data_shelx _audit_creation_method 'SHELXL-2017/1' _shelx_SHELXL_version_number '2017/1' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H20 B2 Fe2 N18 Ni, 7( H2 O)' _chemical_formula_sum 'C24 H34 B2 Fe2 N18 Ni O7' _chemical_formula_weight 878.72 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 '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' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 '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' 'Ni' 'Ni' 0.3393 1.1124 '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 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 28.851(7) _cell_length_b 9.668(2) _cell_length_c 13.718(3) _cell_angle_alpha 90 _cell_angle_beta 101.205(11) _cell_angle_gamma 90 _cell_volume 3753.4(16) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 1051 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 19.77 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_density_diffrn 1.555 _exptl_crystal_F_000 1800 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.09 _exptl_absorpt_coefficient_mu 1.326 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.526 _exptl_absorpt_correction_T_max 0.744 _exptl_absorpt_process_details ; SADABS, Bruker AXS Inc., Madison, Wisconsin, USA. ; _exptl_absorpt_special_details ? _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 5013 _diffrn_reflns_av_unetI/netI 0.0770 _diffrn_reflns_av_R_equivalents 0.0980 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.226 _diffrn_reflns_theta_max 19.797 _diffrn_reflns_theta_full 19.797 _diffrn_measured_fraction_theta_max 0.733 _diffrn_measured_fraction_theta_full 0.733 _diffrn_reflns_Laue_measured_fraction_max 0.733 _diffrn_reflns_Laue_measured_fraction_full 0.733 _diffrn_reflns_point_group_measured_fraction_max 0.733 _diffrn_reflns_point_group_measured_fraction_full 0.733 _reflns_number_total 1250 _reflns_number_gt 780 _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 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2017/1 (Sheldrick, 2017)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 2006)' _computing_publication_material 'WinGX publication routines (Farrugia, 2012)' _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^)+(0.1142P)^2^+88.5885P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary dual _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 1250 _refine_ls_number_parameters 118 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1421 _refine_ls_R_factor_gt 0.0800 _refine_ls_wR_factor_ref 0.2482 _refine_ls_wR_factor_gt 0.1907 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _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 Ni1 Ni 0.500000 0.500000 0.500000 0.0529(13) Uani 1 2 d S . P . . Fe1 Fe 0.37890(9) 0.6457(2) 0.7034(2) 0.0533(11) Uani 1 1 d . . . . . O1 O 0.4909(4) 0.2944(11) 0.5453(10) 0.070(4) Uiso 1 1 d . . . . . O2 O 0.3970(6) 0.1893(14) 0.5087(13) 0.110(5) Uiso 1 1 d . . . . . O3 O 0.500000 0.313(3) 0.750000 0.178(12) Uiso 1 2 d S . P . . O4 O 0.5527(8) 0.095(2) 0.4679(18) 0.171(8) Uiso 1 1 d . . . . . N1 N 0.4586(6) 0.5672(13) 0.5963(12) 0.061(4) Uiso 1 1 d . . . . . N2 N 0.4401(6) 0.5228(13) 0.8904(13) 0.058(4) Uiso 1 1 d . . . . . N3 N 0.3390(7) 0.3638(17) 0.6362(14) 0.089(5) Uiso 1 1 d . . . . . N4 N 0.3257(5) 0.6953(13) 0.7669(12) 0.056(4) Uiso 1 1 d . . . . . N5 N 0.3059(6) 0.8218(13) 0.7494(13) 0.066(4) Uiso 1 1 d . . . . . N6 N 0.3462(6) 0.7325(14) 0.5810(13) 0.067(4) Uiso 1 1 d . . . . . N7 N 0.3226(7) 0.8548(15) 0.5833(14) 0.075(5) Uiso 1 1 d . . . . . N8 N 0.4051(6) 0.8259(13) 0.7435(12) 0.059(4) Uiso 1 1 d . . . . . N9 N 0.3781(6) 0.9399(15) 0.7291(14) 0.073(5) Uiso 1 1 d . . . . . C1 C 0.4295(7) 0.5973(16) 0.6381(15) 0.058(5) Uiso 1 1 d . . . . . C2 C 0.4155(7) 0.5639(16) 0.8212(15) 0.051(5) Uiso 1 1 d . . . . . C3 C 0.3530(7) 0.4721(18) 0.6600(16) 0.067(6) Uiso 1 1 d . . . . . C4 C 0.3031(7) 0.6351(19) 0.8315(16) 0.071(6) Uiso 1 1 d . . . . . H4 H 0.309046 0.546066 0.856467 0.086 Uiso 1 1 calc R U . . . C5 C 0.2696(8) 0.7241(19) 0.8564(17) 0.079(6) Uiso 1 1 d . . . . . H5 H 0.249571 0.706463 0.900452 0.095 Uiso 1 1 calc R U . . . C6 C 0.2716(8) 0.8377(18) 0.8057(16) 0.070(6) Uiso 1 1 d . . . . . H6 H 0.253093 0.916016 0.807370 0.084 Uiso 1 1 calc R U . . . C7 C 0.3400(8) 0.696(2) 0.4824(17) 0.077(6) Uiso 1 1 d . . . . . H7 H 0.352318 0.616690 0.458209 0.093 Uiso 1 1 calc R U . . . C8 C 0.3124(9) 0.795(2) 0.425(2) 0.111(8) Uiso 1 1 d . . . . . H8 H 0.302477 0.794751 0.355861 0.133 Uiso 1 1 calc R U . . . C9 C 0.3035(10) 0.890(3) 0.486(2) 0.108(8) Uiso 1 1 d . . . . . H9 H 0.286352 0.970057 0.467633 0.129 Uiso 1 1 calc R U . . . C10 C 0.4483(8) 0.8652(19) 0.7937(16) 0.077(6) Uiso 1 1 d . . . . . H10 H 0.473493 0.806857 0.817934 0.092 Uiso 1 1 calc R U . . . C11 C 0.4480(10) 1.009(2) 0.803(2) 0.108(8) Uiso 1 1 d . . . . . H11 H 0.473376 1.065633 0.829704 0.130 Uiso 1 1 calc R U . . . C12 C 0.4038(9) 1.049(2) 0.764(2) 0.093(7) Uiso 1 1 d . . . . . H12 H 0.392749 1.139962 0.762405 0.112 Uiso 1 1 calc R U . . . B1 B 0.3280(10) 0.925(2) 0.685(2) 0.077(7) Uiso 1 1 d . . . . . H1 H 0.311663 1.014037 0.679509 0.092 Uiso 1 1 calc R 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 Ni1 0.049(3) 0.071(2) 0.042(2) -0.0061(17) 0.017(3) -0.0016(16) Fe1 0.046(2) 0.0744(17) 0.0404(19) 0.0001(14) 0.012(2) 0.0022(13) _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 Ni1 N1 2.051(15) . ? Ni1 N1 2.051(15) 5_666 ? Ni1 N2 2.071(19) 6_565 ? Ni1 N2 2.071(19) 2_656 ? Ni1 O1 2.114(11) 5_666 ? Ni1 O1 2.114(11) . ? Fe1 C3 1.89(2) . ? Fe1 C1 1.913(19) . ? Fe1 C2 1.92(2) . ? Fe1 N8 1.936(14) . ? Fe1 N6 1.949(17) . ? Fe1 N4 1.967(13) . ? N1 C1 1.143(19) . ? N2 C2 1.14(2) . ? N3 C3 1.15(2) . ? N4 C4 1.33(2) . ? N4 N5 1.351(17) . ? N5 C6 1.38(2) . ? N5 B1 1.55(3) . ? N6 N7 1.368(19) . ? N6 C7 1.38(3) . ? N7 C9 1.38(3) . ? N7 B1 1.53(3) . ? N8 N9 1.341(19) . ? N8 C10 1.36(2) . ? N9 C12 1.33(3) . ? N9 B1 1.47(3) . ? C4 C5 1.39(2) . ? C4 H4 0.9300 . ? C5 C6 1.31(2) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 C8 1.40(3) . ? C7 H7 0.9300 . ? C8 C9 1.31(3) . ? C8 H8 0.9300 . ? C9 H9 0.9300 . ? C10 C11 1.40(3) . ? C10 H10 0.9300 . ? C11 C12 1.34(3) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? B1 H1 0.9800 . ? 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 N1 Ni1 N1 180.0 . 5_666 ? N1 Ni1 N2 89.6(6) . 6_565 ? N1 Ni1 N2 90.4(6) 5_666 6_565 ? N1 Ni1 N2 90.4(6) . 2_656 ? N1 Ni1 N2 89.6(6) 5_666 2_656 ? N2 Ni1 N2 180.0 6_565 2_656 ? N1 Ni1 O1 90.7(5) . 5_666 ? N1 Ni1 O1 89.3(5) 5_666 5_666 ? N2 Ni1 O1 91.2(5) 6_565 5_666 ? N2 Ni1 O1 88.8(5) 2_656 5_666 ? N1 Ni1 O1 89.3(5) . . ? N1 Ni1 O1 90.7(5) 5_666 . ? N2 Ni1 O1 88.8(5) 6_565 . ? N2 Ni1 O1 91.2(5) 2_656 . ? O1 Ni1 O1 180.0 5_666 . ? C3 Fe1 C1 85.8(8) . . ? C3 Fe1 C2 91.1(8) . . ? C1 Fe1 C2 87.0(8) . . ? C3 Fe1 N8 178.1(9) . . ? C1 Fe1 N8 93.5(7) . . ? C2 Fe1 N8 90.6(7) . . ? C3 Fe1 N6 90.9(8) . . ? C1 Fe1 N6 89.3(7) . . ? C2 Fe1 N6 175.7(7) . . ? N8 Fe1 N6 87.3(7) . . ? C3 Fe1 N4 93.5(7) . . ? C1 Fe1 N4 178.4(8) . . ? C2 Fe1 N4 94.4(7) . . ? N8 Fe1 N4 87.1(6) . . ? N6 Fe1 N4 89.3(7) . . ? C1 N1 Ni1 168.7(16) . . ? C2 N2 Ni1 159.7(15) . 2_656 ? C4 N4 N5 105.7(14) . . ? C4 N4 Fe1 135.5(12) . . ? N5 N4 Fe1 118.8(11) . . ? N4 N5 C6 109.0(14) . . ? N4 N5 B1 118.5(15) . . ? C6 N5 B1 132.0(16) . . ? N7 N6 C7 106.1(17) . . ? N7 N6 Fe1 120.8(13) . . ? C7 N6 Fe1 133.1(14) . . ? N6 N7 C9 107.3(18) . . ? N6 N7 B1 116.2(19) . . ? C9 N7 B1 136.1(19) . . ? N9 N8 C10 107.1(15) . . ? N9 N8 Fe1 121.0(13) . . ? C10 N8 Fe1 131.8(13) . . ? C12 N9 N8 110(2) . . ? C12 N9 B1 131.8(19) . . ? N8 N9 B1 118.5(16) . . ? N1 C1 Fe1 177.7(18) . . ? N2 C2 Fe1 174.4(17) . . ? N3 C3 Fe1 177(2) . . ? N4 C4 C5 110.3(17) . . ? N4 C4 H4 124.8 . . ? C5 C4 H4 124.8 . . ? C6 C5 C4 106.6(19) . . ? C6 C5 H5 126.7 . . ? C4 C5 H5 126.7 . . ? C5 C6 N5 108.4(18) . . ? C5 C6 H6 125.8 . . ? N5 C6 H6 125.8 . . ? N6 C7 C8 109.3(19) . . ? N6 C7 H7 125.3 . . ? C8 C7 H7 125.3 . . ? C9 C8 C7 106(3) . . ? C9 C8 H8 127.0 . . ? C7 C8 H8 127.0 . . ? C8 C9 N7 111(2) . . ? C8 C9 H9 124.4 . . ? N7 C9 H9 124.4 . . ? N8 C10 C11 108(2) . . ? N8 C10 H10 126.1 . . ? C11 C10 H10 126.1 . . ? C12 C11 C10 106(2) . . ? C12 C11 H11 127.0 . . ? C10 C11 H11 127.0 . . ? N9 C12 C11 109(2) . . ? N9 C12 H12 125.3 . . ? C11 C12 H12 125.3 . . ? N9 B1 N7 109.9(19) . . ? N9 B1 N5 108(2) . . ? N7 B1 N5 105.0(17) . . ? N9 B1 H1 111.3 . . ? N7 B1 H1 111.3 . . ? N5 B1 H1 111.3 . . ? _refine_diff_density_max 0.689 _refine_diff_density_min -0.435 _refine_diff_density_rms 0.107 _shelx_res_file ; TITL jr240417_0ma_a.res in C2/c shelx.res created by SHELXL-2017/1 at 13:24:47 on 03-Feb-2018 CELL 0.71073 28.8509 9.6682 13.7176 90.000 101.205 90.000 ZERR 4.00 0.0074 0.0023 0.0033 0.000 0.011 0.000 LATT 7 SYMM - X, Y, 1/2 - Z SFAC C H B FE N NI O UNIT 96 136 8 8 72 4 28 MERG 2 OMIT -2.00 50.00 OMIT 2 0 0 OMIT -4 2 3 FMAP 2 PLAN 20 ACTA BOND $H L.S. 8 TEMP 23.00 WGHT 0.114200 88.588509 FVAR 0.20358 NI1 6 0.500000 0.500000 0.500000 10.50000 0.04892 0.07125 = 0.04183 -0.00609 0.01688 -0.00156 FE1 4 0.378903 0.645676 0.703378 11.00000 0.04647 0.07438 = 0.04037 0.00006 0.01189 0.00221 O1 7 0.490854 0.294379 0.545256 11.00000 0.06998 O2 7 0.396981 0.189282 0.508737 11.00000 0.10965 O3 7 0.500000 0.313046 0.750000 10.50000 0.17785 O4 7 0.552705 0.094517 0.467890 11.00000 0.17142 N1 5 0.458622 0.567154 0.596313 11.00000 0.06128 N2 5 0.440075 0.522812 0.890401 11.00000 0.05767 N3 5 0.338986 0.363790 0.636182 11.00000 0.08940 N4 5 0.325658 0.695299 0.766859 11.00000 0.05632 N5 5 0.305919 0.821818 0.749406 11.00000 0.06599 N6 5 0.346229 0.732534 0.580996 11.00000 0.06712 N7 5 0.322630 0.854810 0.583325 11.00000 0.07508 N8 5 0.405098 0.825937 0.743468 11.00000 0.05949 N9 5 0.378139 0.939858 0.729128 11.00000 0.07279 C1 1 0.429494 0.597333 0.638093 11.00000 0.05790 C2 1 0.415524 0.563892 0.821215 11.00000 0.05064 C3 1 0.352959 0.472144 0.660042 11.00000 0.06661 C4 1 0.303129 0.635124 0.831522 11.00000 0.07126 AFIX 43 H4 2 0.309046 0.546066 0.856467 11.00000 -1.20000 AFIX 0 C5 1 0.269606 0.724104 0.856360 11.00000 0.07902 AFIX 43 H5 2 0.249571 0.706463 0.900452 11.00000 -1.20000 AFIX 0 C6 1 0.271650 0.837729 0.805677 11.00000 0.07026 AFIX 43 H6 2 0.253093 0.916016 0.807370 11.00000 -1.20000 AFIX 0 C7 1 0.340038 0.695669 0.482447 11.00000 0.07745 AFIX 43 H7 2 0.352318 0.616690 0.458209 11.00000 -1.20000 AFIX 0 C8 1 0.312443 0.795362 0.424536 11.00000 0.11101 AFIX 43 H8 2 0.302477 0.794751 0.355861 11.00000 -1.20000 AFIX 0 C9 1 0.303471 0.889687 0.486474 11.00000 0.10776 AFIX 43 H9 2 0.286352 0.970057 0.467633 11.00000 -1.20000 AFIX 0 C10 1 0.448254 0.865219 0.793725 11.00000 0.07668 AFIX 43 H10 2 0.473493 0.806857 0.817934 11.00000 -1.20000 AFIX 0 C11 1 0.448017 1.009229 0.802640 11.00000 0.10796 AFIX 43 H11 2 0.473376 1.065633 0.829704 11.00000 -1.20000 AFIX 0 C12 1 0.403771 1.049424 0.764209 11.00000 0.09340 AFIX 43 H12 2 0.392749 1.139962 0.762405 11.00000 -1.20000 AFIX 0 B1 3 0.327956 0.924622 0.684653 11.00000 0.07691 AFIX 13 H1 2 0.311663 1.014037 0.679509 11.00000 -1.20000 AFIX 0 HKLF 4 REM jr240417_0ma_a.res in C2/c REM R1 = 0.0800 for 780 Fo > 4sig(Fo) and 0.1421 for all 1250 data REM 118 parameters refined using 0 restraints END WGHT 0.1141 88.6158 REM Highest difference peak 0.689, deepest hole -0.435, 1-sigma level 0.107 Q1 1 0.4978 0.2153 0.5079 11.00000 0.05 0.69 Q2 1 0.4643 0.3021 0.7370 11.00000 0.05 0.60 Q3 1 0.3804 0.3515 0.7030 11.00000 0.05 0.53 Q4 1 0.2588 0.4911 0.9005 11.00000 0.05 0.51 Q5 1 0.5296 0.3401 0.5385 11.00000 0.05 0.45 Q6 1 0.4881 0.3556 0.5438 11.00000 0.05 0.41 Q7 1 0.2766 0.8092 0.4295 11.00000 0.05 0.38 Q8 1 0.5377 0.5516 0.5027 11.00000 0.05 0.38 Q9 1 0.3290 0.6136 0.7587 11.00000 0.05 0.37 Q10 1 0.3706 0.8438 0.4136 11.00000 0.05 0.36 Q11 1 0.4536 0.2818 0.5385 11.00000 0.05 0.35 Q12 1 0.3789 0.7648 0.7119 11.00000 0.05 0.34 Q13 1 0.3678 0.7675 0.7053 11.00000 0.05 0.34 Q14 1 0.2639 0.6418 0.8588 11.00000 0.05 0.33 Q15 1 0.4120 1.1728 0.8398 11.00000 0.05 0.33 Q16 1 0.3987 0.5010 0.7393 11.00000 0.05 0.32 Q17 1 0.3651 0.3036 0.4406 11.00000 0.05 0.30 Q18 1 0.4718 0.9053 0.8993 11.00000 0.05 0.30 Q19 1 0.4154 0.8802 0.7601 11.00000 0.05 0.29 Q20 1 0.3978 0.1553 0.4809 11.00000 0.05 0.29 ; _shelx_res_checksum 97234 _shelx_hkl_file ; -2 -2 0 2505.35 51.09 2 2 0 2483.25 50.99 -3 -3 0 729.03 19.30 4 4 0 1266.87 29.30 -6 -6 0 57.69 14.10 7 7 0 236.08 20.50 -8 -8 0 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_shelx_hkl_checksum 29263