data_BR9-c2c _audit_creation_method 'SHELXL-2016/6' _shelx_SHELXL_version_number '2016/6' _chemical_name_mineral 'ammoniolasalite' _chemical_compound_source 'Burro mine, Colorado' _chemical_formula_sum 'H45 K0.69 Mg2 N1.31 O48 V10' _chemical_formula_weight 1416.65 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' 'Mg' 'Mg' 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'K' 'K' 0.2009 0.2494 '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' _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_H-M_alt 'C 2/c' _space_group_name_Hall '-C 2yc' _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+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 24.478(3) _cell_length_b 10.9413(4) _cell_length_c 17.5508(12) _cell_angle_alpha 90 _cell_angle_beta 119.257(7) _cell_angle_gamma 90 _cell_volume 4100.9(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _exptl_crystal_density_diffrn 2.295 _exptl_crystal_F_000 2821 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.170 _exptl_crystal_size_min 0.160 _exptl_absorpt_coefficient_mu 2.406 _shelx_estimated_absorpt_T_min 0.645 _shelx_estimated_absorpt_T_max 0.699 _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 17595 _diffrn_reflns_av_unetI/netI 0.0268 _diffrn_reflns_av_R_equivalents 0.0296 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.115 _diffrn_reflns_theta_max 27.476 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measured_fraction_theta_full 0.995 _diffrn_reflns_Laue_measured_fraction_max 0.994 _diffrn_reflns_Laue_measured_fraction_full 0.995 _diffrn_reflns_point_group_measured_fraction_max 0.994 _diffrn_reflns_point_group_measured_fraction_full 0.995 _reflns_number_total 4684 _reflns_number_gt 3628 _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_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-2016/6 (Sheldrick, 2016)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ? _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^)+(0.0506P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refxyz _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 4684 _refine_ls_number_parameters 341 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.0458 _refine_ls_R_factor_gt 0.0357 _refine_ls_wR_factor_ref 0.0884 _refine_ls_wR_factor_gt 0.0831 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.071 _refine_ls_shift/su_max 0.001 _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 V1 V 0.01373(2) 0.09591(3) 0.85111(2) 0.01581(10) Uani 1 1 d . . . . . V2 V -0.07104(2) -0.10769(3) 0.71750(2) 0.01835(11) Uani 1 1 d . . . . . V3 V 0.07055(2) 0.30260(3) 0.78148(2) 0.01857(10) Uani 1 1 d . . . . . V4 V 0.12815(2) 0.09627(3) 0.71820(2) 0.02047(11) Uani 1 1 d . . . . . V5 V 0.15482(2) 0.09919(3) 0.90732(2) 0.02149(11) Uani 1 1 d . . . . . Mg Mg 0.11231(4) 0.59803(6) 0.59049(4) 0.02225(17) Uani 1 1 d . . . . . N N 0.19594(8) 0.18515(16) 0.54271(9) 0.0775(8) Uani 0.650(4) 1 d . . P . . K K 0.19594(8) 0.18515(16) 0.54271(9) 0.0775(8) Uani 0.350(4) 1 d . . P . . O1 O -0.03813(7) 0.09791(12) 0.88788(9) 0.0214(3) Uani 1 1 d . . . . . O2 O 0.08604(7) 0.09625(12) 0.94082(9) 0.0213(3) Uani 1 1 d . . . . . O3 O -0.01123(7) -0.07523(12) 0.67332(9) 0.0174(3) Uani 1 1 d . . . . . O4 O 0.01115(6) 0.26853(12) 0.82651(8) 0.0175(3) Uani 1 1 d . . . . . O5 O -0.06153(7) 0.09706(12) 0.72373(8) 0.0163(3) Uani 1 1 d . . . . . O6 O -0.07131(7) -0.25453(14) 0.71741(9) 0.0289(4) Uani 1 1 d . . . . . O7 O -0.13640(7) -0.06908(13) 0.61253(9) 0.0227(3) Uani 1 1 d . . . . . O8 O -0.11202(7) -0.06959(13) 0.77895(9) 0.0217(3) Uani 1 1 d . . . . . O9 O 0.13631(7) 0.26565(13) 0.88920(9) 0.0223(3) Uani 1 1 d . . . . . O10 O 0.11222(7) 0.26450(13) 0.72161(9) 0.0211(3) Uani 1 1 d . . . . . O11 O 0.16648(8) 0.09591(14) 0.66609(10) 0.0315(4) Uani 1 1 d . . . . . O12 O 0.18838(7) 0.09829(13) 0.83404(9) 0.0233(3) Uani 1 1 d . . . . . O13 O 0.07059(7) 0.44921(15) 0.78067(9) 0.0293(4) Uani 1 1 d . . . . . O14 O 0.21472(8) 0.09774(14) 0.00352(10) 0.0329(4) Uani 1 1 d . . . . . OW1 O 0.11240(9) 0.40853(15) 0.59515(11) 0.0316(4) Uani 1 1 d D . . . . H1A H 0.1170(12) 0.369(2) 0.6379(13) 0.038 Uiso 1 1 d D U . . . H1B H 0.0967(13) 0.376(2) 0.5545(13) 0.038 Uiso 1 1 d D U . . . OW2 O 0.04240(9) 0.40908(16) 0.96422(10) 0.0316(4) Uani 1 1 d D . . . . H2A H 0.0327(12) 0.3592(19) 0.9265(14) 0.038 Uiso 1 1 d D U . . . H2B H 0.0230(12) 0.4696(18) 0.9389(15) 0.038 Uiso 1 1 d D U . . . OW3 O 0.17764(9) 0.60190(16) 0.54574(12) 0.0329(4) Uani 1 1 d D . . . . H3A H 0.2147(10) 0.614(2) 0.5774(15) 0.039 Uiso 1 1 d D U . . . H3B H 0.1684(11) 0.647(2) 0.5028(14) 0.039 Uiso 1 1 d D U . . . OW4 O 0.17833(10) 0.59674(16) 0.71752(11) 0.0404(5) Uani 1 1 d D . . . . H4A H 0.1940(13) 0.6553(19) 0.7409(17) 0.048 Uiso 1 1 d D U . . . H4B H 0.1960(13) 0.5390(19) 0.7491(16) 0.048 Uiso 1 1 d D U . . . OW5 O 0.03886(9) 0.60281(15) 0.62316(11) 0.0311(4) Uani 1 1 d D . . . . H5A H 0.0517(13) 0.604(2) 0.6740(13) 0.037 Uiso 1 1 d D U . . . H5B H 0.0166(11) 0.655(2) 0.5998(14) 0.037 Uiso 1 1 d D U . . . OW6 O 0.11169(9) 0.21342(15) 0.09362(10) 0.0367(5) Uani 1 1 d D . . . . H6A H 0.1131(13) 0.171(2) 0.1301(14) 0.044 Uiso 1 1 d D U . . . H6B H 0.0992(12) 0.173(2) 0.0506(13) 0.044 Uiso 1 1 d D U . . . OW7 O 0.26938(10) -0.31096(18) 0.19557(14) 0.0495(5) Uani 1 1 d D . . . . H7A H 0.2586(14) -0.345(3) 0.2262(18) 0.059 Uiso 1 1 d D U . . . H7B H 0.2948(13) -0.360(3) 0.1939(19) 0.059 Uiso 1 1 d D U . . . OW8 O -0.04867(9) -0.21599(16) 0.52786(11) 0.0376(4) Uani 1 1 d D . . . . H8A H -0.0470(12) -0.176(2) 0.4873(14) 0.045 Uiso 1 1 d D U . . . H8B H -0.0400(13) -0.166(2) 0.5650(14) 0.045 Uiso 1 1 d D U . . . OW9 O 0.17776(15) -0.3853(3) 0.9296(2) 0.0956(11) Uani 1 1 d D . . . . H9A H 0.178(2) -0.449(3) 0.945(3) 0.115 Uiso 1 1 d D U . . . H9B H 0.1501(18) -0.364(4) 0.886(2) 0.115 Uiso 1 1 d D U . . . OW10 O 0.22757(9) 0.61362(17) 0.31000(12) 0.0412(5) Uani 1 1 d D . . . . H10A H 0.2479(13) 0.616(2) 0.3614(14) 0.049 Uiso 1 1 d D U . . . H10B H 0.2007(11) 0.664(2) 0.3028(16) 0.049 Uiso 1 1 d D U . . . 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 V1 0.0182(2) 0.01678(19) 0.01317(18) -0.00030(12) 0.00826(15) 0.00041(14) V2 0.0206(2) 0.0161(2) 0.0196(2) -0.00106(13) 0.01081(16) -0.00259(14) V3 0.0190(2) 0.0163(2) 0.0210(2) -0.00075(13) 0.01022(16) -0.00226(14) V4 0.0201(2) 0.0230(2) 0.0216(2) 0.00094(14) 0.01280(16) 0.00063(15) V5 0.0170(2) 0.0273(2) 0.01721(19) -0.00050(14) 0.00602(15) 0.00094(15) Mg 0.0232(4) 0.0226(4) 0.0196(4) 0.0025(3) 0.0094(3) -0.0008(3) N 0.0942(14) 0.0969(15) 0.0443(9) -0.0178(8) 0.0360(8) -0.0341(10) K 0.0942(14) 0.0969(15) 0.0443(9) -0.0178(8) 0.0360(8) -0.0341(10) O1 0.0237(8) 0.0242(8) 0.0190(7) -0.0002(6) 0.0126(6) 0.0003(6) O2 0.0209(8) 0.0250(8) 0.0171(7) -0.0004(5) 0.0086(6) -0.0004(6) O3 0.0196(8) 0.0176(8) 0.0165(7) -0.0011(5) 0.0100(6) 0.0000(6) O4 0.0192(8) 0.0156(7) 0.0190(7) -0.0023(5) 0.0104(6) -0.0010(6) O5 0.0160(7) 0.0177(8) 0.0149(7) 0.0000(5) 0.0074(6) 0.0005(6) O6 0.0349(10) 0.0192(8) 0.0326(9) 0.0004(6) 0.0166(8) -0.0030(7) O7 0.0224(8) 0.0245(8) 0.0194(7) -0.0039(6) 0.0088(6) -0.0040(6) O8 0.0247(8) 0.0214(8) 0.0233(8) 0.0001(6) 0.0152(7) -0.0036(6) O9 0.0195(8) 0.0242(8) 0.0209(7) -0.0037(6) 0.0081(6) -0.0038(6) O10 0.0227(8) 0.0199(8) 0.0235(7) 0.0004(6) 0.0135(6) -0.0035(6) O11 0.0316(10) 0.0392(10) 0.0323(9) 0.0031(7) 0.0223(8) 0.0022(8) O12 0.0176(8) 0.0278(9) 0.0246(8) 0.0013(6) 0.0104(6) 0.0027(6) O13 0.0324(10) 0.0200(8) 0.0376(10) -0.0006(6) 0.0187(8) -0.0032(7) O14 0.0230(9) 0.0427(11) 0.0239(9) 0.0006(7) 0.0043(7) 0.0010(7) OW1 0.0448(12) 0.0247(9) 0.0245(9) 0.0024(7) 0.0162(9) -0.0030(8) OW2 0.0359(10) 0.0302(10) 0.0200(9) -0.0048(6) 0.0070(7) 0.0096(8) OW3 0.0246(9) 0.0410(11) 0.0334(10) 0.0089(7) 0.0144(8) 0.0012(8) OW4 0.0429(12) 0.0304(10) 0.0278(10) 0.0038(7) 0.0016(8) -0.0030(8) OW5 0.0340(10) 0.0344(10) 0.0265(9) 0.0011(7) 0.0158(8) 0.0014(7) OW6 0.0664(13) 0.0205(9) 0.0264(9) -0.0018(7) 0.0253(9) -0.0030(8) OW7 0.0376(12) 0.0409(13) 0.0679(14) 0.0068(10) 0.0243(10) 0.0075(9) OW8 0.0564(12) 0.0319(10) 0.0293(9) -0.0082(7) 0.0247(9) -0.0088(9) OW9 0.084(2) 0.0641(19) 0.086(2) 0.0252(15) 0.0002(16) 0.0011(16) OW10 0.0341(11) 0.0421(12) 0.0327(10) -0.0046(8) 0.0049(8) 0.0113(8) _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 V1 O1 1.6821(16) . ? V1 O2 1.6994(15) . ? V1 O3 1.9153(14) 2_556 ? V1 O4 1.9315(14) . ? V1 O5 2.0896(14) . ? V1 O5 2.1439(14) 2_556 ? V1 V4 3.0679(6) 2_556 ? V1 V5 3.0937(6) . ? V2 O6 1.6066(16) . ? V2 O7 1.8031(15) . ? V2 O8 1.8441(15) . ? V2 O3 1.9951(15) . ? V2 O3 2.0202(14) 2_556 ? V2 O5 2.2495(13) . ? V2 V2 3.0852(8) 2_556 ? V2 N 4.1563(14) 5_556 ? V3 O13 1.6042(17) . ? V3 O9 1.8314(14) . ? V3 O10 1.8348(15) . ? V3 O4 2.0001(14) . ? V3 O4 2.0064(14) 2_556 ? V3 O5 2.2571(13) 2_556 ? V3 V3 3.0691(8) 2_556 ? V3 V5 3.1037(5) . ? V4 O11 1.5984(16) . ? V4 O12 1.8378(15) . ? V4 O8 1.8630(15) 2_556 ? V4 O10 1.8885(15) . ? V4 O1 2.0766(16) 2_556 ? V4 O5 2.3072(14) 2_556 ? V4 V5 3.0540(5) . ? V4 N 4.2639(15) . ? V5 O14 1.6066(16) 1_556 ? V5 O12 1.8337(16) . ? V5 O9 1.8662(15) . ? V5 O7 1.8869(15) 2_556 ? V5 O2 2.0368(16) . ? V5 O5 2.3176(14) 2_556 ? V5 N 3.7416(16) 6_556 ? Mg OW4 2.0151(19) . ? Mg OW2 2.0345(17) 6_565 ? Mg OW6 2.0640(18) 6_566 ? Mg OW1 2.0750(17) . ? Mg OW3 2.099(2) . ? Mg OW5 2.138(2) . ? N O7 2.6980(19) 5_556 ? N OW7 2.759(2) 6_556 ? N O11 2.773(2) . ? N OW9 2.841(4) 6 ? N OW9 2.987(4) 4_556 ? N OW8 3.206(3) 5_556 ? N O14 3.252(2) 6_556 ? N OW1 3.584(3) . ? OW1 H1A 0.823(19) . ? OW1 H1B 0.717(19) . ? OW2 H2A 0.799(19) . ? OW2 H2B 0.810(19) . ? OW3 H3A 0.81(2) . ? OW3 H3B 0.837(19) . ? OW4 H4A 0.757(19) . ? OW4 H4B 0.812(19) . ? OW5 H5A 0.788(19) . ? OW5 H5B 0.759(19) . ? OW6 H6A 0.779(19) . ? OW6 H6B 0.797(19) . ? OW7 H7A 0.79(2) . ? OW7 H7B 0.84(2) . ? OW8 H8A 0.853(19) . ? OW8 H8B 0.79(2) . ? OW9 H9A 0.75(2) . ? OW9 H9B 0.77(2) . ? OW10 H10A 0.79(2) . ? OW10 H10B 0.82(2) . ? 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 O1 V1 O2 106.50(8) . . ? O1 V1 O3 98.69(6) . 2_556 ? O2 V1 O3 96.57(6) . 2_556 ? O1 V1 O4 97.16(6) . . ? O2 V1 O4 96.34(6) . . ? O3 V1 O4 155.78(6) 2_556 . ? O1 V1 O5 88.53(7) . . ? O2 V1 O5 164.95(7) . . ? O3 V1 O5 81.45(6) 2_556 . ? O4 V1 O5 80.77(5) . . ? O1 V1 O5 167.21(6) . 2_556 ? O2 V1 O5 86.24(7) . 2_556 ? O3 V1 O5 80.55(6) 2_556 2_556 ? O4 V1 O5 79.94(5) . 2_556 ? O5 V1 O5 78.71(6) . 2_556 ? O1 V1 V4 39.80(5) . 2_556 ? O2 V1 V4 146.30(5) . 2_556 ? O3 V1 V4 90.37(4) 2_556 2_556 ? O4 V1 V4 90.18(4) . 2_556 ? O5 V1 V4 48.74(4) . 2_556 ? O5 V1 V4 127.45(4) 2_556 2_556 ? O1 V1 V5 144.26(5) . . ? O2 V1 V5 37.78(5) . . ? O3 V1 V5 89.50(4) 2_556 . ? O4 V1 V5 88.25(4) . . ? O5 V1 V5 127.17(4) . . ? O5 V1 V5 48.46(4) 2_556 . ? V4 V1 V5 175.852(14) 2_556 . ? O6 V2 O7 103.42(7) . . ? O6 V2 O8 102.91(7) . . ? O7 V2 O8 94.58(7) . . ? O6 V2 O3 100.44(7) . . ? O7 V2 O3 90.82(6) . . ? O8 V2 O3 154.07(6) . . ? O6 V2 O3 100.28(6) . 2_556 ? O7 V2 O3 154.59(7) . 2_556 ? O8 V2 O3 88.89(6) . 2_556 ? O3 V2 O3 75.91(6) . 2_556 ? O6 V2 O5 175.03(7) . . ? O7 V2 O5 80.52(6) . . ? O8 V2 O5 79.60(6) . . ? O3 V2 O5 76.31(5) . . ? O3 V2 O5 75.36(5) 2_556 . ? O6 V2 V2 90.22(6) . 2_556 ? O7 V2 V2 130.90(5) . 2_556 ? O8 V2 V2 128.38(5) . 2_556 ? O3 V2 V2 40.09(4) . 2_556 ? O3 V2 V2 39.49(4) 2_556 2_556 ? O5 V2 V2 84.89(4) . 2_556 ? O6 V2 N 78.15(6) . 5_556 ? O7 V2 N 27.90(5) . 5_556 ? O8 V2 N 111.74(5) . 5_556 ? O3 V2 N 83.95(5) . 5_556 ? O3 V2 N 159.22(5) 2_556 5_556 ? O5 V2 N 105.04(4) . 5_556 ? V2 V2 N 119.81(3) 2_556 5_556 ? O13 V3 O9 103.05(7) . . ? O13 V3 O10 102.66(7) . . ? O9 V3 O10 94.98(7) . . ? O13 V3 O4 101.16(7) . . ? O9 V3 O4 89.60(6) . . ? O10 V3 O4 154.02(6) . . ? O13 V3 O4 100.49(7) . 2_556 ? O9 V3 O4 154.36(6) . 2_556 ? O10 V3 O4 89.62(6) . 2_556 ? O4 V3 O4 75.95(6) . 2_556 ? O13 V3 O5 175.14(7) . 2_556 ? O9 V3 O5 80.86(6) . 2_556 ? O10 V3 O5 79.70(6) . 2_556 ? O4 V3 O5 75.80(5) . 2_556 ? O4 V3 O5 75.17(5) 2_556 2_556 ? O13 V3 V3 90.13(6) . 2_556 ? O9 V3 V3 129.68(5) . 2_556 ? O10 V3 V3 129.54(5) . 2_556 ? O4 V3 V3 40.08(4) . 2_556 ? O4 V3 V3 39.93(4) 2_556 2_556 ? O5 V3 V3 85.12(4) 2_556 2_556 ? O13 V3 V5 136.07(5) . . ? O9 V3 V5 33.28(5) . . ? O10 V3 V5 83.25(5) . . ? O4 V3 V5 86.78(4) . . ? O4 V3 V5 123.23(4) 2_556 . ? O5 V3 V5 48.10(4) 2_556 . ? V3 V3 V5 119.722(13) 2_556 . ? O11 V4 O12 104.78(8) . . ? O11 V4 O8 101.79(7) . 2_556 ? O12 V4 O8 92.75(6) . 2_556 ? O11 V4 O10 102.03(7) . . ? O12 V4 O10 91.13(6) . . ? O8 V4 O10 154.00(7) 2_556 . ? O11 V4 O1 98.59(8) . 2_556 ? O12 V4 O1 156.60(7) . 2_556 ? O8 V4 O1 83.49(6) 2_556 2_556 ? O10 V4 O1 82.81(6) . 2_556 ? O11 V4 O5 172.73(7) . 2_556 ? O12 V4 O5 82.49(6) . 2_556 ? O8 V4 O5 77.70(6) 2_556 2_556 ? O10 V4 O5 77.34(6) . 2_556 ? O1 V4 O5 74.14(6) 2_556 2_556 ? O11 V4 V5 138.45(6) . . ? O12 V4 V5 33.67(5) . . ? O8 V4 V5 85.21(4) 2_556 . ? O10 V4 V5 83.87(4) . . ? O1 V4 V5 122.95(4) 2_556 . ? O5 V4 V5 48.82(3) 2_556 . ? O11 V4 V1 129.82(6) . 2_556 ? O12 V4 V1 125.40(5) . 2_556 ? O8 V4 V1 78.21(5) 2_556 2_556 ? O10 V4 V1 78.61(5) . 2_556 ? O1 V4 V1 31.24(4) 2_556 2_556 ? O5 V4 V1 42.91(3) 2_556 2_556 ? V5 V4 V1 91.726(15) . 2_556 ? O11 V4 N 16.84(6) . . ? O12 V4 N 114.29(5) . . ? O8 V4 N 113.83(5) 2_556 . ? O10 V4 N 87.70(5) . . ? O1 V4 N 88.13(5) 2_556 . ? O5 V4 N 157.95(4) 2_556 . ? V5 V4 N 146.18(2) . . ? V1 V4 N 118.60(3) 2_556 . ? O14 V5 O12 104.20(8) 1_556 . ? O14 V5 O9 102.10(7) 1_556 . ? O12 V5 O9 92.31(6) . . ? O14 V5 O7 101.39(7) 1_556 2_556 ? O12 V5 O7 90.78(6) . 2_556 ? O9 V5 O7 154.76(7) . 2_556 ? O14 V5 O2 98.93(8) 1_556 . ? O12 V5 O2 156.82(7) . . ? O9 V5 O2 84.19(6) . . ? O7 V5 O2 83.19(6) 2_556 . ? O14 V5 O5 173.41(8) 1_556 2_556 ? O12 V5 O5 82.28(6) . 2_556 ? O9 V5 O5 78.54(5) . 2_556 ? O7 V5 O5 77.07(5) 2_556 2_556 ? O2 V5 O5 74.56(6) . 2_556 ? O14 V5 V4 137.95(7) 1_556 . ? O12 V5 V4 33.76(5) . . ? O9 V5 V4 85.40(4) . . ? O7 V5 V4 83.35(4) 2_556 . ? O2 V5 V4 123.08(4) . . ? O5 V5 V4 48.53(4) 2_556 . ? O14 V5 V1 129.67(7) 1_556 . ? O12 V5 V1 126.10(5) . . ? O9 V5 V1 79.45(5) . . ? O7 V5 V1 78.53(5) 2_556 . ? O2 V5 V1 30.74(4) . . ? O5 V5 V1 43.82(4) 2_556 . ? V4 V5 V1 92.347(15) . . ? O14 V5 V3 134.64(6) 1_556 . ? O12 V5 V3 82.79(5) . . ? O9 V5 V3 32.58(4) . . ? O7 V5 V3 123.54(5) 2_556 . ? O2 V5 V3 82.02(4) . . ? O5 V5 V3 46.46(3) 2_556 . ? V4 V5 V3 61.275(12) . . ? V1 V5 V3 62.050(12) . . ? O14 V5 N 60.02(6) 1_556 6_556 ? O12 V5 N 111.55(5) . 6_556 ? O9 V5 N 152.54(5) . 6_556 ? O7 V5 N 43.27(5) 2_556 6_556 ? O2 V5 N 78.89(5) . 6_556 ? O5 V5 N 116.79(4) 2_556 6_556 ? V4 V5 N 121.99(3) . 6_556 ? V1 V5 N 96.02(3) . 6_556 ? V3 V5 N 157.99(3) . 6_556 ? OW4 Mg OW2 176.14(8) . 6_565 ? OW4 Mg OW6 89.43(8) . 6_566 ? OW2 Mg OW6 93.09(7) 6_565 6_566 ? OW4 Mg OW1 87.97(7) . . ? OW2 Mg OW1 89.36(7) 6_565 . ? OW6 Mg OW1 176.02(8) 6_566 . ? OW4 Mg OW3 93.93(9) . . ? OW2 Mg OW3 88.98(8) 6_565 . ? OW6 Mg OW3 90.39(8) 6_566 . ? OW1 Mg OW3 92.79(8) . . ? OW4 Mg OW5 91.62(8) . . ? OW2 Mg OW5 85.59(8) 6_565 . ? OW6 Mg OW5 87.15(8) 6_566 . ? OW1 Mg OW5 89.92(7) . . ? OW3 Mg OW5 173.91(7) . . ? O7 N OW7 172.16(9) 5_556 6_556 ? O7 N O11 113.87(7) 5_556 . ? OW7 N O11 73.19(7) 6_556 . ? O7 N OW9 80.47(7) 5_556 6 ? OW7 N OW9 95.74(8) 6_556 6 ? O11 N OW9 143.64(11) . 6 ? O7 N OW9 92.76(8) 5_556 4_556 ? OW7 N OW9 80.79(8) 6_556 4_556 ? O11 N OW9 115.20(10) . 4_556 ? OW9 N OW9 96.25(9) 6 4_556 ? O7 N OW8 73.08(6) 5_556 5_556 ? OW7 N OW8 113.48(8) 6_556 5_556 ? O11 N OW8 70.50(6) . 5_556 ? OW9 N OW8 83.47(9) 6 5_556 ? OW9 N OW8 165.72(8) 4_556 5_556 ? O7 N O14 53.19(5) 5_556 6_556 ? OW7 N O14 126.04(8) 6_556 6_556 ? O11 N O14 87.00(6) . 6_556 ? OW9 N O14 125.17(8) 6 6_556 ? OW9 N O14 63.04(7) 4_556 6_556 ? OW8 N O14 105.48(6) 5_556 6_556 ? O7 N OW1 119.08(7) 5_556 . ? OW7 N OW1 65.94(6) 6_556 . ? O11 N OW1 68.94(5) . . ? OW9 N OW1 74.90(9) 6 . ? OW9 N OW1 144.05(8) 4_556 . ? OW8 N OW1 49.64(5) 5_556 . ? O14 N OW1 149.42(6) 6_556 . ? V1 O1 V4 108.96(7) . 2_556 ? V1 O2 V5 111.47(7) . . ? V1 O2 N 126.57(7) . 6_556 ? V5 O2 N 70.28(5) . 6_556 ? V1 O3 V2 108.16(7) 2_556 . ? V1 O3 V2 106.99(6) 2_556 2_556 ? V2 O3 V2 100.41(6) . 2_556 ? V1 O4 V3 108.65(7) . . ? V1 O4 V3 107.54(6) . 2_556 ? V3 O4 V3 100.00(6) . 2_556 ? V1 O5 V1 101.28(6) . 2_556 ? V1 O5 V2 93.56(5) . . ? V1 O5 V2 92.23(5) 2_556 . ? V1 O5 V3 93.84(5) . 2_556 ? V1 O5 V3 93.04(5) 2_556 2_556 ? V2 O5 V3 169.91(7) . 2_556 ? V1 O5 V4 88.35(5) . 2_556 ? V1 O5 V4 170.34(7) 2_556 2_556 ? V2 O5 V4 86.50(5) . 2_556 ? V3 O5 V4 86.87(5) 2_556 2_556 ? V1 O5 V5 171.00(7) . 2_556 ? V1 O5 V5 87.71(5) 2_556 2_556 ? V2 O5 V5 86.18(5) . 2_556 ? V3 O5 V5 85.43(5) 2_556 2_556 ? V4 O5 V5 82.65(5) 2_556 2_556 ? V2 O6 N 79.51(6) . 5_556 ? V2 O7 V5 115.46(7) . 2_556 ? V2 O7 N 133.88(8) . 5_556 ? V5 O7 N 108.08(7) 2_556 5_556 ? V2 O8 V4 114.77(8) . 2_556 ? V3 O9 V5 114.15(7) . . ? V3 O10 V4 114.88(7) . . ? V4 O11 N 153.55(10) . . ? V5 O12 V4 112.57(8) . . ? V5 O14 N 94.64(7) 1_554 6 ? Mg OW1 N 131.39(8) . . ? Mg OW1 H1A 123.5(18) . . ? N OW1 H1A 92.2(19) . . ? Mg OW1 H1B 118(2) . . ? N OW1 H1B 60(2) . . ? H1A OW1 H1B 115(3) . . ? Mg OW2 H2A 128.9(17) 6_566 . ? Mg OW2 H2B 125.8(17) 6_566 . ? H2A OW2 H2B 104(2) . . ? Mg OW3 H3A 123.4(19) . . ? Mg OW3 H3B 115.5(18) . . ? H3A OW3 H3B 104(2) . . ? Mg OW4 N 165.35(8) . 4_556 ? Mg OW4 H4A 121(2) . . ? N OW4 H4A 45(2) 4_556 . ? Mg OW4 H4B 129.2(19) . . ? N OW4 H4B 65.4(19) 4_556 . ? H4A OW4 H4B 109(3) . . ? Mg OW5 H5A 112(2) . . ? Mg OW5 H5B 110(2) . . ? H5A OW5 H5B 113(2) . . ? Mg OW6 H6A 128.4(19) 6_565 . ? Mg OW6 H6B 122.5(19) 6_565 . ? H6A OW6 H6B 107(2) . . ? N OW7 H7A 128(2) 6 . ? N OW7 H7B 116(2) 6 . ? H7A OW7 H7B 103(3) . . ? N OW8 H8A 97.3(18) 5_556 . ? N OW8 H8B 92(2) 5_556 . ? H8A OW8 H8B 103(2) . . ? N OW9 N 83.75(9) 6_556 4_546 ? N OW9 H9A 119(4) 6_556 . ? N OW9 H9A 111(4) 4_546 . ? N OW9 H9B 103(3) 6_556 . ? N OW9 H9B 114(4) 4_546 . ? H9A OW9 H9B 120(4) . . ? N OW10 H10A 56.9(19) 7_556 . ? N OW10 H10B 137(2) 7_556 . ? H10A OW10 H10B 100(2) . . ? _refine_diff_density_max 1.393 _refine_diff_density_min -0.628 _refine_diff_density_rms 0.201 _shelx_res_file ; TITL PMA-BR-009 BR9-c2c.res created by SHELXL-2016/6 at 19:15:43 on 19-Oct-2017 REM transformed to space group : CELL 0.71075 24.4783 10.9413 17.5508 90.000 119.257 90.000 ZERR 4 0.0028 0.0004 0.0012 0.000 0.007 0.000 LATT 7 SYMM -X,+Y,1/2-Z SFAC H MG N K O V UNIT 180 8 5.25 2.75 192 40 L.S. 20 OMIT -28 6 14 OMIT -1 3 5 OMIT -3 3 5 OMIT 7 3 1 OMIT -4 2 7 OMIT -3 3 6 OMIT -8 2 1 OMIT -5 3 9 OMIT -1 1 2 OMIT -3 3 7 OMIT -4 4 7 BOND $H DFIX 0.82 0.03 OW1 H1a OW1 H1b OW2 H2a OW2 H2b OW3 H3a OW3 H3b DFIX 0.82 0.03 OW4 H4a OW4 H4b OW5 H5a OW5 H5b OW6 H6a OW6 H6b DFIX 0.82 0.03 OW7 H7a OW7 H7b OW8 H8a OW8 H8b OW9 H9a OW9 H9b DFIX 0.82 0.03 OW10 H10a OW10 H10b DFIX 1.30 0.03 H1a H1b H2a H2b H3a H3b H4a H4b H5a H5b DFIX 1.30 0.03 H6a H6b H7a H7b H8a H8b H9a H9b H10a H10b HTAB CONN 8 3.0 N EXYZ N K EADP N K FMAP 2 PLAN 50 ACTA SIZE 0.200 0.170 0.160 WGHT 0.050600 FVAR 0.08562 0.65008 V1 6 0.013730 0.095909 0.851107 11.00000 0.01824 0.01678 = 0.01317 -0.00030 0.00826 0.00041 V2 6 -0.071039 -0.107694 0.717504 11.00000 0.02062 0.01608 = 0.01960 -0.00106 0.01081 -0.00259 V3 6 0.070548 0.302596 0.781481 11.00000 0.01900 0.01631 = 0.02097 -0.00075 0.01022 -0.00226 V4 6 0.128152 0.096265 0.718200 11.00000 0.02007 0.02304 = 0.02165 0.00094 0.01280 0.00063 V5 6 0.154815 0.099189 0.907325 11.00000 0.01697 0.02728 = 0.01721 -0.00050 0.00602 0.00094 MG 2 0.112314 0.598034 0.590491 11.00000 0.02324 0.02256 = 0.01957 0.00254 0.00939 -0.00079 N 3 0.195941 0.185146 0.542710 21.00000 0.09424 0.09686 = 0.04426 -0.01781 0.03605 -0.03414 K 4 0.195941 0.185146 0.542710 -21.00000 0.09424 0.09686 = 0.04426 -0.01781 0.03605 -0.03414 O1 5 -0.038128 0.097905 0.887884 11.00000 0.02370 0.02421 = 0.01896 -0.00017 0.01256 0.00029 O2 5 0.086037 0.096248 0.940825 11.00000 0.02094 0.02502 = 0.01708 -0.00043 0.00862 -0.00045 O3 5 -0.011227 -0.075234 0.673325 11.00000 0.01958 0.01763 = 0.01653 -0.00113 0.00995 0.00004 O4 5 0.011152 0.268529 0.826511 11.00000 0.01921 0.01560 = 0.01899 -0.00229 0.01041 -0.00103 O5 5 -0.061529 0.097064 0.723726 11.00000 0.01595 0.01773 = 0.01491 0.00003 0.00736 0.00047 O6 5 -0.071313 -0.254534 0.717415 11.00000 0.03493 0.01922 = 0.03265 0.00038 0.01661 -0.00296 O7 5 -0.136395 -0.069075 0.612533 11.00000 0.02242 0.02447 = 0.01939 -0.00391 0.00882 -0.00404 O8 5 -0.112022 -0.069589 0.778949 11.00000 0.02475 0.02139 = 0.02328 0.00012 0.01520 -0.00362 O9 5 0.136315 0.265648 0.889195 11.00000 0.01953 0.02418 = 0.02088 -0.00365 0.00813 -0.00378 O10 5 0.112223 0.264496 0.721606 11.00000 0.02270 0.01994 = 0.02355 0.00042 0.01348 -0.00349 O11 5 0.166476 0.095913 0.666092 11.00000 0.03163 0.03916 = 0.03228 0.00311 0.02229 0.00223 O12 5 0.188377 0.098286 0.834036 11.00000 0.01760 0.02779 = 0.02458 0.00127 0.01036 0.00265 O13 5 0.070591 0.449206 0.780674 11.00000 0.03236 0.01996 = 0.03758 -0.00064 0.01874 -0.00323 O14 5 0.214724 0.097744 0.003523 11.00000 0.02295 0.04265 = 0.02390 0.00056 0.00431 0.00096 OW1 5 0.112404 0.408530 0.595155 11.00000 0.04477 0.02466 = 0.02452 0.00237 0.01621 -0.00296 H1A 1 0.117014 0.369458 0.637946 11.00000 -1.20000 H1B 1 0.096692 0.376156 0.554484 11.00000 -1.20000 OW2 5 0.042404 0.409084 0.964215 11.00000 0.03590 0.03025 = 0.02004 -0.00485 0.00701 0.00957 H2A 1 0.032682 0.359249 0.926491 11.00000 -1.20000 H2B 1 0.023025 0.469646 0.938888 11.00000 -1.20000 OW3 5 0.177642 0.601898 0.545735 11.00000 0.02456 0.04102 = 0.03340 0.00886 0.01437 0.00118 H3A 1 0.214706 0.613506 0.577368 11.00000 -1.20000 H3B 1 0.168430 0.647368 0.502790 11.00000 -1.20000 OW4 5 0.178331 0.596738 0.717519 11.00000 0.04290 0.03037 = 0.02776 0.00377 0.00159 -0.00301 H4A 1 0.194002 0.655325 0.740869 11.00000 -1.20000 H4B 1 0.195981 0.538992 0.749076 11.00000 -1.20000 OW5 5 0.038862 0.602811 0.623161 11.00000 0.03395 0.03435 = 0.02646 0.00113 0.01584 0.00141 H5A 1 0.051677 0.603870 0.673985 11.00000 -1.20000 H5B 1 0.016634 0.655346 0.599775 11.00000 -1.20000 OW6 5 0.111688 0.213419 0.093618 11.00000 0.06645 0.02054 = 0.02639 -0.00175 0.02535 -0.00300 H6A 1 0.113136 0.170910 0.130144 11.00000 -1.20000 H6B 1 0.099192 0.172737 0.050638 11.00000 -1.20000 OW7 5 0.269379 -0.310959 0.195569 11.00000 0.03761 0.04092 = 0.06789 0.00677 0.02425 0.00746 H7A 1 0.258610 -0.344509 0.226155 11.00000 -1.20000 H7B 1 0.294788 -0.360344 0.193903 11.00000 -1.20000 OW8 5 -0.048668 -0.215990 0.527856 11.00000 0.05636 0.03191 = 0.02931 -0.00820 0.02472 -0.00881 H8A 1 -0.047016 -0.175979 0.487331 11.00000 -1.20000 H8B 1 -0.040034 -0.166410 0.564993 11.00000 -1.20000 OW9 5 0.177760 -0.385308 0.929611 11.00000 0.08392 0.06411 = 0.08581 0.02516 0.00021 0.00106 H9A 1 0.177857 -0.448974 0.945385 11.00000 -1.20000 H9B 1 0.150141 -0.363589 0.885566 11.00000 -1.20000 OW10 5 0.227575 0.613618 0.310003 11.00000 0.03411 0.04208 = 0.03269 -0.00457 0.00495 0.01131 H10A 1 0.247853 0.615786 0.361398 11.00000 -1.20000 H10B 1 0.200692 0.663556 0.302808 11.00000 -1.20000 HKLF 4 REM PMA-BR-009 REM R1 = 0.0357 for 3628 Fo > 4sig(Fo) and 0.0458 for all 4684 data REM 341 parameters refined using 30 restraints END WGHT 0.0506 0.0000 REM Instructions for potential hydrogen bonds HTAB OW1 O10 EQIV $2 -x, -y, -z+1 HTAB OW1 OW8_$2 HTAB OW2 O4 EQIV $1 -x, y, -z+3/2 HTAB OW2 OW5_$1 EQIV $9 -x+1/2, y+1/2, -z+3/2 HTAB OW3 O12_$9 EQIV $5 x, -y+1, z-1/2 HTAB OW3 O9_$5 EQIV $7 -x+1/2, -y+1/2, -z+1 HTAB OW4 OW7_$7 EQIV $6 x, -y+1, z+1/2 HTAB OW4 OW10_$6 EQIV $12 -x, y+1, -z+3/2 HTAB OW5 O6_$12 HTAB OW5 O13 EQIV $13 x, y+1, z HTAB OW5 OW8_$13 HTAB OW6 O8_$2 EQIV $3 x, y, z-1 HTAB OW6 O2_$3 EQIV $14 x, y-1, z HTAB OW7 OW10_$14 EQIV $15 x+1/2, -y-1/2, z-1/2 HTAB OW7 O8_$15 EQIV $4 x, -y, z-1/2 HTAB OW8 O1_$4 HTAB OW8 O3 EQIV $10 x, -y, z+1/2 HTAB OW9 OW3_$10 HTAB OW9 O6_$1 EQIV $16 -x+1/2, y+1/2, -z+1/2 HTAB OW10 O14_$16 HTAB OW10 O10_$5 REM Highest difference peak 1.393, deepest hole -0.628, 1-sigma level 0.201 Q1 1 -0.0735 -0.1726 0.7148 11.00000 0.05 1.06 Q2 1 0.0691 0.3847 0.7775 11.00000 0.05 0.98 Q3 1 0.1466 0.1583 0.9012 11.00000 0.05 0.82 Q4 1 0.2595 -0.3922 0.1504 11.00000 0.05 0.73 Q5 1 -0.0124 0.7049 0.6506 11.00000 0.05 0.73 Q6 1 0.2884 -0.3994 0.1580 11.00000 0.05 0.71 Q7 1 0.1971 0.5977 0.5328 11.00000 0.05 0.71 Q8 1 -0.0253 0.5978 0.5322 11.00000 0.05 0.70 Q9 1 0.1650 0.1112 0.7056 11.00000 0.05 0.65 Q10 1 0.1526 -0.3088 0.9058 11.00000 0.05 0.64 Q11 1 0.2122 0.6970 0.3482 11.00000 0.05 0.59 Q12 1 0.1236 0.7052 0.7224 11.00000 0.05 0.56 Q13 1 -0.1123 -0.2043 0.4088 11.00000 0.05 0.53 Q14 1 0.1246 0.1710 0.7201 11.00000 0.05 0.51 Q15 1 -0.0267 0.1391 0.8695 11.00000 0.05 0.50 Q16 1 0.2391 0.6912 0.3494 11.00000 0.05 0.48 Q17 1 0.0155 0.5119 0.8383 11.00000 0.05 0.46 Q18 1 0.2166 0.1032 0.5170 11.00000 0.05 0.45 Q19 1 -0.1229 0.0030 0.7757 11.00000 0.05 0.44 Q20 1 0.1185 -0.3971 0.9153 11.00000 0.05 0.44 Q21 1 0.1977 0.2575 0.5220 11.00000 0.05 0.43 Q22 1 -0.1034 -0.1013 0.5139 11.00000 0.05 0.43 Q23 1 0.1619 0.6174 0.6675 11.00000 0.05 0.43 Q24 1 0.1738 -0.4177 1.0333 11.00000 0.05 0.42 Q25 1 0.0869 -0.4087 0.9300 11.00000 0.05 0.41 Q26 1 0.2398 0.6228 0.2833 11.00000 0.05 0.41 Q27 1 0.1126 0.4397 0.7311 11.00000 0.05 0.37 Q28 1 0.2344 0.2019 0.5406 11.00000 0.05 0.37 Q29 1 0.0444 0.0827 0.1006 11.00000 0.05 0.37 Q30 1 0.1870 0.1038 0.5900 11.00000 0.05 0.37 Q31 1 0.1553 -0.4788 0.8879 11.00000 0.05 0.36 Q32 1 0.1230 0.5330 0.7298 11.00000 0.05 0.35 Q33 1 0.2218 0.5374 0.3277 11.00000 0.05 0.34 Q34 1 0.2487 -0.2639 0.1475 11.00000 0.05 0.34 Q35 1 0.2198 0.5997 0.3724 11.00000 0.05 0.33 Q36 1 0.0357 0.2233 -0.0191 11.00000 0.05 0.32 Q37 1 0.0746 0.4017 0.6668 11.00000 0.05 0.31 Q38 1 0.1101 0.0137 0.0856 11.00000 0.05 0.30 Q39 1 0.2274 -0.4069 0.2301 11.00000 0.05 0.30 Q40 1 0.2255 0.5985 0.7223 11.00000 0.05 0.29 Q41 1 0.2245 0.2339 0.5912 11.00000 0.05 0.28 Q42 1 0.0802 0.4014 0.9211 11.00000 0.05 0.28 Q43 1 0.1049 0.1087 0.0632 11.00000 0.05 0.28 Q44 1 -0.0318 -0.0143 0.5217 11.00000 0.05 0.27 Q45 1 0.1967 -0.0246 0.0470 11.00000 0.05 0.25 Q46 1 0.2170 0.7171 0.5244 11.00000 0.05 0.25 Q47 1 0.1466 0.2158 0.5034 11.00000 0.05 0.25 Q48 1 0.2991 -0.2169 0.1675 11.00000 0.05 0.24 Q49 1 0.0894 0.2768 0.9589 11.00000 0.05 0.24 Q50 1 0.1837 0.7790 0.5184 11.00000 0.05 0.23 ; _shelx_res_checksum 5851 _shelx_hkl_file ; 1 -1 -2 1834.96 34.28 -1 1 2 1827.84 34.06 -1 1 2 1865.04 36.52 1 1 -2 1859.90 35.98 -1 -1 2 1875.96 36.20 1 -1 -2 1886.51 36.74 3 -1 -1 47.50 0.46 -3 1 1 45.86 0.44 3 -1 -1 46.26 0.61 -3 1 1 45.34 0.61 3 1 -1 47.51 0.65 3 -1 -2 295.21 3.70 3 -1 -2 308.75 3.72 -3 -1 2 313.02 3.97 -3 1 2 295.29 3.69 -3 1 2 317.62 3.81 3 1 -2 293.79 3.87 -4 0 1 0.07 0.10 4 0 -1 0.08 0.10 -3 1 0 30.95 0.49 3 -1 0 32.94 0.50 3 1 0 32.90 0.46 4 0 -2 21.88 0.37 2 0 -3 0.20 0.12 -2 0 3 0.23 0.13 0 -2 0 20.56 0.54 0 2 0 21.24 0.44 1 -1 2 51.73 0.71 -1 1 -2 51.68 0.71 -1 -1 -2 54.46 0.52 1 -1 2 52.13 0.55 -1 1 -2 53.66 0.61 4 0 0 1084.05 17.89 -4 0 0 1067.10 17.71 4 0 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