.04967 0.02219 = 0.03069 -0.00304 -0.00290 -0.00602 O11 3 0.058046 0.373365 0.907429 11.00000 0.04108 0.03298 = 0.02720 -0.00365 0.00046 -0.00270 O12 3 0.154407 0.042961 0.055833 11.00000 0.03705 0.02803 = 0.02517 -0.00242 0.00024 -0.01103 O13 3 0.006949 0.103095 0.961413 11.00000 0.03007 0.03245 = 0.03117 -0.00395 -0.00132 -0.00163 O14 3 0.221593 0.994162 0.948505 11.00000 0.02426 0.02424 = 0.02913 -0.00398 0.00049 -0.00619 O15 3 0.249455 0.141370 0.971221 11.00000 0.03584 0.02935 = 0.02867 -0.00067 0.00137 -0.01436 O16 3 0.139733 0.773573 0.824013 11.00000 0.05129 0.01855 = 0.03811 0.00061 0.01089 -0.01161 O17 3 0.207532 0.899316 0.864584 11.00000 0.03555 0.01875 = 0.03227 0.00487 0.00458 -0.01244 O18 3 0.988380 0.915877 0.795560 11.00000 0.03967 0.01970 = 0.03900 -0.00209 0.00064 -0.00963 O19 3 0.232904 0.885660 0.747707 11.00000 0.04922 0.02006 = 0.03337 -0.00143 0.00539 -0.00921 O20 3 0.207698 0.923367 0.532082 11.00000 0.05217 0.03004 = 0.03030 -0.01552 0.00503 -0.01093 O21 3 0.033159 0.020954 0.591623 11.00000 0.04044 0.03277 = 0.03114 -0.00953 0.00355 -0.00992 O22 3 0.254898 0.940650 0.643557 11.00000 0.04955 0.02041 = 0.02728 -0.00487 0.00163 -0.00610 O23 3 0.271366 0.060280 0.553785 11.00000 0.03702 0.01746 = 0.03438 -0.00162 0.00199 -0.00871 O24 3 0.283052 0.341262 0.450788 11.00000 0.05089 0.03192 = 0.02662 0.00134 0.00749 -0.00503 O25 3 0.095570 0.319985 0.534569 11.00000 0.03341 0.03207 = 0.04098 0.00533 0.00467 -0.00556 O26 3 0.342809 0.337913 0.563737 11.00000 0.05376 0.01778 = 0.02176 0.00480 0.00087 -0.02096 O27 3 0.300262 0.203201 0.524638 11.00000 0.04581 0.01420 = 0.02696 0.00011 0.00370 -0.00724 O28 3 -0.011154 0.236212 0.879350 11.00000 0.05128 0.02461 = 0.02916 -0.00062 0.00974 -0.00714 O29 3 0.960577 0.045344 0.706856 11.00000 0.04005 0.02789 = 0.03593 -0.00721 0.00580 -0.01072 O30 3 0.025871 0.354114 0.646585 11.00000 0.04539 0.02503 = 0.03355 0.00054 -0.00637 -0.01190 O31 3 -0.123761 0.445659 0.711215 11.00000 0.04320 0.02760 = 0.04489 0.00185 0.00335 -0.00211 O32 3 -0.155034 0.374270 0.843798 11.00000 0.04004 0.03465 = 0.04179 -0.00622 0.00269 -0.00483 O33 3 -0.196044 0.148423 0.891070 11.00000 0.03068 0.03019 = 0.03109 0.00224 0.00449 -0.00214 O34 3 0.795089 0.030606 0.797884 11.00000 0.03275 0.02788 = 0.03747 -0.00182 -0.00015 -0.00305 O35 3 0.826039 0.120557 0.616431 11.00000 0.04450 0.04094 = 0.03686 -0.00490 -0.00342 -0.00538 O36 3 -0.140691 0.298233 0.580608 11.00000 0.04029 0.04068 = 0.03665 -0.00555 -0.00233 -0.00327 O37 3 0.082037 0.411071 0.789294 11.00000 0.02594 0.02358 = 0.02206 -0.00155 -0.00038 -0.01060 O38 3 0.006512 0.028127 0.869321 11.00000 0.02919 0.02673 = 0.02682 -0.00961 0.00103 -0.00646 O39 3 0.061339 0.172507 0.580058 11.00000 0.02990 0.01845 = 0.02937 -0.00002 0.00632 -0.01033 O40 3 0.238735 0.334628 0.718011 11.00000 0.03212 0.02013 = 0.03384 0.00262 0.00540 -0.00857 O41 3 0.214125 0.276548 0.834649 11.00000 0.02328 0.02263 = 0.03162 0.00139 -0.00451 -0.00575 O42 3 0.183554 0.122326 0.866594 11.00000 0.02826 0.02361 = 0.02853 0.00038 -0.00143 -0.00280 O43 3 0.166041 0.024676 0.779490 11.00000 0.03774 0.01336 = 0.03351 -0.00207 -0.00079 -0.01081 O44 3 0.196714 0.083182 0.665295 11.00000 0.03914 0.02181 = 0.02266 -0.00540 0.00085 -0.00169 O45 3 0.232076 0.237882 0.633823 11.00000 0.03108 0.01839 = 0.02980 -0.00387 0.00449 -0.00649 O46 3 0.444596 0.311644 0.790000 11.00000 0.03226 0.02721 = 0.04635 0.00053 0.00035 -0.00694 O47 3 0.415068 0.169586 0.877841 11.00000 0.03278 0.02667 = 0.03811 0.00013 0.00407 -0.00459 O48 3 0.379801 0.006350 0.848614 11.00000 0.02577 0.03386 = 0.03043 -0.00556 0.00241 -0.00934 O49 3 0.398563 0.995311 0.726425 11.00000 0.03182 0.02443 = 0.03111 -0.00061 -0.00956 -0.00960 O50 3 0.429398 0.122841 0.620754 11.00000 0.03375 0.03669 = 0.02989 0.00017 0.00371 -0.00441 O51 3 0.464758 0.272119 0.666746 11.00000 0.04235 0.02734 = 0.04252 -0.00501 0.00543 -0.01202 OW1 3 0.573728 0.043915 0.530992 11.00000 0.04635 0.03312 = 0.04156 -0.00494 0.00843 -0.01048 OW2 3 0.642236 0.177714 0.786674 11.00000 0.04718 0.02893 = 0.06954 -0.00242 -0.01027 -0.00567 OW3 3 0.390152 0.559205 0.389504 11.00000 0.06496 0.04610 = 0.05853 -0.00690 0.00135 -0.01640 OW4 3 0.325823 0.485390 0.507595 11.00000 0.05656 0.03678 = 0.03506 0.00117 0.00068 -0.00876 OW5 3 0.240027 0.671291 0.755719 11.00000 0.11357 0.04268 = 0.03460 -0.00467 0.00471 0.00686 OW6 3 0.126516 0.797454 0.668020 11.00000 0.06721 0.02480 = 0.05422 -0.00315 -0.00043 -0.00194 OW7 3 0.175466 0.697630 0.577849 11.00000 0.05717 0.03714 = 0.04943 -0.00465 -0.01287 -0.00261 OW8 3 1.277991 0.216802 0.395576 11.00000 0.09508 0.03540 = 0.04493 -0.00478 -0.01351 0.00362 OW9 3 0.511954 0.072766 0.031448 11.00000 0.04395 0.03262 = 0.06431 -0.00320 -0.01233 -0.00409 OW10 3 0.462711 0.077447 0.367970 11.00000 0.06392 0.04507 = 0.04530 -0.01321 0.01830 -0.01242 OW11 3 0.543557 0.412271 0.437806 11.00000 0.04274 0.04195 = 0.04723 -0.00758 0.00325 -0.01136 OW12 3 0.395095 0.149818 0.753344 11.00000 0.05019 0.03231 = 0.03169 -0.00229 -0.00585 -0.00326 OW13 3 0.026437 0.644325 0.680740 11.00000 0.07064 0.03300 = 0.11634 -0.00429 0.01343 -0.02310 OW14 3 0.341340 0.323351 0.062236 11.00000 0.14604 0.04366 = 0.06161 -0.01994 -0.04370 0.00640 OW15 3 0.137184 0.497635 0.413898 11.00000 0.06563 0.05312 = 0.06171 0.02396 -0.02289 -0.01545 OW16 3 0.372628 0.413679 0.338160 11.00000 0.09306 0.04517 = 0.05979 -0.00855 0.00201 -0.02816 OW17 3 0.395775 0.721913 0.654279 11.00000 0.04631 0.04483 = 0.04864 -0.00255 0.00149 -0.01947 OW18 3 0.615240 0.038436 0.898398 11.00000 0.04327 0.03806 = 0.03643 -0.00148 -0.00271 -0.00440 OW19 3 0.241691 0.157864 0.101765 11.00000 0.04276 0.04414 = 0.04337 -0.00667 0.00672 -0.01402 OW20 3 0.568083 0.183383 0.448820 11.00000 0.04851 0.04135 = 0.04612 -0.00129 0.00760 -0.00659 OW21 3 0.624464 0.910983 0.796988 11.00000 0.05271 0.04138 = 0.06116 -0.00449 -0.00536 -0.00778 OW22 3 0.537093 0.191539 0.112319 11.00000 0.05212 0.05749 = 0.05042 -0.01133 -0.01905 -0.00126 OW23 3 1.180814 0.066697 0.419674 11.00000 0.05531 0.05132 = 0.05603 -0.01301 0.00140 -0.02432 OW24 3 0.638977 0.052578 0.692740 11.00000 0.04600 0.06707 = 0.04700 -0.00383 -0.00106 -0.01652 OW25 3 0.582347 0.230134 0.976681 11.00000 0.04598 0.10512 = 0.07395 0.02501 0.00674 -0.01922 OW26 3 0.006479 0.574377 0.933532 11.00000 0.16582 0.38094 = 0.24503 -0.20217 -0.06987 0.02466 OW27 3 0.299075 0.681868 0.909256 11.00000 0.14184 0.08825 = 0.21114 -0.01916 -0.05088 -0.00887 OW28 3 0.092955 0.675065 0.995777 11.00000 0.22006 0.09157 = 0.11546 -0.03383 0.09346 -0.07805 OW29 3 0.417255 0.562340 0.017451 11.00000 0.29402 0.27195 = 0.30960 -0.14209 0.12196 -0.04459 OW30 3 0.844676 0.479263 0.937878 11.00000 0.30069 0.12748 = 0.11320 -0.04188 -0.00332 0.07004 OW31 3 0.320126 0.552233 0.860804 11.00000 0.74577 0.09352 = 0.37181 -0.12740 0.06621 -0.14695 OW32 3 -0.394224 0.286803 0.526468 11.00000 0.06003 0.05894 = 0.05226 -0.01421 0.00457 -0.01343 OW33 3 -0.020776 0.167695 0.473119 11.00000 0.04341 0.02787 = 0.04034 -0.00532 -0.00449 -0.01458 OW34 3 0.823911 0.180108 0.026002 11.00000 0.05175 0.03675 = 0.03858 0.00009 0.00974 -0.00999 OW35 3 -0.069536 0.423928 0.462192 11.00000 0.05007 0.03976 = 0.05010 0.00251 -0.00757 -0.00007 OW36 3 0.701480 0.328174 0.705947 11.00000 0.05398 0.05630 = 0.09880 0.00670 -0.00936 -0.02069 OW37 3 0.591315 0.469999 0.752973 11.00000 0.05600 0.07077 = 0.06720 0.00003 0.00819 -0.01998 OW38 3 0.596272 0.349863 0.887673 11.00000 0.06873 0.12367 = 0.07416 0.03160 -0.00637 -0.05298 OW39 3 0.129935 0.127506 0.302108 11.00000 0.09911 0.09341 = 0.07734 -0.01806 -0.03172 -0.02341 OW40 3 0.476229 0.795829 0.747373 11.00000 0.09450 0.09554 = 0.14883 -0.03750 -0.00874 -0.01222 OW41 3 0.914891 0.724078 0.856054 11.00000 0.10926 0.06716 = 0.32085 -0.07267 0.13974 -0.04480 OW42 3 0.229559 0.284896 0.267264 11.00000 0.13563 0.28266 = 0.10870 -0.01755 0.01156 -0.09798 OW43 3 0.522077 0.658088 0.826697 11.00000 0.27712 0.23094 = 0.18872 -0.04344 -0.02600 0.03837 OW44 3 0.726676 0.545416 0.828934 11.00000 0.32059 0.12814 = 0.21340 -0.05792 -0.16620 0.06800 OW45 3 0.027774 0.558636 0.810934 11.00000 0.36592 0.04993 = 0.11751 -0.01713 0.09642 -0.02475 HKLF 4 REM TRPR2 REM R1 = 0.0585 for 7560 Fo > 4sig(Fo) and 0.0870 for all 10623 data REM 1091 parameters refined using 0 restraints END WGHT 0.0825 6.1485 REM No hydrogen bonds found for HTAB generation REM Highest difference peak 1.187, deepest hole -0.895, 1-sigma level 0.163 Q1 1 0.4457 0.5055 0.9074 11.00000 0.05 1.19 Q2 1 0.1654 0.1805 0.7494 11.00000 0.05 1.10 Q3 1 0.3349 0.5338 0.9583 11.00000 0.05 1.03 Q4 1 0.1616 0.5475 0.8510 11.00000 0.05 0.94 Q5 1 0.2316 1.0479 0.9506 11.00000 0.05 0.81 Q6 1 0.3516 0.5726 0.8485 11.00000 0.05 0.74 Q7 1 0.1320 0.3396 0.2236 11.00000 0.05 0.73 Q8 1 1.0544 -0.1093 0.8361 11.00000 0.05 0.73 Q9 1 0.6561 0.1405 0.4537 11.00000 0.05 0.73 Q10 1 0.2254 0.2993 0.2148 11.00000 0.05 0.72 Q11 1 1.0765 -0.1198 0.7699 11.00000 0.05 0.72 Q12 1 -0.0844 0.3017 0.6229 11.00000 0.05 0.69 Q13 1 0.2783 0.9491 0.5499 11.00000 0.05 0.68 Q14 1 0.1653 0.3371 0.4977 11.00000 0.05 0.68 Q15 1 0.2450 0.3047 0.2707 11.00000 0.05 0.68 Q16 1 0.4329 0.5837 0.0124 11.00000 0.05 0.67 Q17 1 0.3040 0.2925 0.4800 11.00000 0.05 0.67 Q18 1 0.1682 0.3232 0.5397 11.00000 0.05 0.66 Q19 1 0.1966 0.8582 0.7700 11.00000 0.05 0.65 Q20 1 0.3111 0.2989 0.5582 11.00000 0.05 0.64 Q21 1 -0.0316 0.3174 0.7913 11.00000 0.05 0.63 Q22 1 0.3092 0.6572 0.7703 11.00000 0.05 0.63 Q23 1 -0.0241 0.7220 0.9748 11.00000 0.05 0.63 Q24 1 -0.0103 0.5357 0.9527 11.00000 0.05 0.63 Q25 1 0.3659 0.1271 0.5749 11.00000 0.05 0.63 Q26 1 0.0406 0.1709 0.5406 11.00000 0.05 0.62 Q27 1 0.0844 0.0855 1.0158 11.00000 0.05 0.62 Q28 1 -0.0319 0.2460 0.7563 11.00000 0.05 0.62 Q29 1 0.1930 0.5148 0.7173 11.00000 0.05 0.60 Q30 1 0.1327 0.4056 0.9398 11.00000 0.05 0.60 ; _shelx_res_checksum 3362 _shelx_hkl_file ; 0 1 -3 1292.86 53.88 0 1 -3 1557.45 62.76 0 -1 3 1587.75 52.49 0 -1 3 1583.70 64.06 1 2 -1 45.48 4.96 -1 -2 1 55.06 6.46 1 2 -1 42.46 4.45 -1 -2 1 47.07 3.22 -1 1 -2 454.75 15.55 1 -1 2 444.82 15.07 -1 1 -2 413.18 12.28 1 -1 2 469.76 16.28 0 2 -2 12.74 4.68 0 2 -2 15.75 2.78 0 -2 2 12.57 4.41 0 -2 2 9.26 2.95 1 2 2 330.75 14.91 -1 -2 -2 324.47 10.97 -1 -2 -2 323.46 16.83 1 2 2 358.40 13.16 1 1 3 870.75 29.14 -1 -1 -3 910.10 30.33 -1 -1 -3 926.44 31.15 -1 -1 -3 886.10 34.96 1 -2 0 364.98 8.72 1 -2 0 304.48 10.69 -1 2 0 301.78 10.76 -1 2 0 365.13 11.23 -1 2 0 326.77 8.36 1 -2 0 347.21 10.86 1 0 3 439.85 22.75 -1 0 -3 454.26 16.61 -1 0 -3 360.48 10.38 0 2 3 646.99 27.01 0 -2 -3 614.99 19.26 0 -2 -3 641.46 32.90 0 -2 -3 627.96 24.51 0 2 3 629.86 25.67 -1 0 3 720.24 23.77 1 0 -3 707.16 25.93 -1 0 3 695.12 32.52 1 0 -3 749.37 29.35 -1 2 1 68.65 6.41 1 -2 -1 62.63 4.19 1 -2 -1 61.78 4.53 -1 2 1 63.00 4.45 -1 2 1 65.87 1.79 -1 2 -1 302.15 9.91 1 -2 1 280.89 7.74 1 -2 1 289.19 9.47 -1 2 -1 274.26 7.90 1 -2 1 295.92 10.23 1 -1 -3 4.04 2.62 1 -1 -3 2.85 3.09 1 -1 -3 8.91 2.09 -1 1 3 1.47 3.08 -1 1 3 4.31 2.46 -1 1 3 5.94 2.24 0 3 1 44.53 4.91 0 3 1 54.46 7.65 0 -3 -1 34.84 7.94 0 -3 -1 53.55 4.66 0 -3 -1 35.42 3.16 0 3 1 39.70 3.10 -1 -2 2 2.17 2.53 -1 -2 2 5.49 3.10 1 2 -2 7.15 3.23 1 2 -2 11.39 2.51 0 -3 0 854.43 33.01 0 -3 0 895.81 37.05 0 -3 0 864.79 33.84 0 3 0 907.41 36.39 0 3 0 913.28 34.38 0 3 0 758.79 31.68 0 0 4 69.88 5.71 0 0 -4 79.71 5.86 0 0 4 62.90 5.40 0 0 -4 76.42 8.08 -1 -1 3 502.10 18.98 1 1 -3 500.87 18.54 0 1 4 19.17 3.52 0 1 4 20.54 3.30 0 -1 -4 29.33 3.71 0 -1 -4 25.56 3.10 0 -1 -4 21.41 3.25 -1 2 2 596.92 23.30 1 -2 -2 698.36 24.93 1 -2 -2 698.87 26.42 -1 2 2 748.96 28.10 1 2 3 40.43 4.42 -1 -2 -3 41.50 4.01 1 2 3 46.87 6.29 -1 -2 -3 55.32 4.83 -1 1 -3 1.26 2.72 1 -1 3 -0.14 2.86 -1 1 -3 1.12 2.09 0 -3 -2 118.39 5.18 0 3 2 108.24 13.45 0 3 2 130.06 8.01 0 -3 -2 136.61 9.07 0 -3 -2 112.91 7.74 0 -3 1 581.46 21.68 0 3 -1 486.92 17.86 0 3 -1 567.81 20.43 0 3 -1 581.78 20.57 0 -3 1 504.22 18.23 0 -3 1 589.49 27.83 0 -2 3 7.01 4.97 0 -2 3 10.71 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