data_12082 _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'H31 As3.50 Ca3 O41 V6' _chemical_formula_weight 1375.35 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'H' 'H' 0.0000 0.0000 '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' 'As' 'As' 0.0499 2.0058 '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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 4 _space_group_name_H-M_alt 'P 21' _space_group_name_Hall 'P 2yb' _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+1/2, -z' _cell_length_a 11.1850(4) _cell_length_b 16.8528(4) _cell_length_c 20.7146(15) _cell_angle_alpha 90 _cell_angle_beta 91.166(6) _cell_angle_gamma 90 _cell_volume 3903.9(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 2.340 _exptl_crystal_F_000 2690 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_absorpt_coefficient_mu 4.835 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_source ? _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 26034 _diffrn_reflns_av_unetI/netI 0.0545 _diffrn_reflns_av_R_equivalents 0.0377 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.027 _diffrn_reflns_theta_max 25.025 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.975 _diffrn_measured_fraction_theta_full 0.952 _diffrn_reflns_Laue_measured_fraction_max 0.975 _diffrn_reflns_Laue_measured_fraction_full 0.952 _diffrn_reflns_point_group_measured_fraction_max 0.978 _diffrn_reflns_point_group_measured_fraction_full 0.955 _reflns_number_total 12556 _reflns_number_gt 9088 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.934 _reflns_Friedel_fraction_max 0.982 _reflns_Friedel_fraction_full 0.957 _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_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refined as a 2-component inversion twin. ; _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^)+(0.0668P)^2^+33.9406P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens . _refine_ls_hydrogen_treatment undef _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack 0.52(3) _chemical_absolute_configuration ? _refine_ls_number_reflns 12556 _refine_ls_number_parameters 842 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0845 _refine_ls_R_factor_gt 0.0533 _refine_ls_wR_factor_ref 0.1602 _refine_ls_wR_factor_gt 0.1315 _refine_ls_goodness_of_fit_ref 1.096 _refine_ls_restrained_S_all 1.096 _refine_ls_shift/su_max 1.308 _refine_ls_shift/su_mean 0.059 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 As1 As 0.27481(12) 0.6636(2) 0.75814(6) 0.0168(3) Uani 1 1 d . . . . . As2 As 0.0376(3) 0.37801(16) 0.84141(16) 0.0228(8) Uani 1 1 d . . . . . As3 As -0.07357(12) 0.6635(3) 0.95731(6) 0.0197(3) Uani 1 1 d . . . . . As4 As 0.0372(3) 0.94880(16) 0.84230(17) 0.0232(8) Uani 1 1 d . . . . . As5 As 0.2793(3) 0.94950(16) 0.60538(17) 0.0264(8) Uani 1 1 d . . . . . As6 As 0.39260(13) 0.6632(3) 0.48857(6) 0.0251(3) Uani 1 1 d . . . . . As7 As 0.2789(4) 0.37688(16) 0.60527(17) 0.0288(9) Uani 1 1 d . . . . . V1 V 0.2689(5) 0.4942(3) 0.8461(3) 0.0264(14) Uani 1 1 d . . . . . V2 V 0.2037(2) 0.6643(4) 0.91695(10) 0.0230(5) Uani 1 1 d . . . . . V3 V 0.2692(5) 0.8319(3) 0.8464(3) 0.0259(14) Uani 1 1 d . . . . . V4 V 0.4088(5) 0.8318(3) 0.7084(3) 0.0266(14) Uani 1 1 d . . . . . V5 V 0.4799(2) 0.6636(4) 0.63798(11) 0.0241(5) Uani 1 1 d . . . . . V6 V 0.4083(6) 0.4949(3) 0.7092(3) 0.0303(15) Uani 1 1 d . . . . . V7 V -0.0208(5) 0.5615(3) 0.8291(2) 0.0183(12) Uani 1 1 d . . . . . V8 V 0.1002(5) 0.8726(3) 0.7058(3) 0.0248(14) Uani 1 1 d . . . . . V9 V 0.2278(5) 0.5611(3) 0.5836(3) 0.0220(13) Uani 1 1 d . . . . . V10 V -0.0226(5) 0.7638(3) 0.8290(3) 0.0198(13) Uani 1 1 d . . . . . V11 V 0.2293(5) 0.7644(3) 0.5849(3) 0.0203(13) Uani 1 1 d . . . . . V12 V 0.0995(5) 0.4553(3) 0.7056(3) 0.0245(14) Uani 1 1 d . . . . . Ca1 Ca -0.2312(6) 0.8650(4) 0.9273(3) 0.0295(17) Uani 1 1 d . . . . . Ca2 Ca -0.2334(6) 0.4625(4) 0.9269(3) 0.0267(16) Uani 1 1 d . . . . . Ca3 Ca 0.2607(7) 0.4533(5) 0.4356(3) 0.0389(19) Uani 1 1 d . . . . . Ca4 Ca 0.2626(7) 0.8715(5) 0.4365(4) 0.041(2) Uani 1 1 d . . . . . Ca5 Ca -0.0064(3) 0.1635(5) 0.88417(15) 0.0349(7) Uani 1 1 d . . . . . Ca6A Ca -0.490(15) 0.570(10) 0.336(8) 0.17(10) Uiso 0.08(4) 1 d . . . . . Ca6B Ca -0.235(2) 0.663(4) 0.4152(9) 0.029(8) Uiso 0.151(14) 1 d . . . . . Ca6C Ca -0.313(2) 0.665(2) 0.4443(11) 0.029(5) Uiso 0.28(3) 1 d . . . . . Ca6D Ca -0.324(2) 0.663(2) 0.4102(16) 0.035(7) Uiso 0.27(4) 1 d . . . . . Ca6E Ca -0.348(6) 0.663(4) 0.428(2) 0.01(2) Uiso 0.12(5) 1 d . . . . . O1 O 0.2889(11) 0.6192(8) 0.8367(6) 0.029(3) Uani 1 1 d . . . . . O2 O 0.4061(11) 0.6193(7) 0.7217(6) 0.027(3) Uani 1 1 d . . . . . O3 O 0.3426(11) 0.7590(7) 0.7794(5) 0.027(3) Uani 1 1 d . . . . . O4 O 0.0374(18) 0.3669(11) 0.7615(10) 0.027(5) Uani 1 1 d . . . . . O5 O -0.008(2) 0.2956(11) 0.8796(11) 0.034(6) Uani 1 1 d . . . . . O6 O 0.176(2) 0.3991(12) 0.8701(11) 0.034(6) Uani 1 1 d . . . . . O7 O -0.0563(19) 0.4544(11) 0.8642(9) 0.024(5) Uani 1 1 d . . . . . O8 O -0.1426(9) 0.6669(15) 1.0280(4) 0.023(2) Uani 1 1 d . . . . . O9 O -0.1039(19) 0.5807(10) 0.9153(10) 0.019(5) Uani 1 1 d . . . . . O10 O 0.0735(9) 0.6617(16) 0.9799(5) 0.032(3) Uani 1 1 d . . . . . O11 O -0.113(2) 0.7457(11) 0.9142(10) 0.026(5) Uani 1 1 d . . . . . O12 O -0.009(2) 1.0278(12) 0.8797(10) 0.038(6) Uani 1 1 d . . . . . O13 O -0.0559(18) 0.8756(11) 0.8591(9) 0.023(5) Uani 1 1 d . . . . . O14 O 0.047(2) 0.9614(11) 0.7626(10) 0.037(6) Uani 1 1 d . . . . . O15 O 0.178(2) 0.9236(12) 0.8696(10) 0.032(6) Uani 1 1 d . . . . . O16 O 0.310(2) 1.0296(13) 0.5627(11) 0.048(7) Uani 1 1 d . . . . . O17 O 0.159(2) 0.9609(10) 0.6513(10) 0.031(6) Uani 1 1 d . . . . . O18 O 0.401(2) 0.9259(12) 0.6542(10) 0.034(6) Uani 1 1 d . . . . . O19 O 0.2646(19) 0.8755(10) 0.5497(9) 0.024(5) Uani 1 1 d . . . . . O20 O 0.4575(10) 0.6643(17) 0.4178(5) 0.039(3) Uani 1 1 d . . . . . O21 O 0.5044(9) 0.6688(16) 0.5434(5) 0.030(3) Uani 1 1 d . . . . . O22 O 0.316(2) 0.7484(11) 0.4996(9) 0.024(5) Uani 1 1 d . . . . . O23 O 0.300(2) 0.5821(12) 0.4945(9) 0.028(5) Uani 1 1 d . . . . . O24 O 0.311(2) 0.2943(11) 0.5658(11) 0.044(7) Uani 1 1 d . . . . . O25 O 0.153(2) 0.3656(13) 0.6485(11) 0.038(6) Uani 1 1 d . . . . . O26 O 0.256(2) 0.4540(13) 0.5530(9) 0.030(5) Uani 1 1 d . . . . . O27 O 0.394(2) 0.4000(12) 0.6547(12) 0.039(6) Uani 1 1 d . . . . . O28 O 0.3089(12) 0.672(2) 0.9694(5) 0.053(5) Uani 1 1 d . . . . . O29 O 0.2059(19) 0.7618(9) 0.8940(7) 0.049(5) Uani 1 1 d . . . . . O30 O 0.1431(14) 0.5479(10) 0.9062(8) 0.039(4) Uani 1 1 d . . . . . O31 O 0.0377(8) 0.6628(14) 0.8415(4) 0.022(2) Uani 1 1 d . . . . . O32 O 0.378(2) 0.4764(17) 0.8897(15) 0.067(9) Uani 1 1 d . . . . . O33 O 0.2818(12) 0.4270(8) 0.7609(6) 0.031(3) Uani 1 1 d . . . . . O34 O 0.0914(18) 0.5222(11) 0.7816(10) 0.019(5) Uani 1 1 d . . . . . O35 O 0.6178(10) 0.667(2) 0.6605(6) 0.054(4) Uani 1 1 d . . . . . O36 O 0.438(3) 0.7723(15) 0.6333(18) 0.118(14) Uani 1 1 d . . . . . O37 O 0.439(2) 0.5553(17) 0.635(2) 0.101(16) Uani 1 1 d . . . . . O38 O 0.2793(8) 0.6619(14) 0.6051(4) 0.020(2) Uani 1 1 d . . . . . O39 O 0.391(2) 0.8556(14) 0.8895(12) 0.053(7) Uani 1 1 d . . . . . O40 O 0.3253(13) 0.8513(9) 0.7731(6) 0.034(3) Uani 1 1 d . . . . . O41 O 0.0974(19) 0.8068(11) 0.7828(9) 0.022(5) Uani 1 1 d . . . . . O42 O -0.020(2) 0.4798(13) 0.6672(10) 0.035(6) Uani 1 1 d . . . . . O43 O 0.2185(19) 0.5217(10) 0.6623(8) 0.016(4) Uani 1 1 d . . . . . O44 O 0.539(2) 0.4753(14) 0.7396(14) 0.057(9) Uani 1 1 d . . . . . O45 O 0.216(2) 0.8081(12) 0.6638(10) 0.025(5) Uani 1 1 d . . . . . O46 O 0.538(3) 0.8511(18) 0.7391(15) 0.076(11) Uani 1 1 d . . . . . O47 O 0.096(2) 0.5730(14) 0.5616(10) 0.032(6) Uani 1 1 d . . . . . O48 O -0.1334(17) 0.5753(12) 0.7766(10) 0.023(5) Uani 1 1 d . . . . . O49 O 0.091(2) 0.7517(11) 0.5619(11) 0.036(6) Uani 1 1 d . . . . . O50 O -0.019(2) 0.8445(14) 0.6696(11) 0.041(7) Uani 1 1 d . . . . . O51 O -0.126(2) 0.7537(13) 0.7810(11) 0.036(6) Uani 1 1 d . . . . . O52 O -0.2555(19) 0.8050(12) 1.0336(9) 0.029(5) Uiso 1 1 d . . . . . O53 O 0.2569(18) 0.9449(12) 0.3342(9) 0.059(5) Uiso 1 1 d . . . . . O54 O 0.410(2) 0.5160(13) 0.3705(11) 0.056(7) Uiso 1 1 d . . . . . O55 O 0.3931(16) 0.8074(10) 0.3627(8) 0.030(4) Uiso 1 1 d . . . . . O56 O 0.265(2) 0.3573(14) 0.3489(12) 0.089(8) Uiso 1 1 d . . . . . O57 O 0.107(3) 0.3614(16) 0.4658(13) 0.080(11) Uiso 0.86(6) 1 d . . . . . O58 O -0.3888(17) 0.5439(11) 0.8891(9) 0.049(5) Uiso 1 1 d . . . . . O59 O -0.313(2) 0.4021(15) 0.8296(13) 0.071(8) Uiso 1 1 d . . . . . O60 O -0.0873(17) 0.171(2) 0.7747(9) 0.099(6) Uiso 1 1 d . . . . . O61 O -0.3953(17) 0.9368(11) 0.9729(9) 0.053(5) Uiso 1 1 d . . . . . O62 O 0.1382(17) 0.9900(11) 0.4589(8) 0.053(5) Uiso 1 1 d . . . . . O63 O -0.0980(18) 0.656(3) 0.6419(10) 0.108(7) Uiso 1 1 d . . . . . O64 O -0.3697(19) 0.3665(12) 0.9706(10) 0.062(6) Uiso 1 1 d . . . . . O65 O 0.1784(14) 0.169(2) 0.8275(7) 0.072(5) Uiso 1 1 d . . . . . O66 O -0.3903(18) 0.7724(11) 0.9048(9) 0.050(5) Uiso 1 1 d . . . . . O67 O 0.0852(16) 0.8113(10) 0.4020(8) 0.058(4) Uiso 1 1 d . . . . . O68 O -0.2182(13) 0.1753(12) 0.9001(7) 0.057(4) Uiso 1 1 d . . . . . O69 O 0.424(2) 0.9596(14) 0.4570(11) 0.052(7) Uiso 1 1 d . . . . . O70 O -0.1152(19) 0.9633(12) 0.9837(10) 0.042(6) Uiso 1 1 d . . . . . O71 O -0.0941(18) 0.3683(11) 0.9865(9) 0.040(6) Uiso 1 1 d . . . . . O72 O -0.253(2) 0.5193(13) 1.0304(11) 0.038(6) Uiso 1 1 d . . . . . O73 O 0.4288(18) 0.3601(12) 0.4659(9) 0.038(5) Uiso 1 1 d . . . . . O74 O -0.315(3) 0.9383(16) 0.8368(14) 0.072(11) Uiso 0.93(6) 1 d . . . . . O75 O -0.380(2) 0.654(3) 0.3170(11) 0.096(12) Uiso 0.80(5) 1 d . . . . . O76 O -0.237(2) 0.671(3) 0.5360(12) 0.100(13) Uiso 0.74(5) 1 d . . . . . O77 O -0.469(2) 0.7636(13) 1.0908(12) 0.095(7) Uiso 1 1 d . . . . . O78 O -0.491(3) 0.6006(17) 1.0349(15) 0.129(10) Uiso 1 1 d . . . . . O79 O -0.359(2) 0.5479(13) 0.2113(11) 0.073(7) Uiso 1 1 d . . . . . O80 O 0.6265(10) 0.6655(19) 0.8039(5) 0.047(3) Uiso 1 1 d . . . . . O81 O -0.237(5) 0.289(3) 0.744(2) 0.16(3) Uiso 0.76(9) 1 d . . . . . O82 O 0.016(3) 0.665(4) 0.4418(14) 0.103(14) Uiso 0.64(5) 1 d . . . . . O83 O 0.319(3) 0.2744(18) 0.7730(15) 0.061(12) Uiso 0.63(6) 1 d . . . . . O84 O -0.200(3) 0.0186(15) 0.7398(13) 0.046(10) Uiso 0.63(6) 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 As1 0.0196(8) 0.0133(6) 0.0178(6) 0.0011(17) 0.0045(5) 0.0005(18) As2 0.031(2) 0.0111(16) 0.0265(19) 0.0013(13) 0.0063(15) 0.0002(14) As3 0.0241(8) 0.0166(6) 0.0188(7) 0.0005(17) 0.0075(5) 0.0010(19) As4 0.029(2) 0.0133(16) 0.0278(19) -0.0023(14) 0.0105(15) 0.0030(14) As5 0.041(2) 0.0119(17) 0.026(2) 0.0019(14) 0.0077(16) -0.0007(16) As6 0.0386(9) 0.0179(7) 0.0191(7) -0.0018(19) 0.0114(6) 0.001(2) As7 0.047(3) 0.0143(18) 0.026(2) -0.0042(14) 0.0107(17) -0.0014(16) V1 0.022(4) 0.022(3) 0.035(4) 0.017(2) 0.000(3) -0.001(3) V2 0.0243(14) 0.0259(12) 0.0189(11) 0.005(3) 0.0041(9) 0.002(3) V3 0.027(4) 0.027(3) 0.024(3) -0.008(2) 0.001(3) 0.005(3) V4 0.026(4) 0.025(3) 0.029(4) 0.008(2) 0.006(3) -0.011(2) V5 0.0231(14) 0.0264(12) 0.0232(12) -0.005(3) 0.0083(9) 0.001(3) V6 0.031(4) 0.028(3) 0.032(4) -0.011(3) -0.005(3) 0.011(3) V7 0.020(4) 0.014(3) 0.021(3) 0.001(2) 0.006(2) 0.000(2) V8 0.031(4) 0.024(3) 0.020(3) 0.005(2) 0.008(3) 0.011(3) V9 0.032(4) 0.013(3) 0.021(3) -0.002(2) 0.005(2) -0.003(2) V10 0.024(4) 0.011(3) 0.025(3) 0.001(2) 0.006(2) 0.001(2) V11 0.029(4) 0.015(3) 0.018(3) -0.001(2) 0.006(2) 0.002(2) V12 0.024(4) 0.031(3) 0.018(3) -0.004(2) 0.003(2) -0.006(3) Ca1 0.030(5) 0.033(4) 0.025(4) -0.008(3) 0.012(3) 0.008(3) Ca2 0.025(4) 0.024(4) 0.031(4) 0.000(3) -0.002(3) -0.002(3) Ca3 0.045(5) 0.043(5) 0.028(4) -0.007(3) 0.010(4) -0.004(4) Ca4 0.036(5) 0.046(5) 0.043(5) 0.009(4) 0.010(4) 0.002(4) Ca5 0.046(2) 0.0162(14) 0.0423(18) -0.006(4) -0.0095(14) -0.002(4) O1 0.026(8) 0.042(7) 0.019(6) -0.008(5) -0.001(5) 0.001(6) O2 0.021(8) 0.029(7) 0.032(7) 0.006(5) -0.001(5) 0.005(5) O3 0.026(8) 0.037(7) 0.018(6) -0.003(5) -0.003(5) -0.003(6) O4 0.021(11) 0.023(11) 0.037(13) 0.002(9) 0.007(9) -0.018(8) O5 0.034(15) 0.014(11) 0.056(16) 0.019(10) 0.018(11) -0.010(9) O6 0.022(15) 0.020(12) 0.059(17) 0.011(10) -0.010(11) -0.004(9) O7 0.030(13) 0.013(9) 0.031(11) -0.001(8) 0.024(9) -0.004(9) O8 0.027(6) 0.023(6) 0.021(5) -0.001(11) 0.011(4) 0.002(11) O9 0.018(12) 0.012(10) 0.026(12) -0.005(8) 0.010(8) -0.011(8) O10 0.022(6) 0.042(6) 0.030(6) -0.019(12) 0.009(4) -0.012(13) O11 0.031(14) 0.024(11) 0.023(12) -0.001(9) 0.008(9) -0.004(9) O12 0.065(18) 0.019(11) 0.031(13) 0.003(9) 0.003(11) -0.009(11) O13 0.023(13) 0.019(10) 0.028(11) -0.006(8) 0.007(9) -0.007(9) O14 0.070(17) 0.014(11) 0.029(13) 0.014(8) 0.008(11) -0.001(10) O15 0.047(17) 0.021(12) 0.028(13) -0.019(9) 0.003(10) 0.007(10) O16 0.059(18) 0.034(13) 0.052(16) 0.011(11) 0.030(13) 0.006(12) O17 0.053(15) 0.012(10) 0.029(12) 0.007(9) 0.025(10) 0.014(9) O18 0.043(16) 0.035(13) 0.026(12) 0.016(9) 0.005(10) -0.011(10) O19 0.047(14) 0.010(9) 0.014(10) 0.005(7) 0.006(9) -0.007(9) O20 0.058(8) 0.028(5) 0.031(6) 0.006(14) 0.020(5) 0.006(17) O21 0.023(6) 0.039(8) 0.029(5) -0.015(10) 0.010(4) -0.004(10) O22 0.032(12) 0.018(9) 0.021(10) -0.007(7) 0.008(8) 0.003(7) O23 0.049(14) 0.021(10) 0.015(10) -0.008(7) 0.001(8) -0.002(8) O24 0.08(2) 0.002(9) 0.047(14) -0.008(9) -0.010(12) 0.012(10) O25 0.037(15) 0.042(15) 0.036(13) -0.007(11) -0.008(10) -0.014(11) O26 0.048(15) 0.032(12) 0.010(10) 0.000(8) 0.008(9) -0.009(10) O27 0.043(17) 0.012(11) 0.062(17) 0.005(10) 0.001(12) 0.009(10) O28 0.036(7) 0.103(15) 0.021(6) 0.006(13) -0.007(5) -0.005(14) O29 0.098(17) 0.030(9) 0.019(8) 0.010(6) -0.022(9) -0.040(10) O30 0.029(10) 0.040(9) 0.047(10) -0.004(7) 0.006(7) 0.013(7) O31 0.028(6) 0.011(4) 0.027(5) -0.010(12) 0.015(4) 0.000(12) O32 0.036(16) 0.074(18) 0.09(2) 0.051(15) -0.036(14) -0.025(13) O33 0.035(9) 0.029(8) 0.030(8) -0.001(6) 0.006(6) -0.001(6) O34 0.014(12) 0.012(10) 0.030(12) 0.005(8) 0.008(9) 0.004(8) O35 0.024(7) 0.098(11) 0.042(7) 0.010(18) 0.007(5) -0.008(18) O36 0.08(2) 0.043(17) 0.24(4) -0.10(2) 0.08(2) -0.020(15) O37 0.001(14) 0.06(2) 0.24(5) 0.07(3) 0.019(19) 0.012(13) O38 0.030(6) 0.014(5) 0.016(4) 0.003(11) 0.002(4) -0.016(11) O39 0.044(16) 0.055(14) 0.059(17) -0.051(12) -0.018(12) 0.011(11) O40 0.041(10) 0.037(8) 0.023(7) -0.005(6) 0.014(6) -0.015(7) O41 0.030(14) 0.015(10) 0.021(11) 0.000(8) 0.008(9) 0.008(9) O42 0.033(15) 0.045(13) 0.026(13) -0.016(9) 0.001(10) -0.015(10) O43 0.029(13) 0.010(9) 0.008(9) -0.003(7) 0.002(8) 0.004(8) O44 0.025(16) 0.054(16) 0.09(2) -0.037(14) -0.026(14) 0.034(12) O45 0.027(14) 0.025(11) 0.023(12) 0.003(9) 0.008(9) 0.009(10) O46 0.05(2) 0.10(2) 0.08(2) 0.044(18) -0.024(17) -0.042(18) O47 0.023(14) 0.048(14) 0.026(13) -0.006(10) 0.005(9) -0.014(10) O48 0.009(10) 0.024(10) 0.037(12) -0.009(8) 0.008(8) 0.001(8) O49 0.058(17) 0.011(10) 0.038(14) -0.007(9) -0.009(11) -0.006(10) O50 0.024(15) 0.065(16) 0.034(15) -0.020(11) -0.005(11) 0.014(12) O51 0.044(15) 0.032(12) 0.031(12) -0.008(9) -0.017(10) 0.001(10) _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 As1 O1 1.794(12) . ? As1 O2 1.825(12) . ? As1 O3 1.827(13) . ? As2 O4 1.67(2) . ? As2 O5 1.684(17) . ? As2 O6 1.69(2) . ? As2 O7 1.733(19) . ? As3 O8 1.670(9) . ? As3 O9 1.675(18) . ? As3 O10 1.701(10) . ? As3 O11 1.70(2) . ? As4 O12 1.63(2) . ? As4 O13 1.655(19) . ? As4 O14 1.67(2) . ? As4 O15 1.71(2) . ? As5 O16 1.65(2) . ? As5 O17 1.67(2) . ? As5 O19 1.705(19) . ? As5 O18 1.73(2) . ? As6 O20 1.649(9) . ? As6 O21 1.675(11) . ? As6 O22 1.692(19) . ? As6 O23 1.72(2) . ? As7 O24 1.657(19) . ? As7 O27 1.67(3) . ? As7 O25 1.69(2) . ? As7 O26 1.71(2) . ? V1 O32 1.54(3) . ? V1 O6 1.98(2) . ? V1 O30 2.101(16) . ? V1 O33 2.105(14) . ? V1 O1 2.128(14) . ? V1 O34 2.42(2) . ? V2 O28 1.590(13) . ? V2 O29 1.711(16) . ? V2 O10 1.974(9) . ? V2 O1 2.078(12) . ? V2 O30 2.086(18) . ? V2 O31 2.402(10) . ? V3 O39 1.66(2) . ? V3 O40 1.687(13) . ? V3 O29 1.703(15) . ? V3 O15 1.92(2) . ? V3 O3 2.039(13) . ? V3 O41 2.34(2) . ? V4 O46 1.60(3) . ? V4 O40 1.680(13) . ? V4 O36 1.89(3) . ? V4 O18 1.94(2) . ? V4 O3 2.064(13) . ? V4 O45 2.36(2) . ? V5 O35 1.603(12) . ? V5 O37 1.88(3) . ? V5 O36 1.89(3) . ? V5 O21 1.985(11) . ? V5 O2 2.074(12) . ? V5 O38 2.332(9) . ? V6 O44 1.61(2) . ? V6 O37 1.88(3) . ? V6 O27 1.96(2) . ? V6 O2 2.112(13) . ? V6 O33 2.127(15) . ? V6 O43 2.36(2) . ? V7 O48 1.66(2) . ? V7 O34 1.741(19) . ? V7 O31 1.84(2) . ? V7 O7 1.989(19) . ? V7 O9 2.06(2) . ? V7 O30 2.416(19) . ? V8 O50 1.59(2) . ? V8 O45 1.92(2) . ? V8 O41 1.94(2) . ? V8 O17 1.989(19) . ? V8 O14 2.00(2) . ? V8 O40 2.876(17) . ? V9 O47 1.55(2) . ? V9 O43 1.764(18) . ? V9 O38 1.85(2) . ? V9 O26 1.94(2) . ? V9 O23 2.06(2) . ? V9 O37 2.58(3) . ? V10 O51 1.52(2) . ? V10 O41 1.82(2) . ? V10 O31 1.85(2) . ? V10 O13 2.02(2) . ? V10 O11 2.08(2) . ? V10 O29 2.87(2) . ? V11 O49 1.62(2) . ? V11 O45 1.80(2) . ? V11 O38 1.86(2) . ? V11 O22 2.05(2) . ? V11 O19 2.050(18) . ? V11 O36 2.53(4) . ? V12 O42 1.60(2) . ? V12 O34 1.94(2) . ? V12 O43 1.97(2) . ? V12 O4 2.019(19) . ? V12 O25 2.02(2) . ? V12 O33 2.368(15) . ? Ca1 O70 2.39(2) . ? Ca1 O66 2.41(2) . ? Ca1 O61 2.41(2) . ? Ca1 O74 2.42(3) . ? Ca1 O11 2.42(2) . ? Ca1 O52 2.44(2) . ? Ca1 O13 2.45(2) . ? Ca2 O58 2.34(2) . ? Ca2 O72 2.36(2) . ? Ca2 O7 2.39(2) . ? Ca2 O59 2.41(3) . ? Ca2 O64 2.41(2) . ? Ca2 O9 2.477(19) . ? Ca2 O71 2.53(2) . ? Ca3 O57 2.41(3) . ? Ca3 O54 2.41(3) . ? Ca3 O56 2.42(3) . ? Ca3 O26 2.43(2) . ? Ca3 O73 2.52(2) . ? Ca3 O23 2.53(2) . ? Ca4 O67 2.33(2) . ? Ca4 O19 2.35(2) . ? Ca4 O69 2.37(2) . ? Ca4 O55 2.392(19) . ? Ca4 O53 2.45(2) . ? Ca4 O62 2.483(19) . ? Ca4 O22 2.52(2) . ? Ca5 O5 2.23(2) . ? Ca5 O12 2.29(2) 1_545 ? Ca5 O65 2.399(15) . ? Ca5 O68 2.407(14) . ? Ca5 O60 2.426(19) . ? Ca5 O8 2.443(10) 2_547 ? Ca5 O10 2.930(10) 2_547 ? Ca6A O20 2.40(17) 1_455 ? Ca6A O18 2.63(17) 2_546 ? Ca6A O16 2.95(17) 2_546 ? Ca6A O79 3.02(17) . ? Ca6B O24 2.41(6) 2_556 ? Ca6B O16 2.44(6) 2_546 ? Ca6B O76 2.51(3) . ? Ca6B O75 2.58(3) . ? Ca6B O82 2.85(4) . ? Ca6C O24 2.19(4) 2_556 ? Ca6C O16 2.28(4) 2_546 ? Ca6C O20 2.61(3) 1_455 ? Ca6C O75 2.73(4) . ? Ca6C O21 2.922(17) 1_455 ? Ca6D O24 2.27(4) 2_556 ? Ca6D O16 2.33(4) 2_546 ? Ca6D O20 2.46(3) 1_455 ? Ca6D O76 2.76(4) . ? Ca6E O20 2.18(7) 1_455 ? Ca6E O24 2.26(7) 2_556 ? Ca6E O16 2.29(8) 2_546 ? Ca6E O75 2.32(6) . ? Ca6E O76 2.54(6) . ? Ca6E O21 2.93(6) 1_455 ? _refine_diff_density_max 2.119 _refine_diff_density_min -0.893 _refine_diff_density_rms 0.223 _shelxl_version_number 2013-4