# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_a00719b _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H24 Br N3' _chemical_formula_weight 386.33 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 21/c' _space_group_name_Hall '-P 2ybc' _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+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.403(4) _cell_length_b 9.077(3) _cell_length_c 20.526(7) _cell_angle_alpha 90 _cell_angle_beta 96.017(5) _cell_angle_gamma 90 _cell_volume 1927.5(12) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 898 _cell_measurement_theta_min 2.955 _cell_measurement_theta_max 24.204 _exptl_crystal_description Block _exptl_crystal_colour colorless _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.331 _exptl_crystal_F_000 800 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.100 _exptl_crystal_size_mid 0.080 _exptl_crystal_size_min 0.050 _exptl_absorpt_coefficient_mu 2.138 _shelx_estimated_absorpt_T_min 0.815 _shelx_estimated_absorpt_T_max 0.901 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.70488 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source ? _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 7748 _diffrn_reflns_av_unetI/netI 0.0728 _diffrn_reflns_av_R_equivalents 0.0521 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.969 _diffrn_reflns_theta_max 25.010 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.995 _diffrn_measured_fraction_theta_full 0.974 _diffrn_reflns_Laue_measured_fraction_max 0.995 _diffrn_reflns_Laue_measured_fraction_full 0.974 _diffrn_reflns_point_group_measured_fraction_max 0.995 _diffrn_reflns_point_group_measured_fraction_full 0.974 _reflns_number_total 3391 _reflns_number_gt 1732 _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 SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1464P)^2^] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 3391 _refine_ls_number_parameters 217 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1283 _refine_ls_R_factor_gt 0.0761 _refine_ls_wR_factor_ref 0.2331 _refine_ls_wR_factor_gt 0.2109 _refine_ls_goodness_of_fit_ref 0.915 _refine_ls_restrained_S_all 0.916 _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 Br1 Br 0.64135(9) 0.43728(8) 0.15089(4) 0.0860(4) Uani 1 1 d . . . . . N1 N 0.6715(4) -0.0581(5) 0.1221(2) 0.0393(11) Uani 1 1 d . . . . . N2 N 0.6409(4) 0.0280(5) 0.2177(2) 0.0358(11) Uani 1 1 d . . . . . N3 N 0.8705(5) 0.2562(6) 0.2511(3) 0.0590(15) Uani 1 1 d . . . . . H3B H 0.8058 0.2528 0.2214 0.071 Uiso 1 1 calc R U . . . C1 C 0.7461(9) -0.0684(9) -0.1495(4) 0.091(3) Uani 1 1 d . . . . . H1A H 0.6878 -0.1380 -0.1720 0.137 Uiso 1 1 calc R U . . . H1B H 0.8335 -0.0950 -0.1554 0.137 Uiso 1 1 calc R U . . . H1C H 0.7280 0.0283 -0.1670 0.137 Uiso 1 1 calc R U . . . C2 C 0.7291(7) -0.0693(7) -0.0783(3) 0.0594(18) Uani 1 1 d . . . . . C3 C 0.6360(6) -0.1561(7) -0.0538(3) 0.0555(17) Uani 1 1 d . . . . . H3A H 0.5869 -0.2185 -0.0825 0.067 Uiso 1 1 calc R U . . . C4 C 0.6123(5) -0.1547(6) 0.0111(3) 0.0496(16) Uani 1 1 d . . . . . C5 C 0.6913(5) -0.0633(6) 0.0545(3) 0.0426(14) Uani 1 1 d . . . . . C6 C 0.7878(5) 0.0254(7) 0.0315(3) 0.0473(15) Uani 1 1 d . . . . . C7 C 0.8014(6) 0.0195(7) -0.0338(3) 0.0599(18) Uani 1 1 d . . . . . H7A H 0.8638 0.0795 -0.0495 0.072 Uiso 1 1 calc R U . . . C8 C 0.5058(6) -0.2472(7) 0.0346(3) 0.0623(18) Uani 1 1 d . . . . . H8A H 0.4632 -0.3016 -0.0016 0.094 Uiso 1 1 calc R U . . . H8B H 0.4443 -0.1844 0.0527 0.094 Uiso 1 1 calc R U . . . H8C H 0.5419 -0.3147 0.0676 0.094 Uiso 1 1 calc R U . . . C9 C 0.8728(6) 0.1268(8) 0.0765(3) 0.0607(18) Uani 1 1 d . . . . . H9A H 0.9326 0.1771 0.0516 0.091 Uiso 1 1 calc R U . . . H9B H 0.9198 0.0698 0.1104 0.091 Uiso 1 1 calc R U . . . H9C H 0.8197 0.1977 0.0958 0.091 Uiso 1 1 calc R U . . . C10 C 0.6482(5) 0.0622(6) 0.1571(3) 0.0402(14) Uani 1 1 d . . . . . H10A H 0.6386 0.1569 0.1400 0.048 Uiso 1 1 calc R U . . . C11 C 0.6786(5) -0.1774(7) 0.1661(3) 0.0511(16) Uani 1 1 d . . . . . H11A H 0.6941 -0.2756 0.1566 0.061 Uiso 1 1 calc R U . . . C12 C 0.6586(5) -0.1211(7) 0.2240(3) 0.0522(16) Uani 1 1 d . . . . . H12A H 0.6569 -0.1744 0.2626 0.063 Uiso 1 1 calc R U . . . C13 C 0.6259(5) 0.1316(7) 0.2722(3) 0.0455(15) Uani 1 1 d . . . . . H13A H 0.5499 0.1049 0.2932 0.055 Uiso 1 1 calc R U . . . H13B H 0.6132 0.2306 0.2549 0.055 Uiso 1 1 calc R U . . . C14 C 0.7428(6) 0.1294(7) 0.3222(3) 0.0484(15) Uani 1 1 d . . . . . C15 C 0.7305(8) 0.0570(8) 0.3812(4) 0.076(2) Uani 1 1 d . . . . . H15A H 0.6514 0.0159 0.3885 0.091 Uiso 1 1 calc R U . . . C16 C 0.8336(12) 0.0457(12) 0.4287(5) 0.110(3) Uani 1 1 d D . . . . H16A H 0.8261 -0.0013 0.4684 0.132 Uiso 1 1 calc R U . . . C17 C 0.9471(11) 0.1064(13) 0.4149(5) 0.124(4) Uani 1 1 d D . . . . H17A H 1.0179 0.0993 0.4464 0.148 Uiso 1 1 calc R U . . . C18 C 0.9638(7) 0.1784(10) 0.3567(4) 0.081(2) Uani 1 1 d . . . . . H18A H 1.0434 0.2188 0.3498 0.097 Uiso 1 1 calc R U . . . C19 C 0.8596(6) 0.1888(7) 0.3094(3) 0.0511(16) Uani 1 1 d . . . . . C20 C 0.9873(7) 0.3343(11) 0.2368(4) 0.092(3) Uani 1 1 d . . . . . H20A H 0.9746 0.3740 0.1932 0.138 Uiso 1 1 calc R U . . . H20B H 1.0589 0.2672 0.2401 0.138 Uiso 1 1 calc R U . . . H20C H 1.0049 0.4131 0.2676 0.138 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 Br1 0.1108(8) 0.0475(5) 0.0976(8) 0.0038(4) 0.0015(5) 0.0125(4) N1 0.035(2) 0.028(2) 0.054(3) 0.003(2) -0.001(2) 0.0005(19) N2 0.030(2) 0.034(3) 0.044(3) 0.010(2) 0.003(2) -0.0013(18) N3 0.039(3) 0.082(4) 0.056(4) -0.009(3) 0.005(2) -0.012(3) C1 0.102(6) 0.092(6) 0.082(6) -0.028(5) 0.016(5) -0.017(5) C2 0.067(4) 0.054(4) 0.056(4) -0.019(3) 0.003(3) 0.010(4) C3 0.065(4) 0.042(4) 0.055(5) -0.017(3) -0.014(3) 0.010(3) C4 0.042(3) 0.031(3) 0.073(5) 0.000(3) -0.009(3) 0.007(3) C5 0.039(3) 0.031(3) 0.057(4) -0.006(3) 0.000(3) 0.011(3) C6 0.043(3) 0.044(4) 0.057(4) -0.015(3) 0.014(3) 0.003(3) C7 0.056(4) 0.049(4) 0.078(5) -0.007(4) 0.022(4) -0.005(3) C8 0.055(4) 0.054(4) 0.075(5) 0.003(3) -0.011(3) -0.007(3) C9 0.049(4) 0.068(5) 0.068(5) -0.018(4) 0.015(3) -0.016(3) C10 0.032(3) 0.029(3) 0.059(4) 0.006(3) 0.003(3) -0.001(2) C11 0.044(4) 0.038(3) 0.068(5) 0.007(3) -0.007(3) 0.002(3) C12 0.049(4) 0.043(3) 0.063(5) 0.018(3) -0.005(3) -0.005(3) C13 0.040(3) 0.051(4) 0.048(4) 0.012(3) 0.016(3) 0.008(3) C14 0.058(4) 0.046(3) 0.042(4) 0.001(3) 0.007(3) 0.013(3) C15 0.091(5) 0.077(5) 0.060(5) 0.011(4) 0.003(4) 0.010(4) C16 0.122(8) 0.122(9) 0.080(7) 0.041(6) -0.019(6) -0.002(7) C17 0.138(10) 0.127(9) 0.090(8) -0.009(7) -0.066(7) 0.046(8) C18 0.062(5) 0.099(6) 0.075(6) -0.009(5) -0.019(4) 0.008(4) C19 0.043(4) 0.058(4) 0.052(4) -0.004(3) 0.006(3) 0.008(3) C20 0.070(5) 0.120(7) 0.091(6) -0.026(5) 0.031(4) -0.045(5) _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 N1 C10 1.342(7) . ? N1 C11 1.407(7) . ? N1 C5 1.425(8) . ? N2 C10 1.293(7) . ? N2 C12 1.370(8) . ? N2 C13 1.482(7) . ? N3 C19 1.358(8) . ? N3 C20 1.463(8) . ? N3 H3B 0.8600 . ? C1 C2 1.491(10) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C7 1.380(9) . ? C2 C3 1.384(9) . ? C3 C4 1.381(8) . ? C3 H3A 0.9300 . ? C4 C5 1.414(8) . ? C4 C8 1.510(9) . ? C5 C6 1.406(8) . ? C6 C7 1.364(9) . ? C6 C9 1.520(8) . ? C7 H7A 0.9300 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9300 . ? C11 C12 1.330(9) . ? C11 H11A 0.9300 . ? C12 H12A 0.9300 . ? C13 C14 1.508(8) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C19 1.380(8) . ? C14 C15 1.395(9) . ? C15 C16 1.377(12) . ? C15 H15A 0.9300 . ? C16 C17 1.359(9) . ? C16 H16A 0.9300 . ? C17 C18 1.389(13) . ? C17 H17A 0.9300 . ? C18 C19 1.382(9) . ? C18 H18A 0.9300 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? 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 C10 N1 C11 106.4(5) . . ? C10 N1 C5 126.9(5) . . ? C11 N1 C5 126.6(5) . . ? C10 N2 C12 107.8(5) . . ? C10 N2 C13 126.6(5) . . ? C12 N2 C13 125.4(5) . . ? C19 N3 C20 122.9(6) . . ? C19 N3 H3B 118.6 . . ? C20 N3 H3B 118.6 . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C7 C2 C3 116.5(6) . . ? C7 C2 C1 122.2(7) . . ? C3 C2 C1 121.2(6) . . ? C4 C3 C2 123.2(6) . . ? C4 C3 H3A 118.4 . . ? C2 C3 H3A 118.4 . . ? C3 C4 C5 117.5(6) . . ? C3 C4 C8 120.9(6) . . ? C5 C4 C8 121.6(6) . . ? C6 C5 C4 120.9(6) . . ? C6 C5 N1 119.3(5) . . ? C4 C5 N1 119.9(5) . . ? C7 C6 C5 117.3(6) . . ? C7 C6 C9 120.4(6) . . ? C5 C6 C9 122.2(6) . . ? C6 C7 C2 124.6(6) . . ? C6 C7 H7A 117.7 . . ? C2 C7 H7A 117.7 . . ? C4 C8 H8A 109.5 . . ? C4 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C4 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 . . ? N2 C10 N1 110.6(5) . . ? N2 C10 H10A 124.7 . . ? N1 C10 H10A 124.7 . . ? C12 C11 N1 106.0(5) . . ? C12 C11 H11A 127.0 . . ? N1 C11 H11A 127.0 . . ? C11 C12 N2 109.1(6) . . ? C11 C12 H12A 125.4 . . ? N2 C12 H12A 125.4 . . ? N2 C13 C14 111.3(4) . . ? N2 C13 H13A 109.4 . . ? C14 C13 H13A 109.4 . . ? N2 C13 H13B 109.4 . . ? C14 C13 H13B 109.4 . . ? H13A C13 H13B 108.0 . . ? C19 C14 C15 120.9(6) . . ? C19 C14 C13 121.9(5) . . ? C15 C14 C13 117.1(6) . . ? C16 C15 C14 120.9(8) . . ? C16 C15 H15A 119.5 . . ? C14 C15 H15A 119.5 . . ? C17 C16 C15 116.9(9) . . ? C17 C16 H16A 121.6 . . ? C15 C16 H16A 121.6 . . ? C16 C17 C18 124.1(8) . . ? C16 C17 H17A 118.0 . . ? C18 C17 H17A 118.0 . . ? C19 C18 C17 118.5(8) . . ? C19 C18 H18A 120.7 . . ? C17 C18 H18A 120.7 . . ? N3 C19 C14 120.0(5) . . ? N3 C19 C18 121.3(6) . . ? C14 C19 C18 118.7(7) . . ? N3 C20 H20A 109.5 . . ? N3 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? N3 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C13 H13B Br1 0.97 2.88 3.743(6) 148.8 . C13 H13A Br1 0.97 2.84 3.775(6) 162.1 2_645 C11 H11A Br1 0.93 2.66 3.529(7) 155.2 1_545 C10 H10A Br1 0.93 2.55 3.407(6) 152.7 . N3 H3B N2 0.86 2.66 3.181(7) 120.1 . N3 H3B Br1 0.86 2.70 3.404(6) 139.6 . C13 H13B Br1 0.97 2.88 3.743(6) 148.8 . C13 H13A Br1 0.97 2.84 3.775(6) 162.1 2_645 C11 H11A Br1 0.93 2.66 3.529(7) 155.2 1_545 C10 H10A Br1 0.93 2.55 3.407(6) 152.7 . N3 H3B N2 0.86 2.66 3.181(7) 120.1 . N3 H3B Br1 0.86 2.70 3.404(6) 139.6 . C13 H13B Br1 0.97 2.88 3.743(6) 148.8 . C13 H13A Br1 0.97 2.84 3.775(6) 162.1 2_645 C11 H11A Br1 0.93 2.66 3.529(7) 155.2 1_545 C10 H10A Br1 0.93 2.55 3.407(6) 152.7 . N3 H3B N2 0.86 2.66 3.181(7) 120.1 . N3 H3B Br1 0.86 2.70 3.404(6) 139.6 . C10 H10A Br1 0.93 2.55 3.407(6) 152.7 . N3 H3B N2 0.86 2.66 3.181(7) 120.1 . N3 H3B Br1 0.86 2.70 3.404(6) 139.6 . _refine_diff_density_max 0.542 _refine_diff_density_min -0.540 _refine_diff_density_rms 0.126 _shelxl_version_number 2013-2 _shelx_res_file ; TITL a00719b in P2(1)/c CELL 0.71073 10.4027 9.0768 20.5264 90.000 96.017 90.000 ZERR 4.00 0.0037 0.0032 0.0073 0.000 0.005 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N Br UNIT 80 96 12 4 omit 0 2 1 omit 2 1 1 omit -1 1 1 omit 0 1 2 omit 0 1 11 omit 0 1 1 OMIT -3.00 50.02 L.S. 10 ACTA BOND $H FMAP 2 PLAN 4 HTAB C13 Br1 HTAB C13 Br1_$2 HTAB C11 Br1_$1 HTAB C10 Br1 HTAB N3 N2 HTAB N3 Br1 HTAB C13 Br1 HTAB C13 Br1_$2 HTAB C11 Br1_$1 HTAB C10 Br1 HTAB N3 N2 HTAB N3 Br1 HTAB C13 Br1 HTAB C13 Br1_$2 EQIV $2 -x+1, y-1/2, -z+1/2 HTAB C11 Br1_$1 EQIV $1 x, y-1, z HTAB C10 Br1 HTAB N3 N2 dfix 1.39 0.01 c16 c17 HTAB N3 Br1 htab htab c10 br1 htab n3 n2 htab n3 br1 size 0.10 0.08 0.05 TEMP 20 WGHT 0.146400 FVAR 0.27549 BR1 4 0.641352 0.437277 0.150885 11.00000 0.11080 0.04754 = 0.09764 0.00378 0.00147 0.01253 N1 3 0.671489 -0.058078 0.122094 11.00000 0.03471 0.02810 = 0.05385 0.00341 -0.00079 0.00054 N2 3 0.640925 0.028022 0.217730 11.00000 0.02964 0.03376 = 0.04387 0.00998 0.00339 -0.00131 N3 3 0.870456 0.256170 0.251140 11.00000 0.03884 0.08205 = 0.05614 -0.00947 0.00510 -0.01194 AFIX 43 H3B 2 0.805845 0.252755 0.221389 11.00000 -1.20000 AFIX 0 C1 1 0.746101 -0.068413 -0.149536 11.00000 0.10212 0.09206 = 0.08169 -0.02752 0.01615 -0.01676 AFIX 33 H1A 2 0.687753 -0.138040 -0.171989 11.00000 -1.50000 H1B 2 0.833455 -0.094976 -0.155433 11.00000 -1.50000 H1C 2 0.728030 0.028339 -0.167047 11.00000 -1.50000 AFIX 0 C2 1 0.729119 -0.069285 -0.078307 11.00000 0.06742 0.05431 = 0.05581 -0.01852 0.00282 0.00977 C3 1 0.635950 -0.156138 -0.053824 11.00000 0.06460 0.04237 = 0.05515 -0.01716 -0.01400 0.01018 AFIX 43 H3A 2 0.586874 -0.218521 -0.082508 11.00000 -1.20000 AFIX 0 C4 1 0.612323 -0.154657 0.011147 11.00000 0.04203 0.03056 = 0.07307 -0.00014 -0.00897 0.00749 C5 1 0.691274 -0.063273 0.054460 11.00000 0.03928 0.03080 = 0.05683 -0.00608 0.00046 0.01085 C6 1 0.787767 0.025388 0.031491 11.00000 0.04334 0.04368 = 0.05688 -0.01493 0.01409 0.00273 C7 1 0.801413 0.019500 -0.033846 11.00000 0.05578 0.04880 = 0.07833 -0.00717 0.02182 -0.00460 AFIX 43 H7A 2 0.863791 0.079514 -0.049509 11.00000 -1.20000 AFIX 0 C8 1 0.505761 -0.247234 0.034607 11.00000 0.05502 0.05350 = 0.07473 0.00253 -0.01097 -0.00712 AFIX 33 H8A 2 0.463239 -0.301559 -0.001577 11.00000 -1.50000 H8B 2 0.444343 -0.184366 0.052705 11.00000 -1.50000 H8C 2 0.541933 -0.314650 0.067613 11.00000 -1.50000 AFIX 0 C9 1 0.872815 0.126849 0.076458 11.00000 0.04873 0.06773 = 0.06752 -0.01775 0.01454 -0.01631 AFIX 33 H9A 2 0.932576 0.177130 0.051601 11.00000 -1.50000 H9B 2 0.919825 0.069758 0.110398 11.00000 -1.50000 H9C 2 0.819746 0.197723 0.095769 11.00000 -1.50000 AFIX 0 C10 1 0.648190 0.062183 0.157054 11.00000 0.03239 0.02862 = 0.05915 0.00574 0.00324 -0.00119 AFIX 43 H10A 2 0.638599 0.156944 0.140007 11.00000 -1.20000 AFIX 0 C11 1 0.678601 -0.177376 0.166082 11.00000 0.04432 0.03778 = 0.06832 0.00728 -0.00746 0.00166 AFIX 43 H11A 2 0.694127 -0.275569 0.156605 11.00000 -1.20000 AFIX 0 C12 1 0.658587 -0.121071 0.223993 11.00000 0.04890 0.04274 = 0.06265 0.01825 -0.00533 -0.00546 AFIX 43 H12A 2 0.656861 -0.174409 0.262576 11.00000 -1.20000 AFIX 0 C13 1 0.625896 0.131629 0.272206 11.00000 0.04008 0.05098 = 0.04785 0.01194 0.01565 0.00787 AFIX 23 H13A 2 0.549885 0.104886 0.293181 11.00000 -1.20000 H13B 2 0.613216 0.230568 0.254854 11.00000 -1.20000 AFIX 0 C14 1 0.742844 0.129393 0.322226 11.00000 0.05829 0.04582 = 0.04151 0.00115 0.00676 0.01325 C15 1 0.730452 0.057028 0.381212 11.00000 0.09052 0.07703 = 0.05970 0.01116 0.00260 0.01029 AFIX 43 H15A 2 0.651364 0.015861 0.388522 11.00000 -1.20000 AFIX 0 C16 1 0.833631 0.045707 0.428740 11.00000 0.12205 0.12207 = 0.08040 0.04078 -0.01947 -0.00193 AFIX 43 H16A 2 0.826054 -0.001267 0.468421 11.00000 -1.20000 AFIX 0 C17 1 0.947065 0.106392 0.414948 11.00000 0.13757 0.12749 = 0.08972 -0.00930 -0.06557 0.04554 AFIX 43 H17A 2 1.017884 0.099255 0.446437 11.00000 -1.20000 AFIX 0 C18 1 0.963822 0.178429 0.356736 11.00000 0.06220 0.09881 = 0.07491 -0.00870 -0.01937 0.00842 AFIX 43 H18A 2 1.043430 0.218778 0.349803 11.00000 -1.20000 AFIX 0 C19 1 0.859612 0.188812 0.309364 11.00000 0.04308 0.05828 = 0.05193 -0.00439 0.00563 0.00756 C20 1 0.987259 0.334335 0.236775 11.00000 0.06957 0.12030 = 0.09071 -0.02551 0.03089 -0.04489 AFIX 33 H20A 2 0.974568 0.373978 0.193216 11.00000 -1.50000 H20B 2 1.058947 0.267189 0.240059 11.00000 -1.50000 H20C 2 1.004880 0.413111 0.267628 11.00000 -1.50000 AFIX 0 HKLF 4 REM a00719b in P2(1)/c REM R1 = 0.0761 for 1732 Fo > 4sig(Fo) and 0.1283 for all 3391 data REM 217 parameters refined using 1 restraints END WGHT 0.1464 0.0000 REM Instructions for potential hydrogen bonds HTAB N3 Br1 HTAB N3 N2 HTAB C10 Br1 HTAB C11 Br1_$1 HTAB C13 Br1_$2 HTAB C13 Br1 REM Highest difference peak 0.542, deepest hole -0.540, 1-sigma level 0.126 Q1 1 0.8154 0.3105 0.2365 11.00000 0.05 0.54 Q2 1 0.9231 0.2884 0.2484 11.00000 0.05 0.54 Q3 1 0.6545 -0.1428 0.1488 11.00000 0.05 0.51 Q4 1 0.7607 -0.0439 -0.0515 11.00000 0.05 0.49 ; _shelx_res_checksum 70050 _shelx_hkl_file ; 1 -2 -26 -0.37 6.90 2 -2 -26 -0.74 5.97 1 -1 -26 2.74 6.41 2 -1 -26 2.99 6.49 1 0 -26 -1.35 6.09 2 0 -26 0.98 6.43 3 0 -26 -3.10 5.55 1 1 -26 -0.80 5.80 2 1 -26 0.21 5.73 1 2 -26 5.76 6.57 2 2 -26 -0.50 6.14 1 3 -26 -0.65 5.72 1 -2 -25 1.92 6.53 2 -2 -25 2.62 6.30 3 -2 -25 1.19 6.40 4 -2 -25 -1.13 5.66 1 -1 -25 -1.22 5.84 2 -1 -25 1.21 5.36 3 -1 -25 2.66 6.25 4 -1 -25 3.27 5.89 1 0 -25 -3.74 5.62 2 0 -25 1.00 5.90 3 0 -25 -1.59 5.20 4 0 -25 4.96 6.70 1 1 -25 -2.07 5.26 2 1 -25 -1.33 5.37 3 1 -25 2.68 5.78 4 1 -25 0.58 5.24 1 2 -25 0.17 5.22 2 2 -25 -1.51 4.62 3 2 -25 3.60 5.03 1 3 -25 0.49 5.05 2 3 -25 -0.59 5.60 3 3 -25 0.77 5.23 1 4 -25 4.86 5.48 1 -2 -24 0.32 4.70 2 -2 -24 2.57 5.97 3 -2 -24 -0.98 5.84 4 -2 -24 2.05 5.73 5 -2 -24 -3.61 6.65 0 -1 -24 6.50 5.58 1 -1 -24 0.79 5.30 2 -1 -24 4.75 5.56 3 -1 -24 -5.07 5.35 4 -1 -24 -3.61 5.76 5 -1 -24 1.05 5.54 0 0 -24 0.32 5.13 1 0 -24 1.83 5.38 2 0 -24 -2.34 5.39 3 0 -24 -2.81 4.68 4 0 -24 0.30 5.96 5 0 -24 3.70 6.38 0 1 -24 1.60 4.78 1 1 -24 -0.28 5.33 2 1 -24 2.92 4.96 3 1 -24 0.88 4.92 4 1 -24 -2.31 5.48 5 1 -24 -0.27 5.13 0 2 -24 2.10 4.89 1 2 -24 1.97 5.08 2 2 -24 0.83 5.10 3 2 -24 4.76 5.28 4 2 -24 -0.13 5.31 5 2 -24 -0.17 5.08 0 3 -24 3.95 4.79 1 3 -24 2.55 4.81 2 3 -24 2.21 5.59 3 3 -24 -1.08 4.40 4 3 -24 -0.08 4.49 0 4 -24 4.33 5.25 1 4 -24 -4.27 5.64 2 4 -24 2.63 5.38 3 4 -24 1.51 5.53 0 5 -24 1.51 6.02 1 5 -24 -0.94 5.73 0 -2 -23 -0.97 5.28 1 -2 -23 0.72 4.95 2 -2 -23 0.71 4.77 3 -2 -23 -0.11 4.87 4 -2 -23 0.96 5.13 5 -2 -23 -5.23 4.83 6 -2 -23 2.08 5.96 0 -1 -23 3.36 4.84 1 -1 -23 -1.58 4.06 2 -1 -23 2.07 5.20 3 -1 -23 1.84 4.68 4 -1 -23 3.62 4.99 5 -1 -23 0.57 4.97 6 -1 -23 -0.57 5.65 0 0 -23 -0.03 4.57 1 0 -23 -2.58 4.72 2 0 -23 1.07 5.01 3 0 -23 0.73 5.13 4 0 -23 1.87 5.34 5 0 -23 -0.29 5.61 6 0 -23 0.43 5.67 7 0 -23 3.92 5.66 0 1 -23 4.77 5.05 1 1 -23 0.99 4.81 2 1 -23 -4.87 4.95 3 1 -23 1.61 4.70 4 1 -23 5.65 5.65 5 1 -23 0.29 5.13 6 1 -23 0.35 5.13 0 2 -23 -0.36 4.54 1 2 -23 -2.56 4.53 2 2 -23 -2.20 4.66 3 2 -23 0.01 4.46 4 2 -23 0.71 4.50 5 2 -23 -0.26 4.66 6 2 -23 -0.65 4.75 0 3 -23 -1.63 4.76 1 3 -23 0.98 4.47 2 3 -23 -0.54 5.10 3 3 -23 -1.54 4.68 4 3 -23 0.17 5.19 5 3 -23 -0.92 4.27 0 4 -23 3.02 5.24 1 4 -23 2.79 5.41 2 4 -23 4.35 4.94 3 4 -23 -0.07 4.93 4 4 -23 -2.74 5.86 0 5 -23 5.06 6.08 1 5 -23 2.43 5.95 2 5 -23 -1.08 5.77 3 5 -23 1.15 6.16 0 6 -23 -0.67 6.00 4 -3 -22 6.43 5.61 5 -3 -22 2.83 5.90 0 -2 -22 2.87 4.08 1 -2 -22 0.57 4.90 2 -2 -22 4.76 4.74 3 -2 -22 3.90 4.85 4 -2 -22 -0.80 4.64 5 -2 -22 1.73 5.18 6 -2 -22 -0.07 5.24 7 -2 -22 -1.62 6.04 0 -1 -22 4.14 4.62 1 -1 -22 1.34 4.59 2 -1 -22 1.47 4.28 3 -1 -22 0.25 4.84 4 -1 -22 0.16 4.51 5 -1 -22 -2.65 5.33 6 -1 -22 1.51 4.84 7 -1 -22 5.89 6.55 0 0 -22 2.58 4.49 1 0 -22 0.67 4.49 2 0 -22 6.79 4.92 3 0 -22 0.28 4.49 4 0 -22 2.57 4.64 5 0 -22 -1.45 4.68 6 0 -22 0.52 5.36 7 0 -22 -0.78 5.37 0 1 -22 0.88 4.45 1 1 -22 3.95 4.47 2 1 -22 2.49 4.48 3 1 -22 2.84 4.66 4 1 -22 1.14 4.90 5 1 -22 0.23 4.80 6 1 -22 -2.17 4.59 7 1 -22 -0.32 5.60 0 2 -22 0.93 4.23 1 2 -22 0.44 3.46 2 2 -22 1.55 3.76 3 2 -22 1.07 4.09 4 2 -22 3.83 4.58 5 2 -22 0.68 5.31 6 2 -22 1.98 5.06 7 2 -22 0.50 5.20 0 3 -22 6.48 4.80 1 3 -22 2.97 4.36 2 3 -22 -1.96 4.69 3 3 -22 2.85 4.43 4 3 -22 3.16 5.27 5 3 -22 2.17 5.59 6 3 -22 2.26 4.28 0 4 -22 3.29 4.35 1 4 -22 -0.69 4.20 2 4 -22 -1.10 4.92 3 4 -22 0.62 4.49 4 4 -22 -2.09 5.27 5 4 -22 -6.34 5.65 0 5 -22 1.96 5.53 1 5 -22 7.85 5.20 2 5 -22 1.53 4.83 3 5 -22 -0.81 5.62 4 5 -22 3.65 6.07 0 6 -22 1.32 5.94 1 6 -22 1.12 6.00 2 6 -22 3.03 6.36 3 -3 -21 -0.37 5.28 4 -3 -21 -3.89 5.68 5 -3 -21 1.89 6.11 6 -3 -21 -0.66 5.10 0 -2 -21 9.19 4.69 1 -2 -21 -1.43 4.66 2 -2 -21 4.03 4.51 3 -2 -21 7.87 4.85 4 -2 -21 2.88 4.87 5 -2 -21 1.29 5.61 6 -2 -21 -0.19 5.48 7 -2 -21 -2.50 5.34 8 -2 -21 4.91 5.22 9 -2 -21 1.49 5.53 -1 -1 -21 2.81 4.36 0 -1 -21 7.62 4.59 1 -1 -21 14.65 5.08 2 -1 -21 5.13 4.82 3 -1 -21 0.88 4.23 4 -1 -21 11.11 5.68 5 -1 -21 5.43 5.48 6 -1 -21 -1.30 4.34 7 -1 -21 -0.40 5.59 8 -1 -21 -0.48 4.83 -1 0 -21 1.67 4.29 0 0 -21 1.22 4.10 1 0 -21 0.76 4.22 2 0 -21 0.77 4.27 3 0 -21 -1.04 4.32 4 0 -21 0.48 4.05 5 0 -21 -3.24 4.92 6 0 -21 -1.36 5.07 7 0 -21 4.43 5.89 8 0 -21 7.04 5.89 -1 1 -21 1.15 4.23 0 1 -21 6.06 4.15 1 1 -21 14.04 4.72 2 1 -21 5.84 3.82 3 1 -21 0.65 4.28 4 1 -21 3.52 4.69 5 1 -21 2.72 4.42 6 1 -21 -0.82 4.47 7 1 -21 0.82 4.85 8 1 -21 3.98 4.69 -1 2 -21 3.69 3.59 0 2 -21 9.36 4.66 1 2 -21 1.54 3.63 2 2 -21 0.44 3.63 3 2 -21 4.56 3.79 4 2 -21 1.24 4.42 5 2 -21 0.38 4.09 6 2 -21 -0.43 4.83 7 2 -21 0.00 5.20 8 2 -21 -3.07 4.39 -1 3 -21 1.97 4.39 0 3 -21 -0.99 4.44 1 3 -21 0.69 4.58 2 3 -21 0.24 4.03 3 3 -21 1.28 4.81 4 3 -21 0.30 4.36 5 3 -21 1.22 4.53 6 3 -21 -0.67 4.35 7 3 -21 1.42 4.12 -1 4 -21 2.88 4.56 0 4 -21 2.50 4.67 1 4 -21 -2.48 4.70 2 4 -21 7.46 5.14 3 4 -21 4.90 4.79 4 4 -21 -3.09 4.92 5 4 -21 3.76 4.79 6 4 -21 -0.76 4.72 7 4 -21 -0.70 4.98 -1 5 -21 -2.82 4.78 0 5 -21 -1.86 4.36 1 5 -21 6.80 5.67 2 5 -21 2.46 5.40 3 5 -21 1.07 4.64 4 5 -21 -1.18 4.48 5 5 -21 -3.47 5.61 -1 6 -21 0.77 5.25 0 6 -21 0.28 4.63 1 6 -21 -1.19 5.63 2 6 -21 1.32 5.05 3 6 -21 3.75 5.88 4 6 -21 2.36 5.50 -1 7 -21 -1.33 5.91 0 7 -21 1.81 5.31 1 7 -21 -1.97 5.10 3 -3 -20 4.36 5.55 4 -3 -20 -3.93 4.61 5 -3 -20 0.23 5.16 6 -3 -20 3.37 5.29 9 -3 -20 -3.78 5.73 -1 -2 -20 10.68 5.07 0 -2 -20 -0.82 3.61 1 -2 -20 10.19 4.97 2 -2 -20 2.42 4.27 3 -2 -20 1.72 4.31 4 -2 -20 -0.13 4.35 5 -2 -20 2.42 5.32 6 -2 -20 -2.55 4.42 7 -2 -20 1.08 5.70 8 -2 -20 0.15 3.76 9 -2 -20 -1.06 3.76 -1 -1 -20 1.58 4.06 0 -1 -20 -0.14 4.15 1 -1 -20 -2.21 4.05 2 -1 -20 -0.98 3.86 3 -1 -20 0.03 4.04 4 -1 -20 -2.35 4.08 5 -1 -20 1.30 4.56 6 -1 -20 1.09 4.40 7 -1 -20 2.34 3.17 8 -1 -20 3.39 5.68 9 -1 -20 -0.07 3.95 -1 0 -20 1.56 3.85 0 0 -20 0.71 3.79 1 0 -20 17.87 4.69 2 0 -20 12.02 4.88 3 0 -20 -0.52 3.71 4 0 -20 18.05 5.32 5 0 -20 5.94 4.43 6 0 -20 -0.36 4.18 7 0 -20 2.32 5.31 8 0 -20 4.23 5.50 9 0 -20 2.84 5.88 -1 1 -20 1.59 3.66 0 1 -20 0.58 3.82 1 1 -20 3.31 4.02 2 1 -20 0.45 4.21 3 1 -20 0.16 3.71 4 1 -20 -0.09 4.22 5 1 -20 3.33 4.08 6 1 -20 -0.33 4.45 7 1 -20 -0.44 4.54 8 1 -20 0.06 4.80 9 1 -20 -2.02 4.63 -1 2 -20 4.69 4.21 0 2 -20 -1.88 3.87 1 2 -20 9.08 4.00 2 2 -20 2.60 4.31 3 2 -20 3.50 4.44 4 2 -20 3.40 3.94 5 2 -20 0.52 3.61 6 2 -20 -2.60 4.51 7 2 -20 3.58 5.31 8 2 -20 -2.44 4.04 9 2 -20 -2.14 4.86 -1 3 -20 1.78 3.38 0 3 -20 1.05 4.09 1 3 -20 1.27 4.25 2 3 -20 15.77 4.50 3 3 -20 9.42 4.64 4 3 -20 -3.00 3.89 5 3 -20 -0.47 4.80 6 3 -20 5.00 5.00 7 3 -20 2.35 4.42 8 3 -20 -1.22 4.91 -1 4 -20 -1.18 4.16 0 4 -20 5.84 4.63 1 4 -20 2.34 4.03 2 4 -20 1.47 3.91 3 4 -20 1.64 4.76 4 4 -20 0.88 4.91 5 4 -20 1.48 4.34 6 4 -20 3.76 5.00 7 4 -20 -1.05 5.09 8 4 -20 4.96 5.95 -1 5 -20 12.22 4.67 0 5 -20 -3.85 3.87 1 5 -20 3.42 4.96 2 5 -20 5.57 4.60 3 5 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5 2 0 29.63 1.90 6 2 0 23.46 1.94 7 2 0 135.29 6.67 8 2 0 3.04 3.51 9 2 0 3.40 3.44 10 2 0 4.42 3.92 11 2 0 11.14 4.78 12 2 0 -0.37 5.32 -6 3 0 222.95 6.93 -5 3 0 64.46 3.96 -4 3 0 6.61 2.26 -3 3 0 218.37 6.22 -2 3 0 308.11 7.20 -1 3 0 320.09 6.98 0 3 0 0.69 1.73 1 3 0 322.74 6.74 2 3 0 314.10 4.66 3 3 0 213.94 4.06 4 3 0 6.45 1.63 5 3 0 71.15 2.84 6 3 0 242.92 5.03 7 3 0 3.14 3.11 8 3 0 22.53 3.98 9 3 0 29.38 5.35 10 3 0 18.33 4.66 11 3 0 -1.72 4.01 12 3 0 6.55 5.57 -6 4 0 11.83 3.28 -5 4 0 4.21 2.68 -4 4 0 20.51 3.24 -3 4 0 239.58 7.60 -2 4 0 4.18 2.60 -1 4 0 1.62 2.18 0 4 0 35.27 3.21 1 4 0 0.14 1.87 2 4 0 4.82 1.57 3 4 0 245.82 4.86 4 4 0 16.68 1.98 5 4 0 3.74 1.82 6 4 0 11.96 2.11 7 4 0 1.03 2.74 8 4 0 4.94 3.31 9 4 0 2.11 3.58 10 4 0 0.12 3.87 11 4 0 1.52 4.89 12 4 0 2.89 5.28 -7 5 0 1.03 3.35 -6 5 0 120.63 6.95 -5 5 0 255.64 8.80 -4 5 0 2.68 3.69 -3 5 0 105.79 5.83 -2 5 0 364.10 9.69 -1 5 0 364.32 9.72 0 5 0 0.00 2.63 1 5 0 337.93 8.89 2 5 0 369.85 6.26 3 5 0 118.33 3.84 4 5 0 3.43 1.97 5 5 0 264.95 7.28 6 5 0 126.71 4.47 7 5 0 1.00 2.94 8 5 0 45.91 5.58 9 5 0 10.58 4.48 10 5 0 2.60 4.45 11 5 0 -2.06 4.98 -7 6 0 8.44 3.92 -6 6 0 3.43 3.84 -5 6 0 19.55 4.25 -4 6 0 18.65 4.07 -3 6 0 30.68 4.10 -2 6 0 7.22 3.09 -1 6 0 49.42 4.61 0 6 0 104.74 5.99 1 6 0 56.69 4.76 2 6 0 5.80 2.00 3 6 0 32.60 2.73 4 6 0 20.36 2.69 5 6 0 21.83 2.62 6 6 0 3.44 2.27 7 6 0 5.57 3.77 8 6 0 7.52 3.65 9 6 0 0.54 3.59 10 6 0 0.20 4.55 11 6 0 0.40 5.66 -7 7 0 7.42 4.51 -6 7 0 23.42 4.69 -5 7 0 10.42 4.04 -4 7 0 0.99 3.53 -3 7 0 -0.47 3.53 -2 7 0 7.15 3.27 -1 7 0 13.95 3.53 0 7 0 -1.74 2.60 1 7 0 15.47 3.74 2 7 0 7.08 2.27 3 7 0 0.26 1.98 4 7 0 -0.36 2.22 5 7 0 11.52 2.58 6 7 0 18.30 2.83 7 7 0 6.42 3.81 8 7 0 7.06 4.16 9 7 0 1.23 4.61 10 7 0 -2.91 4.78 -7 8 0 8.62 4.35 -6 8 0 20.16 4.43 -5 8 0 1.15 3.22 -4 8 0 42.22 5.16 -3 8 0 138.73 8.10 -2 8 0 20.97 4.29 -1 8 0 45.48 5.15 0 8 0 148.82 7.94 1 8 0 48.23 5.09 2 8 0 20.39 2.87 3 8 0 139.80 5.21 4 8 0 44.35 3.70 5 8 0 -0.31 2.33 6 8 0 20.95 3.15 7 8 0 6.27 4.14 8 8 0 1.65 3.68 9 8 0 1.29 4.41 10 8 0 3.08 5.18 -7 9 0 0.79 4.41 -6 9 0 5.22 4.45 -5 9 0 2.75 4.20 -4 9 0 2.51 3.56 -3 9 0 9.30 4.38 -2 9 0 10.01 4.06 -1 9 0 -0.20 3.93 0 9 0 -1.30 3.25 1 9 0 -0.36 3.87 2 9 0 8.36 3.96 3 9 0 17.05 4.80 4 9 0 0.41 3.44 5 9 0 3.90 4.28 -7 10 0 10.44 5.58 -6 10 0 12.24 5.61 -5 10 0 0.45 4.89 -4 10 0 13.89 4.83 -3 10 0 36.30 6.14 -2 10 0 5.38 5.11 -1 10 0 24.92 5.23 0 10 0 69.16 6.75 1 10 0 22.35 4.97 2 10 0 8.84 4.96 3 10 0 34.41 6.03 4 10 0 14.75 4.72 5 10 0 -3.72 4.49 -3 11 0 3.07 5.68 -2 11 0 4.54 4.94 -1 11 0 -1.98 5.35 0 11 0 -2.11 5.03 1 11 0 0.76 4.30 2 11 0 10.66 4.86 3 11 0 2.02 5.06 4 11 0 2.32 5.38 5 11 0 9.00 5.61 5 -8 1 -1.33 4.09 6 -8 1 -0.98 4.20 4 -7 1 25.09 4.84 5 -7 1 0.85 3.89 6 -7 1 26.68 5.43 7 -7 1 25.97 5.47 3 -6 1 23.73 4.65 4 -6 1 83.08 4.09 5 -6 1 18.65 2.94 6 -6 1 20.36 3.14 7 -6 1 7.30 2.59 8 -6 1 0.31 3.62 9 -6 1 1.57 3.93 2 -5 1 22.51 3.92 3 -5 1 17.14 2.29 4 -5 1 2.85 2.06 5 -5 1 4.91 2.31 6 -5 1 6.73 2.31 7 -5 1 14.15 2.65 8 -5 1 0.13 2.45 9 -5 1 -1.72 3.63 10 -5 1 0.74 4.16 11 -5 1 0.46 4.29 12 -5 1 -2.09 4.03 1 -4 1 474.78 10.97 2 -4 1 159.85 3.97 3 -4 1 131.83 4.00 4 -4 1 504.85 7.91 5 -4 1 32.87 2.80 6 -4 1 47.46 3.41 7 -4 1 33.81 3.19 8 -4 1 6.33 2.44 9 -4 1 -0.94 3.38 10 -4 1 2.15 3.76 11 -4 1 0.97 4.17 12 -4 1 -2.26 4.21 1 -3 1 1.35 1.97 2 -3 1 1.84 1.19 3 -3 1 91.84 3.06 4 -3 1 83.58 3.21 5 -3 1 19.83 2.26 6 -3 1 4.87 2.09 7 -3 1 0.28 2.08 8 -3 1 5.70 2.12 9 -3 1 -2.45 3.42 10 -3 1 -2.14 3.77 11 -3 1 -1.55 4.25 12 -3 1 -0.74 4.43 0 -2 1 18.92 2.29 1 -2 1 2424.12 14.01 2 -2 1 1127.82 8.92 3 -2 1 257.73 4.49 4 -2 1 487.26 6.82 5 -2 1 25.35 2.25 6 -2 1 19.06 2.32 7 -2 1 20.82 2.56 8 -2 1 7.81 2.21 9 -2 1 -1.36 3.68 10 -2 1 2.99 3.79 11 -2 1 0.70 4.64 12 -2 1 1.83 4.28 0 -1 1 274.50 4.46 1 -1 1 71.09 1.50 2 -1 1 397.36 4.48 3 -1 1 13.94 1.30 4 -1 1 83.79 2.81 5 -1 1 12.69 2.37 6 -1 1 20.74 3.35 7 -1 1 9.98 2.32 8 -1 1 7.56 2.42 9 -1 1 3.60 1.82 10 -1 1 13.85 4.34 11 -1 1 3.95 4.08 12 -1 1 0.46 4.15 1 0 1 0.74 0.62 2 0 1 0.34 0.94 4 0 1 0.93 1.75 5 0 1 0.77 2.26 6 0 1 -0.08 2.16 7 0 1 -1.97 2.27 8 0 1 2.35 3.06 9 0 1 -0.04 3.15 10 0 1 -0.89 3.55 11 0 1 -0.50 3.73 12 0 1 -1.15 5.05 -6 1 1 21.57 2.50 -5 1 1 4.02 1.79 -4 1 1 10.45 1.87 -3 1 1 27.39 2.14 -1 1 1 383.71 5.37 0 1 1 258.54 3.97 1 1 1 74.26 1.46 2 1 1 388.71 3.75 3 1 1 16.67 1.09 4 1 1 84.01 2.03 5 1 1 12.70 1.31 6 1 1 19.04 3.09 7 1 1 11.39 3.06 8 1 1 10.04 3.76 9 1 1 4.75 4.02 10 1 1 17.96 4.65 11 1 1 9.86 4.80 12 1 1 -1.67 4.16 -7 2 1 18.38 2.98 -6 2 1 282.16 7.35 -5 2 1 12.51 2.47 -4 2 1 29.99 2.56 -3 2 1 438.75 8.12 -2 2 1 708.77 9.77 -1 2 1 491.03 7.67 0 2 1 19.13 1.79 1 2 1 2422.34 19.32 2 2 1 1139.03 8.45 3 2 1 260.73 3.87 4 2 1 512.20 5.84 5 2 1 23.52 1.77 6 2 1 21.47 3.69 7 2 1 20.02 3.66 8 2 1 14.08 3.75 9 2 1 1.84 3.48 10 2 1 5.26 3.85 11 2 1 -0.07 4.06 12 2 1 2.60 4.60 -7 3 1 2.26 2.75 -6 3 1 2.14 2.43 -5 3 1 0.43 1.50 -4 3 1 353.67 8.48 -3 3 1 16.17 2.64 -2 3 1 43.26 3.28 -1 3 1 674.72 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9 1 -3.46 3.86 5 9 1 2.49 4.35 6 9 1 14.38 4.64 7 9 1 4.47 4.81 8 9 1 3.89 5.09 -7 10 1 4.66 5.49 -6 10 1 0.93 5.09 -5 10 1 0.12 4.91 -4 10 1 5.57 5.13 -3 10 1 13.90 5.09 -2 10 1 13.94 5.33 -1 10 1 1.67 4.46 0 10 1 23.43 5.40 1 10 1 51.77 6.50 2 10 1 3.56 4.11 3 10 1 5.04 4.17 4 10 1 10.75 4.49 5 10 1 10.22 5.15 -3 11 1 0.42 5.09 -2 11 1 3.01 5.25 -1 11 1 0.40 4.27 0 11 1 3.27 4.61 1 11 1 -2.27 4.56 2 11 1 4.17 4.98 3 11 1 -1.53 4.90 4 11 1 2.31 5.10 5 11 1 -2.27 5.28 5 -8 2 65.66 7.38 6 -8 2 3.14 3.98 7 -8 2 10.24 4.40 3 -7 2 43.36 6.08 4 -7 2 0.46 3.82 5 -7 2 3.93 3.94 6 -7 2 2.03 4.04 7 -7 2 6.40 4.26 2 -6 2 69.03 6.17 3 -6 2 46.93 5.53 4 -6 2 75.53 3.94 5 -6 2 161.74 5.66 6 -6 2 44.83 3.65 7 -6 2 4.24 2.53 8 -6 2 11.68 4.43 1 -5 2 35.03 4.81 2 -5 2 84.64 5.92 3 -5 2 259.50 5.81 4 -5 2 3.26 2.07 5 -5 2 2.29 2.04 6 -5 2 1.64 2.20 7 -5 2 20.35 2.96 8 -5 2 1.55 2.37 9 -5 2 4.36 3.89 10 -5 2 5.19 4.20 11 -5 2 3.83 4.48 1 -4 2 6.45 2.75 2 -4 2 44.18 2.26 3 -4 2 29.74 2.30 4 -4 2 160.20 4.59 5 -4 2 27.51 2.70 6 -4 2 11.61 2.35 7 -4 2 5.38 2.15 8 -4 2 5.09 2.17 9 -4 2 -2.37 3.50 10 -4 2 -1.72 3.66 12 -4 2 2.40 4.36 0 -3 2 540.16 10.21 1 -3 2 120.72 5.09 2 -3 2 733.96 7.60 3 -3 2 129.89 3.53 4 -3 2 43.78 2.59 5 -3 2 2.69 1.66 6 -3 2 89.40 3.96 7 -3 2 67.37 5.33 8 -3 2 44.91 4.82 9 -3 2 2.46 2.44 10 -3 2 24.81 4.87 11 -3 2 -0.29 4.21 12 -3 2 -0.49 4.53 0 -2 2 124.19 4.15 1 -2 2 2043.72 12.52 2 -2 2 1648.64 11.42 3 -2 2 9.24 1.37 4 -2 2 211.32 4.57 5 -2 2 249.96 5.45 6 -2 2 55.69 3.28 7 -2 2 76.72 3.97 8 -2 2 70.73 4.23 9 -2 2 39.61 3.74 10 -2 2 3.95 4.51 11 -2 2 9.17 4.55 12 -2 2 2.11 4.39 0 -1 2 75.89 2.45 1 -1 2 68.59 1.45 2 -1 2 225.61 4.91 3 -1 2 190.66 3.71 4 -1 2 217.36 5.95 5 -1 2 -0.65 1.85 6 -1 2 -0.57 2.15 7 -1 2 71.59 5.25 8 -1 2 32.56 3.45 9 -1 2 23.40 3.17 10 -1 2 2.63 3.66 11 -1 2 16.28 5.53 12 -1 2 1.11 4.11 1 0 2 208.94 3.45 2 0 2 2870.93 21.47 3 0 2 78.97 3.20 4 0 2 1300.50 15.24 5 0 2 1144.18 16.10 6 0 2 1.74 2.71 7 0 2 32.15 3.70 8 0 2 306.42 10.55 9 0 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2 63.17 5.03 8 3 2 48.04 5.29 9 3 2 2.69 3.42 10 3 2 24.84 5.63 11 3 2 2.88 4.41 12 3 2 -0.86 5.46 -7 4 2 4.11 2.72 -6 4 2 1.07 3.06 -5 4 2 1.46 2.74 -4 4 2 54.86 4.28 -3 4 2 2.47 2.72 -2 4 2 1.39 2.25 -1 4 2 56.45 4.09 0 4 2 19.40 2.91 1 4 2 4.13 2.05 2 4 2 44.41 2.51 3 4 2 25.10 2.06 4 4 2 163.35 4.25 5 4 2 25.86 2.36 6 4 2 13.95 3.31 7 4 2 6.80 3.20 8 4 2 3.50 3.31 9 4 2 1.20 3.61 10 4 2 0.14 4.43 11 4 2 -0.50 4.82 -7 5 2 68.15 5.40 -6 5 2 31.81 4.03 -5 5 2 106.61 6.33 -4 5 2 288.07 9.69 -3 5 2 136.27 6.71 -2 5 2 4.69 2.77 -1 5 2 178.71 7.05 0 5 2 254.62 7.97 1 5 2 28.54 3.48 2 5 2 88.73 3.44 3 5 2 260.05 5.58 4 5 2 4.27 2.02 5 5 2 3.14 1.93 6 5 2 3.95 3.24 7 5 2 18.58 3.68 8 5 2 3.86 3.30 9 5 2 2.58 4.20 10 5 2 3.53 4.30 11 5 2 -0.24 5.41 -7 6 2 2.58 3.28 -6 6 2 17.19 3.89 -5 6 2 15.83 3.77 -4 6 2 6.90 2.98 -3 6 2 56.40 5.24 -2 6 2 133.09 6.81 -1 6 2 35.88 4.17 0 6 2 8.00 3.77 1 6 2 89.16 5.54 2 6 2 66.19 3.38 3 6 2 45.92 3.09 4 6 2 74.81 3.70 5 6 2 164.52 5.18 6 6 2 46.19 4.83 7 6 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5.28 5.03 -3 10 2 9.71 4.65 -2 10 2 28.79 5.66 -1 10 2 15.54 4.61 0 10 2 1.26 3.89 1 10 2 12.43 4.63 2 10 2 14.91 5.10 3 10 2 -0.92 3.94 5 10 2 14.07 5.14 -3 11 2 8.37 6.21 -2 11 2 5.95 5.89 -1 11 2 29.33 5.80 0 11 2 14.74 5.07 1 11 2 -2.19 4.59 2 11 2 5.02 5.02 3 11 2 16.51 5.65 4 11 2 9.70 5.28 6 -9 3 -0.96 4.68 7 -9 3 0.78 4.92 4 -8 3 -2.38 3.35 5 -8 3 -0.16 4.31 6 -8 3 1.91 4.08 7 -8 3 2.23 4.36 3 -7 3 35.98 5.67 4 -7 3 18.39 4.47 5 -7 3 -2.76 3.00 6 -7 3 4.08 3.71 7 -7 3 -0.49 3.40 8 -7 3 0.65 4.00 2 -6 3 41.00 5.00 3 -6 3 68.51 6.26 4 -6 3 8.12 3.60 5 -6 3 64.74 6.17 6 -6 3 44.44 5.59 7 -6 3 1.72 3.28 8 -6 3 5.27 3.99 1 -5 3 89.30 6.09 2 -5 3 8.62 3.41 3 -5 3 92.67 3.60 4 -5 3 12.43 2.33 5 -5 3 0.28 1.94 6 -5 3 3.89 2.18 7 -5 3 0.68 2.34 8 -5 3 3.09 2.51 9 -5 3 0.33 3.71 10 -5 3 -1.18 3.68 0 -4 3 80.72 4.97 1 -4 3 78.60 5.21 2 -4 3 305.69 5.16 3 -4 3 259.43 5.26 4 -4 3 37.05 2.66 5 -4 3 28.57 2.61 6 -4 3 222.88 8.11 7 -4 3 36.23 4.15 8 -4 3 15.29 2.77 9 -4 3 9.99 2.80 10 -4 3 5.85 4.12 11 -4 3 1.65 4.38 12 -4 3 1.91 4.31 0 -3 3 19.31 2.60 1 -3 3 1.08 2.30 2 -3 3 300.03 6.43 3 -3 3 11.49 1.56 4 -3 3 1.04 1.63 5 -3 3 20.08 2.28 6 -3 3 5.08 2.07 7 -3 3 8.54 2.31 8 -3 3 27.30 3.21 9 -3 3 3.39 2.39 10 -3 3 -0.08 3.98 11 -3 3 1.80 4.48 12 -3 3 1.33 4.48 -1 -2 3 3222.56 26.23 0 -2 3 345.82 6.96 1 -2 3 70.34 1.75 2 -2 3 203.58 3.56 3 -2 3 2.00 1.14 4 -2 3 0.59 1.37 5 -2 3 11.39 1.93 6 -2 3 23.97 2.56 7 -2 3 1.84 2.26 8 -2 3 7.35 2.57 9 -2 3 12.01 2.90 10 -2 3 0.17 4.20 11 -2 3 -1.13 3.83 12 -2 3 -2.12 4.10 -1 -1 3 20.09 1.64 0 -1 3 1442.38 13.71 1 -1 3 92.06 1.72 2 -1 3 377.85 4.57 3 -1 3 31.68 1.82 4 -1 3 25.44 2.39 5 -1 3 251.09 7.31 6 -1 3 35.70 3.88 7 -1 3 4.55 2.67 8 -1 3 46.19 3.60 9 -1 3 35.16 3.52 10 -1 3 11.02 3.18 11 -1 3 7.49 4.31 12 -1 3 5.81 4.49 1 0 3 0.06 0.83 2 0 3 0.47 1.26 3 0 3 0.95 1.60 4 0 3 0.69 1.60 5 0 3 1.28 2.37 6 0 3 -0.57 2.36 7 0 3 0.00 2.74 8 0 3 3.19 3.35 9 0 3 1.38 3.26 10 0 3 0.57 4.05 11 0 3 -0.14 3.91 12 0 3 2.30 4.89 -7 1 3 88.21 4.90 0 1 3 1479.14 13.47 1 1 3 100.84 2.71 2 1 3 402.45 4.07 3 1 3 30.33 1.15 4 1 3 25.90 2.56 5 1 3 252.09 7.29 6 1 3 36.74 3.95 7 1 3 3.17 2.94 8 1 3 50.48 5.14 9 1 3 30.13 5.13 10 1 3 9.69 4.06 11 1 3 4.36 4.00 12 1 3 9.50 5.37 -7 2 3 22.22 3.40 -6 2 3 5.58 2.44 -5 2 3 6.01 1.89 -4 2 3 309.59 7.68 -3 2 3 13.19 2.34 -2 2 3 19.74 2.32 -1 2 3 3162.25 25.70 0 2 3 357.53 6.68 1 2 3 78.47 3.14 2 2 3 203.56 3.49 3 2 3 2.85 1.13 4 2 3 0.89 1.95 5 2 3 10.07 1.47 6 2 3 24.58 3.37 7 2 3 1.84 2.63 8 2 3 9.86 3.65 9 2 3 10.45 4.01 10 2 3 0.38 3.56 11 2 3 2.62 4.63 12 2 3 0.66 4.96 -7 3 3 11.24 3.14 -6 3 3 22.06 3.17 -5 3 3 0.69 2.33 -4 3 3 8.55 2.73 -3 3 3 7.18 2.55 -2 3 3 3.18 2.09 -1 3 3 121.36 4.78 0 3 3 17.71 2.44 1 3 3 -0.90 1.41 2 3 3 287.00 4.69 3 3 3 11.39 1.59 4 3 3 0.56 1.45 5 3 3 19.02 1.92 6 3 3 3.49 2.49 7 3 3 8.29 3.03 8 3 3 26.15 4.58 9 3 3 0.77 3.87 10 3 3 1.40 3.98 11 3 3 5.93 4.57 12 3 3 -4.86 5.26 -7 4 3 1.53 3.04 -6 4 3 4.18 3.11 -5 4 3 79.13 5.45 -4 4 3 70.82 4.88 -3 4 3 95.90 5.31 -2 4 3 472.30 10.70 -1 4 3 564.68 11.34 0 4 3 87.40 4.59 1 4 3 70.02 4.30 2 4 3 305.97 7.65 3 4 3 255.19 5.03 4 4 3 33.42 2.39 5 4 3 27.13 2.34 6 4 3 229.64 8.33 7 4 3 37.10 4.40 8 4 3 13.75 3.83 9 4 3 14.83 4.27 10 4 3 5.19 4.08 11 4 3 2.07 4.71 -7 5 3 6.76 3.17 -6 5 3 1.12 2.92 -5 5 3 0.19 2.75 -4 5 3 21.84 3.74 -3 5 3 25.94 3.80 -2 5 3 18.64 3.44 -1 5 3 50.24 4.44 0 5 3 5.29 3.46 1 5 3 83.79 4.89 2 5 3 7.20 2.60 3 5 3 91.95 3.71 4 5 3 10.36 2.22 5 5 3 -0.37 1.82 6 5 3 0.95 2.82 7 5 3 2.18 3.79 8 5 3 1.91 4.01 9 5 3 4.68 3.80 10 5 3 0.24 3.98 11 5 3 2.56 5.38 -7 6 3 8.17 3.60 -6 6 3 -0.09 2.58 -5 6 3 9.63 3.21 -4 6 3 49.38 5.09 -3 6 3 13.76 3.84 -2 6 3 29.60 4.26 -1 6 3 132.79 7.01 0 6 3 38.92 4.26 1 6 3 32.54 4.06 2 6 3 40.38 4.38 3 6 3 63.18 3.39 4 6 3 11.07 2.39 5 6 3 66.39 3.84 6 6 3 48.38 5.18 7 6 3 1.76 3.23 8 6 3 8.39 4.19 9 6 3 7.30 4.13 10 6 3 2.34 4.33 -7 7 3 13.99 5.77 -6 7 3 9.63 4.66 -5 7 3 0.46 3.96 -4 7 3 59.66 6.40 -3 7 3 51.70 5.49 -2 7 3 1.18 3.46 -1 7 3 39.88 4.98 0 7 3 42.95 4.85 1 7 3 20.16 4.18 2 7 3 0.90 2.67 3 7 3 25.94 2.88 4 7 3 20.18 2.64 5 7 3 1.47 2.22 6 7 3 2.61 3.55 7 7 3 2.66 3.96 8 7 3 1.95 4.11 9 7 3 2.93 4.59 10 7 3 -1.62 4.54 -7 8 3 4.60 5.17 -6 8 3 -0.04 4.07 -5 8 3 5.22 4.81 -4 8 3 5.91 4.68 -3 8 3 11.48 4.15 -2 8 3 6.41 4.53 -1 8 3 4.28 3.89 0 8 3 0.92 3.53 1 8 3 1.01 3.23 2 8 3 2.69 2.52 3 8 3 7.42 2.54 4 8 3 -0.61 2.56 5 8 3 -0.02 2.54 6 8 3 3.65 3.54 7 8 3 5.31 4.33 8 8 3 0.68 3.93 9 8 3 0.40 5.15 -7 9 3 12.38 5.35 -6 9 3 7.12 4.66 -5 9 3 0.11 3.78 -4 9 3 23.58 5.11 -3 9 3 27.31 5.68 -2 9 3 0.15 3.85 -1 9 3 13.57 4.26 0 9 3 40.34 5.74 1 9 3 14.95 4.14 2 9 3 0.62 2.63 3 9 3 13.85 3.09 4 9 3 16.08 3.28 5 9 3 6.24 3.12 6 9 3 -1.73 4.02 7 9 3 2.20 4.66 8 9 3 -0.98 4.70 -7 10 3 -1.29 5.12 -6 10 3 1.98 4.61 -5 10 3 3.08 5.20 -4 10 3 8.16 4.71 -3 10 3 1.11 4.92 -2 10 3 14.25 5.56 -1 10 3 12.78 5.06 0 10 3 4.16 4.48 1 10 3 1.95 4.55 2 10 3 20.81 5.32 3 10 3 12.58 5.02 4 10 3 -1.32 4.43 -3 11 3 3.47 6.00 -2 11 3 3.99 5.11 -1 11 3 5.14 5.29 0 11 3 2.09 4.88 1 11 3 -1.63 4.53 2 11 3 1.91 4.85 3 11 3 3.77 5.41 4 11 3 -0.61 4.90 5 -9 4 2.22 4.11 6 -9 4 4.37 4.98 7 -9 4 -2.10 4.03 3 -8 4 99.29 8.76 4 -8 4 26.25 5.63 5 -8 4 8.41 4.48 6 -8 4 35.86 6.15 7 -8 4 21.54 5.07 8 -8 4 0.17 4.38 2 -7 4 -3.23 4.02 3 -7 4 3.73 3.70 4 -7 4 10.07 4.38 5 -7 4 3.01 3.50 6 -7 4 0.83 3.34 7 -7 4 -1.45 3.12 8 -7 4 2.12 3.48 1 -6 4 14.35 4.06 2 -6 4 36.40 4.88 3 -6 4 159.45 8.79 4 -6 4 43.75 5.16 5 -6 4 11.07 3.67 6 -6 4 16.74 4.09 7 -6 4 36.33 5.58 8 -6 4 3.01 3.85 9 -6 4 2.48 3.95 0 -5 4 700.02 15.49 1 -5 4 172.25 8.06 2 -5 4 12.06 3.63 3 -5 4 70.18 3.19 4 -5 4 212.31 5.48 5 -5 4 8.36 2.25 6 -5 4 13.09 2.49 7 -5 4 35.11 3.29 8 -5 4 17.69 3.05 9 -5 4 1.51 3.62 0 -4 4 30.51 3.63 1 -4 4 2.74 2.71 2 -4 4 3.10 1.41 3 -4 4 85.31 3.21 4 -4 4 17.66 2.23 5 -4 4 0.98 1.75 6 -4 4 1.38 1.86 7 -4 4 3.63 2.17 8 -4 4 -1.89 2.04 9 -4 4 -1.11 2.19 10 -4 4 2.44 4.05 11 -4 4 2.05 4.21 12 -4 4 4.35 4.85 -1 -3 4 166.02 5.91 0 -3 4 366.24 8.84 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19 -0.72 4.93 6 -3 19 1.40 5.18 0 -2 19 2.65 3.52 1 -2 19 -0.51 3.87 2 -2 19 10.39 4.63 3 -2 19 -0.40 3.61 4 -2 19 2.13 4.66 5 -2 19 4.67 4.74 6 -2 19 4.02 5.09 7 -2 19 -0.14 5.44 0 -1 19 -1.75 3.25 1 -1 19 42.72 5.62 2 -1 19 23.00 5.12 3 -1 19 -1.16 3.39 4 -1 19 2.91 3.94 5 -1 19 14.01 5.05 6 -1 19 5.90 5.46 7 -1 19 -1.26 4.47 0 0 19 -0.64 2.96 1 0 19 1.64 3.42 2 0 19 -1.16 3.49 3 0 19 1.09 3.94 4 0 19 1.30 3.73 5 0 19 0.26 4.37 6 0 19 -1.79 4.61 7 0 19 3.85 4.49 1 1 19 38.97 5.04 2 1 19 17.00 4.27 7 1 19 3.13 4.09 2 2 19 8.81 3.64 3 2 19 -0.45 3.32 4 2 19 0.42 3.36 5 2 19 0.06 3.59 -9 3 19 2.81 6.72 -8 3 19 -1.89 5.35 -7 3 19 9.73 5.84 -1 3 19 3.44 3.87 0 3 19 7.56 3.92 1 3 19 0.99 3.88 2 3 19 2.48 3.20 3 3 19 1.47 3.63 4 3 19 1.13 3.06 5 3 19 0.06 3.69 6 3 19 0.22 3.82 7 3 19 -0.22 3.87 8 3 19 -1.93 4.68 -8 4 19 -2.39 5.87 -7 4 19 0.56 4.69 -6 4 19 0.54 4.84 -5 4 19 1.93 4.87 -4 4 19 2.37 4.65 -3 4 19 5.75 4.18 -2 4 19 1.29 4.35 -1 4 19 8.27 4.12 0 4 19 11.50 4.67 1 4 19 -0.69 3.73 3 4 19 2.57 3.77 4 4 19 3.78 3.48 5 4 19 0.75 3.94 6 4 19 1.83 3.57 7 4 19 -0.25 4.21 -7 5 19 0.45 6.04 -6 5 19 -1.30 5.07 -5 5 19 -0.79 4.47 -4 5 19 2.96 4.21 -3 5 19 3.61 4.39 -2 5 19 0.40 4.26 -1 5 19 2.25 4.12 0 5 19 -1.69 3.82 1 5 19 3.39 4.20 3 5 19 1.01 3.47 4 5 19 0.81 3.53 5 5 19 2.82 3.77 6 5 19 2.13 4.85 -6 6 19 1.88 6.21 -5 6 19 -1.70 4.84 -4 6 19 2.59 4.68 -3 6 19 0.92 3.89 -2 6 19 3.18 4.17 -1 6 19 0.08 3.96 0 6 19 2.44 4.40 3 6 19 -3.75 4.02 4 6 19 1.34 4.32 -4 7 19 0.66 5.17 -3 7 19 2.85 4.43 -2 7 19 2.82 4.50 -1 7 19 6.53 5.02 0 7 19 -2.51 4.32 -1 8 19 -1.72 4.53 0 8 19 1.90 5.11 -1 -8 20 -1.78 6.35 -1 -7 20 -0.80 5.18 0 -7 20 0.36 4.56 1 -7 20 -0.60 5.61 2 -7 20 1.16 5.50 -1 -6 20 -6.49 4.23 0 -6 20 -0.12 4.50 1 -6 20 1.27 4.47 2 -6 20 1.14 4.26 3 -6 20 0.62 4.55 0 -5 20 -3.76 4.13 1 -5 20 11.78 5.28 2 -5 20 6.26 4.69 3 -5 20 -0.46 4.46 4 -5 20 2.38 5.19 0 -4 20 0.49 3.85 1 -4 20 -1.21 4.12 2 -4 20 1.39 4.52 3 -4 20 -1.33 4.67 4 -4 20 1.92 5.12 5 -4 20 2.45 4.54 0 -3 20 -1.07 3.89 1 -3 20 2.36 4.23 2 -3 20 17.70 5.15 3 -3 20 1.86 4.63 4 -3 20 7.51 4.77 5 -3 20 9.42 5.00 6 -3 20 4.00 5.46 0 -2 20 0.12 3.80 1 -2 20 4.97 4.08 2 -2 20 1.73 3.88 3 -2 20 5.06 4.56 4 -2 20 -1.32 3.99 5 -2 20 -1.69 4.69 6 -2 20 0.75 4.93 1 -1 20 2.37 3.96 2 -1 20 1.77 4.18 3 -1 20 3.75 3.71 4 -1 20 2.62 4.07 5 -1 20 -0.16 4.16 6 -1 20 2.36 5.13 7 -1 20 3.90 5.26 1 0 20 1.47 3.49 2 0 20 4.45 4.00 3 0 20 14.01 4.92 4 0 20 0.84 4.41 5 0 20 1.37 4.64 6 0 20 7.58 5.11 7 0 20 4.46 4.75 1 1 20 3.74 3.53 2 1 20 3.32 3.79 3 1 20 2.99 4.16 4 1 20 -3.79 3.93 5 1 20 2.14 4.59 6 1 20 -0.54 3.75 7 1 20 -1.22 4.27 -8 3 20 3.33 6.01 -7 3 20 0.21 5.22 -1 3 20 0.04 4.26 0 3 20 0.15 4.23 1 3 20 2.05 4.20 2 3 20 13.06 4.21 3 3 20 0.49 3.18 4 3 20 4.13 3.27 5 3 20 4.99 3.98 6 3 20 4.22 4.09 -7 4 20 -1.10 4.97 -6 4 20 0.44 4.92 -5 4 20 -1.53 4.69 -4 4 20 -4.18 4.19 -3 4 20 -3.69 3.86 -2 4 20 -2.71 4.14 -1 4 20 0.02 3.56 0 4 20 3.40 4.29 4 4 20 1.14 3.48 5 4 20 2.29 3.64 6 4 20 -0.95 3.99 -6 5 20 4.99 6.23 -5 5 20 2.23 4.77 -4 5 20 3.74 5.22 -3 5 20 5.45 4.89 -2 5 20 2.93 4.76 -1 5 20 1.95 3.82 0 5 20 -1.56 4.07 3 5 20 0.04 3.58 4 5 20 1.74 3.53 5 5 20 8.05 4.59 -5 6 20 -1.28 4.81 -4 6 20 0.81 4.76 -3 6 20 -2.19 4.19 -2 6 20 1.30 4.80 -1 6 20 -0.06 4.43 0 6 20 3.75 4.71 3 6 20 -0.29 4.36 -3 7 20 4.21 5.44 -2 7 20 3.10 5.31 -1 7 20 2.19 4.58 0 7 20 -2.25 4.38 0 -7 21 -2.86 4.37 0 -6 21 -5.34 4.81 1 -6 21 1.20 4.98 2 -6 21 2.05 5.43 1 -5 21 1.64 4.91 2 -5 21 10.94 5.87 3 -5 21 0.39 4.82 4 -5 21 -0.67 5.53 0 -4 21 3.24 4.55 1 -4 21 2.11 4.48 3 -4 21 5.70 5.34 4 -4 21 0.48 5.14 5 -4 21 -1.14 4.64 1 -3 21 -1.18 4.22 2 -3 21 -2.27 4.14 3 -3 21 0.29 4.11 4 -3 21 -0.54 4.44 5 -3 21 2.45 4.45 1 -2 21 2.78 4.32 2 -2 21 2.39 4.33 3 -2 21 1.97 4.03 4 -2 21 2.14 4.67 5 -2 21 1.20 4.27 6 -2 21 4.27 4.92 1 -1 21 -0.44 3.73 2 -1 21 6.10 4.41 3 -1 21 10.90 4.66 4 -1 21 0.05 3.92 5 -1 21 0.99 4.09 6 -1 21 5.62 5.26 1 0 21 -0.62 3.69 2 0 21 0.64 3.91 3 0 21 0.43 4.20 4 0 21 0.95 4.65 5 0 21 4.33 4.60 6 0 21 -2.01 4.07 2 1 21 4.03 4.17 3 1 21 9.34 4.73 4 1 21 2.98 4.51 5 1 21 1.54 4.05 6 1 21 9.08 5.33 -7 3 21 5.36 6.56 -2 3 21 -1.59 3.97 -1 3 21 2.19 3.96 0 3 21 -1.27 4.18 2 3 21 1.31 3.64 3 3 21 -0.62 3.56 4 3 21 -3.35 3.38 -7 4 21 -3.46 5.43 -6 4 21 -0.18 5.14 -5 4 21 -0.09 4.93 -4 4 21 1.44 5.30 -3 4 21 3.54 4.79 -2 4 21 3.93 4.18 -1 4 21 1.09 3.93 0 4 21 2.41 4.39 2 4 21 3.77 4.06 3 4 21 1.97 4.01 4 4 21 1.98 3.58 5 4 21 0.11 3.47 6 4 21 -0.29 4.45 -5 5 21 -1.65 4.75 -4 5 21 -1.90 4.69 -3 5 21 -0.57 4.58 -2 5 21 -2.10 4.41 -1 5 21 1.50 4.20 0 5 21 0.52 4.21 2 5 21 4.61 4.30 3 5 21 -0.32 4.20 4 5 21 1.05 4.26 -4 6 21 -1.23 4.51 -3 6 21 4.39 4.99 -2 6 21 -1.26 4.58 -1 6 21 -1.40 3.95 0 6 21 0.32 4.79 2 6 21 3.58 4.87 -2 7 21 0.85 5.49 -1 7 21 -2.62 5.10 0 7 21 0.97 4.33 1 -6 22 -0.28 4.98 1 -5 22 -5.92 4.54 2 -5 22 -1.67 5.14 3 -5 22 0.74 5.15 1 -4 22 3.03 4.59 2 -4 22 1.13 5.00 3 -4 22 1.19 4.93 4 -4 22 -0.01 5.19 1 -3 22 -0.94 4.25 2 -3 22 3.04 4.26 3 -3 22 7.10 5.16 4 -3 22 0.07 4.97 1 -2 22 4.54 4.30 2 -2 22 0.15 4.27 3 -2 22 0.56 4.57 4 -2 22 3.17 4.96 5 -2 22 5.49 5.23 2 -1 22 2.77 4.32 4 -1 22 -0.88 4.12 5 -1 22 -0.14 4.42 2 0 22 5.19 4.26 3 0 22 -0.31 4.31 4 0 22 0.05 4.04 5 0 22 1.75 4.78 2 1 22 2.15 3.97 3 1 22 0.73 4.20 4 1 22 -0.56 4.01 5 1 22 0.85 4.55 -2 3 22 5.05 5.00 -1 3 22 3.27 4.76 0 3 22 3.48 4.48 -6 4 22 -4.22 4.91 -5 4 22 0.35 5.35 -4 4 22 -1.56 4.12 -3 4 22 1.30 4.69 -2 4 22 1.47 4.13 -1 4 22 186.97 11.89 0 4 22 9.63 5.02 2 4 22 0.53 3.49 3 4 22 -3.07 3.84 4 4 22 0.35 3.82 5 4 22 4.09 3.99 -4 5 22 0.43 4.83 -3 5 22 0.52 5.07 -2 5 22 1.97 4.78 -1 5 22 3.54 4.52 0 5 22 0.26 4.23 2 5 22 -1.22 3.53 3 5 22 -0.89 4.26 -2 6 22 1.95 4.42 -1 6 22 1.17 4.66 1 -5 23 8.39 5.35 2 -5 23 -0.49 4.73 2 -4 23 0.29 4.75 3 -4 23 6.79 5.58 2 -3 23 0.88 4.83 3 -3 23 -0.33 4.71 4 -3 23 -0.14 4.70 2 -2 23 3.08 4.40 3 -2 23 -1.49 4.86 4 -2 23 -4.33 4.16 2 -1 23 -1.28 4.10 3 -1 23 0.41 4.53 4 -1 23 0.43 4.82 5 -1 23 -1.11 4.72 3 0 23 -1.23 3.85 4 0 23 -1.07 4.58 5 0 23 -2.09 4.77 3 1 23 -1.85 3.62 4 1 23 3.22 4.49 5 1 23 2.37 5.18 3 2 23 -0.29 4.15 4 2 23 2.16 4.10 5 2 23 2.92 4.99 -3 3 23 -2.00 4.24 -2 3 23 -0.64 4.84 -1 3 23 -0.02 4.80 0 3 23 -0.52 4.36 -4 4 23 0.91 5.02 -3 4 23 0.70 4.33 -2 4 23 3.85 4.99 -1 4 23 0.72 4.80 2 4 23 5.82 4.30 -3 5 23 -1.23 5.30 -2 5 23 5.04 5.38 -1 5 23 -1.78 3.82 2 5 23 2.77 4.57 -1 6 23 -1.20 5.29 2 -4 24 0.57 4.84 3 -3 24 -2.94 4.45 3 -2 24 -0.38 4.51 4 -2 24 2.36 4.81 3 -1 24 1.11 4.50 4 -1 24 1.91 4.97 3 0 24 3.58 4.65 4 0 24 4.05 4.55 4 1 24 1.74 4.55 4 2 24 1.34 4.51 -4 3 24 2.28 5.52 -3 3 24 5.46 5.05 -2 3 24 9.90 5.49 -1 3 24 2.82 4.98 -3 4 24 -5.36 4.75 -2 4 24 -4.65 4.53 -1 4 24 -2.93 4.49 -2 5 24 0.82 5.60 -1 5 24 -5.17 4.41 3 -2 25 -2.00 5.22 -3 3 25 4.01 5.35 -2 3 25 11.92 6.11 -1 3 25 2.12 5.06 -2 4 25 -4.16 5.14 -1 4 25 0.05 5.12 -1 3 26 5.28 6.05 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 20689 _database_code_depnum_ccdc_archive 'CCDC 877556' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_a00919a _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H46 Br2 N6 Ni' _chemical_formula_weight 829.36 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 21/n' _space_group_name_Hall '-P 2yn' _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+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.573(3) _cell_length_b 15.870(6) _cell_length_c 14.351(5) _cell_angle_alpha 90 _cell_angle_beta 91.024(5) _cell_angle_gamma 90 _cell_volume 1952.2(12) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 797 _cell_measurement_theta_min 2.567 _cell_measurement_theta_max 24.317 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.411 _exptl_crystal_F_000 852 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.150 _exptl_crystal_size_mid 0.130 _exptl_crystal_size_min 0.120 _exptl_absorpt_coefficient_mu 2.579 _shelx_estimated_absorpt_T_min 0.698 _shelx_estimated_absorpt_T_max 0.747 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.673550 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source ? _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 8928 _diffrn_reflns_av_unetI/netI 0.0537 _diffrn_reflns_av_R_equivalents 0.0414 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.913 _diffrn_reflns_theta_max 26.299 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_point_group_measured_fraction_full 1.000 _reflns_number_total 3961 _reflns_number_gt 2598 _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 SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0334P)^2^] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 3961 _refine_ls_number_parameters 231 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0559 _refine_ls_R_factor_gt 0.0341 _refine_ls_wR_factor_ref 0.0715 _refine_ls_wR_factor_gt 0.0684 _refine_ls_goodness_of_fit_ref 0.857 _refine_ls_restrained_S_all 0.857 _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 0.0000 0.5000 0.5000 0.04228(13) Uani 1 2 d S . P . . Br1 Br 0.22276(3) 0.58104(2) 0.52617(2) 0.06203(12) Uani 1 1 d . . . . . C1 C 0.0665(3) 0.42799(14) 0.59956(16) 0.0412(6) Uani 1 1 d . . . . . C2 C 0.1001(3) 0.36536(17) 0.73894(18) 0.0561(7) Uani 1 1 d . . . . . H2 H 0.0865 0.3515 0.8012 0.067 Uiso 1 1 calc R U . . . C3 C 0.2051(3) 0.33287(17) 0.68217(18) 0.0551(7) Uani 1 1 d . . . . . H3 H 0.2791 0.2920 0.6973 0.066 Uiso 1 1 calc R U . . . C4 C 0.2780(3) 0.35429(17) 0.51353(17) 0.0517(7) Uani 1 1 d . . . . . H5A H 0.3788 0.3814 0.5213 0.062 Uiso 1 1 calc R U . . . H5B H 0.2263 0.3789 0.4594 0.062 Uiso 1 1 calc R U . . . C5 C 0.3020(3) 0.26205(17) 0.49675(17) 0.0478(6) Uani 1 1 d . . . . . C6 C 0.4505(3) 0.22828(18) 0.50374(18) 0.0548(7) Uani 1 1 d . . . . . H10 H 0.5337 0.2636 0.5191 0.066 Uiso 1 1 calc R U . . . C7 C 0.4791(4) 0.14384(19) 0.48861(19) 0.0629(8) Uani 1 1 d . . . . . H12 H 0.5799 0.1224 0.4930 0.076 Uiso 1 1 calc R U . . . C8 C 0.3554(4) 0.09222(19) 0.4669(2) 0.0676(8) Uani 1 1 d . . . . . H17 H 0.3727 0.0350 0.4573 0.081 Uiso 1 1 calc R U . . . C9 C 0.2072(4) 0.1235(2) 0.4593(2) 0.0667(8) Uani 1 1 d . . . . . H15 H 0.1252 0.0872 0.4447 0.080 Uiso 1 1 calc R U . . . C10 C 0.1768(3) 0.20880(18) 0.47292(18) 0.0538(7) Uani 1 1 d . . . . . C11 C -0.1039(4) 0.1898(2) 0.4359(3) 0.1063(13) Uani 1 1 d . . . . . H19A H -0.0813 0.1593 0.3800 0.159 Uiso 1 1 calc R U . . . H19B H -0.1923 0.2258 0.4249 0.159 Uiso 1 1 calc R U . . . H19C H -0.1270 0.1507 0.4848 0.159 Uiso 1 1 calc R U . . . C12 C -0.1157(3) 0.47258(15) 0.72110(16) 0.0435(6) Uani 1 1 d . . . . . C13 C -0.0914(3) 0.55488(16) 0.75033(17) 0.0492(7) Uani 1 1 d . . . . . C14 C -0.2214(3) 0.60224(17) 0.7736(2) 0.0628(8) Uani 1 1 d . . . . . H9 H -0.2073 0.6576 0.7933 0.075 Uiso 1 1 calc R U . . . C15 C -0.3702(4) 0.56984(19) 0.7684(2) 0.0671(8) Uani 1 1 d . . . . . C16 C -0.3882(3) 0.48632(19) 0.7439(2) 0.0625(8) Uani 1 1 d . . . . . H16 H -0.4879 0.4632 0.7424 0.075 Uiso 1 1 calc R U . . . C17 C -0.2629(3) 0.43593(16) 0.72148(17) 0.0505(7) Uani 1 1 d . . . . . C18 C 0.0688(3) 0.5920(2) 0.7599(2) 0.0748(9) Uani 1 1 d . . . . . H18A H 0.1381 0.5513 0.7879 0.112 Uiso 1 1 calc R U . . . H18B H 0.0651 0.6413 0.7985 0.112 Uiso 1 1 calc R U . . . H18C H 0.1060 0.6071 0.6994 0.112 Uiso 1 1 calc R U . . . C19 C -0.5117(4) 0.6242(2) 0.7897(3) 0.1061(13) Uani 1 1 d . . . . . H20A H -0.5533 0.6476 0.7329 0.159 Uiso 1 1 calc R U . . . H20B H -0.4811 0.6689 0.8312 0.159 Uiso 1 1 calc R U . . . H20C H -0.5899 0.5902 0.8186 0.159 Uiso 1 1 calc R U . . . C20 C -0.2863(4) 0.34269(17) 0.7021(2) 0.0715(9) Uani 1 1 d . . . . . H11A H -0.2633 0.3110 0.7577 0.107 Uiso 1 1 calc R U . . . H11B H -0.2178 0.3253 0.6536 0.107 Uiso 1 1 calc R U . . . H11C H -0.3925 0.3328 0.6828 0.107 Uiso 1 1 calc R U . . . H1 H 0.016(3) 0.2917(17) 0.4742(17) 0.054(9) Uiso 1 1 d . . . . . N1 N 0.0148(2) 0.42375(12) 0.68776(13) 0.0437(5) Uani 1 1 d . . . . . N2 N 0.1836(2) 0.37107(12) 0.59693(13) 0.0441(5) Uani 1 1 d . . . . . N3 N 0.0288(3) 0.2399(2) 0.4629(2) 0.0787(8) 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 Ni1 0.0422(3) 0.0437(3) 0.0409(2) 0.0046(2) 0.0025(2) 0.0053(2) Br1 0.05455(19) 0.0647(2) 0.0666(2) 0.01028(15) -0.00477(14) -0.00816(15) C1 0.0396(14) 0.0393(14) 0.0447(14) -0.0008(11) 0.0009(11) 0.0008(12) C2 0.0672(19) 0.0601(18) 0.0411(14) 0.0071(13) 0.0005(14) 0.0155(15) C3 0.0603(18) 0.0566(16) 0.0482(15) 0.0091(14) -0.0018(14) 0.0168(14) C4 0.0476(15) 0.0591(18) 0.0489(15) 0.0054(13) 0.0099(13) 0.0048(13) C5 0.0482(16) 0.0541(16) 0.0413(14) -0.0028(12) 0.0071(12) 0.0061(14) C6 0.0489(16) 0.0604(18) 0.0554(17) -0.0032(14) 0.0091(13) 0.0062(14) C7 0.061(2) 0.065(2) 0.0631(18) 0.0012(15) 0.0084(16) 0.0176(17) C8 0.088(2) 0.0523(18) 0.0627(19) -0.0051(15) 0.0099(17) 0.0115(19) C9 0.067(2) 0.067(2) 0.067(2) -0.0144(16) -0.0017(16) -0.0018(17) C10 0.0524(17) 0.0607(18) 0.0484(16) -0.0064(13) 0.0021(13) 0.0081(15) C11 0.055(2) 0.103(3) 0.159(4) -0.035(3) -0.027(2) -0.003(2) C12 0.0465(15) 0.0447(15) 0.0392(13) 0.0007(11) 0.0026(12) 0.0054(12) C13 0.0507(17) 0.0487(16) 0.0484(15) -0.0060(12) 0.0053(13) -0.0005(13) C14 0.067(2) 0.0463(17) 0.075(2) -0.0134(14) 0.0068(17) 0.0033(15) C15 0.0538(18) 0.065(2) 0.082(2) -0.0092(17) 0.0061(16) 0.0124(17) C16 0.0472(16) 0.069(2) 0.0714(19) -0.0052(16) 0.0051(15) -0.0052(16) C17 0.0564(17) 0.0475(16) 0.0477(15) -0.0002(12) 0.0079(14) -0.0051(14) C18 0.062(2) 0.082(2) 0.081(2) -0.0265(18) 0.0097(17) -0.0182(17) C19 0.071(2) 0.098(3) 0.150(4) -0.028(3) 0.005(2) 0.031(2) C20 0.085(2) 0.0562(18) 0.074(2) -0.0105(16) 0.0182(17) -0.0194(17) N1 0.0452(12) 0.0471(12) 0.0389(11) 0.0015(10) 0.0040(10) 0.0090(10) N2 0.0453(12) 0.0449(12) 0.0421(12) -0.0002(10) 0.0035(10) 0.0099(10) N3 0.0544(17) 0.0691(19) 0.112(2) -0.0231(17) -0.0130(15) 0.0036(15) _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 C1 1.909(2) . ? Ni1 C1 1.909(2) 3_566 ? Ni1 Br1 2.3274(7) 3_566 ? Ni1 Br1 2.3274(7) . ? C1 N1 1.350(3) . ? C1 N2 1.351(3) . ? C2 C3 1.329(4) . ? C2 N1 1.383(3) . ? C2 H2 0.9300 . ? C3 N2 1.375(3) . ? C3 H3 0.9300 . ? C4 N2 1.481(3) . ? C4 C5 1.498(4) . ? C4 H5A 0.9700 . ? C4 H5B 0.9700 . ? C5 C6 1.383(3) . ? C5 C10 1.404(4) . ? C6 C7 1.380(4) . ? C6 H10 0.9300 . ? C7 C8 1.371(4) . ? C7 H12 0.9300 . ? C8 C9 1.367(4) . ? C8 H17 0.9300 . ? C9 C10 1.393(4) . ? C9 H15 0.9300 . ? C10 N3 1.366(4) . ? C11 N3 1.437(4) . ? C11 H19A 0.9600 . ? C11 H19B 0.9600 . ? C11 H19C 0.9600 . ? C12 C13 1.386(3) . ? C12 C17 1.390(3) . ? C12 N1 1.449(3) . ? C13 C14 1.389(4) . ? C13 C18 1.499(4) . ? C14 C15 1.377(4) . ? C14 H9 0.9300 . ? C15 C16 1.379(4) . ? C15 C19 1.524(4) . ? C16 C17 1.382(4) . ? C16 H16 0.9300 . ? C17 C20 1.518(4) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H20A 0.9600 . ? C19 H20B 0.9600 . ? C19 H20C 0.9600 . ? C20 H11A 0.9600 . ? C20 H11B 0.9600 . ? C20 H11C 0.9600 . ? N3 H1 0.85(3) . ? 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 C1 Ni1 C1 180.0 . 3_566 ? C1 Ni1 Br1 91.33(7) . 3_566 ? C1 Ni1 Br1 88.67(7) 3_566 3_566 ? C1 Ni1 Br1 88.67(7) . . ? C1 Ni1 Br1 91.33(7) 3_566 . ? Br1 Ni1 Br1 180.000(12) 3_566 . ? N1 C1 N2 104.43(19) . . ? N1 C1 Ni1 129.27(17) . . ? N2 C1 Ni1 126.25(18) . . ? C3 C2 N1 107.0(2) . . ? C3 C2 H2 126.5 . . ? N1 C2 H2 126.5 . . ? C2 C3 N2 107.0(2) . . ? C2 C3 H3 126.5 . . ? N2 C3 H3 126.5 . . ? N2 C4 C5 112.6(2) . . ? N2 C4 H5A 109.1 . . ? C5 C4 H5A 109.1 . . ? N2 C4 H5B 109.1 . . ? C5 C4 H5B 109.1 . . ? H5A C4 H5B 107.8 . . ? C6 C5 C10 118.9(3) . . ? C6 C5 C4 119.7(3) . . ? C10 C5 C4 121.4(2) . . ? C7 C6 C5 122.0(3) . . ? C7 C6 H10 119.0 . . ? C5 C6 H10 119.0 . . ? C8 C7 C6 118.5(3) . . ? C8 C7 H12 120.7 . . ? C6 C7 H12 120.7 . . ? C9 C8 C7 121.0(3) . . ? C9 C8 H17 119.5 . . ? C7 C8 H17 119.5 . . ? C8 C9 C10 121.2(3) . . ? C8 C9 H15 119.4 . . ? C10 C9 H15 119.4 . . ? N3 C10 C9 120.8(3) . . ? N3 C10 C5 120.8(3) . . ? C9 C10 C5 118.3(3) . . ? N3 C11 H19A 109.5 . . ? N3 C11 H19B 109.5 . . ? H19A C11 H19B 109.5 . . ? N3 C11 H19C 109.5 . . ? H19A C11 H19C 109.5 . . ? H19B C11 H19C 109.5 . . ? C13 C12 C17 121.6(2) . . ? C13 C12 N1 119.4(2) . . ? C17 C12 N1 118.9(2) . . ? C12 C13 C14 117.8(2) . . ? C12 C13 C18 122.0(2) . . ? C14 C13 C18 120.2(2) . . ? C15 C14 C13 122.1(3) . . ? C15 C14 H9 119.0 . . ? C13 C14 H9 119.0 . . ? C14 C15 C16 118.2(3) . . ? C14 C15 C19 121.2(3) . . ? C16 C15 C19 120.6(3) . . ? C15 C16 C17 122.1(3) . . ? C15 C16 H16 118.9 . . ? C17 C16 H16 118.9 . . ? C16 C17 C12 117.9(2) . . ? C16 C17 C20 120.4(3) . . ? C12 C17 C20 121.6(2) . . ? C13 C18 H18A 109.5 . . ? C13 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C13 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C15 C19 H20A 109.5 . . ? C15 C19 H20B 109.5 . . ? H20A C19 H20B 109.5 . . ? C15 C19 H20C 109.5 . . ? H20A C19 H20C 109.5 . . ? H20B C19 H20C 109.5 . . ? C17 C20 H11A 109.5 . . ? C17 C20 H11B 109.5 . . ? H11A C20 H11B 109.5 . . ? C17 C20 H11C 109.5 . . ? H11A C20 H11C 109.5 . . ? H11B C20 H11C 109.5 . . ? C1 N1 C2 110.6(2) . . ? C1 N1 C12 123.44(19) . . ? C2 N1 C12 125.9(2) . . ? C1 N2 C3 111.0(2) . . ? C1 N2 C4 124.0(2) . . ? C3 N2 C4 125.0(2) . . ? C10 N3 C11 123.9(3) . . ? C10 N3 H1 117.1(18) . . ? C11 N3 H1 119.0(18) . . ? _refine_diff_density_max 0.525 _refine_diff_density_min -0.233 _refine_diff_density_rms 0.056 _shelxl_version_number 2013-2 _shelx_res_file ; TITL a00919a in P2(1)/n CELL 0.71073 8.5734 15.8697 14.3508 90.000 91.024 90.000 ZERR 2.00 0.0031 0.0055 0.0051 0.000 0.005 0.000 LATT 1 SYMM 0.5-X, 0.5+Y, 0.5-Z SFAC C H N Ni Br UNIT 80 92 12 2 4 OMIT 0.00 52.60 L.S. 10 ACTA BOND $H FMAP 2 PLAN 10 size 0.15 0.13 0.12 TEMP 20 WGHT 0.033400 FVAR 0.12911 NI1 4 0.000000 0.500000 0.500000 10.50000 0.04222 0.04373 = 0.04094 0.00461 0.00245 0.00533 BR1 5 0.222757 0.581040 0.526168 11.00000 0.05455 0.06469 = 0.06662 0.01028 -0.00477 -0.00816 C1 1 0.066498 0.427985 0.599555 11.00000 0.03964 0.03928 = 0.04469 -0.00075 0.00085 0.00082 C2 1 0.100056 0.365355 0.738943 11.00000 0.06723 0.06010 = 0.04110 0.00710 0.00051 0.01551 AFIX 43 H2 2 0.086462 0.351465 0.801230 11.00000 -1.20000 AFIX 0 C3 1 0.205102 0.332872 0.682166 11.00000 0.06033 0.05664 = 0.04816 0.00912 -0.00176 0.01682 AFIX 43 H3 2 0.279143 0.292035 0.697252 11.00000 -1.20000 AFIX 0 C4 1 0.278005 0.354291 0.513533 11.00000 0.04757 0.05909 = 0.04890 0.00537 0.00986 0.00480 AFIX 23 H5A 2 0.378818 0.381395 0.521255 11.00000 -1.20000 H5B 2 0.226339 0.378908 0.459361 11.00000 -1.20000 AFIX 0 C5 1 0.302034 0.262054 0.496753 11.00000 0.04825 0.05407 = 0.04128 -0.00277 0.00709 0.00611 C6 1 0.450505 0.228282 0.503735 11.00000 0.04888 0.06038 = 0.05540 -0.00322 0.00906 0.00625 AFIX 43 H10 2 0.533667 0.263567 0.519100 11.00000 -1.20000 AFIX 0 C7 1 0.479063 0.143841 0.488606 11.00000 0.06114 0.06478 = 0.06313 0.00117 0.00841 0.01763 AFIX 43 H12 2 0.579908 0.122441 0.493014 11.00000 -1.20000 AFIX 0 C8 1 0.355439 0.092215 0.466933 11.00000 0.08821 0.05232 = 0.06267 -0.00510 0.00993 0.01150 AFIX 43 H17 2 0.372677 0.035044 0.457291 11.00000 -1.20000 AFIX 0 C9 1 0.207179 0.123521 0.459281 11.00000 0.06654 0.06676 = 0.06677 -0.01445 -0.00173 -0.00175 AFIX 43 H15 2 0.125168 0.087211 0.444705 11.00000 -1.20000 AFIX 0 C10 1 0.176753 0.208799 0.472920 11.00000 0.05243 0.06070 = 0.04836 -0.00640 0.00215 0.00813 C11 1 -0.103948 0.189777 0.435917 11.00000 0.05520 0.10324 = 0.15936 -0.03533 -0.02747 -0.00332 AFIX 137 H19A 2 -0.081282 0.159343 0.379954 11.00000 -1.50000 H19B 2 -0.192308 0.225819 0.424934 11.00000 -1.50000 H19C 2 -0.126975 0.150655 0.484804 11.00000 -1.50000 AFIX 0 C12 1 -0.115665 0.472582 0.721104 11.00000 0.04654 0.04471 = 0.03921 0.00070 0.00262 0.00539 C13 1 -0.091439 0.554878 0.750326 11.00000 0.05072 0.04870 = 0.04836 -0.00595 0.00533 -0.00046 C14 1 -0.221352 0.602242 0.773613 11.00000 0.06725 0.04630 = 0.07518 -0.01342 0.00679 0.00327 AFIX 43 H9 2 -0.207301 0.657589 0.793336 11.00000 -1.20000 AFIX 0 C15 1 -0.370236 0.569839 0.768417 11.00000 0.05377 0.06531 = 0.08231 -0.00916 0.00613 0.01237 C16 1 -0.388201 0.486323 0.743908 11.00000 0.04723 0.06905 = 0.07143 -0.00517 0.00513 -0.00516 AFIX 43 H16 2 -0.487870 0.463176 0.742434 11.00000 -1.20000 AFIX 0 C17 1 -0.262950 0.435932 0.721477 11.00000 0.05637 0.04754 = 0.04774 -0.00016 0.00792 -0.00509 C18 1 0.068839 0.591987 0.759916 11.00000 0.06244 0.08151 = 0.08084 -0.02655 0.00971 -0.01821 AFIX 137 H18A 2 0.138067 0.551339 0.787941 11.00000 -1.50000 H18B 2 0.065088 0.641335 0.798503 11.00000 -1.50000 H18C 2 0.106002 0.607052 0.699447 11.00000 -1.50000 AFIX 0 C19 1 -0.511745 0.624171 0.789748 11.00000 0.07069 0.09796 = 0.14977 -0.02750 0.00461 0.03143 AFIX 137 H20A 2 -0.553299 0.647636 0.732864 11.00000 -1.50000 H20B 2 -0.481148 0.668916 0.831215 11.00000 -1.50000 H20C 2 -0.589932 0.590187 0.818603 11.00000 -1.50000 AFIX 0 C20 1 -0.286299 0.342693 0.702103 11.00000 0.08486 0.05625 = 0.07393 -0.01053 0.01815 -0.01937 AFIX 137 H11A 2 -0.263349 0.311046 0.757686 11.00000 -1.50000 H11B 2 -0.217786 0.325264 0.653553 11.00000 -1.50000 H11C 2 -0.392527 0.332809 0.682820 11.00000 -1.50000 AFIX 0 H1 2 0.015927 0.291720 0.474213 11.00000 0.05374 N1 3 0.014818 0.423746 0.687757 11.00000 0.04524 0.04706 = 0.03890 0.00152 0.00404 0.00899 N2 3 0.183570 0.371072 0.596926 11.00000 0.04532 0.04491 = 0.04211 -0.00015 0.00345 0.00991 N3 3 0.028822 0.239933 0.462942 11.00000 0.05439 0.06910 = 0.11209 -0.02307 -0.01303 0.00362 HKLF 4 REM a00919a in P2(1)/n REM R1 = 0.0341 for 2598 Fo > 4sig(Fo) and 0.0559 for all 3961 data REM 231 parameters refined using 0 restraints END WGHT 0.0334 0.0000 REM Highest difference peak 0.525, deepest hole -0.233, 1-sigma level 0.056 Q1 1 0.1560 0.5836 0.5863 11.00000 0.05 0.52 Q2 1 0.0611 0.4981 0.4413 11.00000 0.05 0.41 Q3 1 0.0497 0.4590 0.5420 11.00000 0.05 0.36 Q4 1 0.2483 0.6365 0.5610 11.00000 0.05 0.30 Q5 1 0.2709 0.5384 0.5606 11.00000 0.05 0.26 Q6 1 0.2128 0.3634 0.5579 11.00000 0.05 0.26 Q7 1 0.2922 0.5770 0.4565 11.00000 0.05 0.26 Q8 1 0.1786 0.6368 0.5053 11.00000 0.05 0.24 Q9 1 -0.2760 0.3965 0.7206 11.00000 0.05 0.22 Q10 1 0.0307 0.5528 0.5391 11.00000 0.05 0.22 ; _shelx_res_checksum 89675 _shelx_hkl_file ; 2 -2 -18 0.75 0.84 2 -1 -18 0.07 0.87 1 0 -18 0.15 0.74 2 0 -18 2.12 0.91 1 1 -18 1.01 0.82 2 1 -18 0.35 0.86 0 2 -18 -0.07 0.77 1 2 -18 0.83 0.82 2 2 -18 0.63 0.81 0 3 -18 0.18 0.83 1 3 -18 0.17 0.81 -1 4 -18 0.15 0.79 0 4 -18 2.44 0.89 1 4 -18 0.52 0.82 3 -5 -17 0.42 0.89 3 -4 -17 1.25 0.85 2 -3 -17 1.29 0.78 3 -3 -17 2.46 0.99 4 -3 -17 0.63 0.90 2 -2 -17 -0.51 0.77 3 -2 -17 0.24 0.84 4 -2 -17 0.06 0.88 1 -1 -17 0.73 0.70 2 -1 -17 3.93 0.89 3 -1 -17 0.22 0.90 4 -1 -17 -0.32 0.86 1 0 -17 2.44 0.79 2 0 -17 0.15 0.74 3 0 -17 0.71 0.82 0 1 -17 0.18 0.63 1 1 -17 1.02 0.72 2 1 -17 4.28 0.90 3 1 -17 0.64 0.78 0 2 -17 0.10 0.68 1 2 -17 2.01 0.81 2 2 -17 -0.02 0.77 3 2 -17 0.02 0.77 -1 3 -17 0.62 0.66 0 3 -17 0.40 0.69 1 3 -17 0.95 0.77 2 3 -17 1.47 0.84 3 3 -17 1.79 0.84 -1 4 -17 1.14 0.70 0 4 -17 1.09 0.74 1 4 -17 0.34 0.77 2 4 -17 0.42 0.73 3 4 -17 1.32 0.87 -2 5 -17 0.34 0.77 -1 5 -17 -0.06 0.70 0 5 -17 3.88 0.94 1 5 -17 0.28 0.74 2 5 -17 -0.44 0.77 -2 6 -17 0.35 0.75 -1 6 -17 2.49 0.87 0 6 -17 0.80 0.76 1 6 -17 1.01 0.78 -1 7 -17 0.56 0.82 0 7 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0.25 0.69 3 4 -16 0.57 0.74 4 4 -16 1.19 0.78 -1 5 -16 1.97 0.75 0 5 -16 0.91 0.69 1 5 -16 0.42 0.67 2 5 -16 0.19 0.70 3 5 -16 0.14 0.71 4 5 -16 0.43 0.80 -1 6 -16 1.02 0.74 0 6 -16 5.82 0.93 1 6 -16 -0.11 0.68 2 6 -16 0.75 0.76 3 6 -16 -0.18 0.69 0 7 -16 0.13 0.70 1 7 -16 -0.27 0.68 2 7 -16 0.49 0.73 3 7 -16 1.20 0.83 0 8 -16 2.43 0.87 1 8 -16 0.06 0.75 2 8 -16 0.20 0.75 0 9 -16 0.25 0.80 4 -9 -15 0.34 0.81 4 -8 -15 -0.12 0.75 3 -7 -15 1.58 0.74 4 -7 -15 7.25 1.09 5 -7 -15 -0.01 0.83 3 -6 -15 1.48 0.74 4 -6 -15 0.57 0.78 5 -6 -15 1.66 0.90 2 -5 -15 0.01 0.63 3 -5 -15 0.04 0.71 4 -5 -15 4.93 1.01 5 -5 -15 1.58 0.91 1 -4 -15 0.94 0.65 2 -4 -15 0.83 0.72 3 -4 -15 1.75 0.78 4 -4 -15 0.48 0.79 5 -4 -15 1.74 0.94 1 -3 -15 1.52 0.69 2 -3 -15 3.61 0.79 3 -3 -15 4.52 0.92 4 -3 -15 0.28 0.73 5 -3 -15 3.09 0.94 0 -2 -15 0.83 0.56 1 -2 -15 6.26 0.84 2 -2 -15 1.26 0.74 3 -2 -15 0.38 0.68 4 -2 -15 0.76 0.79 5 -2 -15 2.71 0.90 0 -1 -15 0.00 0.55 1 -1 -15 0.34 0.58 2 -1 -15 4.93 0.84 3 -1 -15 1.85 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173.67 1.52 4 -4 2 7.20 0.39 5 -4 2 14.30 2.49 6 -4 2 36.12 0.93 7 -4 2 11.49 0.64 8 -4 2 0.12 0.37 -1 -3 2 9.36 0.38 0 -3 2 33.18 0.70 1 -3 2 103.34 0.90 2 -3 2 5.30 0.25 3 -3 2 7.78 0.93 4 -3 2 20.64 0.85 5 -3 2 5.83 0.40 6 -3 2 20.28 0.70 7 -3 2 2.35 0.41 8 -3 2 6.80 0.56 9 -3 2 1.83 0.73 -1 -2 2 302.78 2.46 0 -2 2 58.74 0.70 1 -2 2 106.87 1.30 2 -2 2 21.48 1.92 3 -2 2 41.82 0.71 4 -2 2 73.84 1.05 5 -2 2 13.88 0.54 6 -2 2 0.51 0.31 7 -2 2 1.20 0.34 8 -2 2 2.69 0.67 9 -2 2 1.86 0.68 10 -2 2 -0.20 0.64 0 -1 2 4.86 0.16 1 -1 2 1.24 0.12 2 -1 2 57.30 0.69 3 -1 2 18.94 0.48 4 -1 2 16.31 0.52 5 -1 2 58.01 1.02 6 -1 2 8.72 0.50 7 -1 2 0.66 0.37 8 -1 2 5.57 0.79 9 -1 2 10.42 1.05 10 -1 2 2.06 0.78 11 -1 2 0.59 0.89 0 0 2 297.87 2.08 1 0 2 -0.03 0.08 2 0 2 253.39 2.23 3 0 2 0.12 0.18 4 0 2 322.62 2.33 5 0 2 0.00 0.26 6 0 2 0.35 0.28 7 0 2 -0.06 0.51 8 0 2 4.42 0.76 9 0 2 -0.06 0.59 10 0 2 0.67 0.69 11 0 2 0.28 0.80 -1 1 2 259.92 1.58 0 1 2 4.27 0.76 1 1 2 1.27 0.10 2 1 2 56.64 0.61 3 1 2 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-2 7 16 0.11 0.57 -1 7 16 -0.10 0.59 0 7 16 0.63 0.70 1 7 16 1.91 0.78 2 7 16 0.16 0.86 3 7 16 -0.03 0.74 -1 8 16 0.67 0.64 0 8 16 2.81 0.85 1 8 16 1.10 0.75 2 8 16 -0.11 0.86 3 8 16 0.43 0.83 1 9 16 1.57 0.80 2 9 16 0.88 0.94 0 -7 17 2.95 0.99 1 -7 17 0.25 0.82 2 -7 17 -0.03 0.53 0 -6 17 0.56 0.87 1 -6 17 1.94 0.95 2 -6 17 0.00 0.81 -1 -5 17 0.51 0.84 0 -5 17 4.25 0.99 1 -5 17 -0.38 0.79 2 -5 17 0.70 0.82 -1 -4 17 0.20 0.80 0 -4 17 1.63 0.88 1 -4 17 1.06 0.85 2 -4 17 0.89 0.90 3 -4 17 0.47 0.89 -1 -3 17 1.44 0.88 0 -3 17 0.31 0.79 1 -3 17 0.10 0.73 2 -3 17 0.56 0.82 3 -3 17 0.12 0.83 -1 -2 17 3.10 0.93 0 -2 17 -0.18 0.77 1 -2 17 0.42 0.78 2 -2 17 1.02 0.82 3 -2 17 1.88 0.89 -2 -1 17 4.24 0.99 -1 -1 17 0.80 0.72 0 -1 17 0.12 0.77 1 -1 17 0.07 0.82 2 -1 17 3.85 0.98 3 -1 17 -0.12 0.84 -2 0 17 0.30 0.67 -1 0 17 2.35 0.85 0 0 17 -0.06 0.65 1 0 17 0.35 0.67 2 0 17 0.10 0.82 3 0 17 4.86 1.05 -2 1 17 4.13 0.93 -1 1 17 0.88 0.71 0 1 17 -0.02 0.64 1 1 17 0.23 0.69 2 1 17 3.32 0.90 3 1 17 0.08 0.86 -2 2 17 -0.15 0.65 -1 2 17 2.39 0.81 0 2 17 0.29 0.64 1 2 17 0.47 0.73 2 2 17 0.64 0.74 -2 3 17 1.67 0.74 -1 3 17 0.81 0.69 0 3 17 0.32 0.65 1 3 17 0.48 0.74 2 3 17 0.77 0.77 -2 4 17 0.49 0.69 -1 4 17 0.37 0.70 0 4 17 1.88 0.83 1 4 17 0.44 0.75 2 4 17 0.81 0.79 -2 5 17 -0.41 0.62 -1 5 17 0.54 0.73 0 5 17 4.98 0.99 1 5 17 0.16 0.76 2 5 17 0.24 0.80 -2 6 17 -0.02 0.65 -1 6 17 0.66 0.72 0 6 17 1.18 0.80 1 6 17 2.77 0.89 -2 7 17 0.33 0.69 -1 7 17 0.04 0.76 0 7 17 2.66 0.89 1 7 17 0.47 0.81 0 8 17 -0.05 0.74 1 8 17 2.01 0.90 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 64544 _database_code_depnum_ccdc_archive 'CCDC 877557' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_a20106a _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H42 Br2 N6 Ni' _chemical_formula_weight 705.22 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 21/c' _space_group_name_Hall '-P 2ybc' _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+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.292(6) _cell_length_b 13.510(8) _cell_length_c 12.261(7) _cell_angle_alpha 90 _cell_angle_beta 111.141(8) _cell_angle_gamma 90 _cell_volume 1590.1(15) _cell_formula_units_Z 2 _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 1.473 _exptl_crystal_F_000 724 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.250 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.100 _exptl_absorpt_coefficient_mu 3.152 _shelx_estimated_absorpt_T_min 0.506 _shelx_estimated_absorpt_T_max 0.743 _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 0.71073 _diffrn_radiation_type MoK\a _diffrn_source ? _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 7123 _diffrn_reflns_av_unetI/netI 0.0657 _diffrn_reflns_av_R_equivalents 0.0443 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.122 _diffrn_reflns_theta_max 26.006 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_point_group_measured_fraction_max 0.996 _diffrn_reflns_point_group_measured_fraction_full 0.996 _reflns_number_total 3114 _reflns_number_gt 1717 _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-2013 (Sheldrick, 2013)' _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^)+(0.0480P)^2^] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 3114 _refine_ls_number_parameters 207 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0808 _refine_ls_R_factor_gt 0.0419 _refine_ls_wR_factor_ref 0.0998 _refine_ls_wR_factor_gt 0.0914 _refine_ls_goodness_of_fit_ref 0.846 _refine_ls_restrained_S_all 0.849 _refine_ls_shift/su_max 0.010 _refine_ls_shift/su_mean 0.001 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 0.0000 0.5000 1.0000 0.0580(2) Uani 1 2 d S . P . . Br1 Br 0.18510(5) 0.46677(3) 1.17268(4) 0.0866(2) Uani 1 1 d . . . . . N1 N -0.3480(5) 0.2810(3) 0.7780(4) 0.1074(14) Uani 1 1 d . . . . . H1D H -0.2946 0.3316 0.8022 0.129 Uiso 1 1 calc R U . . . N2 N -0.0301(4) 0.2915(2) 0.9482(3) 0.0699(9) Uani 1 1 d . . . . . N3 N 0.1208(3) 0.3461(2) 0.8789(3) 0.0674(9) Uani 1 1 d . . . . . C1 C -0.4460(6) 0.2800(4) 0.6611(6) 0.128(2) Uani 1 1 d . . . . . H1A H -0.4341 0.2207 0.6226 0.192 Uiso 1 1 calc R U . . . H1B H -0.4310 0.3367 0.6199 0.192 Uiso 1 1 calc R U . . . H1C H -0.5388 0.2820 0.6621 0.192 Uiso 1 1 calc R U . . . C2 C -0.3365(5) 0.2039(3) 0.8528(5) 0.0842(14) Uani 1 1 d . . . . . C3 C -0.4313(5) 0.1253(4) 0.8180(5) 0.0922(15) Uani 1 1 d . . . . . H3 H -0.5039 0.1272 0.7459 0.111 Uiso 1 1 calc R U . . . C4 C -0.4170(7) 0.0474(4) 0.8888(6) 0.1083(18) Uani 1 1 d . . . . . H4 H -0.4792 -0.0050 0.8632 0.130 Uiso 1 1 calc R U . . . C5 C -0.3141(7) 0.0416(4) 0.9982(6) 0.1078(18) Uani 1 1 d . . . . . H5 H -0.3063 -0.0134 1.0457 0.129 Uiso 1 1 calc R U . . . C6 C -0.2227(6) 0.1208(4) 1.0349(5) 0.0978(15) Uani 1 1 d . . . . . H6 H -0.1539 0.1196 1.1091 0.117 Uiso 1 1 calc R U . . . C7 C -0.2323(5) 0.2022(3) 0.9621(5) 0.0787(13) Uani 1 1 d . . . . . C8 C -0.1331(5) 0.2870(3) 1.0055(4) 0.0788(13) Uani 1 1 d . . . . . H8A H -0.1853 0.3484 0.9915 0.095 Uiso 1 1 calc R U . . . H8B H -0.0849 0.2803 1.0893 0.095 Uiso 1 1 calc R U . . . C9 C 0.0165(5) 0.2114(3) 0.9033(4) 0.0840(14) Uani 1 1 d . . . . . H9 H -0.0118 0.1460 0.9029 0.101 Uiso 1 1 calc R U . . . C10 C 0.1090(5) 0.2452(3) 0.8607(4) 0.0838(14) Uani 1 1 d . . . . . H10 H 0.1577 0.2075 0.8247 0.101 Uiso 1 1 calc R U . . . C11 C 0.0360(4) 0.3763(3) 0.9357(3) 0.0601(10) Uani 1 1 d . . . . . C12 C 0.2181(5) 0.4057(3) 0.8400(4) 0.0818(13) Uani 1 1 d D . . . . C13 C 0.2145(15) 0.5119(6) 0.8663(15) 0.130(6) Uani 0.702(17) 1 d D . P A 1 H13A H 0.1348 0.5421 0.8085 0.195 Uiso 0.702(17) 1 calc R U P A 1 H13B H 0.2978 0.5433 0.8653 0.195 Uiso 0.702(17) 1 calc R U P A 1 H13C H 0.2086 0.5197 0.9422 0.195 Uiso 0.702(17) 1 calc R U P A 1 C14 C 0.1722(15) 0.3871(10) 0.7065(8) 0.139(6) Uani 0.702(17) 1 d . . P A 1 H14A H 0.0725 0.3820 0.6732 0.208 Uiso 0.702(17) 1 calc R U P A 1 H14B H 0.2132 0.3267 0.6931 0.208 Uiso 0.702(17) 1 calc R U P A 1 H14C H 0.2024 0.4412 0.6707 0.208 Uiso 0.702(17) 1 calc R U P A 1 C15 C 0.3608(9) 0.3650(9) 0.8891(15) 0.142(5) Uani 0.702(17) 1 d . . P A 1 H15A H 0.3720 0.3146 0.8380 0.214 Uiso 0.702(17) 1 calc R U P A 1 H15B H 0.3761 0.3369 0.9647 0.214 Uiso 0.702(17) 1 calc R U P A 1 H15C H 0.4270 0.4170 0.8966 0.214 Uiso 0.702(17) 1 calc R U P A 1 C13' C 0.337(2) 0.438(3) 0.9525(18) 0.136(16) Uani 0.298(17) 1 d . . P A 2 H13D H 0.3007 0.4501 1.0131 0.204 Uiso 0.298(17) 1 calc R U P A 2 H13E H 0.3790 0.4976 0.9376 0.204 Uiso 0.298(17) 1 calc R U P A 2 H13F H 0.4062 0.3867 0.9769 0.204 Uiso 0.298(17) 1 calc R U P A 2 C14' C 0.135(3) 0.4989(16) 0.788(2) 0.098(8) Uani 0.298(17) 1 d . . P A 2 H14D H 0.0573 0.4820 0.7195 0.147 Uiso 0.298(17) 1 calc R U P A 2 H14E H 0.1942 0.5449 0.7682 0.147 Uiso 0.298(17) 1 calc R U P A 2 H14F H 0.1028 0.5286 0.8449 0.147 Uiso 0.298(17) 1 calc R U P A 2 C15' C 0.268(4) 0.355(2) 0.756(3) 0.146(11) Uani 0.298(17) 1 d D U P A 2 H15D H 0.1902 0.3407 0.6858 0.220 Uiso 0.298(17) 1 calc R U P A 2 H15E H 0.3133 0.2943 0.7898 0.220 Uiso 0.298(17) 1 calc R U P A 2 H15F H 0.3327 0.3969 0.7379 0.220 Uiso 0.298(17) 1 calc R U P A 2 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 0.0562(4) 0.0600(4) 0.0586(4) -0.0047(3) 0.0215(4) -0.0058(3) Br1 0.0831(4) 0.0841(3) 0.0748(3) 0.0027(2) 0.0070(3) -0.0013(2) N1 0.113(4) 0.088(3) 0.121(4) 0.007(3) 0.041(3) -0.011(3) N2 0.082(2) 0.060(2) 0.079(2) -0.0106(17) 0.043(2) -0.0105(19) N3 0.069(2) 0.068(2) 0.074(2) -0.0055(18) 0.037(2) -0.0059(18) C1 0.116(5) 0.132(5) 0.142(6) 0.021(4) 0.054(5) 0.016(4) C2 0.088(4) 0.071(3) 0.117(5) -0.004(3) 0.064(4) -0.004(3) C3 0.083(3) 0.092(4) 0.117(4) -0.018(3) 0.054(3) -0.024(3) C4 0.119(5) 0.099(4) 0.135(6) -0.018(4) 0.080(5) -0.032(4) C5 0.141(5) 0.086(4) 0.125(5) 0.006(4) 0.083(5) -0.024(4) C6 0.113(4) 0.099(4) 0.101(4) 0.010(3) 0.061(3) -0.014(3) C7 0.084(3) 0.080(3) 0.086(4) -0.008(3) 0.048(3) -0.010(3) C8 0.090(3) 0.084(3) 0.080(3) -0.016(2) 0.051(3) -0.021(3) C9 0.107(4) 0.063(3) 0.096(4) -0.018(2) 0.054(3) -0.012(3) C10 0.095(4) 0.072(3) 0.102(4) -0.017(3) 0.058(3) -0.001(3) C11 0.056(2) 0.067(3) 0.060(3) -0.003(2) 0.024(2) -0.004(2) C12 0.082(4) 0.090(3) 0.088(4) -0.008(3) 0.049(3) -0.016(3) C13 0.129(12) 0.103(7) 0.212(17) -0.021(9) 0.126(13) -0.031(7) C14 0.150(11) 0.198(12) 0.092(7) -0.036(7) 0.074(8) -0.082(9) C15 0.070(6) 0.146(9) 0.215(16) 0.009(9) 0.057(8) 0.012(6) C13' 0.061(14) 0.24(4) 0.107(17) 0.017(18) 0.029(12) -0.08(2) C14' 0.100(16) 0.088(14) 0.100(16) 0.051(12) 0.027(12) -0.034(11) C15' 0.136(18) 0.165(17) 0.18(2) -0.013(14) 0.113(16) 0.006(14) _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 C11 1.940(4) . ? Ni1 C11 1.940(4) 3_567 ? Ni1 Br1 2.3247(10) . ? Ni1 Br1 2.3247(10) 3_567 ? N1 C2 1.364(6) . ? N1 C1 1.425(6) . ? N1 H1D 0.8600 . ? N2 C11 1.369(4) . ? N2 C9 1.376(5) . ? N2 C8 1.469(5) . ? N3 C11 1.360(4) . ? N3 C10 1.380(5) . ? N3 C12 1.491(5) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C7 1.381(6) . ? C2 C3 1.400(6) . ? C3 C4 1.338(7) . ? C3 H3 0.9300 . ? C4 C5 1.379(7) . ? C4 H4 0.9300 . ? C5 C6 1.388(7) . ? C5 H5 0.9300 . ? C6 C7 1.398(6) . ? C6 H6 0.9300 . ? C7 C8 1.499(6) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.321(5) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C12 C13 1.475(7) . ? C12 C15' 1.474(10) . ? C12 C15 1.478(10) . ? C12 C14' 1.52(2) . ? C12 C14 1.551(9) . ? C12 C13' 1.54(2) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C13' H13D 0.9600 . ? C13' H13E 0.9600 . ? C13' H13F 0.9600 . ? C14' H14D 0.9600 . ? C14' H14E 0.9600 . ? C14' H14F 0.9600 . ? C15' H15D 0.9600 . ? C15' H15E 0.9600 . ? C15' H15F 0.9600 . ? 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 C11 Ni1 C11 180.0(2) . 3_567 ? C11 Ni1 Br1 89.42(11) . . ? C11 Ni1 Br1 90.58(11) 3_567 . ? C11 Ni1 Br1 90.58(11) . 3_567 ? C11 Ni1 Br1 89.42(11) 3_567 3_567 ? Br1 Ni1 Br1 180.0 . 3_567 ? C2 N1 C1 121.9(5) . . ? C2 N1 H1D 119.1 . . ? C1 N1 H1D 119.1 . . ? C11 N2 C9 110.7(3) . . ? C11 N2 C8 124.2(3) . . ? C9 N2 C8 125.1(3) . . ? C11 N3 C10 110.1(3) . . ? C11 N3 C12 129.1(3) . . ? C10 N3 C12 120.8(3) . . ? N1 C1 H1A 109.5 . . ? N1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? N1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 C7 120.9(5) . . ? N1 C2 C3 119.5(5) . . ? C7 C2 C3 119.7(5) . . ? C4 C3 C2 119.8(6) . . ? C4 C3 H3 120.1 . . ? C2 C3 H3 120.1 . . ? C3 C4 C5 122.8(6) . . ? C3 C4 H4 118.6 . . ? C5 C4 H4 118.6 . . ? C4 C5 C6 117.7(5) . . ? C4 C5 H5 121.2 . . ? C6 C5 H5 121.2 . . ? C5 C6 C7 121.0(5) . . ? C5 C6 H6 119.5 . . ? C7 C6 H6 119.5 . . ? C2 C7 C6 119.0(5) . . ? C2 C7 C8 121.6(4) . . ? C6 C7 C8 119.5(5) . . ? N2 C8 C7 112.2(3) . . ? N2 C8 H8A 109.2 . . ? C7 C8 H8A 109.2 . . ? N2 C8 H8B 109.2 . . ? C7 C8 H8B 109.2 . . ? H8A C8 H8B 107.9 . . ? C10 C9 N2 107.0(4) . . ? C10 C9 H9 126.5 . . ? N2 C9 H9 126.5 . . ? C9 C10 N3 108.1(4) . . ? C9 C10 H10 125.9 . . ? N3 C10 H10 125.9 . . ? N3 C11 N2 104.1(3) . . ? N3 C11 Ni1 135.9(3) . . ? N2 C11 Ni1 120.0(3) . . ? C13 C12 C15 111.9(7) . . ? C13 C12 N3 112.5(5) . . ? C15' C12 N3 114.6(12) . . ? C15 C12 N3 110.6(5) . . ? C15' C12 C14' 112.1(16) . . ? N3 C12 C14' 103.9(9) . . ? C13 C12 C14 111.5(8) . . ? C15 C12 C14 104.4(7) . . ? N3 C12 C14 105.4(5) . . ? C15' C12 C13' 113.1(16) . . ? N3 C12 C13' 106.0(7) . . ? C14' C12 C13' 106.4(15) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C12 C13' H13D 109.5 . . ? C12 C13' H13E 109.5 . . ? H13D C13' H13E 109.5 . . ? C12 C13' H13F 109.5 . . ? H13D C13' H13F 109.5 . . ? H13E C13' H13F 109.5 . . ? C12 C14' H14D 109.5 . . ? C12 C14' H14E 109.5 . . ? H14D C14' H14E 109.5 . . ? C12 C14' H14F 109.5 . . ? H14D C14' H14F 109.5 . . ? H14E C14' H14F 109.5 . . ? C12 C15' H15D 109.5 . . ? C12 C15' H15E 109.5 . . ? H15D C15' H15E 109.5 . . ? C12 C15' H15F 109.5 . . ? H15D C15' H15F 109.5 . . ? H15E C15' H15F 109.5 . . ? _refine_diff_density_max 0.415 _refine_diff_density_min -0.267 _refine_diff_density_rms 0.064 _shelxl_version_number 2013-2 _shelx_res_file ; TITL a20106a in P2(1)/c CELL 0.71073 10.2920 13.5100 12.2613 90.000 111.141 90.000 ZERR 2.00 0.0058 0.0075 0.0069 0.000 0.008 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N Ni Br UNIT 60 84 12 2 4 OMIT -3.00 52.02 L.S. 10 ACTA BOND $H FMAP 2 PLAN 4 isor 0.01 c15' dfix 1.5 0.01 c12 c15' c12 c13 size 0.25 0.15 0.10 TEMP 20 WGHT 0.048000 FVAR 0.34763 0.70227 NI1 4 0.000000 0.500000 1.000000 10.50000 0.05619 0.05995 = 0.05864 -0.00465 0.02153 -0.00582 BR1 5 0.185103 0.466773 1.172675 11.00000 0.08306 0.08414 = 0.07478 0.00265 0.00695 -0.00127 N1 3 -0.347986 0.280964 0.778024 11.00000 0.11294 0.08784 = 0.12084 0.00743 0.04133 -0.01142 AFIX 43 H1D 2 -0.294593 0.331566 0.802154 11.00000 -1.20000 AFIX 0 N2 3 -0.030125 0.291487 0.948199 11.00000 0.08210 0.06037 = 0.07874 -0.01062 0.04298 -0.01049 N3 3 0.120795 0.346123 0.878938 11.00000 0.06921 0.06811 = 0.07438 -0.00550 0.03717 -0.00586 C1 1 -0.445950 0.280011 0.661107 11.00000 0.11624 0.13216 = 0.14173 0.02096 0.05366 0.01565 AFIX 137 H1A 2 -0.434095 0.220706 0.622577 11.00000 -1.50000 H1B 2 -0.431018 0.336676 0.619853 11.00000 -1.50000 H1C 2 -0.538757 0.282009 0.662097 11.00000 -1.50000 AFIX 0 C2 1 -0.336480 0.203858 0.852803 11.00000 0.08774 0.07087 = 0.11658 -0.00394 0.06418 -0.00422 C3 1 -0.431290 0.125292 0.817984 11.00000 0.08265 0.09163 = 0.11727 -0.01801 0.05398 -0.02444 AFIX 43 H3 2 -0.503941 0.127212 0.745856 11.00000 -1.20000 AFIX 0 C4 1 -0.417015 0.047446 0.888829 11.00000 0.11934 0.09880 = 0.13492 -0.01773 0.07972 -0.03229 AFIX 43 H4 2 -0.479152 -0.005006 0.863206 11.00000 -1.20000 AFIX 0 C5 1 -0.314130 0.041645 0.998202 11.00000 0.14077 0.08596 = 0.12548 0.00613 0.08269 -0.02441 AFIX 43 H5 2 -0.306310 -0.013385 1.045725 11.00000 -1.20000 AFIX 0 C6 1 -0.222654 0.120779 1.034903 11.00000 0.11253 0.09865 = 0.10088 0.00994 0.06086 -0.01405 AFIX 43 H6 2 -0.153853 0.119613 1.109117 11.00000 -1.20000 AFIX 0 C7 1 -0.232332 0.202192 0.962058 11.00000 0.08420 0.07998 = 0.08594 -0.00755 0.04777 -0.01021 C8 1 -0.133115 0.286966 1.005530 11.00000 0.08976 0.08381 = 0.07987 -0.01551 0.05128 -0.02136 AFIX 23 H8A 2 -0.185317 0.348421 0.991463 11.00000 -1.20000 H8B 2 -0.084894 0.280287 1.089260 11.00000 -1.20000 AFIX 0 C9 1 0.016467 0.211430 0.903264 11.00000 0.10704 0.06264 = 0.09643 -0.01805 0.05370 -0.01191 AFIX 43 H9 2 -0.011801 0.146011 0.902923 11.00000 -1.20000 AFIX 0 C10 1 0.108992 0.245182 0.860700 11.00000 0.09536 0.07238 = 0.10237 -0.01690 0.05816 -0.00135 AFIX 43 H10 2 0.157694 0.207483 0.824712 11.00000 -1.20000 AFIX 0 C11 1 0.035988 0.376274 0.935696 11.00000 0.05648 0.06671 = 0.05993 -0.00257 0.02422 -0.00441 C12 1 0.218103 0.405690 0.840005 11.00000 0.08248 0.08975 = 0.08815 -0.00832 0.04875 -0.01557 PART 1 C13 1 0.214515 0.511941 0.866291 21.00000 0.12886 0.10314 = 0.21163 -0.02104 0.12569 -0.03058 AFIX 33 H13A 2 0.134797 0.542058 0.808486 21.00000 -1.50000 H13B 2 0.297820 0.543252 0.865313 21.00000 -1.50000 H13C 2 0.208591 0.519686 0.942188 21.00000 -1.50000 AFIX 0 C14 1 0.172167 0.387120 0.706525 21.00000 0.15020 0.19806 = 0.09242 -0.03628 0.07365 -0.08179 AFIX 33 H14A 2 0.072506 0.381969 0.673175 21.00000 -1.50000 H14B 2 0.213150 0.326706 0.693056 21.00000 -1.50000 H14C 2 0.202421 0.441194 0.670748 21.00000 -1.50000 AFIX 0 C15 1 0.360806 0.364989 0.889096 21.00000 0.07013 0.14576 = 0.21541 0.00911 0.05653 0.01230 AFIX 33 H15A 2 0.371975 0.314601 0.837968 21.00000 -1.50000 H15B 2 0.376135 0.336915 0.964655 21.00000 -1.50000 H15C 2 0.427007 0.417011 0.896556 21.00000 -1.50000 PART 2 AFIX 0 C13' 1 0.337259 0.438059 0.952509 -21.00000 0.06150 0.23875 = 0.10743 0.01684 0.02941 -0.07628 AFIX 33 H13D 2 0.300723 0.450092 1.013116 -21.00000 -1.50000 H13E 2 0.379048 0.497565 0.937576 -21.00000 -1.50000 H13F 2 0.406188 0.386673 0.976876 -21.00000 -1.50000 AFIX 0 C14' 1 0.135449 0.498909 0.788368 -21.00000 0.09952 0.08827 = 0.09969 0.05090 0.02737 -0.03385 AFIX 33 H14D 2 0.057318 0.481972 0.719545 -21.00000 -1.50000 H14E 2 0.194194 0.544931 0.768158 -21.00000 -1.50000 H14F 2 0.102763 0.528551 0.844870 -21.00000 -1.50000 AFIX 0 C15' 1 0.267916 0.354958 0.756037 -21.00000 0.13590 0.16475 = 0.18444 -0.01337 0.11330 0.00616 AFIX 33 H15D 2 0.190244 0.340671 0.685784 -21.00000 -1.50000 H15E 2 0.313280 0.294294 0.789796 -21.00000 -1.50000 H15F 2 0.332663 0.396873 0.737853 -21.00000 -1.50000 PART 0 AFIX 0 HKLF 4 REM a20106a in P2(1)/c REM R1 = 0.0419 for 1717 Fo > 4sig(Fo) and 0.0808 for all 3114 data REM 207 parameters refined using 8 restraints END WGHT 0.0483 0.0000 REM Highest difference peak 0.415, deepest hole -0.267, 1-sigma level 0.064 Q1 1 0.1161 0.4915 1.2086 11.00000 0.05 0.42 Q2 1 0.1550 0.4057 1.1206 11.00000 0.05 0.37 Q3 1 0.2135 0.5045 1.1241 11.00000 0.05 0.33 Q4 1 0.0871 0.4923 1.1169 11.00000 0.05 0.31 ; _shelx_res_checksum 42857 _shelx_hkl_file ; 4 -3 -15 6.75 5.50 5 -3 -15 0.23 4.77 3 -2 -15 -1.15 5.04 4 -2 -15 2.88 5.22 5 -2 -15 0.75 5.07 6 -2 -15 -2.33 4.72 3 -1 -15 14.55 5.56 4 -1 -15 7.80 5.37 5 -1 -15 -0.72 4.77 6 -1 -15 1.37 5.28 7 -1 -15 2.23 5.46 2 0 -15 -0.92 4.55 3 0 -15 -2.47 4.41 4 0 -15 1.33 4.77 5 0 -15 -2.30 4.63 6 0 -15 0.96 5.00 7 0 -15 0.35 4.87 2 1 -15 1.64 4.70 3 1 -15 11.66 5.06 4 1 -15 9.53 5.16 5 1 -15 0.75 4.73 6 1 -15 1.21 4.99 7 1 -15 2.78 5.20 3 2 -15 1.41 4.21 4 2 -15 0.78 4.45 5 2 -15 0.34 4.50 6 2 -15 0.25 4.75 7 2 -15 0.05 4.99 4 3 -15 2.75 4.66 5 3 -15 -0.73 4.70 6 3 -15 2.72 5.03 7 3 -15 4.23 5.35 4 4 -15 5.48 4.70 5 4 -15 2.46 4.71 6 4 -15 0.54 4.91 7 4 -15 2.67 5.00 5 5 -15 3.93 4.83 6 5 -15 2.68 4.90 5 -6 -14 2.51 6.27 6 -6 -14 3.61 5.58 7 -6 -14 1.69 5.40 4 -5 -14 0.76 5.26 5 -5 -14 -4.69 4.76 6 -5 -14 -0.96 5.97 7 -5 -14 2.83 5.66 8 -5 -14 -2.60 5.73 4 -4 -14 -2.21 4.44 5 -4 -14 6.49 5.26 6 -4 -14 -0.13 5.07 7 -4 -14 2.00 6.25 8 -4 -14 3.70 6.20 3 -3 -14 1.35 4.66 4 -3 -14 -2.61 3.92 5 -3 -14 -1.64 4.59 6 -3 -14 3.60 5.22 7 -3 -14 2.17 5.59 8 -3 -14 1.52 5.65 3 -2 -14 8.64 4.80 4 -2 -14 4.81 4.61 5 -2 -14 2.27 4.59 6 -2 -14 5.15 5.11 7 -2 -14 6.09 5.71 8 -2 -14 15.42 6.83 9 -2 -14 7.61 6.86 2 -1 -14 0.06 4.30 3 -1 -14 -2.86 3.94 4 -1 -14 1.02 4.43 5 -1 -14 2.80 4.57 6 -1 -14 -0.47 4.27 7 -1 -14 -0.16 4.80 8 -1 -14 -0.34 5.56 9 -1 -14 -2.03 6.41 2 0 -14 21.54 5.56 3 0 -14 15.67 5.10 4 0 -14 0.79 4.38 5 0 -14 4.38 4.78 6 0 -14 2.66 4.27 7 0 -14 6.50 5.00 8 0 -14 3.31 5.54 9 0 -14 -0.78 6.18 2 1 -14 -1.06 3.70 3 1 -14 0.28 3.96 4 1 -14 1.62 4.44 5 1 -14 0.47 4.20 6 1 -14 1.66 4.39 7 1 -14 0.13 4.53 8 1 -14 0.24 4.76 9 1 -14 -1.99 5.28 2 2 -14 16.37 4.90 3 2 -14 12.29 4.71 4 2 -14 3.66 4.54 5 2 -14 0.19 4.20 6 2 -14 3.92 4.35 7 2 -14 12.20 5.25 8 2 -14 11.83 6.18 3 3 -14 -1.09 3.99 4 3 -14 0.76 4.21 5 3 -14 -0.45 4.05 6 3 -14 -1.29 4.14 7 3 -14 2.05 5.18 8 3 -14 0.41 5.58 4 4 -14 2.98 4.27 5 4 -14 -0.57 4.09 6 4 -14 0.25 4.04 7 4 -14 2.50 6.09 8 4 -14 -0.09 6.20 5 5 -14 0.02 4.03 6 5 -14 6.03 5.24 7 5 -14 -0.21 5.68 8 5 -14 4.98 6.06 5 6 -14 7.15 4.78 6 6 -14 3.26 5.51 7 6 -14 4.30 6.27 6 7 -14 -4.18 5.30 7 7 -14 1.08 5.61 5 -9 -13 8.21 6.47 6 -9 -13 6.74 6.22 7 -9 -13 -2.49 5.54 6 -8 -13 -0.67 3.69 7 -8 -13 1.52 3.80 8 -8 -13 1.30 4.23 5 -7 -13 3.02 5.37 6 -7 -13 5.24 3.61 7 -7 -13 0.80 3.51 8 -7 -13 0.01 5.51 9 -7 -13 1.85 5.87 4 -6 -13 2.06 4.81 5 -6 -13 7.74 5.35 6 -6 -13 5.45 3.47 7 -6 -13 0.43 4.90 8 -6 -13 0.72 5.58 9 -6 -13 -0.45 6.03 4 -5 -13 -2.94 3.88 5 -5 -13 2.94 4.79 6 -5 -13 3.12 5.04 7 -5 -13 6.15 5.12 8 -5 -13 6.66 5.94 9 -5 -13 2.89 5.93 10 -5 -13 -0.40 5.90 3 -4 -13 5.81 4.88 4 -4 -13 3.31 4.52 5 -4 -13 1.73 4.67 6 -4 -13 1.76 4.97 7 -4 -13 4.50 5.37 8 -4 -13 0.91 4.95 9 -4 -13 -1.38 6.13 10 -4 -13 3.59 6.63 3 -3 -13 -1.43 4.01 4 -3 -13 -2.74 3.65 5 -3 -13 -0.81 3.44 6 -3 -13 16.91 5.93 7 -3 -13 12.91 5.67 8 -3 -13 2.91 5.43 9 -3 -13 1.53 5.75 10 -3 -13 0.58 6.85 2 -2 -13 1.86 4.04 3 -2 -13 2.25 4.12 4 -2 -13 -0.48 4.01 5 -2 -13 2.52 4.74 6 -2 -13 -2.29 4.25 7 -2 -13 1.24 4.67 8 -2 -13 1.02 5.29 9 -2 -13 4.34 6.21 10 -2 -13 2.53 7.87 2 -1 -13 29.76 5.88 3 -1 -13 2.14 3.96 4 -1 -13 0.93 4.17 5 -1 -13 10.47 4.89 6 -1 -13 15.41 5.58 7 -1 -13 17.87 6.06 8 -1 -13 4.15 5.69 9 -1 -13 0.86 5.32 10 -1 -13 0.97 5.37 1 0 -13 -2.51 3.89 2 0 -13 0.77 3.93 3 0 -13 0.89 3.81 4 0 -13 1.16 4.02 5 0 -13 -1.04 3.76 6 0 -13 -0.54 4.12 7 0 -13 1.82 4.82 8 0 -13 0.55 4.88 9 0 -13 1.55 5.12 10 0 -13 0.67 5.15 1 1 -13 39.01 6.64 2 1 -13 23.36 5.28 3 1 -13 0.58 3.84 4 1 -13 1.14 4.18 5 1 -13 5.68 4.47 6 1 -13 10.53 4.79 7 1 -13 21.74 6.24 8 1 -13 3.80 5.14 9 1 -13 -2.11 4.97 10 1 -13 -1.44 5.32 1 2 -13 2.66 3.77 2 2 -13 1.14 3.88 3 2 -13 -0.96 4.12 4 2 -13 -3.42 3.53 5 2 -13 1.41 4.10 6 2 -13 2.80 3.91 7 2 -13 -0.86 4.87 8 2 -13 0.49 5.23 9 2 -13 -1.66 5.08 10 2 -13 3.99 6.10 2 3 -13 20.92 5.30 3 3 -13 -0.28 3.67 4 3 -13 3.87 3.95 5 3 -13 1.50 4.06 6 3 -13 20.24 5.91 7 3 -13 15.95 6.00 8 3 -13 5.48 5.18 9 3 -13 0.66 5.07 3 4 -13 2.33 4.21 4 4 -13 2.54 3.95 5 4 -13 0.18 3.76 6 4 -13 3.64 5.07 7 4 -13 -1.11 4.89 8 4 -13 -0.42 5.08 9 4 -13 1.29 5.79 4 5 -13 0.44 4.10 5 5 -13 1.15 4.50 6 5 -13 2.64 4.87 7 5 -13 6.21 5.13 8 5 -13 8.28 5.97 9 5 -13 -0.41 5.83 5 6 -13 7.80 4.92 6 6 -13 4.92 5.12 7 6 -13 0.14 4.97 8 6 -13 -4.52 5.13 9 6 -13 2.91 5.62 6 7 -13 4.30 5.17 7 7 -13 2.92 5.29 8 7 -13 -0.69 5.52 7 8 -13 -1.68 4.91 8 8 -13 2.84 5.37 4 -10 -12 0.68 5.31 5 -10 -12 -0.83 5.55 6 -10 -12 -1.34 5.38 7 -10 -12 5.08 6.62 4 -9 -12 3.69 5.16 5 -9 -12 1.82 5.07 6 -9 -12 0.31 5.18 7 -9 -12 4.49 4.01 8 -9 -12 -0.23 3.91 5 -8 -12 6.10 5.20 6 -8 -12 3.25 3.57 7 -8 -12 4.46 3.66 8 -8 -12 8.11 4.07 9 -8 -12 2.71 3.92 5 -7 -12 2.79 3.51 6 -7 -12 1.08 3.31 7 -7 -12 -0.03 3.33 8 -7 -12 3.85 3.42 9 -7 -12 3.46 5.98 10 -7 -12 2.72 6.21 4 -6 -12 3.33 4.90 5 -6 -12 5.35 3.27 6 -6 -12 9.79 3.76 7 -6 -12 10.52 3.75 8 -6 -12 6.43 5.50 9 -6 -12 0.02 5.34 10 -6 -12 -1.88 5.66 3 -5 -12 -0.56 3.45 4 -5 -12 4.42 4.67 5 -5 -12 -0.51 2.87 6 -5 -12 2.89 3.09 7 -5 -12 2.26 5.26 8 -5 -12 1.93 5.47 9 -5 -12 1.13 5.15 10 -5 -12 1.10 5.91 3 -4 -12 3.56 4.38 4 -4 -12 -1.74 4.27 5 -4 -12 8.18 5.01 6 -4 -12 12.58 3.35 7 -4 -12 2.29 4.95 8 -4 -12 1.83 5.23 9 -4 -12 -2.15 5.38 10 -4 -12 1.90 6.30 11 -4 -12 2.70 7.49 2 -3 -12 7.38 4.54 3 -3 -12 0.06 3.93 4 -3 -12 24.69 5.78 5 -3 -12 8.89 5.15 6 -3 -12 1.32 4.75 7 -3 -12 6.76 5.08 8 -3 -12 -0.18 5.09 9 -3 -12 -0.51 5.96 10 -3 -12 -1.68 7.10 11 -3 -12 -0.55 5.51 2 -2 -12 2.36 3.77 3 -2 -12 2.65 4.02 4 -2 -12 4.74 4.54 5 -2 -12 26.34 6.03 6 -2 -12 39.63 6.82 7 -2 -12 7.89 5.27 8 -2 -12 2.03 5.61 9 -2 -12 3.92 4.89 10 -2 -12 8.19 5.54 11 -2 -12 2.43 5.54 1 -1 -12 0.69 3.88 2 -1 -12 -1.22 3.29 3 -1 -12 6.09 4.14 4 -1 -12 2.10 4.27 5 -1 -12 3.33 4.42 6 -1 -12 6.72 4.92 7 -1 -12 5.43 4.98 8 -1 -12 0.85 4.31 9 -1 -12 0.65 4.61 10 -1 -12 -2.19 4.52 11 -1 -12 0.76 5.13 1 0 -12 29.74 5.66 2 0 -12 4.54 3.77 3 0 -12 0.15 3.89 4 0 -12 -0.35 3.78 5 0 -12 45.80 6.24 6 0 -12 48.53 6.93 7 0 -12 8.66 4.98 8 0 -12 -0.34 4.51 9 0 -12 2.39 4.71 10 0 -12 3.30 4.77 11 0 -12 6.21 5.63 1 1 -12 -1.08 3.38 2 1 -12 -0.19 3.66 3 1 -12 4.65 4.13 4 1 -12 -0.35 3.73 5 1 -12 6.80 4.38 6 1 -12 10.58 5.28 7 1 -12 3.37 4.95 8 1 -12 -3.07 4.20 9 1 -12 1.76 3.84 10 1 -12 1.82 5.05 11 1 -12 1.57 5.59 1 2 -12 41.88 5.77 2 2 -12 0.37 3.80 3 2 -12 2.33 3.80 4 2 -12 5.67 4.13 5 2 -12 20.80 5.10 6 2 -12 46.09 7.27 7 2 -12 14.18 5.61 8 2 -12 7.89 5.16 9 2 -12 5.02 5.08 10 2 -12 10.66 5.83 11 2 -12 2.65 5.22 1 3 -12 2.47 3.63 2 3 -12 7.65 4.20 3 3 -12 0.03 3.64 4 3 -12 21.81 5.11 5 3 -12 9.64 4.93 6 3 -12 -0.45 4.62 7 3 -12 -1.18 4.37 8 3 -12 -1.87 4.80 9 3 -12 1.86 5.10 10 3 -12 -0.17 4.76 2 4 -12 0.87 3.77 3 4 -12 2.88 4.12 4 4 -12 -0.91 3.65 5 4 -12 6.69 4.85 6 4 -12 17.99 5.62 7 4 -12 5.54 5.15 8 4 -12 -1.17 4.58 9 4 -12 -2.02 4.30 10 4 -12 0.93 6.96 3 5 -12 2.34 4.18 4 5 -12 3.87 4.32 5 5 -12 -0.84 4.79 6 5 -12 2.59 4.68 7 5 -12 4.45 5.32 8 5 -12 0.63 4.38 9 5 -12 0.42 6.58 10 5 -12 3.79 6.50 4 6 -12 5.98 4.45 5 6 -12 9.47 4.80 6 6 -12 15.90 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9 1 0 0.93 2.78 10 1 0 2.62 4.42 11 1 0 1.33 4.85 0 2 0 141.98 3.23 1 2 0 365.29 6.76 2 2 0 601.24 10.55 3 2 0 432.58 10.12 4 2 0 192.40 7.51 5 2 0 840.12 11.80 6 2 0 284.91 7.50 7 2 0 6.27 2.53 8 2 0 29.59 3.66 9 2 0 0.27 2.95 10 2 0 36.89 4.68 -1 3 0 1312.12 12.92 0 3 0 -0.08 0.82 1 3 0 1300.76 15.50 2 3 0 222.73 6.91 3 3 0 29.42 3.38 4 3 0 92.67 5.73 5 3 0 44.95 4.82 6 3 0 110.75 5.13 7 3 0 82.70 4.93 8 3 0 -0.73 2.52 9 3 0 1.75 2.94 10 3 0 1.44 3.25 11 3 0 3.42 4.67 -2 4 0 3.62 1.17 -1 4 0 649.88 8.61 0 4 0 2104.03 20.28 1 4 0 663.85 11.53 2 4 0 5.50 2.17 3 4 0 3.68 2.45 4 4 0 46.55 4.76 5 4 0 211.64 9.65 6 4 0 229.52 7.08 7 4 0 20.98 3.47 8 4 0 1.39 2.69 9 4 0 4.60 3.03 10 4 0 17.39 5.77 11 4 0 9.33 5.34 -3 5 0 151.29 3.56 -2 5 0 497.52 7.17 -1 5 0 187.34 5.00 0 5 0 0.44 1.59 1 5 0 183.64 6.44 2 5 0 496.02 11.86 3 5 0 149.31 7.38 4 5 0 445.21 13.41 5 5 0 14.93 3.62 6 5 0 49.93 5.94 7 5 0 24.48 8.67 8 5 0 0.90 2.64 9 5 0 21.59 5.40 10 5 0 9.20 5.37 11 5 0 1.78 5.00 -3 6 0 8.45 1.45 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-5 11 3.39 4.56 -5 -5 11 2.21 4.29 -4 -5 11 15.06 5.13 -3 -5 11 0.90 3.98 -2 -5 11 0.30 4.36 -1 -5 11 3.68 4.40 0 -5 11 29.32 6.47 2 -5 11 4.88 5.34 3 -5 11 -3.11 4.82 4 -5 11 -0.43 5.75 -4 -4 11 6.74 4.83 -3 -4 11 16.50 4.85 -2 -4 11 3.17 3.88 -1 -4 11 37.57 6.54 1 -4 11 5.75 5.04 2 -4 11 13.12 6.15 3 -4 11 0.04 5.76 4 -4 11 5.82 6.63 5 -4 11 0.98 6.56 -2 -3 11 3.60 3.60 -1 -3 11 12.06 4.50 0 -3 11 63.87 7.80 1 -3 11 51.43 6.82 2 -3 11 9.70 5.57 3 -3 11 5.17 6.19 4 -3 11 0.31 5.72 5 -3 11 5.90 7.10 -1 -2 11 3.72 4.10 2 -2 11 7.27 5.00 3 -2 11 4.82 5.76 4 -2 11 0.09 5.78 5 -2 11 -0.62 6.37 1 -1 11 57.08 6.19 3 -1 11 7.34 5.80 4 -1 11 2.16 5.54 5 -1 11 10.36 7.26 0 0 11 -0.58 3.11 1 0 11 1.40 3.37 2 0 11 -0.81 3.45 4 0 11 -0.70 5.66 5 0 11 -0.96 6.35 0 1 11 60.41 6.77 1 1 11 52.81 6.50 2 1 11 4.15 3.87 3 1 11 3.96 3.69 5 1 11 7.15 6.47 0 2 11 -0.38 3.54 1 2 11 -0.54 3.49 2 2 11 4.62 4.18 3 2 11 1.55 3.72 -1 3 11 8.44 4.19 0 3 11 45.85 6.41 1 3 11 41.46 6.25 2 3 11 4.37 4.06 3 3 11 -0.27 3.74 4 3 11 -3.34 3.54 -1 4 11 23.61 5.43 0 4 11 2.07 3.97 1 4 11 4.69 4.43 2 4 11 8.17 4.34 3 4 11 1.17 4.10 4 4 11 4.39 4.32 5 4 11 2.83 5.25 -2 5 11 -0.36 3.91 -1 5 11 0.75 3.79 0 5 11 18.84 5.06 1 5 11 19.46 5.68 2 5 11 1.84 3.91 3 5 11 0.86 4.08 4 5 11 0.07 4.30 -3 6 11 6.02 4.75 -2 6 11 1.17 4.19 -1 6 11 14.22 5.34 0 6 11 1.51 4.12 1 6 11 1.87 4.48 2 6 11 19.89 5.55 3 6 11 -0.87 4.06 4 6 11 3.59 4.83 -3 7 11 15.66 5.62 -2 7 11 13.89 5.28 -1 7 11 4.85 4.59 0 7 11 5.71 4.81 1 7 11 6.64 4.48 2 7 11 0.36 4.40 3 7 11 0.19 4.55 -4 8 11 8.83 4.91 -3 8 11 12.38 5.36 -2 8 11 -1.52 4.28 -1 8 11 20.94 6.54 0 8 11 4.48 5.12 1 8 11 6.08 5.03 2 8 11 9.54 5.46 3 8 11 0.04 4.91 -5 9 11 0.46 4.65 -4 9 11 3.72 4.82 -3 9 11 5.10 5.40 -2 9 11 8.59 5.24 -1 9 11 7.70 5.61 0 9 11 -0.36 4.52 1 9 11 1.70 4.93 2 9 11 -0.10 5.20 -6 10 11 4.28 5.12 -5 10 11 1.22 4.68 -4 10 11 -1.59 4.84 -3 10 11 3.97 5.25 -2 10 11 -0.51 5.05 -1 10 11 -1.16 5.22 0 10 11 -1.10 4.62 1 10 11 0.87 5.34 -6 11 11 7.32 5.73 -5 11 11 1.90 5.40 -4 11 11 0.27 4.77 -3 11 11 7.31 6.00 -2 11 11 16.92 7.09 -1 11 11 3.28 5.52 -5 12 11 2.03 5.80 -4 12 11 0.54 6.10 -3 12 11 -0.05 5.80 -2 12 11 -1.76 5.18 -5 -11 12 1.77 6.47 -4 -11 12 1.27 6.36 -3 -11 12 -0.35 6.93 -7 -10 12 1.30 5.62 -6 -10 12 0.62 5.40 -5 -10 12 0.74 5.93 -4 -10 12 0.41 6.22 -3 -10 12 0.76 6.94 -2 -10 12 10.71 7.13 -1 -10 12 3.49 6.43 -8 -9 12 -0.72 4.99 -7 -9 12 -1.84 4.48 -6 -9 12 0.80 5.36 -5 -9 12 0.94 5.75 -4 -9 12 5.70 6.35 -3 -9 12 -0.49 5.57 -2 -9 12 1.29 5.96 -1 -9 12 2.31 5.80 0 -9 12 4.14 6.31 -7 -8 12 4.80 5.19 -6 -8 12 0.29 4.86 -5 -8 12 1.86 5.74 -4 -8 12 4.82 5.50 -2 -8 12 9.30 5.47 -1 -8 12 3.00 5.31 0 -8 12 5.44 5.73 1 -8 12 3.15 5.94 -6 -7 12 -5.19 4.35 -5 -7 12 5.08 5.39 -4 -7 12 12.74 5.82 -3 -7 12 3.43 5.02 -2 -7 12 8.98 5.44 -1 -7 12 8.32 5.47 0 -7 12 1.64 5.49 1 -7 12 9.45 5.99 2 -7 12 4.71 6.04 -5 -6 12 8.27 4.97 -4 -6 12 6.28 4.91 -3 -6 12 5.02 5.05 -2 -6 12 5.91 4.93 -1 -6 12 7.62 5.14 0 -6 12 8.63 5.61 1 -6 12 0.95 5.16 -3 -5 12 -1.25 4.40 -2 -5 12 20.69 6.05 -1 -5 12 8.03 5.26 0 -5 12 5.48 4.92 -1 -4 12 27.02 6.21 2 -4 12 3.44 5.81 3 -4 12 -0.78 6.08 4 -4 12 6.20 7.53 1 -3 12 13.97 5.48 2 -3 12 4.06 5.72 3 -3 12 -0.04 5.67 4 -3 12 4.97 6.73 2 -2 12 1.58 5.18 3 -2 12 5.55 6.50 4 -2 12 9.23 7.14 0 -1 12 3.85 3.79 3 -1 12 0.42 5.24 4 -1 12 0.91 6.55 0 0 12 34.23 5.66 1 0 12 2.90 3.48 4 0 12 7.70 6.47 0 1 12 2.56 3.47 1 1 12 1.12 3.43 2 1 12 -0.51 3.58 -1 2 12 39.14 6.01 0 2 12 40.20 6.02 1 2 12 2.86 3.83 2 2 12 2.25 3.84 3 2 12 1.53 3.87 -1 3 12 2.77 4.10 0 3 12 -0.17 3.60 1 3 12 8.51 4.50 2 3 12 0.82 3.77 3 3 12 7.83 4.55 -2 4 12 4.36 4.28 -1 4 12 14.92 4.82 0 4 12 19.76 5.52 1 4 12 5.89 4.44 2 4 12 2.97 3.83 3 4 12 0.15 4.03 4 4 12 1.93 4.77 -2 5 12 16.71 5.29 -1 5 12 5.93 4.47 0 5 12 3.92 4.31 1 5 12 12.81 5.36 2 5 12 -0.52 4.06 3 5 12 -0.51 4.30 -3 6 12 1.53 4.32 -2 6 12 3.97 4.38 -1 6 12 9.24 4.95 0 6 12 2.72 4.82 1 6 12 3.01 4.24 2 6 12 1.59 4.35 3 6 12 1.29 4.75 -4 7 12 6.61 5.04 -3 7 12 0.38 4.60 -2 7 12 6.04 4.34 -1 7 12 5.65 4.83 0 7 12 1.80 4.66 1 7 12 6.73 4.76 2 7 12 1.06 4.55 -5 8 12 4.13 5.13 -4 8 12 7.43 5.63 -3 8 12 18.99 6.15 -2 8 12 6.76 5.55 -1 8 12 -0.08 4.99 0 8 12 3.05 5.24 1 8 12 1.40 5.12 -6 9 12 0.92 5.14 -5 9 12 0.67 5.24 -4 9 12 6.46 5.53 -3 9 12 4.41 5.62 -2 9 12 6.19 5.42 -1 9 12 2.30 5.50 0 9 12 -0.16 5.10 -7 10 12 0.58 5.76 -6 10 12 2.54 5.66 -5 10 12 2.14 5.50 -4 10 12 -0.79 5.36 -3 10 12 4.02 5.69 -2 10 12 4.23 6.05 -6 11 12 7.21 6.19 -5 11 12 1.57 6.54 -4 11 12 0.89 5.52 -3 11 12 -0.42 6.00 -5 -10 13 0.50 7.16 -4 -10 13 -2.94 6.72 -6 -9 13 -3.62 6.05 -5 -9 13 4.33 6.42 -4 -9 13 3.77 6.81 -3 -9 13 8.43 7.06 -2 -9 13 -0.69 6.67 -1 -9 13 -2.95 6.41 -5 -8 13 1.61 5.53 -4 -8 13 -2.82 5.28 -3 -8 13 1.69 5.95 -2 -8 13 2.72 6.00 -1 -8 13 2.61 6.06 0 -8 13 5.38 6.40 -3 -7 13 11.46 6.08 -2 -7 13 7.29 5.42 -1 -7 13 3.45 5.59 0 -7 13 3.45 6.21 1 -7 13 -1.82 5.38 -2 -6 13 3.09 4.91 -1 -6 13 5.83 5.48 0 -6 13 7.35 5.69 1 -6 13 2.69 5.47 0 -5 13 4.26 4.91 1 -5 13 5.18 5.59 1 -2 13 5.59 5.26 2 -2 13 0.95 5.45 3 -2 13 2.40 7.12 0 -1 13 4.79 3.61 2 -1 13 4.47 6.43 3 -1 13 2.54 6.33 -1 0 13 1.59 3.55 0 0 13 1.43 3.37 3 0 13 5.81 7.27 0 1 13 2.98 3.63 1 1 13 -0.57 3.44 -1 2 13 4.18 4.24 0 2 13 2.63 3.95 1 2 13 2.31 4.01 2 2 13 0.16 3.77 -2 3 13 14.69 5.22 -1 3 13 14.34 4.76 0 3 13 -0.55 3.75 1 3 13 -0.25 3.78 2 3 13 3.50 4.30 -2 4 13 6.84 4.53 -1 4 13 1.12 3.92 0 4 13 0.25 3.66 1 4 13 0.38 4.28 2 4 13 1.64 4.42 -3 5 13 2.47 4.42 -2 5 13 1.69 4.04 -1 5 13 6.97 4.50 0 5 13 -0.16 3.93 1 5 13 -1.69 4.42 2 5 13 -0.30 4.79 -3 6 13 3.99 4.71 -2 6 13 1.20 4.11 -1 6 13 1.27 4.80 0 6 13 4.36 5.00 1 6 13 -0.22 4.53 -4 7 13 9.78 5.36 -3 7 13 7.13 5.17 -2 7 13 10.27 5.58 -1 7 13 3.02 5.62 0 7 13 -0.61 5.08 -5 8 13 2.85 5.66 -4 8 13 1.52 5.48 -3 8 13 5.03 5.41 -2 8 13 3.80 5.28 -6 9 13 2.90 5.89 -5 9 13 2.81 5.83 -4 9 13 6.11 6.07 -3 9 13 2.20 5.76 -1 -1 14 4.05 4.25 -1 0 14 6.74 4.16 0 0 14 2.47 3.80 -1 1 14 1.79 4.03 0 1 14 -0.91 3.81 -2 2 14 15.06 5.24 -1 2 14 1.91 3.83 0 2 14 -1.82 3.73 1 2 14 1.91 4.48 -2 3 14 0.57 3.88 -1 3 14 0.05 4.03 0 3 14 5.60 4.37 1 3 14 1.62 4.69 -3 4 14 2.77 4.64 -2 4 14 1.23 4.28 -1 4 14 1.07 4.46 0 4 14 -1.40 4.45 -3 5 14 3.73 5.19 -2 5 14 -0.95 3.99 -1 5 14 0.92 4.69 -4 6 14 1.71 5.00 -3 6 14 3.04 5.19 -2 6 14 1.37 4.88 -5 7 14 3.21 5.72 -4 7 14 0.28 5.51 -1 0 15 -1.53 4.12 -2 1 15 4.80 4.84 -1 1 15 -2.36 3.99 -2 2 15 0.69 4.59 -1 2 15 -2.21 4.17 -3 3 15 7.92 5.43 -2 3 15 -0.91 4.60 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 62738 _database_code_depnum_ccdc_archive 'CCDC 877558' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_a01009b _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H46 Cl2 N6 Ni' _chemical_formula_weight 740.44 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' Ni Ni 0.3393 1.1124 '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' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 21/c' _space_group_name_Hall '-P 2ybc' _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+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 21.256(9) _cell_length_b 8.957(4) _cell_length_c 19.814(8) _cell_angle_alpha 90 _cell_angle_beta 95.989(6) _cell_angle_gamma 90 _cell_volume 3752(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 950 _cell_measurement_theta_min 2.370 _cell_measurement_theta_max 20.476 _exptl_crystal_description block _exptl_crystal_colour pink _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.311 _exptl_crystal_F_000 1560 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.120 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.080 _exptl_absorpt_coefficient_mu 0.696 _shelx_estimated_absorpt_T_min 0.921 _shelx_estimated_absorpt_T_max 0.946 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.704881 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source ? _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 16480 _diffrn_reflns_av_unetI/netI 0.0959 _diffrn_reflns_av_R_equivalents 0.0635 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.927 _diffrn_reflns_theta_max 26.010 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.996 _diffrn_reflns_point_group_measured_fraction_full 0.998 _reflns_number_total 7348 _reflns_number_gt 4381 _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 SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0452P)^2^] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 7348 _refine_ls_number_parameters 442 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1009 _refine_ls_R_factor_gt 0.0533 _refine_ls_wR_factor_ref 0.1174 _refine_ls_wR_factor_gt 0.1029 _refine_ls_goodness_of_fit_ref 0.908 _refine_ls_restrained_S_all 0.908 _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 Ni1 Ni 0.25818(2) 0.48882(5) 0.48338(2) 0.03479(14) Uani 1 1 d . . . . . Cl1 Cl 0.25765(5) 0.28866(10) 0.41791(5) 0.0531(3) Uani 1 1 d . . . . . Cl2 Cl 0.26228(6) 0.34126(12) 0.57375(5) 0.0689(4) Uani 1 1 d . . . . . N1 N 0.33942(19) 0.2980(4) 0.29047(19) 0.0789(12) Uani 1 1 d . . . . . H1A H 0.3168 0.3200 0.3226 0.095 Uiso 1 1 calc R U . . . N2 N 0.1610(2) 0.4280(6) 0.6819(2) 0.0924(15) Uani 1 1 d . . . . . H2B H 0.1878 0.4297 0.6523 0.111 Uiso 1 1 calc R U . . . N3 N 0.29803(13) 0.6176(3) 0.36163(13) 0.0358(7) Uani 1 1 d . . . . . N4 N 0.20309(13) 0.6857(3) 0.37379(13) 0.0373(7) Uani 1 1 d . . . . . N5 N 0.30668(14) 0.7542(3) 0.55917(14) 0.0395(7) Uani 1 1 d . . . . . N6 N 0.21127(14) 0.7003(3) 0.57520(14) 0.0408(8) Uani 1 1 d . . . . . C1 C 0.25301(16) 0.6073(4) 0.40459(16) 0.0315(8) Uani 1 1 d . . . . . C2 C 0.21807(19) 0.7426(5) 0.31235(19) 0.0568(12) Uani 1 1 d . . . . . H2A H 0.1916 0.7985 0.2817 0.068 Uiso 1 1 calc R U . . . C3 C 0.27694(19) 0.7026(4) 0.30546(18) 0.0526(11) Uani 1 1 d . . . . . H3A H 0.2999 0.7271 0.2696 0.063 Uiso 1 1 calc R U . . . C4 C 0.36283(16) 0.5569(4) 0.37485(17) 0.0391(9) Uani 1 1 d . . . . . H4A H 0.3613 0.4630 0.3990 0.047 Uiso 1 1 calc R U . . . H4B H 0.3886 0.6258 0.4037 0.047 Uiso 1 1 calc R U . . . C5 C 0.39325(17) 0.5320(4) 0.31033(18) 0.0422(9) Uani 1 1 d . . . . . C6 C 0.43546(19) 0.6360(5) 0.2901(2) 0.0576(11) Uani 1 1 d . . . . . H6A H 0.4452 0.7197 0.3170 0.069 Uiso 1 1 calc R U . . . C7 C 0.4638(2) 0.6182(6) 0.2302(2) 0.0680(13) Uani 1 1 d . . . . . H7A H 0.4919 0.6894 0.2169 0.082 Uiso 1 1 calc R U . . . C8 C 0.4497(2) 0.4950(6) 0.1917(2) 0.0713(14) Uani 1 1 d . . . . . H8A H 0.4683 0.4830 0.1515 0.086 Uiso 1 1 calc R U . . . C9 C 0.4092(2) 0.3883(5) 0.2103(2) 0.0644(13) Uani 1 1 d . . . . . H9A H 0.4009 0.3047 0.1830 0.077 Uiso 1 1 calc R U . . . C10 C 0.37948(19) 0.4033(5) 0.27060(19) 0.0512(10) Uani 1 1 d . . . . . C11 C 0.3326(2) 0.1516(5) 0.2608(2) 0.0829(15) Uani 1 1 d . . . . . H11A H 0.3015 0.0963 0.2823 0.124 Uiso 1 1 calc R U . . . H11B H 0.3724 0.1003 0.2671 0.124 Uiso 1 1 calc R U . . . H11C H 0.3192 0.1605 0.2132 0.124 Uiso 1 1 calc R U . . . C12 C 0.14029(17) 0.7014(4) 0.39522(17) 0.0367(9) Uani 1 1 d . . . . . C13 C 0.12282(17) 0.8380(4) 0.42019(18) 0.0398(9) Uani 1 1 d . . . . . C14 C 0.06108(18) 0.8513(4) 0.43660(18) 0.0471(10) Uani 1 1 d . . . . . H14A H 0.0481 0.9429 0.4524 0.057 Uiso 1 1 calc R U . . . C15 C 0.01826(18) 0.7355(5) 0.4305(2) 0.0495(10) Uani 1 1 d . . . . . C16 C 0.03769(18) 0.6033(4) 0.40408(19) 0.0508(10) Uani 1 1 d . . . . . H16A H 0.0093 0.5240 0.3991 0.061 Uiso 1 1 calc R U . . . C17 C 0.09784(18) 0.5837(4) 0.38457(18) 0.0449(10) Uani 1 1 d . . . . . C18 C 0.1148(2) 0.4428(5) 0.3498(2) 0.0802(16) Uani 1 1 d . . . . . H18A H 0.1581 0.4479 0.3401 0.120 Uiso 1 1 calc R U . . . H18B H 0.0878 0.4313 0.3082 0.120 Uiso 1 1 calc R U . . . H18C H 0.1095 0.3590 0.3789 0.120 Uiso 1 1 calc R U . . . C19 C 0.16679(19) 0.9674(4) 0.4311(2) 0.0650(13) Uani 1 1 d . . . . . H19A H 0.2074 0.9407 0.4176 0.097 Uiso 1 1 calc R U . . . H19B H 0.1713 0.9943 0.4783 0.097 Uiso 1 1 calc R U . . . H19C H 0.1500 1.0507 0.4045 0.097 Uiso 1 1 calc R U . . . C20 C -0.04778(19) 0.7512(5) 0.4514(3) 0.0796(16) Uani 1 1 d . . . . . H20A H -0.0701 0.6585 0.4438 0.119 Uiso 1 1 calc R U . . . H20B H -0.0698 0.8285 0.4250 0.119 Uiso 1 1 calc R U . . . H20C H -0.0454 0.7766 0.4987 0.119 Uiso 1 1 calc R U . . . C21 C 0.25937(16) 0.6563(4) 0.54034(16) 0.0348(8) Uani 1 1 d . . . . . C22 C 0.28703(19) 0.8569(5) 0.6051(2) 0.0592(12) Uani 1 1 d . . . . . H22A H 0.3110 0.9346 0.6255 0.071 Uiso 1 1 calc R U . . . C23 C 0.2278(2) 0.8239(5) 0.6145(2) 0.0556(11) Uani 1 1 d . . . . . H23A H 0.2022 0.8745 0.6423 0.067 Uiso 1 1 calc R U . . . C24 C 0.14791(17) 0.6305(4) 0.56783(17) 0.0452(10) Uani 1 1 d . . . . . H24A H 0.1523 0.5251 0.5582 0.054 Uiso 1 1 calc R U . . . H24B H 0.1227 0.6753 0.5295 0.054 Uiso 1 1 calc R U . . . C25 C 0.1138(2) 0.6477(5) 0.6303(2) 0.0566(12) Uani 1 1 d . . . . . C26 C 0.0729(2) 0.7659(6) 0.6340(2) 0.0786(15) Uani 1 1 d . . . . . H26A H 0.0684 0.8339 0.5983 0.094 Uiso 1 1 calc R U . . . C27 C 0.0381(3) 0.7878(8) 0.6886(3) 0.106(2) Uani 1 1 d . . . . . H27A H 0.0120 0.8706 0.6911 0.127 Uiso 1 1 calc R U . . . C28 C 0.0441(3) 0.6811(10) 0.7391(3) 0.114(3) Uani 1 1 d . . . . . H28A H 0.0205 0.6913 0.7758 0.137 Uiso 1 1 calc R U . . . C29 C 0.0827(3) 0.5629(9) 0.7372(2) 0.099(2) Uani 1 1 d . . . . . H29A H 0.0849 0.4931 0.7721 0.118 Uiso 1 1 calc R U . . . C30 C 0.1200(2) 0.5430(7) 0.6829(2) 0.0699(16) Uani 1 1 d . . . . . C31 C 0.1622(3) 0.3026(7) 0.7275(3) 0.135(3) Uani 1 1 d . . . . . H31A H 0.1950 0.2347 0.7178 0.203 Uiso 1 1 calc R U . . . H31B H 0.1221 0.2523 0.7217 0.203 Uiso 1 1 calc R U . . . H31C H 0.1703 0.3372 0.7735 0.203 Uiso 1 1 calc R U . . . C32 C 0.37039(16) 0.7514(4) 0.54031(17) 0.0358(8) Uani 1 1 d . . . . . C33 C 0.41464(19) 0.6591(4) 0.57699(18) 0.0440(9) Uani 1 1 d . . . . . C34 C 0.47520(19) 0.6605(4) 0.5584(2) 0.0521(11) Uani 1 1 d . . . . . H34A H 0.5051 0.5978 0.5812 0.062 Uiso 1 1 calc R U . . . C35 C 0.49354(18) 0.7505(4) 0.5077(2) 0.0450(10) Uani 1 1 d . . . . . C36 C 0.44905(18) 0.8439(4) 0.47475(19) 0.0441(9) Uani 1 1 d . . . . . H36A H 0.4611 0.9071 0.4411 0.053 Uiso 1 1 calc R U . . . C37 C 0.38657(16) 0.8470(4) 0.49003(17) 0.0361(9) Uani 1 1 d . . . . . C38 C 0.33908(18) 0.9482(4) 0.4524(2) 0.0566(11) Uani 1 1 d . . . . . H38A H 0.2988 0.9356 0.4694 0.085 Uiso 1 1 calc R U . . . H38B H 0.3354 0.9240 0.4049 0.085 Uiso 1 1 calc R U . . . H38C H 0.3526 1.0500 0.4586 0.085 Uiso 1 1 calc R U . . . C39 C 0.56003(19) 0.7438(5) 0.4873(2) 0.0709(14) Uani 1 1 d . . . . . H39A H 0.5642 0.8139 0.4514 0.106 Uiso 1 1 calc R U . . . H39B H 0.5685 0.6449 0.4719 0.106 Uiso 1 1 calc R U . . . H39C H 0.5896 0.7684 0.5256 0.106 Uiso 1 1 calc R U . . . C40 C 0.3970(2) 0.5655(5) 0.6352(2) 0.0714(14) Uani 1 1 d . . . . . H40A H 0.4333 0.5100 0.6541 0.107 Uiso 1 1 calc R U . . . H40B H 0.3638 0.4975 0.6192 0.107 Uiso 1 1 calc R U . . . H40C H 0.3826 0.6292 0.6694 0.107 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 0.0417(3) 0.0325(3) 0.0298(2) 0.0014(2) 0.00184(18) -0.0035(2) Cl1 0.0713(7) 0.0336(5) 0.0551(6) -0.0066(5) 0.0101(5) -0.0031(5) Cl2 0.1071(10) 0.0544(7) 0.0444(6) 0.0178(5) 0.0041(6) -0.0084(6) N1 0.109(3) 0.066(3) 0.069(3) -0.032(2) 0.043(2) -0.021(2) N2 0.080(3) 0.135(4) 0.063(3) 0.048(3) 0.008(2) -0.022(3) N3 0.0374(19) 0.0407(18) 0.0289(15) 0.0043(14) 0.0022(14) 0.0050(14) N4 0.0361(19) 0.0456(18) 0.0312(16) 0.0060(14) 0.0078(14) 0.0087(14) N5 0.0377(19) 0.0418(18) 0.0404(17) -0.0090(15) 0.0105(15) -0.0084(14) N6 0.045(2) 0.0468(19) 0.0321(16) -0.0094(14) 0.0114(14) -0.0155(15) C1 0.036(2) 0.0299(19) 0.0284(18) -0.0046(15) 0.0045(16) -0.0030(16) C2 0.049(3) 0.080(3) 0.043(2) 0.024(2) 0.013(2) 0.026(2) C3 0.055(3) 0.067(3) 0.037(2) 0.017(2) 0.013(2) 0.017(2) C4 0.036(2) 0.044(2) 0.037(2) -0.0031(17) 0.0007(17) 0.0058(17) C5 0.034(2) 0.050(3) 0.044(2) -0.0023(19) 0.0076(17) 0.0145(18) C6 0.050(3) 0.066(3) 0.057(3) 0.001(2) 0.010(2) 0.004(2) C7 0.055(3) 0.087(4) 0.065(3) 0.012(3) 0.023(2) 0.001(3) C8 0.071(3) 0.097(4) 0.051(3) 0.000(3) 0.027(2) 0.023(3) C9 0.076(3) 0.071(3) 0.048(3) -0.010(2) 0.017(2) 0.019(3) C10 0.053(3) 0.058(3) 0.045(2) -0.003(2) 0.013(2) 0.013(2) C11 0.104(4) 0.071(3) 0.074(3) -0.029(3) 0.011(3) -0.010(3) C12 0.031(2) 0.047(2) 0.0313(19) 0.0027(17) 0.0006(16) 0.0037(17) C13 0.035(2) 0.041(2) 0.043(2) 0.0012(18) 0.0063(17) -0.0030(17) C14 0.045(3) 0.045(2) 0.053(2) -0.0099(19) 0.009(2) 0.0042(19) C15 0.039(2) 0.057(3) 0.052(2) -0.009(2) 0.0046(19) -0.001(2) C16 0.041(3) 0.050(3) 0.060(3) -0.012(2) 0.002(2) -0.0119(19) C17 0.043(3) 0.048(2) 0.043(2) -0.0109(19) -0.0026(19) 0.0025(19) C18 0.054(3) 0.070(3) 0.114(4) -0.051(3) -0.005(3) -0.001(2) C19 0.056(3) 0.048(3) 0.093(3) -0.003(2) 0.019(3) -0.004(2) C20 0.042(3) 0.090(4) 0.110(4) -0.036(3) 0.021(3) -0.009(2) C21 0.038(2) 0.041(2) 0.0254(17) 0.0042(16) 0.0048(16) -0.0045(17) C22 0.052(3) 0.064(3) 0.065(3) -0.035(2) 0.018(2) -0.022(2) C23 0.055(3) 0.063(3) 0.053(2) -0.026(2) 0.021(2) -0.012(2) C24 0.042(2) 0.059(3) 0.036(2) -0.0026(19) 0.0074(18) -0.0150(19) C25 0.044(3) 0.084(3) 0.043(2) -0.009(2) 0.012(2) -0.030(2) C26 0.063(4) 0.106(4) 0.071(3) -0.026(3) 0.030(3) -0.020(3) C27 0.073(4) 0.147(6) 0.107(5) -0.056(5) 0.046(4) -0.033(4) C28 0.068(5) 0.213(9) 0.066(4) -0.064(5) 0.030(4) -0.065(5) C29 0.063(4) 0.199(8) 0.035(3) -0.012(4) 0.011(3) -0.073(4) C30 0.046(3) 0.123(5) 0.040(2) -0.005(3) 0.004(2) -0.043(3) C31 0.146(6) 0.161(6) 0.094(4) 0.075(4) -0.007(4) -0.049(5) C32 0.035(2) 0.035(2) 0.038(2) -0.0127(17) 0.0078(17) -0.0099(16) C33 0.048(3) 0.043(2) 0.040(2) 0.0029(18) -0.0002(19) -0.0068(19) C34 0.041(3) 0.048(2) 0.066(3) 0.009(2) -0.003(2) -0.0001(19) C35 0.035(2) 0.039(2) 0.062(3) -0.008(2) 0.011(2) -0.0055(18) C36 0.045(3) 0.043(2) 0.045(2) -0.0003(19) 0.0086(19) -0.0093(19) C37 0.033(2) 0.034(2) 0.041(2) -0.0044(17) 0.0000(17) -0.0066(16) C38 0.050(3) 0.048(2) 0.071(3) 0.010(2) -0.001(2) -0.0048(19) C39 0.049(3) 0.055(3) 0.110(4) -0.004(3) 0.016(3) -0.003(2) C40 0.071(3) 0.085(3) 0.057(3) 0.024(3) 0.001(2) -0.008(3) _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 C21 1.876(4) . ? Ni1 C1 1.881(3) . ? Ni1 Cl1 2.2123(12) . ? Ni1 Cl2 2.2198(13) . ? N1 C10 1.357(5) . ? N1 C11 1.438(5) . ? N1 H1A 0.8600 . ? N2 C30 1.350(6) . ? N2 C31 1.441(6) . ? N2 H2B 0.8600 . ? N3 C1 1.349(4) . ? N3 C3 1.384(4) . ? N3 C4 1.478(4) . ? N4 C1 1.362(4) . ? N4 C2 1.387(4) . ? N4 C12 1.449(4) . ? N5 C21 1.357(4) . ? N5 C22 1.389(4) . ? N5 C32 1.442(4) . ? N6 C21 1.351(4) . ? N6 C23 1.378(4) . ? N6 C24 1.478(4) . ? C2 C3 1.322(5) . ? C2 H2A 0.9300 . ? C3 H3A 0.9300 . ? C4 C5 1.508(5) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.382(5) . ? C5 C10 1.409(5) . ? C6 C7 1.396(5) . ? C6 H6A 0.9300 . ? C7 C8 1.357(6) . ? C7 H7A 0.9300 . ? C8 C9 1.363(6) . ? C8 H8A 0.9300 . ? C9 C10 1.415(5) . ? C9 H9A 0.9300 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 C13 1.385(5) . ? C12 C17 1.390(5) . ? C13 C14 1.390(5) . ? C13 C19 1.491(5) . ? C14 C15 1.377(5) . ? C14 H14A 0.9300 . ? C15 C16 1.376(5) . ? C15 C20 1.511(5) . ? C16 C17 1.385(5) . ? C16 H16A 0.9300 . ? C17 C18 1.500(5) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C22 C23 1.326(5) . ? C22 H22A 0.9300 . ? C23 H23A 0.9300 . ? C24 C25 1.507(5) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C26 1.376(6) . ? C25 C30 1.398(6) . ? C26 C27 1.388(6) . ? C26 H26A 0.9300 . ? C27 C28 1.380(9) . ? C27 H27A 0.9300 . ? C28 C29 1.342(9) . ? C28 H28A 0.9300 . ? C29 C30 1.414(6) . ? C29 H29A 0.9300 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 C37 1.384(5) . ? C32 C33 1.398(5) . ? C33 C34 1.375(5) . ? C33 C40 1.505(5) . ? C34 C35 1.377(5) . ? C34 H34A 0.9300 . ? C35 C36 1.375(5) . ? C35 C39 1.511(5) . ? C36 C37 1.393(5) . ? C36 H36A 0.9300 . ? C37 C38 1.497(5) . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? 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 C21 Ni1 C1 92.54(14) . . ? C21 Ni1 Cl1 178.86(11) . . ? C1 Ni1 Cl1 88.52(10) . . ? C21 Ni1 Cl2 89.64(11) . . ? C1 Ni1 Cl2 177.57(10) . . ? Cl1 Ni1 Cl2 89.31(5) . . ? C10 N1 C11 123.7(4) . . ? C10 N1 H1A 118.1 . . ? C11 N1 H1A 118.1 . . ? C30 N2 C31 123.7(5) . . ? C30 N2 H2B 118.1 . . ? C31 N2 H2B 118.1 . . ? C1 N3 C3 110.7(3) . . ? C1 N3 C4 124.9(3) . . ? C3 N3 C4 124.2(3) . . ? C1 N4 C2 110.1(3) . . ? C1 N4 C12 128.1(3) . . ? C2 N4 C12 121.6(3) . . ? C21 N5 C22 110.1(3) . . ? C21 N5 C32 127.3(3) . . ? C22 N5 C32 122.4(3) . . ? C21 N6 C23 111.3(3) . . ? C21 N6 C24 123.8(3) . . ? C23 N6 C24 124.8(3) . . ? N3 C1 N4 104.6(3) . . ? N3 C1 Ni1 125.4(2) . . ? N4 C1 Ni1 129.6(3) . . ? C3 C2 N4 107.3(3) . . ? C3 C2 H2A 126.4 . . ? N4 C2 H2A 126.4 . . ? C2 C3 N3 107.3(3) . . ? C2 C3 H3A 126.4 . . ? N3 C3 H3A 126.4 . . ? N3 C4 C5 112.2(3) . . ? N3 C4 H4A 109.2 . . ? C5 C4 H4A 109.2 . . ? N3 C4 H4B 109.2 . . ? C5 C4 H4B 109.2 . . ? H4A C4 H4B 107.9 . . ? C6 C5 C10 119.5(4) . . ? C6 C5 C4 119.6(4) . . ? C10 C5 C4 120.8(3) . . ? C5 C6 C7 121.4(4) . . ? C5 C6 H6A 119.3 . . ? C7 C6 H6A 119.3 . . ? C8 C7 C6 118.8(4) . . ? C8 C7 H7A 120.6 . . ? C6 C7 H7A 120.6 . . ? C7 C8 C9 121.8(4) . . ? C7 C8 H8A 119.1 . . ? C9 C8 H8A 119.1 . . ? C8 C9 C10 120.8(4) . . ? C8 C9 H9A 119.6 . . ? C10 C9 H9A 119.6 . . ? N1 C10 C5 120.4(4) . . ? N1 C10 C9 121.9(4) . . ? C5 C10 C9 117.7(4) . . ? N1 C11 H11A 109.5 . . ? N1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C13 C12 C17 122.0(3) . . ? C13 C12 N4 118.7(3) . . ? C17 C12 N4 119.0(3) . . ? C12 C13 C14 117.0(3) . . ? C12 C13 C19 123.5(3) . . ? C14 C13 C19 119.5(3) . . ? C15 C14 C13 123.1(4) . . ? C15 C14 H14A 118.4 . . ? C13 C14 H14A 118.4 . . ? C16 C15 C14 117.4(4) . . ? C16 C15 C20 120.6(4) . . ? C14 C15 C20 122.0(4) . . ? C15 C16 C17 122.5(4) . . ? C15 C16 H16A 118.7 . . ? C17 C16 H16A 118.7 . . ? C16 C17 C12 117.7(4) . . ? C16 C17 C18 120.6(4) . . ? C12 C17 C18 121.6(4) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C13 C19 H19A 109.5 . . ? C13 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C13 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C15 C20 H20A 109.5 . . ? C15 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C15 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N6 C21 N5 104.4(3) . . ? N6 C21 Ni1 125.3(3) . . ? N5 C21 Ni1 130.2(3) . . ? C23 C22 N5 107.4(3) . . ? C23 C22 H22A 126.3 . . ? N5 C22 H22A 126.3 . . ? C22 C23 N6 106.8(3) . . ? C22 C23 H23A 126.6 . . ? N6 C23 H23A 126.6 . . ? N6 C24 C25 112.8(3) . . ? N6 C24 H24A 109.0 . . ? C25 C24 H24A 109.0 . . ? N6 C24 H24B 109.0 . . ? C25 C24 H24B 109.0 . . ? H24A C24 H24B 107.8 . . ? C26 C25 C30 119.2(5) . . ? C26 C25 C24 118.9(4) . . ? C30 C25 C24 121.8(5) . . ? C25 C26 C27 122.7(6) . . ? C25 C26 H26A 118.6 . . ? C27 C26 H26A 118.6 . . ? C28 C27 C26 116.8(7) . . ? C28 C27 H27A 121.6 . . ? C26 C27 H27A 121.6 . . ? C29 C28 C27 122.4(7) . . ? C29 C28 H28A 118.8 . . ? C27 C28 H28A 118.8 . . ? C28 C29 C30 121.0(7) . . ? C28 C29 H29A 119.5 . . ? C30 C29 H29A 119.5 . . ? N2 C30 C25 120.9(4) . . ? N2 C30 C29 121.4(6) . . ? C25 C30 C29 117.7(6) . . ? N2 C31 H31A 109.5 . . ? N2 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? N2 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C37 C32 C33 122.4(3) . . ? C37 C32 N5 119.1(3) . . ? C33 C32 N5 118.4(3) . . ? C34 C33 C32 117.0(3) . . ? C34 C33 C40 121.7(4) . . ? C32 C33 C40 121.3(4) . . ? C33 C34 C35 123.0(4) . . ? C33 C34 H34A 118.5 . . ? C35 C34 H34A 118.5 . . ? C36 C35 C34 118.0(4) . . ? C36 C35 C39 120.9(4) . . ? C34 C35 C39 121.1(4) . . ? C35 C36 C37 122.2(4) . . ? C35 C36 H36A 118.9 . . ? C37 C36 H36A 118.9 . . ? C32 C37 C36 117.3(3) . . ? C32 C37 C38 121.9(3) . . ? C36 C37 C38 120.8(3) . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C35 C39 H39A 109.5 . . ? C35 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C35 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C33 C40 H40A 109.5 . . ? C33 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C33 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? _refine_diff_density_max 0.401 _refine_diff_density_min -0.339 _refine_diff_density_rms 0.058 _shelxl_version_number 2013-2 _shelx_res_file ; TITL a01009b in P2(1)/c CELL 0.71073 21.2560 8.9566 19.8140 90.000 95.989 90.000 ZERR 4.00 0.0088 0.0038 0.0082 0.000 0.006 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N Ni Cl UNIT 160 184 24 4 8 OMIT -3.00 52.02 L.S. 4 ACTA BOND $H FMAP 2 PLAN 4 size 0.12 0.10 0.08 TEMP 20 WGHT 0.045200 FVAR 0.18427 NI1 4 0.258178 0.488818 0.483383 11.00000 0.04169 0.03248 = 0.02978 0.00141 0.00184 -0.00345 CL1 5 0.257652 0.288658 0.417907 11.00000 0.07125 0.03360 = 0.05510 -0.00662 0.01012 -0.00307 CL2 5 0.262281 0.341265 0.573747 11.00000 0.10706 0.05437 = 0.04444 0.01784 0.00412 -0.00844 N1 3 0.339418 0.297982 0.290466 11.00000 0.10851 0.06628 = 0.06902 -0.03237 0.04259 -0.02071 AFIX 43 H1A 2 0.316835 0.319986 0.322643 11.00000 -1.20000 AFIX 0 N2 3 0.160966 0.427999 0.681863 11.00000 0.07959 0.13474 = 0.06309 0.04751 0.00818 -0.02194 AFIX 43 H2B 2 0.187843 0.429673 0.652298 11.00000 -1.20000 AFIX 0 N3 3 0.298026 0.617605 0.361625 11.00000 0.03744 0.04068 = 0.02893 0.00428 0.00225 0.00504 N4 3 0.203095 0.685650 0.373787 11.00000 0.03612 0.04556 = 0.03124 0.00599 0.00780 0.00866 N5 3 0.306677 0.754231 0.559166 11.00000 0.03775 0.04179 = 0.04039 -0.00903 0.01052 -0.00845 N6 3 0.211271 0.700318 0.575197 11.00000 0.04502 0.04676 = 0.03211 -0.00936 0.01142 -0.01546 C1 1 0.253015 0.607279 0.404591 11.00000 0.03637 0.02995 = 0.02835 -0.00464 0.00450 -0.00297 C2 1 0.218070 0.742611 0.312350 11.00000 0.04891 0.08001 = 0.04318 0.02355 0.01293 0.02615 AFIX 43 H2A 2 0.191615 0.798550 0.281695 11.00000 -1.20000 AFIX 0 C3 1 0.276937 0.702616 0.305462 11.00000 0.05522 0.06724 = 0.03722 0.01671 0.01342 0.01654 AFIX 43 H3A 2 0.299898 0.727068 0.269551 11.00000 -1.20000 AFIX 0 C4 1 0.362825 0.556934 0.374850 11.00000 0.03552 0.04435 = 0.03669 -0.00314 0.00066 0.00581 AFIX 23 H4A 2 0.361322 0.462979 0.398978 11.00000 -1.20000 H4B 2 0.388555 0.625810 0.403685 11.00000 -1.20000 AFIX 0 C5 1 0.393246 0.531977 0.310327 11.00000 0.03382 0.05002 = 0.04355 -0.00226 0.00758 0.01448 C6 1 0.435464 0.636000 0.290115 11.00000 0.05010 0.06621 = 0.05739 0.00098 0.01003 0.00400 AFIX 43 H6A 2 0.445188 0.719655 0.317000 11.00000 -1.20000 AFIX 0 C7 1 0.463839 0.618161 0.230167 11.00000 0.05461 0.08749 = 0.06543 0.01205 0.02282 0.00139 AFIX 43 H7A 2 0.491882 0.689412 0.216859 11.00000 -1.20000 AFIX 0 C8 1 0.449747 0.494979 0.191692 11.00000 0.07053 0.09725 = 0.05064 0.00049 0.02745 0.02290 AFIX 43 H8A 2 0.468262 0.482968 0.151535 11.00000 -1.20000 AFIX 0 C9 1 0.409183 0.388336 0.210304 11.00000 0.07636 0.07106 = 0.04798 -0.01049 0.01749 0.01903 AFIX 43 H9A 2 0.400932 0.304661 0.183020 11.00000 -1.20000 AFIX 0 C10 1 0.379478 0.403328 0.270595 11.00000 0.05291 0.05766 = 0.04469 -0.00294 0.01333 0.01252 C11 1 0.332565 0.151605 0.260782 11.00000 0.10350 0.07117 = 0.07437 -0.02851 0.01144 -0.00960 AFIX 33 H11A 2 0.301509 0.096337 0.282314 11.00000 -1.50000 H11B 2 0.372392 0.100264 0.267066 11.00000 -1.50000 H11C 2 0.319221 0.160499 0.213152 11.00000 -1.50000 AFIX 0 C12 1 0.140295 0.701399 0.395217 11.00000 0.03149 0.04666 = 0.03128 0.00270 0.00055 0.00369 C13 1 0.122822 0.837968 0.420188 11.00000 0.03548 0.04097 = 0.04327 0.00119 0.00627 -0.00302 C14 1 0.061079 0.851329 0.436600 11.00000 0.04457 0.04493 = 0.05263 -0.00994 0.00892 0.00416 AFIX 43 H14A 2 0.048063 0.942851 0.452424 11.00000 -1.20000 AFIX 0 C15 1 0.018255 0.735493 0.430546 11.00000 0.03887 0.05748 = 0.05211 -0.00888 0.00457 -0.00067 C16 1 0.037689 0.603258 0.404084 11.00000 0.04108 0.05021 = 0.06025 -0.01229 0.00170 -0.01192 AFIX 43 H16A 2 0.009333 0.523972 0.399108 11.00000 -1.20000 AFIX 0 C17 1 0.097845 0.583658 0.384574 11.00000 0.04254 0.04767 = 0.04295 -0.01087 -0.00255 0.00253 C18 1 0.114831 0.442782 0.349809 11.00000 0.05357 0.06991 = 0.11427 -0.05080 -0.00511 -0.00058 AFIX 33 H18A 2 0.158085 0.447933 0.340080 11.00000 -1.50000 H18B 2 0.087773 0.431264 0.308219 11.00000 -1.50000 H18C 2 0.109507 0.358965 0.378873 11.00000 -1.50000 AFIX 0 C19 1 0.166786 0.967442 0.431110 11.00000 0.05615 0.04802 = 0.09320 -0.00293 0.01941 -0.00410 AFIX 33 H19A 2 0.207367 0.940711 0.417573 11.00000 -1.50000 H19B 2 0.171283 0.994285 0.478274 11.00000 -1.50000 H19C 2 0.150018 1.050701 0.404516 11.00000 -1.50000 AFIX 0 C20 1 -0.047784 0.751217 0.451386 11.00000 0.04157 0.09038 = 0.10959 -0.03624 0.02148 -0.00896 AFIX 33 H20A 2 -0.070052 0.658497 0.443763 11.00000 -1.50000 H20B 2 -0.069845 0.828515 0.424988 11.00000 -1.50000 H20C 2 -0.045424 0.776633 0.498651 11.00000 -1.50000 AFIX 0 C21 1 0.259367 0.656270 0.540342 11.00000 0.03807 0.04125 = 0.02542 0.00420 0.00484 -0.00446 C22 1 0.287029 0.856942 0.605121 11.00000 0.05165 0.06385 = 0.06463 -0.03540 0.01841 -0.02178 AFIX 43 H22A 2 0.311035 0.934611 0.625540 11.00000 -1.20000 AFIX 0 C23 1 0.227754 0.823930 0.614540 11.00000 0.05462 0.06252 = 0.05292 -0.02613 0.02075 -0.01233 AFIX 43 H23A 2 0.202230 0.874459 0.642338 11.00000 -1.20000 AFIX 0 C24 1 0.147912 0.630495 0.567827 11.00000 0.04160 0.05928 = 0.03552 -0.00256 0.00744 -0.01496 AFIX 23 H24A 2 0.152302 0.525051 0.558179 11.00000 -1.20000 H24B 2 0.122668 0.675349 0.529503 11.00000 -1.20000 AFIX 0 C25 1 0.113754 0.647703 0.630281 11.00000 0.04395 0.08430 = 0.04314 -0.00950 0.01229 -0.03006 C26 1 0.072886 0.765878 0.633954 11.00000 0.06339 0.10580 = 0.07148 -0.02579 0.02967 -0.01958 AFIX 43 H26A 2 0.068378 0.833879 0.598306 11.00000 -1.20000 AFIX 0 C27 1 0.038119 0.787816 0.688633 11.00000 0.07262 0.14660 = 0.10686 -0.05589 0.04636 -0.03291 AFIX 43 H27A 2 0.012039 0.870567 0.691149 11.00000 -1.20000 AFIX 0 C28 1 0.044074 0.681051 0.739088 11.00000 0.06835 0.21259 = 0.06575 -0.06421 0.02973 -0.06474 AFIX 43 H28A 2 0.020463 0.691312 0.775777 11.00000 -1.20000 AFIX 0 C29 1 0.082692 0.562931 0.737161 11.00000 0.06333 0.19862 = 0.03529 -0.01164 0.01069 -0.07318 AFIX 43 H29A 2 0.084911 0.493126 0.772076 11.00000 -1.20000 AFIX 0 C30 1 0.120045 0.543027 0.682860 11.00000 0.04650 0.12338 = 0.03970 -0.00477 0.00392 -0.04333 C31 1 0.162181 0.302563 0.727516 11.00000 0.14620 0.16132 = 0.09438 0.07541 -0.00749 -0.04900 AFIX 33 H31A 2 0.194999 0.234684 0.717772 11.00000 -1.50000 H31B 2 0.122097 0.252273 0.721731 11.00000 -1.50000 H31C 2 0.170257 0.337161 0.773460 11.00000 -1.50000 AFIX 0 C32 1 0.370392 0.751375 0.540315 11.00000 0.03524 0.03541 = 0.03767 -0.01271 0.00780 -0.00993 C33 1 0.414644 0.659116 0.576992 11.00000 0.04768 0.04342 = 0.03976 0.00289 -0.00025 -0.00675 C34 1 0.475200 0.660541 0.558426 11.00000 0.04092 0.04752 = 0.06584 0.00879 -0.00343 -0.00008 AFIX 43 H34A 2 0.505148 0.597803 0.581217 11.00000 -1.20000 AFIX 0 C35 1 0.493541 0.750541 0.507663 11.00000 0.03498 0.03923 = 0.06195 -0.00831 0.01081 -0.00554 C36 1 0.449046 0.843870 0.474747 11.00000 0.04526 0.04290 = 0.04504 -0.00026 0.00858 -0.00932 AFIX 43 H36A 2 0.461071 0.907062 0.441129 11.00000 -1.20000 AFIX 0 C37 1 0.386571 0.847012 0.490031 11.00000 0.03259 0.03411 = 0.04078 -0.00445 0.00004 -0.00657 C38 1 0.339079 0.948211 0.452355 11.00000 0.04951 0.04778 = 0.07114 0.01020 -0.00052 -0.00482 AFIX 33 H38A 2 0.298768 0.935580 0.469410 11.00000 -1.50000 H38B 2 0.335390 0.923969 0.404911 11.00000 -1.50000 H38C 2 0.352621 1.049986 0.458580 11.00000 -1.50000 AFIX 0 C39 1 0.560033 0.743820 0.487291 11.00000 0.04911 0.05550 = 0.10971 -0.00354 0.01573 -0.00340 AFIX 33 H39A 2 0.564208 0.813922 0.451380 11.00000 -1.50000 H39B 2 0.568509 0.644910 0.471911 11.00000 -1.50000 H39C 2 0.589625 0.768356 0.525641 11.00000 -1.50000 AFIX 0 C40 1 0.396979 0.565479 0.635178 11.00000 0.07126 0.08475 = 0.05682 0.02442 0.00066 -0.00842 AFIX 33 H40A 2 0.433253 0.510018 0.654109 11.00000 -1.50000 H40B 2 0.363812 0.497521 0.619152 11.00000 -1.50000 H40C 2 0.382601 0.629153 0.669397 11.00000 -1.50000 AFIX 0 HKLF 4 REM a01009b in P2(1)/c REM R1 = 0.0533 for 4381 Fo > 4sig(Fo) and 0.1009 for all 7348 data REM 442 parameters refined using 0 restraints END WGHT 0.0452 0.0000 REM Highest difference peak 0.401, deepest hole -0.339, 1-sigma level 0.058 Q1 1 0.2206 0.4980 0.4505 11.00000 0.05 0.40 Q2 1 0.2565 0.3842 0.4462 11.00000 0.05 0.40 Q3 1 0.2612 0.3901 0.5226 11.00000 0.05 0.39 Q4 1 0.3192 1.0272 0.4890 11.00000 0.05 0.38 ; _shelx_res_checksum 82429 _shelx_hkl_file ; -3 0 -25 1.43 3.76 -3 1 -25 3.29 3.97 -4 -3 -24 1.13 3.49 -6 -2 -24 13.33 5.56 -5 -2 -24 1.25 3.77 -4 -2 -24 7.67 4.58 -3 -2 -24 7.22 3.91 -6 -1 -24 -1.11 4.21 -5 -1 -24 8.67 4.18 -4 -1 -24 3.44 3.71 -3 -1 -24 3.11 3.22 -6 0 -24 2.09 4.14 -5 0 -24 24.22 5.81 -4 0 -24 1.03 3.49 -3 0 -24 12.75 4.26 -2 0 -24 0.84 2.82 -6 1 -24 2.25 4.17 -5 1 -24 8.11 4.21 -4 1 -24 2.04 3.49 -3 1 -24 4.71 3.50 -2 1 -24 2.28 2.84 -5 2 -24 2.86 4.09 -4 2 -24 0.98 3.98 -3 2 -24 -0.34 3.90 -2 2 -24 12.01 3.84 -1 2 -24 6.83 3.49 -4 3 -24 -0.55 3.59 -3 3 -24 2.42 4.19 -2 3 -24 -1.29 3.49 -1 3 -24 2.74 3.26 0 4 -24 3.69 4.14 -5 -4 -23 3.93 4.61 -4 -4 -23 1.80 4.53 -6 -3 -23 19.57 5.95 -5 -3 -23 7.17 4.66 -4 -3 -23 10.43 4.25 -3 -3 -23 7.91 3.28 -7 -2 -23 3.69 4.66 -6 -2 -23 3.10 4.18 -5 -2 -23 4.50 3.41 -4 -2 -23 3.23 3.06 -3 -2 -23 0.64 2.85 -2 -2 -23 2.87 2.62 -8 -1 -23 0.68 4.35 -7 -1 -23 5.57 4.59 -6 -1 -23 2.53 3.52 -5 -1 -23 23.17 5.21 -4 -1 -23 0.29 2.55 -3 -1 -23 19.56 4.28 -2 -1 -23 2.90 2.57 -8 0 -23 0.55 4.08 -7 0 -23 2.76 3.73 -6 0 -23 3.20 3.84 -5 0 -23 2.83 2.95 -4 0 -23 0.75 2.62 -3 0 -23 0.95 2.31 -2 0 -23 1.04 2.76 -1 0 -23 0.19 2.81 -8 1 -23 -3.59 3.08 -7 1 -23 8.49 4.54 -6 1 -23 1.14 3.61 -5 1 -23 26.92 5.19 -4 1 -23 5.07 3.23 -3 1 -23 18.60 4.34 -2 1 -23 3.21 2.99 -1 1 -23 7.38 3.26 -7 2 -23 4.79 4.69 -6 2 -23 3.75 4.23 -5 2 -23 3.20 4.04 -4 2 -23 0.92 3.40 -3 2 -23 1.09 3.14 -2 2 -23 2.27 3.02 -1 2 -23 2.60 2.73 0 2 -23 1.85 2.83 -6 3 -23 14.64 5.36 -5 3 -23 5.33 4.57 -4 3 -23 9.49 4.68 -3 3 -23 8.03 3.73 -2 3 -23 8.86 3.50 -1 3 -23 6.17 3.26 0 3 -23 10.93 3.97 -4 4 -23 -1.32 4.02 -3 4 -23 -1.56 3.98 -2 4 -23 0.81 3.43 -1 4 -23 2.89 3.38 0 4 -23 2.01 3.22 1 4 -23 6.13 3.40 -1 5 -23 1.49 4.16 0 5 -23 3.19 4.23 1 5 -23 2.20 4.57 -5 -5 -22 3.31 4.70 -4 -5 -22 6.04 4.91 -3 -5 -22 4.31 3.79 -7 -4 -22 4.84 4.76 -6 -4 -22 1.61 3.67 -5 -4 -22 6.79 3.91 -4 -4 -22 16.44 4.51 -3 -4 -22 10.16 3.53 -8 -3 -22 4.37 4.73 -7 -3 -22 2.94 3.92 -6 -3 -22 6.49 3.57 -5 -3 -22 4.93 3.17 -4 -3 -22 3.19 3.01 -3 -3 -22 3.85 3.18 -2 -3 -22 10.27 3.63 -9 -2 -22 8.68 4.71 -8 -2 -22 3.23 3.77 -7 -2 -22 5.21 3.84 -6 -2 -22 4.83 3.08 -5 -2 -22 16.50 4.22 -4 -2 -22 2.61 3.11 -3 -2 -22 14.77 3.99 -2 -2 -22 5.19 3.06 -1 -2 -22 5.82 3.07 -10 -1 -22 0.78 3.99 -9 -1 -22 2.01 4.09 -8 -1 -22 4.52 3.81 -7 -1 -22 7.97 3.52 -6 -1 -22 5.20 3.21 -5 -1 -22 4.65 3.12 -4 -1 -22 6.01 3.38 -3 -1 -22 1.80 2.72 -2 -1 -22 -1.86 2.39 -1 -1 -22 3.92 2.92 -10 0 -22 0.63 3.85 -9 0 -22 7.37 4.71 -8 0 -22 8.37 4.37 -7 0 -22 45.21 6.58 -6 0 -22 8.95 3.44 -5 0 -22 14.32 3.79 -4 0 -22 13.96 3.85 -3 0 -22 12.27 3.77 -2 0 -22 2.95 2.60 -1 0 -22 16.72 4.01 0 0 -22 6.42 3.02 -9 1 -22 -0.19 3.72 -8 1 -22 3.61 4.04 -7 1 -22 3.43 3.80 -6 1 -22 -0.52 2.62 -5 1 -22 2.91 3.04 -4 1 -22 4.93 3.07 -3 1 -22 0.47 2.54 -2 1 -22 2.33 2.42 -1 1 -22 1.70 2.64 0 1 -22 3.52 2.76 -9 2 -22 7.84 4.57 -8 2 -22 0.33 4.07 -7 2 -22 1.62 3.49 -6 2 -22 -0.02 3.14 -5 2 -22 18.18 4.60 -4 2 -22 1.70 2.77 -3 2 -22 12.89 4.13 -2 2 -22 -0.26 2.56 -1 2 -22 9.35 3.58 0 2 -22 3.33 2.91 1 2 -22 6.28 3.40 -8 3 -22 9.67 4.91 -7 3 -22 4.08 4.07 -6 3 -22 6.61 4.04 -5 3 -22 3.79 3.28 -4 3 -22 2.65 3.31 -3 3 -22 3.35 2.79 -2 3 -22 5.42 3.21 -1 3 -22 3.78 2.87 0 3 -22 10.91 3.61 1 3 -22 6.32 3.35 -6 4 -22 0.38 4.18 -5 4 -22 4.66 4.29 -4 4 -22 4.73 3.76 -3 4 -22 8.75 4.24 -2 4 -22 13.17 4.29 -1 4 -22 -0.19 2.93 0 4 -22 0.97 3.10 1 4 -22 2.35 2.59 -4 5 -22 -0.51 3.73 -3 5 -22 5.17 4.51 -2 5 -22 -2.98 4.06 -1 5 -22 -2.19 3.98 0 5 -22 -3.41 3.49 1 5 -22 4.24 3.31 2 5 -22 1.82 3.19 -5 -6 -21 1.50 4.88 -4 -6 -21 5.47 5.03 -3 -6 -21 4.06 4.63 -7 -5 -21 -0.25 4.65 -6 -5 -21 2.54 4.18 -5 -5 -21 3.81 4.23 -4 -5 -21 7.77 4.24 -3 -5 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12.01 4.88 -3 4 21 2.02 4.47 -2 4 21 17.79 5.06 -1 4 21 1.64 2.96 0 4 21 9.03 4.05 1 4 21 -0.85 3.10 2 4 21 -1.66 3.49 3 4 21 0.25 3.81 4 4 21 0.97 4.03 5 4 21 5.13 4.38 6 4 21 -5.53 3.92 7 4 21 0.66 4.36 8 4 21 1.15 4.44 9 4 21 -0.21 3.83 -10 5 21 1.60 5.16 -9 5 21 2.53 4.78 -8 5 21 -0.44 4.62 -7 5 21 -4.00 4.75 -6 5 21 10.75 5.95 -5 5 21 -4.24 5.04 -4 5 21 9.26 5.59 -3 5 21 -1.76 4.34 -2 5 21 6.76 4.83 -1 5 21 1.79 4.28 0 5 21 13.97 5.21 1 5 21 7.20 4.26 2 5 21 -0.22 3.98 3 5 21 4.14 4.11 4 5 21 4.63 4.69 5 5 21 -2.26 4.04 6 5 21 1.52 4.48 7 5 21 -1.23 4.58 8 5 21 -3.97 4.62 -3 6 21 -1.78 5.24 -2 6 21 0.40 5.44 -2 -6 22 18.66 6.68 -1 -6 22 10.36 5.72 -10 -3 22 11.77 3.70 -9 -3 22 3.29 2.98 -8 -3 22 4.71 3.13 -7 -3 22 4.78 3.32 -13 -2 22 7.43 3.63 -12 -2 22 18.10 4.66 -11 -2 22 0.24 2.54 -10 -2 22 8.65 3.54 -9 -2 22 3.00 3.10 -7 -2 22 10.75 3.79 -6 -2 22 11.77 3.99 -5 -2 22 9.05 3.61 -14 -1 22 5.53 3.10 -13 -1 22 3.30 3.03 -12 -1 22 3.62 2.54 -11 -1 22 -0.40 2.37 -10 -1 22 8.39 3.29 -9 -1 22 0.20 2.88 -8 -1 22 2.56 2.92 -7 -1 22 1.83 3.13 -6 -1 22 5.51 3.47 -5 -1 22 2.61 2.94 -4 -1 22 4.99 3.42 -3 -1 22 -1.23 2.77 -2 -1 22 9.24 3.70 -14 0 22 0.65 2.67 -13 0 22 2.84 3.01 -12 0 22 15.11 3.88 -11 0 22 3.93 2.57 -10 0 22 16.74 4.24 -9 0 22 3.36 3.12 -8 0 22 14.99 4.35 -7 0 22 13.50 4.14 -6 0 22 2.54 3.11 -5 0 22 5.27 3.27 -4 0 22 15.11 4.48 -3 0 22 21.43 4.93 -2 0 22 15.22 4.47 -1 0 22 30.64 5.94 0 0 22 5.22 4.24 -14 1 22 0.63 3.85 -13 1 22 -1.00 2.89 -12 1 22 1.71 3.11 -11 1 22 1.78 2.50 -10 1 22 6.63 2.70 -9 1 22 6.71 3.44 -8 1 22 5.37 3.01 -7 1 22 -1.04 3.08 -6 1 22 5.27 3.82 -5 1 22 2.21 3.77 -4 1 22 -0.81 3.11 -3 1 22 -0.10 3.36 -2 1 22 8.99 3.90 -1 1 22 -1.62 3.06 0 1 22 0.13 3.57 1 1 22 1.45 3.36 2 1 22 1.12 3.17 -13 2 22 2.54 3.70 -12 2 22 9.90 4.51 -11 2 22 3.23 3.79 -10 2 22 6.34 4.02 -9 2 22 -3.22 2.50 -8 2 22 21.89 4.69 -7 2 22 12.01 3.80 -6 2 22 14.89 4.40 -5 2 22 6.95 3.86 -4 2 22 19.34 5.07 -3 2 22 14.77 4.90 -2 2 22 13.34 4.38 -1 2 22 4.71 3.97 0 2 22 -4.46 3.05 2 2 22 1.86 3.16 3 2 22 11.07 4.49 4 2 22 1.05 3.72 -12 3 22 1.47 3.80 -11 3 22 1.06 3.51 -10 3 22 7.96 4.48 -9 3 22 1.87 4.32 -8 3 22 -1.55 3.60 -7 3 22 -0.49 4.05 -6 3 22 1.33 2.59 -5 3 22 6.43 3.07 -4 3 22 -3.51 2.27 -3 3 22 3.64 3.49 -2 3 22 4.04 3.83 -1 3 22 3.27 3.56 0 3 22 3.89 3.76 1 3 22 -2.37 3.32 2 3 22 2.50 3.46 3 3 22 0.20 3.39 4 3 22 -1.56 3.61 5 3 22 3.80 4.21 6 3 22 8.14 4.45 -10 4 22 2.53 5.26 -9 4 22 -5.53 4.11 -8 4 22 2.10 4.41 -7 4 22 -7.27 4.28 -6 4 22 -0.78 4.32 -5 4 22 -3.36 3.59 -4 4 22 1.69 4.29 -3 4 22 3.07 3.82 -2 4 22 3.01 3.73 -1 4 22 2.89 3.31 0 4 22 -0.75 3.38 1 4 22 1.87 3.75 2 4 22 8.13 5.03 3 4 22 -0.20 4.35 4 4 22 7.78 4.75 5 4 22 1.95 4.09 6 4 22 -1.14 4.18 7 4 22 1.94 4.46 8 4 22 0.13 4.44 -6 5 22 -0.76 5.50 -5 5 22 1.40 6.09 -4 5 22 -5.71 4.69 -3 5 22 -3.06 4.27 -2 5 22 -0.93 4.31 -1 5 22 0.87 4.33 0 5 22 -4.25 4.21 1 5 22 -0.56 4.58 2 5 22 -2.24 4.11 3 5 22 0.46 4.81 4 5 22 1.62 4.73 -12 -3 23 12.05 4.65 -11 -3 23 3.39 3.89 -10 -3 23 7.92 4.08 -9 -3 23 1.15 3.35 -8 -3 23 1.28 3.32 -12 -2 23 1.24 3.37 -11 -2 23 7.78 4.18 -10 -2 23 3.52 3.29 -9 -2 23 3.98 3.46 -8 -2 23 3.67 3.25 -7 -2 23 0.66 3.14 -6 -2 23 1.12 3.10 -13 -1 23 0.35 3.32 -12 -1 23 14.64 4.67 -11 -1 23 4.44 3.81 -10 -1 23 4.90 3.70 -9 -1 23 -0.27 3.20 -8 -1 23 19.64 4.94 -7 -1 23 3.28 3.19 -6 -1 23 15.52 4.30 -5 -1 23 10.24 3.83 -4 -1 23 8.68 3.72 -3 -1 23 14.83 4.38 -13 0 23 1.18 3.49 -12 0 23 0.63 3.30 -11 0 23 -3.72 2.48 -10 0 23 0.62 3.19 -9 0 23 1.81 3.45 -8 0 23 0.32 2.89 -7 0 23 -3.01 2.52 -6 0 23 -3.37 2.79 -5 0 23 -1.83 2.72 -4 0 23 -0.79 3.14 -3 0 23 0.15 3.47 -2 0 23 -0.88 3.13 -1 0 23 -1.02 3.84 -12 1 23 14.63 5.00 -11 1 23 4.42 3.69 -10 1 23 11.98 4.14 -9 1 23 4.48 2.81 -8 1 23 22.42 5.03 -7 1 23 -1.20 2.78 -6 1 23 11.97 4.20 -5 1 23 12.49 4.51 -4 1 23 7.06 3.96 -3 1 23 12.39 4.71 -1 1 23 20.53 5.03 0 1 23 3.06 3.92 1 1 23 9.41 4.16 -11 2 23 -2.70 3.66 -10 2 23 4.32 4.20 -9 2 23 -3.68 2.81 -8 2 23 5.27 3.42 -7 2 23 0.51 3.14 -6 2 23 -4.63 2.82 -5 2 23 2.24 3.28 -4 2 23 -4.15 3.16 -3 2 23 3.42 3.85 -2 2 23 -0.83 3.30 -1 2 23 0.43 3.63 0 2 23 -2.33 3.28 1 2 23 -1.59 3.38 2 2 23 -3.79 3.10 3 2 23 -2.35 3.38 -9 3 23 -1.98 4.30 -8 3 23 -4.19 3.80 -7 3 23 2.66 3.61 -6 3 23 7.92 4.03 -5 3 23 -1.07 3.47 -4 3 23 3.67 3.97 -3 3 23 -0.70 3.62 -2 3 23 16.91 5.06 -1 3 23 -2.19 3.60 0 3 23 10.05 4.55 1 3 23 -5.50 3.18 2 3 23 1.34 4.35 3 3 23 1.24 4.37 4 3 23 -0.05 4.43 5 3 23 5.59 4.87 -6 4 23 -2.03 4.80 -5 4 23 -0.99 4.58 -4 4 23 1.39 4.24 -3 4 23 2.48 4.19 -2 4 23 1.60 4.09 -1 4 23 0.78 4.08 0 4 23 0.81 4.52 1 4 23 2.80 4.51 2 4 23 -0.87 4.86 3 4 23 -5.40 3.70 4 4 23 0.55 4.90 5 4 23 0.31 4.94 -9 -3 24 2.24 3.69 -11 -2 24 1.62 4.10 -10 -2 24 17.80 5.38 -9 -2 24 0.76 3.88 -8 -2 24 11.97 4.55 -7 -2 24 2.51 3.35 -11 -1 24 2.98 4.19 -10 -1 24 -4.55 3.32 -9 -1 24 1.93 3.73 -8 -1 24 7.01 4.36 -7 -1 24 2.98 3.66 -6 -1 24 6.76 3.82 -5 -1 24 -0.82 3.01 -4 -1 24 4.11 3.74 -10 0 24 7.65 4.75 -9 0 24 -0.82 3.89 -8 0 24 1.62 3.64 -7 0 24 1.50 3.80 -6 0 24 2.06 3.83 -5 0 24 5.40 4.05 -4 0 24 6.53 3.83 -3 0 24 27.41 5.89 -2 0 24 6.38 4.31 -10 1 24 -2.37 3.50 -9 1 24 -1.24 3.44 -8 1 24 8.76 4.36 -7 1 24 -0.46 4.02 -6 1 24 4.84 4.42 -5 1 24 -5.34 3.54 -4 1 24 5.85 4.65 -3 1 24 -2.68 3.52 -2 1 24 -4.24 3.50 -1 1 24 -0.57 3.83 0 1 24 0.34 3.25 -8 2 24 19.70 6.08 -7 2 24 -2.35 3.49 -6 2 24 32.17 6.64 -5 2 24 3.40 4.18 -4 2 24 13.78 5.44 -3 2 24 -0.10 4.44 -2 2 24 12.54 5.15 -1 2 24 -1.11 3.85 0 2 24 13.10 4.84 1 2 24 4.44 4.51 2 2 24 8.67 4.83 -5 3 24 -4.91 4.22 -4 3 24 -0.32 4.64 -3 3 24 1.41 4.58 -2 3 24 -1.17 4.31 -1 3 24 2.75 4.32 0 3 24 -1.86 4.58 1 3 24 1.12 4.69 2 3 24 -2.13 4.72 3 3 24 -1.71 4.79 4 3 24 -7.14 4.41 -8 -1 25 16.62 5.71 -7 -1 25 1.78 4.46 -6 -1 25 4.28 4.52 -8 0 25 -3.70 3.47 -7 0 25 -1.94 4.20 -6 0 25 -2.77 3.95 -5 0 25 -1.43 4.13 -4 0 25 -1.33 4.20 -3 0 25 -5.25 3.76 -6 1 25 -1.44 3.88 -5 1 25 -1.35 4.64 -4 1 25 5.26 4.29 -3 1 25 4.92 4.97 -2 1 25 -1.82 4.62 -1 1 25 2.22 5.03 -4 2 25 -1.36 4.52 -3 2 25 -2.03 4.98 -2 2 25 1.70 4.85 -1 2 25 0.27 4.64 0 2 25 -0.15 4.68 1 2 25 -0.47 4.77 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 80813 _database_code_depnum_ccdc_archive 'CCDC 877559' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_a20712a _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H42 Ag2 Br Cl N6' _chemical_formula_weight 817.79 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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 21/c' _space_group_name_Hall '-P 2ybc' _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+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.868(5) _cell_length_b 12.316(5) _cell_length_c 11.078(5) _cell_angle_alpha 90 _cell_angle_beta 108.620(5) _cell_angle_gamma 90 _cell_volume 1663.8(12) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 853 _cell_measurement_theta_min 3.706 _cell_measurement_theta_max 26.542 _exptl_crystal_description sheet _exptl_crystal_colour purple _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.632 _exptl_crystal_F_000 820 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.450 _exptl_crystal_size_mid 0.400 _exptl_crystal_size_min 0.180 _exptl_absorpt_coefficient_mu 2.487 _shelx_estimated_absorpt_T_min 0.401 _shelx_estimated_absorpt_T_max 0.663 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4193 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source ? _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 7364 _diffrn_reflns_av_unetI/netI 0.0363 _diffrn_reflns_av_R_equivalents 0.0379 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.670 _diffrn_reflns_theta_max 25.998 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_point_group_measured_fraction_full 0.998 _reflns_number_total 3258 _reflns_number_gt 2298 _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 SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0873P)^2^] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0021(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3258 _refine_ls_number_parameters 186 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0629 _refine_ls_R_factor_gt 0.0457 _refine_ls_wR_factor_ref 0.1455 _refine_ls_wR_factor_gt 0.1361 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.059 _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 Ag1 Ag 0.95520(3) 1.01606(3) 0.15115(4) 0.0685(2) Uani 1 1 d . . . . . Br1 Br 1.12993(7) 1.05445(10) 0.12195(9) 0.0923(4) Uani 0.5 1 d . . P . . Cl1 Cl 1.12993(7) 1.05445(10) 0.12195(9) 0.0923(4) Uani 0.5 1 d . . P . . N1 N 0.8199(3) 1.0517(3) 0.3415(3) 0.0537(9) Uani 1 1 d . . . . . N2 N 0.7824(3) 0.9004(3) 0.2401(3) 0.0501(9) Uani 1 1 d . . . . . N3 N 0.6353(3) 0.9476(4) -0.0410(4) 0.0650(11) Uani 1 1 d . . . . . H3A H 0.6977 0.9690 0.0093 0.078 Uiso 1 1 calc R U . . . C1 C 0.8413(3) 0.9925(4) 0.2502(4) 0.0504(11) Uani 1 1 d . . . . . C2 C 0.7497(4) 0.9943(5) 0.3902(5) 0.0692(15) Uani 1 1 d . . . . . H2 H 0.7241 1.0166 0.4558 0.083 Uiso 1 1 calc R U . . . C3 C 0.7260(4) 0.9021(5) 0.3264(5) 0.0668(14) Uani 1 1 d . . . . . H3 H 0.6795 0.8481 0.3379 0.080 Uiso 1 1 calc R U . . . C4 C 0.7795(4) 0.8112(4) 0.1538(5) 0.0577(11) Uani 1 1 d . . . . . H4A H 0.8158 0.7488 0.2026 0.069 Uiso 1 1 calc R U . . . H4B H 0.8197 0.8316 0.0966 0.069 Uiso 1 1 calc R U . . . C5 C 0.6635(3) 0.7798(4) 0.0758(4) 0.0539(11) Uani 1 1 d . . . . . C6 C 0.6247(4) 0.6812(5) 0.1006(5) 0.0714(14) Uani 1 1 d . . . . . H6 H 0.6687 0.6365 0.1641 0.086 Uiso 1 1 calc R U . . . C7 C 0.5181(5) 0.6482(6) 0.0294(7) 0.094(2) Uani 1 1 d . . . . . H7 H 0.4904 0.5822 0.0462 0.112 Uiso 1 1 calc R U . . . C8 C 0.4561(5) 0.7147(6) -0.0646(6) 0.0902(19) Uani 1 1 d . . . . . H8 H 0.3860 0.6927 -0.1129 0.108 Uiso 1 1 calc R U . . . C9 C 0.4935(4) 0.8104(5) -0.0890(5) 0.0710(14) Uani 1 1 d . . . . . H9 H 0.4488 0.8534 -0.1539 0.085 Uiso 1 1 calc R U . . . C10 C 0.5984(4) 0.8479(4) -0.0194(4) 0.0535(11) Uani 1 1 d . . . . . C11 C 0.5766(5) 1.0193(5) -0.1427(5) 0.0792(16) Uani 1 1 d . . . . . H11A H 0.5606 0.9821 -0.2228 0.119 Uiso 1 1 calc R U . . . H11B H 0.6207 1.0821 -0.1431 0.119 Uiso 1 1 calc R U . . . H11C H 0.5093 1.0415 -0.1301 0.119 Uiso 1 1 calc R U . . . C12 C 0.8660(4) 1.1607(4) 0.3894(5) 0.0614(12) Uani 1 1 d . . . . . C13 C 0.8800(10) 1.2259(6) 0.2850(9) 0.175(5) Uani 1 1 d . . . . . H13A H 0.8969 1.2994 0.3131 0.263 Uiso 1 1 calc R U . . . H13B H 0.8134 1.2244 0.2141 0.263 Uiso 1 1 calc R U . . . H13C H 0.9388 1.1964 0.2594 0.263 Uiso 1 1 calc R U . . . C14 C 0.9671(8) 1.1472(7) 0.4881(12) 0.242(9) Uani 1 1 d . . . . . H14A H 1.0190 1.1129 0.4545 0.362 Uiso 1 1 calc R U . . . H14B H 0.9561 1.1026 0.5541 0.362 Uiso 1 1 calc R U . . . H14C H 0.9947 1.2169 0.5226 0.362 Uiso 1 1 calc R U . . . C15 C 0.7857(8) 1.2245(8) 0.4350(11) 0.150(4) Uani 1 1 d . . . . . H15A H 0.7878 1.1987 0.5175 0.225 Uiso 1 1 calc R U . . . H15B H 0.7131 1.2152 0.3761 0.225 Uiso 1 1 calc R U . . . H15C H 0.8050 1.3000 0.4404 0.225 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 Ag1 0.0685(3) 0.0685(3) 0.0869(4) 0.0096(2) 0.0508(2) 0.00199(18) Br1 0.0719(5) 0.1261(8) 0.0931(7) -0.0327(6) 0.0462(5) -0.0328(5) Cl1 0.0719(5) 0.1261(8) 0.0931(7) -0.0327(6) 0.0462(5) -0.0328(5) N1 0.051(2) 0.071(2) 0.041(2) 0.0010(18) 0.0182(17) -0.0062(18) N2 0.0457(19) 0.063(2) 0.0436(19) 0.0030(17) 0.0172(16) -0.0044(16) N3 0.054(2) 0.065(2) 0.067(3) 0.012(2) 0.008(2) 0.003(2) C1 0.042(2) 0.067(3) 0.042(2) 0.008(2) 0.0135(19) 0.0020(19) C2 0.065(3) 0.098(4) 0.056(3) -0.012(3) 0.036(3) -0.015(3) C3 0.060(3) 0.087(4) 0.061(3) 0.003(3) 0.031(2) -0.016(3) C4 0.053(2) 0.062(3) 0.059(3) 0.006(2) 0.019(2) 0.004(2) C5 0.055(2) 0.057(3) 0.055(3) -0.006(2) 0.025(2) -0.005(2) C6 0.080(3) 0.066(3) 0.070(3) -0.004(3) 0.027(3) -0.013(3) C7 0.104(5) 0.088(4) 0.095(5) -0.022(4) 0.041(4) -0.047(4) C8 0.078(4) 0.114(5) 0.075(4) -0.020(4) 0.019(3) -0.036(4) C9 0.060(3) 0.094(4) 0.057(3) -0.009(3) 0.017(2) -0.005(3) C10 0.049(2) 0.064(3) 0.050(3) -0.009(2) 0.020(2) 0.000(2) C11 0.085(4) 0.080(4) 0.069(4) 0.010(3) 0.020(3) 0.017(3) C12 0.060(3) 0.072(3) 0.053(3) -0.006(2) 0.018(2) -0.005(2) C13 0.352(15) 0.071(5) 0.140(8) -0.021(5) 0.132(10) -0.037(7) C14 0.163(8) 0.072(5) 0.331(16) -0.026(7) -0.144(10) -0.004(5) C15 0.156(7) 0.105(6) 0.216(11) -0.053(7) 0.098(8) -0.020(6) _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 Ag1 C1 2.112(4) . ? Ag1 Br1 2.4184(12) . ? Ag1 Br1 2.9984(15) 3_775 ? Br1 Ag1 2.9984(15) 3_775 ? N1 C1 1.346(6) . ? N1 C2 1.385(6) . ? N1 C12 1.495(6) . ? N2 C1 1.349(6) . ? N2 C3 1.373(6) . ? N2 C4 1.449(6) . ? N3 C10 1.365(6) . ? N3 C11 1.441(7) . ? N3 H3A 0.8600 . ? C2 C3 1.321(7) . ? C2 H2 0.9300 . ? C3 H3 0.9300 . ? C4 C5 1.517(6) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.374(7) . ? C5 C10 1.396(6) . ? C6 C7 1.406(8) . ? C6 H6 0.9300 . ? C7 C8 1.364(10) . ? C7 H7 0.9300 . ? C8 C9 1.332(9) . ? C8 H8 0.9300 . ? C9 C10 1.402(7) . ? C9 H9 0.9300 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 C14 1.417(9) . ? C12 C13 1.465(9) . ? C12 C15 1.508(9) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? 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 C1 Ag1 Br1 157.69(12) . . ? C1 Ag1 Br1 113.19(12) . 3_775 ? Br1 Ag1 Br1 88.70(3) . 3_775 ? Ag1 Br1 Ag1 91.29(3) . 3_775 ? C1 N1 C2 109.4(4) . . ? C1 N1 C12 126.9(4) . . ? C2 N1 C12 123.7(4) . . ? C1 N2 C3 109.7(4) . . ? C1 N2 C4 126.0(4) . . ? C3 N2 C4 124.2(4) . . ? C10 N3 C11 124.3(5) . . ? C10 N3 H3A 117.8 . . ? C11 N3 H3A 117.8 . . ? N1 C1 N2 105.9(4) . . ? N1 C1 Ag1 131.2(3) . . ? N2 C1 Ag1 122.5(3) . . ? C3 C2 N1 107.4(4) . . ? C3 C2 H2 126.3 . . ? N1 C2 H2 126.3 . . ? C2 C3 N2 107.6(4) . . ? C2 C3 H3 126.2 . . ? N2 C3 H3 126.2 . . ? N2 C4 C5 112.5(4) . . ? N2 C4 H4A 109.1 . . ? C5 C4 H4A 109.1 . . ? N2 C4 H4B 109.1 . . ? C5 C4 H4B 109.1 . . ? H4A C4 H4B 107.8 . . ? C6 C5 C10 120.9(4) . . ? C6 C5 C4 117.7(4) . . ? C10 C5 C4 121.4(4) . . ? C5 C6 C7 119.6(6) . . ? C5 C6 H6 120.2 . . ? C7 C6 H6 120.2 . . ? C8 C7 C6 118.9(6) . . ? C8 C7 H7 120.6 . . ? C6 C7 H7 120.6 . . ? C9 C8 C7 121.6(6) . . ? C9 C8 H8 119.2 . . ? C7 C8 H8 119.2 . . ? C8 C9 C10 121.8(6) . . ? C8 C9 H9 119.1 . . ? C10 C9 H9 119.1 . . ? N3 C10 C5 120.9(4) . . ? N3 C10 C9 121.8(5) . . ? C5 C10 C9 117.2(5) . . ? N3 C11 H11A 109.5 . . ? N3 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N3 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C14 C12 C13 111.1(8) . . ? C14 C12 N1 109.3(5) . . ? C13 C12 N1 110.3(5) . . ? C14 C12 C15 111.2(8) . . ? C13 C12 C15 104.5(7) . . ? N1 C12 C15 110.4(5) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? _refine_diff_density_max 1.201 _refine_diff_density_min -0.800 _refine_diff_density_rms 0.097 _shelxl_version_number 2013-2 _shelx_res_file ; TITL a20712a in P2(1)/c CELL 0.71073 12.8683 12.3159 11.0777 90.000 108.620 90.000 ZERR 2.00 0.0051 0.0050 0.0045 0.000 0.005 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N Cl Ag Br UNIT 60 84 12 2 4 2 OMIT -2.00 52.02 L.S. 8 ACTA BOND $H FMAP 2 PLAN 4 eadp br1 cl1 exyz br1 cl1 size 0.45 0.40 0.18 TEMP 20 WGHT 0.087300 EXTI 0.002071 FVAR 0.18893 AG1 5 0.955198 1.016060 0.151152 11.00000 0.06850 0.06852 = 0.08692 0.00964 0.05084 0.00199 BR1 6 1.129928 1.054454 0.121945 10.50000 0.07192 0.12611 = 0.09305 -0.03267 0.04620 -0.03278 CL1 4 1.129928 1.054454 0.121945 10.50000 0.07192 0.12611 = 0.09305 -0.03267 0.04620 -0.03278 N1 3 0.819877 1.051748 0.341525 11.00000 0.05127 0.07101 = 0.04121 0.00104 0.01818 -0.00620 N2 3 0.782441 0.900402 0.240098 11.00000 0.04568 0.06307 = 0.04357 0.00304 0.01717 -0.00444 N3 3 0.635338 0.947580 -0.041041 11.00000 0.05439 0.06502 = 0.06742 0.01161 0.00801 0.00268 AFIX 43 H3A 2 0.697747 0.969001 0.009306 11.00000 -1.20000 AFIX 0 C1 1 0.841337 0.992479 0.250211 11.00000 0.04223 0.06675 = 0.04212 0.00821 0.01345 0.00204 C2 1 0.749728 0.994343 0.390244 11.00000 0.06468 0.09820 = 0.05643 -0.01194 0.03587 -0.01529 AFIX 43 H2 2 0.724054 1.016599 0.455802 11.00000 -1.20000 AFIX 0 C3 1 0.725989 0.902102 0.326405 11.00000 0.06006 0.08722 = 0.06117 0.00316 0.03062 -0.01580 AFIX 43 H3 2 0.679476 0.848113 0.337850 11.00000 -1.20000 AFIX 0 C4 1 0.779474 0.811224 0.153784 11.00000 0.05267 0.06235 = 0.05913 0.00646 0.01926 0.00444 AFIX 23 H4A 2 0.815820 0.748775 0.202564 11.00000 -1.20000 H4B 2 0.819686 0.831642 0.096640 11.00000 -1.20000 AFIX 0 C5 1 0.663503 0.779831 0.075757 11.00000 0.05491 0.05711 = 0.05498 -0.00573 0.02490 -0.00458 C6 1 0.624726 0.681210 0.100578 11.00000 0.08007 0.06593 = 0.07041 -0.00378 0.02711 -0.01260 AFIX 43 H6 2 0.668744 0.636490 0.164106 11.00000 -1.20000 AFIX 0 C7 1 0.518143 0.648248 0.029427 11.00000 0.10378 0.08800 = 0.09543 -0.02207 0.04085 -0.04682 AFIX 43 H7 2 0.490405 0.582244 0.046173 11.00000 -1.20000 AFIX 0 C8 1 0.456084 0.714723 -0.064606 11.00000 0.07847 0.11352 = 0.07478 -0.02026 0.01898 -0.03604 AFIX 43 H8 2 0.385987 0.692726 -0.112861 11.00000 -1.20000 AFIX 0 C9 1 0.493475 0.810384 -0.088970 11.00000 0.06036 0.09435 = 0.05702 -0.00931 0.01710 -0.00451 AFIX 43 H9 2 0.448780 0.853447 -0.153869 11.00000 -1.20000 AFIX 0 C10 1 0.598436 0.847868 -0.019357 11.00000 0.04915 0.06436 = 0.05005 -0.00879 0.02010 0.00024 C11 1 0.576597 1.019298 -0.142744 11.00000 0.08496 0.08000 = 0.06916 0.01023 0.01982 0.01690 AFIX 137 H11A 2 0.560628 0.982080 -0.222753 11.00000 -1.50000 H11B 2 0.620735 1.082066 -0.143088 11.00000 -1.50000 H11C 2 0.509301 1.041521 -0.130135 11.00000 -1.50000 AFIX 0 C12 1 0.866034 1.160748 0.389371 11.00000 0.06001 0.07187 = 0.05273 -0.00552 0.01839 -0.00470 C13 1 0.879997 1.225877 0.284979 11.00000 0.35222 0.07143 = 0.13993 -0.02138 0.13216 -0.03702 AFIX 137 H13A 2 0.896933 1.299432 0.313057 11.00000 -1.50000 H13B 2 0.813406 1.224449 0.214087 11.00000 -1.50000 H13C 2 0.938802 1.196434 0.259379 11.00000 -1.50000 AFIX 0 C14 1 0.967117 1.147204 0.488130 11.00000 0.16266 0.07200 = 0.33123 -0.02601 -0.14449 -0.00361 AFIX 137 H14A 2 1.019019 1.112904 0.454548 11.00000 -1.50000 H14B 2 0.956145 1.102649 0.554135 11.00000 -1.50000 H14C 2 0.994668 1.216884 0.522615 11.00000 -1.50000 AFIX 0 C15 1 0.785681 1.224452 0.434952 11.00000 0.15634 0.10533 = 0.21632 -0.05269 0.09815 -0.02029 AFIX 137 H15A 2 0.787752 1.198674 0.517473 11.00000 -1.50000 H15B 2 0.713108 1.215249 0.376054 11.00000 -1.50000 H15C 2 0.805020 1.299994 0.440351 11.00000 -1.50000 AFIX 0 HKLF 4 REM a20712a in P2(1)/c REM R1 = 0.0457 for 2298 Fo > 4sig(Fo) and 0.0629 for all 3258 data REM 186 parameters refined using 0 restraints END WGHT 0.0873 0.0000 REM Highest difference peak 1.201, deepest hole -0.800, 1-sigma level 0.097 Q1 1 0.9001 1.0055 0.0870 11.00000 0.05 1.20 Q2 1 0.9710 0.9972 0.1686 11.00000 0.05 0.70 Q3 1 0.8621 1.1724 0.5201 11.00000 0.05 0.46 Q4 1 0.9770 1.1644 0.5211 11.00000 0.05 0.45 ; _shelx_res_checksum 83793 _shelx_hkl_file ; -9 0 -8 1.34 1.10 -9 1 -8 -0.61 1.03 -8 1 -8 0.02 0.92 -7 1 -8 0.02 0.88 -9 2 -8 1.12 0.84 -8 2 -8 1.68 0.95 -7 2 -8 3.57 0.96 -9 3 -8 -0.38 0.94 -8 3 -8 0.02 0.87 -7 3 -8 0.88 0.89 -6 3 -8 1.20 0.85 -8 4 -8 0.10 0.89 -7 4 -8 1.87 0.93 -6 4 -8 5.64 1.05 -8 5 -8 -0.59 0.83 -7 5 -8 0.56 0.86 -6 5 -8 0.88 0.85 -5 5 -8 1.48 0.83 -8 6 -8 -0.20 0.88 -7 6 -8 2.60 0.99 -6 6 -8 3.10 0.99 -5 6 -8 5.22 1.00 -8 7 -8 0.82 1.02 -7 7 -8 0.88 0.94 -6 7 -8 0.91 0.87 -5 7 -8 0.45 0.79 -7 8 -8 0.08 0.95 -6 8 -8 0.37 0.90 -10 -2 -7 -0.05 1.10 -9 -2 -7 -0.09 0.96 -8 -2 -7 0.34 0.99 -10 -1 -7 -1.17 0.95 -9 -1 -7 -0.27 0.95 -8 -1 -7 1.30 0.98 -7 -1 -7 2.03 0.93 -10 0 -7 -1.04 0.97 -9 0 -7 -0.47 0.87 -8 0 -7 -0.18 0.85 -7 0 -7 0.11 0.67 -6 0 -7 0.20 0.82 -10 1 -7 -0.42 0.99 -9 1 -7 -0.28 0.97 -8 1 -7 1.07 0.92 -7 1 -7 1.72 0.90 -6 1 -7 1.96 0.79 -5 1 -7 0.77 0.73 -10 2 -7 -0.45 1.00 -9 2 -7 0.88 0.97 -8 2 -7 0.86 0.90 -7 2 -7 3.77 0.94 -6 2 -7 0.97 0.76 -5 2 -7 2.44 0.78 -4 2 -7 0.49 0.70 -10 3 -7 3.23 1.13 -9 3 -7 0.08 0.89 -8 3 -7 0.05 0.84 -7 3 -7 0.87 0.83 -6 3 -7 -0.06 0.56 -5 3 -7 0.18 0.53 -4 3 -7 2.33 0.73 -9 4 -7 -0.31 0.84 -8 4 -7 1.33 0.77 -7 4 -7 5.76 1.06 -6 4 -7 2.90 0.85 -5 4 -7 0.78 0.69 -4 4 -7 -0.21 0.70 -9 5 -7 0.05 0.93 -8 5 -7 0.76 0.90 -7 5 -7 0.84 0.83 -6 5 -7 2.70 0.73 -5 5 -7 9.39 0.96 -4 5 -7 3.60 0.78 -9 6 -7 0.36 0.95 -8 6 -7 1.26 0.92 -7 6 -7 3.72 0.99 -6 6 -7 1.25 0.81 -5 6 -7 2.12 0.77 -4 6 -7 2.51 0.78 -9 7 -7 1.01 1.06 -8 7 -7 1.41 1.03 -7 7 -7 -0.71 0.77 -6 7 -7 4.23 0.90 -5 7 -7 3.73 0.87 -4 7 -7 3.80 0.80 -8 8 -7 0.94 0.97 -7 8 -7 0.21 0.89 -6 8 -7 2.21 0.85 -5 8 -7 4.17 0.85 -4 8 -7 2.07 0.80 -11 -4 -6 1.56 1.32 -10 -4 -6 0.62 1.07 -9 -4 -6 -0.17 1.04 -11 -3 -6 -0.43 1.09 -10 -3 -6 -0.46 0.98 -9 -3 -6 1.38 0.98 -8 -3 -6 0.34 0.96 -7 -3 -6 6.13 1.02 -11 -2 -6 -0.11 1.15 -10 -2 -6 -0.82 0.94 -9 -2 -6 1.78 0.96 -8 -2 -6 2.86 0.96 -7 -2 -6 16.22 1.29 -6 -2 -6 8.71 1.09 -11 -1 -6 -0.83 1.10 -10 -1 -6 -0.51 1.04 -9 -1 -6 -0.41 0.94 -8 -1 -6 -0.09 0.87 -7 -1 -6 1.18 0.85 -6 -1 -6 5.31 0.95 -5 -1 -6 7.07 0.96 -11 0 -6 -0.84 1.04 -10 0 -6 -0.45 0.93 -9 0 -6 2.16 0.97 -8 0 -6 11.66 1.25 -7 0 -6 4.22 0.97 -6 0 -6 70.13 2.14 -5 0 -6 2.80 0.83 -4 0 -6 2.14 0.62 -11 1 -6 -0.59 1.03 -10 1 -6 -0.45 0.95 -9 1 -6 -0.12 0.90 -8 1 -6 0.18 0.83 -7 1 -6 1.60 0.84 -6 1 -6 5.93 0.96 -5 1 -6 5.76 0.88 -4 1 -6 4.20 0.78 -11 2 -6 0.09 1.06 -10 2 -6 -0.46 0.93 -9 2 -6 1.30 0.91 -8 2 -6 3.19 0.93 -7 2 -6 16.19 1.22 -6 2 -6 8.06 0.97 -5 2 -6 12.83 1.10 -4 2 -6 7.25 0.85 -3 2 -6 7.60 0.83 -11 3 -6 -0.95 0.70 -10 3 -6 0.09 0.82 -9 3 -6 1.18 0.84 -8 3 -6 0.68 0.66 -7 3 -6 5.72 0.97 -6 3 -6 3.32 0.83 -5 3 -6 0.11 0.72 -4 3 -6 5.13 0.82 -3 3 -6 1.69 0.55 -10 4 -6 -0.48 0.82 -9 4 -6 -0.49 0.75 -8 4 -6 1.23 0.79 -7 4 -6 7.90 1.01 -6 4 -6 7.26 0.95 -5 4 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-8 -1 12 0.48 0.91 -7 -1 12 0.02 0.86 -6 -1 12 -0.13 0.82 -5 -1 12 0.18 0.89 -4 -1 12 0.48 0.92 -3 -1 12 -0.27 0.81 -2 -1 12 0.56 0.92 -1 -1 12 0.80 0.96 0 -1 12 1.12 0.98 1 -1 12 -0.11 0.98 2 -1 12 0.75 0.85 3 -1 12 1.06 0.91 -12 0 12 1.33 1.29 -11 0 12 -0.39 1.07 -10 0 12 4.36 1.14 -9 0 12 -0.13 0.95 -8 0 12 0.03 0.87 -7 0 12 -0.17 0.82 -6 0 12 12.10 1.28 -5 0 12 26.40 1.60 -4 0 12 26.59 1.56 -3 0 12 5.95 0.93 -2 0 12 2.71 0.87 -1 0 12 3.71 0.95 0 0 12 1.40 0.85 1 0 12 1.97 0.94 2 0 12 0.37 0.81 3 0 12 1.05 0.86 -11 1 12 -0.04 1.02 -10 1 12 0.92 1.01 -9 1 12 1.30 0.89 -8 1 12 0.44 0.88 -7 1 12 -0.05 0.84 -6 1 12 0.26 0.97 -5 1 12 0.25 0.86 -4 1 12 0.22 0.62 -3 1 12 -0.23 0.82 -2 1 12 1.19 0.94 -1 1 12 0.46 0.89 0 1 12 0.44 0.94 1 1 12 0.05 0.90 2 1 12 -0.44 0.89 -11 2 12 -0.51 1.07 -10 2 12 -0.87 0.93 -9 2 12 1.18 0.97 -8 2 12 -0.30 0.69 -7 2 12 2.06 0.98 -6 2 12 8.97 1.19 -5 2 12 18.64 1.42 -4 2 12 19.81 1.03 -3 2 12 3.32 0.70 -2 2 12 4.35 1.03 -1 2 12 3.36 1.02 0 2 12 0.15 0.85 1 2 12 0.17 0.92 2 2 12 0.45 0.82 -11 3 12 1.45 1.18 -10 3 12 5.74 1.09 -9 3 12 5.26 1.31 -8 3 12 1.65 1.01 -7 3 12 2.20 0.99 -6 3 12 0.19 0.86 -5 3 12 1.08 0.87 -4 3 12 0.07 0.55 -3 3 12 0.24 0.57 -2 3 12 0.41 0.84 -1 3 12 0.50 0.84 0 3 12 0.62 0.89 1 3 12 -0.37 0.85 2 3 12 0.92 0.94 -10 4 12 0.51 1.18 -9 4 12 0.68 1.05 -8 4 12 0.33 0.95 -7 4 12 8.16 1.12 -6 4 12 14.54 1.30 -5 4 12 9.17 1.11 -4 4 12 8.12 0.77 -3 4 12 1.41 0.62 -2 4 12 1.78 0.61 -1 4 12 0.36 0.91 0 4 12 0.93 0.96 1 4 12 0.42 0.91 2 4 12 0.09 0.91 -10 5 12 3.97 1.26 -9 5 12 9.02 1.33 -8 5 12 5.69 1.15 -7 5 12 0.84 0.90 -6 5 12 0.91 0.84 -5 5 12 1.35 0.79 -4 5 12 0.84 0.60 -3 5 12 -0.16 0.56 -2 5 12 0.22 0.57 -1 5 12 1.05 0.94 0 5 12 0.21 0.95 1 5 12 0.84 0.97 -8 6 12 4.89 1.13 -7 6 12 4.24 1.05 -6 6 12 8.86 1.14 -5 6 12 4.07 0.94 -4 6 12 0.36 0.56 -3 6 12 -0.01 0.58 -2 6 12 1.41 0.59 -1 6 12 0.40 0.58 0 6 12 -0.17 1.00 -7 7 12 1.08 0.94 -6 7 12 -0.24 0.86 -5 7 12 0.40 0.80 -4 7 12 0.09 0.63 -3 7 12 0.00 0.60 -2 7 12 0.40 0.63 -1 7 12 -0.09 1.07 -3 8 12 0.56 0.63 -2 8 12 0.06 1.01 -3 -6 13 1.99 1.04 -3 -5 13 0.49 1.00 -2 -5 13 0.45 1.14 -10 -4 13 2.61 1.43 -9 -4 13 3.26 1.38 -3 -4 13 3.24 1.13 -2 -4 13 0.83 0.98 -1 -4 13 1.26 1.07 -10 -3 13 10.12 1.65 -9 -3 13 6.58 1.53 -8 -3 13 5.23 1.40 -3 -3 13 2.09 1.08 -2 -3 13 2.24 1.08 -1 -3 13 0.09 1.00 0 -3 13 -0.30 0.97 -10 -2 13 1.32 1.27 -9 -2 13 0.96 1.18 -8 -2 13 1.45 1.20 -7 -2 13 0.44 1.02 -3 -2 13 2.36 1.06 -2 -2 13 3.03 1.16 -1 -2 13 0.64 1.06 0 -2 13 0.08 1.02 -10 -1 13 9.93 1.53 -9 -1 13 8.56 1.35 -8 -1 13 4.79 1.25 -7 -1 13 2.14 1.10 -3 -1 13 5.62 1.16 -2 -1 13 0.13 0.94 -1 -1 13 0.37 0.95 0 -1 13 1.14 1.03 -10 0 13 -0.55 1.08 -9 0 13 -0.36 1.09 -8 0 13 0.07 0.99 -7 0 13 0.09 0.98 -6 0 13 -0.18 0.87 -3 0 13 1.55 1.05 -2 0 13 0.08 0.92 -1 0 13 0.67 0.81 0 0 13 -0.49 0.76 -10 1 13 8.14 1.27 -9 1 13 7.63 1.37 -8 1 13 5.36 1.12 -7 1 13 1.99 1.00 -6 1 13 -0.30 0.87 -5 1 13 2.90 1.18 -3 1 13 5.47 1.11 -2 1 13 1.02 0.96 -1 1 13 -0.45 0.91 0 1 13 1.01 1.01 -10 2 13 1.03 1.14 -9 2 13 0.68 1.07 -8 2 13 1.06 0.99 -7 2 13 -0.09 1.05 -6 2 13 0.96 0.98 -5 2 13 -0.36 0.91 -3 2 13 1.88 1.02 -2 2 13 1.89 1.05 -1 2 13 0.10 0.93 0 2 13 -0.32 1.01 -9 3 13 8.02 1.44 -8 3 13 4.72 1.21 -7 3 13 -0.54 0.91 -6 3 13 0.24 1.00 -5 3 13 3.00 1.03 -4 3 13 6.03 1.15 -3 3 13 2.05 0.99 -2 3 13 0.89 0.92 -1 3 13 0.22 0.90 0 3 13 -0.62 0.94 -8 4 13 -0.45 1.01 -7 4 13 -0.73 0.89 -6 4 13 -0.47 0.91 -5 4 13 0.20 0.87 -4 4 13 2.11 0.97 -3 4 13 2.72 1.00 -2 4 13 0.47 0.89 -1 4 13 0.68 1.00 -7 5 13 -0.57 0.97 -6 5 13 1.51 0.98 -5 5 13 0.27 0.88 -4 5 13 1.24 0.91 -3 5 13 0.32 0.65 -2 5 13 0.21 1.02 -5 6 13 1.14 0.97 -4 6 13 2.45 0.98 -3 6 13 1.14 0.69 -2 6 13 0.46 0.69 -3 -3 14 1.14 1.13 -3 -2 14 -0.16 1.08 -8 -1 14 -0.11 1.16 -3 -1 14 0.62 1.13 -2 -1 14 0.50 1.17 -8 0 14 9.21 1.52 -7 0 14 3.58 1.30 -3 0 14 1.11 1.15 -2 0 14 0.38 1.09 -8 1 14 1.19 1.17 -7 1 14 -0.19 1.05 -3 1 14 0.23 0.85 -2 1 14 0.20 0.87 -7 2 14 0.69 1.08 -6 2 14 0.00 1.13 -3 2 14 -0.10 1.00 -6 3 14 -0.86 1.00 -3 3 14 1.56 1.11 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 43062 _database_code_depnum_ccdc_archive 'CCDC 933724' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_a01003as _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H63 Ag4 Br4 P4' _chemical_formula_weight 1803.22 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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 '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 24.39(8) _cell_length_b 12.08(3) _cell_length_c 48.24(13) _cell_angle_alpha 90 _cell_angle_beta 100.90(7) _cell_angle_gamma 90 _cell_volume 13960(7) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 899 _cell_measurement_theta_min 2.448 _cell_measurement_theta_max 24.115 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.716 _exptl_crystal_F_000 7064 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.180 _exptl_crystal_size_min 0.120 _exptl_absorpt_coefficient_mu 3.527 _shelx_estimated_absorpt_T_min 0.539 _shelx_estimated_absorpt_T_max 0.677 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6426 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source ? _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 23746 _diffrn_reflns_av_unetI/netI 0.0763 _diffrn_reflns_av_R_equivalents 0.0524 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -52 _diffrn_reflns_limit_l_max 57 _diffrn_reflns_theta_min 1.720 _diffrn_reflns_theta_max 25.009 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.990 _diffrn_measured_fraction_theta_full 0.964 _diffrn_reflns_Laue_measured_fraction_max 0.990 _diffrn_reflns_Laue_measured_fraction_full 0.964 _diffrn_reflns_point_group_measured_fraction_max 0.990 _diffrn_reflns_point_group_measured_fraction_full 0.964 _reflns_number_total 12185 _reflns_number_gt 6816 _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 SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1453P)^2^] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 12185 _refine_ls_number_parameters 783 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.1182 _refine_ls_R_factor_gt 0.0753 _refine_ls_wR_factor_ref 0.2444 _refine_ls_wR_factor_gt 0.2256 _refine_ls_goodness_of_fit_ref 0.994 _refine_ls_restrained_S_all 0.994 _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 Ag1 Ag 0.14532(4) 0.90131(9) 0.12478(2) 0.0725(3) Uani 1 1 d . . . . . Ag2 Ag 0.16461(3) 1.13235(7) 0.07394(2) 0.0553(3) Uani 1 1 d . . . . . Ag3 Ag 0.23858(4) 1.12375(9) 0.14987(2) 0.0717(3) Uani 1 1 d . . . . . Ag4 Ag 0.26878(3) 0.90459(7) 0.10054(2) 0.0562(3) Uani 1 1 d . . . . . Br1 Br 0.27475(5) 1.11905(11) 0.09825(3) 0.0701(4) Uani 1 1 d . . . . . Br2 Br 0.15494(5) 0.90947(11) 0.07125(3) 0.0699(4) Uani 1 1 d . . . . . Br3 Br 0.13412(6) 1.14262(12) 0.12641(3) 0.0749(4) Uani 1 1 d . . . . . Br4 Br 0.25048(6) 0.89216(12) 0.15619(3) 0.0740(4) Uani 1 1 d . . . . . P1 P 0.11767(10) 1.2440(2) 0.03554(6) 0.0416(6) Uani 1 1 d . . . . . P2 P 0.08047(12) 0.8007(3) 0.14694(6) 0.0533(8) Uani 1 1 d . . . . . P3 P 0.31391(11) 0.7420(2) 0.08756(6) 0.0428(6) Uani 1 1 d . . . . . P4 P 0.29947(13) 1.2063(3) 0.18929(7) 0.0656(9) Uani 1 1 d . . . . . C1 C 0.1614(4) 1.3164(8) 0.0146(2) 0.043(2) Uani 1 1 d . . . . . C2 C 0.2169(4) 1.3380(9) 0.0272(3) 0.057(3) Uani 1 1 d . . . . . H2A H 0.2308 1.3170 0.0457 0.069 Uiso 1 1 calc R U . . . C3 C 0.2500(5) 1.3901(10) 0.0117(3) 0.066(3) Uani 1 1 d . . . . . H3A H 0.2866 1.4072 0.0201 0.079 Uiso 1 1 calc R U . . . C4 C 0.2313(6) 1.4177(11) -0.0155(4) 0.084(5) Uani 1 1 d . . . . . H4A H 0.2554 1.4518 -0.0256 0.101 Uiso 1 1 calc R U . . . C5 C 0.1775(6) 1.3964(9) -0.0284(3) 0.069(3) Uani 1 1 d . . . . . H5A H 0.1650 1.4153 -0.0473 0.083 Uiso 1 1 calc R U . . . C6 C 0.1423(5) 1.3469(10) -0.0132(2) 0.061(3) Uani 1 1 d . . . . . H6A H 0.1053 1.3337 -0.0216 0.073 Uiso 1 1 calc R U . . . C7 C 0.0717(4) 1.1663(8) 0.0082(2) 0.042(2) Uani 1 1 d . . . . . C8 C 0.0928(4) 1.0708(8) -0.0023(2) 0.047(3) Uani 1 1 d . . . . . H8A H 0.1290 1.0480 0.0052 0.056 Uiso 1 1 calc R U . . . C9 C 0.0610(6) 1.0098(10) -0.0236(2) 0.063(3) Uani 1 1 d . . . . . H9A H 0.0761 0.9470 -0.0304 0.075 Uiso 1 1 calc R U . . . C10 C 0.0052(6) 1.0422(12) -0.0353(3) 0.073(4) Uani 1 1 d . . . . . H10A H -0.0163 1.0021 -0.0499 0.087 Uiso 1 1 calc R U . . . C11 C -0.0152(4) 1.1315(11) -0.0248(3) 0.060(3) Uani 1 1 d . . . . . H11A H -0.0522 1.1511 -0.0315 0.072 Uiso 1 1 calc R U . . . C12 C 0.0173(4) 1.1982(9) -0.0035(2) 0.053(3) Uani 1 1 d . . . . . H12A H 0.0024 1.2626 0.0026 0.063 Uiso 1 1 calc R U . . . C13 C 0.0717(4) 1.3479(9) 0.0459(2) 0.050(3) Uani 1 1 d . . . . . C14 C 0.0660(6) 1.4520(10) 0.0359(3) 0.079(4) Uani 1 1 d . . . . . H14A H 0.0858 1.4746 0.0222 0.095 Uiso 1 1 calc R U . . . C15 C 0.0310(7) 1.5251(12) 0.0458(4) 0.092(5) Uani 1 1 d . . . . . H15A H 0.0283 1.5972 0.0389 0.111 Uiso 1 1 calc R U . . . C16 C 0.0011(6) 1.4963(11) 0.0649(3) 0.074(4) Uani 1 1 d . . . . . H16A H -0.0231 1.5470 0.0708 0.089 Uiso 1 1 calc R U . . . C17 C 0.0058(5) 1.3923(13) 0.0758(3) 0.078(4) Uani 1 1 d . . . . . H17A H -0.0159 1.3710 0.0889 0.093 Uiso 1 1 calc R U . . . C18 C 0.0435(5) 1.3165(10) 0.0675(2) 0.058(3) Uani 1 1 d . . . . . H18A H 0.0495 1.2475 0.0760 0.069 Uiso 1 1 calc R U . . . C19 C 0.0098(4) 0.7968(9) 0.1266(2) 0.046(3) Uani 1 1 d . . . . . C20 C 0.0024(5) 0.7939(10) 0.0979(3) 0.061(3) Uani 1 1 d . . . . . H20A H 0.0334 0.7948 0.0893 0.074 Uiso 1 1 calc R U . . . C21 C -0.0509(5) 0.7896(11) 0.0814(3) 0.074(4) Uani 1 1 d . . . . . H21A H -0.0555 0.7892 0.0618 0.089 Uiso 1 1 calc R U . . . C22 C -0.0960(5) 0.7862(12) 0.0941(3) 0.070(4) Uani 1 1 d . . . . . H22A H -0.1313 0.7771 0.0830 0.084 Uiso 1 1 calc R U . . . C23 C -0.0911(6) 0.7956(16) 0.1222(3) 0.102(5) Uani 1 1 d . . . . . H23A H -0.1100 0.7329 0.1287 0.122 Uiso 1 1 calc R U . . . H23B H -0.1111 0.8617 0.1259 0.122 Uiso 1 1 calc R U . . . C24 C -0.0353(6) 0.8013(17) 0.1391(3) 0.104(6) Uani 1 1 d . . . . . H24A H -0.0305 0.8080 0.1587 0.125 Uiso 1 1 calc R U . . . C25 C 0.0748(4) 0.8615(11) 0.1808(2) 0.056(3) Uani 1 1 d . . . . . C26 C 0.0850(6) 0.9674(13) 0.1845(3) 0.079(4) Uani 1 1 d . . . . . H26A H 0.0966 1.0066 0.1700 0.094 Uiso 1 1 calc R U . . . C27 C 0.0793(8) 1.0253(14) 0.2091(4) 0.107(6) Uani 1 1 d . . . . . H27A H 0.0853 1.1013 0.2104 0.129 Uiso 1 1 calc R U . . . C28 C 0.0658(8) 0.9725(18) 0.2297(4) 0.111(6) Uani 1 1 d . . . . . H28A H 0.0644 1.0096 0.2465 0.134 Uiso 1 1 calc R U . . . C29 C 0.0528(6) 0.8579(18) 0.2275(3) 0.098(6) Uani 1 1 d . . . . . H29A H 0.0413 0.8203 0.2422 0.118 Uiso 1 1 calc R U . . . C30 C 0.0579(5) 0.8019(11) 0.2020(2) 0.068(3) Uani 1 1 d . . . . . H30A H 0.0499 0.7268 0.1997 0.082 Uiso 1 1 calc R U . . . C31 C 0.0966(5) 0.6570(10) 0.1550(3) 0.059(3) Uani 1 1 d . . . . . C32 C 0.0675(6) 0.5703(13) 0.1415(3) 0.082(4) Uani 1 1 d . . . . . H32A H 0.0371 0.5837 0.1271 0.098 Uiso 1 1 calc R U . . . C33 C 0.0827(8) 0.4621(14) 0.1490(4) 0.107(5) Uani 1 1 d . . . . . H33A H 0.0626 0.4052 0.1387 0.128 Uiso 1 1 calc R U . . . C34 C 0.1245(9) 0.4348(17) 0.1700(4) 0.114(6) Uani 1 1 d . . . . . H34A H 0.1329 0.3615 0.1750 0.137 Uiso 1 1 calc R U . . . C35 C 0.1544(8) 0.5215(19) 0.1837(5) 0.139(8) Uani 1 1 d . . . . . H35A H 0.1838 0.5061 0.1985 0.166 Uiso 1 1 calc R U . . . C36 C 0.1422(6) 0.6350(13) 0.1761(4) 0.106(6) Uani 1 1 d . . . . . H36A H 0.1643 0.6920 0.1850 0.127 Uiso 1 1 calc R U . . . C37 C 0.3261(4) 0.7399(8) 0.0510(2) 0.048(3) Uani 1 1 d . . . . . C38 C 0.3627(5) 0.8177(11) 0.0440(3) 0.072(4) Uani 1 1 d . . . . . H38A H 0.3806 0.8654 0.0580 0.086 Uiso 1 1 calc R U . . . C39 C 0.3739(6) 0.8274(11) 0.0170(3) 0.080(4) Uani 1 1 d . . . . . H39A H 0.3990 0.8800 0.0129 0.096 Uiso 1 1 calc R U . . . C40 C 0.3468(6) 0.7571(12) -0.0036(3) 0.074(4) Uani 1 1 d . . . . . H40A H 0.3526 0.7643 -0.0220 0.089 Uiso 1 1 calc R U . . . C41 C 0.3120(5) 0.6777(11) 0.0026(2) 0.064(3) Uani 1 1 d . . . . . H41A H 0.2951 0.6283 -0.0112 0.077 Uiso 1 1 calc R U . . . C42 C 0.3019(4) 0.6714(10) 0.0298(3) 0.057(3) Uani 1 1 d . . . . . H42A H 0.2773 0.6176 0.0338 0.069 Uiso 1 1 calc R U . . . C43 C 0.3837(4) 0.7165(8) 0.1078(2) 0.045(2) Uani 1 1 d . . . . . C44 C 0.4203(5) 0.6441(10) 0.1007(3) 0.064(3) Uani 1 1 d . . . . . H44A H 0.4098 0.6021 0.0844 0.077 Uiso 1 1 calc R U . . . C45 C 0.4729(5) 0.6300(10) 0.1167(4) 0.077(4) Uani 1 1 d . . . . . H45A H 0.4977 0.5808 0.1107 0.092 Uiso 1 1 calc R U . . . C46 C 0.4882(5) 0.6859(12) 0.1403(3) 0.075(4) Uani 1 1 d . . . . . H46A H 0.5241 0.6760 0.1506 0.090 Uiso 1 1 calc R U . . . C47 C 0.4532(5) 0.7583(13) 0.1504(3) 0.079(4) Uani 1 1 d . . . . . H47A H 0.4639 0.7946 0.1675 0.095 Uiso 1 1 calc R U . . . C48 C 0.4005(5) 0.7745(10) 0.1335(3) 0.064(3) Uani 1 1 d . . . . . H48A H 0.3760 0.8245 0.1393 0.076 Uiso 1 1 calc R U . . . C49 C 0.2734(4) 0.6201(8) 0.0916(2) 0.046(3) Uani 1 1 d . . . . . C50 C 0.2965(5) 0.5124(9) 0.0957(3) 0.063(3) Uani 1 1 d . . . . . H50A H 0.3340 0.5014 0.0953 0.076 Uiso 1 1 calc R U . . . C51 C 0.2641(6) 0.4243(9) 0.1003(3) 0.071(4) Uani 1 1 d . . . . . H51A H 0.2800 0.3547 0.1042 0.086 Uiso 1 1 calc R U . . . C52 C 0.2068(6) 0.4402(11) 0.0991(3) 0.072(4) Uani 1 1 d . . . . . H52A H 0.1841 0.3797 0.1008 0.087 Uiso 1 1 calc R U . . . C53 C 0.1852(6) 0.5385(12) 0.0957(4) 0.088(5) Uani 1 1 d . . . . . H53A H 0.1473 0.5485 0.0953 0.106 Uiso 1 1 calc R U . . . C54 C 0.2197(5) 0.6311(10) 0.0924(3) 0.080(4) Uani 1 1 d . . . . . H54A H 0.2040 0.7015 0.0908 0.095 Uiso 1 1 calc R U . . . C55 C 0.3238(6) 1.3440(12) 0.1839(2) 0.069(4) Uani 1 1 d . . . . . C56 C 0.2832(7) 1.4181(16) 0.1723(3) 0.097(5) Uani 1 1 d . . . . . H56A H 0.2552 1.4201 0.1841 0.116 Uiso 1 1 calc R U . . . H56B H 0.2653 1.3903 0.1540 0.116 Uiso 1 1 calc R U . . . C57 C 0.3018(11) 1.5323(16) 0.1687(4) 0.119(7) Uani 1 1 d . . . . . H57A H 0.2761 1.5853 0.1606 0.142 Uiso 1 1 calc R U . . . C58 C 0.3552(14) 1.561(3) 0.1770(6) 0.156(11) Uani 1 1 d . . . . . H58A H 0.3659 1.6340 0.1758 0.187 Uiso 1 1 calc R U . . . C59 C 0.3940(11) 1.483(2) 0.1872(5) 0.142(10) Uani 1 1 d . . . . . H59A H 0.4314 1.5033 0.1910 0.170 Uiso 1 1 calc R U . . . C60 C 0.3810(6) 1.3750(15) 0.1920(3) 0.093(5) Uani 1 1 d . . . . . H60A H 0.3926 1.3603 0.2120 0.112 Uiso 1 1 calc R U . . . H60B H 0.4029 1.3274 0.1821 0.112 Uiso 1 1 calc R U . . . C61 C 0.2718(6) 1.2158(11) 0.2218(2) 0.072(4) Uani 1 1 d . . . . . C62 C 0.2886(6) 1.2962(13) 0.2414(3) 0.089(5) Uani 1 1 d . . . . . H62A H 0.3153 1.3476 0.2385 0.106 Uiso 1 1 calc R U . . . C63 C 0.2661(8) 1.3020(17) 0.2659(3) 0.114(6) Uani 1 1 d . . . . . H63A H 0.2746 1.3612 0.2783 0.137 Uiso 1 1 calc R U . . . C64 C 0.2323(8) 1.221(2) 0.2712(4) 0.141(8) Uani 1 1 d . U . . . H64A H 0.2177 1.2224 0.2877 0.170 Uiso 1 1 calc R U . . . C65 C 0.2194(11) 1.139(2) 0.2527(4) 0.183(13) Uani 1 1 d . U . . . H65A H 0.1978 1.0808 0.2573 0.219 Uiso 1 1 calc R U . . . C66 C 0.2366(8) 1.1357(16) 0.2267(3) 0.125(8) Uani 1 1 d . . . . . H66A H 0.2244 1.0808 0.2134 0.150 Uiso 1 1 calc R U . . . C67 C 0.3667(6) 1.1324(13) 0.1954(4) 0.080(9) Uani 0.65(2) 1 d G . P A 1 C68 C 0.3849(7) 1.0893(13) 0.1736(4) 0.080(7) Uani 0.65(2) 1 d G . P A 1 H68A H 0.3631 1.0937 0.1556 0.096 Uiso 0.65(2) 1 calc R U P A 1 C69 C 0.4343(8) 1.0400(13) 0.1774(5) 0.102(11) Uani 0.65(2) 1 d G . P A 1 H69A H 0.4471 1.0097 0.1621 0.122 Uiso 0.65(2) 1 calc R U P A 1 C70 C 0.4654(7) 1.0338(15) 0.2030(5) 0.133(14) Uani 0.65(2) 1 d G . P A 1 H70A H 0.5000 0.9991 0.2057 0.159 Uiso 0.65(2) 1 calc R U P A 1 C71 C 0.4471(8) 1.0768(18) 0.2248(5) 0.17(2) Uani 0.65(2) 1 d G U P A 1 H71A H 0.4689 1.0724 0.2428 0.210 Uiso 0.65(2) 1 calc R U P A 1 C72 C 0.3977(8) 1.1261(16) 0.2210(4) 0.134(13) Uani 0.65(2) 1 d G U P A 1 H72A H 0.3849 1.1564 0.2363 0.161 Uiso 0.65(2) 1 calc R U P A 1 C67' C 0.3608(6) 1.1045(15) 0.2058(4) 0.085(17) Uani 0.35(2) 1 d G . P A 2 C68' C 0.3923(5) 1.0847(9) 0.1895(3) 0.10(2) Uani 0.35(2) 1 d G U P A 2 H68B H 0.3883 1.1226 0.1724 0.126 Uiso 0.35(2) 1 calc R U P A 2 C69' C 0.4290(6) 1.0150(10) 0.1956(4) 0.27(9) Uani 0.35(2) 1 d G . P A 2 H69B H 0.4530 1.0000 0.1831 0.321 Uiso 0.35(2) 1 calc R U P A 2 C70' C 0.4342(9) 0.9650(17) 0.2180(4) 0.17(5) Uani 0.35(2) 1 d G . P A 2 H70B H 0.4621 0.9120 0.2226 0.209 Uiso 0.35(2) 1 calc R U P A 2 C71' C 0.4027(12) 0.985(2) 0.2343(4) 0.25(8) Uani 0.35(2) 1 d G . P A 2 H71B H 0.4067 0.9468 0.2514 0.302 Uiso 0.35(2) 1 calc R U P A 2 C72' C 0.3660(10) 1.054(2) 0.2282(4) 0.12(2) Uani 0.35(2) 1 d G . P A 2 H72B H 0.3420 1.0695 0.2407 0.142 Uiso 0.35(2) 1 calc R U P A 2 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 Ag1 0.0614(6) 0.0893(8) 0.0722(7) 0.0037(6) 0.0264(5) -0.0174(5) Ag2 0.0572(5) 0.0522(5) 0.0527(5) 0.0138(4) 0.0007(4) 0.0087(4) Ag3 0.0665(6) 0.0865(8) 0.0571(6) -0.0162(5) -0.0011(5) -0.0065(5) Ag4 0.0543(5) 0.0403(5) 0.0760(6) -0.0047(4) 0.0176(4) 0.0082(4) Br1 0.0687(8) 0.0597(8) 0.0809(9) 0.0043(7) 0.0118(7) -0.0045(6) Br2 0.0696(8) 0.0658(8) 0.0710(9) -0.0009(7) 0.0049(6) -0.0021(6) Br3 0.0663(8) 0.0819(10) 0.0787(9) 0.0041(7) 0.0194(7) 0.0034(6) Br4 0.0715(8) 0.0842(10) 0.0660(8) 0.0098(7) 0.0126(6) -0.0021(7) P1 0.0393(14) 0.0418(15) 0.0417(15) 0.0084(12) 0.0025(11) -0.0018(11) P2 0.0457(16) 0.071(2) 0.0468(17) -0.0017(15) 0.0177(13) -0.0098(14) P3 0.0445(14) 0.0316(14) 0.0534(17) 0.0016(12) 0.0123(12) 0.0036(11) P4 0.0604(19) 0.071(2) 0.060(2) -0.0148(17) -0.0019(16) -0.0023(16) C1 0.050(6) 0.036(6) 0.044(6) -0.003(5) 0.010(5) -0.012(4) C2 0.049(7) 0.054(7) 0.069(8) -0.009(6) 0.010(6) 0.004(5) C3 0.052(7) 0.072(9) 0.076(9) -0.005(7) 0.020(6) -0.026(6) C4 0.093(11) 0.060(9) 0.119(14) -0.010(9) 0.072(10) -0.017(7) C5 0.081(9) 0.047(7) 0.083(10) 0.007(7) 0.024(7) -0.014(6) C6 0.053(7) 0.071(8) 0.058(7) 0.021(6) 0.008(6) -0.007(6) C7 0.040(5) 0.038(6) 0.052(6) 0.009(5) 0.013(5) -0.006(4) C8 0.039(5) 0.043(6) 0.056(7) 0.016(5) 0.003(5) -0.001(4) C9 0.094(10) 0.053(7) 0.043(7) -0.009(6) 0.017(7) -0.008(6) C10 0.094(10) 0.082(10) 0.039(7) -0.007(7) 0.007(7) -0.048(8) C11 0.039(6) 0.077(9) 0.061(8) 0.016(7) -0.002(5) -0.013(6) C12 0.040(6) 0.056(7) 0.059(7) 0.019(6) -0.001(5) -0.003(5) C13 0.050(6) 0.052(7) 0.044(6) 0.006(5) -0.002(5) 0.003(5) C14 0.109(11) 0.046(7) 0.089(10) 0.026(7) 0.034(8) 0.027(7) C15 0.116(12) 0.055(9) 0.107(13) 0.029(9) 0.024(10) 0.027(8) C16 0.089(10) 0.064(9) 0.070(9) 0.002(7) 0.013(8) 0.034(7) C17 0.074(9) 0.104(12) 0.063(9) 0.006(8) 0.034(7) 0.014(8) C18 0.067(7) 0.054(7) 0.059(7) 0.018(6) 0.029(6) 0.006(6) C19 0.036(5) 0.053(7) 0.050(7) -0.002(5) 0.013(5) -0.009(4) C20 0.049(7) 0.077(9) 0.059(8) 0.009(7) 0.012(6) -0.017(6) C21 0.068(8) 0.088(10) 0.062(8) 0.002(7) 0.002(7) -0.021(7) C22 0.046(7) 0.102(11) 0.057(8) 0.004(7) -0.004(6) -0.004(6) C23 0.067(9) 0.154(17) 0.084(12) 0.010(11) 0.015(8) 0.010(9) C24 0.077(10) 0.191(19) 0.046(8) 0.018(10) 0.012(7) -0.002(10) C25 0.046(6) 0.072(9) 0.052(7) 0.001(6) 0.013(5) -0.003(5) C26 0.090(10) 0.090(11) 0.055(9) 0.006(8) 0.012(7) -0.017(8) C27 0.176(18) 0.080(12) 0.075(11) -0.003(10) 0.048(12) -0.013(11) C28 0.123(15) 0.119(16) 0.081(13) -0.021(12) -0.009(11) 0.034(12) C29 0.076(10) 0.174(19) 0.053(9) 0.018(11) 0.035(7) 0.014(11) C30 0.087(9) 0.076(9) 0.045(7) -0.003(7) 0.021(6) 0.004(7) C31 0.060(7) 0.063(8) 0.059(8) -0.004(6) 0.026(6) 0.000(6) C32 0.097(10) 0.079(11) 0.069(9) 0.009(8) 0.012(8) -0.014(8) C33 0.115(14) 0.068(11) 0.136(16) -0.016(11) 0.022(12) -0.019(10) C34 0.137(17) 0.104(15) 0.104(15) 0.010(12) 0.031(13) 0.028(13) C35 0.115(15) 0.14(2) 0.141(19) -0.024(15) -0.018(13) 0.049(14) C36 0.077(10) 0.079(11) 0.145(16) -0.014(10) -0.019(10) 0.029(8) C37 0.053(6) 0.034(6) 0.062(7) 0.010(5) 0.021(5) 0.015(5) C38 0.088(9) 0.064(8) 0.063(9) -0.004(7) 0.016(7) -0.012(7) C39 0.113(11) 0.059(8) 0.079(10) 0.010(8) 0.048(9) -0.003(8) C40 0.093(10) 0.080(10) 0.054(8) 0.022(8) 0.028(7) 0.035(8) C41 0.079(8) 0.068(8) 0.040(7) -0.010(6) -0.001(6) 0.003(7) C42 0.051(6) 0.054(7) 0.064(8) -0.009(6) 0.002(6) 0.001(5) C43 0.040(5) 0.035(6) 0.061(7) 0.012(5) 0.016(5) -0.002(4) C44 0.060(7) 0.057(7) 0.075(9) 0.000(6) 0.013(6) 0.015(6) C45 0.053(8) 0.051(8) 0.128(13) 0.010(8) 0.023(8) 0.018(6) C46 0.050(7) 0.078(10) 0.092(11) 0.024(8) -0.002(7) -0.004(7) C47 0.059(8) 0.102(11) 0.071(9) -0.013(8) -0.001(7) -0.004(7) C48 0.054(7) 0.061(8) 0.077(9) -0.002(7) 0.015(6) -0.007(6) C49 0.046(6) 0.040(6) 0.056(7) 0.011(5) 0.021(5) 0.001(4) C50 0.067(7) 0.033(6) 0.088(9) -0.004(6) 0.011(7) 0.009(5) C51 0.098(10) 0.027(6) 0.080(9) 0.000(6) -0.004(8) -0.005(6) C52 0.088(10) 0.060(9) 0.072(9) -0.001(7) 0.025(7) -0.015(7) C53 0.074(9) 0.062(9) 0.136(14) 0.012(9) 0.040(9) -0.006(7) C54 0.072(9) 0.035(7) 0.136(13) -0.002(7) 0.031(8) -0.007(6) C55 0.089(9) 0.092(10) 0.031(6) -0.018(7) 0.022(6) -0.011(8) C56 0.119(13) 0.131(16) 0.044(8) -0.001(9) 0.028(8) 0.021(11) C57 0.19(2) 0.081(14) 0.090(14) 0.013(11) 0.030(14) 0.005(14) C58 0.22(4) 0.15(3) 0.11(2) 0.006(17) 0.07(2) -0.06(2) C59 0.16(2) 0.18(3) 0.105(18) -0.050(17) 0.071(16) -0.104(19) C60 0.068(9) 0.143(16) 0.076(10) -0.040(10) 0.032(8) -0.034(9) C61 0.109(11) 0.062(8) 0.043(7) 0.002(6) 0.007(7) -0.022(7) C62 0.108(11) 0.098(12) 0.063(9) -0.011(8) 0.024(8) -0.034(9) C63 0.172(18) 0.132(16) 0.042(8) 0.000(9) 0.029(10) -0.025(14) C64 0.131(16) 0.21(2) 0.097(15) -0.011(13) 0.048(12) -0.064(16) C65 0.25(3) 0.22(3) 0.087(15) -0.008(14) 0.043(16) -0.17(2) C66 0.147(16) 0.157(18) 0.069(11) -0.027(11) 0.011(10) -0.103(14) C67 0.074(16) 0.074(16) 0.082(19) 0.022(16) -0.014(13) 0.013(13) C68 0.098(18) 0.083(16) 0.063(16) -0.014(12) 0.025(13) 0.025(13) C69 0.09(2) 0.059(15) 0.15(3) -0.013(17) 0.013(18) 0.017(14) C70 0.073(19) 0.09(2) 0.24(5) 0.02(3) 0.03(2) 0.027(16) C71 0.20(4) 0.14(4) 0.15(3) -0.01(3) -0.05(3) 0.05(3) C72 0.15(3) 0.11(3) 0.11(2) -0.02(2) -0.05(2) -0.001(19) C67' 0.10(4) 0.08(4) 0.06(3) -0.01(3) -0.02(3) -0.01(3) C68' 0.10(2) 0.10(2) 0.11(2) 0.000(2) 0.020(4) 0.000(2) C69' 0.09(6) 0.5(2) 0.19(10) -0.25(13) 0.03(6) -0.11(10) C70' 0.07(4) 0.15(7) 0.26(12) 0.05(7) -0.08(6) -0.02(4) C71' 0.30(12) 0.29(12) 0.10(5) 0.12(6) -0.13(7) -0.23(11) C72' 0.10(4) 0.16(6) 0.07(4) 0.02(4) -0.02(3) 0.04(4) _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 Ag1 P2 2.401(5) . ? Ag1 Br2 2.638(7) . ? Ag1 Br4 2.724(7) . ? Ag1 Br3 2.931(8) . ? Ag2 P1 2.400(5) . ? Ag2 Br2 2.704(7) . ? Ag2 Br1 2.726(8) . ? Ag2 Br3 2.773(7) . ? Ag3 P4 2.398(6) . ? Ag3 Br3 2.595(8) . ? Ag3 Br1 2.795(7) . ? Ag3 Br4 2.824(8) . ? Ag4 P3 2.392(5) . ? Ag4 Br1 2.599(7) . ? Ag4 Br4 2.807(7) . ? Ag4 Br2 2.868(8) . ? P1 C13 1.814(12) . ? P1 C7 1.822(11) . ? P1 C1 1.825(10) . ? P2 C31 1.806(13) . ? P2 C19 1.816(11) . ? P2 C25 1.820(13) . ? P3 C49 1.805(10) . ? P3 C43 1.823(11) . ? P3 C37 1.843(12) . ? P4 C55 1.801(15) . ? P4 C61 1.822(14) . ? P4 C67 1.841(14) . ? P4 C67' 1.984(17) . ? C1 C6 1.384(15) . ? C1 C2 1.401(15) . ? C2 C3 1.354(16) . ? C2 H2A 0.9300 . ? C3 C4 1.347(19) . ? C3 H3A 0.9300 . ? C4 C5 1.37(2) . ? C4 H4A 0.9300 . ? C5 C6 1.368(15) . ? C5 H5A 0.9300 . ? C6 H6A 0.9300 . ? C7 C12 1.395(14) . ? C7 C8 1.397(14) . ? C8 C9 1.378(15) . ? C8 H8A 0.9300 . ? C9 C10 1.428(19) . ? C9 H9A 0.9300 . ? C10 C11 1.329(18) . ? C10 H10A 0.9300 . ? C11 C12 1.422(16) . ? C11 H11A 0.9300 . ? C12 H12A 0.9300 . ? C13 C14 1.345(16) . ? C13 C18 1.403(15) . ? C14 C15 1.377(19) . ? C14 H14A 0.9300 . ? C15 C16 1.33(2) . ? C15 H15A 0.9300 . ? C16 C17 1.359(18) . ? C16 H16A 0.9300 . ? C17 C18 1.409(17) . ? C17 H17A 0.9300 . ? C18 H18A 0.9300 . ? C19 C24 1.354(16) . ? C19 C20 1.359(15) . ? C20 C21 1.391(16) . ? C20 H20A 0.9300 . ? C21 C22 1.356(16) . ? C21 H21A 0.9300 . ? C22 C23 1.344(18) . ? C22 H22A 0.9300 . ? C23 C24 1.45(2) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 H24A 0.9300 . ? C25 C26 1.309(18) . ? C25 C30 1.376(16) . ? C26 C27 1.41(2) . ? C26 H26A 0.9300 . ? C27 C28 1.27(2) . ? C27 H27A 0.9300 . ? C28 C29 1.42(2) . ? C28 H28A 0.9300 . ? C29 C30 1.431(19) . ? C29 H29A 0.9300 . ? C30 H30A 0.9300 . ? C31 C32 1.360(18) . ? C31 C36 1.383(19) . ? C32 C33 1.39(2) . ? C32 H32A 0.9300 . ? C33 C34 1.34(2) . ? C33 H33A 0.9300 . ? C34 C35 1.37(3) . ? C34 H34A 0.9300 . ? C35 C36 1.44(3) . ? C35 H35A 0.9300 . ? C36 H36A 0.9300 . ? C37 C42 1.360(15) . ? C37 C38 1.382(16) . ? C38 C39 1.385(18) . ? C38 H38A 0.9300 . ? C39 C40 1.377(19) . ? C39 H39A 0.9300 . ? C40 C41 1.352(18) . ? C40 H40A 0.9300 . ? C41 C42 1.381(16) . ? C41 H41A 0.9300 . ? C42 H42A 0.9300 . ? C43 C44 1.340(14) . ? C43 C48 1.414(16) . ? C44 C45 1.378(18) . ? C44 H44A 0.9300 . ? C45 C46 1.316(19) . ? C45 H45A 0.9300 . ? C46 C47 1.374(19) . ? C46 H46A 0.9300 . ? C47 C48 1.398(17) . ? C47 H47A 0.9300 . ? C48 H48A 0.9300 . ? C49 C54 1.325(16) . ? C49 C50 1.417(14) . ? C50 C51 1.366(17) . ? C50 H50A 0.9300 . ? C51 C52 1.401(18) . ? C51 H51A 0.9300 . ? C52 C53 1.297(19) . ? C52 H52A 0.9300 . ? C53 C54 1.426(17) . ? C53 H53A 0.9300 . ? C54 H54A 0.9300 . ? C55 C56 1.37(2) . ? C55 C60 1.426(19) . ? C56 C57 1.47(2) . ? C56 H56A 0.9700 . ? C56 H56B 0.9700 . ? C57 C58 1.33(3) . ? C57 H57A 0.9300 . ? C58 C59 1.36(3) . ? C58 H58A 0.9300 . ? C59 C60 1.37(3) . ? C59 H59A 0.9300 . ? C60 H60A 0.9700 . ? C60 H60B 0.9700 . ? C61 C66 1.345(18) . ? C61 C62 1.365(18) . ? C62 C63 1.393(19) . ? C62 H62A 0.9300 . ? C63 C64 1.33(2) . ? C63 H63A 0.9300 . ? C64 C65 1.34(3) . ? C64 H64A 0.9300 . ? C65 C66 1.40(2) . ? C65 H65A 0.9300 . ? C66 H66A 0.9300 . ? C67 C68 1.324(9) . ? C67 C72 1.324(9) . ? C68 C69 1.324(10) . ? C68 H68A 0.9300 . ? C69 C70 1.324(9) . ? C69 H69A 0.9300 . ? C70 C71 1.324(9) . ? C70 H70A 0.9300 . ? C71 C72 1.324(10) . ? C71 H71A 0.9300 . ? C72 H72A 0.9300 . ? C67' C72' 1.224(9) . ? C67' C68' 1.225(9) . ? C68' C69' 1.225(9) . ? C68' H68B 0.9300 . ? C69' C70' 1.224(9) . ? C69' H69B 0.9300 . ? C70' C71' 1.224(9) . ? C70' H70B 0.9300 . ? C71' C72' 1.224(9) . ? C71' H71B 0.9300 . ? C72' H72B 0.9300 . ? 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 P2 Ag1 Br2 130.00(11) . . ? P2 Ag1 Br4 111.2(2) . . ? Br2 Ag1 Br4 107.29(16) . . ? P2 Ag1 Br3 114.79(14) . . ? Br2 Ag1 Br3 90.87(5) . . ? Br4 Ag1 Br3 96.21(5) . . ? P1 Ag2 Br2 119.89(13) . . ? P1 Ag2 Br1 130.76(9) . . ? Br2 Ag2 Br1 91.83(6) . . ? P1 Ag2 Br3 120.54(17) . . ? Br2 Ag2 Br3 93.00(5) . . ? Br1 Ag2 Br3 91.29(17) . . ? P4 Ag3 Br3 135.99(12) . . ? P4 Ag3 Br1 117.6(2) . . ? Br3 Ag3 Br1 93.59(18) . . ? P4 Ag3 Br4 106.91(14) . . ? Br3 Ag3 Br4 101.92(5) . . ? Br1 Ag3 Br4 91.88(6) . . ? P3 Ag4 Br1 140.84(14) . . ? P3 Ag4 Br4 111.75(11) . . ? Br1 Ag4 Br4 96.56(5) . . ? P3 Ag4 Br2 109.79(14) . . ? Br1 Ag4 Br2 90.88(5) . . ? Br4 Ag4 Br2 99.08(17) . . ? Ag4 Br1 Ag2 91.06(5) . . ? Ag4 Br1 Ag3 87.30(5) . . ? Ag2 Br1 Ag3 86.03(18) . . ? Ag1 Br2 Ag2 90.77(5) . . ? Ag1 Br2 Ag4 76.95(15) . . ? Ag2 Br2 Ag4 85.95(5) . . ? Ag3 Br3 Ag2 89.05(17) . . ? Ag3 Br3 Ag1 80.53(5) . . ? Ag2 Br3 Ag1 83.60(5) . . ? Ag1 Br4 Ag4 76.66(17) . . ? Ag1 Br4 Ag3 80.38(5) . . ? Ag4 Br4 Ag3 82.84(5) . . ? C13 P1 C7 103.2(5) . . ? C13 P1 C1 106.1(5) . . ? C7 P1 C1 101.0(5) . . ? C13 P1 Ag2 113.9(4) . . ? C7 P1 Ag2 114.0(4) . . ? C1 P1 Ag2 116.9(4) . . ? C31 P2 C19 103.8(5) . . ? C31 P2 C25 104.2(6) . . ? C19 P2 C25 105.7(5) . . ? C31 P2 Ag1 116.5(4) . . ? C19 P2 Ag1 114.2(4) . . ? C25 P2 Ag1 111.3(4) . . ? C49 P3 C43 106.2(5) . . ? C49 P3 C37 106.4(5) . . ? C43 P3 C37 102.0(5) . . ? C49 P3 Ag4 110.7(4) . . ? C43 P3 Ag4 115.3(4) . . ? C37 P3 Ag4 115.3(3) . . ? C55 P4 C61 104.5(6) . . ? C55 P4 C67 99.4(8) . . ? C61 P4 C67 110.9(8) . . ? C55 P4 C67' 112.8(8) . . ? C61 P4 C67' 93.8(7) . . ? C55 P4 Ag3 116.2(4) . . ? C61 P4 Ag3 115.7(5) . . ? C67 P4 Ag3 108.9(5) . . ? C67' P4 Ag3 111.6(5) . . ? C6 C1 C2 119.4(10) . . ? C6 C1 P1 122.6(8) . . ? C2 C1 P1 117.9(8) . . ? C3 C2 C1 118.4(12) . . ? C3 C2 H2A 120.8 . . ? C1 C2 H2A 120.8 . . ? C4 C3 C2 121.7(12) . . ? C4 C3 H3A 119.2 . . ? C2 C3 H3A 119.2 . . ? C3 C4 C5 121.2(12) . . ? C3 C4 H4A 119.4 . . ? C5 C4 H4A 119.4 . . ? C6 C5 C4 118.8(13) . . ? C6 C5 H5A 120.6 . . ? C4 C5 H5A 120.6 . . ? C5 C6 C1 120.4(11) . . ? C5 C6 H6A 119.8 . . ? C1 C6 H6A 119.8 . . ? C12 C7 C8 117.9(10) . . ? C12 C7 P1 124.0(8) . . ? C8 C7 P1 118.1(7) . . ? C9 C8 C7 121.2(10) . . ? C9 C8 H8A 119.4 . . ? C7 C8 H8A 119.4 . . ? C8 C9 C10 120.6(11) . . ? C8 C9 H9A 119.7 . . ? C10 C9 H9A 119.7 . . ? C11 C10 C9 117.9(11) . . ? C11 C10 H10A 121.0 . . ? C9 C10 H10A 121.0 . . ? C10 C11 C12 122.6(11) . . ? C10 C11 H11A 118.7 . . ? C12 C11 H11A 118.7 . . ? C7 C12 C11 119.6(11) . . ? C7 C12 H12A 120.2 . . ? C11 C12 H12A 120.2 . . ? C14 C13 C18 119.1(11) . . ? C14 C13 P1 125.1(9) . . ? C18 C13 P1 115.7(8) . . ? C13 C14 C15 120.2(13) . . ? C13 C14 H14A 119.9 . . ? C15 C14 H14A 119.9 . . ? C16 C15 C14 122.2(13) . . ? C16 C15 H15A 118.9 . . ? C14 C15 H15A 118.9 . . ? C15 C16 C17 119.6(12) . . ? C15 C16 H16A 120.2 . . ? C17 C16 H16A 120.2 . . ? C16 C17 C18 120.1(12) . . ? C16 C17 H17A 120.0 . . ? C18 C17 H17A 120.0 . . ? C13 C18 C17 118.4(11) . . ? C13 C18 H18A 120.8 . . ? C17 C18 H18A 120.8 . . ? C24 C19 C20 119.5(11) . . ? C24 C19 P2 121.7(9) . . ? C20 C19 P2 118.7(8) . . ? C19 C20 C21 120.9(11) . . ? C19 C20 H20A 119.6 . . ? C21 C20 H20A 119.6 . . ? C22 C21 C20 119.6(12) . . ? C22 C21 H21A 120.2 . . ? C20 C21 H21A 120.2 . . ? C23 C22 C21 121.7(12) . . ? C23 C22 H22A 119.1 . . ? C21 C22 H22A 119.1 . . ? C22 C23 C24 117.9(13) . . ? C22 C23 H23A 107.8 . . ? C24 C23 H23A 107.8 . . ? C22 C23 H23B 107.8 . . ? C24 C23 H23B 107.8 . . ? H23A C23 H23B 107.2 . . ? C19 C24 C23 120.0(13) . . ? C19 C24 H24A 120.0 . . ? C23 C24 H24A 120.0 . . ? C26 C25 C30 119.2(12) . . ? C26 C25 P2 118.1(10) . . ? C30 C25 P2 122.7(10) . . ? C25 C26 C27 123.5(14) . . ? C25 C26 H26A 118.3 . . ? C27 C26 H26A 118.3 . . ? C28 C27 C26 119.4(17) . . ? C28 C27 H27A 120.3 . . ? C26 C27 H27A 120.3 . . ? C27 C28 C29 121.2(17) . . ? C27 C28 H28A 119.4 . . ? C29 C28 H28A 119.4 . . ? C28 C29 C30 118.1(14) . . ? C28 C29 H29A 121.0 . . ? C30 C29 H29A 121.0 . . ? C25 C30 C29 118.6(14) . . ? C25 C30 H30A 120.7 . . ? C29 C30 H30A 120.7 . . ? C32 C31 C36 118.5(13) . . ? C32 C31 P2 124.4(11) . . ? C36 C31 P2 117.1(11) . . ? C31 C32 C33 120.8(15) . . ? C31 C32 H32A 119.6 . . ? C33 C32 H32A 119.6 . . ? C34 C33 C32 123.8(17) . . ? C34 C33 H33A 118.1 . . ? C32 C33 H33A 118.1 . . ? C33 C34 C35 115.9(19) . . ? C33 C34 H34A 122.1 . . ? C35 C34 H34A 122.1 . . ? C34 C35 C36 122.7(19) . . ? C34 C35 H35A 118.6 . . ? C36 C35 H35A 118.6 . . ? C31 C36 C35 118.1(16) . . ? C31 C36 H36A 121.0 . . ? C35 C36 H36A 121.0 . . ? C42 C37 C38 116.0(11) . . ? C42 C37 P3 127.1(9) . . ? C38 C37 P3 116.9(9) . . ? C37 C38 C39 122.6(13) . . ? C37 C38 H38A 118.7 . . ? C39 C38 H38A 118.7 . . ? C40 C39 C38 118.2(13) . . ? C40 C39 H39A 120.9 . . ? C38 C39 H39A 120.9 . . ? C41 C40 C39 120.9(12) . . ? C41 C40 H40A 119.5 . . ? C39 C40 H40A 119.5 . . ? C40 C41 C42 118.8(12) . . ? C40 C41 H41A 120.6 . . ? C42 C41 H41A 120.6 . . ? C37 C42 C41 123.4(11) . . ? C37 C42 H42A 118.3 . . ? C41 C42 H42A 118.3 . . ? C44 C43 C48 116.9(11) . . ? C44 C43 P3 124.9(9) . . ? C48 C43 P3 118.2(8) . . ? C43 C44 C45 122.2(13) . . ? C43 C44 H44A 118.9 . . ? C45 C44 H44A 118.9 . . ? C46 C45 C44 120.1(12) . . ? C46 C45 H45A 119.9 . . ? C44 C45 H45A 119.9 . . ? C45 C46 C47 122.7(13) . . ? C45 C46 H46A 118.7 . . ? C47 C46 H46A 118.7 . . ? C46 C47 C48 116.6(13) . . ? C46 C47 H47A 121.7 . . ? C48 C47 H47A 121.7 . . ? C47 C48 C43 121.5(12) . . ? C47 C48 H48A 119.3 . . ? C43 C48 H48A 119.3 . . ? C54 C49 C50 117.2(10) . . ? C54 C49 P3 119.0(8) . . ? C50 C49 P3 123.6(8) . . ? C51 C50 C49 120.8(12) . . ? C51 C50 H50A 119.6 . . ? C49 C50 H50A 119.6 . . ? C50 C51 C52 119.3(11) . . ? C50 C51 H51A 120.4 . . ? C52 C51 H51A 120.4 . . ? C53 C52 C51 120.5(12) . . ? C53 C52 H52A 119.7 . . ? C51 C52 H52A 119.7 . . ? C52 C53 C54 120.0(13) . . ? C52 C53 H53A 120.0 . . ? C54 C53 H53A 120.0 . . ? C49 C54 C53 122.1(12) . . ? C49 C54 H54A 119.0 . . ? C53 C54 H54A 119.0 . . ? C56 C55 C60 122.2(16) . . ? C56 C55 P4 115.4(12) . . ? C60 C55 P4 122.3(13) . . ? C55 C56 C57 116.4(17) . . ? C55 C56 H56A 108.2 . . ? C57 C56 H56A 108.2 . . ? C55 C56 H56B 108.2 . . ? C57 C56 H56B 108.2 . . ? H56A C56 H56B 107.3 . . ? C58 C57 C56 121(2) . . ? C58 C57 H57A 119.7 . . ? C56 C57 H57A 119.7 . . ? C57 C58 C59 120(3) . . ? C57 C58 H58A 119.8 . . ? C59 C58 H58A 119.8 . . ? C58 C59 C60 123(3) . . ? C58 C59 H59A 118.3 . . ? C60 C59 H59A 118.3 . . ? C59 C60 C55 116.8(19) . . ? C59 C60 H60A 108.1 . . ? C55 C60 H60A 108.1 . . ? C59 C60 H60B 108.1 . . ? C55 C60 H60B 108.1 . . ? H60A C60 H60B 107.3 . . ? C66 C61 C62 120.5(13) . . ? C66 C61 P4 117.3(11) . . ? C62 C61 P4 122.1(10) . . ? C61 C62 C63 120.7(15) . . ? C61 C62 H62A 119.7 . . ? C63 C62 H62A 119.7 . . ? C64 C63 C62 118.9(18) . . ? C64 C63 H63A 120.5 . . ? C62 C63 H63A 120.5 . . ? C63 C64 C65 119.4(18) . . ? C63 C64 H64A 120.3 . . ? C65 C64 H64A 120.3 . . ? C64 C65 C66 123.4(17) . . ? C64 C65 H65A 118.3 . . ? C66 C65 H65A 118.3 . . ? C61 C66 C65 116.6(15) . . ? C61 C66 H66A 121.7 . . ? C65 C66 H66A 121.7 . . ? C68 C67 C72 120.0 . . ? C68 C67 P4 119.2(10) . . ? C72 C67 P4 120.8(10) . . ? C67 C68 C69 120.0 . . ? C67 C68 H68A 120.0 . . ? C69 C68 H68A 120.0 . . ? C68 C69 C70 120.0 . . ? C68 C69 H69A 120.0 . . ? C70 C69 H69A 120.0 . . ? C71 C70 C69 120.0 . . ? C71 C70 H70A 120.0 . . ? C69 C70 H70A 120.0 . . ? C70 C71 C72 120.0 . . ? C70 C71 H71A 120.0 . . ? C72 C71 H71A 120.0 . . ? C71 C72 C67 120.0 . . ? C71 C72 H72A 120.0 . . ? C67 C72 H72A 120.0 . . ? C72' C67' C68' 120.0 . . ? C72' C67' P4 127.3(10) . . ? C68' C67' P4 112.3(10) . . ? C69' C68' C67' 120.0 . . ? C69' C68' H68B 120.0 . . ? C67' C68' H68B 120.0 . . ? C70' C69' C68' 120.0 . . ? C70' C69' H69B 120.0 . . ? C68' C69' H69B 120.0 . . ? C69' C70' C71' 120.0 . . ? C69' C70' H70B 120.0 . . ? C71' C70' H70B 120.0 . . ? C70' C71' C72' 120.0 . . ? C70' C71' H71B 120.0 . . ? C72' C71' H71B 120.0 . . ? C67' C72' C71' 120.0 . . ? C67' C72' H72B 120.0 . . ? C71' C72' H72B 120.0 . . ? _refine_diff_density_max 0.960 _refine_diff_density_min -2.406 _refine_diff_density_rms 0.174 _shelxl_version_number 2013-2 _shelx_res_file ; TITL a01003a in C2/c CELL 0.71073 24.3939 12.0814 48.2387 90.000 100.896 90.000 ZERR 8.00 0.0782 0.0323 0.1317 0.000 0.072 0.000 LATT 7 SYMM -X, Y, 0.5-Z SFAC C H Ag P Br UNIT 576 504 32 32 32 OMIT -3.00 50.02 L.S. 8 ACTA BOND $H FMAP 2 PLAN 4 size 0.20 0.18 0.12 delu c71 c72 delu c64 c65 isor 0.002 c68' BIND Ag1 Br3 TEMP 20 WGHT 0.145300 FVAR 0.47649 0.64507 AG1 3 0.145319 0.901309 0.124777 11.00000 0.06138 0.08930 = 0.07218 0.00370 0.02642 -0.01736 AG2 3 0.164607 1.132348 0.073938 11.00000 0.05723 0.05219 = 0.05265 0.01384 0.00071 0.00871 AG3 3 0.238582 1.123749 0.149866 11.00000 0.06653 0.08652 = 0.05711 -0.01617 -0.00112 -0.00651 AG4 3 0.268784 0.904589 0.100536 11.00000 0.05426 0.04031 = 0.07602 -0.00474 0.01758 0.00822 BR1 5 0.274747 1.119053 0.098253 11.00000 0.06874 0.05973 = 0.08094 0.00430 0.01182 -0.00445 BR2 5 0.154941 0.909472 0.071249 11.00000 0.06959 0.06577 = 0.07103 -0.00087 0.00488 -0.00212 BR3 5 0.134120 1.142622 0.126411 11.00000 0.06630 0.08188 = 0.07870 0.00413 0.01944 0.00342 BR4 5 0.250479 0.892157 0.156186 11.00000 0.07153 0.08415 = 0.06604 0.00984 0.01264 -0.00211 P1 4 0.117666 1.244043 0.035541 11.00000 0.03926 0.04176 = 0.04169 0.00841 0.00251 -0.00178 P2 4 0.080469 0.800656 0.146942 11.00000 0.04574 0.07088 = 0.04680 -0.00168 0.01768 -0.00976 P3 4 0.313913 0.741987 0.087556 11.00000 0.04446 0.03162 = 0.05340 0.00160 0.01234 0.00363 P4 4 0.299469 1.206293 0.189293 11.00000 0.06044 0.07090 = 0.06013 -0.01484 -0.00192 -0.00234 C1 1 0.161378 1.316399 0.014600 11.00000 0.05010 0.03602 = 0.04401 -0.00266 0.01044 -0.01194 C2 1 0.216942 1.337980 0.027187 11.00000 0.04905 0.05351 = 0.06921 -0.00936 0.01013 0.00422 AFIX 43 H2A 2 0.230780 1.317014 0.045740 11.00000 -1.20000 AFIX 0 C3 1 0.250014 1.390076 0.011703 11.00000 0.05160 0.07234 = 0.07610 -0.00484 0.02007 -0.02553 AFIX 43 H3A 2 0.286575 1.407238 0.020054 11.00000 -1.20000 AFIX 0 C4 1 0.231308 1.417675 -0.015487 11.00000 0.09290 0.05988 = 0.11935 -0.00970 0.07208 -0.01700 AFIX 43 H4A 2 0.255424 1.451779 -0.025644 11.00000 -1.20000 AFIX 0 C5 1 0.177452 1.396427 -0.028431 11.00000 0.08086 0.04748 = 0.08261 0.00671 0.02371 -0.01395 AFIX 43 H5A 2 0.164965 1.415298 -0.047257 11.00000 -1.20000 AFIX 0 C6 1 0.142288 1.346943 -0.013201 11.00000 0.05260 0.07063 = 0.05774 0.02071 0.00755 -0.00662 AFIX 43 H6A 2 0.105307 1.333737 -0.021585 11.00000 -1.20000 AFIX 0 C7 1 0.071724 1.166315 0.008203 11.00000 0.03955 0.03766 = 0.05184 0.00890 0.01260 -0.00571 C8 1 0.092801 1.070807 -0.002317 11.00000 0.03868 0.04317 = 0.05609 0.01568 0.00273 -0.00073 AFIX 43 H8A 2 0.128964 1.047966 0.005199 11.00000 -1.20000 AFIX 0 C9 1 0.061024 1.009815 -0.023618 11.00000 0.09441 0.05284 = 0.04302 -0.00882 0.01688 -0.00827 AFIX 43 H9A 2 0.076097 0.946973 -0.030421 11.00000 -1.20000 AFIX 0 C10 1 0.005158 1.042227 -0.035342 11.00000 0.09423 0.08245 = 0.03900 -0.00725 0.00704 -0.04780 AFIX 43 H10A 2 -0.016301 1.002130 -0.049935 11.00000 -1.20000 AFIX 0 C11 1 -0.015232 1.131489 -0.024753 11.00000 0.03866 0.07655 = 0.06068 0.01614 -0.00201 -0.01305 AFIX 43 H11A 2 -0.052210 1.151098 -0.031511 11.00000 -1.20000 AFIX 0 C12 1 0.017305 1.198174 -0.003490 11.00000 0.03956 0.05551 = 0.05873 0.01887 -0.00121 -0.00311 AFIX 43 H12A 2 0.002383 1.262629 0.002579 11.00000 -1.20000 AFIX 0 C13 1 0.071690 1.347855 0.045893 11.00000 0.04981 0.05221 = 0.04431 0.00608 -0.00190 0.00300 C14 1 0.066017 1.451984 0.035876 11.00000 0.10851 0.04615 = 0.08910 0.02641 0.03438 0.02711 AFIX 43 H14A 2 0.085809 1.474640 0.022183 11.00000 -1.20000 AFIX 0 C15 1 0.031004 1.525127 0.045831 11.00000 0.11603 0.05547 = 0.10666 0.02916 0.02402 0.02687 AFIX 43 H15A 2 0.028266 1.597188 0.038927 11.00000 -1.20000 AFIX 0 C16 1 0.001060 1.496276 0.064930 11.00000 0.08899 0.06383 = 0.06953 0.00203 0.01324 0.03436 AFIX 43 H16A 2 -0.023053 1.546955 0.070824 11.00000 -1.20000 AFIX 0 C17 1 0.005793 1.392262 0.075846 11.00000 0.07401 0.10433 = 0.06301 0.00629 0.03446 0.01392 AFIX 43 H17A 2 -0.015860 1.371018 0.088868 11.00000 -1.20000 AFIX 0 C18 1 0.043481 1.316542 0.067456 11.00000 0.06668 0.05399 = 0.05871 0.01784 0.02855 0.00595 AFIX 43 H18A 2 0.049508 1.247481 0.076005 11.00000 -1.20000 AFIX 0 C19 1 0.009802 0.796807 0.126564 11.00000 0.03624 0.05285 = 0.05020 -0.00234 0.01253 -0.00884 C20 1 0.002398 0.793929 0.097943 11.00000 0.04878 0.07664 = 0.05949 0.00911 0.01207 -0.01709 AFIX 43 H20A 2 0.033362 0.794832 0.089275 11.00000 -1.20000 AFIX 0 C21 1 -0.050884 0.789648 0.081431 11.00000 0.06839 0.08818 = 0.06173 0.00160 0.00157 -0.02114 AFIX 43 H21A 2 -0.055517 0.789154 0.061847 11.00000 -1.20000 AFIX 0 C22 1 -0.096022 0.786200 0.094052 11.00000 0.04637 0.10214 = 0.05721 0.00402 -0.00373 -0.00381 AFIX 43 H22A 2 -0.131297 0.777103 0.082956 11.00000 -1.20000 AFIX 0 C23 1 -0.091136 0.795578 0.122171 11.00000 0.06732 0.15386 = 0.08403 0.01008 0.01509 0.01041 AFIX 23 H23A 2 -0.110030 0.732902 0.128726 11.00000 -1.20000 H23B 2 -0.111109 0.861651 0.125931 11.00000 -1.20000 AFIX 0 C24 1 -0.035284 0.801295 0.139139 11.00000 0.07675 0.19087 = 0.04591 0.01792 0.01235 -0.00166 AFIX 43 H24A 2 -0.030491 0.808043 0.158654 11.00000 -1.20000 AFIX 0 C25 1 0.074817 0.861507 0.180797 11.00000 0.04556 0.07235 = 0.05154 0.00116 0.01348 -0.00253 C26 1 0.085006 0.967420 0.184455 11.00000 0.09013 0.08998 = 0.05482 0.00644 0.01224 -0.01683 AFIX 43 H26A 2 0.096636 1.006587 0.170007 11.00000 -1.20000 AFIX 0 C27 1 0.079282 1.025318 0.209149 11.00000 0.17642 0.07950 = 0.07499 -0.00294 0.04820 -0.01290 AFIX 43 H27A 2 0.085307 1.101315 0.210408 11.00000 -1.20000 AFIX 0 C28 1 0.065775 0.972458 0.229712 11.00000 0.12279 0.11897 = 0.08124 -0.02076 -0.00923 0.03381 AFIX 43 H28A 2 0.064407 1.009597 0.246454 11.00000 -1.20000 AFIX 0 C29 1 0.052779 0.857873 0.227512 11.00000 0.07634 0.17398 = 0.05318 0.01849 0.03481 0.01424 AFIX 43 H29A 2 0.041295 0.820267 0.242241 11.00000 -1.20000 AFIX 0 C30 1 0.057862 0.801937 0.201982 11.00000 0.08666 0.07593 = 0.04534 -0.00260 0.02125 0.00437 AFIX 43 H30A 2 0.049868 0.726837 0.199749 11.00000 -1.20000 AFIX 0 C31 1 0.096650 0.657014 0.154991 11.00000 0.06007 0.06253 = 0.05935 -0.00418 0.02551 -0.00020 C32 1 0.067549 0.570276 0.141523 11.00000 0.09663 0.07913 = 0.06874 0.00873 0.01169 -0.01382 AFIX 43 H32A 2 0.037085 0.583675 0.127140 11.00000 -1.20000 AFIX 0 C33 1 0.082721 0.462095 0.148963 11.00000 0.11547 0.06821 = 0.13582 -0.01560 0.02217 -0.01925 AFIX 43 H33A 2 0.062615 0.405221 0.138728 11.00000 -1.20000 AFIX 0 C34 1 0.124546 0.434790 0.169980 11.00000 0.13666 0.10420 = 0.10416 0.00978 0.03059 0.02820 AFIX 43 H34A 2 0.132877 0.361537 0.175018 11.00000 -1.20000 AFIX 0 C35 1 0.154424 0.521482 0.183662 11.00000 0.11521 0.14309 = 0.14113 -0.02356 -0.01814 0.04862 AFIX 43 H35A 2 0.183793 0.506106 0.198476 11.00000 -1.20000 AFIX 0 C36 1 0.142235 0.634988 0.176058 11.00000 0.07721 0.07911 = 0.14514 -0.01378 -0.01933 0.02939 AFIX 43 H36A 2 0.164346 0.692016 0.185037 11.00000 -1.20000 AFIX 0 C37 1 0.326057 0.739875 0.050994 11.00000 0.05277 0.03372 = 0.06241 0.01016 0.02122 0.01536 C38 1 0.362708 0.817683 0.044008 11.00000 0.08827 0.06380 = 0.06335 -0.00370 0.01615 -0.01161 AFIX 43 H38A 2 0.380551 0.865379 0.057981 11.00000 -1.20000 AFIX 0 C39 1 0.373907 0.827412 0.017008 11.00000 0.11314 0.05937 = 0.07855 0.01002 0.04792 -0.00265 AFIX 43 H39A 2 0.399037 0.880015 0.012899 11.00000 -1.20000 AFIX 0 C40 1 0.346833 0.757110 -0.003579 11.00000 0.09308 0.07994 = 0.05385 0.02229 0.02755 0.03457 AFIX 43 H40A 2 0.352607 0.764324 -0.022006 11.00000 -1.20000 AFIX 0 C41 1 0.311979 0.677750 0.002615 11.00000 0.07920 0.06833 = 0.03966 -0.01015 -0.00069 0.00331 AFIX 43 H41A 2 0.295101 0.628319 -0.011171 11.00000 -1.20000 AFIX 0 C42 1 0.301902 0.671446 0.029794 11.00000 0.05071 0.05416 = 0.06354 -0.00949 0.00221 0.00050 AFIX 43 H42A 2 0.277308 0.617577 0.033807 11.00000 -1.20000 AFIX 0 C43 1 0.383730 0.716534 0.107840 11.00000 0.04015 0.03486 = 0.06144 0.01171 0.01566 -0.00213 C44 1 0.420267 0.644148 0.100686 11.00000 0.05990 0.05652 = 0.07514 0.00037 0.01272 0.01489 AFIX 43 H44A 2 0.409751 0.602078 0.084403 11.00000 -1.20000 AFIX 0 C45 1 0.472909 0.629988 0.116658 11.00000 0.05347 0.05080 = 0.12780 0.01004 0.02287 0.01753 AFIX 43 H45A 2 0.497700 0.580846 0.110742 11.00000 -1.20000 AFIX 0 C46 1 0.488179 0.685894 0.140279 11.00000 0.05026 0.07817 = 0.09162 0.02371 -0.00242 -0.00370 AFIX 43 H46A 2 0.524135 0.676017 0.150555 11.00000 -1.20000 AFIX 0 C47 1 0.453157 0.758262 0.150375 11.00000 0.05870 0.10216 = 0.07054 -0.01309 -0.00059 -0.00447 AFIX 43 H47A 2 0.463927 0.794576 0.167541 11.00000 -1.20000 AFIX 0 C48 1 0.400500 0.774484 0.133512 11.00000 0.05439 0.06102 = 0.07650 -0.00159 0.01530 -0.00695 AFIX 43 H48A 2 0.375960 0.824498 0.139308 11.00000 -1.20000 AFIX 0 C49 1 0.273412 0.620062 0.091605 11.00000 0.04646 0.04038 = 0.05637 0.01058 0.02148 0.00109 C50 1 0.296471 0.512360 0.095725 11.00000 0.06670 0.03292 = 0.08809 -0.00361 0.01076 0.00895 AFIX 43 H50A 2 0.334048 0.501430 0.095318 11.00000 -1.20000 AFIX 0 C51 1 0.264129 0.424345 0.100291 11.00000 0.09835 0.02715 = 0.08011 0.00047 -0.00413 -0.00504 AFIX 43 H51A 2 0.279981 0.354706 0.104157 11.00000 -1.20000 AFIX 0 C52 1 0.206820 0.440163 0.099084 11.00000 0.08806 0.06049 = 0.07243 -0.00115 0.02484 -0.01500 AFIX 43 H52A 2 0.184077 0.379694 0.100754 11.00000 -1.20000 AFIX 0 C53 1 0.185247 0.538468 0.095656 11.00000 0.07407 0.06215 = 0.13558 0.01218 0.03978 -0.00641 AFIX 43 H53A 2 0.147325 0.548534 0.095305 11.00000 -1.20000 AFIX 0 C54 1 0.219715 0.631123 0.092424 11.00000 0.07153 0.03533 = 0.13612 -0.00200 0.03063 -0.00734 AFIX 43 H54A 2 0.204002 0.701514 0.090842 11.00000 -1.20000 AFIX 0 C55 1 0.323783 1.343986 0.183915 11.00000 0.08919 0.09157 = 0.03107 -0.01835 0.02175 -0.01071 C56 1 0.283242 1.418072 0.172336 11.00000 0.11945 0.13125 = 0.04409 -0.00055 0.02837 0.02114 AFIX 23 H56A 2 0.255185 1.420147 0.184144 11.00000 -1.20000 H56B 2 0.265303 1.390315 0.153988 11.00000 -1.20000 AFIX 0 C57 1 0.301833 1.532331 0.168733 11.00000 0.18620 0.08113 = 0.09027 0.01338 0.03020 0.00479 AFIX 43 H57A 2 0.276056 1.585252 0.160597 11.00000 -1.20000 AFIX 0 C58 1 0.355180 1.560536 0.177014 11.00000 0.22163 0.14754 = 0.11128 0.00612 0.06702 -0.05925 AFIX 43 H58A 2 0.365946 1.633972 0.175845 11.00000 -1.20000 AFIX 0 C59 1 0.394045 1.482503 0.187182 11.00000 0.15824 0.17993 = 0.10483 -0.04993 0.07050 -0.10445 AFIX 43 H59A 2 0.431414 1.503348 0.191036 11.00000 -1.20000 AFIX 0 C60 1 0.380982 1.375007 0.192023 11.00000 0.06776 0.14308 = 0.07570 -0.03956 0.03198 -0.03380 AFIX 23 H60A 2 0.392575 1.360268 0.212041 11.00000 -1.20000 H60B 2 0.402892 1.327423 0.182119 11.00000 -1.20000 AFIX 0 C61 1 0.271815 1.215808 0.221760 11.00000 0.10916 0.06181 = 0.04331 0.00211 0.00740 -0.02232 C62 1 0.288566 1.296188 0.241427 11.00000 0.10768 0.09812 = 0.06289 -0.01063 0.02379 -0.03426 AFIX 43 H62A 2 0.315252 1.347595 0.238472 11.00000 -1.20000 AFIX 0 C63 1 0.266100 1.302016 0.265884 11.00000 0.17206 0.13225 = 0.04190 -0.00015 0.02902 -0.02470 AFIX 43 H63A 2 0.274572 1.361200 0.278281 11.00000 -1.20000 AFIX 0 C64 1 0.232255 1.221354 0.271222 11.00000 0.13131 0.20580 = 0.09737 -0.01131 0.04755 -0.06407 AFIX 43 H64A 2 0.217742 1.222432 0.287714 11.00000 -1.20000 AFIX 0 C65 1 0.219392 1.138998 0.252663 11.00000 0.24609 0.21955 = 0.08670 -0.00814 0.04315 -0.16934 AFIX 43 H65A 2 0.197825 1.080833 0.257292 11.00000 -1.20000 AFIX 0 C66 1 0.236625 1.135656 0.226680 11.00000 0.14706 0.15690 = 0.06861 -0.02657 0.01121 -0.10312 AFIX 43 H66A 2 0.224384 1.080758 0.213439 11.00000 -1.20000 PART 1 AFIX 9 C67 1 0.366667 1.132355 0.195375 21.00000 0.07387 0.07400 = 0.08182 0.02207 -0.01437 0.01280 C68 1 0.384949 1.089300 0.173576 21.00000 0.09828 0.08302 = 0.06329 -0.01357 0.02527 0.02498 AFIX 43 H68A 2 0.363138 1.093680 0.155579 21.00000 -1.20000 AFIX 5 C69 1 0.434291 1.039994 0.177393 21.00000 0.09406 0.05887 = 0.14794 -0.01274 0.01300 0.01650 AFIX 43 H69A 2 0.447131 1.009748 0.162078 21.00000 -1.20000 AFIX 5 C70 1 0.465352 1.033757 0.203021 21.00000 0.07255 0.09196 = 0.23525 0.01618 0.03392 0.02707 AFIX 43 H70A 2 0.500006 0.999140 0.205705 21.00000 -1.20000 AFIX 5 C71 1 0.447057 1.076820 0.224820 21.00000 0.20465 0.13523 = 0.15039 -0.01363 -0.05436 0.05459 AFIX 43 H71A 2 0.468864 1.072440 0.242818 21.00000 -1.20000 AFIX 5 C72 1 0.397723 1.126116 0.221004 21.00000 0.14709 0.11441 = 0.11117 -0.01819 -0.05357 -0.00140 AFIX 43 H72A 2 0.384881 1.156356 0.236319 21.00000 -1.20000 PART 2 AFIX 5 C67' 1 0.360758 1.104452 0.205825 -21.00000 0.09744 0.08353 = 0.05965 -0.00990 -0.02280 -0.01388 C68' 1 0.392278 1.084692 0.189475 -21.00000 0.10485 0.10482 = 0.10502 -0.00011 0.01978 0.00029 AFIX 43 H68B 2 0.388318 1.122640 0.172438 -21.00000 -1.20000 AFIX 5 C69' 1 0.429012 1.014961 0.195560 -21.00000 0.09493 0.51956 = 0.19161 -0.24829 0.03438 -0.11368 AFIX 43 H69B 2 0.452960 0.999968 0.183147 -21.00000 -1.20000 AFIX 5 C70' 1 0.434218 0.964982 0.217982 -21.00000 0.07206 0.14511 = 0.26416 0.04527 -0.07588 -0.02326 AFIX 43 H70B 2 0.462111 0.912004 0.222598 -21.00000 -1.20000 AFIX 5 C71' 1 0.402706 0.984739 0.234331 -21.00000 0.30427 0.28656 = 0.09871 0.12341 -0.12738 -0.23365 AFIX 43 H71B 2 0.406670 0.946793 0.251368 -21.00000 -1.20000 AFIX 5 C72' 1 0.365971 1.054465 0.228247 -21.00000 0.10224 0.16428 = 0.07323 0.01681 -0.01920 0.03590 AFIX 43 H72B 2 0.342025 1.069453 0.240662 -21.00000 -1.20000 PART 0 AFIX 0 HKLF 4 REM a01003a in C2/c REM R1 = 0.0753 for 6816 Fo > 4sig(Fo) and 0.1182 for all 12185 data REM 783 parameters refined using 8 restraints END WGHT 0.1453 0.0000 REM Highest difference peak 0.960, deepest hole -2.406, 1-sigma level 0.174 Q1 1 0.1818 1.0874 0.0848 11.00000 0.05 0.96 Q2 1 0.1608 0.8372 0.1303 11.00000 0.05 0.86 Q3 1 0.2241 1.0838 0.1435 11.00000 0.05 0.85 Q4 1 0.2326 1.1786 0.1436 11.00000 0.05 0.85 ; _shelx_res_checksum 2392 _shelx_hkl_file ; 15 5 -56 302 578 280 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