data_global _audit_creation_method 'APEX2 v2014.9-0' _publ_requested_journal ? _publ_contact_author_name ? _publ_contact_author_address ; ; _publ_contact_author_email ? _publ_contact_author_fax ? _publ_contact_author_phone ? _publ_section_title ; ; _publ_section_abstract ; ; _publ_section_references ; ; _publ_section_comment ; ; data_I _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety 'C30 H54 N6 Ru, Cl6 Ru2,2(C H2 Cl2)' _chemical_formula_sum 'C32 H58 Cl10 N6 Ru3' _chemical_formula_iupac ? _chemical_formula_weight 1184.55 _chemical_melting_point ? _space_group_crystal_system monoclinic _space_group_name_H-M_alt 'C 1 2/m 1' _space_group_name_Hall '-C 2y' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 21.221(7) _cell_length_b 13.810(4) _cell_length_c 9.163(3) _cell_angle_alpha 90 _cell_angle_beta 103.056(7) _cell_angle_gamma 90 _cell_volume 2615.9(14) _cell_formula_units_Z 2 _cell_measurement_reflns_used 3262 _cell_measurement_theta_min 2.66 _cell_measurement_theta_max 28.17 _cell_measurement_temperature 100.(2) _exptl_crystal_description 'Block' _exptl_crystal_colour 'colourless' _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.130 _exptl_crystal_size_min 0.100 _exptl_crystal_density_diffrn 1.504 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1188 _exptl_absorpt_coefficient_mu 1.393 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS V2014/5 (Bruker AXS Inc.)' _exptl_absorpt_correction_T_min 0.77 _exptl_absorpt_correction_T_max 0.87 _exptl_special_details ; ; _diffrn_ambient_temperature 100.(2) _diffrn_radiation_type 'MoK\a' _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator 'graphite' _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_wavelength 0.71073 _diffrn_detector_area_resol_mean 8.3333 _diffrn_reflns_number 13063 _diffrn_reflns_av_R_equivalents 0.0554 _diffrn_reflns_av_unetI/netI 0.0542 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 28.76 _diffrn_reflns_theta_full 28.76 _diffrn_measured_fraction_theta_max 0.974 _diffrn_measured_fraction_theta_full 0.974 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _refine_special_details ; ; _reflns_number_total 3453 _reflns_number_gt 2663 _reflns_threshold_expression 'I > 2\s(I)' _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all 0.0867 _refine_ls_R_factor_gt 0.0656 _refine_ls_wR_factor_gt 0.2019 _refine_ls_wR_factor_ref 0.2187 _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_restrained_S_all 1.092 _refine_ls_number_reflns 3453 _refine_ls_number_parameters 139 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_hydrogen_treatment mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1171P)^2^+46.0038P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 3.586 _refine_diff_density_min -3.024 _refine_ls_extinction_method none _refine_ls_extinction_coef ? 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _computing_data_collection 'Bruker Instrument Service v2014.11.0.1' _computing_cell_refinement 'SAINT V8.34A (Bruker AXS Inc., 2013)' _computing_data_reduction 'SAINT V8.34A (Bruker AXS Inc., 2013)' _computing_structure_solution 'SHELXS-2014/7 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_refinement_flags_posn _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C C1 0.5805(4) 0.5 0.7496(9) 0.0093(15) Uani d T P S 1 . . C C2 0.6261(4) 0.5 0.6486(9) 0.0094(15) Uani d T P S 1 . . C C3 0.6677(3) 0.5910(5) 0.6828(8) 0.0175(12) Uani d . . . 1 . . H H3A 0.6405 0.6484 0.6546 0.026 Uiso calc U . R 1 . . H H3B 0.7015 0.5896 0.6255 0.026 Uiso calc U . R 1 . . H H3C 0.6877 0.5934 0.7901 0.026 Uiso calc U . R 1 . . C C4 0.5873(5) 0.5 0.4859(11) 0.027(2) Uani d T P S 1 . . H H4A 0.568(5) 0.448(7) 0.476(11) 0.041 Uiso d U P . 0.5 . . H H4B 0.619(8) 0.5 0.448(17) 0.041 Uiso d U P S 1 . . H H4C 0.568(5) 0.552(7) 0.476(11) 0.041 Uiso d U P . 0.5 . . C C5 0.4092(3) 0.3272(4) 0.8635(6) 0.0108(11) Uani d . . . 1 . . C C6 0.3685(3) 0.2394(4) 0.8227(7) 0.0120(11) Uani d . . . 1 . . C C7 0.3106(3) 0.2498(5) 0.8987(8) 0.0203(13) Uani d . . . 1 . . H H7A 0.3263 0.2478 1.0077 0.03 Uiso calc U . R 1 . . H H7B 0.2801 0.1965 0.8668 0.03 Uiso calc U . R 1 . . H H7C 0.2887 0.3116 0.8695 0.03 Uiso calc U . R 1 . . C C8 0.4093(3) 0.1504(4) 0.8823(7) 0.0162(12) Uani d . . . 1 . . H H8A 0.4474 0.1479 0.8386 0.024 Uiso calc U . R 1 . . H H8B 0.3834 0.0916 0.8549 0.024 Uiso calc U . R 1 . . H H8C 0.4233 0.1546 0.9916 0.024 Uiso calc U . R 1 . . C C9 0.3451(3) 0.2358(5) 0.6517(7) 0.0201(13) Uani d . . . 1 . . H H9A 0.3165 0.291 0.6179 0.03 Uiso calc U . R 1 . . H H9B 0.3213 0.1754 0.6227 0.03 Uiso calc U . R 1 . . H H9C 0.3824 0.2387 0.6054 0.03 Uiso calc U . R 1 . . C C10 0.3186(5) 0 0.2554(11) 0.0210(19) Uani d T P S 1 . . H H10A 0.3463 -0.0581 0.2803 0.025 Uiso calc U P R 0.5 . . H H10B 0.3463 0.0581 0.2803 0.025 Uiso calc U P R 0.5 . . Cl Cl1 0.28151(13) 0 0.0604(3) 0.0263(5) Uani d T P S 1 . . Cl Cl2 0.25861(15) 0 0.3623(3) 0.0348(6) Uani d T P S 1 . . Cl Cl3 0.43430(10) 0 0.5770(2) 0.0146(4) Uani d T P S 1 . . Cl Cl4 0.55620(9) 0.20306(13) 0.69054(18) 0.0250(4) Uani d . . . 1 . . N N1 0.5484(3) 0.5 0.8333(7) 0.0078(12) Uani d T P S 1 . . N N2 0.4396(2) 0.3930(3) 0.9004(5) 0.0083(9) Uani d . . . 1 . . Ru Ru1 0.5 0.5 1.0 0.0040(2) Uani d T P S 1 . . Ru Ru2 0.5 0.11788(7) 0.5 0.0313(3) Uani d T P S 1 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 C1 0.005(3) 0.013(4) 0.010(3) 0 0.001(3) 0 C2 0.004(3) 0.017(4) 0.008(3) 0 0.003(3) 0 C3 0.018(3) 0.015(3) 0.025(3) -0.002(2) 0.014(2) 0.003(2) C4 0.012(5) 0.060(8) 0.010(4) 0 0.003(3) 0 C5 0.013(3) 0.010(3) 0.011(2) 0.002(2) 0.008(2) -0.001(2) C6 0.011(3) 0.010(3) 0.016(3) -0.006(2) 0.005(2) -0.004(2) C7 0.015(3) 0.017(3) 0.033(4) -0.007(2) 0.014(3) -0.007(3) C8 0.019(3) 0.010(3) 0.019(3) -0.002(2) 0.005(2) -0.003(2) C9 0.022(3) 0.021(3) 0.016(3) -0.006(3) 0.001(2) -0.005(2) C10 0.021(5) 0.024(5) 0.019(4) 0 0.005(4) 0 Cl1 0.0344(14) 0.0244(12) 0.0192(11) 0 0.0042(10) 0 Cl2 0.0306(14) 0.0471(17) 0.0329(14) 0 0.0199(11) 0 Cl3 0.0159(10) 0.0136(9) 0.0173(9) 0 0.0098(8) 0 Cl4 0.0342(9) 0.0236(8) 0.0193(7) -0.0141(7) 0.0105(7) -0.0082(6) N1 0.010(3) 0.007(3) 0.007(3) 0 0.004(2) 0 N2 0.009(2) 0.007(2) 0.011(2) 0.0002(17) 0.0070(17) 0.0004(17) Ru1 0.0044(4) 0.0019(4) 0.0075(4) 0 0.0048(3) 0 Ru2 0.0358(6) 0.0289(5) 0.0309(5) 0 0.0112(4) 0 _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_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag C1 N1 . 1.135(11) ? C1 C2 . 1.481(11) ? C2 C3 . 1.527(8) ? C2 C3 6_565 1.527(8) ? C2 C4 . 1.531(12) ? C3 H3A . 0.98 ? C3 H3B . 0.98 ? C3 H3C . 0.98 ? C4 H4A . 0.82(10) ? C4 H4B . 0.82(17) ? C4 H4C . 0.82(10) ? C5 N2 . 1.122(8) ? C5 C6 . 1.487(8) ? C6 C8 . 1.531(9) ? C6 C9 . 1.533(9) ? C6 C7 . 1.551(8) ? C7 H7A . 0.98 ? C7 H7B . 0.98 ? C7 H7C . 0.98 ? C8 H8A . 0.98 ? C8 H8B . 0.98 ? C8 H8C . 0.98 ? C9 H9A . 0.98 ? C9 H9B . 0.98 ? C9 H9C . 0.98 ? C10 Cl2 . 1.773(10) ? C10 Cl1 . 1.782(10) ? C10 H10A . 0.99 ? C10 H10B . 0.99 ? Cl3 Ru2 . 2.3528(17) ? Cl3 Ru2 5_656 2.3528(17) ? Cl4 Ru2 . 2.2167(17) ? N1 Ru1 . 2.025(7) ? N2 Ru1 . 2.032(5) ? Ru1 N1 5_667 2.025(7) ? Ru1 N2 5_667 2.032(5) ? Ru1 N2 6_565 2.032(5) ? Ru1 N2 2_657 2.032(5) ? Ru2 Cl4 2_656 2.2167(17) ? Ru2 Cl3 5_656 2.3528(17) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N1 C1 C2 . . 176.3(8) ? C1 C2 C3 . . 107.5(4) ? C1 C2 C3 . 6_565 107.5(4) ? C3 C2 C3 . 6_565 110.8(7) ? C1 C2 C4 . . 109.0(7) ? C3 C2 C4 . . 111.0(5) ? C3 C2 C4 6_565 . 111.0(5) ? C2 C3 H3A . . 109.5 ? C2 C3 H3B . . 109.5 ? H3A C3 H3B . . 109.5 ? C2 C3 H3C . . 109.5 ? H3A C3 H3C . . 109.5 ? H3B C3 H3C . . 109.5 ? C2 C4 H4A . . 105.(7) ? C2 C4 H4B . . 96.(10) ? H4A C4 H4B . . 113.(8) ? C2 C4 H4C . . 105.(7) ? H4A C4 H4C . . 122.(10) ? H4B C4 H4C . . 113.(8) ? N2 C5 C6 . . 177.0(6) ? C5 C6 C8 . . 108.4(5) ? C5 C6 C9 . . 108.6(5) ? C8 C6 C9 . . 111.4(5) ? C5 C6 C7 . . 106.6(5) ? C8 C6 C7 . . 110.8(5) ? C9 C6 C7 . . 110.7(5) ? C6 C7 H7A . . 109.5 ? C6 C7 H7B . . 109.5 ? H7A C7 H7B . . 109.5 ? C6 C7 H7C . . 109.5 ? H7A C7 H7C . . 109.5 ? H7B C7 H7C . . 109.5 ? C6 C8 H8A . . 109.5 ? C6 C8 H8B . . 109.5 ? H8A C8 H8B . . 109.5 ? C6 C8 H8C . . 109.5 ? H8A C8 H8C . . 109.5 ? H8B C8 H8C . . 109.5 ? C6 C9 H9A . . 109.5 ? C6 C9 H9B . . 109.5 ? H9A C9 H9B . . 109.5 ? C6 C9 H9C . . 109.5 ? H9A C9 H9C . . 109.5 ? H9B C9 H9C . . 109.5 ? Cl2 C10 Cl1 . . 110.1(5) ? Cl2 C10 H10A . . 109.6 ? Cl1 C10 H10A . . 109.6 ? Cl2 C10 H10B . . 109.6 ? Cl1 C10 H10B . . 109.6 ? H10A C10 H10B . . 108.1 ? Ru2 Cl3 Ru2 . 5_656 87.56(8) ? C1 N1 Ru1 . . 173.9(7) ? C5 N2 Ru1 . . 170.4(5) ? N1 Ru1 N1 5_667 . 180.0 ? N1 Ru1 N2 5_667 . 87.86(18) ? N1 Ru1 N2 . . 92.14(18) ? N1 Ru1 N2 5_667 5_667 92.14(18) ? N1 Ru1 N2 . 5_667 87.86(18) ? N2 Ru1 N2 . 5_667 180.0 ? N1 Ru1 N2 5_667 6_565 87.86(18) ? N1 Ru1 N2 . 6_565 92.14(18) ? N2 Ru1 N2 . 6_565 93.3(3) ? N2 Ru1 N2 5_667 6_565 86.7(3) ? N1 Ru1 N2 5_667 2_657 92.14(18) ? N1 Ru1 N2 . 2_657 87.86(18) ? N2 Ru1 N2 . 2_657 86.7(3) ? N2 Ru1 N2 5_667 2_657 93.3(3) ? N2 Ru1 N2 6_565 2_657 180.0 ? Cl4 Ru2 Cl4 . 2_656 115.89(11) ? Cl4 Ru2 Cl3 . 5_656 110.70(7) ? Cl4 Ru2 Cl3 2_656 5_656 112.39(7) ? Cl4 Ru2 Cl3 . . 112.39(7) ? Cl4 Ru2 Cl3 2_656 . 110.70(7) ? Cl3 Ru2 Cl3 5_656 . 92.44(8) ? _shelx_res_file ; TITL mo_MS_Catalyst_2_1R_0m in C2/m CELL 0.71073 21.2214 13.8100 9.1632 90.000 103.056 90.000 ZERR 2.00 0.0067 0.0042 0.0030 0.000 0.007 0.000 LATT 7 SYMM -X, Y, -Z SFAC C H N Cl Ru UNIT 64 116 12 20 6 MERG 2 OMIT 8 2 0 OMIT 0 0 3 OMIT -2 0 3 OMIT -1 3 1 OMIT 8 0 0 OMIT 6 0 1 OMIT 6 2 0 OMIT -3 1 2 BOND $H FMAP 2 PLAN 20 L.S. 15 ACTA CONF HTAB SIZE 0.100 0.130 0.200 TEMP -173.150 WGHT 0.117100 46.003799 FVAR 0.24792 0.56793 0.44803 0.47572 0.61871 0.44786 C1 1 0.580546 0.500000 0.749618 10.50000 0.00465 0.01287 = 0.01004 0.00000 0.00077 0.00000 C2 1 0.626072 0.500000 0.648605 10.50000 0.00371 0.01725 = 0.00822 0.00000 0.00349 0.00000 C3 1 0.667663 0.591020 0.682770 11.00000 0.01756 0.01483 = 0.02456 0.00338 0.01386 -0.00178 AFIX 137 H3A 2 0.640488 0.648423 0.654585 11.00000 -1.50000 H3B 2 0.701481 0.589627 0.625543 11.00000 -1.50000 H3C 2 0.687710 0.593420 0.790107 11.00000 -1.50000 AFIX 0 C4 1 0.587339 0.500000 0.485875 10.50000 0.01235 0.05966 = 0.01037 0.00000 0.00296 0.00000 H4A 2 21.000000 31.000000 41.000000 10.50000 -1.50000 H4B 2 51.000000 10.500000 61.000000 10.50000 -1.50000 H4C 2 21.000000 -31.000000 41.000000 10.50000 -1.50000 C5 1 0.409243 0.327153 0.863474 11.00000 0.01330 0.01029 = 0.01122 -0.00091 0.00773 0.00229 C6 1 0.368522 0.239365 0.822673 11.00000 0.01112 0.01018 = 0.01554 -0.00443 0.00457 -0.00568 C7 1 0.310585 0.249777 0.898666 11.00000 0.01489 0.01713 = 0.03315 -0.00679 0.01449 -0.00728 AFIX 137 H7A 2 0.326324 0.247817 1.007740 11.00000 -1.50000 H7B 2 0.280104 0.196468 0.866770 11.00000 -1.50000 H7C 2 0.288708 0.311626 0.869521 11.00000 -1.50000 AFIX 0 C8 1 0.409321 0.150360 0.882326 11.00000 0.01906 0.01040 = 0.01942 -0.00282 0.00465 -0.00229 AFIX 137 H8A 2 0.447380 0.147919 0.838580 11.00000 -1.50000 H8B 2 0.383410 0.091650 0.854929 11.00000 -1.50000 H8C 2 0.423281 0.154558 0.991640 11.00000 -1.50000 AFIX 0 C9 1 0.345059 0.235783 0.651733 11.00000 0.02237 0.02064 = 0.01579 -0.00491 0.00131 -0.00619 AFIX 137 H9A 2 0.316512 0.291024 0.617850 11.00000 -1.50000 H9B 2 0.321299 0.175374 0.622683 11.00000 -1.50000 H9C 2 0.382369 0.238660 0.605421 11.00000 -1.50000 AFIX 0 C10 1 0.318608 0.000000 0.255420 10.50000 0.02064 0.02408 = 0.01864 0.00000 0.00521 0.00000 AFIX 23 H10A 2 0.346324 -0.058051 0.280331 10.50000 -1.20000 H10B 2 0.346324 0.058051 0.280331 10.50000 -1.20000 AFIX 0 CL1 4 0.281514 0.000000 0.060444 10.50000 0.03442 0.02435 = 0.01924 0.00000 0.00415 0.00000 CL2 4 0.258612 0.000000 0.362297 10.50000 0.03064 0.04708 = 0.03286 0.00000 0.01993 0.00000 CL3 4 0.434303 0.000000 0.576978 10.50000 0.01585 0.01357 = 0.01730 0.00000 0.00976 0.00000 CL4 4 0.556196 0.203063 0.690536 11.00000 0.03418 0.02359 = 0.01929 -0.00823 0.01045 -0.01412 N1 3 0.548439 0.500000 0.833291 10.50000 0.01015 0.00747 = 0.00661 0.00000 0.00352 0.00000 N2 3 0.439618 0.393033 0.900409 11.00000 0.00897 0.00736 = 0.01098 0.00043 0.00701 0.00017 RU1 5 0.500000 0.500000 1.000000 10.25000 0.00438 0.00188 = 0.00754 0.00000 0.00484 0.00000 RU2 5 0.500000 0.117878 0.500000 10.50000 0.03578 0.02890 = 0.03089 0.00000 0.01122 0.00000 HKLF 4 REM mo_MS_Catalyst_2_1R_0m in C2/m REM R1 = 0.0656 for 2663 Fo > 4sig(Fo) and 0.0867 for all 3453 data REM 139 parameters refined using 0 restraints END WGHT 0.1177 44.9987 REM Instructions for potential hydrogen bonds EQIV $1 -x+1, -y, -z+1 HTAB C10 Cl4_$1 EQIV $2 -x+1, y, -z+1 HTAB C10 Cl4_$2 REM Highest difference peak 3.586, deepest hole -3.024, 1-sigma level 0.264 Q1 1 0.2985 0.0000 0.0823 10.50000 0.05 1.65 Q2 1 0.4477 0.0000 0.5611 10.50000 0.05 1.46 Q3 1 0.2866 0.0000 0.0226 10.50000 0.05 1.30 Q4 1 0.5554 0.2044 0.7389 11.00000 0.05 1.18 Q5 1 0.5503 0.5000 0.7621 10.50000 0.05 1.08 Q6 1 0.5564 0.2054 0.6292 11.00000 0.05 1.07 Q7 1 0.2699 0.0190 0.3584 11.00000 0.05 1.06 Q8 1 0.5372 0.2215 0.6666 11.00000 0.05 1.04 Q9 1 0.2419 0.0000 0.3304 10.50000 0.05 1.01 Q10 1 0.4558 0.4089 0.9344 11.00000 0.05 0.83 Q11 1 0.3535 0.2382 0.7476 11.00000 0.05 0.82 Q12 1 0.6197 0.5000 0.5956 10.50000 0.05 0.78 Q13 1 0.4996 0.1173 0.3827 11.00000 0.05 0.78 Q14 1 0.5003 0.1523 0.3952 11.00000 0.05 0.69 Q15 1 0.6226 0.5000 0.8891 10.50000 0.05 0.67 Q16 1 0.5000 0.5890 1.0000 10.50000 0.05 0.66 Q17 1 0.6005 0.5000 0.7547 10.50000 0.05 0.63 Q18 1 0.4314 0.3776 0.9341 11.00000 0.05 0.63 Q19 1 0.4400 0.3529 0.8623 11.00000 0.05 0.61 Q20 1 0.4401 0.4062 0.8195 11.00000 0.05 0.58 ; _shelx_res_checksum 67949 _shelx_hkl_file ; 2 0 0 4250.37 118.29 -2 0 0 4532.95 119.89 -2 0 0 4268.37 118.69 -4 0 0 1141.29 37.50 -4 0 0 1058.09 34.50 4 0 0 1067.69 33.80 -6 0 0 2.70 10.20 -6 0 0 -0.40 8.60 6 0 0 8.50 7.70 -8 0 0 103.19 15.60 -8 0 0 101.69 13.20 8 0 0 119.09 12.20 -10 0 0 92.39 16.80 -10 0 0 94.09 14.20 10 0 0 102.19 13.00 -12 0 0 1735.63 65.49 -12 0 0 1599.64 58.19 12 0 0 1663.73 56.59 -14 0 0 2001.20 77.29 -14 0 0 1931.61 68.89 14 0 0 1961.60 66.39 16 0 0 2142.09 71.99 -16 0 0 1981.90 74.19 -16 0 0 2164.18 83.79 -18 0 0 1315.97 57.99 18 0 0 1303.37 53.19 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