# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email matilde.fondo@usc.es _publ_contact_author_name 'Matilde Fondo' loop_ _publ_author_name M.Fondo A.Garcia-Deibe N.Ocampo I.Garcia-Santos J.Sanmartin J.L.Perez-Lustres A.J.Mota data_H4L _database_code_depnum_ccdc_archive 'CCDC 825862' #TrackingRef '- cifs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H36 Br4 Cl4 N6 O4' _chemical_formula_sum 'C38 H36 Br4 Cl4 N6 O4' _chemical_formula_weight 1102.17 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' O O 0.0106 0.0060 '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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_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 26.362(7) _cell_length_b 12.458(3) _cell_length_c 26.554(6) _cell_angle_alpha 90.00 _cell_angle_beta 106.879(5) _cell_angle_gamma 90.00 _cell_volume 8345(4) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 301 _cell_measurement_theta_min 2.976 _cell_measurement_theta_max 12.6515 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.755 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4368 _exptl_absorpt_coefficient_mu 4.162 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6886 _exptl_absorpt_correction_T_max 0.9214 _exptl_absorpt_process_details 'SADABS (Bruker, 2009)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 KappaAPEXII' _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22552 _diffrn_reflns_av_R_equivalents 0.0856 _diffrn_reflns_av_sigmaI/netI 0.1661 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 18.84 _reflns_number_total 3289 _reflns_number_gt 1777 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER APEX2' _computing_cell_refinement 'BRUKER APEX2' _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0422P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3289 _refine_ls_number_parameters 267 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1462 _refine_ls_R_factor_gt 0.0596 _refine_ls_wR_factor_ref 0.1420 _refine_ls_wR_factor_gt 0.1076 _refine_ls_goodness_of_fit_ref 0.978 _refine_ls_restrained_S_all 0.978 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Br11 Br 0.52337(8) 0.22251(16) 0.56907(7) 0.0376(7) Uani 1 1 d . . . Br12 Br 0.96456(9) -0.42541(19) 1.17556(8) 0.0548(8) Uani 1 1 d . . . Br13 Br 0.69636(8) 0.33003(16) 0.89511(7) 0.0291(6) Uani 1 1 d . . . Br14 Br 0.87055(8) 0.09227(16) 0.72365(7) 0.0346(7) Uani 1 1 d . . . Cl11 Cl 0.7916(2) -0.5960(4) 1.02609(17) 0.0359(15) Uani 1 1 d . . . Cl12 Cl 0.57329(18) 0.1955(3) 0.78584(16) 0.0239(14) Uani 1 1 d . . . Cl13 Cl 1.05182(19) -0.0687(4) 0.86474(16) 0.0260(14) Uani 1 1 d . . . Cl14 Cl 0.72074(19) 0.7714(4) 0.89688(16) 0.0248(14) Uani 1 1 d . . . N101 N 0.8775(6) -0.1238(11) 1.0260(5) 0.021(4) Uiso 1 1 d . . . N102 N 0.7012(5) 0.4618(10) 0.6584(5) 0.018(4) Uiso 1 1 d . . . N103 N 0.8833(5) 0.1264(10) 0.9495(5) 0.017(4) Uiso 1 1 d . . . N104 N 0.8011(5) 0.4930(10) 0.7484(5) 0.016(4) Uiso 1 1 d . . . N105 N 0.8981(5) 0.2828(10) 0.9115(4) 0.016(4) Uiso 1 1 d . . . N106 N 0.8644(5) 0.4393(10) 0.8230(4) 0.015(4) Uiso 1 1 d . . . O101 O 0.9363(5) -0.2368(10) 1.1035(5) 0.042(4) Uiso 1 1 d . . . H1 H 0.9199 -0.1787 1.0947 0.062 Uiso 1 1 calc R . . O102 O 0.6256(4) 0.3483(9) 0.5998(4) 0.029(3) Uiso 1 1 d . . . H2 H 0.6536 0.3849 0.6083 0.043 Uiso 1 1 calc R . . O103 O 0.8554(4) 0.1832(8) 0.8225(4) 0.022(3) Uiso 1 1 d . . . H3 H 0.8516 0.2079 0.8506 0.033 Uiso 1 1 calc R . . O104 O 0.7744(4) 0.3461(8) 0.8334(4) 0.015(3) Uiso 1 1 d . . . H4 H 0.8010 0.3484 0.8221 0.022 Uiso 1 1 calc R . . C100 C 0.9048(8) -0.3188(15) 1.0816(7) 0.033(6) Uiso 1 1 d . . . C101 C 0.9096(7) -0.4195(15) 1.1103(6) 0.033(5) Uiso 1 1 d . . . C102 C 0.8769(7) -0.5033(15) 1.0925(7) 0.031(6) Uiso 1 1 d . . . H102 H 0.8815 -0.5691 1.1113 0.037 Uiso 1 1 calc R . . C103 C 0.8369(8) -0.4910(14) 1.0463(7) 0.033(6) Uiso 1 1 d . . . C104 C 0.8301(7) -0.3994(14) 1.0168(6) 0.028(5) Uiso 1 1 d . . . H104 H 0.8024 -0.3944 0.9847 0.034 Uiso 1 1 calc R . . C105 C 0.8648(7) -0.3128(13) 1.0346(6) 0.017(5) Uiso 1 1 d . . . C106 C 0.8545(7) -0.2088(14) 1.0076(6) 0.025(5) Uiso 1 1 d . . . H106 H 0.8289 -0.2061 0.9740 0.030 Uiso 1 1 calc R . . C107 C 0.8588(7) -0.0227(13) 0.9958(6) 0.021(5) Uiso 1 1 d . . . H10A H 0.8439 0.0262 1.0173 0.026 Uiso 1 1 calc R . . H10B H 0.8303 -0.0399 0.9632 0.026 Uiso 1 1 calc R . . C108 C 0.9042(7) 0.0331(13) 0.9815(6) 0.020(5) Uiso 1 1 d . . . H10C H 0.9317 0.0555 1.0139 0.024 Uiso 1 1 calc R . . H10D H 0.9206 -0.0167 0.9618 0.024 Uiso 1 1 calc R . . C109 C 0.8647(7) 0.2111(12) 0.9777(6) 0.024(5) Uiso 1 1 d . . . H10E H 0.8849 0.2102 1.0155 0.029 Uiso 1 1 calc R . . H10F H 0.8267 0.2013 0.9744 0.029 Uiso 1 1 calc R . . C110 C 0.8737(7) 0.3175(12) 0.9523(6) 0.016(5) Uiso 1 1 d . . . H11A H 0.8397 0.3553 0.9365 0.019 Uiso 1 1 calc R . . H11B H 0.8978 0.3653 0.9783 0.019 Uiso 1 1 calc R . . C111 C 0.9329(6) 0.3647(12) 0.8984(6) 0.014(5) Uiso 1 1 d . . . H11C H 0.9511 0.3327 0.8742 0.017 Uiso 1 1 calc R . . H11D H 0.9604 0.3859 0.9310 0.017 Uiso 1 1 calc R . . C112 C 0.9034(6) 0.4627(12) 0.8732(5) 0.018(5) Uiso 1 1 d . . . H11E H 0.8852 0.4948 0.8974 0.022 Uiso 1 1 calc R . . H11F H 0.9291 0.5161 0.8676 0.022 Uiso 1 1 calc R . . C113 C 0.8877(7) 0.4171(14) 0.7794(5) 0.024(5) Uiso 1 1 d . . . H11G H 0.8989 0.3412 0.7798 0.029 Uiso 1 1 calc R . . H11H H 0.9186 0.4641 0.7817 0.029 Uiso 1 1 calc R . . C114 C 0.8429(7) 0.4414(14) 0.7308(6) 0.026(5) Uiso 1 1 d . . . H11I H 0.8552 0.4899 0.7072 0.031 Uiso 1 1 calc R . . H11J H 0.8295 0.3743 0.7115 0.031 Uiso 1 1 calc R . . C115 C 0.7729(7) 0.5807(13) 0.7153(5) 0.020(5) Uiso 1 1 d . . . H11K H 0.7986 0.6365 0.7124 0.024 Uiso 1 1 calc R . . H11L H 0.7477 0.6136 0.7321 0.024 Uiso 1 1 calc R . . C116 C 0.7420(7) 0.5403(13) 0.6591(6) 0.025(5) Uiso 1 1 d . . . H11M H 0.7254 0.6027 0.6375 0.030 Uiso 1 1 calc R . . H11N H 0.7676 0.5083 0.6425 0.030 Uiso 1 1 calc R . . C117 C 0.6894(7) 0.4218(13) 0.6990(6) 0.024(5) Uiso 1 1 d . . . H117 H 0.7106 0.4408 0.7333 0.028 Uiso 1 1 calc R . . C118 C 0.6455(7) 0.3501(13) 0.6935(6) 0.017(5) Uiso 1 1 d . . . C119 C 0.6140(7) 0.3192(14) 0.6412(6) 0.026(5) Uiso 1 1 d . . . C120 C 0.5683(7) 0.2548(13) 0.6386(6) 0.017(5) Uiso 1 1 d . . . C121 C 0.5557(7) 0.2220(13) 0.6818(6) 0.023(5) Uiso 1 1 d . . . H121 H 0.5243 0.1816 0.6785 0.027 Uiso 1 1 calc R . . C122 C 0.5885(7) 0.2472(14) 0.7305(6) 0.023(5) Uiso 1 1 d . . . C123 C 0.6318(7) 0.3082(13) 0.7371(6) 0.018(5) Uiso 1 1 d . . . H123 H 0.6537 0.3234 0.7716 0.022 Uiso 1 1 calc R . . C124 C 0.9221(7) 0.1788(13) 0.9295(6) 0.022(5) Uiso 1 1 d . . . H124 H 0.9554 0.1898 0.9588 0.027 Uiso 1 1 calc R . . C125 C 0.9345(7) 0.1195(13) 0.8852(6) 0.015(5) Uiso 1 1 d . . . C126 C 0.9817(7) 0.0613(12) 0.8942(6) 0.016(5) Uiso 1 1 d . . . H126 H 1.0064 0.0598 0.9283 0.019 Uiso 1 1 calc R . . C127 C 0.9920(7) 0.0053(13) 0.8528(6) 0.017(5) Uiso 1 1 d . . . C128 C 0.9603(7) 0.0151(13) 0.8021(6) 0.022(5) Uiso 1 1 d . . . H128 H 0.9690 -0.0204 0.7741 0.026 Uiso 1 1 calc R . . C129 C 0.9164(7) 0.0762(13) 0.7929(6) 0.013(5) Uiso 1 1 d . . . C130 C 0.9015(7) 0.1252(13) 0.8333(6) 0.023(5) Uiso 1 1 d . . . C131 C 0.8272(7) 0.5274(13) 0.8031(5) 0.016(5) Uiso 1 1 d . . . H131 H 0.8467 0.5964 0.8036 0.019 Uiso 1 1 calc R . . C132 C 0.7884(6) 0.5374(13) 0.8345(5) 0.008(4) Uiso 1 1 d . . . C133 C 0.7647(6) 0.4431(13) 0.8486(5) 0.009(4) Uiso 1 1 d . . . C134 C 0.7282(7) 0.4549(14) 0.8764(6) 0.022(5) Uiso 1 1 d . . . C135 C 0.7146(6) 0.5563(13) 0.8914(5) 0.014(5) Uiso 1 1 d . . . H135 H 0.6891 0.5633 0.9101 0.017 Uiso 1 1 calc R . . C136 C 0.7389(7) 0.6454(13) 0.8785(6) 0.016(5) Uiso 1 1 d . . . C137 C 0.7743(7) 0.6358(13) 0.8498(6) 0.020(5) Uiso 1 1 d . . . H137 H 0.7894 0.6988 0.8401 0.024 Uiso 1 1 calc R . . 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 Br11 0.0348(17) 0.0367(16) 0.0330(13) -0.0019(11) -0.0031(11) -0.0015(13) Br12 0.0287(17) 0.076(2) 0.0540(15) 0.0337(13) 0.0028(12) -0.0099(15) Br13 0.0307(15) 0.0284(14) 0.0336(13) 0.0049(10) 0.0177(11) -0.0063(12) Br14 0.0401(17) 0.0360(16) 0.0271(12) -0.0042(10) 0.0087(11) -0.0017(13) Cl11 0.048(4) 0.022(4) 0.045(3) 0.001(3) 0.024(3) -0.005(3) Cl12 0.018(3) 0.028(4) 0.030(3) 0.007(2) 0.013(2) -0.005(3) Cl13 0.025(4) 0.021(3) 0.037(3) -0.003(2) 0.017(3) 0.007(3) Cl14 0.030(4) 0.018(3) 0.034(3) 0.000(2) 0.021(3) 0.005(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 Br11 C120 1.924(15) . ? Br12 C101 1.909(17) . ? Br13 C134 1.901(17) . ? Br14 C129 1.895(15) . ? Cl11 C103 1.747(19) . ? Cl12 C122 1.753(16) . ? Cl13 C127 1.774(17) . ? Cl14 C136 1.751(16) . ? N101 C106 1.247(18) . ? N101 C107 1.498(18) . ? N102 C117 1.305(17) . ? N102 C116 1.449(18) . ? N103 C124 1.438(19) . ? N103 C108 1.450(17) . ? N103 C109 1.457(18) . ? N104 C115 1.463(17) . ? N104 C114 1.464(19) . ? N104 C131 1.480(17) . ? N105 C124 1.460(18) . ? N105 C110 1.476(18) . ? N105 C111 1.480(17) . ? N106 C112 1.458(17) . ? N106 C131 1.464(18) . ? N106 C113 1.485(18) . ? O101 C100 1.338(19) . ? O101 H1 0.8400 . ? O102 C119 1.278(17) . ? O102 H2 0.8400 . ? O103 C130 1.371(18) . ? O103 H3 0.8400 . ? O104 C133 1.322(16) . ? O104 H4 0.8400 . ? C100 C105 1.38(2) . ? C100 C101 1.45(2) . ? C101 C102 1.35(2) . ? C102 C103 1.37(2) . ? C102 H102 0.9500 . ? C103 C104 1.37(2) . ? C104 C105 1.41(2) . ? C104 H104 0.9500 . ? C105 C106 1.47(2) . ? C106 H106 0.9500 . ? C107 C108 1.52(2) . ? C107 H10A 0.9900 . ? C107 H10B 0.9900 . ? C108 H10C 0.9900 . ? C108 H10D 0.9900 . ? C109 C110 1.54(2) . ? C109 H10E 0.9900 . ? C109 H10F 0.9900 . ? C110 H11A 0.9900 . ? C110 H11B 0.9900 . ? C111 C112 1.496(19) . ? C111 H11C 0.9900 . ? C111 H11D 0.9900 . ? C112 H11E 0.9900 . ? C112 H11F 0.9900 . ? C113 C114 1.50(2) . ? C113 H11G 0.9900 . ? C113 H11H 0.9900 . ? C114 H11I 0.9900 . ? C114 H11J 0.9900 . ? C115 C116 1.562(19) . ? C115 H11K 0.9900 . ? C115 H11L 0.9900 . ? C116 H11M 0.9900 . ? C116 H11N 0.9900 . ? C117 C118 1.44(2) . ? C117 H117 0.9500 . ? C118 C123 1.41(2) . ? C118 C119 1.45(2) . ? C119 C120 1.43(2) . ? C120 C121 1.348(19) . ? C121 C122 1.37(2) . ? C121 H121 0.9500 . ? C122 C123 1.34(2) . ? C123 H123 0.9500 . ? C124 C125 1.50(2) . ? C124 H124 1.0000 . ? C125 C126 1.40(2) . ? C125 C130 1.40(2) . ? C126 C127 1.395(19) . ? C126 H126 0.9500 . ? C127 C128 1.368(19) . ? C128 C129 1.35(2) . ? C128 H128 0.9500 . ? C129 C130 1.39(2) . ? C131 C132 1.50(2) . ? C131 H131 1.0000 . ? C132 C137 1.376(19) . ? C132 C133 1.43(2) . ? C133 C134 1.38(2) . ? C134 C135 1.40(2) . ? C135 C136 1.373(19) . ? C135 H135 0.9500 . ? C136 C137 1.37(2) . ? C137 H137 0.9500 . ? 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 C106 N101 C107 117.2(14) . . ? C117 N102 C116 126.9(14) . . ? C124 N103 C108 113.0(14) . . ? C124 N103 C109 104.0(13) . . ? C108 N103 C109 114.0(12) . . ? C115 N104 C114 115.8(12) . . ? C115 N104 C131 112.6(12) . . ? C114 N104 C131 105.2(12) . . ? C124 N105 C110 105.0(12) . . ? C124 N105 C111 116.7(13) . . ? C110 N105 C111 113.7(12) . . ? C112 N106 C131 113.7(12) . . ? C112 N106 C113 114.2(13) . . ? C131 N106 C113 104.1(11) . . ? C100 O101 H1 109.5 . . ? C119 O102 H2 109.5 . . ? C130 O103 H3 109.5 . . ? C133 O104 H4 109.5 . . ? O101 C100 C105 124.4(17) . . ? O101 C100 C101 118.9(16) . . ? C105 C100 C101 116.6(17) . . ? C102 C101 C100 122.2(17) . . ? C102 C101 Br12 121.9(14) . . ? C100 C101 Br12 115.9(14) . . ? C101 C102 C103 118.3(18) . . ? C101 C102 H102 120.8 . . ? C103 C102 H102 120.8 . . ? C104 C103 C102 123.0(19) . . ? C104 C103 Cl11 118.9(15) . . ? C102 C103 Cl11 118.1(15) . . ? C103 C104 C105 118.9(17) . . ? C103 C104 H104 120.6 . . ? C105 C104 H104 120.6 . . ? C100 C105 C104 121.0(17) . . ? C100 C105 C106 118.3(17) . . ? C104 C105 C106 120.2(16) . . ? N101 C106 C105 123.9(16) . . ? N101 C106 H106 118.1 . . ? C105 C106 H106 118.1 . . ? N101 C107 C108 110.9(14) . . ? N101 C107 H10A 109.5 . . ? C108 C107 H10A 109.5 . . ? N101 C107 H10B 109.5 . . ? C108 C107 H10B 109.5 . . ? H10A C107 H10B 108.0 . . ? N103 C108 C107 108.6(14) . . ? N103 C108 H10C 110.0 . . ? C107 C108 H10C 110.0 . . ? N103 C108 H10D 110.0 . . ? C107 C108 H10D 110.0 . . ? H10C C108 H10D 108.3 . . ? N103 C109 C110 106.4(12) . . ? N103 C109 H10E 110.4 . . ? C110 C109 H10E 110.4 . . ? N103 C109 H10F 110.4 . . ? C110 C109 H10F 110.4 . . ? H10E C109 H10F 108.6 . . ? N105 C110 C109 103.0(12) . . ? N105 C110 H11A 111.2 . . ? C109 C110 H11A 111.2 . . ? N105 C110 H11B 111.2 . . ? C109 C110 H11B 111.2 . . ? H11A C110 H11B 109.1 . . ? N105 C111 C112 112.9(14) . . ? N105 C111 H11C 109.0 . . ? C112 C111 H11C 109.0 . . ? N105 C111 H11D 109.0 . . ? C112 C111 H11D 109.0 . . ? H11C C111 H11D 107.8 . . ? N106 C112 C111 112.5(13) . . ? N106 C112 H11E 109.1 . . ? C111 C112 H11E 109.1 . . ? N106 C112 H11F 109.1 . . ? C111 C112 H11F 109.1 . . ? H11E C112 H11F 107.8 . . ? N106 C113 C114 103.4(14) . . ? N106 C113 H11G 111.1 . . ? C114 C113 H11G 111.1 . . ? N106 C113 H11H 111.1 . . ? C114 C113 H11H 111.1 . . ? H11G C113 H11H 109.0 . . ? N104 C114 C113 106.9(12) . . ? N104 C114 H11I 110.3 . . ? C113 C114 H11I 110.3 . . ? N104 C114 H11J 110.3 . . ? C113 C114 H11J 110.3 . . ? H11I C114 H11J 108.6 . . ? N104 C115 C116 111.5(13) . . ? N104 C115 H11K 109.3 . . ? C116 C115 H11K 109.3 . . ? N104 C115 H11L 109.3 . . ? C116 C115 H11L 109.3 . . ? H11K C115 H11L 108.0 . . ? N102 C116 C115 114.2(13) . . ? N102 C116 H11M 108.7 . . ? C115 C116 H11M 108.7 . . ? N102 C116 H11N 108.7 . . ? C115 C116 H11N 108.7 . . ? H11M C116 H11N 107.6 . . ? N102 C117 C118 122.1(15) . . ? N102 C117 H117 118.9 . . ? C118 C117 H117 118.9 . . ? C123 C118 C117 122.5(15) . . ? C123 C118 C119 118.5(16) . . ? C117 C118 C119 118.9(15) . . ? O102 C119 C120 121.8(15) . . ? O102 C119 C118 122.4(17) . . ? C120 C119 C118 115.8(15) . . ? C121 C120 C119 122.7(15) . . ? C121 C120 Br11 121.3(14) . . ? C119 C120 Br11 116.0(11) . . ? C120 C121 C122 119.4(17) . . ? C120 C121 H121 120.3 . . ? C122 C121 H121 120.3 . . ? C123 C122 C121 122.3(16) . . ? C123 C122 Cl12 119.5(12) . . ? C121 C122 Cl12 118.2(14) . . ? C122 C123 C118 121.0(15) . . ? C122 C123 H123 119.5 . . ? C118 C123 H123 119.5 . . ? N103 C124 N105 103.7(14) . . ? N103 C124 C125 114.0(14) . . ? N105 C124 C125 110.6(13) . . ? N103 C124 H124 109.4 . . ? N105 C124 H124 109.4 . . ? C125 C124 H124 109.4 . . ? C126 C125 C130 117.5(15) . . ? C126 C125 C124 120.4(14) . . ? C130 C125 C124 122.0(16) . . ? C127 C126 C125 119.4(15) . . ? C127 C126 H126 120.3 . . ? C125 C126 H126 120.3 . . ? C128 C127 C126 121.9(17) . . ? C128 C127 Cl13 118.7(13) . . ? C126 C127 Cl13 119.1(13) . . ? C129 C128 C127 118.5(16) . . ? C129 C128 H128 120.7 . . ? C127 C128 H128 120.7 . . ? C128 C129 C130 121.9(15) . . ? C128 C129 Br14 120.6(12) . . ? C130 C129 Br14 117.4(13) . . ? O103 C130 C129 120.2(15) . . ? O103 C130 C125 119.5(15) . . ? C129 C130 C125 120.3(17) . . ? N106 C131 N104 102.1(12) . . ? N106 C131 C132 110.8(13) . . ? N104 C131 C132 111.8(14) . . ? N106 C131 H131 110.6 . . ? N104 C131 H131 110.6 . . ? C132 C131 H131 110.6 . . ? C137 C132 C133 118.5(15) . . ? C137 C132 C131 121.7(15) . . ? C133 C132 C131 119.8(15) . . ? O104 C133 C134 119.1(15) . . ? O104 C133 C132 122.2(14) . . ? C134 C133 C132 118.6(15) . . ? C133 C134 C135 121.5(16) . . ? C133 C134 Br13 118.8(13) . . ? C135 C134 Br13 119.7(13) . . ? C136 C135 C134 118.8(16) . . ? C136 C135 H135 120.6 . . ? C134 C135 H135 120.6 . . ? C137 C136 C135 120.6(16) . . ? C137 C136 Cl14 121.2(13) . . ? C135 C136 Cl14 118.1(13) . . ? C136 C137 C132 121.9(16) . . ? C136 C137 H137 119.0 . . ? C132 C137 H137 119.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O101 C100 C101 C102 175.5(16) . . . . ? C105 C100 C101 C102 0(3) . . . . ? O101 C100 C101 Br12 -4(2) . . . . ? C105 C100 C101 Br12 -179.3(13) . . . . ? C100 C101 C102 C103 -2(3) . . . . ? Br12 C101 C102 C103 177.1(13) . . . . ? C101 C102 C103 C104 3(3) . . . . ? C101 C102 C103 Cl11 -175.1(14) . . . . ? C102 C103 C104 C105 -1(3) . . . . ? Cl11 C103 C104 C105 176.5(13) . . . . ? O101 C100 C105 C104 -173.9(16) . . . . ? C101 C100 C105 C104 2(3) . . . . ? O101 C100 C105 C106 -2(3) . . . . ? C101 C100 C105 C106 173.0(15) . . . . ? C103 C104 C105 C100 -1(3) . . . . ? C103 C104 C105 C106 -172.2(16) . . . . ? C107 N101 C106 C105 -174.2(15) . . . . ? C100 C105 C106 N101 -5(3) . . . . ? C104 C105 C106 N101 166.8(16) . . . . ? C106 N101 C107 C108 -123.1(16) . . . . ? C124 N103 C108 C107 -174.1(13) . . . . ? C109 N103 C108 C107 67.5(17) . . . . ? N101 C107 C108 N103 176.3(12) . . . . ? C124 N103 C109 C110 25.7(17) . . . . ? C108 N103 C109 C110 149.2(14) . . . . ? C124 N105 C110 C109 -23.9(16) . . . . ? C111 N105 C110 C109 -152.7(13) . . . . ? N103 C109 C110 N105 -1.0(17) . . . . ? C124 N105 C111 C112 171.9(12) . . . . ? C110 N105 C111 C112 -65.5(16) . . . . ? C131 N106 C112 C111 167.3(13) . . . . ? C113 N106 C112 C111 -73.5(17) . . . . ? N105 C111 C112 N106 -62.5(17) . . . . ? C112 N106 C113 C114 -157.3(13) . . . . ? C131 N106 C113 C114 -32.8(16) . . . . ? C115 N104 C114 C113 141.5(14) . . . . ? C131 N104 C114 C113 16.6(17) . . . . ? N106 C113 C114 N104 9.8(17) . . . . ? C114 N104 C115 C116 63.5(18) . . . . ? C131 N104 C115 C116 -175.4(13) . . . . ? C117 N102 C116 C115 -2(2) . . . . ? N104 C115 C116 N102 61.9(19) . . . . ? C116 N102 C117 C118 175.3(16) . . . . ? N102 C117 C118 C123 -178.8(15) . . . . ? N102 C117 C118 C119 1(3) . . . . ? C123 C118 C119 O102 -175.6(15) . . . . ? C117 C118 C119 O102 4(3) . . . . ? C123 C118 C119 C120 5(2) . . . . ? C117 C118 C119 C120 -175.0(15) . . . . ? O102 C119 C120 C121 179.0(16) . . . . ? C118 C119 C120 C121 -2(3) . . . . ? O102 C119 C120 Br11 -4(2) . . . . ? C118 C119 C120 Br11 175.5(11) . . . . ? C119 C120 C121 C122 -2(3) . . . . ? Br11 C120 C121 C122 -179.6(12) . . . . ? C120 C121 C122 C123 3(3) . . . . ? C120 C121 C122 Cl12 -175.7(13) . . . . ? C121 C122 C123 C118 0(3) . . . . ? Cl12 C122 C123 C118 179.4(12) . . . . ? C117 C118 C123 C122 175.5(17) . . . . ? C119 C118 C123 C122 -5(2) . . . . ? C108 N103 C124 N105 -165.3(12) . . . . ? C109 N103 C124 N105 -41.1(15) . . . . ? C108 N103 C124 C125 74.4(18) . . . . ? C109 N103 C124 C125 -161.5(14) . . . . ? C110 N105 C124 N103 41.0(15) . . . . ? C111 N105 C124 N103 168.0(12) . . . . ? C110 N105 C124 C125 163.6(13) . . . . ? C111 N105 C124 C125 -69.4(17) . . . . ? N103 C124 C125 C126 -103.7(19) . . . . ? N105 C124 C125 C126 139.9(16) . . . . ? N103 C124 C125 C130 80(2) . . . . ? N105 C124 C125 C130 -36(2) . . . . ? C130 C125 C126 C127 -5(2) . . . . ? C124 C125 C126 C127 178.9(15) . . . . ? C125 C126 C127 C128 7(3) . . . . ? C125 C126 C127 Cl13 -179.8(12) . . . . ? C126 C127 C128 C129 -4(3) . . . . ? Cl13 C127 C128 C129 -176.4(13) . . . . ? C127 C128 C129 C130 -3(3) . . . . ? C127 C128 C129 Br14 -179.5(12) . . . . ? C128 C129 C130 O103 -177.3(16) . . . . ? Br14 C129 C130 O103 -1(2) . . . . ? C128 C129 C130 C125 5(3) . . . . ? Br14 C129 C130 C125 -177.8(12) . . . . ? C126 C125 C130 O103 -178.7(14) . . . . ? C124 C125 C130 O103 -2(2) . . . . ? C126 C125 C130 C129 -1(2) . . . . ? C124 C125 C130 C129 174.9(15) . . . . ? C112 N106 C131 N104 168.0(12) . . . . ? C113 N106 C131 N104 43.2(15) . . . . ? C112 N106 C131 C132 -72.8(17) . . . . ? C113 N106 C131 C132 162.4(13) . . . . ? C115 N104 C131 N106 -163.8(13) . . . . ? C114 N104 C131 N106 -36.8(15) . . . . ? C115 N104 C131 C132 77.8(17) . . . . ? C114 N104 C131 C132 -155.3(13) . . . . ? N106 C131 C132 C137 137.4(15) . . . . ? N104 C131 C132 C137 -109.5(17) . . . . ? N106 C131 C132 C133 -43(2) . . . . ? N104 C131 C132 C133 69.7(18) . . . . ? C137 C132 C133 O104 176.9(14) . . . . ? C131 C132 C133 O104 -2(2) . . . . ? C137 C132 C133 C134 1(2) . . . . ? C131 C132 C133 C134 -178.5(15) . . . . ? O104 C133 C134 C135 -177.0(13) . . . . ? C132 C133 C134 C135 -1(2) . . . . ? O104 C133 C134 Br13 3(2) . . . . ? C132 C133 C134 Br13 179.8(11) . . . . ? C133 C134 C135 C136 -1(2) . . . . ? Br13 C134 C135 C136 178.6(12) . . . . ? C134 C135 C136 C137 3(2) . . . . ? C134 C135 C136 Cl14 179.2(12) . . . . ? C135 C136 C137 C132 -3(3) . . . . ? Cl14 C136 C137 C132 -179.2(12) . . . . ? C133 C132 C137 C136 1(2) . . . . ? C131 C132 C137 C136 -179.9(15) . . . . ? 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 O101 H1 N101 0.84 1.97 2.600(17) 132 . O102 H2 N102 0.84 1.81 2.567(17) 148 . O103 H3 N105 0.84 1.96 2.616(15) 135 . O103 H3 O104 0.84 2.60 3.020(15) 112 . O104 H4 N104 0.84 2.66 3.141(15) 118 . O104 H4 O103 0.84 2.51 3.020(15) 121 . _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 18.84 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.634 _refine_diff_density_min -0.684 _refine_diff_density_rms 0.146 #END data_1.0.25H2O.2.5MeOH _database_code_depnum_ccdc_archive 'CCDC 825863' #TrackingRef '- cifs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; 'C42 H38 Br4 Cl4 Cu N6 Ni2 O8, 2.5(C H4 O), 0.25 O' ; _chemical_formula_sum 'C44.50 H48 Br4 Cl4 Cu N6 Ni2 O10.75' _chemical_formula_weight 1481.29 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' O O 0.0106 0.0060 '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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.0857(9) _cell_length_b 13.6167(10) _cell_length_c 17.0194(12) _cell_angle_alpha 72.997(4) _cell_angle_beta 88.993(4) _cell_angle_gamma 67.063(4) _cell_volume 2654.7(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1817 _cell_measurement_theta_min 2.416 _cell_measurement_theta_max 22.2665 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.853 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1472 _exptl_absorpt_coefficient_mu 4.373 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6817 _exptl_absorpt_correction_T_max 0.8772 _exptl_absorpt_process_details 'SABADS (Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 KappaAPEXII' _diffrn_measurement_method 'omega and phi scans' _diffrn_reflns_number 57665 _diffrn_reflns_av_R_equivalents 0.0691 _diffrn_reflns_av_sigmaI/netI 0.0834 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.26 _diffrn_reflns_theta_max 25.35 _reflns_number_total 9650 _reflns_number_gt 6311 _reflns_threshold_expression >2\s(I) _computing_data_collection 'BRUKER APEX2' _computing_cell_refinement 'BRUKER APEX2' _computing_data_reduction ? _computing_structure_solution 'SIR-2004 (Burla, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0611P)^2^+3.7503P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9652 _refine_ls_number_parameters 669 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0997 _refine_ls_R_factor_gt 0.0517 _refine_ls_wR_factor_ref 0.1346 _refine_ls_wR_factor_gt 0.1140 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _refine_ls_shift/su_max 0.007 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni11 Ni 0.36012(7) 0.44442(6) 0.58544(5) 0.0154(2) Uani 1 1 d . . . Ni12 Ni 0.31132(6) 0.37048(6) 0.76756(5) 0.0166(2) Uani 1 1 d . . . Cu13 Cu 0.16714(7) 0.49648(7) 0.88801(5) 0.0232(2) Uani 1 1 d . . . O101 O 0.2629(4) 0.5978(4) 0.5297(3) 0.0246(11) Uani 1 1 d . . . O102 O 0.1335(4) 0.6524(4) 0.8422(3) 0.0341(12) Uani 1 1 d . . . O103 O 0.2550(3) 0.3541(3) 0.6636(3) 0.0208(10) Uani 1 1 d . . . O104 O 0.3499(3) 0.4154(3) 0.8628(2) 0.0177(10) Uani 1 1 d . . . N101 N 0.3674(5) 0.4024(4) 0.4861(3) 0.0238(13) Uani 1 1 d . . . N102 N 0.1742(4) 0.5025(5) 0.9997(3) 0.0234(13) Uani 1 1 d . . . N103 N 0.5007(4) 0.2894(4) 0.6317(3) 0.0188(12) Uani 1 1 d . . . N104 N 0.1683(4) 0.3378(4) 0.9432(3) 0.0198(12) Uani 1 1 d . . . N105 N 0.4680(4) 0.2333(4) 0.7681(3) 0.0153(11) Uani 1 1 d . . . N106 N 0.2791(4) 0.2401(4) 0.8599(3) 0.0188(12) Uani 1 1 d . . . O10 O 0.3615(3) 0.4800(3) 0.6856(2) 0.0178(10) Uani 1 1 d . . . O20 O 0.1514(3) 0.4872(3) 0.7768(3) 0.0221(10) Uani 1 1 d . . . C10 C 0.3785(11) 0.5667(8) 0.6849(5) 0.061(3) Uani 1 1 d . . . C11 C 0.3345(9) 0.6373(10) 0.7294(7) 0.091(4) Uani 1 1 d . . . H11A H 0.3707 0.6883 0.7210 0.136 Uiso 1 1 calc R . . H11B H 0.3453 0.5952 0.7869 0.136 Uiso 1 1 calc R . . H11C H 0.2561 0.6790 0.7119 0.136 Uiso 1 1 calc R . . O11 O 0.4678(7) 0.5731(7) 0.6413(6) 0.103(3) Uani 1 1 d . . . C20 C 0.0554(6) 0.5552(5) 0.7337(4) 0.0249(16) Uani 1 1 d . . . C21 C 0.0541(6) 0.5956(6) 0.6434(4) 0.038(2) Uani 1 1 d . . . H21A H -0.0205 0.6220 0.6177 0.057 Uiso 1 1 calc R . . H21B H 0.1031 0.5353 0.6247 0.057 Uiso 1 1 calc R . . H21C H 0.0787 0.6558 0.6289 0.057 Uiso 1 1 calc R . . O21 O -0.0296(4) 0.5858(4) 0.7698(3) 0.0356(13) Uani 1 1 d . . . C100 C 0.2180(5) 0.6419(5) 0.4537(4) 0.0202(15) Uani 1 1 d . . . C101 C 0.1506(5) 0.7587(5) 0.4230(4) 0.0205(15) Uani 1 1 d . . . Br11 Br 0.12872(7) 0.84566(6) 0.49465(4) 0.0358(2) Uani 1 1 d . . . C102 C 0.1019(5) 0.8114(5) 0.3418(4) 0.0224(15) Uani 1 1 d . . . H102 H 0.0578 0.8880 0.3233 0.027 Uiso 1 1 calc R . . C103 C 0.1208(5) 0.7468(6) 0.2886(4) 0.0245(16) Uani 1 1 d . . . Cl11 Cl 0.06221(14) 0.81598(15) 0.18481(10) 0.0300(4) Uani 1 1 d . . . C104 C 0.1849(5) 0.6347(6) 0.3131(4) 0.0239(16) Uani 1 1 d . . . H104 H 0.1968 0.5939 0.2760 0.029 Uiso 1 1 calc R . . C105 C 0.2333(5) 0.5814(5) 0.3962(4) 0.0187(14) Uani 1 1 d . . . C106 C 0.3098(5) 0.4650(5) 0.4154(4) 0.0204(15) Uani 1 1 d . . . H106 H 0.3182 0.4324 0.3734 0.024 Uiso 1 1 calc R . . C107 C 0.4497(6) 0.2885(5) 0.4929(4) 0.0272(17) Uani 1 1 d . . . H10A H 0.4772 0.2858 0.4399 0.033 Uiso 1 1 calc R . . H10B H 0.4160 0.2347 0.5105 0.033 Uiso 1 1 calc R . . C108 C 0.5444(6) 0.2621(6) 0.5565(4) 0.0260(16) Uani 1 1 d . . . H10C H 0.5932 0.1830 0.5712 0.031 Uiso 1 1 calc R . . H10D H 0.5879 0.3050 0.5329 0.031 Uiso 1 1 calc R . . C109 C 0.5860(5) 0.3032(6) 0.6815(4) 0.0222(15) Uani 1 1 d . . . H10E H 0.6612 0.2562 0.6744 0.027 Uiso 1 1 calc R . . H10F H 0.5777 0.3806 0.6643 0.027 Uiso 1 1 calc R . . C110 C 0.5633(5) 0.2676(6) 0.7704(4) 0.0210(15) Uani 1 1 d . . . H11D H 0.6285 0.2052 0.8038 0.025 Uiso 1 1 calc R . . H11E H 0.5434 0.3292 0.7932 0.025 Uiso 1 1 calc R . . C111 C 0.4775(5) 0.1393(5) 0.8423(4) 0.0206(15) Uani 1 1 d . . . H11F H 0.5051 0.1498 0.8905 0.025 Uiso 1 1 calc R . . H11G H 0.5305 0.0695 0.8360 0.025 Uiso 1 1 calc R . . C112 C 0.3652(5) 0.1326(5) 0.8553(4) 0.0191(15) Uani 1 1 d . . . H11H H 0.3417 0.1137 0.8100 0.023 Uiso 1 1 calc R . . H11I H 0.3724 0.0735 0.9061 0.023 Uiso 1 1 calc R . . C113 C 0.1637(5) 0.2479(6) 0.8416(4) 0.0226(15) Uani 1 1 d . . . H11J H 0.1634 0.1738 0.8546 0.027 Uiso 1 1 calc R . . H11K H 0.1363 0.2881 0.7838 0.027 Uiso 1 1 calc R . . C114 C 0.0921(5) 0.3116(6) 0.8968(4) 0.0251(16) Uani 1 1 d . . . H11L H 0.0321 0.3800 0.8637 0.030 Uiso 1 1 calc R . . H11M H 0.0599 0.2658 0.9346 0.030 Uiso 1 1 calc R . . C115 C 0.1322(6) 0.3396(6) 1.0265(4) 0.0251(16) Uani 1 1 d . . . H11N H 0.1545 0.2632 1.0626 0.030 Uiso 1 1 calc R . . H11O H 0.0515 0.3764 1.0219 0.030 Uiso 1 1 calc R . . C116 C 0.1829(6) 0.4005(5) 1.0644(4) 0.0266(16) Uani 1 1 d . . . H11P H 0.1430 0.4194 1.1100 0.032 Uiso 1 1 calc R . . H11Q H 0.2605 0.3531 1.0851 0.032 Uiso 1 1 calc R . . C117 C 0.1770(5) 0.5846(6) 1.0213(4) 0.0258(16) Uani 1 1 d . . . H117 H 0.1874 0.5739 1.0776 0.031 Uiso 1 1 calc R . . C118 C 0.1654(6) 0.6922(6) 0.9653(4) 0.0259(16) Uani 1 1 d . . . C119 C 0.1737(6) 0.7707(6) 1.0004(5) 0.0339(18) Uani 1 1 d . . . H119 H 0.1880 0.7514 1.0574 0.041 Uiso 1 1 calc R . . C120 C 0.1612(7) 0.8738(7) 0.9522(5) 0.039(2) Uani 1 1 d . . . Cl12 Cl 0.1759(2) 0.97096(17) 0.99540(13) 0.0549(6) Uani 1 1 d . . . C121 C 0.1392(6) 0.9052(6) 0.8655(5) 0.039(2) Uani 1 1 d . A . H121 H 0.1313 0.9759 0.8322 0.047 Uiso 1 1 calc R . . C122 C 0.1300(7) 0.8295(6) 0.8319(4) 0.039(2) Uani 1 1 d . . . Br2' Br 0.0763(7) 0.8799(10) 0.7206(8) 0.036(3) Uiso 0.24(3) 1 d P A 3 Br12 Br 0.1044(13) 0.8710(5) 0.7142(3) 0.0754(14) Uani 0.76(3) 1 d P A 4 C123 C 0.1423(6) 0.7190(6) 0.8780(5) 0.0327(18) Uani 1 1 d . A . C130 C 0.4816(5) 0.1978(5) 0.6933(4) 0.0177(14) Uani 1 1 d . . . H130 H 0.5500 0.1293 0.7040 0.021 Uiso 1 1 calc R . . C131 C 0.3878(5) 0.1755(5) 0.6634(4) 0.0219(15) Uani 1 1 d . . . C132 C 0.4125(6) 0.0757(5) 0.6455(4) 0.0245(16) Uani 1 1 d . . . H132 H 0.4848 0.0203 0.6578 0.029 Uiso 1 1 calc R . . C133 C 0.3293(7) 0.0595(6) 0.6093(4) 0.0301(18) Uani 1 1 d . . . Cl13 Cl 0.35926(19) -0.06634(16) 0.58592(12) 0.0444(5) Uani 1 1 d . . . C134 C 0.2222(6) 0.1404(6) 0.5906(4) 0.0306(18) Uani 1 1 d . . . H134 H 0.1664 0.1290 0.5663 0.037 Uiso 1 1 calc R . . C135 C 0.1989(6) 0.2389(6) 0.6086(4) 0.0247(16) Uani 1 1 d . . . Br13 Br 0.05500(6) 0.35637(6) 0.57620(5) 0.0346(2) Uani 1 1 d . . . C136 C 0.2778(5) 0.2606(5) 0.6470(4) 0.0174(14) Uani 1 1 d . . . C140 C 0.2788(5) 0.2439(5) 0.9471(4) 0.0178(14) Uani 1 1 d . . . H140 H 0.2763 0.1742 0.9831 0.021 Uiso 1 1 calc R . . C141 C 0.3773(5) 0.2569(5) 0.9794(4) 0.0162(14) Uani 1 1 d . . . C142 C 0.4343(5) 0.1854(5) 1.0568(4) 0.0192(15) Uani 1 1 d . . . H142 H 0.4124 0.1294 1.0873 0.023 Uiso 1 1 calc R . . C143 C 0.5225(5) 0.1989(5) 1.0872(4) 0.0208(15) Uani 1 1 d . . . Cl14 Cl 0.59047(15) 0.11433(14) 1.18651(10) 0.0295(4) Uani 1 1 d . . . C144 C 0.5572(5) 0.2807(5) 1.0432(4) 0.0231(15) Uani 1 1 d . . . H144 H 0.6172 0.2888 1.0648 0.028 Uiso 1 1 calc R . . C145 C 0.5016(5) 0.3498(5) 0.9673(4) 0.0218(15) Uani 1 1 d . . . Br14 Br 0.54846(6) 0.46134(6) 0.90447(4) 0.02671(18) Uani 1 1 d . . . C146 C 0.4081(5) 0.3436(5) 0.9328(4) 0.0174(14) Uani 1 1 d . . . O1S O -0.2777(5) 0.9261(5) 0.8104(4) 0.0243(14) Uani 0.75 1 d P . . H1S H -0.2568 0.8713 0.7938 0.036 Uiso 0.75 1 calc PR . . C1S C -0.1944(8) 0.9663(9) 0.8057(7) 0.045(3) Uani 0.75 1 d P . . H1S1 H -0.2165 1.0268 0.8290 0.068 Uiso 0.75 1 calc PR . . H1S2 H -0.1828 0.9928 0.7489 0.068 Uiso 0.75 1 calc PR . . H1S3 H -0.1264 0.9070 0.8359 0.068 Uiso 0.75 1 calc PR . . O2S O -0.2669(7) 0.5795(7) 0.7616(5) 0.048(2) Uiso 0.75 1 d P B 3 H2S H -0.2309 0.6066 0.7290 0.072 Uiso 0.75 1 calc PR B 3 C2S C -0.3850(13) 0.6683(12) 0.7555(9) 0.070(4) Uiso 0.75 1 d P B 3 H2S1 H -0.4014 0.6753 0.8093 0.104 Uiso 0.75 1 calc PR B 3 H2S2 H -0.4376 0.6463 0.7346 0.104 Uiso 0.75 1 calc PR B 3 H2S3 H -0.3902 0.7390 0.7188 0.104 Uiso 0.75 1 calc PR B 3 O1W O -0.328(3) 0.624(3) 0.755(2) 0.070(9) Uiso 0.25 1 d P C 4 O3S O -0.1886(11) 0.7989(11) 0.7178(8) 0.051(4) Uiso 0.50 1 d P D 5 H3S H -0.1375 0.7366 0.7278 0.077 Uiso 0.50 1 calc PR D 5 C3S C -0.1984(17) 0.8598(16) 0.6315(11) 0.055(5) Uiso 0.50 1 d P D 5 H3S1 H -0.2586 0.9324 0.6197 0.083 Uiso 0.50 1 calc PR D 5 H3S2 H -0.2130 0.8192 0.5987 0.083 Uiso 0.50 1 calc PR D 5 H3S3 H -0.1300 0.8683 0.6187 0.083 Uiso 0.50 1 calc PR D 5 O3S' O -0.2158(10) 0.7712(10) 0.7160(7) 0.041(3) Uiso 0.50 1 d P E 6 H3S' H -0.2358 0.7190 0.7282 0.061 Uiso 0.50 1 calc PR E 6 C3S' C -0.2321(18) 0.8219(17) 0.6264(12) 0.062(6) Uiso 0.50 1 d P E 6 H3S4 H -0.2956 0.8925 0.6116 0.093 Uiso 0.50 1 calc PR E 6 H3S5 H -0.2445 0.7728 0.6008 0.093 Uiso 0.50 1 calc PR E 6 H3S6 H -0.1669 0.8337 0.6080 0.093 Uiso 0.50 1 calc PR E 6 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 Ni11 0.0203(4) 0.0147(4) 0.0067(4) 0.0000(3) -0.0023(3) -0.0046(4) Ni12 0.0145(4) 0.0171(4) 0.0120(4) 0.0000(3) -0.0032(3) -0.0031(3) Cu13 0.0219(4) 0.0218(5) 0.0147(4) -0.0010(4) -0.0026(4) -0.0005(4) O101 0.028(3) 0.024(3) 0.013(2) -0.002(2) -0.002(2) -0.005(2) O102 0.046(3) 0.023(3) 0.022(3) -0.005(2) -0.009(2) -0.002(2) O103 0.021(2) 0.021(3) 0.016(2) -0.005(2) -0.001(2) -0.005(2) O104 0.018(2) 0.016(2) 0.012(2) 0.0010(19) -0.0036(19) -0.0029(19) N101 0.031(3) 0.018(3) 0.017(3) -0.004(3) -0.001(3) -0.006(3) N102 0.024(3) 0.022(3) 0.016(3) 0.001(3) 0.002(3) -0.006(3) N103 0.017(3) 0.022(3) 0.013(3) -0.005(2) 0.001(2) -0.004(2) N104 0.015(3) 0.021(3) 0.015(3) 0.000(2) 0.002(2) -0.002(2) N105 0.020(3) 0.016(3) 0.007(3) 0.000(2) -0.002(2) -0.007(2) N106 0.015(3) 0.026(3) 0.013(3) -0.005(2) 0.001(2) -0.006(2) O10 0.020(2) 0.015(2) 0.015(2) -0.0002(19) -0.0006(19) -0.0078(19) O20 0.017(2) 0.022(3) 0.016(2) -0.002(2) -0.002(2) 0.002(2) C10 0.122(10) 0.046(6) 0.019(5) -0.001(4) -0.011(5) -0.044(6) C11 0.071(8) 0.090(9) 0.077(8) 0.009(7) 0.006(7) -0.021(7) O11 0.118(7) 0.086(6) 0.122(7) -0.038(5) 0.043(6) -0.055(5) C20 0.019(4) 0.023(4) 0.023(4) -0.004(3) -0.002(3) -0.001(3) C21 0.031(4) 0.037(5) 0.023(4) -0.002(4) -0.005(4) 0.006(4) O21 0.020(3) 0.041(3) 0.023(3) -0.001(2) -0.002(2) 0.005(2) C100 0.020(4) 0.024(4) 0.015(4) -0.002(3) 0.002(3) -0.011(3) C101 0.020(4) 0.019(4) 0.018(4) -0.002(3) 0.000(3) -0.006(3) Br11 0.0507(5) 0.0243(4) 0.0218(4) -0.0061(3) 0.0000(4) -0.0047(4) C102 0.016(3) 0.021(4) 0.019(4) -0.002(3) -0.003(3) 0.000(3) C103 0.012(3) 0.037(4) 0.018(4) -0.003(3) -0.003(3) -0.007(3) Cl11 0.0260(9) 0.0349(10) 0.0167(9) -0.0004(8) -0.0079(7) -0.0046(8) C104 0.023(4) 0.029(4) 0.018(4) -0.004(3) -0.002(3) -0.010(3) C105 0.017(3) 0.025(4) 0.012(3) -0.005(3) -0.002(3) -0.007(3) C106 0.023(4) 0.025(4) 0.014(4) -0.005(3) 0.003(3) -0.012(3) C107 0.040(4) 0.020(4) 0.013(4) -0.003(3) -0.003(3) -0.005(3) C108 0.030(4) 0.020(4) 0.020(4) -0.003(3) 0.002(3) -0.005(3) C109 0.014(3) 0.025(4) 0.024(4) -0.005(3) -0.003(3) -0.006(3) C110 0.015(3) 0.033(4) 0.013(3) -0.004(3) -0.001(3) -0.009(3) C111 0.019(4) 0.022(4) 0.014(3) -0.004(3) 0.002(3) -0.003(3) C112 0.021(4) 0.012(3) 0.015(3) 0.004(3) 0.002(3) -0.003(3) C113 0.019(4) 0.028(4) 0.019(4) -0.003(3) -0.001(3) -0.010(3) C114 0.017(4) 0.029(4) 0.024(4) -0.002(3) 0.001(3) -0.007(3) C115 0.023(4) 0.030(4) 0.018(4) -0.005(3) 0.006(3) -0.010(3) C116 0.027(4) 0.023(4) 0.019(4) 0.000(3) 0.003(3) -0.003(3) C117 0.016(4) 0.036(4) 0.017(4) -0.008(3) 0.002(3) -0.002(3) C118 0.022(4) 0.026(4) 0.023(4) -0.005(3) 0.002(3) -0.004(3) C119 0.034(4) 0.031(5) 0.028(4) -0.007(4) 0.003(4) -0.007(4) C120 0.041(5) 0.041(5) 0.039(5) -0.018(4) 0.009(4) -0.018(4) Cl12 0.0942(18) 0.0401(13) 0.0433(13) -0.0170(11) 0.0159(13) -0.0378(13) C121 0.046(5) 0.026(4) 0.033(5) -0.003(4) 0.009(4) -0.006(4) C122 0.050(5) 0.022(4) 0.022(4) 0.005(3) -0.004(4) 0.000(4) Br12 0.149(4) 0.0277(14) 0.0231(13) 0.0064(9) -0.016(2) -0.018(2) C123 0.025(4) 0.027(4) 0.028(4) 0.001(4) -0.005(3) 0.002(3) C130 0.014(3) 0.016(3) 0.016(3) 0.000(3) -0.004(3) -0.001(3) C131 0.026(4) 0.021(4) 0.014(3) -0.002(3) -0.002(3) -0.008(3) C132 0.031(4) 0.021(4) 0.012(3) 0.002(3) -0.006(3) -0.005(3) C133 0.054(5) 0.019(4) 0.012(4) 0.003(3) -0.008(4) -0.015(4) Cl13 0.0721(15) 0.0301(11) 0.0354(11) -0.0133(9) -0.0094(11) -0.0222(10) C134 0.045(5) 0.038(5) 0.014(4) 0.000(3) -0.004(3) -0.028(4) C135 0.025(4) 0.028(4) 0.013(4) 0.001(3) 0.000(3) -0.009(3) Br13 0.0225(4) 0.0457(5) 0.0276(4) -0.0005(4) -0.0100(3) -0.0128(3) C136 0.019(4) 0.020(4) 0.010(3) 0.001(3) -0.002(3) -0.009(3) C140 0.011(3) 0.014(3) 0.018(3) 0.004(3) 0.003(3) 0.000(3) C141 0.012(3) 0.014(3) 0.014(3) -0.004(3) -0.002(3) 0.004(3) C142 0.021(4) 0.020(4) 0.014(3) -0.001(3) 0.004(3) -0.009(3) C143 0.026(4) 0.021(4) 0.009(3) -0.003(3) -0.005(3) -0.004(3) Cl14 0.0383(10) 0.0249(10) 0.0154(9) 0.0043(7) -0.0136(8) -0.0097(8) C144 0.021(4) 0.024(4) 0.018(4) -0.004(3) -0.007(3) -0.004(3) C145 0.021(4) 0.019(4) 0.017(4) -0.004(3) -0.002(3) -0.001(3) Br14 0.0340(4) 0.0288(4) 0.0177(4) -0.0008(3) -0.0046(3) -0.0174(3) C146 0.015(3) 0.018(4) 0.013(3) -0.003(3) -0.003(3) -0.002(3) O1S 0.015(3) 0.017(3) 0.028(4) 0.002(3) 0.008(3) 0.001(3) C1S 0.028(6) 0.035(6) 0.059(8) -0.001(6) 0.008(6) -0.010(5) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Ni11 O10 1.906(4) . ? Ni11 O101 1.921(4) . ? Ni11 N101 1.927(5) . ? Ni11 N103 2.124(5) . ? Ni11 O103 2.339(4) . ? Ni12 O104 2.027(4) . ? Ni12 O10 2.029(4) . ? Ni12 O103 2.031(4) . ? Ni12 O20 2.115(4) . ? Ni12 N105 2.167(5) . ? Ni12 N106 2.175(5) . ? Cu13 O102 1.904(5) . ? Cu13 N102 1.932(5) . ? Cu13 O20 1.954(4) . ? Cu13 N104 2.082(5) . ? Cu13 O104 2.303(4) . ? O101 C100 1.296(7) . ? O102 C123 1.271(8) . ? O103 C136 1.305(7) . ? O104 C146 1.312(7) . ? N101 C106 1.294(8) . ? N101 C107 1.475(8) . ? N102 C117 1.289(8) . ? N102 C116 1.464(8) . ? N103 C108 1.480(8) . ? N103 C130 1.479(8) . ? N103 C109 1.512(8) . ? N104 C114 1.488(8) . ? N104 C115 1.492(8) . ? N104 C140 1.498(7) . ? N105 C130 1.474(8) . ? N105 C111 1.478(8) . ? N105 C110 1.497(7) . ? N106 C112 1.482(8) . ? N106 C140 1.499(8) . ? N106 C113 1.503(8) . ? O10 C10 1.280(9) . ? O20 C20 1.304(7) . ? C10 C11 1.345(14) . ? C10 O11 1.392(13) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C20 O21 1.246(8) . ? C20 C21 1.471(9) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C100 C105 1.418(9) . ? C100 C101 1.421(9) . ? C101 C102 1.387(9) . ? C101 Br11 1.881(6) . ? C102 C103 1.394(9) . ? C102 H102 0.9300 . ? C103 C104 1.361(9) . ? C103 Cl11 1.762(7) . ? C104 C105 1.415(9) . ? C104 H104 0.9300 . ? C105 C106 1.447(9) . ? C106 H106 0.9300 . ? C107 C108 1.520(9) . ? C107 H10A 0.9700 . ? C107 H10B 0.9700 . ? C108 H10C 0.9700 . ? C108 H10D 0.9700 . ? C109 C110 1.511(8) . ? C109 H10E 0.9700 . ? C109 H10F 0.9700 . ? C110 H11D 0.9700 . ? C110 H11E 0.9700 . ? C111 C112 1.516(8) . ? C111 H11F 0.9700 . ? C111 H11G 0.9700 . ? C112 H11H 0.9700 . ? C112 H11I 0.9700 . ? C113 C114 1.524(9) . ? C113 H11J 0.9700 . ? C113 H11K 0.9700 . ? C114 H11L 0.9700 . ? C114 H11M 0.9700 . ? C115 C116 1.515(9) . ? C115 H11N 0.9700 . ? C115 H11O 0.9700 . ? C116 H11P 0.9700 . ? C116 H11Q 0.9700 . ? C117 C118 1.446(9) . ? C117 H117 0.9300 . ? C118 C119 1.407(9) . ? C118 C123 1.430(10) . ? C119 C120 1.350(10) . ? C119 H119 0.9300 . ? C120 C121 1.411(10) . ? C120 Cl12 1.762(8) . ? C121 C122 1.360(10) . ? C121 H121 0.9300 . ? C122 C123 1.424(10) . ? C122 Br2' 1.861(15) . ? C122 Br12 1.912(9) . ? C130 C131 1.504(9) . ? C130 H130 0.9800 . ? C131 C132 1.394(9) . ? C131 C136 1.420(9) . ? C132 C133 1.380(9) . ? C132 H132 0.9300 . ? C133 C134 1.374(10) . ? C133 Cl13 1.765(7) . ? C134 C135 1.379(9) . ? C134 H134 0.9300 . ? C135 C136 1.398(9) . ? C135 Br13 1.893(7) . ? C140 C141 1.503(8) . ? C140 H140 0.9800 . ? C141 C142 1.399(8) . ? C141 C146 1.413(9) . ? C142 C143 1.370(9) . ? C142 H142 0.9300 . ? C143 C144 1.379(9) . ? C143 Cl14 1.757(6) . ? C144 C145 1.368(9) . ? C144 H144 0.9300 . ? C145 C146 1.410(9) . ? C145 Br14 1.891(7) . ? O1S C1S 1.389(11) . ? O1S H1S 0.8200 . ? C1S H1S1 0.9600 . ? C1S H1S2 0.9600 . ? C1S H1S3 0.9600 . ? O2S C2S 1.529(16) . ? O2S H2S 0.8200 . ? C2S H2S1 0.9600 . ? C2S H2S2 0.9600 . ? C2S H2S3 0.9600 . ? O3S C3S 1.44(2) . ? O3S H3S 0.8200 . ? C3S H3S1 0.9600 . ? C3S H3S2 0.9600 . ? C3S H3S3 0.9600 . ? O3S' C3S' 1.46(2) . ? O3S' H3S' 0.8200 . ? C3S' H3S4 0.9600 . ? C3S' H3S5 0.9600 . ? C3S' H3S6 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 O10 Ni11 O101 89.76(18) . . ? O10 Ni11 N101 176.7(2) . . ? O101 Ni11 N101 92.9(2) . . ? O10 Ni11 N103 92.83(18) . . ? O101 Ni11 N103 164.5(2) . . ? N101 Ni11 N103 84.1(2) . . ? O10 Ni11 O103 78.17(16) . . ? O101 Ni11 O103 108.72(17) . . ? N101 Ni11 O103 102.68(19) . . ? N103 Ni11 O103 86.75(17) . . ? O104 Ni12 O10 91.47(16) . . ? O104 Ni12 O103 170.05(16) . . ? O10 Ni12 O103 83.27(17) . . ? O104 Ni12 O20 80.49(16) . . ? O10 Ni12 O20 97.48(17) . . ? O103 Ni12 O20 91.78(17) . . ? O104 Ni12 N105 100.43(17) . . ? O10 Ni12 N105 90.30(17) . . ? O103 Ni12 N105 88.08(17) . . ? O20 Ni12 N105 172.15(17) . . ? O104 Ni12 N106 86.86(18) . . ? O10 Ni12 N106 173.00(18) . . ? O103 Ni12 N106 99.35(18) . . ? O20 Ni12 N106 88.96(18) . . ? N105 Ni12 N106 83.32(18) . . ? O102 Cu13 N102 92.2(2) . . ? O102 Cu13 O20 89.65(19) . . ? N102 Cu13 O20 176.1(2) . . ? O102 Cu13 N104 167.7(2) . . ? N102 Cu13 N104 84.9(2) . . ? O20 Cu13 N104 92.51(19) . . ? O102 Cu13 O104 102.37(19) . . ? N102 Cu13 O104 105.54(19) . . ? O20 Cu13 O104 77.44(16) . . ? N104 Cu13 O104 89.91(17) . . ? C100 O101 Ni11 128.1(4) . . ? C123 O102 Cu13 128.5(4) . . ? C136 O103 Ni12 126.5(4) . . ? C136 O103 Ni11 107.9(4) . . ? Ni12 O103 Ni11 90.23(16) . . ? C146 O104 Ni12 124.0(4) . . ? C146 O104 Cu13 108.0(3) . . ? Ni12 O104 Cu13 94.26(16) . . ? C106 N101 C107 118.5(5) . . ? C106 N101 Ni11 126.3(4) . . ? C107 N101 Ni11 115.3(4) . . ? C117 N102 C116 118.6(6) . . ? C117 N102 Cu13 126.2(5) . . ? C116 N102 Cu13 115.1(4) . . ? C108 N103 C130 114.1(5) . . ? C108 N103 C109 111.3(5) . . ? C130 N103 C109 100.9(5) . . ? C108 N103 Ni11 104.0(4) . . ? C130 N103 Ni11 116.6(4) . . ? C109 N103 Ni11 110.1(4) . . ? C114 N104 C115 110.4(5) . . ? C114 N104 C140 102.3(5) . . ? C115 N104 C140 112.8(5) . . ? C114 N104 Cu13 113.5(4) . . ? C115 N104 Cu13 104.4(4) . . ? C140 N104 Cu13 113.7(4) . . ? C130 N105 C111 111.0(5) . . ? C130 N105 C110 102.1(4) . . ? C111 N105 C110 111.4(5) . . ? C130 N105 Ni12 115.8(4) . . ? C111 N105 Ni12 106.3(4) . . ? C110 N105 Ni12 110.5(4) . . ? C112 N106 C140 110.5(5) . . ? C112 N106 C113 111.0(5) . . ? C140 N106 C113 102.3(4) . . ? C112 N106 Ni12 105.5(4) . . ? C140 N106 Ni12 117.0(4) . . ? C113 N106 Ni12 110.7(4) . . ? C10 O10 Ni11 119.5(5) . . ? C10 O10 Ni12 135.8(5) . . ? Ni11 O10 Ni12 104.12(19) . . ? C20 O20 Cu13 115.0(4) . . ? C20 O20 Ni12 142.2(4) . . ? Cu13 O20 Ni12 102.69(18) . . ? O10 C10 C11 128.8(11) . . ? O10 C10 O11 111.6(9) . . ? C11 C10 O11 118.7(9) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? O21 C20 O20 119.8(6) . . ? O21 C20 C21 122.9(6) . . ? O20 C20 C21 117.3(6) . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? O101 C100 C105 124.3(6) . . ? O101 C100 C101 119.7(6) . . ? C105 C100 C101 116.1(6) . . ? C102 C101 C100 122.5(6) . . ? C102 C101 Br11 118.8(5) . . ? C100 C101 Br11 118.7(5) . . ? C101 C102 C103 118.4(6) . . ? C101 C102 H102 120.8 . . ? C103 C102 H102 120.8 . . ? C104 C103 C102 122.7(6) . . ? C104 C103 Cl11 119.5(5) . . ? C102 C103 Cl11 117.8(5) . . ? C103 C104 C105 118.5(6) . . ? C103 C104 H104 120.7 . . ? C105 C104 H104 120.7 . . ? C104 C105 C100 121.9(6) . . ? C104 C105 C106 115.3(6) . . ? C100 C105 C106 122.4(6) . . ? N101 C106 C105 125.5(6) . . ? N101 C106 H106 117.3 . . ? C105 C106 H106 117.3 . . ? N101 C107 C108 106.5(5) . . ? N101 C107 H10A 110.4 . . ? C108 C107 H10A 110.4 . . ? N101 C107 H10B 110.4 . . ? C108 C107 H10B 110.4 . . ? H10A C107 H10B 108.6 . . ? N103 C108 C107 110.9(5) . . ? N103 C108 H10C 109.5 . . ? C107 C108 H10C 109.5 . . ? N103 C108 H10D 109.5 . . ? C107 C108 H10D 109.5 . . ? H10C C108 H10D 108.0 . . ? C110 C109 N103 105.6(5) . . ? C110 C109 H10E 110.6 . . ? N103 C109 H10E 110.6 . . ? C110 C109 H10F 110.6 . . ? N103 C109 H10F 110.6 . . ? H10E C109 H10F 108.7 . . ? N105 C110 C109 105.2(5) . . ? N105 C110 H11D 110.7 . . ? C109 C110 H11D 110.7 . . ? N105 C110 H11E 110.7 . . ? C109 C110 H11E 110.7 . . ? H11D C110 H11E 108.8 . . ? N105 C111 C112 110.7(5) . . ? N105 C111 H11F 109.5 . . ? C112 C111 H11F 109.5 . . ? N105 C111 H11G 109.5 . . ? C112 C111 H11G 109.5 . . ? H11F C111 H11G 108.1 . . ? N106 C112 C111 111.6(5) . . ? N106 C112 H11H 109.3 . . ? C111 C112 H11H 109.3 . . ? N106 C112 H11I 109.3 . . ? C111 C112 H11I 109.3 . . ? H11H C112 H11I 108.0 . . ? N106 C113 C114 105.1(5) . . ? N106 C113 H11J 110.7 . . ? C114 C113 H11J 110.7 . . ? N106 C113 H11K 110.7 . . ? C114 C113 H11K 110.7 . . ? H11J C113 H11K 108.8 . . ? N104 C114 C113 106.0(5) . . ? N104 C114 H11L 110.5 . . ? C113 C114 H11L 110.5 . . ? N104 C114 H11M 110.5 . . ? C113 C114 H11M 110.5 . . ? H11L C114 H11M 108.7 . . ? N104 C115 C116 111.6(5) . . ? N104 C115 H11N 109.3 . . ? C116 C115 H11N 109.3 . . ? N104 C115 H11O 109.3 . . ? C116 C115 H11O 109.3 . . ? H11N C115 H11O 108.0 . . ? N102 C116 C115 107.6(5) . . ? N102 C116 H11P 110.2 . . ? C115 C116 H11P 110.2 . . ? N102 C116 H11Q 110.2 . . ? C115 C116 H11Q 110.2 . . ? H11P C116 H11Q 108.5 . . ? N102 C117 C118 125.4(6) . . ? N102 C117 H117 117.3 . . ? C118 C117 H117 117.3 . . ? C119 C118 C123 121.4(7) . . ? C119 C118 C117 117.3(6) . . ? C123 C118 C117 121.3(6) . . ? C120 C119 C118 120.7(7) . . ? C120 C119 H119 119.7 . . ? C118 C119 H119 119.7 . . ? C119 C120 C121 120.8(7) . . ? C119 C120 Cl12 120.9(6) . . ? C121 C120 Cl12 118.3(6) . . ? C122 C121 C120 118.4(7) . . ? C122 C121 H121 120.8 . . ? C120 C121 H121 120.8 . . ? C121 C122 C123 124.6(7) . . ? C121 C122 Br2' 117.8(7) . . ? C123 C122 Br2' 117.0(7) . . ? C121 C122 Br12 118.2(6) . . ? C123 C122 Br12 117.2(6) . . ? O102 C123 C122 121.1(7) . . ? O102 C123 C118 124.7(7) . . ? C122 C123 C118 114.2(7) . . ? N105 C130 N103 103.0(5) . . ? N105 C130 C131 116.7(5) . . ? N103 C130 C131 112.5(5) . . ? N105 C130 H130 108.1 . . ? N103 C130 H130 108.1 . . ? C131 C130 H130 108.1 . . ? C132 C131 C136 121.4(6) . . ? C132 C131 C130 119.0(6) . . ? C136 C131 C130 119.3(6) . . ? C133 C132 C131 119.6(6) . . ? C133 C132 H132 120.2 . . ? C131 C132 H132 120.2 . . ? C134 C133 C132 121.0(6) . . ? C134 C133 Cl13 118.8(6) . . ? C132 C133 Cl13 120.3(6) . . ? C133 C134 C135 118.8(7) . . ? C133 C134 H134 120.6 . . ? C135 C134 H134 120.6 . . ? C134 C135 C136 123.7(6) . . ? C134 C135 Br13 119.8(5) . . ? C136 C135 Br13 116.4(5) . . ? O103 C136 C135 123.3(6) . . ? O103 C136 C131 121.3(6) . . ? C135 C136 C131 115.4(6) . . ? N106 C140 N104 101.8(5) . . ? N106 C140 C141 115.4(5) . . ? N104 C140 C141 114.8(5) . . ? N106 C140 H140 108.2 . . ? N104 C140 H140 108.2 . . ? C141 C140 H140 108.2 . . ? C142 C141 C146 121.3(6) . . ? C142 C141 C140 119.1(6) . . ? C146 C141 C140 119.6(5) . . ? C143 C142 C141 119.2(6) . . ? C143 C142 H142 120.4 . . ? C141 C142 H142 120.4 . . ? C142 C143 C144 121.7(6) . . ? C142 C143 Cl14 119.8(5) . . ? C144 C143 Cl14 118.5(5) . . ? C145 C144 C143 118.8(6) . . ? C145 C144 H144 120.6 . . ? C143 C144 H144 120.6 . . ? C144 C145 C146 123.0(6) . . ? C144 C145 Br14 120.0(5) . . ? C146 C145 Br14 117.0(5) . . ? O104 C146 C145 122.8(6) . . ? O104 C146 C141 121.2(5) . . ? C145 C146 C141 116.0(6) . . ? C1S O1S H1S 109.5 . . ? O1S C1S H1S1 109.5 . . ? O1S C1S H1S2 109.5 . . ? H1S1 C1S H1S2 109.5 . . ? O1S C1S H1S3 109.5 . . ? H1S1 C1S H1S3 109.5 . . ? H1S2 C1S H1S3 109.5 . . ? C2S O2S H2S 109.4 . . ? C3S O3S H3S 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O10 Ni11 O101 C100 -177.0(5) . . . . ? N101 Ni11 O101 C100 4.8(5) . . . . ? N103 Ni11 O101 C100 83.2(9) . . . . ? O103 Ni11 O101 C100 -99.6(5) . . . . ? N102 Cu13 O102 C123 14.2(6) . . . . ? O20 Cu13 O102 C123 -169.3(6) . . . . ? N104 Cu13 O102 C123 90.5(11) . . . . ? O104 Cu13 O102 C123 -92.2(6) . . . . ? O10 Ni12 O103 C136 126.6(5) . . . . ? O20 Ni12 O103 C136 -136.1(5) . . . . ? N105 Ni12 O103 C136 36.1(5) . . . . ? N106 Ni12 O103 C136 -46.8(5) . . . . ? O10 Ni12 O103 Ni11 13.92(15) . . . . ? O20 Ni12 O103 Ni11 111.24(16) . . . . ? N105 Ni12 O103 Ni11 -76.61(16) . . . . ? N106 Ni12 O103 Ni11 -159.52(16) . . . . ? O10 Ni11 O103 C136 -143.9(4) . . . . ? O101 Ni11 O103 C136 130.5(4) . . . . ? N101 Ni11 O103 C136 32.9(4) . . . . ? N103 Ni11 O103 C136 -50.3(4) . . . . ? O10 Ni11 O103 Ni12 -15.07(16) . . . . ? O101 Ni11 O103 Ni12 -100.74(18) . . . . ? N101 Ni11 O103 Ni12 161.70(19) . . . . ? N103 Ni11 O103 Ni12 78.51(18) . . . . ? O10 Ni12 O104 C146 -131.9(4) . . . . ? O20 Ni12 O104 C146 130.8(4) . . . . ? N105 Ni12 O104 C146 -41.3(5) . . . . ? N106 Ni12 O104 C146 41.3(4) . . . . ? O10 Ni12 O104 Cu13 112.99(16) . . . . ? O20 Ni12 O104 Cu13 15.66(15) . . . . ? N105 Ni12 O104 Cu13 -156.43(16) . . . . ? N106 Ni12 O104 Cu13 -73.81(17) . . . . ? O102 Cu13 O104 C146 128.1(4) . . . . ? N102 Cu13 O104 C146 32.3(4) . . . . ? O20 Cu13 O104 C146 -145.0(4) . . . . ? N104 Cu13 O104 C146 -52.4(4) . . . . ? O102 Cu13 O104 Ni12 -104.00(19) . . . . ? N102 Cu13 O104 Ni12 160.16(19) . . . . ? O20 Cu13 O104 Ni12 -17.17(16) . . . . ? N104 Cu13 O104 Ni12 75.42(19) . . . . ? O101 Ni11 N101 C106 -6.9(6) . . . . ? N103 Ni11 N101 C106 -171.6(6) . . . . ? O103 Ni11 N101 C106 103.1(5) . . . . ? O101 Ni11 N101 C107 171.3(5) . . . . ? N103 Ni11 N101 C107 6.6(5) . . . . ? O103 Ni11 N101 C107 -78.7(5) . . . . ? O102 Cu13 N102 C117 -12.2(6) . . . . ? N104 Cu13 N102 C117 179.8(6) . . . . ? O104 Cu13 N102 C117 91.3(5) . . . . ? O102 Cu13 N102 C116 171.1(5) . . . . ? N104 Cu13 N102 C116 3.1(4) . . . . ? O104 Cu13 N102 C116 -85.4(5) . . . . ? O10 Ni11 N103 C108 -159.7(4) . . . . ? O101 Ni11 N103 C108 -60.3(8) . . . . ? N101 Ni11 N103 C108 19.2(4) . . . . ? O103 Ni11 N103 C108 122.3(4) . . . . ? O10 Ni11 N103 C130 73.8(4) . . . . ? O101 Ni11 N103 C130 173.1(6) . . . . ? N101 Ni11 N103 C130 -107.3(4) . . . . ? O103 Ni11 N103 C130 -4.2(4) . . . . ? O10 Ni11 N103 C109 -40.3(4) . . . . ? O101 Ni11 N103 C109 59.1(8) . . . . ? N101 Ni11 N103 C109 138.6(4) . . . . ? O103 Ni11 N103 C109 -118.2(4) . . . . ? O102 Cu13 N104 C114 63.2(11) . . . . ? N102 Cu13 N104 C114 140.3(4) . . . . ? O20 Cu13 N104 C114 -36.7(4) . . . . ? O104 Cu13 N104 C114 -114.1(4) . . . . ? O102 Cu13 N104 C115 -57.0(11) . . . . ? N102 Cu13 N104 C115 20.0(4) . . . . ? O20 Cu13 N104 C115 -157.0(4) . . . . ? O104 Cu13 N104 C115 125.6(4) . . . . ? N102 Cu13 N104 C140 -103.3(4) . . . . ? O20 Cu13 N104 C140 79.7(4) . . . . ? O104 Cu13 N104 C140 2.3(4) . . . . ? O104 Ni12 N105 C130 -164.7(4) . . . . ? O10 Ni12 N105 C130 -73.1(4) . . . . ? O103 Ni12 N105 C130 10.1(4) . . . . ? N106 Ni12 N105 C130 109.8(4) . . . . ? O104 Ni12 N105 C111 71.6(4) . . . . ? O10 Ni12 N105 C111 163.2(4) . . . . ? O103 Ni12 N105 C111 -113.6(4) . . . . ? N106 Ni12 N105 C111 -13.9(4) . . . . ? O104 Ni12 N105 C110 -49.3(4) . . . . ? O10 Ni12 N105 C110 42.2(4) . . . . ? O103 Ni12 N105 C110 125.5(4) . . . . ? N106 Ni12 N105 C110 -134.9(4) . . . . ? O104 Ni12 N106 C112 -114.4(4) . . . . ? O103 Ni12 N106 C112 73.4(4) . . . . ? O20 Ni12 N106 C112 165.1(4) . . . . ? N105 Ni12 N106 C112 -13.5(4) . . . . ? O104 Ni12 N106 C140 8.9(4) . . . . ? O103 Ni12 N106 C140 -163.3(4) . . . . ? O20 Ni12 N106 C140 -71.7(4) . . . . ? N105 Ni12 N106 C140 109.8(4) . . . . ? O104 Ni12 N106 C113 125.4(4) . . . . ? O103 Ni12 N106 C113 -46.7(4) . . . . ? O20 Ni12 N106 C113 44.9(4) . . . . ? N105 Ni12 N106 C113 -133.7(4) . . . . ? O101 Ni11 O10 C10 -47.5(7) . . . . ? N103 Ni11 O10 C10 117.2(7) . . . . ? O103 Ni11 O10 C10 -156.7(7) . . . . ? O101 Ni11 O10 Ni12 124.8(2) . . . . ? N103 Ni11 O10 Ni12 -70.5(2) . . . . ? O103 Ni11 O10 Ni12 15.56(16) . . . . ? O104 Ni12 O10 C10 -18.9(9) . . . . ? O103 Ni12 O10 C10 152.6(9) . . . . ? O20 Ni12 O10 C10 61.7(9) . . . . ? N105 Ni12 O10 C10 -119.4(9) . . . . ? O104 Ni12 O10 Ni11 170.74(19) . . . . ? O103 Ni12 O10 Ni11 -17.73(19) . . . . ? O20 Ni12 O10 Ni11 -108.65(19) . . . . ? N105 Ni12 O10 Ni11 70.3(2) . . . . ? O102 Cu13 O20 C20 -56.5(5) . . . . ? N104 Cu13 O20 C20 111.4(4) . . . . ? O104 Cu13 O20 C20 -159.3(5) . . . . ? O102 Cu13 O20 Ni12 119.6(2) . . . . ? N104 Cu13 O20 Ni12 -72.5(2) . . . . ? O104 Cu13 O20 Ni12 16.81(16) . . . . ? O104 Ni12 O20 C20 155.2(7) . . . . ? O10 Ni12 O20 C20 65.0(7) . . . . ? O103 Ni12 O20 C20 -18.4(7) . . . . ? N106 Ni12 O20 C20 -117.8(7) . . . . ? O104 Ni12 O20 Cu13 -18.98(18) . . . . ? O10 Ni12 O20 Cu13 -109.22(19) . . . . ? O103 Ni12 O20 Cu13 167.34(19) . . . . ? N106 Ni12 O20 Cu13 68.0(2) . . . . ? Ni11 O10 C10 C11 145.0(9) . . . . ? Ni12 O10 C10 C11 -24.3(17) . . . . ? Ni11 O10 C10 O11 -46.1(10) . . . . ? Ni12 O10 C10 O11 144.7(6) . . . . ? Cu13 O20 C20 O21 -28.0(8) . . . . ? Ni12 O20 C20 O21 158.3(5) . . . . ? Cu13 O20 C20 C21 149.9(5) . . . . ? Ni12 O20 C20 C21 -23.9(11) . . . . ? Ni11 O101 C100 C105 0.4(9) . . . . ? Ni11 O101 C100 C101 -178.0(4) . . . . ? O101 C100 C101 C102 178.8(6) . . . . ? C105 C100 C101 C102 0.2(9) . . . . ? O101 C100 C101 Br11 -0.1(8) . . . . ? C105 C100 C101 Br11 -178.7(5) . . . . ? C100 C101 C102 C103 -0.4(10) . . . . ? Br11 C101 C102 C103 178.5(5) . . . . ? C101 C102 C103 C104 -0.1(10) . . . . ? C101 C102 C103 Cl11 -177.9(5) . . . . ? C102 C103 C104 C105 0.8(10) . . . . ? Cl11 C103 C104 C105 178.5(5) . . . . ? C103 C104 C105 C100 -1.0(10) . . . . ? C103 C104 C105 C106 -173.7(6) . . . . ? O101 C100 C105 C104 -178.0(6) . . . . ? C101 C100 C105 C104 0.5(9) . . . . ? O101 C100 C105 C106 -5.8(10) . . . . ? C101 C100 C105 C106 172.7(6) . . . . ? C107 N101 C106 C105 -174.2(6) . . . . ? Ni11 N101 C106 C105 4.0(9) . . . . ? C104 C105 C106 N101 176.2(6) . . . . ? C100 C105 C106 N101 3.5(10) . . . . ? C106 N101 C107 C108 148.0(6) . . . . ? Ni11 N101 C107 C108 -30.4(7) . . . . ? C130 N103 C108 C107 86.8(6) . . . . ? C109 N103 C108 C107 -159.9(5) . . . . ? Ni11 N103 C108 C107 -41.3(6) . . . . ? N101 C107 C108 N103 47.9(7) . . . . ? C108 N103 C109 C110 -149.8(5) . . . . ? C130 N103 C109 C110 -28.5(6) . . . . ? Ni11 N103 C109 C110 95.3(5) . . . . ? C130 N105 C110 C109 27.2(6) . . . . ? C111 N105 C110 C109 145.7(5) . . . . ? Ni12 N105 C110 C109 -96.5(5) . . . . ? N103 C109 C110 N105 0.9(6) . . . . ? C130 N105 C111 C112 -87.3(6) . . . . ? C110 N105 C111 C112 159.7(5) . . . . ? Ni12 N105 C111 C112 39.3(5) . . . . ? C140 N106 C112 C111 -88.0(6) . . . . ? C113 N106 C112 C111 159.3(5) . . . . ? Ni12 N106 C112 C111 39.3(6) . . . . ? N105 C111 C112 N106 -55.4(7) . . . . ? C112 N106 C113 C114 145.3(5) . . . . ? C140 N106 C113 C114 27.5(6) . . . . ? Ni12 N106 C113 C114 -97.9(5) . . . . ? C115 N104 C114 C113 -148.4(5) . . . . ? C140 N104 C114 C113 -28.1(6) . . . . ? Cu13 N104 C114 C113 94.8(5) . . . . ? N106 C113 C114 N104 0.4(6) . . . . ? C114 N104 C115 C116 -162.0(5) . . . . ? C140 N104 C115 C116 84.3(6) . . . . ? Cu13 N104 C115 C116 -39.6(6) . . . . ? C117 N102 C116 C115 157.6(6) . . . . ? Cu13 N102 C116 C115 -25.4(6) . . . . ? N104 C115 C116 N102 43.6(7) . . . . ? C116 N102 C117 C118 -177.6(6) . . . . ? Cu13 N102 C117 C118 5.9(10) . . . . ? N102 C117 C118 C119 -178.3(6) . . . . ? N102 C117 C118 C123 3.9(11) . . . . ? C123 C118 C119 C120 -0.7(11) . . . . ? C117 C118 C119 C120 -178.5(7) . . . . ? C118 C119 C120 C121 0.1(12) . . . . ? C118 C119 C120 Cl12 -177.9(5) . . . . ? C119 C120 C121 C122 0.6(12) . . . . ? Cl12 C120 C121 C122 178.8(6) . . . . ? C120 C121 C122 C123 -0.9(12) . . . . ? C120 C121 C122 Br2' 169.3(7) . . . . ? C120 C121 C122 Br12 -178.3(8) . . . . ? Cu13 O102 C123 C122 170.2(5) . . . . ? Cu13 O102 C123 C118 -9.4(11) . . . . ? C121 C122 C123 O102 -179.3(7) . . . . ? Br2' C122 C123 O102 10.4(10) . . . . ? Br12 C122 C123 O102 -1.9(11) . . . . ? C121 C122 C123 C118 0.3(11) . . . . ? Br2' C122 C123 C118 -169.9(6) . . . . ? Br12 C122 C123 C118 177.7(7) . . . . ? C119 C118 C123 O102 -179.9(7) . . . . ? C117 C118 C123 O102 -2.2(11) . . . . ? C119 C118 C123 C122 0.5(10) . . . . ? C117 C118 C123 C122 178.2(6) . . . . ? C111 N105 C130 N103 -165.1(5) . . . . ? C110 N105 C130 N103 -46.3(5) . . . . ? Ni12 N105 C130 N103 73.7(5) . . . . ? C111 N105 C130 C131 71.1(7) . . . . ? C110 N105 C130 C131 -170.1(5) . . . . ? Ni12 N105 C130 C131 -50.0(6) . . . . ? C108 N103 C130 N105 165.7(5) . . . . ? C109 N103 C130 N105 46.3(5) . . . . ? Ni11 N103 C130 N105 -72.9(5) . . . . ? C108 N103 C130 C131 -67.7(7) . . . . ? C109 N103 C130 C131 172.8(5) . . . . ? Ni11 N103 C130 C131 53.7(6) . . . . ? N105 C130 C131 C132 -130.5(6) . . . . ? N103 C130 C131 C132 110.7(6) . . . . ? N105 C130 C131 C136 55.2(8) . . . . ? N103 C130 C131 C136 -63.6(8) . . . . ? C136 C131 C132 C133 1.4(10) . . . . ? C130 C131 C132 C133 -172.8(6) . . . . ? C131 C132 C133 C134 0.0(10) . . . . ? C131 C132 C133 Cl13 179.9(5) . . . . ? C132 C133 C134 C135 0.1(10) . . . . ? Cl13 C133 C134 C135 -179.8(5) . . . . ? C133 C134 C135 C136 -1.7(10) . . . . ? C133 C134 C135 Br13 175.3(5) . . . . ? Ni12 O103 C136 C135 140.2(5) . . . . ? Ni11 O103 C136 C135 -115.6(6) . . . . ? Ni12 O103 C136 C131 -43.1(8) . . . . ? Ni11 O103 C136 C131 61.1(6) . . . . ? C134 C135 C136 O103 179.9(6) . . . . ? Br13 C135 C136 O103 2.8(8) . . . . ? C134 C135 C136 C131 3.0(9) . . . . ? Br13 C135 C136 C131 -174.1(4) . . . . ? C132 C131 C136 O103 -179.8(6) . . . . ? C130 C131 C136 O103 -5.6(9) . . . . ? C132 C131 C136 C135 -2.8(9) . . . . ? C130 C131 C136 C135 171.4(5) . . . . ? C112 N106 C140 N104 -163.5(5) . . . . ? C113 N106 C140 N104 -45.3(5) . . . . ? Ni12 N106 C140 N104 75.9(5) . . . . ? C112 N106 C140 C141 71.6(6) . . . . ? C113 N106 C140 C141 -170.2(5) . . . . ? Ni12 N106 C140 C141 -49.1(6) . . . . ? C114 N104 C140 N106 45.6(5) . . . . ? C115 N104 C140 N106 164.1(5) . . . . ? Cu13 N104 C140 N106 -77.2(5) . . . . ? C114 N104 C140 C141 170.9(5) . . . . ? C115 N104 C140 C141 -70.6(7) . . . . ? Cu13 N104 C140 C141 48.1(6) . . . . ? N106 C140 C141 C142 -131.5(6) . . . . ? N104 C140 C141 C142 110.6(6) . . . . ? N106 C140 C141 C146 50.9(8) . . . . ? N104 C140 C141 C146 -66.9(7) . . . . ? C146 C141 C142 C143 -1.0(9) . . . . ? C140 C141 C142 C143 -178.5(6) . . . . ? C141 C142 C143 C144 -0.4(10) . . . . ? C141 C142 C143 Cl14 176.9(5) . . . . ? C142 C143 C144 C145 0.0(10) . . . . ? Cl14 C143 C144 C145 -177.4(5) . . . . ? C143 C144 C145 C146 2.0(10) . . . . ? C143 C144 C145 Br14 -178.9(5) . . . . ? Ni12 O104 C146 C145 128.9(5) . . . . ? Cu13 O104 C146 C145 -122.8(5) . . . . ? Ni12 O104 C146 C141 -53.2(7) . . . . ? Cu13 O104 C146 C141 55.0(6) . . . . ? C144 C145 C146 O104 174.7(6) . . . . ? Br14 C145 C146 O104 -4.4(8) . . . . ? C144 C145 C146 C141 -3.2(9) . . . . ? Br14 C145 C146 C141 177.7(4) . . . . ? C142 C141 C146 O104 -175.2(5) . . . . ? C140 C141 C146 O104 2.3(9) . . . . ? C142 C141 C146 C145 2.7(9) . . . . ? C140 C141 C146 C145 -179.8(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 O1S H1S O3S 0.82 1.86 2.608(14) 150.9 . O1S H1S O3S' 0.82 2.09 2.879(13) 162.0 . O2S H2S O3S' 0.82 2.27 2.832(15) 125.9 . O2S H2S O21 0.82 2.62 3.145(10) 123.3 . O3S H3S O21 0.82 1.91 2.718(14) 169.6 . O3S' H3S' O1W 0.82 2.05 2.84(3) 164.4 . _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.899 _refine_diff_density_min -0.857 _refine_diff_density_rms 0.147 #END data_2.3.25H2O.0.5MeOH _database_code_depnum_ccdc_archive 'CCDC 825864' #TrackingRef '- cifs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C42 H40 Br4 Cl4 Cu2 N6 Ni O9), 0.5(C H4 O), 0.75(H2 O),1.5 O' _chemical_formula_sum 'C42.50 H43.50 Br4 Cl4 Cu2 N6 Ni O11.75' _chemical_formula_weight 1473.56 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' O O 0.0106 0.0060 '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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.9250(2) _cell_length_b 19.1020(5) _cell_length_c 33.3420(8) _cell_angle_alpha 90.00 _cell_angle_beta 98.0390(10) _cell_angle_gamma 90.00 _cell_volume 6259.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9045 _cell_measurement_theta_min 2.335 _cell_measurement_theta_max 25.145 _exptl_crystal_description green _exptl_crystal_colour needle _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.564 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2914 _exptl_absorpt_coefficient_mu 3.749 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6023 _exptl_absorpt_correction_T_max 0.7693 _exptl_absorpt_process_details 'SADABS, Bruker (2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 KappaAPEXII' _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 148281 _diffrn_reflns_av_R_equivalents 0.0537 _diffrn_reflns_av_sigmaI/netI 0.0312 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 26.37 _reflns_number_total 12796 _reflns_number_gt 10345 _reflns_threshold_expression >2\s(I) _computing_data_collection 'BRUKER APEX2' _computing_cell_refinement 'BRUKER APEX2' _computing_data_reduction ? _computing_structure_solution 'SIR-2004 (Burla, 2004)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0651P)^2^+66.3067P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12796 _refine_ls_number_parameters 662 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0847 _refine_ls_R_factor_gt 0.0662 _refine_ls_wR_factor_ref 0.1787 _refine_ls_wR_factor_gt 0.1716 _refine_ls_goodness_of_fit_ref 1.095 _refine_ls_restrained_S_all 1.095 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu11 Cu 0.34064(7) 0.03366(4) 0.36137(2) 0.02045(18) Uani 1 1 d . . . Ni12 Ni 0.37650(8) -0.12964(5) 0.35110(2) 0.02124(19) Uani 1 1 d . . . Cu13 Cu 0.57464(8) -0.22628(5) 0.30862(2) 0.0265(2) Uani 1 1 d . . . O101 O 0.4922(4) 0.0867(3) 0.34738(14) 0.0266(11) Uani 1 1 d . . . O102 O 0.6793(6) -0.1709(3) 0.27636(16) 0.0432(14) Uani 1 1 d . . . O103 O 0.4189(4) -0.0671(2) 0.40099(13) 0.0214(9) Uani 1 1 d . . . O104 O 0.3596(5) -0.1813(3) 0.29732(14) 0.0288(11) Uani 1 1 d . . . N101 N 0.3074(5) 0.1028(3) 0.40162(17) 0.0243(12) Uani 1 1 d . . . N102 N 0.5695(6) -0.3049(3) 0.27164(17) 0.0281(13) Uani 1 1 d . . . N103 N 0.1432(5) 0.0008(3) 0.36466(16) 0.0211(12) Uani 1 1 d . . . N105 N 0.1624(5) -0.1201(3) 0.35854(16) 0.0223(12) Uani 1 1 d . . . N104 N 0.5063(6) -0.2980(3) 0.34831(17) 0.0257(13) Uani 1 1 d . . . N106 N 0.3605(5) -0.2300(3) 0.38052(16) 0.0227(12) Uani 1 1 d . . . O10 O 0.3675(4) -0.0358(3) 0.32138(13) 0.0248(10) Uani 1 1 d . . . O20 O 0.5827(4) -0.1494(3) 0.34857(13) 0.0234(10) Uani 1 1 d . . . O11 O 0.2980(7) 0.0274(4) 0.2675(2) 0.0612(19) Uani 1 1 d . . . C10 C 0.3840(9) -0.0180(4) 0.2841(2) 0.0364(18) Uani 1 1 d . . . C11 C 0.4788(11) -0.0510(6) 0.2624(3) 0.062(3) Uani 1 1 d . . . H11A H 0.4485 -0.0989 0.2554 0.093 Uiso 1 1 calc R . . H11B H 0.5681 -0.0525 0.2792 0.093 Uiso 1 1 calc R . . H11C H 0.4857 -0.0247 0.2375 0.093 Uiso 1 1 calc R . . O21 O 0.8047(5) -0.1567(3) 0.3681(2) 0.0460(15) Uani 1 1 d . . . C20 C 0.6985(7) -0.1217(4) 0.3633(2) 0.0264(15) Uani 1 1 d . . . C21 C 0.7003(7) -0.0463(4) 0.3741(2) 0.0271(15) Uani 1 1 d . . . H21A H 0.7892 -0.0342 0.3891 0.041 Uiso 1 1 calc R . . H21B H 0.6290 -0.0369 0.3910 0.041 Uiso 1 1 calc R . . H21C H 0.6837 -0.0181 0.3494 0.041 Uiso 1 1 calc R . . C100 C 0.5573(6) 0.1369(4) 0.3675(2) 0.0261(15) Uani 1 1 d . . . C101 C 0.6813(7) 0.1617(4) 0.3562(2) 0.0306(16) Uani 1 1 d . . . Br11 Br 0.74313(7) 0.11985(5) 0.31078(2) 0.0352(2) Uani 1 1 d . . . C102 C 0.7558(7) 0.2145(4) 0.3761(3) 0.0374(18) Uani 1 1 d . . . H102 H 0.8380 0.2298 0.3674 0.045 Uiso 1 1 calc R . . C103 C 0.7102(8) 0.2453(5) 0.4092(3) 0.047(2) Uani 1 1 d . . . Cl11 Cl 0.8107(3) 0.31045(17) 0.43629(9) 0.0719(8) Uani 1 1 d . . . C104 C 0.5878(8) 0.2260(5) 0.4215(2) 0.0391(19) Uani 1 1 d . . . H104 H 0.5561 0.2492 0.4436 0.047 Uiso 1 1 calc R . . C105 C 0.5113(7) 0.1719(4) 0.4011(2) 0.0283(15) Uani 1 1 d . . . C106 C 0.3841(7) 0.1543(4) 0.4149(2) 0.0262(15) Uani 1 1 d . . . H106 H 0.3548 0.1830 0.4353 0.031 Uiso 1 1 calc R . . C107 C 0.1762(6) 0.0934(4) 0.4166(2) 0.0247(14) Uani 1 1 d . . . H10A H 0.1412 0.1390 0.4247 0.030 Uiso 1 1 calc R . . H10B H 0.1870 0.0620 0.4405 0.030 Uiso 1 1 calc R . . C108 C 0.0792(6) 0.0617(4) 0.3826(2) 0.0246(14) Uani 1 1 d . . . H10C H -0.0046 0.0462 0.3930 0.030 Uiso 1 1 calc R . . H10D H 0.0535 0.0974 0.3614 0.030 Uiso 1 1 calc R . . C109 C 0.0659(6) -0.0173(4) 0.3239(2) 0.0264(15) Uani 1 1 d . . . H10E H 0.1048 0.0074 0.3021 0.032 Uiso 1 1 calc R . . H10F H -0.0311 -0.0041 0.3226 0.032 Uiso 1 1 calc R . . C110 C 0.0804(6) -0.0960(4) 0.31977(19) 0.0253(15) Uani 1 1 d . . . H11D H -0.0100 -0.1188 0.3158 0.030 Uiso 1 1 calc R . . H11E H 0.1278 -0.1074 0.2964 0.030 Uiso 1 1 calc R . . C111 C 0.1200(7) -0.1901(4) 0.3716(2) 0.0289(16) Uani 1 1 d . . . H11F H 0.0926 -0.2195 0.3473 0.035 Uiso 1 1 calc R . . H11G H 0.0399 -0.1847 0.3860 0.035 Uiso 1 1 calc R . . C112 C 0.2326(6) -0.2266(4) 0.3990(2) 0.0266(15) Uani 1 1 d . . . H11H H 0.2501 -0.2011 0.4251 0.032 Uiso 1 1 calc R . . H11I H 0.2031 -0.2746 0.4047 0.032 Uiso 1 1 calc R . . C113 C 0.4813(7) -0.2434(4) 0.41201(19) 0.0234(14) Uani 1 1 d . . . H11J H 0.4534 -0.2674 0.4358 0.028 Uiso 1 1 calc R . . H11K H 0.5273 -0.1990 0.4210 0.028 Uiso 1 1 calc R . . C114 C 0.5751(7) -0.2900(4) 0.3911(2) 0.0274(15) Uani 1 1 d . . . H11L H 0.6656 -0.2679 0.3916 0.033 Uiso 1 1 calc R . . H11M H 0.5870 -0.3362 0.4046 0.033 Uiso 1 1 calc R . . C115 C 0.5404(7) -0.3681(4) 0.3318(2) 0.0296(16) Uani 1 1 d . . . H11N H 0.6382 -0.3783 0.3399 0.035 Uiso 1 1 calc R . . H11O H 0.4869 -0.4051 0.3431 0.035 Uiso 1 1 calc R . . C116 C 0.5086(8) -0.3680(4) 0.2864(2) 0.0328(17) Uani 1 1 d . . . H11P H 0.5470 -0.4103 0.2750 0.039 Uiso 1 1 calc R . . H11Q H 0.4089 -0.3679 0.2780 0.039 Uiso 1 1 calc R . . C117 C 0.6185(7) -0.3069(4) 0.2380(2) 0.0292(16) Uani 1 1 d . . . H117 H 0.6099 -0.3497 0.2234 0.035 Uiso 1 1 calc R . . C118 C 0.6853(7) -0.2499(4) 0.2204(2) 0.0297(16) Uani 1 1 d . . . C119 C 0.7305(7) -0.2622(4) 0.1830(2) 0.0296(16) Uani 1 1 d . . . H119 H 0.7137 -0.3063 0.1700 0.036 Uiso 1 1 calc R . . C120 C 0.7985(7) -0.2115(5) 0.1651(2) 0.0364(19) Uani 1 1 d . . . Cl12 Cl 0.8598(2) -0.22687(13) 0.11903(6) 0.0480(5) Uani 1 1 d . . . C121 C 0.8226(8) -0.1467(5) 0.1829(2) 0.0385(19) Uani 1 1 d . A . H121 H 0.8687 -0.1114 0.1701 0.046 Uiso 1 1 calc R . . C122 C 0.7790(8) -0.1337(5) 0.2195(2) 0.040(2) Uani 1 1 d . . . Br12 Br 0.8269(6) -0.0491(2) 0.24328(5) 0.0243(9) Uani 0.66(2) 1 d P A 1 Br2' Br 0.7742(18) -0.0299(7) 0.24084(16) 0.043(2) Uani 0.34(2) 1 d P A 2 C123 C 0.7105(7) -0.1848(5) 0.2409(2) 0.0335(17) Uani 1 1 d . A . C124 C 0.1288(6) -0.0653(4) 0.38741(19) 0.0230(14) Uani 1 1 d . . . H124 H 0.0306 -0.0706 0.3905 0.028 Uiso 1 1 calc R . . C125 C 0.2103(6) -0.0708(4) 0.4288(2) 0.0224(14) Uani 1 1 d . . . C126 C 0.1420(7) -0.0763(3) 0.4624(2) 0.0225(13) Uani 1 1 d . . . H126 H 0.0454 -0.0741 0.4590 0.027 Uiso 1 1 calc R . . C127 C 0.2138(7) -0.0849(4) 0.5006(2) 0.0278(15) Uani 1 1 d . . . Cl13 Cl 0.1285(2) -0.09002(12) 0.54260(5) 0.0402(5) Uani 1 1 d . . . C128 C 0.3542(7) -0.0879(4) 0.5057(2) 0.0285(15) Uani 1 1 d . . . H128 H 0.4042 -0.0936 0.5319 0.034 Uiso 1 1 calc R . . C129 C 0.4212(6) -0.0826(4) 0.4723(2) 0.0231(14) Uani 1 1 d . . . Br13 Br 0.61429(7) -0.09007(4) 0.47938(2) 0.02903(17) Uani 1 1 d . . . C130 C 0.3529(6) -0.0727(3) 0.43269(19) 0.0197(13) Uani 1 1 d . . . C131 C 0.3602(6) -0.2930(4) 0.3538(2) 0.0265(15) Uani 1 1 d . . . H131 H 0.3364 -0.3349 0.3694 0.032 Uiso 1 1 calc R . . C132 C 0.2604(7) -0.2881(4) 0.3151(2) 0.0275(15) Uani 1 1 d . . . C133 C 0.1599(7) -0.3387(4) 0.3077(2) 0.0322(17) Uani 1 1 d . . . H133 H 0.1566 -0.3768 0.3258 0.039 Uiso 1 1 calc R . . C134 C 0.0647(7) -0.3327(5) 0.2735(3) 0.042(2) Uani 1 1 d . . . Cl14 Cl -0.0659(2) -0.39402(12) 0.26341(8) 0.0538(7) Uani 1 1 d . . . C135 C 0.0697(8) -0.2785(5) 0.2462(2) 0.041(2) Uani 1 1 d . . . H135 H 0.0038 -0.2750 0.2227 0.049 Uiso 1 1 calc R . . C136 C 0.1719(7) -0.2299(5) 0.2537(2) 0.0352(18) Uani 1 1 d . . . Br14 Br 0.18564(9) -0.15653(6) 0.21580(2) 0.0467(2) Uani 1 1 d . . . C137 C 0.2685(7) -0.2309(4) 0.2891(2) 0.0316(17) Uani 1 1 d . . . O1W O 0.8411(7) -0.2858(4) 0.3399(2) 0.063(2) Uani 1 1 d . . . H1W1 H 0.8286 -0.2371 0.3536 0.076 Uiso 1 1 d . . . H1W2 H 0.8550 -0.2995 0.3100 0.076 Uiso 1 1 d . . . O2W O 0.2455(10) 0.0018(5) 0.1812(3) 0.067(3) Uiso 0.75 1 d P . . H2W1 H 0.3112 -0.0129 0.1687 0.080 Uiso 0.75 1 d P . . H2W2 H 0.2612 0.0095 0.2074 0.080 Uiso 0.75 1 d P . . O1S O 0.4484(15) -0.0453(8) 0.1407(4) 0.063(4) Uiso 0.50 1 d P . . H1S H 0.5207 -0.0277 0.1349 0.094 Uiso 0.50 1 calc PR . . C1S C 0.4651(16) -0.1134(8) 0.1464(5) 0.032(3) Uiso 0.50 1 d P . . H1S1 H 0.4956 -0.1227 0.1751 0.048 Uiso 0.50 1 calc PR . . H1S2 H 0.5336 -0.1305 0.1302 0.048 Uiso 0.50 1 calc PR . . H1S3 H 0.3786 -0.1375 0.1380 0.048 Uiso 0.50 1 calc PR . . O3W O 0.951(2) -0.3641(13) 0.4035(7) 0.044(6) Uiso 0.25 1 d P . . O4W O 0.613(2) 0.0944(12) 0.0527(7) 0.041(5) Uiso 0.25 1 d P . . O5W O 0.713(3) 0.0159(16) 0.1200(9) 0.065(8) Uiso 0.25 1 d P . . O6W O 0.984(3) 0.0010(17) 0.1285(10) 0.073(8) Uiso 0.25 1 d P . . O7W O 0.382(4) 0.0137(19) 0.0645(11) 0.081(9) Uiso 0.25 1 d P . . O8W O 0.907(2) -0.2339(10) 0.4726(6) 0.029(4) Uiso 0.25 1 d P . . 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 Cu11 0.0136(4) 0.0305(4) 0.0182(4) 0.0026(3) 0.0059(3) 0.0060(3) Ni12 0.0138(4) 0.0351(5) 0.0148(4) -0.0004(3) 0.0021(3) 0.0017(3) Cu13 0.0226(4) 0.0370(5) 0.0209(4) -0.0088(4) 0.0068(3) -0.0039(4) O101 0.018(2) 0.040(3) 0.024(2) 0.006(2) 0.0084(19) 0.006(2) O102 0.051(3) 0.052(4) 0.030(3) -0.017(3) 0.020(3) -0.022(3) O103 0.015(2) 0.033(3) 0.016(2) 0.0015(19) 0.0040(17) 0.0023(19) O104 0.022(2) 0.046(3) 0.018(2) -0.008(2) 0.0018(19) 0.000(2) N101 0.016(3) 0.037(3) 0.022(3) 0.003(2) 0.006(2) 0.002(2) N102 0.020(3) 0.041(4) 0.023(3) -0.005(3) 0.005(2) -0.002(3) N103 0.012(2) 0.035(3) 0.016(3) -0.002(2) 0.003(2) 0.008(2) N105 0.016(3) 0.031(3) 0.019(3) -0.001(2) 0.000(2) 0.001(2) N104 0.018(3) 0.036(3) 0.023(3) -0.009(2) 0.004(2) 0.001(2) N106 0.012(2) 0.035(3) 0.020(3) -0.006(2) 0.001(2) 0.002(2) O10 0.019(2) 0.036(3) 0.019(2) 0.004(2) 0.0020(18) 0.003(2) O20 0.016(2) 0.036(3) 0.018(2) -0.005(2) 0.0032(17) 0.0023(19) O11 0.049(4) 0.078(5) 0.058(4) 0.025(4) 0.013(3) 0.019(4) C10 0.054(5) 0.035(4) 0.024(4) 0.005(3) 0.016(3) 0.010(4) C11 0.062(6) 0.075(7) 0.050(6) 0.014(5) 0.012(5) 0.021(6) O21 0.016(2) 0.049(4) 0.070(4) -0.022(3) -0.003(3) 0.006(2) C20 0.018(3) 0.039(4) 0.022(3) -0.001(3) 0.004(3) 0.000(3) C21 0.018(3) 0.030(4) 0.033(4) 0.000(3) 0.005(3) -0.001(3) C100 0.016(3) 0.037(4) 0.025(3) 0.009(3) 0.002(3) 0.006(3) C101 0.022(3) 0.044(4) 0.026(4) 0.010(3) 0.005(3) 0.006(3) Br11 0.0209(3) 0.0549(5) 0.0322(4) 0.0148(3) 0.0118(3) 0.0066(3) C102 0.019(3) 0.047(5) 0.047(5) 0.011(4) 0.007(3) -0.002(3) C103 0.030(4) 0.057(6) 0.054(5) -0.006(4) 0.006(4) -0.017(4) Cl11 0.0517(14) 0.084(2) 0.0845(19) -0.0262(16) 0.0238(14) -0.0353(14) C104 0.032(4) 0.052(5) 0.035(4) -0.003(4) 0.010(3) -0.004(4) C105 0.019(3) 0.038(4) 0.028(4) 0.005(3) 0.003(3) 0.005(3) C106 0.024(3) 0.034(4) 0.021(3) 0.005(3) 0.006(3) 0.006(3) C107 0.019(3) 0.032(4) 0.025(3) -0.003(3) 0.010(3) 0.008(3) C108 0.017(3) 0.034(4) 0.024(3) 0.003(3) 0.006(3) 0.007(3) C109 0.016(3) 0.045(4) 0.018(3) -0.004(3) -0.001(2) 0.011(3) C110 0.016(3) 0.042(4) 0.017(3) -0.002(3) -0.002(2) 0.003(3) C111 0.017(3) 0.042(4) 0.030(4) -0.007(3) 0.007(3) -0.002(3) C112 0.017(3) 0.036(4) 0.029(4) 0.001(3) 0.009(3) 0.003(3) C113 0.021(3) 0.030(4) 0.018(3) -0.002(3) 0.001(3) -0.001(3) C114 0.017(3) 0.043(4) 0.022(3) -0.004(3) 0.002(3) 0.004(3) C115 0.026(4) 0.035(4) 0.028(4) -0.007(3) 0.007(3) 0.002(3) C116 0.028(4) 0.039(4) 0.034(4) -0.010(3) 0.011(3) 0.000(3) C117 0.019(3) 0.043(4) 0.024(3) -0.013(3) 0.001(3) -0.002(3) C118 0.020(3) 0.046(4) 0.023(3) -0.010(3) 0.001(3) -0.006(3) C119 0.019(3) 0.049(5) 0.021(3) -0.010(3) 0.001(3) -0.002(3) C120 0.021(3) 0.070(6) 0.019(3) -0.011(4) 0.006(3) -0.007(4) Cl12 0.0478(12) 0.0702(15) 0.0301(10) -0.0129(10) 0.0205(9) -0.0158(11) C121 0.027(4) 0.063(6) 0.025(4) -0.004(4) 0.002(3) -0.017(4) C122 0.037(4) 0.055(5) 0.028(4) -0.011(4) 0.003(3) -0.022(4) Br12 0.0217(16) 0.0253(11) 0.0248(6) -0.0054(5) 0.0002(6) 0.0000(9) Br2' 0.042(5) 0.049(3) 0.0379(15) -0.0101(17) 0.0082(19) -0.009(4) C123 0.025(4) 0.053(5) 0.023(4) -0.010(3) 0.004(3) -0.009(3) C124 0.012(3) 0.036(4) 0.022(3) 0.001(3) 0.006(2) 0.003(3) C125 0.019(3) 0.025(3) 0.024(3) 0.002(3) 0.006(3) -0.001(3) C126 0.020(3) 0.025(3) 0.024(3) -0.002(3) 0.007(3) 0.002(3) C127 0.033(4) 0.033(4) 0.020(3) -0.001(3) 0.012(3) 0.000(3) Cl13 0.0391(10) 0.0646(13) 0.0205(8) 0.0021(8) 0.0169(7) 0.0071(9) C128 0.035(4) 0.037(4) 0.013(3) -0.002(3) 0.001(3) 0.005(3) C129 0.016(3) 0.029(4) 0.023(3) -0.001(3) -0.001(3) 0.003(3) Br13 0.0211(3) 0.0417(4) 0.0222(3) -0.0035(3) -0.0042(3) 0.0055(3) C130 0.018(3) 0.023(3) 0.018(3) -0.002(3) 0.003(2) 0.002(3) C131 0.015(3) 0.038(4) 0.026(3) -0.014(3) 0.005(3) 0.001(3) C132 0.018(3) 0.041(4) 0.023(3) -0.014(3) 0.002(3) 0.002(3) C133 0.023(3) 0.041(4) 0.033(4) -0.020(3) 0.003(3) 0.003(3) C134 0.021(4) 0.060(6) 0.044(5) -0.036(4) -0.001(3) 0.000(4) Cl14 0.0244(9) 0.0547(13) 0.0766(16) -0.0431(12) -0.0128(10) 0.0023(9) C135 0.027(4) 0.064(6) 0.030(4) -0.023(4) -0.004(3) 0.012(4) C136 0.027(4) 0.050(5) 0.028(4) -0.010(3) 0.002(3) 0.009(3) Br14 0.0374(4) 0.0802(7) 0.0208(4) -0.0039(4) -0.0022(3) 0.0140(4) C137 0.021(3) 0.053(5) 0.021(3) -0.015(3) 0.003(3) 0.006(3) O1W 0.046(4) 0.068(5) 0.078(5) -0.030(4) 0.016(3) -0.009(3) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Cu11 O101 1.924(5) . ? Cu11 O10 1.925(5) . ? Cu11 N101 1.944(6) . ? Cu11 N103 2.076(5) . ? Cu11 O103 2.401(5) . ? Ni12 O104 2.033(5) . ? Ni12 O103 2.044(5) . ? Ni12 O10 2.044(5) . ? Ni12 O20 2.094(4) . ? Ni12 N106 2.169(6) . ? Ni12 N105 2.181(5) . ? Cu13 O102 1.916(5) . ? Cu13 N102 1.939(6) . ? Cu13 O20 1.977(5) . ? Cu13 N104 2.083(6) . ? Cu13 O104 2.282(5) . ? O101 C100 1.291(9) . ? O102 C123 1.291(9) . ? O103 C130 1.324(7) . ? O104 C137 1.313(9) . ? N101 C106 1.283(9) . ? N101 C107 1.470(8) . ? N102 C117 1.285(9) . ? N102 C116 1.465(10) . ? N103 C124 1.489(9) . ? N103 C108 1.489(9) . ? N103 C109 1.503(8) . ? N105 C111 1.485(9) . ? N105 C124 1.491(9) . ? N105 C110 1.500(8) . ? N104 C131 1.489(8) . ? N104 C114 1.500(8) . ? N104 C115 1.504(9) . ? N106 C112 1.489(8) . ? N106 C131 1.497(9) . ? N106 C113 1.502(8) . ? O10 C10 1.322(8) . ? O20 C20 1.297(8) . ? O11 C10 1.285(10) . ? C10 C11 1.414(12) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? O21 C20 1.239(9) . ? C20 C21 1.484(10) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C100 C101 1.419(10) . ? C100 C105 1.431(10) . ? C101 C102 1.367(11) . ? C101 Br11 1.889(8) . ? C102 C103 1.381(12) . ? C102 H102 0.9500 . ? C103 C104 1.386(11) . ? C103 Cl11 1.762(9) . ? C104 C105 1.400(11) . ? C104 H104 0.9500 . ? C105 C106 1.443(10) . ? C106 H106 0.9500 . ? C107 C108 1.510(9) . ? C107 H10A 0.9900 . ? C107 H10B 0.9900 . ? C108 H10C 0.9900 . ? C108 H10D 0.9900 . ? C109 C110 1.518(10) . ? C109 H10E 0.9900 . ? C109 H10F 0.9900 . ? C110 H11D 0.9900 . ? C110 H11E 0.9900 . ? C111 C112 1.512(10) . ? C111 H11F 0.9900 . ? C111 H11G 0.9900 . ? C112 H11H 0.9900 . ? C112 H11I 0.9900 . ? C113 C114 1.526(9) . ? C113 H11J 0.9900 . ? C113 H11K 0.9900 . ? C114 H11L 0.9900 . ? C114 H11M 0.9900 . ? C115 C116 1.503(10) . ? C115 H11N 0.9900 . ? C115 H11O 0.9900 . ? C116 H11P 0.9900 . ? C116 H11Q 0.9900 . ? C117 C118 1.441(11) . ? C117 H117 0.9500 . ? C118 C119 1.403(10) . ? C118 C123 1.425(11) . ? C119 C120 1.365(11) . ? C119 H119 0.9500 . ? C120 C121 1.380(12) . ? C120 Cl12 1.755(7) . ? C121 C122 1.371(11) . ? C121 H121 0.9500 . ? C122 C123 1.435(11) . ? C122 Br12 1.835(9) . ? C122 Br2' 2.111(16) . ? C124 C125 1.501(9) . ? C124 H124 1.0000 . ? C125 C126 1.392(9) . ? C125 C130 1.404(9) . ? C126 C127 1.382(10) . ? C126 H126 0.9500 . ? C127 C128 1.381(10) . ? C127 Cl13 1.737(7) . ? C128 C129 1.376(10) . ? C128 H128 0.9500 . ? C129 C130 1.411(9) . ? C129 Br13 1.903(6) . ? C131 C132 1.518(9) . ? C131 H131 1.0000 . ? C132 C133 1.386(10) . ? C132 C137 1.402(11) . ? C133 C134 1.379(11) . ? C133 H133 0.9500 . ? C134 C135 1.384(13) . ? C134 Cl14 1.744(8) . ? C135 C136 1.372(12) . ? C135 H135 0.9500 . ? C136 C137 1.412(10) . ? C136 Br14 1.905(9) . ? O1W H1W1 1.0513 . ? O1W H1W2 1.0579 . ? O2W H2W1 0.8690 . ? O2W H2W2 0.8765 . ? O1S C1S 1.32(2) . ? O1S H1S 0.8400 . ? C1S H1S1 0.9800 . ? C1S H1S2 0.9800 . ? C1S H1S3 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O101 Cu11 O10 90.4(2) . . ? O101 Cu11 N101 91.3(2) . . ? O10 Cu11 N101 178.1(2) . . ? O101 Cu11 N103 161.5(2) . . ? O10 Cu11 N103 92.9(2) . . ? N101 Cu11 N103 85.2(2) . . ? O101 Cu11 O103 110.58(17) . . ? O10 Cu11 O103 76.32(17) . . ? N101 Cu11 O103 103.8(2) . . ? N103 Cu11 O103 87.91(19) . . ? O104 Ni12 O103 169.71(19) . . ? O104 Ni12 O10 90.3(2) . . ? O103 Ni12 O10 82.63(18) . . ? O104 Ni12 O20 80.65(18) . . ? O103 Ni12 O20 92.69(17) . . ? O10 Ni12 O20 96.62(19) . . ? O104 Ni12 N106 88.2(2) . . ? O103 Ni12 N106 99.69(19) . . ? O10 Ni12 N106 173.28(19) . . ? O20 Ni12 N106 89.59(19) . . ? O104 Ni12 N105 100.3(2) . . ? O103 Ni12 N105 87.21(19) . . ? O10 Ni12 N105 90.3(2) . . ? O20 Ni12 N105 173.1(2) . . ? N106 Ni12 N105 83.6(2) . . ? O102 Cu13 N102 92.2(2) . . ? O102 Cu13 O20 89.6(2) . . ? N102 Cu13 O20 177.2(2) . . ? O102 Cu13 N104 166.1(3) . . ? N102 Cu13 N104 85.0(2) . . ? O20 Cu13 N104 92.7(2) . . ? O102 Cu13 O104 105.5(2) . . ? N102 Cu13 O104 104.2(2) . . ? O20 Cu13 O104 77.31(17) . . ? N104 Cu13 O104 88.4(2) . . ? C100 O101 Cu11 128.0(4) . . ? C123 O102 Cu13 128.2(5) . . ? C130 O103 Ni12 122.2(4) . . ? C130 O103 Cu11 110.3(4) . . ? Ni12 O103 Cu11 90.39(16) . . ? C137 O104 Ni12 120.3(4) . . ? C137 O104 Cu13 111.3(4) . . ? Ni12 O104 Cu13 94.44(18) . . ? C106 N101 C107 119.2(6) . . ? C106 N101 Cu11 127.5(5) . . ? C107 N101 Cu11 113.3(4) . . ? C117 N102 C116 119.5(6) . . ? C117 N102 Cu13 126.8(5) . . ? C116 N102 Cu13 113.6(4) . . ? C124 N103 C108 112.4(5) . . ? C124 N103 C109 101.1(5) . . ? C108 N103 C109 110.5(5) . . ? C124 N103 Cu11 116.2(4) . . ? C108 N103 Cu11 104.1(4) . . ? C109 N103 Cu11 112.8(4) . . ? C111 N105 C124 110.2(5) . . ? C111 N105 C110 112.7(5) . . ? C124 N105 C110 101.4(5) . . ? C111 N105 Ni12 106.2(4) . . ? C124 N105 Ni12 116.2(4) . . ? C110 N105 Ni12 110.3(4) . . ? C131 N104 C114 101.4(5) . . ? C131 N104 C115 112.0(5) . . ? C114 N104 C115 110.0(5) . . ? C131 N104 Cu13 116.4(5) . . ? C114 N104 Cu13 113.0(4) . . ? C115 N104 Cu13 104.0(4) . . ? C112 N106 C131 110.6(5) . . ? C112 N106 C113 111.2(5) . . ? C131 N106 C113 102.3(5) . . ? C112 N106 Ni12 105.7(4) . . ? C131 N106 Ni12 115.9(4) . . ? C113 N106 Ni12 111.4(4) . . ? C10 O10 Cu11 121.4(5) . . ? C10 O10 Ni12 132.8(5) . . ? Cu11 O10 Ni12 105.6(2) . . ? C20 O20 Cu13 120.5(4) . . ? C20 O20 Ni12 136.9(4) . . ? Cu13 O20 Ni12 102.3(2) . . ? O11 C10 O10 114.6(7) . . ? O11 C10 C11 122.0(7) . . ? O10 C10 C11 123.0(7) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? O21 C20 O20 121.4(7) . . ? O21 C20 C21 120.7(6) . . ? O20 C20 C21 117.8(6) . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? O101 C100 C101 119.9(6) . . ? O101 C100 C105 124.3(6) . . ? C101 C100 C105 115.8(7) . . ? C102 C101 C100 123.1(7) . . ? C102 C101 Br11 119.2(6) . . ? C100 C101 Br11 117.7(6) . . ? C101 C102 C103 119.2(7) . . ? C101 C102 H102 120.4 . . ? C103 C102 H102 120.4 . . ? C102 C103 C104 121.4(8) . . ? C102 C103 Cl11 119.0(6) . . ? C104 C103 Cl11 119.5(7) . . ? C103 C104 C105 119.4(8) . . ? C103 C104 H104 120.3 . . ? C105 C104 H104 120.3 . . ? C104 C105 C100 120.9(7) . . ? C104 C105 C106 117.2(7) . . ? C100 C105 C106 121.9(7) . . ? N101 C106 C105 124.9(7) . . ? N101 C106 H106 117.5 . . ? C105 C106 H106 117.5 . . ? N101 C107 C108 107.2(5) . . ? N101 C107 H10A 110.3 . . ? C108 C107 H10A 110.3 . . ? N101 C107 H10B 110.3 . . ? C108 C107 H10B 110.3 . . ? H10A C107 H10B 108.5 . . ? N103 C108 C107 110.6(5) . . ? N103 C108 H10C 109.5 . . ? C107 C108 H10C 109.5 . . ? N103 C108 H10D 109.5 . . ? C107 C108 H10D 109.5 . . ? H10C C108 H10D 108.1 . . ? N103 C109 C110 105.5(5) . . ? N103 C109 H10E 110.6 . . ? C110 C109 H10E 110.6 . . ? N103 C109 H10F 110.6 . . ? C110 C109 H10F 110.6 . . ? H10E C109 H10F 108.8 . . ? N105 C110 C109 105.8(5) . . ? N105 C110 H11D 110.6 . . ? C109 C110 H11D 110.6 . . ? N105 C110 H11E 110.6 . . ? C109 C110 H11E 110.6 . . ? H11D C110 H11E 108.7 . . ? N105 C111 C112 112.1(6) . . ? N105 C111 H11F 109.2 . . ? C112 C111 H11F 109.2 . . ? N105 C111 H11G 109.2 . . ? C112 C111 H11G 109.2 . . ? H11F C111 H11G 107.9 . . ? N106 C112 C111 111.7(6) . . ? N106 C112 H11H 109.3 . . ? C111 C112 H11H 109.3 . . ? N106 C112 H11I 109.3 . . ? C111 C112 H11I 109.3 . . ? H11H C112 H11I 107.9 . . ? N106 C113 C114 105.0(5) . . ? N106 C113 H11J 110.7 . . ? C114 C113 H11J 110.7 . . ? N106 C113 H11K 110.7 . . ? C114 C113 H11K 110.7 . . ? H11J C113 H11K 108.8 . . ? N104 C114 C113 105.6(5) . . ? N104 C114 H11L 110.6 . . ? C113 C114 H11L 110.6 . . ? N104 C114 H11M 110.6 . . ? C113 C114 H11M 110.6 . . ? H11L C114 H11M 108.8 . . ? C116 C115 N104 110.0(6) . . ? C116 C115 H11N 109.7 . . ? N104 C115 H11N 109.7 . . ? C116 C115 H11O 109.7 . . ? N104 C115 H11O 109.7 . . ? H11N C115 H11O 108.2 . . ? N102 C116 C115 107.5(6) . . ? N102 C116 H11P 110.2 . . ? C115 C116 H11P 110.2 . . ? N102 C116 H11Q 110.2 . . ? C115 C116 H11Q 110.2 . . ? H11P C116 H11Q 108.5 . . ? N102 C117 C118 125.8(7) . . ? N102 C117 H117 117.1 . . ? C118 C117 H117 117.1 . . ? C119 C118 C123 121.2(7) . . ? C119 C118 C117 117.2(7) . . ? C123 C118 C117 121.6(6) . . ? C120 C119 C118 120.5(7) . . ? C120 C119 H119 119.7 . . ? C118 C119 H119 119.7 . . ? C119 C120 C121 121.0(7) . . ? C119 C120 Cl12 121.1(6) . . ? C121 C120 Cl12 117.9(6) . . ? C122 C121 C120 119.2(8) . . ? C122 C121 H121 120.4 . . ? C120 C121 H121 120.4 . . ? C121 C122 C123 123.4(8) . . ? C121 C122 Br12 116.6(6) . . ? C123 C122 Br12 119.7(6) . . ? C121 C122 Br2' 119.6(7) . . ? C123 C122 Br2' 115.8(6) . . ? Br12 C122 Br2' 16.7(3) . . ? O102 C123 C118 124.8(7) . . ? O102 C123 C122 120.5(7) . . ? C118 C123 C122 114.7(6) . . ? N103 C124 N105 102.7(5) . . ? N103 C124 C125 116.8(6) . . ? N105 C124 C125 113.7(5) . . ? N103 C124 H124 107.7 . . ? N105 C124 H124 107.7 . . ? C125 C124 H124 107.7 . . ? C126 C125 C130 121.4(6) . . ? C126 C125 C124 119.0(6) . . ? C130 C125 C124 119.6(6) . . ? C127 C126 C125 120.4(6) . . ? C127 C126 H126 119.8 . . ? C125 C126 H126 119.8 . . ? C128 C127 C126 119.9(6) . . ? C128 C127 Cl13 119.8(5) . . ? C126 C127 Cl13 120.3(5) . . ? C129 C128 C127 119.5(6) . . ? C129 C128 H128 120.3 . . ? C127 C128 H128 120.3 . . ? C128 C129 C130 122.9(6) . . ? C128 C129 Br13 119.1(5) . . ? C130 C129 Br13 118.0(5) . . ? O103 C130 C125 121.9(6) . . ? O103 C130 C129 122.2(6) . . ? C125 C130 C129 115.9(6) . . ? N104 C131 N106 101.8(5) . . ? N104 C131 C132 115.4(6) . . ? N106 C131 C132 113.7(6) . . ? N104 C131 H131 108.5 . . ? N106 C131 H131 108.5 . . ? C132 C131 H131 108.5 . . ? C133 C132 C137 122.3(7) . . ? C133 C132 C131 118.4(7) . . ? C137 C132 C131 119.2(6) . . ? C134 C133 C132 118.8(8) . . ? C134 C133 H133 120.6 . . ? C132 C133 H133 120.6 . . ? C133 C134 C135 121.4(8) . . ? C133 C134 Cl14 120.6(8) . . ? C135 C134 Cl14 118.0(6) . . ? C136 C135 C134 118.7(7) . . ? C136 C135 H135 120.7 . . ? C134 C135 H135 120.7 . . ? C135 C136 C137 122.8(8) . . ? C135 C136 Br14 119.7(6) . . ? C137 C136 Br14 117.5(6) . . ? O104 C137 C132 122.1(6) . . ? O104 C137 C136 122.1(8) . . ? C132 C137 C136 115.8(7) . . ? H1W1 O1W H1W2 131.9 . . ? H2W1 O2W H2W2 119.5 . . ? C1S O1S H1S 109.5 . . ? O1S C1S H1S1 109.5 . . ? O1S C1S H1S2 109.5 . . ? H1S1 C1S H1S2 109.5 . . ? O1S C1S H1S3 109.5 . . ? H1S1 C1S H1S3 109.5 . . ? H1S2 C1S H1S3 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 O1W H1W1 O21 1.05 1.64 2.681(9) 171.5 . O1W H1W2 Cl14 1.06 2.57 3.505(7) 146.4 1_655 O2W H2W1 O1S 0.87 1.86 2.730(18) 178.4 . O2W H2W2 O11 0.88 2.01 2.890(13) 179.8 . O1S H1S O5W 0.84 2.20 3.04(3) 178.5 . _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 2.296 _refine_diff_density_min -2.415 _refine_diff_density_rms 0.166 #END