data_[Cu2(1)2(1-H)2Cl2].CH3OH _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H38 Cl2 Cu2 N4 O5' _chemical_formula_weight 720.61 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' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c 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 13.4562(16) _cell_length_b 14.3942(17) _cell_length_c 15.9350(19) _cell_angle_alpha 90.00 _cell_angle_beta 90.273(2) _cell_angle_gamma 90.00 _cell_volume 3086.4(6) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 9999 _cell_measurement_theta_min 1.28 _cell_measurement_theta_max 27.93 _exptl_crystal_description block _exptl_crystal_colour 'pale green' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.551 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1488 _exptl_absorpt_coefficient_mu 1.596 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7408 _exptl_absorpt_correction_T_max 0.7958 _exptl_absorpt_process_details SADBAS _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 APEX' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19043 _diffrn_reflns_av_R_equivalents 0.0626 _diffrn_reflns_av_sigmaI/netI 0.0879 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.28 _diffrn_reflns_theta_max 27.93 _reflns_number_total 7073 _reflns_number_gt 4973 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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^)+(0.0640P)^2^+6.9792P] 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 7073 _refine_ls_number_parameters 393 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1059 _refine_ls_R_factor_gt 0.0708 _refine_ls_wR_factor_ref 0.1625 _refine_ls_wR_factor_gt 0.1459 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.004 _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 Cu1 Cu 0.74966(7) 0.48569(5) 0.83964(4) 0.02066(18) Uani 1 1 d . . . Cu2 Cu 0.74443(7) 0.48367(5) 0.56034(4) 0.02197(18) Uani 1 1 d . . . Cl1 Cl 0.74225(17) 0.50919(12) 0.98481(9) 0.0382(4) Uani 1 1 d . . . Cl2 Cl 0.73187(16) 0.47445(12) 0.41395(10) 0.0397(5) Uani 1 1 d . . . N1 N 0.8667(4) 0.5725(3) 0.8305(3) 0.0197(11) Uani 1 1 d . . . C11 C 0.9598(5) 0.5551(5) 0.8604(4) 0.0251(15) Uani 1 1 d . . . C12 C 1.0296(5) 0.6252(5) 0.8596(5) 0.0365(18) Uani 1 1 d . . . H12 H 1.0930 0.6130 0.8801 0.044 Uiso 1 1 calc R . . C13 C 1.0085(6) 0.7126(5) 0.8292(5) 0.0395(19) Uani 1 1 d . . . H13 H 1.0564 0.7592 0.8288 0.047 Uiso 1 1 calc R . . C14 C 0.9134(5) 0.7285(5) 0.7994(5) 0.0317(16) Uani 1 1 d . . . H14 H 0.8957 0.7867 0.7789 0.038 Uiso 1 1 calc R . . C15 C 0.8447(5) 0.6570(4) 0.8004(4) 0.0242(14) Uani 1 1 d . . . C16 C 0.7396(5) 0.6732(4) 0.7698(4) 0.0262(14) Uani 1 1 d . . . H16A H 0.7085 0.7202 0.8045 0.031 Uiso 1 1 calc R . . H16B H 0.7414 0.6964 0.7126 0.031 Uiso 1 1 calc R . . C17 C 0.9817(5) 0.4604(5) 0.8935(5) 0.0339(18) Uani 1 1 d . . . H17A H 0.9286 0.4408 0.9294 0.051 Uiso 1 1 calc R . . H17B H 1.0428 0.4617 0.9248 0.051 Uiso 1 1 calc R . . H17C H 0.9877 0.4177 0.8475 0.051 Uiso 1 1 calc R . . O18 O 0.6825(3) 0.5916(3) 0.7722(3) 0.0249(11) Uani 1 1 d . . . N2 N 0.6343(4) 0.3952(3) 0.8354(3) 0.0178(11) Uani 1 1 d . . . C21 C 0.5413(5) 0.4096(5) 0.8627(4) 0.0240(15) Uani 1 1 d . . . C22 C 0.4747(5) 0.3359(5) 0.8678(5) 0.0321(17) Uani 1 1 d . . . H22 H 0.4097 0.3464 0.8849 0.039 Uiso 1 1 calc R . . C23 C 0.5051(5) 0.2478(5) 0.8476(5) 0.0353(18) Uani 1 1 d . . . H23 H 0.4623 0.1977 0.8543 0.042 Uiso 1 1 calc R . . C24 C 0.5991(5) 0.2344(5) 0.8175(4) 0.0311(17) Uani 1 1 d . . . H24 H 0.6198 0.1756 0.8008 0.037 Uiso 1 1 calc R . . C25 C 0.6626(5) 0.3089(4) 0.8124(4) 0.0206(14) Uani 1 1 d . . . O28 O 0.8167(3) 0.3844(3) 0.7744(3) 0.0252(10) Uani 1 1 d . . . C27 C 0.5092(5) 0.5053(5) 0.8849(5) 0.0301(16) Uani 1 1 d . . . H27A H 0.5526 0.5299 0.9274 0.045 Uiso 1 1 calc R . . H27B H 0.4423 0.5038 0.9056 0.045 Uiso 1 1 calc R . . H27C H 0.5120 0.5442 0.8359 0.045 Uiso 1 1 calc R . . C26 C 0.7660(5) 0.2991(4) 0.7783(4) 0.0218(14) Uani 1 1 d . . . H26A H 0.8033 0.2566 0.8136 0.026 Uiso 1 1 calc R . . H26B H 0.7624 0.2725 0.7224 0.026 Uiso 1 1 calc R . . N3 N 0.6488(4) 0.3778(3) 0.5756(3) 0.0194(11) Uani 1 1 d . . . C31 C 0.6645(5) 0.2881(5) 0.5548(4) 0.0241(15) Uani 1 1 d . . . C32 C 0.5916(6) 0.2225(5) 0.5693(5) 0.0328(17) Uani 1 1 d . . . H32 H 0.6029 0.1606 0.5556 0.039 Uiso 1 1 calc R . . C33 C 0.5026(6) 0.2484(5) 0.6038(5) 0.040(2) Uani 1 1 d . . . H33 H 0.4536 0.2043 0.6138 0.049 Uiso 1 1 calc R . . C34 C 0.4863(5) 0.3405(5) 0.6235(5) 0.0324(17) Uani 1 1 d . . . H34 H 0.4260 0.3597 0.6460 0.039 Uiso 1 1 calc R . . C35 C 0.5616(5) 0.4035(4) 0.6090(4) 0.0220(14) Uani 1 1 d . . . C36 C 0.5493(5) 0.5057(4) 0.6249(5) 0.0242(15) Uani 1 1 d . . . H36A H 0.5074 0.5321 0.5813 0.029 Uiso 1 1 calc R . . H36B H 0.5161 0.5145 0.6782 0.029 Uiso 1 1 calc R . . C37 C 0.7615(6) 0.2619(5) 0.5162(4) 0.0331(15) Uani 1 1 d . . . H37A H 0.7634 0.1960 0.5075 0.050 Uiso 1 1 calc R . . H37B H 0.8148 0.2798 0.5530 0.050 Uiso 1 1 calc R . . H37C H 0.7685 0.2932 0.4634 0.050 Uiso 1 1 calc R . . O38 O 0.6398(3) 0.5527(3) 0.6264(3) 0.0204(9) Uani 1 1 d . . . N4 N 0.8438(4) 0.5890(4) 0.5631(3) 0.0224(12) Uani 1 1 d . . . C41 C 0.8281(5) 0.6765(5) 0.5350(4) 0.0272(15) Uani 1 1 d . . . C42 C 0.9043(6) 0.7434(5) 0.5393(5) 0.0378(18) Uani 1 1 d . . . H42 H 0.8936 0.8037 0.5206 0.045 Uiso 1 1 calc R . . C43 C 0.9955(6) 0.7172(5) 0.5720(5) 0.043(2) Uani 1 1 d . . . H43 H 1.0472 0.7600 0.5746 0.051 Uiso 1 1 calc R . . C44 C 1.0098(6) 0.6286(5) 0.6006(5) 0.0362(18) Uani 1 1 d . . . H44 H 1.0707 0.6110 0.6233 0.043 Uiso 1 1 calc R . . C45 C 0.9333(5) 0.5661(4) 0.5953(4) 0.0217(14) Uani 1 1 d . . . C46 C 0.9449(5) 0.4665(5) 0.6256(5) 0.0272(16) Uani 1 1 d . . . H46A H 0.9890 0.4335 0.5881 0.033 Uiso 1 1 calc R . . H46B H 0.9752 0.4667 0.6810 0.033 Uiso 1 1 calc R . . C47 C 0.7313(6) 0.7000(5) 0.4963(5) 0.0390(19) Uani 1 1 d . . . H47A H 0.7242 0.7663 0.4936 0.058 Uiso 1 1 calc R . . H47B H 0.6787 0.6744 0.5296 0.058 Uiso 1 1 calc R . . H47C H 0.7281 0.6746 0.4407 0.058 Uiso 1 1 calc R . . O48 O 0.8544(3) 0.4201(3) 0.6293(3) 0.0230(10) Uani 1 1 d . . . C99 C 0.7576(8) 0.5488(9) 0.2046(6) 0.084(3) Uani 1 1 d . . . H99A H 0.7619 0.4873 0.1818 0.126 Uiso 1 1 calc R . . H99B H 0.7658 0.5935 0.1605 0.126 Uiso 1 1 calc R . . H99C H 0.6938 0.5572 0.2303 0.126 Uiso 1 1 calc R . . O100 O 0.8286(10) 0.5606(8) 0.2618(6) 0.155(5) Uani 1 1 d . . . H28 H 0.838(7) 0.400(7) 0.690(7) 0.09(4) Uiso 1 1 d . . . H18 H 0.660(5) 0.576(5) 0.724(5) 0.04(2) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0230(4) 0.0166(3) 0.0223(4) -0.0011(3) 0.0006(4) -0.0048(4) Cu2 0.0221(4) 0.0200(4) 0.0239(4) -0.0001(3) -0.0011(4) -0.0039(4) Cl1 0.0453(10) 0.0465(10) 0.0228(8) -0.0055(7) 0.0056(9) -0.0136(10) Cl2 0.0578(14) 0.0376(10) 0.0238(8) 0.0025(7) -0.0019(9) -0.0097(9) N1 0.020(3) 0.018(3) 0.021(3) -0.006(2) -0.001(2) -0.003(2) C11 0.027(4) 0.027(4) 0.021(3) -0.005(3) 0.003(3) 0.000(3) C12 0.020(4) 0.036(4) 0.053(5) -0.007(4) 0.003(3) -0.003(3) C13 0.033(4) 0.035(4) 0.051(5) -0.007(4) 0.007(4) -0.013(3) C14 0.030(4) 0.025(4) 0.039(4) -0.009(3) 0.006(3) -0.007(3) C15 0.026(3) 0.025(4) 0.022(3) -0.006(3) 0.001(3) -0.005(3) C16 0.031(4) 0.017(3) 0.030(3) -0.002(2) -0.005(3) -0.003(3) C17 0.029(4) 0.031(4) 0.042(4) -0.009(3) -0.012(3) -0.001(3) O18 0.029(3) 0.021(3) 0.024(3) 0.0046(19) -0.007(2) -0.0077(19) N2 0.019(3) 0.016(3) 0.018(3) 0.002(2) 0.001(2) 0.002(2) C21 0.025(4) 0.027(4) 0.020(3) 0.007(3) -0.005(3) -0.002(3) C22 0.024(4) 0.030(4) 0.043(4) 0.010(3) 0.004(3) -0.005(3) C23 0.032(4) 0.025(4) 0.049(5) 0.010(3) 0.001(4) -0.010(3) C24 0.036(4) 0.018(4) 0.039(4) 0.003(3) -0.004(3) 0.000(3) C25 0.025(3) 0.018(3) 0.018(3) 0.006(2) -0.004(3) -0.001(2) O28 0.025(2) 0.024(3) 0.027(3) -0.0057(19) 0.008(2) -0.0047(19) C27 0.029(4) 0.024(4) 0.038(4) 0.002(3) 0.009(3) 0.004(3) C26 0.028(4) 0.015(3) 0.023(3) 0.003(2) 0.002(3) 0.005(3) N3 0.022(3) 0.016(3) 0.020(3) 0.000(2) -0.002(2) 0.000(2) C31 0.029(4) 0.025(4) 0.018(3) -0.002(3) -0.004(3) 0.000(3) C32 0.040(4) 0.014(3) 0.045(5) -0.006(3) 0.000(4) -0.006(3) C33 0.034(4) 0.027(4) 0.060(5) 0.004(4) 0.003(4) -0.014(3) C34 0.024(4) 0.026(4) 0.047(5) -0.003(3) 0.000(3) -0.006(3) C35 0.025(3) 0.022(4) 0.019(3) 0.003(3) -0.008(3) -0.001(3) C36 0.022(3) 0.020(4) 0.031(4) -0.004(3) -0.005(3) -0.001(3) C37 0.040(4) 0.027(3) 0.032(4) -0.006(3) -0.004(4) 0.009(3) O38 0.019(2) 0.017(2) 0.026(2) -0.0060(18) 0.0001(19) 0.0019(17) N4 0.023(3) 0.022(3) 0.022(3) 0.000(2) -0.001(2) -0.006(2) C41 0.038(4) 0.022(4) 0.021(3) 0.002(3) 0.009(3) -0.003(3) C42 0.048(5) 0.024(4) 0.041(4) -0.001(3) 0.004(4) -0.003(4) C43 0.036(4) 0.031(4) 0.061(5) -0.008(4) 0.015(4) -0.011(3) C44 0.027(4) 0.039(5) 0.043(5) -0.001(3) -0.002(3) -0.009(3) C45 0.022(3) 0.019(3) 0.024(3) -0.001(3) 0.002(3) -0.001(3) C46 0.020(3) 0.036(4) 0.026(4) 0.002(3) -0.001(3) 0.005(3) C47 0.046(5) 0.022(4) 0.049(5) 0.008(3) -0.005(4) 0.001(3) O48 0.017(2) 0.026(3) 0.026(2) 0.0034(19) -0.002(2) -0.0036(18) C99 0.060(7) 0.147(11) 0.045(5) 0.003(6) -0.017(7) 0.018(7) O100 0.250(14) 0.148(9) 0.066(6) 0.007(6) -0.012(7) -0.114(9) _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 Cu1 O28 2.008(4) . ? Cu1 N1 2.016(5) . ? Cu1 N2 2.027(5) . ? Cu1 O18 2.071(4) . ? Cu1 Cl1 2.3405(16) . ? Cu2 N3 2.010(5) . ? Cu2 N4 2.022(5) . ? Cu2 O38 2.023(4) . ? Cu2 O48 2.054(4) . ? Cu2 Cl2 2.3417(18) . ? N1 C15 1.341(8) . ? N1 C11 1.362(8) . ? C11 C12 1.377(10) . ? C11 C17 1.490(10) . ? C12 C13 1.378(11) . ? C13 C14 1.382(10) . ? C14 C15 1.383(9) . ? C15 C16 1.511(9) . ? C16 O18 1.404(7) . ? N2 C21 1.344(8) . ? N2 C25 1.350(8) . ? C21 C22 1.390(9) . ? C21 C27 1.488(9) . ? C22 C23 1.372(10) . ? C23 C24 1.369(10) . ? C24 C25 1.374(9) . ? C25 C26 1.504(9) . ? O28 C26 1.405(7) . ? N3 C35 1.341(8) . ? N3 C31 1.350(8) . ? C31 C32 1.381(9) . ? C31 C37 1.493(10) . ? C32 C33 1.372(11) . ? C33 C34 1.380(10) . ? C34 C35 1.380(9) . ? C35 C36 1.503(9) . ? C36 O38 1.393(7) . ? N4 C45 1.349(8) . ? N4 C41 1.353(8) . ? C41 C42 1.407(10) . ? C41 C47 1.478(10) . ? C42 C43 1.383(11) . ? C43 C44 1.368(10) . ? C44 C45 1.369(9) . ? C45 C46 1.520(9) . ? C46 O48 1.391(8) . ? C99 O100 1.327(12) . ? 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 O28 Cu1 N1 93.4(2) . . ? O28 Cu1 N2 82.05(19) . . ? N1 Cu1 N2 173.7(2) . . ? O28 Cu1 O18 117.54(18) . . ? N1 Cu1 O18 81.1(2) . . ? N2 Cu1 O18 97.11(19) . . ? O28 Cu1 Cl1 129.66(15) . . ? N1 Cu1 Cl1 91.07(15) . . ? N2 Cu1 Cl1 95.14(15) . . ? O18 Cu1 Cl1 112.70(15) . . ? N3 Cu2 N4 171.7(2) . . ? N3 Cu2 O38 82.04(19) . . ? N4 Cu2 O38 94.7(2) . . ? N3 Cu2 O48 93.30(19) . . ? N4 Cu2 O48 81.3(2) . . ? O38 Cu2 O48 116.22(17) . . ? N3 Cu2 Cl2 91.99(15) . . ? N4 Cu2 Cl2 96.23(16) . . ? O38 Cu2 Cl2 119.96(14) . . ? O48 Cu2 Cl2 123.77(15) . . ? C15 N1 C11 119.5(5) . . ? C15 N1 Cu1 114.7(4) . . ? C11 N1 Cu1 125.4(4) . . ? N1 C11 C12 119.3(6) . . ? N1 C11 C17 118.1(6) . . ? C12 C11 C17 122.6(6) . . ? C11 C12 C13 122.2(7) . . ? C12 C13 C14 117.4(7) . . ? C13 C14 C15 119.5(7) . . ? N1 C15 C14 122.2(6) . . ? N1 C15 C16 117.4(5) . . ? C14 C15 C16 120.4(6) . . ? O18 C16 C15 112.0(5) . . ? C16 O18 Cu1 113.1(4) . . ? C21 N2 C25 119.6(5) . . ? C21 N2 Cu1 127.2(4) . . ? C25 N2 Cu1 112.6(4) . . ? N2 C21 C22 120.2(6) . . ? N2 C21 C27 119.4(6) . . ? C22 C21 C27 120.3(7) . . ? C23 C22 C21 119.9(7) . . ? C24 C23 C22 119.4(7) . . ? C23 C24 C25 119.1(7) . . ? N2 C25 C24 121.8(6) . . ? N2 C25 C26 116.5(5) . . ? C24 C25 C26 121.7(6) . . ? C26 O28 Cu1 113.1(4) . . ? O28 C26 C25 112.6(5) . . ? C35 N3 C31 119.9(5) . . ? C35 N3 Cu2 113.6(4) . . ? C31 N3 Cu2 126.4(5) . . ? N3 C31 C32 120.0(6) . . ? N3 C31 C37 118.7(6) . . ? C32 C31 C37 121.2(6) . . ? C33 C32 C31 120.2(6) . . ? C32 C33 C34 119.5(7) . . ? C33 C34 C35 118.4(7) . . ? N3 C35 C34 122.0(6) . . ? N3 C35 C36 115.7(6) . . ? C34 C35 C36 122.2(6) . . ? O38 C36 C35 112.4(5) . . ? C36 O38 Cu2 111.3(4) . . ? C45 N4 C41 119.4(6) . . ? C45 N4 Cu2 114.5(4) . . ? C41 N4 Cu2 126.1(5) . . ? N4 C41 C42 120.5(7) . . ? N4 C41 C47 119.1(6) . . ? C42 C41 C47 120.3(6) . . ? C43 C42 C41 118.5(7) . . ? C44 C43 C42 120.1(7) . . ? C43 C44 C45 119.2(7) . . ? N4 C45 C44 122.2(6) . . ? N4 C45 C46 116.2(5) . . ? C44 C45 C46 121.6(6) . . ? O48 C46 C45 112.2(5) . . ? C46 O48 Cu2 113.1(4) . . ? _diffrn_measured_fraction_theta_max 0.955 _diffrn_reflns_theta_full 27.93 _diffrn_measured_fraction_theta_full 0.955 _refine_diff_density_max 0.778 _refine_diff_density_min -0.884 _refine_diff_density_rms 0.118 #END data_[Cu2(1)2(1-H)2Br2].H2O _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H36 Br2 Cu2 N4 O5' _chemical_formula_weight 795.51 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' '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 P2(1)/c 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 13.606(2) _cell_length_b 14.407(3) _cell_length_c 15.591(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.107(3) _cell_angle_gamma 90.00 _cell_volume 3056.3(9) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 9999 _cell_measurement_theta_min 2.44 _cell_measurement_theta_max 23.26 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.729 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1600 _exptl_absorpt_coefficient_mu 4.050 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.3763 _exptl_absorpt_correction_T_max 0.4980 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13642 _diffrn_reflns_av_R_equivalents 0.0881 _diffrn_reflns_av_sigmaI/netI 0.1790 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.44 _diffrn_reflns_theta_max 23.26 _reflns_number_total 4369 _reflns_number_gt 1739 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _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^)+(0.0297P)^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 fixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4369 _refine_ls_number_parameters 375 _refine_ls_number_restraints 190 _refine_ls_R_factor_all 0.1271 _refine_ls_R_factor_gt 0.0413 _refine_ls_wR_factor_ref 0.0858 _refine_ls_wR_factor_gt 0.0720 _refine_ls_goodness_of_fit_ref 0.661 _refine_ls_restrained_S_all 0.651 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.74837(16) 0.49249(10) 0.05654(7) 0.0356(3) Uani 1 1 d . . . Cu2 Cu 0.74964(16) 0.49357(10) 0.33353(7) 0.0338(3) Uani 1 1 d . . . Br3 Br 0.74047(16) 0.48889(10) -0.10467(7) 0.0597(4) Uani 1 1 d . . . Br4 Br 0.74570(15) 0.50458(9) 0.49659(6) 0.0464(3) Uani 1 1 d . . . N1 N 0.8445(7) 0.5975(6) 0.0645(7) 0.029(3) Uani 1 1 d . . . N10 N 0.6514(8) 0.3853(6) 0.0681(7) 0.032(3) Uani 1 1 d . . . N20 N 0.8638(7) 0.5814(6) 0.3273(7) 0.026(3) Uani 1 1 d . . . N30 N 0.6343(8) 0.4038(6) 0.3277(8) 0.037(3) Uani 1 1 d . . . O9 O 0.8550(6) 0.4270(5) 0.1249(6) 0.035(3) Uani 1 1 d . . . O18 O 0.6430(6) 0.5606(5) 0.1230(6) 0.036(3) Uani 1 1 d D . . O28 O 0.6842(6) 0.5987(6) 0.2721(6) 0.037(3) Uani 1 1 d D . . O38 O 0.8173(6) 0.3895(5) 0.2704(6) 0.036(3) Uani 1 1 d . . . C2 C 0.8303(9) 0.6854(9) 0.0395(9) 0.038(3) Uani 1 1 d U . . C3 C 0.9031(9) 0.7510(9) 0.0463(10) 0.044(3) Uani 1 1 d U . . H3 H 0.8919 0.8132 0.0284 0.053 Uiso 1 1 calc R . . C4 C 0.9915(10) 0.7249(9) 0.0791(10) 0.047(3) Uani 1 1 d U . . H4 H 1.0425 0.7697 0.0837 0.057 Uiso 1 1 calc R . . C5 C 1.0090(9) 0.6360(8) 0.1056(10) 0.038(3) Uani 1 1 d U . . H5 H 1.0705 0.6184 0.1295 0.046 Uiso 1 1 calc R . . C6 C 0.9330(9) 0.5724(8) 0.0960(10) 0.031(3) Uani 1 1 d U . . C7 C 0.9467(8) 0.4738(8) 0.1211(10) 0.033(3) Uani 1 1 d U . . H7A H 0.9897 0.4425 0.0789 0.039 Uiso 1 1 calc R . . H7B H 0.9792 0.4707 0.1779 0.039 Uiso 1 1 calc R . . C8 C 0.7326(9) 0.7122(7) 0.0021(8) 0.037(3) Uani 1 1 d U . . H8A H 0.6800 0.6803 0.0334 0.055 Uiso 1 1 calc R . . H8B H 0.7302 0.6942 -0.0584 0.055 Uiso 1 1 calc R . . H8C H 0.7236 0.7794 0.0071 0.055 Uiso 1 1 calc R . . C11 C 0.5652(9) 0.4131(8) 0.1005(10) 0.031(3) Uani 1 1 d U . . C12 C 0.4896(9) 0.3484(8) 0.1103(10) 0.037(3) Uani 1 1 d U . . H12 H 0.4275 0.3673 0.1318 0.045 Uiso 1 1 calc R . . C13 C 0.5057(9) 0.2582(9) 0.0886(10) 0.046(3) Uani 1 1 d U . . H13 H 0.4548 0.2137 0.0958 0.055 Uiso 1 1 calc R . . C14 C 0.5954(9) 0.2311(7) 0.0562(9) 0.040(3) Uani 1 1 d U . . H14 H 0.6071 0.1679 0.0422 0.048 Uiso 1 1 calc R . . C15 C 0.6682(9) 0.2969(7) 0.0444(10) 0.036(3) Uani 1 1 d U . . C16 C 0.7665(9) 0.2713(7) 0.0094(9) 0.047(4) Uani 1 1 d U . . H16A H 0.8168 0.2805 0.0537 0.070 Uiso 1 1 calc R . . H16B H 0.7814 0.3105 -0.0403 0.070 Uiso 1 1 calc R . . H16C H 0.7659 0.2060 -0.0083 0.070 Uiso 1 1 calc R . . C17 C 0.5536(8) 0.5135(8) 0.1225(10) 0.035(3) Uani 1 1 d U . . H17A H 0.5091 0.5430 0.0802 0.042 Uiso 1 1 calc R . . H17B H 0.5227 0.5189 0.1797 0.042 Uiso 1 1 calc R . . C21 C 0.9562(10) 0.5644(8) 0.3556(10) 0.037(3) Uani 1 1 d U . . C22 C 1.0268(10) 0.6352(8) 0.3556(9) 0.042(3) Uani 1 1 d U . . H22 H 1.0922 0.6223 0.3734 0.050 Uiso 1 1 calc R . . C23 C 1.0023(10) 0.7209(8) 0.3304(10) 0.045(3) Uani 1 1 d U . . H23 H 1.0496 0.7694 0.3331 0.054 Uiso 1 1 calc R . . C24 C 0.9080(9) 0.7395(8) 0.3004(9) 0.038(3) Uani 1 1 d U . . H24 H 0.8900 0.7998 0.2813 0.045 Uiso 1 1 calc R . . C25 C 0.8408(9) 0.6665(8) 0.2992(10) 0.032(3) Uani 1 1 d U . . C26 C 0.9812(8) 0.4682(8) 0.3873(10) 0.047(4) Uani 1 1 d U . . H26A H 0.9493 0.4575 0.4427 0.071 Uiso 1 1 calc R . . H26B H 1.0526 0.4626 0.3940 0.071 Uiso 1 1 calc R . . H26C H 0.9580 0.4221 0.3457 0.071 Uiso 1 1 calc R . . C27 C 0.7378(9) 0.6802(7) 0.2698(8) 0.029(3) Uani 1 1 d U . . H27A H 0.7056 0.7269 0.3068 0.034 Uiso 1 1 calc R . . H27B H 0.7382 0.7045 0.2104 0.034 Uiso 1 1 calc R . . C31 C 0.5393(9) 0.4194(8) 0.3537(9) 0.034(3) Uani 1 1 d U . . C32 C 0.4740(9) 0.3483(8) 0.3581(9) 0.039(3) Uani 1 1 d U . . H32 H 0.4085 0.3593 0.3765 0.046 Uiso 1 1 calc R . . C33 C 0.5041(9) 0.2583(10) 0.3353(10) 0.046(3) Uani 1 1 d U . . H33 H 0.4589 0.2082 0.3386 0.055 Uiso 1 1 calc R . . C34 C 0.5981(9) 0.2428(8) 0.3084(9) 0.039(3) Uani 1 1 d U . . H34 H 0.6198 0.1823 0.2932 0.047 Uiso 1 1 calc R . . C35 C 0.6601(8) 0.3177(8) 0.3041(10) 0.030(3) Uani 1 1 d U . . C36 C 0.5125(8) 0.5160(8) 0.3788(9) 0.039(3) Uani 1 1 d U . . H36A H 0.5647 0.5422 0.4149 0.058 Uiso 1 1 calc R . . H36B H 0.4507 0.5152 0.4110 0.058 Uiso 1 1 calc R . . H36C H 0.5046 0.5541 0.3272 0.058 Uiso 1 1 calc R . . C37 C 0.7666(9) 0.3039(7) 0.2757(8) 0.031(3) Uani 1 1 d U . . H37A H 0.8006 0.2629 0.3171 0.037 Uiso 1 1 calc R . . H37B H 0.7675 0.2731 0.2189 0.037 Uiso 1 1 calc R . . O99 O 0.7773(10) 0.5867(8) -0.2951(8) 0.185(6) Uani 1 1 d . . . H18 H 0.6648 0.5799 0.2164 0.050 Uiso 1 1 d D . . H9 H 0.8376 0.4103 0.1733 0.050 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0195(6) 0.0282(7) 0.0590(8) -0.0042(9) -0.0044(12) -0.0014(8) Cu2 0.0208(6) 0.0233(6) 0.0573(8) -0.0003(9) -0.0053(12) -0.0047(8) Br3 0.0596(10) 0.0594(8) 0.0601(7) -0.0145(10) -0.0187(12) 0.0225(9) Br4 0.0428(7) 0.0403(7) 0.0561(6) -0.0045(9) 0.0037(12) -0.0121(8) N1 0.014(6) 0.031(6) 0.043(9) 0.004(6) -0.005(6) -0.007(5) N10 0.025(7) 0.020(6) 0.051(9) -0.009(6) -0.016(6) 0.000(5) N20 0.011(6) 0.031(6) 0.035(8) 0.004(6) -0.002(6) 0.004(5) N30 0.044(8) 0.013(5) 0.053(10) 0.006(6) -0.002(7) 0.001(5) O9 0.028(6) 0.025(5) 0.051(8) 0.007(5) -0.011(5) 0.002(4) O18 0.021(5) 0.026(5) 0.060(8) -0.012(5) -0.005(5) -0.004(4) O28 0.033(6) 0.032(5) 0.046(7) 0.002(5) -0.018(5) 0.001(5) O38 0.015(5) 0.022(5) 0.072(9) -0.018(5) -0.004(5) 0.000(4) C2 0.024(5) 0.038(6) 0.051(8) 0.000(6) 0.000(6) 0.001(4) C3 0.032(5) 0.032(5) 0.069(8) 0.004(5) 0.001(6) -0.001(4) C4 0.026(4) 0.038(4) 0.077(7) 0.006(6) 0.000(5) -0.009(4) C5 0.017(5) 0.038(4) 0.059(7) 0.000(6) -0.003(6) -0.004(4) C6 0.020(5) 0.032(4) 0.041(7) -0.005(6) -0.002(6) -0.002(4) C7 0.018(6) 0.033(4) 0.047(8) -0.003(6) 0.002(6) 0.003(5) C8 0.031(6) 0.024(5) 0.056(9) 0.007(6) -0.001(7) 0.007(5) C11 0.017(5) 0.020(4) 0.057(8) 0.000(6) -0.004(6) 0.001(4) C12 0.014(5) 0.025(4) 0.072(7) -0.002(6) 0.003(6) 0.001(3) C13 0.026(4) 0.022(4) 0.089(8) -0.003(6) 0.001(5) -0.005(4) C14 0.031(5) 0.010(5) 0.079(8) -0.008(5) -0.002(5) -0.001(3) C15 0.025(5) 0.014(5) 0.070(8) -0.012(6) 0.001(5) 0.000(3) C16 0.026(5) 0.023(6) 0.091(11) -0.011(7) 0.003(7) 0.008(5) C17 0.023(6) 0.022(4) 0.062(9) -0.002(7) -0.001(6) 0.004(5) C21 0.031(6) 0.028(5) 0.052(8) -0.003(6) -0.006(6) 0.000(4) C22 0.021(5) 0.038(5) 0.067(8) -0.004(5) -0.002(5) -0.001(4) C23 0.028(4) 0.036(4) 0.071(7) 0.003(6) -0.001(6) -0.011(4) C24 0.030(4) 0.023(5) 0.061(7) 0.003(5) 0.002(6) -0.006(3) C25 0.025(5) 0.025(5) 0.046(7) 0.000(6) 0.003(6) -0.005(4) C26 0.031(8) 0.035(5) 0.075(11) 0.005(7) -0.015(8) 0.006(5) C27 0.030(5) 0.018(5) 0.039(7) -0.007(5) -0.002(6) 0.001(5) C31 0.014(6) 0.028(4) 0.061(8) 0.003(6) 0.005(6) -0.005(4) C32 0.012(5) 0.032(4) 0.072(8) 0.007(5) 0.005(5) -0.007(3) C33 0.026(4) 0.030(4) 0.083(8) 0.001(5) 0.002(6) -0.011(4) C34 0.029(4) 0.016(4) 0.072(7) 0.006(5) 0.001(6) -0.003(3) C35 0.017(4) 0.019(5) 0.054(7) 0.002(6) -0.006(5) 0.000(3) C36 0.029(7) 0.026(4) 0.061(9) 0.012(7) 0.013(7) 0.000(5) C37 0.023(4) 0.020(5) 0.051(8) 0.002(5) 0.000(6) 0.005(4) O99 0.176(15) 0.149(11) 0.230(14) -0.080(11) 0.099(13) -0.050(11) _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 Cu1 N1 2.004(9) . ? Cu1 O18 2.024(9) . ? Cu1 O9 2.031(8) . ? Cu1 N10 2.039(10) . ? Cu1 Br3 2.5159(18) . ? Cu2 O28 2.000(8) . ? Cu2 N20 2.006(10) . ? Cu2 O38 2.017(8) . ? Cu2 N30 2.036(10) . ? Cu2 Br4 2.5479(17) . ? N1 C2 1.339(14) . ? N1 C6 1.349(14) . ? N10 C11 1.339(14) . ? N10 C15 1.346(13) . ? N20 C25 1.338(14) . ? N20 C21 1.355(14) . ? N30 C35 1.341(13) . ? N30 C31 1.373(15) . ? O9 C7 1.419(12) . ? O18 C17 1.393(12) . ? O28 C27 1.383(12) . ? O38 C37 1.415(12) . ? C2 C3 1.373(15) . ? C2 C8 1.501(15) . ? C3 C4 1.360(16) . ? C4 C5 1.368(16) . ? C5 C6 1.390(14) . ? C6 C7 1.485(14) . ? C11 C12 1.396(15) . ? C11 C17 1.495(13) . ? C12 C13 1.361(16) . ? C13 C14 1.378(16) . ? C14 C15 1.383(15) . ? C15 C16 1.492(16) . ? C21 C22 1.400(15) . ? C21 C26 1.510(15) . ? C22 C23 1.338(16) . ? C23 C24 1.392(16) . ? C24 C25 1.393(15) . ? C25 C27 1.487(15) . ? C31 C32 1.358(15) . ? C31 C36 1.492(15) . ? C32 C33 1.406(17) . ? C33 C34 1.366(16) . ? C34 C35 1.372(14) . ? C35 C37 1.529(16) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cu1 O18 93.7(4) . . ? N1 Cu1 O9 81.5(4) . . ? O18 Cu1 O9 117.5(2) . . ? N1 Cu1 N10 171.4(3) . . ? O18 Cu1 N10 82.1(4) . . ? O9 Cu1 N10 93.6(3) . . ? N1 Cu1 Br3 96.0(3) . . ? O18 Cu1 Br3 119.5(3) . . ? O9 Cu1 Br3 123.0(3) . . ? N10 Cu1 Br3 92.7(3) . . ? O28 Cu2 N20 81.0(4) . . ? O28 Cu2 O38 122.2(3) . . ? N20 Cu2 O38 95.2(4) . . ? O28 Cu2 N30 96.7(4) . . ? N20 Cu2 N30 174.7(3) . . ? O38 Cu2 N30 81.9(4) . . ? O28 Cu2 Br4 114.9(3) . . ? N20 Cu2 Br4 91.5(3) . . ? O38 Cu2 Br4 123.0(3) . . ? N30 Cu2 Br4 93.8(3) . . ? C2 N1 C6 119.2(11) . . ? C2 N1 Cu1 127.0(9) . . ? C6 N1 Cu1 113.7(8) . . ? C11 N10 C15 122.4(11) . . ? C11 N10 Cu1 112.0(7) . . ? C15 N10 Cu1 125.6(9) . . ? C25 N20 C21 119.2(11) . . ? C25 N20 Cu2 114.4(8) . . ? C21 N20 Cu2 126.1(8) . . ? C35 N30 C31 118.7(11) . . ? C35 N30 Cu2 113.4(9) . . ? C31 N30 Cu2 127.5(8) . . ? C7 O9 Cu1 112.6(7) . . ? C17 O18 Cu1 112.4(7) . . ? C27 O28 Cu2 114.9(7) . . ? C37 O38 Cu2 113.3(7) . . ? N1 C2 C3 121.7(12) . . ? N1 C2 C8 118.9(11) . . ? C3 C2 C8 119.4(11) . . ? C4 C3 C2 118.5(12) . . ? C5 C4 C3 121.7(12) . . ? C4 C5 C6 117.2(12) . . ? N1 C6 C5 121.7(12) . . ? N1 C6 C7 117.6(10) . . ? C5 C6 C7 120.6(11) . . ? O9 C7 C6 110.8(9) . . ? N10 C11 C12 119.2(11) . . ? N10 C11 C17 117.9(10) . . ? C12 C11 C17 122.8(12) . . ? C13 C12 C11 119.4(12) . . ? C12 C13 C14 120.3(11) . . ? C13 C14 C15 119.3(11) . . ? N10 C15 C14 119.3(12) . . ? N10 C15 C16 119.1(11) . . ? C14 C15 C16 121.5(10) . . ? O18 C17 C11 112.3(9) . . ? N20 C21 C22 120.3(12) . . ? N20 C21 C26 118.8(11) . . ? C22 C21 C26 120.9(12) . . ? C23 C22 C21 120.1(12) . . ? C22 C23 C24 120.3(12) . . ? C23 C24 C25 117.7(11) . . ? N20 C25 C24 122.3(12) . . ? N20 C25 C27 116.2(10) . . ? C24 C25 C27 121.5(11) . . ? O28 C27 C25 112.1(9) . . ? C32 C31 N30 120.6(12) . . ? C32 C31 C36 122.0(12) . . ? N30 C31 C36 117.4(10) . . ? C31 C32 C33 119.5(12) . . ? C34 C33 C32 120.1(12) . . ? C33 C34 C35 117.6(12) . . ? N30 C35 C34 123.5(12) . . ? N30 C35 C37 116.7(10) . . ? C34 C35 C37 119.7(10) . . ? O38 C37 C35 111.5(9) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 23.26 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.163 _refine_diff_density_min -0.421 _refine_diff_density_rms 0.099 #END data_[Cu2(1)2(1-H)2](ClO4)2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H34 Cl2 Cu2 N4 O12' _chemical_formula_weight 816.57 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' 'Cu' 'Cu' 0.3201 1.2651 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c 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 10.0579(6) _cell_length_b 11.7112(7) _cell_length_c 13.7986(8) _cell_angle_alpha 90.00 _cell_angle_beta 105.2620(10) _cell_angle_gamma 90.00 _cell_volume 1568.02(16) _cell_formula_units_Z 2 _cell_measurement_temperature 220(2) _cell_measurement_reflns_used 9572 _cell_measurement_theta_min 2.10 _cell_measurement_theta_max 27.90 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.730 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 836 _exptl_absorpt_coefficient_mu 1.598 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7405 _exptl_absorpt_correction_T_max 0.9687 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 220(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 P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9572 _diffrn_reflns_av_R_equivalents 0.0284 _diffrn_reflns_av_sigmaI/netI 0.0385 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 27.90 _reflns_number_total 3603 _reflns_number_gt 3149 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0479P)^2^+3.1071P] 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 3603 _refine_ls_number_parameters 223 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0484 _refine_ls_R_factor_gt 0.0409 _refine_ls_wR_factor_ref 0.1050 _refine_ls_wR_factor_gt 0.1009 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _refine_ls_shift/su_max 0.009 _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 Cu1 Cu 0.89211(3) 0.07560(3) 0.43344(2) 0.01246(11) Uani 1 1 d . . . Cl1 Cl 0.72445(7) 0.60369(6) 0.35753(5) 0.01511(16) Uani 1 1 d . . . N1 N 0.7192(2) 0.11968(19) 0.47397(17) 0.0119(4) Uani 1 1 d . . . C2 C 0.6168(3) 0.1938(2) 0.4306(2) 0.0139(5) Uani 1 1 d . . . C3 C 0.5098(3) 0.2156(3) 0.4744(2) 0.0173(6) Uani 1 1 d . . . H3 H 0.4403 0.2665 0.4441 0.021 Uiso 1 1 calc R . . C4 C 0.5063(3) 0.1616(3) 0.5631(2) 0.0198(6) Uani 1 1 d . . . H4 H 0.4345 0.1756 0.5924 0.024 Uiso 1 1 calc R . . C5 C 0.6106(3) 0.0869(2) 0.6073(2) 0.0160(6) Uani 1 1 d . . . H5 H 0.6105 0.0497 0.6668 0.019 Uiso 1 1 calc R . . C6 C 0.7158(3) 0.0683(2) 0.5613(2) 0.0129(5) Uani 1 1 d . . . C7 C 0.8344(3) -0.0101(2) 0.6071(2) 0.0148(6) Uani 1 1 d . . . H7A H 0.8622 -0.0001 0.6794 0.018 Uiso 1 1 calc R . . H7B H 0.8065 -0.0889 0.5928 0.018 Uiso 1 1 calc R . . O8 O 0.9452(2) 0.01565(18) 0.56643(15) 0.0163(4) Uani 1 1 d . . . C9 C 0.6235(3) 0.2536(3) 0.3359(2) 0.0174(6) Uani 1 1 d . . . H9A H 0.7139 0.2852 0.3443 0.026 Uiso 1 1 calc R . . H9B H 0.5564 0.3138 0.3214 0.026 Uiso 1 1 calc R . . H9C H 0.6044 0.2000 0.2813 0.026 Uiso 1 1 calc R . . N11 N 0.8579(2) 0.10772(19) 0.28786(17) 0.0112(4) Uani 1 1 d . . . C12 C 0.7843(3) 0.0329(2) 0.2204(2) 0.0159(6) Uani 1 1 d . . . C13 C 0.7749(3) 0.0428(3) 0.1194(2) 0.0200(6) Uani 1 1 d . . . H13 H 0.7222 -0.0086 0.0737 0.024 Uiso 1 1 calc R . . C14 C 0.8451(3) 0.1302(3) 0.0870(2) 0.0202(6) Uani 1 1 d . . . H14 H 0.8418 0.1370 0.0193 0.024 Uiso 1 1 calc R . . C15 C 0.9198(3) 0.2073(3) 0.1555(2) 0.0189(6) Uani 1 1 d . . . H15 H 0.9663 0.2671 0.1344 0.023 Uiso 1 1 calc R . . C16 C 0.9248(3) 0.1942(2) 0.2565(2) 0.0133(5) Uani 1 1 d . . . C17 C 1.0064(3) 0.2769(2) 0.3330(2) 0.0170(6) Uani 1 1 d . . . H17A H 1.1027 0.2739 0.3327 0.020 Uiso 1 1 calc R . . H17B H 0.9732 0.3539 0.3154 0.020 Uiso 1 1 calc R . . O18 O 0.9937(3) 0.2498(2) 0.42942(17) 0.0254(5) Uani 1 1 d . . . C19 C 0.7116(3) -0.0602(3) 0.2628(2) 0.0219(6) Uani 1 1 d . . . H19A H 0.7723 -0.0896 0.3234 0.033 Uiso 1 1 calc R . . H19B H 0.6858 -0.1207 0.2145 0.033 Uiso 1 1 calc R . . H19C H 0.6306 -0.0293 0.2773 0.033 Uiso 1 1 calc R . . O1 O 0.8239(2) 0.51338(19) 0.36917(17) 0.0257(5) Uani 1 1 d . . . O2 O 0.7123(3) 0.6611(2) 0.26373(17) 0.0319(6) Uani 1 1 d . . . O3 O 0.7688(2) 0.6855(2) 0.43877(17) 0.0285(5) Uani 1 1 d . . . O4 O 0.5932(3) 0.5592(2) 0.3603(2) 0.0353(6) Uani 1 1 d . . . H18 H 1.082(6) 0.288(5) 0.484(4) 0.073(17) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.01212(18) 0.01761(19) 0.00853(18) 0.00425(13) 0.00427(13) 0.00533(13) Cl1 0.0172(3) 0.0143(3) 0.0132(3) -0.0013(2) 0.0029(3) 0.0010(2) N1 0.0129(11) 0.0116(11) 0.0111(11) -0.0004(9) 0.0028(9) 0.0006(9) C2 0.0142(13) 0.0131(13) 0.0136(13) 0.0019(10) 0.0022(11) 0.0024(10) C3 0.0142(13) 0.0186(14) 0.0183(15) 0.0039(11) 0.0030(11) 0.0061(11) C4 0.0156(14) 0.0245(15) 0.0227(16) 0.0008(12) 0.0114(12) 0.0045(12) C5 0.0172(14) 0.0170(14) 0.0159(14) 0.0033(11) 0.0079(11) 0.0029(11) C6 0.0143(13) 0.0134(13) 0.0111(13) -0.0012(10) 0.0033(10) 0.0007(10) C7 0.0168(14) 0.0183(14) 0.0113(13) 0.0055(10) 0.0072(11) 0.0051(11) O8 0.0141(10) 0.0239(11) 0.0124(10) 0.0082(8) 0.0063(8) 0.0082(8) C9 0.0154(13) 0.0189(14) 0.0180(14) 0.0060(11) 0.0048(11) 0.0069(11) N11 0.0127(11) 0.0109(11) 0.0097(11) 0.0009(8) 0.0026(9) 0.0029(8) C12 0.0162(14) 0.0128(13) 0.0165(14) -0.0004(11) 0.0004(11) 0.0022(10) C13 0.0244(15) 0.0199(15) 0.0133(14) -0.0065(11) 0.0006(12) -0.0001(12) C14 0.0265(16) 0.0225(15) 0.0115(14) 0.0025(11) 0.0050(12) 0.0071(12) C15 0.0218(15) 0.0172(14) 0.0204(15) 0.0051(12) 0.0101(12) 0.0024(12) C16 0.0139(13) 0.0134(13) 0.0134(13) 0.0024(10) 0.0049(10) 0.0034(10) C17 0.0178(14) 0.0159(14) 0.0176(14) 0.0025(11) 0.0050(11) -0.0020(11) O18 0.0286(12) 0.0258(12) 0.0213(12) -0.0014(9) 0.0058(10) -0.0037(10) C19 0.0220(16) 0.0181(15) 0.0258(16) -0.0032(12) 0.0067(13) -0.0046(12) O1 0.0305(13) 0.0192(11) 0.0279(13) 0.0044(9) 0.0089(10) 0.0101(9) O2 0.0477(16) 0.0298(13) 0.0193(12) 0.0089(10) 0.0106(11) 0.0134(11) O3 0.0226(12) 0.0337(13) 0.0240(12) -0.0160(10) -0.0029(9) 0.0033(10) O4 0.0213(12) 0.0322(14) 0.0531(17) -0.0036(12) 0.0107(12) -0.0068(10) _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 Cu1 O8 1.9051(19) . ? Cu1 O8 1.9542(19) 3_756 ? Cu1 N11 1.983(2) . ? Cu1 N1 2.029(2) . ? Cu1 O18 2.289(2) . ? Cu1 Cu1 3.0200(7) 3_756 ? Cl1 O4 1.430(3) . ? Cl1 O2 1.435(2) . ? Cl1 O1 1.435(2) . ? Cl1 O3 1.452(2) . ? N1 C6 1.356(3) . ? N1 C2 1.360(4) . ? C2 C3 1.389(4) . ? C2 C9 1.500(4) . ? C3 C4 1.386(4) . ? C4 C5 1.380(4) . ? C5 C6 1.386(4) . ? C6 C7 1.505(4) . ? C7 O8 1.406(3) . ? O8 Cu1 1.9542(19) 3_756 ? N11 C16 1.349(4) . ? N11 C12 1.349(4) . ? C12 C13 1.376(4) . ? C12 C19 1.513(4) . ? C13 C14 1.383(5) . ? C14 C15 1.378(4) . ? C15 C16 1.390(4) . ? C16 C17 1.506(4) . ? C17 O18 1.407(4) . ? 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 O8 Cu1 O8 77.02(9) . 3_756 ? O8 Cu1 N11 167.34(9) . . ? O8 Cu1 N11 91.53(9) 3_756 . ? O8 Cu1 N1 82.61(9) . . ? O8 Cu1 N1 156.54(9) 3_756 . ? N11 Cu1 N1 107.35(9) . . ? O8 Cu1 O18 109.76(9) . . ? O8 Cu1 O18 96.22(9) 3_756 . ? N11 Cu1 O18 76.46(9) . . ? N1 Cu1 O18 101.56(9) . . ? O8 Cu1 Cu1 39.09(6) . 3_756 ? O8 Cu1 Cu1 37.93(6) 3_756 3_756 ? N11 Cu1 Cu1 129.26(7) . 3_756 ? N1 Cu1 Cu1 120.83(7) . 3_756 ? O18 Cu1 Cu1 106.46(6) . 3_756 ? O4 Cl1 O2 109.57(17) . . ? O4 Cl1 O1 110.47(15) . . ? O2 Cl1 O1 109.75(14) . . ? O4 Cl1 O3 108.53(16) . . ? O2 Cl1 O3 108.85(15) . . ? O1 Cl1 O3 109.63(14) . . ? C6 N1 C2 118.7(2) . . ? C6 N1 Cu1 110.87(18) . . ? C2 N1 Cu1 130.29(19) . . ? N1 C2 C3 120.7(3) . . ? N1 C2 C9 118.6(2) . . ? C3 C2 C9 120.7(2) . . ? C4 C3 C2 120.2(3) . . ? C5 C4 C3 119.1(3) . . ? C4 C5 C6 118.7(3) . . ? N1 C6 C5 122.5(3) . . ? N1 C6 C7 116.2(2) . . ? C5 C6 C7 121.3(2) . . ? O8 C7 C6 109.0(2) . . ? C7 O8 Cu1 114.37(16) . . ? C7 O8 Cu1 129.36(17) . 3_756 ? Cu1 O8 Cu1 102.98(9) . 3_756 ? C16 N11 C12 119.7(2) . . ? C16 N11 Cu1 119.95(19) . . ? C12 N11 Cu1 119.55(19) . . ? N11 C12 C13 121.5(3) . . ? N11 C12 C19 115.7(3) . . ? C13 C12 C19 122.7(3) . . ? C12 C13 C14 119.0(3) . . ? C15 C14 C13 119.8(3) . . ? C14 C15 C16 119.0(3) . . ? N11 C16 C15 121.0(3) . . ? N11 C16 C17 118.9(2) . . ? C15 C16 C17 120.0(3) . . ? O18 C17 C16 110.5(2) . . ? C17 O18 Cu1 112.10(18) . . ? _diffrn_measured_fraction_theta_max 0.959 _diffrn_reflns_theta_full 27.90 _diffrn_measured_fraction_theta_full 0.959 _refine_diff_density_max 1.758 _refine_diff_density_min -0.683 _refine_diff_density_rms 0.105 #END data_[Cu(2)2Cl]Cl.H2O _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H24 Cl2 Cu N2 O3' _chemical_formula_weight 426.81 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' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 9.1495(8) _cell_length_b 8.6211(7) _cell_length_c 12.9070(11) _cell_angle_alpha 90.00 _cell_angle_beta 97.6750(10) _cell_angle_gamma 90.00 _cell_volume 1008.97(15) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 6093 _cell_measurement_theta_min 1.59 _cell_measurement_theta_max 27.87 _exptl_crystal_description plate _exptl_crystal_colour blue-green _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.405 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 442 _exptl_absorpt_coefficient_mu 1.362 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.887348 _exptl_absorpt_correction_T_max 1 _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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 APEX' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6093 _diffrn_reflns_av_R_equivalents 0.0227 _diffrn_reflns_av_sigmaI/netI 0.0473 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 27.87 _reflns_number_total 3286 _reflns_number_gt 3026 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _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^)+(0.0214P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.015(9) _refine_ls_number_reflns 3286 _refine_ls_number_parameters 237 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0296 _refine_ls_R_factor_gt 0.0260 _refine_ls_wR_factor_ref 0.0551 _refine_ls_wR_factor_gt 0.0544 _refine_ls_goodness_of_fit_ref 0.986 _refine_ls_restrained_S_all 0.986 _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 Cu1 Cu 0.25587(3) 0.25479(3) 0.22326(2) 0.01431(8) Uani 1 1 d . . . N1 N 0.0396(2) 0.2480(3) 0.17036(15) 0.0150(4) Uani 1 1 d . . . Cl1 Cl 0.33533(8) 0.16479(9) 0.07666(6) 0.02611(17) Uani 1 1 d . . . C2 C -0.0324(3) 0.3383(3) 0.0950(2) 0.0204(6) Uani 1 1 d . . . C3 C -0.1835(3) 0.3241(4) 0.0665(2) 0.0258(7) Uani 1 1 d . . . H3 H -0.2326 0.3891 0.0158 0.031 Uiso 1 1 calc R . . C4 C -0.2604(3) 0.2127(3) 0.1141(2) 0.0282(7) Uani 1 1 d . . . H4 H -0.3615 0.2013 0.0950 0.034 Uiso 1 1 calc R . . C5 C -0.1865(3) 0.1189(3) 0.1897(2) 0.0215(6) Uani 1 1 d . . . H5 H -0.2364 0.0422 0.2216 0.026 Uiso 1 1 calc R . . C6 C -0.0364(3) 0.1406(3) 0.2174(2) 0.0163(6) Uani 1 1 d . . . C7 C 0.0505(3) 0.0392(3) 0.2982(2) 0.0175(6) Uani 1 1 d . . . H7 H -0.0092 0.0164 0.3540 0.021 Uiso 1 1 calc R . . C8 C 0.0939(3) -0.1115(3) 0.2501(2) 0.0246(7) Uani 1 1 d . . . H8A H 0.1535 -0.0895 0.1961 0.037 Uiso 1 1 calc R . . H8B H 0.0067 -0.1662 0.2207 0.037 Uiso 1 1 calc R . . H8C H 0.1490 -0.1743 0.3030 0.037 Uiso 1 1 calc R . . O9 O 0.1827(2) 0.1184(2) 0.34155(16) 0.0169(4) Uani 1 1 d . . . C10 C 0.0533(3) 0.4558(4) 0.0426(3) 0.0314(8) Uani 1 1 d . . . H10A H 0.1000 0.5270 0.0939 0.047 Uiso 1 1 calc R . . H10B H -0.0122 0.5116 -0.0085 0.047 Uiso 1 1 calc R . . H10C H 0.1271 0.4041 0.0090 0.047 Uiso 1 1 calc R . . N12 N 0.4531(2) 0.2745(3) 0.31211(16) 0.0158(4) Uani 1 1 d . . . C13 C 0.5397(3) 0.1548(3) 0.3515(2) 0.0191(6) Uani 1 1 d . . . C14 C 0.6670(3) 0.1830(4) 0.4197(3) 0.0249(7) Uani 1 1 d . . . H14 H 0.7246 0.1005 0.4479 0.030 Uiso 1 1 calc R . . C15 C 0.7083(3) 0.3333(4) 0.4460(3) 0.0280(7) Uani 1 1 d . . . H15 H 0.7946 0.3526 0.4909 0.034 Uiso 1 1 calc R . . C16 C 0.6214(3) 0.4544(4) 0.4053(2) 0.0259(7) Uani 1 1 d . . . H16 H 0.6478 0.5564 0.4222 0.031 Uiso 1 1 calc R . . C17 C 0.4937(3) 0.4217(3) 0.3387(2) 0.0181(6) Uani 1 1 d . . . C18 C 0.3970(3) 0.5494(3) 0.2871(2) 0.0213(6) Uani 1 1 d . . . H18 H 0.3927 0.6345 0.3369 0.026 Uiso 1 1 calc R . . C19 C 0.4572(3) 0.6103(4) 0.1905(3) 0.0318(8) Uani 1 1 d . . . H19A H 0.4561 0.5287 0.1398 0.048 Uiso 1 1 calc R . . H19B H 0.5566 0.6458 0.2097 0.048 Uiso 1 1 calc R . . H19C H 0.3970 0.6947 0.1612 0.048 Uiso 1 1 calc R . . O20 O 0.2521(2) 0.4925(2) 0.25541(16) 0.0194(4) Uani 1 1 d . . . C21 C 0.4952(3) -0.0066(3) 0.3192(2) 0.0228(6) Uani 1 1 d . . . H21A H 0.4157 -0.0394 0.3556 0.034 Uiso 1 1 calc R . . H21B H 0.5778 -0.0751 0.3359 0.034 Uiso 1 1 calc R . . H21C H 0.4637 -0.0091 0.2452 0.034 Uiso 1 1 calc R . . Cl98 Cl 0.85709(7) 0.78633(7) 0.45943(5) 0.02125(16) Uani 1 1 d . . . O99 O 0.0548(3) 0.5350(3) 0.3740(2) 0.0417(7) Uani 1 1 d . . . H9 H 0.160(4) 0.163(5) 0.388(3) 0.048(13) Uiso 1 1 d . . . H20 H 0.201(3) 0.514(4) 0.298(3) 0.032(10) Uiso 1 1 d . . . H99A H 0.056(4) 0.474(5) 0.422(3) 0.040(11) Uiso 1 1 d . . . H99B H 0.014(5) 0.587(5) 0.390(4) 0.054(16) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.01233(15) 0.01354(15) 0.01697(15) -0.00044(14) 0.00158(11) -0.00151(15) N1 0.0127(10) 0.0142(10) 0.0187(10) 0.0012(11) 0.0038(8) 0.0006(11) Cl1 0.0173(4) 0.0386(4) 0.0233(4) -0.0117(3) 0.0057(3) -0.0051(3) C2 0.0216(15) 0.0206(15) 0.0185(15) 0.0019(11) 0.0012(12) 0.0039(12) C3 0.0194(16) 0.0293(17) 0.0268(18) 0.0019(13) -0.0037(13) 0.0067(13) C4 0.0145(14) 0.040(2) 0.0295(17) -0.0037(13) 0.0013(12) 0.0014(13) C5 0.0142(14) 0.0253(16) 0.0264(16) -0.0020(12) 0.0078(12) -0.0035(12) C6 0.0166(14) 0.0150(13) 0.0182(14) -0.0043(10) 0.0057(11) -0.0017(10) C7 0.0180(14) 0.0171(14) 0.0185(15) 0.0011(11) 0.0057(12) -0.0046(11) C8 0.0298(16) 0.0146(15) 0.0283(17) 0.0018(12) 0.0000(13) -0.0061(13) O9 0.0160(10) 0.0184(10) 0.0163(10) 0.0001(8) 0.0024(8) -0.0011(8) C10 0.0304(18) 0.0301(18) 0.0314(19) 0.0139(14) -0.0049(14) -0.0034(14) N12 0.0135(10) 0.0162(12) 0.0182(11) 0.0008(10) 0.0036(8) -0.0004(10) C13 0.0154(14) 0.0223(15) 0.0205(15) -0.0007(12) 0.0061(12) 0.0004(11) C14 0.0197(16) 0.0319(17) 0.0230(17) -0.0009(13) 0.0026(13) 0.0028(14) C15 0.0179(16) 0.0384(19) 0.0261(18) -0.0059(14) -0.0030(13) -0.0025(14) C16 0.0194(16) 0.0276(16) 0.0298(18) -0.0086(13) -0.0003(13) -0.0083(13) C17 0.0183(15) 0.0189(15) 0.0182(15) -0.0040(11) 0.0064(12) -0.0039(11) C18 0.0210(15) 0.0158(14) 0.0262(16) -0.0056(11) -0.0005(12) -0.0060(12) C19 0.0319(18) 0.0237(17) 0.041(2) 0.0055(14) 0.0088(15) -0.0069(14) O20 0.0169(11) 0.0159(10) 0.0255(11) -0.0036(8) 0.0028(9) -0.0002(8) C21 0.0191(15) 0.0166(14) 0.0326(17) 0.0012(12) 0.0034(13) 0.0029(12) Cl98 0.0252(3) 0.0147(4) 0.0249(4) 0.0014(2) 0.0073(3) -0.0007(3) O99 0.0510(17) 0.0326(15) 0.0482(18) 0.0183(14) 0.0307(14) 0.0206(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N1 2.0059(19) . ? Cu1 N12 2.012(2) . ? Cu1 O20 2.092(2) . ? Cu1 O9 2.1059(19) . ? Cu1 Cl1 2.2534(7) . ? N1 C2 1.347(3) . ? N1 C6 1.350(3) . ? C2 C3 1.387(4) . ? C2 C10 1.497(4) . ? C3 C4 1.383(4) . ? C4 C5 1.374(4) . ? C5 C6 1.386(4) . ? C6 C7 1.503(4) . ? C7 O9 1.436(3) . ? C7 C8 1.516(4) . ? N12 C17 1.353(3) . ? N12 C13 1.358(4) . ? C13 C14 1.385(4) . ? C13 C21 1.493(4) . ? C14 C15 1.380(4) . ? C15 C16 1.374(4) . ? C16 C17 1.384(4) . ? C17 C18 1.511(4) . ? C18 O20 1.422(3) . ? C18 C19 1.522(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cu1 N12 164.86(8) . . ? N1 Cu1 O20 93.11(9) . . ? N12 Cu1 O20 80.88(9) . . ? N1 Cu1 O9 80.56(8) . . ? N12 Cu1 O9 88.94(8) . . ? O20 Cu1 O9 112.82(8) . . ? N1 Cu1 Cl1 96.80(6) . . ? N12 Cu1 Cl1 98.19(6) . . ? O20 Cu1 Cl1 121.30(6) . . ? O9 Cu1 Cl1 125.87(6) . . ? C2 N1 C6 119.3(2) . . ? C2 N1 Cu1 126.46(18) . . ? C6 N1 Cu1 114.23(18) . . ? N1 C2 C3 121.0(3) . . ? N1 C2 C10 118.8(2) . . ? C3 C2 C10 120.2(3) . . ? C4 C3 C2 119.4(3) . . ? C5 C4 C3 119.5(3) . . ? C4 C5 C6 118.8(3) . . ? N1 C6 C5 121.9(3) . . ? N1 C6 C7 117.1(2) . . ? C5 C6 C7 121.0(2) . . ? O9 C7 C6 109.5(2) . . ? O9 C7 C8 108.3(2) . . ? C6 C7 C8 111.0(2) . . ? C7 O9 Cu1 108.40(16) . . ? C17 N12 C13 119.4(2) . . ? C17 N12 Cu1 114.77(18) . . ? C13 N12 Cu1 125.69(19) . . ? N12 C13 C14 120.3(3) . . ? N12 C13 C21 118.7(2) . . ? C14 C13 C21 121.0(3) . . ? C15 C14 C13 120.1(3) . . ? C16 C15 C14 119.6(3) . . ? C15 C16 C17 118.7(3) . . ? N12 C17 C16 122.0(3) . . ? N12 C17 C18 116.5(2) . . ? C16 C17 C18 121.4(3) . . ? O20 C18 C17 110.1(2) . . ? O20 C18 C19 108.0(2) . . ? C17 C18 C19 110.9(2) . . ? C18 O20 Cu1 110.85(16) . . ? _diffrn_measured_fraction_theta_max 0.933 _diffrn_reflns_theta_full 27.87 _diffrn_measured_fraction_theta_full 0.933 _refine_diff_density_max 0.503 _refine_diff_density_min -0.206 _refine_diff_density_rms 0.059 #END data_[Cu2(2)3(2-H)Br2]Br.2(H2O) _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H47 Br3 Cu2 N4 O6' _chemical_formula_weight 950.5505 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' '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 P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 10.5843(3) _cell_length_b 16.3320(4) _cell_length_c 11.9571(3) _cell_angle_alpha 90.00 _cell_angle_beta 115.0370(10) _cell_angle_gamma 90.00 _cell_volume 1872.72(8) _cell_formula_units_Z 2 _cell_measurement_temperature 199(2) _cell_measurement_reflns_used 9999 _cell_measurement_theta_min 1.88 _cell_measurement_theta_max 29.60 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.41 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.686 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 956 _exptl_absorpt_coefficient_mu 4.382 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.2605 _exptl_absorpt_correction_T_max 0.4597 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 199(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33306 _diffrn_reflns_av_R_equivalents 0.0412 _diffrn_reflns_av_sigmaI/netI 0.0457 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 29.60 _reflns_number_total 10494 _reflns_number_gt 9402 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0373P)^2^+0.0572P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.024(6) _refine_ls_number_reflns 10494 _refine_ls_number_parameters 440 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0345 _refine_ls_R_factor_gt 0.0292 _refine_ls_wR_factor_ref 0.0770 _refine_ls_wR_factor_gt 0.0709 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.65939(3) 0.162617(18) 0.85505(3) 0.02240(7) Uani 1 1 d . . . Cu2 Cu 0.14062(3) 0.32035(2) 0.63592(3) 0.02475(7) Uani 1 1 d . . . Br1 Br 0.87615(3) 0.09679(2) 0.88447(4) 0.04030(8) Uani 1 1 d . . . Br2 Br -0.10793(3) 0.30269(2) 0.50319(3) 0.03882(8) Uani 1 1 d . . . Br3 Br 0.47665(4) 0.563594(19) 0.79988(3) 0.03924(8) Uani 1 1 d . . . O1 O 0.5523(3) 0.09008(14) 0.9430(2) 0.0324(5) Uani 1 1 d . . . O2 O 0.52528(18) 0.24884(11) 0.76574(18) 0.0228(4) Uani 1 1 d . . . O3 O 0.2871(2) 0.24543(13) 0.7413(2) 0.0286(4) Uani 1 1 d . . . O4 O 0.2232(3) 0.44272(16) 0.6332(3) 0.0384(6) Uani 1 1 d . . . N3 N 0.1162(2) 0.33658(14) 0.7905(2) 0.0260(5) Uani 1 1 d . . . C15 C 0.6856(3) 0.32594(16) 0.9381(3) 0.0236(5) Uani 1 1 d . . . C14 C 0.7312(3) 0.39654(18) 1.0076(3) 0.0310(6) Uani 1 1 d . . . H14 H 0.6987 0.4486 0.9714 0.037 Uiso 1 1 calc R . . N1 N 0.5455(2) 0.08263(14) 0.7203(2) 0.0260(5) Uani 1 1 d . . . C10 C 0.8215(3) 0.24435(19) 1.1066(3) 0.0293(6) Uani 1 1 d . . . C21 C 0.0801(4) 0.3303(2) 1.0053(3) 0.0444(8) Uani 1 1 d . . . H21 H 0.0651 0.3275 1.0781 0.053 Uiso 1 1 calc R . . C11 C 0.8656(4) 0.1614(2) 1.1623(3) 0.0403(7) Uani 1 1 d . . . H11A H 0.8295 0.1197 1.0974 0.060 Uiso 1 1 calc R . . H11B H 0.8285 0.1515 1.2236 0.060 Uiso 1 1 calc R . . H11C H 0.9676 0.1585 1.2024 0.060 Uiso 1 1 calc R . . C23 C 0.1778(3) 0.27746(18) 0.8736(3) 0.0272(6) Uani 1 1 d . . . N4 N 0.2004(2) 0.31079(16) 0.4975(2) 0.0280(5) Uani 1 1 d . . . N2 N 0.7327(2) 0.25119(14) 0.9849(2) 0.0244(5) Uani 1 1 d . . . C6 C 0.3913(3) -0.03269(18) 0.6634(3) 0.0334(7) Uani 1 1 d . . . H6 H 0.3436 -0.0740 0.6863 0.040 Uiso 1 1 calc R . . C22 C 0.1608(4) 0.2721(2) 0.9828(3) 0.0374(7) Uani 1 1 d . . . H22 H 0.2037 0.2293 1.0402 0.045 Uiso 1 1 calc R . . C2 C 0.5298(3) 0.08898(18) 0.6015(3) 0.0288(6) Uani 1 1 d . . . C7 C 0.4797(3) 0.02231(16) 0.7511(3) 0.0258(5) Uani 1 1 d . . . C5 C 0.3746(3) -0.0260(2) 0.5429(3) 0.0360(7) Uani 1 1 d . . . H5 H 0.3157 -0.0628 0.4814 0.043 Uiso 1 1 calc R . . C30 C 0.2912(4) 0.3795(3) 0.3719(3) 0.0447(8) Uani 1 1 d . . . H30 H 0.3163 0.4292 0.3451 0.054 Uiso 1 1 calc R . . C31 C 0.2404(3) 0.3801(2) 0.4614(3) 0.0328(6) Uani 1 1 d . . . C16 C 0.5793(3) 0.32877(15) 0.8035(3) 0.0241(5) Uani 1 1 d . . . H16 H 0.5008 0.3653 0.7973 0.029 Uiso 1 1 calc R . . C18 C 0.0406(3) 0.39544(18) 0.8146(3) 0.0306(6) Uani 1 1 d . . . C24 C 0.2637(3) 0.21550(18) 0.8408(3) 0.0308(6) Uani 1 1 d . . . H24 H 0.3550 0.2065 0.9135 0.037 Uiso 1 1 calc R . . C29 C 0.3047(4) 0.3060(3) 0.3227(3) 0.0522(10) Uani 1 1 d . . . H29 H 0.3447 0.3039 0.2651 0.063 Uiso 1 1 calc R . . C20 C 0.0222(3) 0.3919(2) 0.9226(3) 0.0385(7) Uani 1 1 d . . . H20 H -0.0314 0.4329 0.9391 0.046 Uiso 1 1 calc R . . C33 C 0.0950(5) 0.5066(3) 0.4379(4) 0.0580(11) Uani 1 1 d . . . H33A H 0.0919 0.5578 0.4795 0.087 Uiso 1 1 calc R . . H33B H 0.0128 0.4735 0.4249 0.087 Uiso 1 1 calc R . . H33C H 0.0959 0.5191 0.3581 0.087 Uiso 1 1 calc R . . C32 C 0.2259(4) 0.4595(2) 0.5173(3) 0.0367(7) Uani 1 1 d . . . H32 H 0.3089 0.4944 0.5316 0.044 Uiso 1 1 calc R . . C13 C 0.8248(4) 0.3905(2) 1.1309(3) 0.0379(7) Uani 1 1 d . . . H13 H 0.8576 0.4382 1.1805 0.046 Uiso 1 1 calc R . . C8 C 0.5035(3) 0.01362(17) 0.8838(3) 0.0282(6) Uani 1 1 d . . . H8 H 0.4125 0.0007 0.8867 0.034 Uiso 1 1 calc R . . C19 C -0.0184(4) 0.4640(2) 0.7230(4) 0.0406(8) Uani 1 1 d . . . H19A H 0.0581 0.4971 0.7214 0.061 Uiso 1 1 calc R . . H19B H -0.0785 0.4984 0.7472 0.061 Uiso 1 1 calc R . . H19C H -0.0731 0.4411 0.6408 0.061 Uiso 1 1 calc R . . C9 C 0.6062(4) -0.0557(2) 0.9467(4) 0.0441(8) Uani 1 1 d . . . H9A H 0.6978 -0.0417 0.9502 0.066 Uiso 1 1 calc R . . H9B H 0.5726 -0.1064 0.8996 0.066 Uiso 1 1 calc R . . H9C H 0.6140 -0.0634 1.0307 0.066 Uiso 1 1 calc R . . C28 C 0.2602(4) 0.2353(3) 0.3570(3) 0.0445(8) Uani 1 1 d . . . H28 H 0.2656 0.1845 0.3207 0.053 Uiso 1 1 calc R . . C17 C 0.6415(4) 0.3625(2) 0.7197(3) 0.0383(7) Uani 1 1 d . . . H17A H 0.7219 0.3291 0.7279 0.057 Uiso 1 1 calc R . . H17B H 0.6716 0.4192 0.7431 0.057 Uiso 1 1 calc R . . H17C H 0.5712 0.3611 0.6339 0.057 Uiso 1 1 calc R . . C25 C 0.1832(4) 0.1341(2) 0.8036(4) 0.0465(9) Uani 1 1 d . . . H25A H 0.0886 0.1445 0.7406 0.070 Uiso 1 1 calc R . . H25B H 0.1784 0.1091 0.8762 0.070 Uiso 1 1 calc R . . H25C H 0.2314 0.0969 0.7703 0.070 Uiso 1 1 calc R . . C27 C 0.1583(4) 0.1623(2) 0.4850(3) 0.0422(8) Uani 1 1 d . . . H27A H 0.2254 0.1471 0.5684 0.063 Uiso 1 1 calc R . . H27B H 0.1503 0.1175 0.4278 0.063 Uiso 1 1 calc R . . H27C H 0.0670 0.1725 0.4850 0.063 Uiso 1 1 calc R . . C12 C 0.8692(3) 0.3133(2) 1.1800(3) 0.0349(6) Uani 1 1 d . . . H12 H 0.9326 0.3076 1.2644 0.042 Uiso 1 1 calc R . . C26 C 0.2076(3) 0.2386(2) 0.4447(3) 0.0323(6) Uani 1 1 d . . . C4 C 0.4449(3) 0.0350(2) 0.5139(3) 0.0346(7) Uani 1 1 d . . . H4 H 0.4347 0.0400 0.4313 0.041 Uiso 1 1 calc R . . C3 C 0.6060(4) 0.1552(2) 0.5705(3) 0.0372(7) Uani 1 1 d . . . H3A H 0.5613 0.2080 0.5694 0.056 Uiso 1 1 calc R . . H3B H 0.6039 0.1447 0.4891 0.056 Uiso 1 1 calc R . . H3C H 0.7029 0.1567 0.6327 0.056 Uiso 1 1 calc R . . O99 O -0.4252(4) 0.2657(2) 0.2432(5) 0.0874(12) Uani 1 1 d . . . O98 O 0.8112(5) 0.5821(3) 0.8481(5) 0.1083(15) Uani 1 1 d . . . H80 H 0.269(4) 0.461(2) 0.670(3) 0.010(9) Uiso 1 1 d . . . H81 H 0.558(4) 0.090(2) 0.996(4) 0.023(11) Uiso 1 1 d . . . H101 H 0.4060 0.2470 0.7530 0.089(17) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.01999(14) 0.02201(14) 0.02436(16) 0.00130(13) 0.00856(13) 0.00106(11) Cu2 0.02064(14) 0.03010(16) 0.02233(16) 0.00156(13) 0.00795(13) 0.00130(12) Br1 0.02526(14) 0.04711(18) 0.0488(2) 0.00026(15) 0.01597(14) 0.00789(12) Br2 0.02232(13) 0.0563(2) 0.03133(16) -0.00484(14) 0.00510(12) 0.00116(12) Br3 0.04795(19) 0.03873(16) 0.03002(16) -0.00145(13) 0.01552(14) 0.00236(13) O1 0.0464(14) 0.0297(10) 0.0285(12) -0.0012(9) 0.0229(11) -0.0061(9) O2 0.0166(8) 0.0246(9) 0.0245(10) 0.0014(7) 0.0060(8) -0.0002(7) O3 0.0202(9) 0.0376(10) 0.0283(10) 0.0081(8) 0.0105(8) 0.0033(7) O4 0.0455(15) 0.0401(13) 0.0283(13) -0.0015(11) 0.0144(12) -0.0137(12) N3 0.0198(10) 0.0312(12) 0.0256(12) -0.0032(9) 0.0083(9) -0.0034(8) C15 0.0226(11) 0.0257(12) 0.0261(13) 0.0016(10) 0.0137(11) 0.0003(9) C14 0.0343(15) 0.0273(13) 0.0314(16) -0.0013(11) 0.0139(13) 0.0038(11) N1 0.0242(11) 0.0257(11) 0.0285(12) 0.0013(9) 0.0116(10) 0.0015(8) C10 0.0235(13) 0.0392(15) 0.0247(14) 0.0059(12) 0.0095(11) 0.0018(11) C21 0.0436(18) 0.061(2) 0.0369(18) -0.0126(16) 0.0249(16) -0.0131(16) C11 0.0417(18) 0.0393(16) 0.0304(16) 0.0127(14) 0.0061(14) 0.0071(14) C23 0.0197(12) 0.0328(13) 0.0264(14) -0.0009(11) 0.0072(11) -0.0062(10) N4 0.0231(10) 0.0355(12) 0.0219(11) 0.0023(10) 0.0062(9) 0.0000(9) N2 0.0231(11) 0.0266(11) 0.0225(11) 0.0025(9) 0.0087(9) 0.0000(8) C6 0.0317(15) 0.0290(14) 0.0387(18) -0.0048(12) 0.0140(14) -0.0042(11) C22 0.0385(17) 0.0439(17) 0.0313(17) 0.0024(13) 0.0164(14) -0.0047(13) C2 0.0286(14) 0.0310(13) 0.0288(14) 0.0012(11) 0.0141(12) 0.0057(11) C7 0.0253(13) 0.0227(12) 0.0308(15) -0.0001(11) 0.0131(12) 0.0014(10) C5 0.0328(16) 0.0373(15) 0.0357(17) -0.0132(13) 0.0124(14) -0.0034(12) C30 0.0413(19) 0.065(2) 0.0320(18) -0.0005(16) 0.0193(16) -0.0143(16) C31 0.0253(14) 0.0449(16) 0.0240(15) 0.0039(12) 0.0063(12) -0.0072(12) C16 0.0236(12) 0.0213(11) 0.0251(13) 0.0018(10) 0.0082(10) 0.0007(9) C18 0.0230(13) 0.0308(14) 0.0369(17) -0.0067(12) 0.0117(12) -0.0057(11) C24 0.0257(14) 0.0364(15) 0.0306(16) 0.0078(12) 0.0122(12) 0.0038(11) C29 0.046(2) 0.085(3) 0.0327(17) -0.009(2) 0.0237(16) -0.008(2) C20 0.0308(15) 0.0439(17) 0.045(2) -0.0136(15) 0.0194(15) -0.0058(13) C33 0.069(3) 0.055(2) 0.042(2) 0.0152(18) 0.017(2) 0.011(2) C32 0.0386(17) 0.0433(17) 0.0289(16) 0.0029(13) 0.0151(14) -0.0098(13) C13 0.0397(18) 0.0399(17) 0.0339(17) -0.0126(13) 0.0152(15) 0.0000(13) C8 0.0296(14) 0.0249(12) 0.0324(16) 0.0047(11) 0.0153(13) -0.0011(10) C19 0.0383(18) 0.0315(15) 0.048(2) -0.0052(14) 0.0140(16) 0.0050(12) C9 0.048(2) 0.0348(16) 0.046(2) 0.0087(15) 0.0169(17) 0.0122(14) C28 0.0388(19) 0.061(2) 0.0304(17) -0.0062(16) 0.0115(15) 0.0073(16) C17 0.0429(18) 0.0411(17) 0.0270(16) 0.0053(13) 0.0109(14) -0.0134(14) C25 0.056(2) 0.0271(14) 0.073(3) 0.0041(16) 0.044(2) 0.0008(14) C27 0.051(2) 0.0325(14) 0.0380(18) -0.0036(14) 0.0138(16) 0.0063(15) C12 0.0324(14) 0.0503(18) 0.0209(13) -0.0011(14) 0.0101(12) 0.0027(13) C26 0.0234(13) 0.0425(16) 0.0238(14) 0.0005(12) 0.0030(12) 0.0066(11) C4 0.0351(16) 0.0436(17) 0.0246(15) -0.0049(13) 0.0122(13) 0.0053(13) C3 0.0491(18) 0.0404(16) 0.0296(15) 0.0010(13) 0.0239(14) -0.0018(14) O99 0.085(3) 0.0517(19) 0.121(4) -0.001(2) 0.039(3) 0.0042(17) O98 0.108(3) 0.112(4) 0.115(4) -0.003(3) 0.058(3) -0.003(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 Cu1 O2 1.9635(18) . ? Cu1 N2 2.021(2) . ? Cu1 N1 2.027(2) . ? Cu1 O1 2.191(2) . ? Cu1 Br1 2.4208(4) . ? Cu2 O3 1.958(2) . ? Cu2 N3 1.989(2) . ? Cu2 N4 2.013(2) . ? Cu2 O4 2.187(3) . ? Cu2 Br2 2.4472(4) . ? O1 C8 1.420(4) . ? O2 C16 1.420(3) . ? O3 C24 1.401(4) . ? O4 C32 1.424(4) . ? N3 C23 1.341(4) . ? N3 C18 1.358(4) . ? C15 N2 1.347(3) . ? C15 C14 1.383(4) . ? C15 C16 1.525(4) . ? C14 C13 1.389(5) . ? N1 C7 1.345(4) . ? N1 C2 1.363(4) . ? C10 N2 1.363(4) . ? C10 C12 1.385(5) . ? C10 C11 1.495(4) . ? C21 C20 1.361(6) . ? C21 C22 1.379(5) . ? C23 C22 1.394(5) . ? C23 C24 1.519(4) . ? N4 C31 1.342(4) . ? N4 C26 1.355(4) . ? C6 C5 1.379(5) . ? C6 C7 1.397(4) . ? C2 C4 1.373(4) . ? C2 C3 1.487(4) . ? C7 C8 1.505(4) . ? C5 C4 1.374(5) . ? C30 C29 1.371(6) . ? C30 C31 1.387(5) . ? C31 C32 1.496(5) . ? C16 C17 1.516(4) . ? C18 C20 1.386(5) . ? C18 C19 1.504(5) . ? C24 C25 1.540(5) . ? C29 C28 1.373(6) . ? C33 C32 1.516(5) . ? C13 C12 1.387(5) . ? C8 C9 1.528(4) . ? C28 C26 1.381(5) . ? C27 C26 1.507(5) . ? 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 O2 Cu1 N2 81.86(9) . . ? O2 Cu1 N1 88.86(9) . . ? N2 Cu1 N1 167.74(9) . . ? O2 Cu1 O1 104.30(9) . . ? N2 Cu1 O1 97.28(9) . . ? N1 Cu1 O1 77.19(10) . . ? O2 Cu1 Br1 145.10(6) . . ? N2 Cu1 Br1 100.04(7) . . ? N1 Cu1 Br1 92.16(7) . . ? O1 Cu1 Br1 109.94(7) . . ? O3 Cu2 N3 82.20(9) . . ? O3 Cu2 N4 92.41(9) . . ? N3 Cu2 N4 169.77(9) . . ? O3 Cu2 O4 111.60(10) . . ? N3 Cu2 O4 95.87(10) . . ? N4 Cu2 O4 77.98(10) . . ? O3 Cu2 Br2 133.20(6) . . ? N3 Cu2 Br2 95.24(7) . . ? N4 Cu2 Br2 94.78(7) . . ? O4 Cu2 Br2 115.14(8) . . ? C8 O1 Cu1 112.93(19) . . ? C16 O2 Cu1 112.66(15) . . ? C24 O3 Cu2 112.84(17) . . ? C32 O4 Cu2 111.3(2) . . ? C23 N3 C18 119.9(3) . . ? C23 N3 Cu2 112.3(2) . . ? C18 N3 Cu2 127.7(2) . . ? N2 C15 C14 122.2(3) . . ? N2 C15 C16 116.3(2) . . ? C14 C15 C16 121.5(2) . . ? C15 C14 C13 119.3(3) . . ? C7 N1 C2 119.5(3) . . ? C7 N1 Cu1 117.2(2) . . ? C2 N1 Cu1 123.26(19) . . ? N2 C10 C12 120.8(3) . . ? N2 C10 C11 119.6(3) . . ? C12 C10 C11 119.5(3) . . ? C20 C21 C22 119.6(3) . . ? N3 C23 C22 121.6(3) . . ? N3 C23 C24 116.4(3) . . ? C22 C23 C24 121.9(3) . . ? C31 N4 C26 119.8(3) . . ? C31 N4 Cu2 116.8(2) . . ? C26 N4 Cu2 123.3(2) . . ? C15 N2 C10 119.0(3) . . ? C15 N2 Cu1 112.05(19) . . ? C10 N2 Cu1 129.0(2) . . ? C5 C6 C7 118.9(3) . . ? C21 C22 C23 118.4(3) . . ? N1 C2 C4 119.9(3) . . ? N1 C2 C3 118.4(3) . . ? C4 C2 C3 121.8(3) . . ? N1 C7 C6 121.7(3) . . ? N1 C7 C8 118.9(3) . . ? C6 C7 C8 119.4(3) . . ? C4 C5 C6 118.5(3) . . ? C29 C30 C31 118.8(3) . . ? N4 C31 C30 121.4(3) . . ? N4 C31 C32 118.8(3) . . ? C30 C31 C32 119.9(3) . . ? O2 C16 C17 110.7(2) . . ? O2 C16 C15 109.0(2) . . ? C17 C16 C15 112.1(2) . . ? N3 C18 C20 119.8(3) . . ? N3 C18 C19 118.2(3) . . ? C20 C18 C19 122.0(3) . . ? O3 C24 C23 109.1(2) . . ? O3 C24 C25 109.3(3) . . ? C23 C24 C25 109.4(2) . . ? C30 C29 C28 119.8(3) . . ? C21 C20 C18 120.6(3) . . ? O4 C32 C31 108.4(3) . . ? O4 C32 C33 108.5(3) . . ? C31 C32 C33 113.5(3) . . ? C12 C13 C14 118.4(3) . . ? O1 C8 C7 107.8(2) . . ? O1 C8 C9 111.9(3) . . ? C7 C8 C9 110.8(3) . . ? C29 C28 C26 119.6(4) . . ? C10 C12 C13 120.2(3) . . ? N4 C26 C28 120.5(3) . . ? N4 C26 C27 118.4(3) . . ? C28 C26 C27 121.1(3) . . ? C2 C4 C5 121.6(3) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 29.60 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.950 _refine_diff_density_min -0.519 _refine_diff_density_rms 0.088 #END data_[Zn(1-H)Cl] _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C7 H8 Cl N O Zn' _chemical_formula_weight 222.96 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zn' 'Zn' 0.2839 1.4301 '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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 5.0670(6) _cell_length_b 9.1795(10) _cell_length_c 18.293(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 850.83(17) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 5197 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 27.92 _exptl_crystal_description colourless _exptl_crystal_colour needle _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.741 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 448 _exptl_absorpt_coefficient_mu 3.138 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.2546 _exptl_absorpt_correction_T_max 0.8589 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5197 _diffrn_reflns_av_R_equivalents 0.0296 _diffrn_reflns_av_sigmaI/netI 0.0328 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.23 _diffrn_reflns_theta_max 27.92 _reflns_number_total 1938 _reflns_number_gt 1832 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0516P)^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 fixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.494(16) _refine_ls_number_reflns 1938 _refine_ls_number_parameters 102 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0325 _refine_ls_R_factor_gt 0.0310 _refine_ls_wR_factor_ref 0.0744 _refine_ls_wR_factor_gt 0.0740 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _refine_ls_shift/su_max 0.017 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.87652(7) 0.22221(3) 0.062796(16) 0.01544(11) Uani 1 1 d . . . Cl2 Cl 0.72703(16) 0.03273(8) 0.12493(4) 0.02182(17) Uani 1 1 d . . . O3 O 1.1258(5) 0.1542(2) -0.00962(10) 0.0187(4) Uani 1 1 d . . . C4 C 1.1814(6) 0.0035(3) -0.01429(16) 0.0172(6) Uani 1 1 d . . . H4A H 1.0200 -0.0487 -0.0255 0.021 Uiso 1 1 calc R . . H4B H 1.2447 -0.0306 0.0327 0.021 Uiso 1 1 calc R . . C5 C 1.3853(6) -0.0300(3) -0.07199(14) 0.0161(5) Uani 1 1 d . . . C6 C 1.4525(7) -0.1733(3) -0.08924(17) 0.0200(7) Uani 1 1 d . . . H6 H 1.3713 -0.2508 -0.0655 0.024 Uiso 1 1 calc R . . C7 C 1.6409(7) -0.1982(3) -0.14196(15) 0.0226(6) Uani 1 1 d . . . H7 H 1.6905 -0.2929 -0.1536 0.027 Uiso 1 1 calc R . . C8 C 1.7562(7) -0.0812(3) -0.17748(17) 0.0222(7) Uani 1 1 d . . . H8 H 1.8839 -0.0968 -0.2132 0.027 Uiso 1 1 calc R . . C9 C 1.6798(6) 0.0594(3) -0.15947(16) 0.0189(7) Uani 1 1 d . . . C10 C 1.7919(7) 0.1905(3) -0.19743(18) 0.0238(7) Uani 1 1 d . . . H10A H 1.6505 0.2504 -0.2152 0.036 Uiso 1 1 calc R . . H10B H 1.8997 0.1595 -0.2377 0.036 Uiso 1 1 calc R . . H10C H 1.8973 0.2454 -0.1636 0.036 Uiso 1 1 calc R . . N11 N 0.9976(6) 0.4164(3) 0.10642(13) 0.0164(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.02065(18) 0.00754(16) 0.01813(17) 0.00040(13) 0.00068(15) 0.00108(13) Cl2 0.0311(4) 0.0099(3) 0.0244(4) 0.0030(3) 0.0078(3) 0.0020(3) O3 0.0233(11) 0.0080(9) 0.0246(10) 0.0010(8) 0.0054(11) 0.0016(9) C4 0.0243(17) 0.0083(12) 0.0190(14) 0.0000(10) 0.0028(11) 0.0000(11) C5 0.0195(13) 0.0119(12) 0.0169(13) -0.0003(10) -0.0032(13) -0.0006(12) C6 0.0309(18) 0.0093(12) 0.0198(13) 0.0012(11) 0.0006(12) -0.0008(12) C7 0.0319(17) 0.0108(14) 0.0251(14) -0.0027(11) -0.0028(14) 0.0018(13) C8 0.0291(18) 0.0191(14) 0.0184(15) -0.0034(13) 0.0027(13) 0.0006(13) C9 0.0243(17) 0.0146(14) 0.0177(14) -0.0017(11) -0.0012(12) -0.0030(12) C10 0.0329(17) 0.0144(14) 0.0242(15) -0.0008(12) 0.0063(13) -0.0033(13) N11 0.0210(13) 0.0112(11) 0.0170(12) 0.0000(9) 0.0015(10) 0.0011(11) _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 Zn1 O3 1.934(2) . ? Zn1 O3 1.961(2) 3_455 ? Zn1 N11 2.047(2) . ? Zn1 Cl2 2.2115(8) . ? O3 C4 1.414(3) . ? O3 Zn1 1.961(2) 3 ? C4 C5 1.508(4) . ? C5 N11 1.344(4) 3 ? C5 C6 1.395(4) . ? C6 C7 1.376(4) . ? C7 C8 1.385(4) . ? C8 C9 1.388(4) . ? C9 N11 1.358(4) 3 ? C9 C10 1.501(4) . ? N11 C5 1.344(4) 3_455 ? N11 C9 1.358(4) 3_455 ? 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 O3 Zn1 O3 105.66(4) . 3_455 ? O3 Zn1 N11 110.63(10) . . ? O3 Zn1 N11 83.32(9) 3_455 . ? O3 Zn1 Cl2 108.78(6) . . ? O3 Zn1 Cl2 119.21(7) 3_455 . ? N11 Zn1 Cl2 125.95(7) . . ? C4 O3 Zn1 119.15(18) . . ? C4 O3 Zn1 114.01(18) . 3 ? Zn1 O3 Zn1 125.18(10) . 3 ? O3 C4 C5 112.2(2) . . ? N11 C5 C6 121.5(3) 3 . ? N11 C5 C4 117.4(2) 3 . ? C6 C5 C4 121.2(3) . . ? C7 C6 C5 119.0(3) . . ? C6 C7 C8 119.5(3) . . ? C7 C8 C9 119.5(3) . . ? N11 C9 C8 120.8(3) 3 . ? N11 C9 C10 117.2(3) 3 . ? C8 C9 C10 122.0(3) . . ? C5 N11 C9 119.8(3) 3_455 3_455 ? C5 N11 Zn1 111.5(2) 3_455 . ? C9 N11 Zn1 128.6(2) 3_455 . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 27.92 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 2.166 _refine_diff_density_min -0.280 _refine_diff_density_rms 0.112 #END data_[Ni4(1-H)4Cl4] _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H48 Cl4 N4 Ni4 O8' _chemical_formula_weight 993.30 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c 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 16.2641(7) _cell_length_b 15.0302(7) _cell_length_c 16.6497(11) _cell_angle_alpha 90.00 _cell_angle_beta 100.9830(10) _cell_angle_gamma 90.00 _cell_volume 3995.5(4) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 9999 _cell_measurement_theta_min 1.86 _cell_measurement_theta_max 27.87 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.651 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2048 _exptl_absorpt_coefficient_mu 2.175 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5165 _exptl_absorpt_correction_T_max 0.6702 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 APEX' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12349 _diffrn_reflns_av_R_equivalents 0.0244 _diffrn_reflns_av_sigmaI/netI 0.0318 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 27.87 _reflns_number_total 4620 _reflns_number_gt 4023 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution SHELXL _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^)+(0.0678P)^2^+11.1826P] 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 4620 _refine_ls_number_parameters 247 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0528 _refine_ls_R_factor_gt 0.0459 _refine_ls_wR_factor_ref 0.1326 _refine_ls_wR_factor_gt 0.1281 _refine_ls_goodness_of_fit_ref 1.104 _refine_ls_restrained_S_all 1.104 _refine_ls_shift/su_max 0.127 _refine_ls_shift/su_mean 0.003 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 Ni1 Ni 0.02093(3) 0.27919(3) 0.16126(2) 0.02560(14) Uani 1 1 d . . . Ni3 Ni 0.09587(3) 0.13266(3) 0.29022(2) 0.02638(14) Uani 1 1 d . . . Cl5 Cl -0.04594(7) 0.26853(6) 0.01946(5) 0.0408(2) Uani 1 1 d . . . Cl7 Cl 0.23060(6) 0.14509(8) 0.25133(7) 0.0468(3) Uani 1 1 d . . . O7 O 0.07988(14) 0.26895(15) 0.28473(14) 0.0252(5) Uani 1 1 d . . . O38 O 0.02248(15) 0.14109(15) 0.17738(14) 0.0259(5) Uani 1 1 d . . . O60 O 0.1400(2) 0.2775(2) 0.13352(19) 0.0410(7) Uani 1 1 d . . . O70 O -0.14795(19) 0.1336(2) 0.08622(17) 0.0435(7) Uani 1 1 d . . . N1 N -0.0198(2) 0.4135(2) 0.15365(18) 0.0381(7) Uani 1 1 d . . . N31 N 0.0963(3) -0.0026(2) 0.2552(2) 0.0508(9) Uani 1 1 d . . . C1 C 0.0160(3) 0.4893(3) 0.1330(3) 0.0508(11) Uani 1 1 d . . . C2 C -0.0263(5) 0.5693(3) 0.1271(3) 0.0721(17) Uani 1 1 d . . . H2 H 0.0004 0.6210 0.1150 0.087 Uiso 1 1 calc R . . C3 C -0.1077(5) 0.5731(3) 0.1391(4) 0.0762(19) Uani 1 1 d . . . H3 H -0.1365 0.6269 0.1346 0.091 Uiso 1 1 calc R . . C4 C -0.1455(4) 0.4967(3) 0.1577(3) 0.0567(12) Uani 1 1 d . . . H4 H -0.2004 0.4974 0.1661 0.068 Uiso 1 1 calc R . . C5 C -0.1002(3) 0.4177(3) 0.1638(2) 0.0397(9) Uani 1 1 d . . . C6 C 0.1409(2) 0.3327(2) 0.3183(2) 0.0360(8) Uani 1 1 d . . . H6A H 0.1777 0.3441 0.2799 0.043 Uiso 1 1 calc R . . H6B H 0.1745 0.3095 0.3683 0.043 Uiso 1 1 calc R . . C8 C 0.1046(4) 0.4843(4) 0.1210(4) 0.0717(16) Uani 1 1 d . . . H8A H 0.1054 0.4684 0.0653 0.108 Uiso 1 1 calc R . . H8B H 0.1342 0.4402 0.1570 0.108 Uiso 1 1 calc R . . H8C H 0.1310 0.5411 0.1329 0.108 Uiso 1 1 calc R . . C32 C -0.1217(3) -0.0773(3) 0.2027(3) 0.0467(10) Uani 1 1 d . . . C33 C -0.1311(4) -0.1566(4) 0.2419(4) 0.0743(17) Uani 1 1 d . . . H33 H -0.1493 -0.2072 0.2114 0.089 Uiso 1 1 calc R . . C34 C -0.1138(4) -0.1609(4) 0.3253(3) 0.0727(17) Uani 1 1 d . . . H34 H -0.1205 -0.2139 0.3521 0.087 Uiso 1 1 calc R . . C35 C 0.0861(4) -0.0854(3) 0.1308(3) 0.0608(13) Uani 1 1 d . . . H35 H 0.0726 -0.0867 0.0740 0.073 Uiso 1 1 calc R . . C36 C 0.0788(3) -0.0072(3) 0.1734(3) 0.0477(10) Uani 1 1 d . . . C37 C 0.0482(3) 0.0774(3) 0.1249(2) 0.0422(9) Uani 1 1 d . . . H37A H 0.0930 0.1017 0.1006 0.051 Uiso 1 1 calc R . . H37B H 0.0017 0.0629 0.0812 0.051 Uiso 1 1 calc R . . C38 C -0.1408(5) -0.0735(4) 0.1104(3) 0.0761(18) Uani 1 1 d . . . H38A H -0.0937 -0.0488 0.0911 0.114 Uiso 1 1 calc R . . H38B H -0.1892 -0.0369 0.0926 0.114 Uiso 1 1 calc R . . H38C H -0.1516 -0.1325 0.0889 0.114 Uiso 1 1 calc R . . C61 C 0.1664(3) 0.2671(4) 0.0575(3) 0.0616(14) Uani 1 1 d . . . H10A H 0.1708 0.3245 0.0333 0.092 Uiso 1 1 calc R . . H10B H 0.1264 0.2316 0.0215 0.092 Uiso 1 1 calc R . . H10C H 0.2201 0.2382 0.0664 0.092 Uiso 1 1 calc R . . C71 C -0.2312(4) 0.1301(5) 0.0441(3) 0.0762(18) Uani 1 1 d . . . H71A H -0.2631 0.1758 0.0642 0.114 Uiso 1 1 calc R . . H71B H -0.2546 0.0730 0.0526 0.114 Uiso 1 1 calc R . . H71C H -0.2329 0.1390 -0.0133 0.114 Uiso 1 1 calc R . . H61 H 0.156(3) 0.241(3) 0.154(3) 0.022(12) Uiso 1 1 d . . . H70 H -0.124(3) 0.173(3) 0.070(3) 0.044(13) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0304(2) 0.0242(2) 0.0231(2) -0.00003(15) 0.00737(17) -0.00218(16) Ni3 0.0266(2) 0.0259(2) 0.0246(2) -0.00287(15) -0.00030(17) 0.00417(16) Cl5 0.0550(6) 0.0411(5) 0.0248(4) 0.0039(3) 0.0040(4) -0.0077(4) Cl7 0.0313(5) 0.0550(6) 0.0549(6) -0.0043(5) 0.0101(4) 0.0099(4) O7 0.0252(11) 0.0238(11) 0.0260(11) -0.0044(8) 0.0033(9) -0.0045(9) O38 0.0308(12) 0.0236(11) 0.0222(10) -0.0012(8) 0.0024(9) 0.0028(9) O60 0.0401(16) 0.0506(19) 0.0357(15) 0.0024(14) 0.0157(13) -0.0024(14) O70 0.0441(16) 0.0505(18) 0.0307(14) 0.0081(12) -0.0063(12) -0.0165(14) N1 0.060(2) 0.0263(15) 0.0292(15) 0.0021(12) 0.0128(14) -0.0023(15) N31 0.056(2) 0.0401(19) 0.050(2) -0.0077(16) -0.0050(17) 0.0100(17) C1 0.083(3) 0.0276(19) 0.048(2) 0.0039(17) 0.028(2) -0.013(2) C2 0.126(6) 0.030(2) 0.070(3) 0.012(2) 0.043(4) -0.003(3) C3 0.129(6) 0.035(2) 0.071(3) 0.014(2) 0.036(4) 0.027(3) C4 0.077(3) 0.043(2) 0.054(3) 0.011(2) 0.022(2) 0.022(2) C5 0.053(2) 0.036(2) 0.0297(18) 0.0030(15) 0.0092(17) 0.0073(18) C6 0.0358(19) 0.0348(19) 0.0360(18) -0.0076(15) 0.0030(15) -0.0119(16) C8 0.094(4) 0.049(3) 0.079(4) -0.001(3) 0.035(3) -0.032(3) C32 0.061(3) 0.0273(18) 0.044(2) -0.0015(16) -0.0102(19) -0.0090(18) C33 0.098(5) 0.044(3) 0.073(4) 0.001(2) -0.004(3) -0.022(3) C34 0.092(4) 0.052(3) 0.066(3) 0.019(3) -0.006(3) -0.020(3) C35 0.080(4) 0.046(3) 0.054(3) -0.014(2) 0.005(2) 0.010(2) C36 0.053(3) 0.048(2) 0.039(2) -0.0068(18) 0.0024(18) 0.008(2) C37 0.068(3) 0.0303(19) 0.0295(18) -0.0068(14) 0.0118(18) 0.0036(18) C38 0.107(5) 0.058(3) 0.055(3) -0.004(2) -0.004(3) -0.027(3) C61 0.059(3) 0.088(4) 0.044(3) -0.003(2) 0.027(2) -0.003(3) C71 0.055(3) 0.112(5) 0.051(3) 0.011(3) -0.016(2) -0.019(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 O7 2.021(2) 2 ? Ni1 O60 2.074(3) . ? Ni1 O38 2.092(2) . ? Ni1 O7 2.102(2) . ? Ni1 N1 2.121(3) . ? Ni1 Cl5 2.4091(10) . ? Ni3 O38 2.029(2) . ? Ni3 O7 2.065(2) . ? Ni3 O70 2.070(3) 2 ? Ni3 O38 2.100(2) 2 ? Ni3 N31 2.115(4) . ? Ni3 Cl7 2.4075(11) . ? O7 C6 1.416(4) . ? O7 Ni1 2.021(2) 2 ? O38 C37 1.412(4) . ? O38 Ni3 2.100(2) 2 ? O60 C61 1.421(5) . ? O60 H61 0.67(4) . ? O70 C71 1.402(6) . ? O70 Ni3 2.070(3) 2 ? O70 H70 0.79(5) . ? N1 C5 1.351(6) . ? N1 C1 1.353(5) . ? N31 C36 1.340(6) . ? N31 C32 1.346(5) 2 ? C1 C2 1.380(7) . ? C1 C8 1.493(8) . ? C2 C3 1.378(9) . ? C2 H2 0.9300 . ? C3 C4 1.366(8) . ? C3 H3 0.9300 . ? C4 C5 1.390(6) . ? C4 H4 0.9300 . ? C5 C6 1.495(6) 2 ? C6 C5 1.495(6) 2 ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C32 N31 1.346(5) 2 ? C32 C33 1.381(7) . ? C32 C38 1.509(7) . ? C33 C34 1.366(8) . ? C33 H33 0.9300 . ? C34 C35 1.379(7) 2 ? C34 H34 0.9300 . ? C35 C34 1.379(7) 2 ? C35 C36 1.389(6) . ? C35 H35 0.9300 . ? C36 C37 1.537(6) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C61 H10A 0.9600 . ? C61 H10B 0.9600 . ? C61 H10C 0.9600 . ? C71 H71A 0.9600 . ? C71 H71B 0.9600 . ? C71 H71C 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 O7 Ni1 O60 165.72(11) 2 . ? O7 Ni1 O38 81.86(9) 2 . ? O60 Ni1 O38 91.59(12) . . ? O7 Ni1 O7 79.44(10) 2 . ? O60 Ni1 O7 86.89(11) . . ? O38 Ni1 O7 79.04(9) . . ? O7 Ni1 N1 80.12(11) 2 . ? O60 Ni1 N1 106.99(14) . . ? O38 Ni1 N1 161.42(12) . . ? O7 Ni1 N1 101.95(11) . . ? O7 Ni1 Cl5 100.25(7) 2 . ? O60 Ni1 Cl5 92.71(9) . . ? O38 Ni1 Cl5 92.97(7) . . ? O7 Ni1 Cl5 171.98(7) . . ? N1 Ni1 Cl5 85.83(9) . . ? O38 Ni3 O7 81.38(9) . . ? O38 Ni3 O70 167.67(11) . 2 ? O7 Ni3 O70 93.51(11) . 2 ? O38 Ni3 O38 80.08(10) . 2 ? O7 Ni3 O38 80.66(9) . 2 ? O70 Ni3 O38 88.04(11) 2 2 ? O38 Ni3 N31 80.64(12) . . ? O7 Ni3 N31 161.52(12) . . ? O70 Ni3 N31 104.96(14) 2 . ? O38 Ni3 N31 100.37(13) 2 . ? O38 Ni3 Cl7 98.69(7) . . ? O7 Ni3 Cl7 91.41(7) . . ? O70 Ni3 Cl7 92.62(10) 2 . ? O38 Ni3 Cl7 172.06(7) 2 . ? N31 Ni3 Cl7 87.11(12) . . ? C6 O7 Ni1 109.9(2) . 2 ? C6 O7 Ni3 125.5(2) . . ? Ni1 O7 Ni3 99.31(10) 2 . ? C6 O7 Ni1 119.4(2) . . ? Ni1 O7 Ni1 99.91(10) 2 . ? Ni3 O7 Ni1 98.40(9) . . ? C37 O38 Ni3 109.8(2) . . ? C37 O38 Ni1 126.2(2) . . ? Ni3 O38 Ni1 99.86(10) . . ? C37 O38 Ni3 120.8(2) . 2 ? Ni3 O38 Ni3 99.48(10) . 2 ? Ni1 O38 Ni3 95.95(9) . 2 ? C61 O60 Ni1 130.8(3) . . ? C61 O60 H61 103(4) . . ? Ni1 O60 H61 100(4) . . ? C71 O70 Ni3 132.0(3) . 2 ? C71 O70 H70 111(4) . . ? Ni3 O70 H70 102(3) 2 . ? C5 N1 C1 117.8(4) . . ? C5 N1 Ni1 109.6(2) . . ? C1 N1 Ni1 132.2(3) . . ? C36 N31 C32 118.1(4) . 2 ? C36 N31 Ni3 108.5(3) . . ? C32 N31 Ni3 132.5(3) 2 . ? N1 C1 C2 121.2(5) . . ? N1 C1 C8 117.7(4) . . ? C2 C1 C8 121.0(4) . . ? C3 C2 C1 120.4(5) . . ? C3 C2 H2 119.8 . . ? C1 C2 H2 119.8 . . ? C4 C3 C2 118.9(5) . . ? C4 C3 H3 120.5 . . ? C2 C3 H3 120.5 . . ? C3 C4 C5 118.7(5) . . ? C3 C4 H4 120.7 . . ? C5 C4 H4 120.7 . . ? N1 C5 C4 122.9(4) . . ? N1 C5 C6 117.5(3) . 2 ? C4 C5 C6 119.7(4) . 2 ? O7 C6 C5 110.7(3) . 2 ? O7 C6 H6A 109.5 . . ? C5 C6 H6A 109.5 2 . ? O7 C6 H6B 109.5 . . ? C5 C6 H6B 109.5 2 . ? H6A C6 H6B 108.1 . . ? C1 C8 H8A 109.5 . . ? C1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N31 C32 C33 121.7(4) 2 . ? N31 C32 C38 118.7(4) 2 . ? C33 C32 C38 119.6(4) . . ? C34 C33 C32 120.1(5) . . ? C34 C33 H33 120.0 . . ? C32 C33 H33 120.0 . . ? C33 C34 C35 118.9(5) . 2 ? C33 C34 H34 120.5 . . ? C35 C34 H34 120.5 2 . ? C34 C35 C36 118.5(5) 2 . ? C34 C35 H35 120.8 2 . ? C36 C35 H35 120.8 . . ? N31 C36 C35 122.7(4) . . ? N31 C36 C37 118.5(4) . . ? C35 C36 C37 118.8(4) . . ? O38 C37 C36 109.9(3) . . ? O38 C37 H37A 109.7 . . ? C36 C37 H37A 109.7 . . ? O38 C37 H37B 109.7 . . ? C36 C37 H37B 109.7 . . ? H37A C37 H37B 108.2 . . ? C32 C38 H38A 109.5 . . ? C32 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C32 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? O60 C61 H10A 109.5 . . ? O60 C61 H10B 109.5 . . ? H10A C61 H10B 109.5 . . ? O60 C61 H10C 109.5 . . ? H10A C61 H10C 109.5 . . ? H10B C61 H10C 109.5 . . ? O70 C71 H71A 109.5 . . ? O70 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? O70 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 27.87 _diffrn_measured_fraction_theta_full 0.969 _refine_diff_density_max 1.503 _refine_diff_density_min -0.487 _refine_diff_density_rms 0.117 #END data_[Ni4(1-H)4(OAc)2Cl2(MeOH)2] _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C69 H96 Cl4 N8 Ni8 O21' _chemical_formula_weight 1985.02 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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pca2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, z+1/2' _cell_length_a 15.9492(13) _cell_length_b 35.895(3) _cell_length_c 13.9089(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7962.8(11) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9999 _cell_measurement_theta_min 1.40 _cell_measurement_theta_max 27.92 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.656 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4104 _exptl_absorpt_coefficient_mu 2.058 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6272 _exptl_absorpt_correction_T_max 0.8207 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 47874 _diffrn_reflns_av_R_equivalents 0.0439 _diffrn_reflns_av_sigmaI/netI 0.0689 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -45 _diffrn_reflns_limit_k_max 47 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.40 _diffrn_reflns_theta_max 27.92 _reflns_number_total 18174 _reflns_number_gt 14121 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _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^)+(0.0607P)^2^+17.9916P] 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 fixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(3) _refine_ls_number_reflns 18174 _refine_ls_number_parameters 1002 _refine_ls_number_restraints 440 _refine_ls_R_factor_all 0.0776 _refine_ls_R_factor_gt 0.0575 _refine_ls_wR_factor_ref 0.1391 _refine_ls_wR_factor_gt 0.1320 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.024 _refine_ls_shift/su_max 0.015 _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 N1 N 0.4690(4) 0.70826(15) 0.2142(4) 0.0246(13) Uani 1 1 d . . . C2 C 0.3896(5) 0.69682(19) 0.2122(5) 0.0277(13) Uani 1 1 d U . . C3 C 0.3219(5) 0.7198(2) 0.1956(5) 0.0311(13) Uani 1 1 d U . . H3 H 0.2665 0.7101 0.1955 0.037 Uiso 1 1 calc R . . C4 C 0.3362(5) 0.7574(2) 0.1791(5) 0.0345(12) Uani 1 1 d U . . H4 H 0.2915 0.7740 0.1644 0.041 Uiso 1 1 calc R . . C5 C 0.4186(5) 0.7699(2) 0.1848(5) 0.0305(12) Uani 1 1 d U . . H5 H 0.4306 0.7956 0.1766 0.037 Uiso 1 1 calc R . . C6 C 0.4823(5) 0.74546(19) 0.2022(4) 0.0281(13) Uani 1 1 d U . . C7 C 0.3740(5) 0.65554(19) 0.2270(6) 0.0340(16) Uani 1 1 d U . . H7A H 0.3227 0.6521 0.2661 0.041 Uiso 1 1 calc R . . H7B H 0.3649 0.6434 0.1639 0.041 Uiso 1 1 calc R . . O8 O 0.4406(3) 0.63897(12) 0.2725(4) 0.0263(12) Uani 1 1 d . . . C9 C 0.5696(5) 0.7602(2) 0.2098(5) 0.0347(15) Uani 1 1 d U . . H9A H 0.5930 0.7636 0.1452 0.052 Uiso 1 1 calc R . . H9B H 0.6044 0.7426 0.2458 0.052 Uiso 1 1 calc R . . H9C H 0.5688 0.7842 0.2434 0.052 Uiso 1 1 calc R . . N11 N 0.4444(4) 0.70139(14) 0.4411(4) 0.0255(13) Uani 1 1 d . . . C12 C 0.5213(5) 0.71780(18) 0.4417(5) 0.0264(12) Uani 1 1 d U . . C13 C 0.5322(5) 0.75568(19) 0.4556(5) 0.0358(14) Uani 1 1 d U . . H13 H 0.5868 0.7663 0.4550 0.043 Uiso 1 1 calc R . . C14 C 0.4636(6) 0.7775(2) 0.4701(5) 0.0413(14) Uani 1 1 d U . . H14 H 0.4693 0.8035 0.4808 0.050 Uiso 1 1 calc R . . C15 C 0.3869(5) 0.7612(2) 0.4690(5) 0.0376(14) Uani 1 1 d U . . H15 H 0.3385 0.7763 0.4778 0.045 Uiso 1 1 calc R . . C16 C 0.3772(5) 0.72334(19) 0.4554(5) 0.0319(14) Uani 1 1 d U . . C17 C 0.5952(4) 0.69253(17) 0.4247(5) 0.0239(13) Uani 1 1 d U . . H17A H 0.6380 0.7060 0.3867 0.029 Uiso 1 1 calc R . . H17B H 0.6206 0.6858 0.4872 0.029 Uiso 1 1 calc R . . O18 O 0.5722(3) 0.65991(13) 0.3756(3) 0.0236(11) Uani 1 1 d . . . C19 C 0.2933(4) 0.7061(2) 0.4568(5) 0.0366(16) Uani 1 1 d U . . H19A H 0.2894 0.6875 0.4054 0.055 Uiso 1 1 calc R . . H19B H 0.2506 0.7253 0.4470 0.055 Uiso 1 1 calc R . . H19C H 0.2841 0.6940 0.5191 0.055 Uiso 1 1 calc R . . N21 N 0.6357(4) 0.54871(16) 0.4225(4) 0.0318(14) Uani 1 1 d . . . C22 C 0.5612(5) 0.53400(19) 0.4541(5) 0.0309(14) Uani 1 1 d U . . C23 C 0.5592(5) 0.4979(2) 0.4888(5) 0.0404(15) Uani 1 1 d U . . H23 H 0.5085 0.4884 0.5151 0.049 Uiso 1 1 calc R . . C24 C 0.6283(6) 0.4757(2) 0.4862(6) 0.0469(16) Uani 1 1 d U . . H24 H 0.6265 0.4508 0.5098 0.056 Uiso 1 1 calc R . . C25 C 0.7007(5) 0.4903(2) 0.4486(6) 0.0445(15) Uani 1 1 d U . . H25 H 0.7490 0.4749 0.4429 0.053 Uiso 1 1 calc R . . C26 C 0.7045(5) 0.5269(2) 0.4187(6) 0.0398(16) Uani 1 1 d U . . C27 C 0.4889(5) 0.55943(18) 0.4576(5) 0.0305(15) Uani 1 1 d U . . H27A H 0.4374 0.5457 0.4394 0.037 Uiso 1 1 calc R . . H27B H 0.4816 0.5687 0.5241 0.037 Uiso 1 1 calc R . . O28 O 0.5001(3) 0.59013(13) 0.3943(3) 0.0242(11) Uani 1 1 d . . . C29 C 0.7845(5) 0.5435(2) 0.3831(7) 0.054(2) Uani 1 1 d U . . H29A H 0.7745 0.5560 0.3214 0.080 Uiso 1 1 calc R . . H29B H 0.8264 0.5238 0.3745 0.080 Uiso 1 1 calc R . . H29C H 0.8052 0.5617 0.4299 0.080 Uiso 1 1 calc R . . N31 N 0.5558(5) 0.53714(16) 0.2142(5) 0.0393(17) Uani 1 1 d . . . C32 C 0.6322(5) 0.5479(2) 0.1840(6) 0.0333(15) Uani 1 1 d U . . C33 C 0.6942(6) 0.5239(2) 0.1550(6) 0.0433(16) Uani 1 1 d U . . H33 H 0.7464 0.5329 0.1314 0.052 Uiso 1 1 calc R . . C34 C 0.6775(6) 0.4855(2) 0.1616(6) 0.0467(15) Uani 1 1 d U . . H34 H 0.7194 0.4678 0.1450 0.056 Uiso 1 1 calc R . . C35 C 0.6010(6) 0.4741(2) 0.1918(6) 0.0492(16) Uani 1 1 d U . . H35 H 0.5891 0.4482 0.1951 0.059 Uiso 1 1 calc R . . C36 C 0.5395(6) 0.4997(2) 0.2182(6) 0.0408(15) Uani 1 1 d U . . C37 C 0.6484(5) 0.58851(18) 0.1840(5) 0.0266(14) Uani 1 1 d U . . H37A H 0.7077 0.5930 0.2013 0.032 Uiso 1 1 calc R . . H37B H 0.6392 0.5984 0.1184 0.032 Uiso 1 1 calc R . . O38 O 0.5969(3) 0.60748(12) 0.2482(4) 0.0285(11) Uani 1 1 d . . . C39 C 0.4563(6) 0.4872(2) 0.2521(7) 0.0493(18) Uani 1 1 d U . . H39A H 0.4222 0.5090 0.2691 0.074 Uiso 1 1 calc R . . H39B H 0.4631 0.4713 0.3087 0.074 Uiso 1 1 calc R . . H39C H 0.4283 0.4732 0.2009 0.074 Uiso 1 1 calc R . . N41 N 0.4411(4) 0.96113(15) 0.9806(4) 0.0312(15) Uani 1 1 d . . . C42 C 0.3684(6) 0.9488(2) 1.0131(5) 0.0375(16) Uani 1 1 d U . . C43 C 0.3088(7) 0.9727(2) 1.0497(6) 0.056(2) Uani 1 1 d U . . H43 H 0.2564 0.9633 1.0713 0.067 Uiso 1 1 calc R . . C44 C 0.3252(7) 1.0098(2) 1.0546(7) 0.071(2) Uani 1 1 d U . . H44 H 0.2857 1.0264 1.0824 0.085 Uiso 1 1 calc R . . C45 C 0.3987(7) 1.0228(2) 1.0193(6) 0.0552(18) Uani 1 1 d U . . H45 H 0.4099 1.0488 1.0179 0.066 Uiso 1 1 calc R . . C46 C 0.4577(6) 0.9974(2) 0.9850(5) 0.0419(15) Uani 1 1 d U . . C47 C 0.3507(5) 0.90694(18) 1.0079(5) 0.0308(16) Uani 1 1 d U . . H47A H 0.3634 0.8950 1.0704 0.037 Uiso 1 1 calc R . . H47B H 0.2908 0.9026 0.9928 0.037 Uiso 1 1 calc R . . O48 O 0.4022(3) 0.89158(11) 0.9346(3) 0.0185(9) Uani 1 1 d . . . C49 C 0.5405(6) 1.0107(2) 0.9509(6) 0.054(2) Uani 1 1 d U . . H49A H 0.5557 0.9975 0.8917 0.080 Uiso 1 1 calc R . . H49B H 0.5829 1.0058 1.0003 0.080 Uiso 1 1 calc R . . H49C H 0.5378 1.0375 0.9381 0.080 Uiso 1 1 calc R . . N51 N 0.5337(4) 0.79043(14) 0.9465(4) 0.0232(12) Uani 1 1 d . . . C52 C 0.6137(4) 0.80332(19) 0.9501(5) 0.0250(12) Uani 1 1 d U . . C53 C 0.6813(5) 0.7790(2) 0.9638(6) 0.0372(15) Uani 1 1 d U . . H53 H 0.7371 0.7883 0.9640 0.045 Uiso 1 1 calc R . . C54 C 0.6673(5) 0.7431(2) 0.9764(6) 0.0434(16) Uani 1 1 d U . . H54 H 0.7129 0.7268 0.9887 0.052 Uiso 1 1 calc R . . C55 C 0.5857(5) 0.7291(2) 0.9718(6) 0.0404(16) Uani 1 1 d U . . H55 H 0.5759 0.7031 0.9797 0.048 Uiso 1 1 calc R . . C56 C 0.5193(5) 0.75314(18) 0.9557(5) 0.0284(14) Uani 1 1 d U . . C57 C 0.6278(4) 0.84399(18) 0.9429(5) 0.0230(12) Uani 1 1 d U . . H57A H 0.6360 0.8544 1.0081 0.028 Uiso 1 1 calc R . . H57B H 0.6794 0.8488 0.9053 0.028 Uiso 1 1 calc R . . O58 O 0.5587(3) 0.86206(11) 0.8980(3) 0.0176(10) Uani 1 1 d . . . C59 C 0.4322(5) 0.73918(18) 0.9491(6) 0.0327(15) Uani 1 1 d U . . H59A H 0.3935 0.7583 0.9729 0.049 Uiso 1 1 calc R . . H59B H 0.4265 0.7166 0.9882 0.049 Uiso 1 1 calc R . . H59C H 0.4189 0.7334 0.8820 0.049 Uiso 1 1 calc R . . N61 N 0.5566(4) 0.80544(15) 0.7196(4) 0.0246(13) Uani 1 1 d . . . C62 C 0.4828(5) 0.78853(17) 0.7207(4) 0.0233(13) Uani 1 1 d U . . C63 C 0.4723(5) 0.75090(18) 0.7021(4) 0.0319(13) Uani 1 1 d U . . H63 H 0.4180 0.7400 0.7010 0.038 Uiso 1 1 calc R . . C64 C 0.5425(6) 0.7298(2) 0.6853(5) 0.0428(14) Uani 1 1 d U . . H64 H 0.5373 0.7039 0.6725 0.051 Uiso 1 1 calc R . . C65 C 0.6217(6) 0.7464(2) 0.6870(5) 0.0431(14) Uani 1 1 d U . . H65 H 0.6708 0.7319 0.6776 0.052 Uiso 1 1 calc R . . C66 C 0.6274(5) 0.7842(2) 0.7027(5) 0.0357(15) Uani 1 1 d U . . C67 C 0.4066(4) 0.81218(15) 0.7417(4) 0.0200(12) Uani 1 1 d U . . H67A H 0.3805 0.8203 0.6806 0.024 Uiso 1 1 calc R . . H67B H 0.3648 0.7973 0.7779 0.024 Uiso 1 1 calc R . . O68 O 0.4298(3) 0.84341(10) 0.7956(3) 0.0166(9) Uani 1 1 d . . . C69 C 0.7109(5) 0.8034(2) 0.7017(6) 0.0427(17) Uani 1 1 d U . . H69A H 0.7152 0.8190 0.6442 0.064 Uiso 1 1 calc R . . H69B H 0.7558 0.7847 0.7009 0.064 Uiso 1 1 calc R . . H69C H 0.7164 0.8189 0.7592 0.064 Uiso 1 1 calc R . . N71 N 0.3553(4) 0.95444(15) 0.7724(4) 0.0282(14) Uani 1 1 d . . . C72 C 0.4258(5) 0.97067(16) 0.7445(5) 0.0276(13) Uani 1 1 d U . . C73 C 0.4291(5) 1.00867(17) 0.7177(5) 0.0339(13) Uani 1 1 d U . . H73 H 0.4795 1.0195 0.6943 0.041 Uiso 1 1 calc R . . C74 C 0.3577(6) 1.02923(19) 0.7267(5) 0.0434(14) Uani 1 1 d U . . H74 H 0.3575 1.0549 0.7098 0.052 Uiso 1 1 calc R . . C75 C 0.2859(5) 1.01252(19) 0.7602(6) 0.0439(15) Uani 1 1 d U . . H75 H 0.2366 1.0268 0.7701 0.053 Uiso 1 1 calc R . . C76 C 0.2862(5) 0.97457(19) 0.7795(5) 0.0342(15) Uani 1 1 d U . . C77 C 0.5038(4) 0.94717(16) 0.7353(4) 0.0245(13) Uani 1 1 d U . . H77A H 0.5122 0.9402 0.6671 0.029 Uiso 1 1 calc R . . H77B H 0.5532 0.9618 0.7562 0.029 Uiso 1 1 calc R . . O78 O 0.4976(3) 0.91483(11) 0.7913(3) 0.0210(10) Uani 1 1 d . . . C79 C 0.2082(5) 0.9562(2) 0.8125(8) 0.057(2) Uani 1 1 d U . . H79A H 0.1838 0.9419 0.7594 0.086 Uiso 1 1 calc R . . H79B H 0.1681 0.9752 0.8339 0.086 Uiso 1 1 calc R . . H79C H 0.2211 0.9394 0.8661 0.086 Uiso 1 1 calc R . . C101 C 0.5677(6) 0.6263(2) 0.5888(6) 0.0355(18) Uani 1 1 d U . . C102 C 0.5878(6) 0.6265(2) 0.6943(6) 0.050(2) Uani 1 1 d U . . H10A H 0.5933 0.6008 0.7174 0.076 Uiso 1 1 calc R . . H10B H 0.5426 0.6390 0.7295 0.076 Uiso 1 1 calc R . . H10C H 0.6406 0.6398 0.7049 0.076 Uiso 1 1 calc R . . O103 O 0.6247(4) 0.61451(14) 0.5388(4) 0.0325(12) Uani 1 1 d . . . O104 O 0.4948(4) 0.63864(13) 0.5645(4) 0.0369(14) Uani 1 1 d . . . C111 C 0.4927(6) 0.6200(2) 0.0554(6) 0.042(2) Uani 1 1 d U . . C112 C 0.4792(8) 0.6192(3) -0.0506(7) 0.082(4) Uani 1 1 d U . . H11A H 0.5115 0.5987 -0.0787 0.122 Uiso 1 1 calc R . . H11B H 0.4977 0.6429 -0.0785 0.122 Uiso 1 1 calc R . . H11C H 0.4195 0.6155 -0.0641 0.122 Uiso 1 1 calc R . . O113 O 0.5257(3) 0.64989(14) 0.0873(4) 0.0324(12) Uani 1 1 d . . . O114 O 0.4676(4) 0.59287(14) 0.1016(4) 0.0354(13) Uani 1 1 d . . . C121 C 0.4251(4) 0.88115(16) 0.5885(4) 0.0167(13) Uani 1 1 d U . . C122 C 0.4046(5) 0.87962(19) 0.4829(4) 0.0248(14) Uani 1 1 d U . . H12A H 0.3657 0.8590 0.4707 0.037 Uiso 1 1 calc R . . H12B H 0.4562 0.8757 0.4460 0.037 Uiso 1 1 calc R . . H12C H 0.3785 0.9031 0.4632 0.037 Uiso 1 1 calc R . . O123 O 0.3685(3) 0.89290(12) 0.6441(3) 0.0190(10) Uani 1 1 d . . . O124 O 0.4992(3) 0.87030(12) 0.6135(3) 0.0208(10) Uani 1 1 d . . . C131 C 0.5203(5) 0.8739(2) 1.1220(5) 0.0282(16) Uani 1 1 d U . . C132 C 0.5456(6) 0.8725(2) 1.2279(5) 0.0427(19) Uani 1 1 d U . . H13A H 0.6057 0.8670 1.2329 0.064 Uiso 1 1 calc R . . H13B H 0.5136 0.8529 1.2604 0.064 Uiso 1 1 calc R . . H13C H 0.5337 0.8965 1.2582 0.064 Uiso 1 1 calc R . . O133 O 0.5386(4) 0.90454(13) 1.0808(3) 0.0319(13) Uani 1 1 d . . . O134 O 0.4820(3) 0.84688(14) 1.0859(3) 0.0296(12) Uani 1 1 d . . . Ni1 Ni 0.55158(6) 0.66122(2) 0.22832(6) 0.0234(2) Uani 1 1 d . . . Ni2 Ni 0.61981(6) 0.60692(2) 0.39321(6) 0.0246(2) Uani 1 1 d . . . Ni3 Ni 0.47994(6) 0.58488(2) 0.24713(7) 0.0285(2) Uani 1 1 d . . . Ni4 Ni 0.45733(6) 0.64313(2) 0.42027(6) 0.0234(2) Uani 1 1 d . . . Ni5 Ni 0.51695(6) 0.91437(2) 0.93816(6) 0.0230(2) Uani 1 1 d . . . Ni6 Ni 0.54274(5) 0.86325(2) 0.75180(6) 0.01803(18) Uani 1 1 d . . . Ni7 Ni 0.45010(5) 0.83806(2) 0.94379(6) 0.01678(17) Uani 1 1 d . . . Ni8 Ni 0.37731(6) 0.89594(2) 0.78978(6) 0.01741(18) Uani 1 1 d . . . Cl1 Cl 0.69190(15) 0.68120(6) 0.19691(16) 0.0459(5) Uani 1 1 d . . . Cl2 Cl 0.33947(13) 0.56443(5) 0.26837(15) 0.0417(5) Uani 1 1 d . . . Cl3 Cl 0.67518(11) 0.89368(5) 0.72361(12) 0.0343(4) Uani 1 1 d . . . Cl4 Cl 0.31035(10) 0.81699(4) 0.97535(11) 0.0219(3) Uani 1 1 d . . . O201 O 0.2620(3) 0.87245(12) 0.8193(3) 0.0275(6) Uani 1 1 d D . . C202 C 0.2052(4) 0.85686(18) 0.7510(4) 0.0287(15) Uani 1 1 d D . . H20A H 0.1668 0.8763 0.7283 0.043 Uiso 1 1 calc R . . H20B H 0.1731 0.8368 0.7814 0.043 Uiso 1 1 calc R . . H20C H 0.2369 0.8468 0.6965 0.043 Uiso 1 1 calc R . . O211 O 0.6365(4) 0.93436(14) 0.9108(4) 0.0429(15) Uani 1 1 d D . . O221 O 0.3353(3) 0.62049(13) 0.4347(4) 0.0349(11) Uani 1 1 d D . . C222 C 0.2948(6) 0.6070(3) 0.5196(6) 0.078(3) Uani 1 1 d DU . . H22A H 0.3332 0.5905 0.5546 0.117 Uiso 1 1 calc R . . H22B H 0.2442 0.5932 0.5017 0.117 Uiso 1 1 calc R . . H22C H 0.2794 0.6281 0.5607 0.117 Uiso 1 1 calc R . . O231 O 0.7419(3) 0.63097(13) 0.3655(3) 0.0275(6) Uani 1 1 d DU . . C232 C 0.7958(7) 0.6448(3) 0.4376(8) 0.093(4) Uani 1 1 d DU . . H23A H 0.7661 0.6453 0.4992 0.139 Uiso 1 1 calc R . . H23B H 0.8135 0.6701 0.4208 0.139 Uiso 1 1 calc R . . H23C H 0.8452 0.6287 0.4428 0.139 Uiso 1 1 calc R . . C211 C 0.6948(10) 0.9451(6) 0.9832(12) 0.176(8) Uani 1 1 d DU . . O301 O 0.3738(4) 0.66787(19) 0.6824(5) 0.073(2) Uani 1 1 d D . . C302 C 0.3523(11) 0.6359(4) 0.7399(12) 0.159(7) Uani 1 1 d DU . . H30A H 0.4034 0.6251 0.7674 0.239 Uiso 1 1 calc R . . H30B H 0.3243 0.6173 0.6996 0.239 Uiso 1 1 calc R . . H30C H 0.3146 0.6435 0.7919 0.239 Uiso 1 1 calc R . . H21A H 0.7523 0.9480 0.9445 0.239 Uiso 1 1 d . . . H21B H 0.7164 0.9133 1.0036 0.239 Uiso 1 1 d . . . H21C H 0.6865 0.9546 1.0297 0.239 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.023(3) 0.030(3) 0.021(3) 0.009(2) 0.000(2) -0.001(2) C2 0.036(3) 0.032(2) 0.015(3) 0.005(2) -0.001(3) -0.001(2) C3 0.035(3) 0.038(2) 0.021(3) 0.000(2) -0.002(3) 0.0010(18) C4 0.046(2) 0.039(2) 0.019(3) 0.011(3) 0.000(3) 0.006(2) C5 0.050(3) 0.029(3) 0.012(3) 0.006(2) 0.003(3) 0.0004(18) C6 0.042(3) 0.031(3) 0.011(3) 0.006(2) 0.002(3) -0.0040(18) C7 0.039(4) 0.034(2) 0.029(4) 0.006(3) -0.004(3) -0.007(3) O8 0.034(3) 0.020(2) 0.025(3) -0.0004(18) 0.000(2) -0.0045(19) C9 0.049(3) 0.029(4) 0.026(4) 0.008(3) -0.007(3) -0.010(3) N11 0.037(4) 0.028(3) 0.012(2) 0.000(2) 0.002(2) 0.009(2) C12 0.036(3) 0.029(2) 0.015(3) 0.002(2) 0.006(3) 0.000(2) C13 0.050(3) 0.028(2) 0.030(3) 0.003(3) 0.011(3) -0.001(2) C14 0.061(3) 0.029(2) 0.034(4) 0.001(3) 0.009(3) 0.0065(16) C15 0.051(3) 0.033(2) 0.028(3) 0.003(3) 0.008(3) 0.016(2) C16 0.034(3) 0.035(2) 0.026(3) 0.002(3) 0.003(3) 0.012(2) C17 0.025(3) 0.029(2) 0.018(3) -0.002(2) -0.002(3) -0.006(2) O18 0.025(3) 0.032(3) 0.014(2) 0.0007(18) 0.000(2) 0.003(2) C19 0.032(3) 0.049(3) 0.029(4) 0.011(3) 0.012(3) 0.012(2) N21 0.040(4) 0.028(3) 0.027(3) 0.002(2) -0.004(3) 0.010(3) C22 0.038(3) 0.030(2) 0.025(3) 0.007(2) 0.005(3) -0.003(2) C23 0.054(3) 0.027(2) 0.040(4) 0.006(3) 0.008(3) -0.002(2) C24 0.061(4) 0.030(3) 0.049(4) 0.004(3) -0.002(3) 0.005(2) C25 0.053(3) 0.033(3) 0.048(4) -0.001(3) -0.002(3) 0.011(3) C26 0.046(4) 0.035(3) 0.038(4) 0.001(3) -0.003(3) 0.006(3) C27 0.033(3) 0.027(3) 0.031(4) 0.001(3) 0.002(3) -0.007(2) O28 0.022(3) 0.028(2) 0.022(2) 0.0068(19) -0.004(2) -0.0009(19) C29 0.047(4) 0.050(4) 0.064(6) 0.019(4) 0.014(4) 0.019(3) N31 0.066(5) 0.021(3) 0.031(3) -0.010(2) 0.007(3) -0.001(3) C32 0.037(4) 0.030(2) 0.033(3) -0.012(3) 0.003(3) 0.001(2) C33 0.052(4) 0.035(2) 0.043(4) -0.011(3) 0.003(3) 0.013(2) C34 0.064(3) 0.033(2) 0.043(4) -0.009(3) -0.017(3) 0.015(3) C35 0.076(4) 0.029(3) 0.043(4) -0.007(3) -0.011(3) 0.005(2) C36 0.063(3) 0.026(3) 0.034(4) -0.001(3) -0.006(3) -0.004(2) C37 0.025(4) 0.029(2) 0.026(3) -0.002(3) 0.007(3) 0.005(2) O38 0.038(3) 0.023(2) 0.025(3) -0.003(2) 0.001(3) 0.005(2) C39 0.078(4) 0.025(3) 0.045(5) -0.001(3) 0.005(4) -0.016(3) N41 0.061(4) 0.024(3) 0.009(2) -0.004(2) -0.002(3) -0.002(3) C42 0.070(5) 0.023(2) 0.020(3) 0.002(2) 0.015(3) 0.003(2) C43 0.091(5) 0.030(2) 0.048(4) 0.005(3) 0.035(4) 0.012(3) C44 0.121(5) 0.027(2) 0.065(5) 0.006(3) 0.044(4) 0.018(3) C45 0.108(5) 0.022(3) 0.036(4) 0.004(3) 0.009(4) 0.004(2) C46 0.082(4) 0.029(3) 0.014(3) -0.001(3) 0.000(3) -0.006(2) C47 0.055(5) 0.025(2) 0.012(3) 0.004(2) 0.012(3) -0.001(3) O48 0.026(3) 0.017(2) 0.012(2) 0.0039(17) 0.006(2) 0.0008(18) C49 0.098(5) 0.031(4) 0.032(4) -0.004(3) 0.009(4) -0.024(3) N51 0.027(3) 0.027(3) 0.016(2) 0.008(2) -0.003(2) 0.000(2) C52 0.013(3) 0.039(2) 0.023(3) 0.012(3) -0.004(3) -0.0015(18) C53 0.017(3) 0.049(2) 0.045(4) 0.016(3) 0.005(3) 0.0066(18) C54 0.030(2) 0.045(2) 0.055(4) 0.011(3) 0.004(3) 0.012(2) C55 0.033(2) 0.031(3) 0.057(4) 0.009(3) 0.006(3) 0.0104(18) C56 0.031(2) 0.024(3) 0.030(4) 0.005(3) -0.001(3) 0.0045(18) C57 0.010(3) 0.040(2) 0.019(3) 0.007(3) -0.009(3) -0.006(2) O58 0.016(2) 0.023(2) 0.013(2) 0.0054(16) -0.0028(19) -0.0006(17) C59 0.032(2) 0.022(3) 0.045(4) 0.006(3) 0.002(3) 0.003(2) N61 0.031(3) 0.033(3) 0.011(2) 0.003(2) 0.000(2) 0.005(2) C62 0.038(3) 0.0218(19) 0.010(2) -0.004(2) -0.006(3) 0.006(2) C63 0.057(3) 0.021(2) 0.017(3) -0.005(2) -0.004(3) 0.008(2) C64 0.072(3) 0.028(2) 0.028(3) -0.005(3) 0.001(3) 0.0197(18) C65 0.061(3) 0.044(2) 0.024(3) -0.004(3) 0.008(3) 0.027(2) C66 0.043(3) 0.044(2) 0.020(3) 0.000(3) -0.003(3) 0.018(2) C67 0.030(3) 0.017(2) 0.013(3) 0.002(2) -0.003(3) 0.0005(19) O68 0.023(3) 0.0094(19) 0.018(2) -0.0017(16) 0.004(2) -0.0022(17) C69 0.033(3) 0.062(4) 0.033(4) 0.003(4) 0.003(3) 0.023(2) N71 0.055(4) 0.021(3) 0.009(3) 0.0020(19) 0.009(2) -0.001(3) C72 0.050(3) 0.0174(19) 0.015(3) 0.001(2) 0.004(3) -0.003(2) C73 0.061(3) 0.020(2) 0.021(3) 0.006(2) -0.005(3) -0.005(2) C74 0.076(4) 0.023(2) 0.031(3) 0.003(3) -0.007(3) 0.0082(18) C75 0.067(3) 0.025(2) 0.040(4) -0.002(3) 0.003(3) 0.021(2) C76 0.049(4) 0.028(2) 0.026(3) 0.005(2) 0.006(3) 0.018(2) C77 0.042(3) 0.018(2) 0.014(3) 0.003(2) 0.002(3) -0.0098(19) O78 0.036(3) 0.0106(19) 0.017(2) 0.0027(16) 0.005(2) -0.0071(18) C79 0.040(4) 0.047(4) 0.085(7) 0.023(5) 0.014(5) 0.026(3) C101 0.051(5) 0.020(3) 0.035(3) 0.003(3) -0.006(4) -0.006(3) C102 0.072(6) 0.039(4) 0.041(4) 0.011(3) -0.020(4) 0.008(4) O103 0.043(3) 0.035(3) 0.019(2) 0.003(2) -0.002(2) -0.001(2) O104 0.056(4) 0.029(3) 0.026(3) 0.003(2) -0.019(3) -0.007(2) C111 0.059(6) 0.038(4) 0.029(3) -0.002(3) 0.000(4) -0.021(4) C112 0.119(9) 0.097(8) 0.029(3) 0.009(5) -0.005(5) -0.055(7) O113 0.037(3) 0.033(3) 0.027(3) -0.001(2) 0.002(2) -0.004(2) O114 0.042(4) 0.029(3) 0.035(3) -0.003(2) 0.004(3) -0.009(2) C121 0.025(3) 0.013(3) 0.012(2) 0.002(2) -0.002(2) -0.007(2) C122 0.032(4) 0.030(3) 0.013(2) 0.003(2) -0.006(3) -0.002(3) O123 0.019(2) 0.022(2) 0.017(2) -0.0048(16) 0.0022(18) -0.0004(17) O124 0.024(3) 0.026(2) 0.013(2) 0.0018(17) 0.0060(19) 0.0023(19) C131 0.034(4) 0.039(4) 0.012(3) 0.003(3) -0.002(3) -0.009(3) C132 0.065(5) 0.047(4) 0.016(3) 0.011(3) -0.013(3) -0.016(4) O133 0.057(4) 0.030(3) 0.009(2) 0.0052(19) -0.002(2) -0.023(3) O134 0.045(3) 0.033(3) 0.011(2) 0.0056(19) -0.001(2) -0.009(2) Ni1 0.0310(5) 0.0202(4) 0.0189(4) 0.0014(3) -0.0003(4) -0.0024(4) Ni2 0.0270(5) 0.0232(4) 0.0234(5) 0.0016(3) 0.0004(4) 0.0012(4) Ni3 0.0375(6) 0.0227(4) 0.0253(5) -0.0006(4) -0.0009(4) -0.0075(4) Ni4 0.0271(5) 0.0238(4) 0.0192(4) 0.0037(3) 0.0020(4) -0.0020(4) Ni5 0.0377(6) 0.0219(4) 0.0093(4) -0.0009(3) 0.0020(4) -0.0109(4) Ni6 0.0206(4) 0.0224(4) 0.0111(4) 0.0001(3) 0.0012(4) -0.0012(3) Ni7 0.0180(4) 0.0202(4) 0.0122(4) 0.0036(3) 0.0017(4) -0.0017(3) Ni8 0.0245(5) 0.0156(4) 0.0121(4) 0.0021(3) 0.0035(3) 0.0013(3) Cl1 0.0539(15) 0.0364(10) 0.0474(12) 0.0029(9) 0.0007(11) -0.0029(9) Cl2 0.0434(11) 0.0394(10) 0.0424(11) 0.0012(8) -0.0040(9) -0.0161(8) Cl3 0.0307(9) 0.0528(10) 0.0193(7) 0.0019(7) 0.0048(7) -0.0138(8) Cl4 0.0179(8) 0.0250(8) 0.0229(8) 0.0093(6) 0.0027(7) -0.0022(6) O201 0.0241(13) 0.0346(14) 0.0239(13) 0.0122(11) 0.0087(11) 0.0135(11) C202 0.023(3) 0.044(4) 0.019(3) 0.004(3) -0.004(3) 0.000(3) O211 0.070(4) 0.037(3) 0.022(2) -0.005(2) 0.010(3) -0.026(3) O221 0.024(3) 0.043(3) 0.038(3) 0.000(2) 0.001(2) 0.002(2) C222 0.074(5) 0.070(5) 0.090(5) -0.008(4) -0.009(4) -0.005(4) O231 0.0241(13) 0.0346(14) 0.0239(13) 0.0122(11) 0.0087(11) 0.0135(11) C232 0.091(6) 0.085(5) 0.102(6) 0.000(4) 0.013(4) -0.002(4) C211 0.174(9) 0.180(9) 0.175(9) 0.004(5) 0.002(5) 0.001(5) O301 0.069(5) 0.067(4) 0.082(5) -0.020(4) 0.017(4) -0.004(3) C302 0.156(8) 0.166(8) 0.155(8) 0.009(5) -0.002(5) 0.008(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C2 1.331(9) . ? N1 C6 1.363(9) . ? N1 Ni1 2.151(6) . ? C2 C3 1.379(10) . ? C2 C7 1.516(9) . ? C3 C4 1.387(10) . ? C4 C5 1.390(11) . ? C5 C6 1.363(10) . ? C6 C9 1.494(11) . ? C7 O8 1.371(9) . ? O8 Ni1 2.037(5) . ? O8 Ni3 2.070(4) . ? O8 Ni4 2.078(5) . ? N11 C16 1.345(9) . ? N11 C12 1.361(9) . ? N11 Ni4 2.122(5) . ? C12 C13 1.384(9) . ? C12 C17 1.506(9) . ? C13 C14 1.361(11) . ? C14 C15 1.356(11) . ? C15 C16 1.382(10) . ? C16 C19 1.475(10) . ? C17 O18 1.404(7) . ? O18 Ni4 2.026(5) . ? O18 Ni2 2.063(5) . ? O18 Ni1 2.076(5) . ? N21 C26 1.349(10) . ? N21 C22 1.374(9) . ? N21 Ni2 2.144(6) . ? C22 C23 1.383(9) . ? C22 C27 1.471(10) . ? C23 C24 1.362(11) . ? C24 C25 1.372(12) . ? C25 C26 1.380(10) . ? C26 C29 1.494(11) . ? C27 O28 1.421(8) . ? O28 Ni2 2.002(5) . ? O28 Ni4 2.053(5) . ? O28 Ni3 2.081(5) . ? N31 C32 1.345(10) . ? N31 C36 1.370(9) . ? N31 Ni3 2.147(6) . ? C32 C33 1.371(11) . ? C32 C37 1.481(10) . ? C33 C34 1.407(11) . ? C34 C35 1.355(12) . ? C35 C36 1.394(12) . ? C36 C39 1.478(11) . ? C37 O38 1.391(8) . ? O38 Ni3 2.035(5) . ? O38 Ni2 2.049(5) . ? O38 Ni1 2.079(5) . ? N41 C42 1.322(10) . ? N41 C46 1.332(9) . ? N41 Ni5 2.152(6) . ? C42 C43 1.378(11) . ? C42 C47 1.530(10) . ? C43 C44 1.356(12) . ? C44 C45 1.354(14) . ? C45 C46 1.392(12) . ? C46 C49 1.482(11) . ? C47 O48 1.421(8) . ? O48 Ni5 2.006(5) . ? O48 Ni8 2.058(5) . ? O48 Ni7 2.072(4) . ? N51 C52 1.358(8) . ? N51 C56 1.364(8) . ? N51 Ni7 2.168(5) . ? C52 C53 1.402(9) . ? C52 C57 1.481(9) . ? C53 C54 1.317(11) . ? C54 C55 1.397(11) . ? C55 C56 1.385(10) . ? C56 C59 1.480(10) . ? C57 O58 1.422(7) . ? O58 Ni7 2.037(5) . ? O58 Ni6 2.050(5) . ? O58 Ni5 2.069(4) . ? N61 C62 1.325(9) . ? N61 C66 1.383(9) . ? N61 Ni6 2.134(5) . ? C62 C63 1.386(9) . ? C62 C67 1.511(9) . ? C63 C64 1.373(11) . ? C64 C65 1.397(12) . ? C65 C66 1.375(11) . ? C66 C69 1.501(11) . ? C67 O68 1.398(7) . ? O68 Ni6 2.031(4) . ? O68 Ni8 2.064(4) . ? O68 Ni7 2.095(5) . ? N71 C76 1.322(9) . ? N71 C72 1.325(9) . ? N71 Ni8 2.143(5) . ? C72 C73 1.415(8) . ? C72 C77 1.509(10) . ? C73 C74 1.363(11) . ? C74 C75 1.374(11) . ? C75 C76 1.389(10) . ? C76 C79 1.480(11) . ? C77 O78 1.402(7) . ? O78 Ni8 2.035(5) . ? O78 Ni6 2.061(4) . ? O78 Ni5 2.066(5) . ? C101 O103 1.219(10) . ? C101 O104 1.289(10) . ? C101 C102 1.503(12) . ? O103 Ni2 2.045(5) . ? O104 Ni4 2.100(5) . ? C111 O114 1.233(9) . ? C111 O113 1.275(9) . ? C111 C112 1.490(12) . ? O113 Ni1 2.046(5) . ? O114 Ni3 2.054(6) . ? C121 O123 1.261(8) . ? C121 O124 1.293(8) . ? C121 C122 1.507(8) . ? O123 Ni8 2.034(5) . ? O124 Ni6 2.060(5) . ? C131 O134 1.252(8) . ? C131 O133 1.273(8) . ? C131 C132 1.527(9) . ? O133 Ni5 2.045(4) . ? O134 Ni7 2.066(5) . ? Ni1 Cl1 2.390(3) . ? Ni1 Ni3 2.9803(12) . ? Ni2 O231 2.165(5) . ? Ni2 Ni4 2.9234(14) . ? Ni3 Cl2 2.376(2) . ? Ni4 O221 2.119(5) . ? Ni5 O211 2.073(6) . ? Ni5 Ni7 2.9405(11) . ? Ni6 Cl3 2.4101(19) . ? Ni6 Ni8 2.9356(12) . ? Ni7 Cl4 2.3943(18) . ? Ni8 O201 2.065(5) . ? O201 C202 1.426(4) . ? O211 C211 1.423(5) . ? O221 C222 1.430(5) . ? O231 C232 1.411(5) . ? O301 C302 1.440(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 N1 C6 116.6(6) . . ? C2 N1 Ni1 110.0(4) . . ? C6 N1 Ni1 133.2(5) . . ? N1 C2 C3 124.3(7) . . ? N1 C2 C7 117.0(6) . . ? C3 C2 C7 118.7(7) . . ? C2 C3 C4 118.8(8) . . ? C5 C4 C3 117.3(7) . . ? C6 C5 C4 120.5(7) . . ? C5 C6 N1 122.4(7) . . ? C5 C6 C9 118.6(7) . . ? N1 C6 C9 119.0(7) . . ? O8 C7 C2 111.1(6) . . ? C7 O8 Ni1 111.3(4) . . ? C7 O8 Ni3 124.2(4) . . ? Ni1 O8 Ni3 93.0(2) . . ? C7 O8 Ni4 121.6(5) . . ? Ni1 O8 Ni4 99.1(2) . . ? Ni3 O8 Ni4 101.4(2) . . ? C16 N11 C12 117.7(6) . . ? C16 N11 Ni4 132.4(5) . . ? C12 N11 Ni4 109.9(4) . . ? N11 C12 C13 122.6(7) . . ? N11 C12 C17 116.3(5) . . ? C13 C12 C17 121.0(7) . . ? C14 C13 C12 119.0(8) . . ? C15 C14 C13 118.5(7) . . ? C14 C15 C16 121.7(7) . . ? N11 C16 C15 120.5(7) . . ? N11 C16 C19 118.7(6) . . ? C15 C16 C19 120.8(6) . . ? O18 C17 C12 112.0(6) . . ? C17 O18 Ni4 109.6(4) . . ? C17 O18 Ni2 128.0(4) . . ? Ni4 O18 Ni2 91.29(19) . . ? C17 O18 Ni1 120.1(4) . . ? Ni4 O18 Ni1 99.6(2) . . ? Ni2 O18 Ni1 101.3(2) . . ? C26 N21 C22 119.5(6) . . ? C26 N21 Ni2 130.9(5) . . ? C22 N21 Ni2 109.5(4) . . ? N21 C22 C23 119.5(7) . . ? N21 C22 C27 116.8(6) . . ? C23 C22 C27 123.5(7) . . ? C24 C23 C22 121.4(8) . . ? C23 C24 C25 117.9(7) . . ? C24 C25 C26 121.0(8) . . ? N21 C26 C25 120.4(8) . . ? N21 C26 C29 118.4(7) . . ? C25 C26 C29 121.2(7) . . ? O28 C27 C22 111.2(6) . . ? C27 O28 Ni2 111.0(4) . . ? C27 O28 Ni4 124.6(4) . . ? Ni2 O28 Ni4 92.3(2) . . ? C27 O28 Ni3 121.3(4) . . ? Ni2 O28 Ni3 99.6(2) . . ? Ni4 O28 Ni3 101.84(19) . . ? C32 N31 C36 117.7(7) . . ? C32 N31 Ni3 110.4(5) . . ? C36 N31 Ni3 131.9(6) . . ? N31 C32 C33 124.5(7) . . ? N31 C32 C37 116.1(6) . . ? C33 C32 C37 119.4(7) . . ? C32 C33 C34 117.2(8) . . ? C35 C34 C33 119.3(8) . . ? C34 C35 C36 121.0(8) . . ? N31 C36 C35 120.2(8) . . ? N31 C36 C39 118.7(7) . . ? C35 C36 C39 121.0(7) . . ? O38 C37 C32 112.3(6) . . ? C37 O38 Ni3 109.9(4) . . ? C37 O38 Ni2 121.5(4) . . ? Ni3 O38 Ni2 99.6(2) . . ? C37 O38 Ni1 125.0(4) . . ? Ni3 O38 Ni1 92.9(2) . . ? Ni2 O38 Ni1 101.7(2) . . ? C42 N41 C46 119.2(7) . . ? C42 N41 Ni5 109.0(5) . . ? C46 N41 Ni5 131.6(6) . . ? N41 C42 C43 121.4(7) . . ? N41 C42 C47 118.3(7) . . ? C43 C42 C47 120.2(8) . . ? C44 C43 C42 119.8(9) . . ? C43 C44 C45 119.1(9) . . ? C44 C45 C46 119.0(7) . . ? N41 C46 C45 121.3(8) . . ? N41 C46 C49 118.5(7) . . ? C45 C46 C49 120.2(7) . . ? O48 C47 C42 108.0(6) . . ? C47 O48 Ni5 110.6(4) . . ? C47 O48 Ni8 124.1(4) . . ? Ni5 O48 Ni8 99.75(19) . . ? C47 O48 Ni7 121.9(4) . . ? Ni5 O48 Ni7 92.29(19) . . ? Ni8 O48 Ni7 101.67(19) . . ? C52 N51 C56 119.2(6) . . ? C52 N51 Ni7 108.0(4) . . ? C56 N51 Ni7 132.2(5) . . ? N51 C52 C53 121.0(6) . . ? N51 C52 C57 118.4(6) . . ? C53 C52 C57 120.5(6) . . ? C54 C53 C52 119.8(7) . . ? C53 C54 C55 120.3(7) . . ? C56 C55 C54 119.6(7) . . ? N51 C56 C55 119.9(7) . . ? N51 C56 C59 118.9(6) . . ? C55 C56 C59 121.1(6) . . ? O58 C57 C52 111.2(5) . . ? C57 O58 Ni7 109.2(4) . . ? C57 O58 Ni6 122.8(4) . . ? Ni7 O58 Ni6 102.3(2) . . ? C57 O58 Ni5 123.0(4) . . ? Ni7 O58 Ni5 91.46(19) . . ? Ni6 O58 Ni5 102.03(18) . . ? C62 N61 C66 118.3(6) . . ? C62 N61 Ni6 110.5(4) . . ? C66 N61 Ni6 131.1(5) . . ? N61 C62 C63 123.5(7) . . ? N61 C62 C67 117.4(5) . . ? C63 C62 C67 119.1(7) . . ? C64 C63 C62 118.1(8) . . ? C63 C64 C65 120.0(7) . . ? C66 C65 C64 118.9(7) . . ? C65 C66 N61 121.2(8) . . ? C65 C66 C69 120.6(7) . . ? N61 C66 C69 118.2(6) . . ? O68 C67 C62 110.0(5) . . ? C67 O68 Ni6 110.8(4) . . ? C67 O68 Ni8 127.2(4) . . ? Ni6 O68 Ni8 91.58(16) . . ? C67 O68 Ni7 119.7(3) . . ? Ni6 O68 Ni7 100.9(2) . . ? Ni8 O68 Ni7 100.67(18) . . ? C76 N71 C72 119.3(6) . . ? C76 N71 Ni8 131.6(5) . . ? C72 N71 Ni8 108.9(4) . . ? N71 C72 C73 122.2(7) . . ? N71 C72 C77 118.6(5) . . ? C73 C72 C77 119.1(6) . . ? C74 C73 C72 117.8(7) . . ? C73 C74 C75 119.4(6) . . ? C74 C75 C76 119.5(7) . . ? N71 C76 C75 121.6(7) . . ? N71 C76 C79 118.7(6) . . ? C75 C76 C79 119.7(7) . . ? O78 C77 C72 110.9(5) . . ? C77 O78 Ni8 109.7(4) . . ? C77 O78 Ni6 124.8(4) . . ? Ni8 O78 Ni6 91.57(17) . . ? C77 O78 Ni5 123.1(4) . . ? Ni8 O78 Ni5 98.5(2) . . ? Ni6 O78 Ni5 101.77(19) . . ? O103 C101 O104 130.0(8) . . ? O103 C101 C102 113.5(8) . . ? O104 C101 C102 116.5(8) . . ? C101 O103 Ni2 125.6(5) . . ? C101 O104 Ni4 122.2(5) . . ? O114 C111 O113 128.2(8) . . ? O114 C111 C112 116.9(7) . . ? O113 C111 C112 114.8(7) . . ? C111 O113 Ni1 125.7(5) . . ? C111 O114 Ni3 126.3(5) . . ? O123 C121 O124 126.2(5) . . ? O123 C121 C122 117.1(6) . . ? O124 C121 C122 116.7(6) . . ? C121 O123 Ni8 125.4(4) . . ? C121 O124 Ni6 126.6(4) . . ? O134 C131 O133 126.9(6) . . ? O134 C131 C132 119.2(6) . . ? O133 C131 C132 113.8(6) . . ? C131 O133 Ni5 123.2(4) . . ? C131 O134 Ni7 128.5(4) . . ? O8 Ni1 O113 92.1(2) . . ? O8 Ni1 O18 80.3(2) . . ? O113 Ni1 O18 166.9(2) . . ? O8 Ni1 O38 84.2(2) . . ? O113 Ni1 O38 90.8(2) . . ? O18 Ni1 O38 78.03(19) . . ? O8 Ni1 N1 78.6(2) . . ? O113 Ni1 N1 86.8(2) . . ? O18 Ni1 N1 101.8(2) . . ? O38 Ni1 N1 162.5(2) . . ? O8 Ni1 Cl1 170.55(16) . . ? O113 Ni1 Cl1 94.19(17) . . ? O18 Ni1 Cl1 92.24(16) . . ? O38 Ni1 Cl1 88.68(16) . . ? N1 Ni1 Cl1 108.74(16) . . ? O8 Ni1 Ni3 43.92(13) . . ? O113 Ni1 Ni3 79.87(15) . . ? O18 Ni1 Ni3 87.32(13) . . ? O38 Ni1 Ni3 42.99(15) . . ? N1 Ni1 Ni3 119.66(16) . . ? Cl1 Ni1 Ni3 130.61(6) . . ? O28 Ni2 O103 93.9(2) . . ? O28 Ni2 O38 80.9(2) . . ? O103 Ni2 O38 168.5(2) . . ? O28 Ni2 O18 85.8(2) . . ? O103 Ni2 O18 90.5(2) . . ? O38 Ni2 O18 78.98(18) . . ? O28 Ni2 N21 79.5(2) . . ? O103 Ni2 N21 86.4(2) . . ? O38 Ni2 N21 102.6(2) . . ? O18 Ni2 N21 164.8(2) . . ? O28 Ni2 O231 168.31(18) . . ? O103 Ni2 O231 95.1(2) . . ? O38 Ni2 O231 88.9(2) . . ? O18 Ni2 O231 86.71(18) . . ? N21 Ni2 O231 108.4(2) . . ? O28 Ni2 Ni4 44.56(14) . . ? O103 Ni2 Ni4 81.19(16) . . ? O38 Ni2 Ni4 87.97(15) . . ? O18 Ni2 Ni4 43.85(14) . . ? N21 Ni2 Ni4 120.91(18) . . ? O231 Ni2 Ni4 130.03(12) . . ? O38 Ni3 O114 92.3(2) . . ? O38 Ni3 O8 84.42(19) . . ? O114 Ni3 O8 90.5(2) . . ? O38 Ni3 O28 79.3(2) . . ? O114 Ni3 O28 166.36(18) . . ? O8 Ni3 O28 78.14(19) . . ? O38 Ni3 N31 78.6(2) . . ? O114 Ni3 N31 87.4(2) . . ? O8 Ni3 N31 162.8(2) . . ? O28 Ni3 N31 101.3(2) . . ? O38 Ni3 Cl2 170.74(15) . . ? O114 Ni3 Cl2 94.31(17) . . ? O8 Ni3 Cl2 89.03(16) . . ? O28 Ni3 Cl2 92.96(15) . . ? N31 Ni3 Cl2 108.1(2) . . ? O38 Ni3 Ni1 44.15(13) . . ? O114 Ni3 Ni1 79.74(14) . . ? O8 Ni3 Ni1 43.03(15) . . ? O28 Ni3 Ni1 86.78(13) . . ? N31 Ni3 Ni1 119.94(19) . . ? Cl2 Ni3 Ni1 131.04(6) . . ? O18 Ni4 O28 85.47(19) . . ? O18 Ni4 O8 80.46(19) . . ? O28 Ni4 O8 78.60(18) . . ? O18 Ni4 O104 93.3(2) . . ? O28 Ni4 O104 90.1(2) . . ? O8 Ni4 O104 167.5(2) . . ? O18 Ni4 O221 166.86(19) . . ? O28 Ni4 O221 88.10(19) . . ? O8 Ni4 O221 87.0(2) . . ? O104 Ni4 O221 98.1(2) . . ? O18 Ni4 N11 80.6(2) . . ? O28 Ni4 N11 165.9(2) . . ? O8 Ni4 N11 101.2(2) . . ? O104 Ni4 N11 88.4(2) . . ? O221 Ni4 N11 106.0(2) . . ? O18 Ni4 Ni2 44.87(13) . . ? O28 Ni4 Ni2 43.17(14) . . ? O8 Ni4 Ni2 87.39(15) . . ? O104 Ni4 Ni2 80.60(18) . . ? O221 Ni4 Ni2 131.00(13) . . ? N11 Ni4 Ni2 122.80(17) . . ? O48 Ni5 O133 96.2(2) . . ? O48 Ni5 O78 80.91(19) . . ? O133 Ni5 O78 170.44(18) . . ? O48 Ni5 O58 85.25(17) . . ? O133 Ni5 O58 92.92(19) . . ? O78 Ni5 O58 77.80(17) . . ? O48 Ni5 O211 167.52(19) . . ? O133 Ni5 O211 94.7(2) . . ? O78 Ni5 O211 87.3(2) . . ? O58 Ni5 O211 88.2(2) . . ? O48 Ni5 N41 79.1(2) . . ? O133 Ni5 N41 87.9(2) . . ? O78 Ni5 N41 100.4(2) . . ? O58 Ni5 N41 164.4(2) . . ? O211 Ni5 N41 107.3(2) . . ? O48 Ni5 Ni7 44.75(12) . . ? O133 Ni5 Ni7 82.79(13) . . ? O78 Ni5 Ni7 88.83(11) . . ? O58 Ni5 Ni7 43.83(13) . . ? O211 Ni5 Ni7 131.38(15) . . ? N41 Ni5 Ni7 121.03(18) . . ? O68 Ni6 O58 78.79(18) . . ? O68 Ni6 O124 91.40(18) . . ? O58 Ni6 O124 166.06(19) . . ? O68 Ni6 O78 85.70(18) . . ? O58 Ni6 O78 78.35(17) . . ? O124 Ni6 O78 91.18(18) . . ? O68 Ni6 N61 79.28(19) . . ? O58 Ni6 N61 100.06(19) . . ? O124 Ni6 N61 87.64(19) . . ? O78 Ni6 N61 164.9(2) . . ? O68 Ni6 Cl3 170.15(13) . . ? O58 Ni6 Cl3 93.54(14) . . ? O124 Ni6 Cl3 95.02(14) . . ? O78 Ni6 Cl3 86.70(14) . . ? N61 Ni6 Cl3 108.40(17) . . ? O68 Ni6 Ni8 44.66(11) . . ? O58 Ni6 Ni8 86.66(13) . . ? O124 Ni6 Ni8 79.41(13) . . ? O78 Ni6 Ni8 43.86(14) . . ? N61 Ni6 Ni8 121.30(16) . . ? Cl3 Ni6 Ni8 129.48(6) . . ? O58 Ni7 O134 91.4(2) . . ? O58 Ni7 O48 84.39(17) . . ? O134 Ni7 O48 90.46(19) . . ? O58 Ni7 O68 77.62(17) . . ? O134 Ni7 O68 164.89(18) . . ? O48 Ni7 O68 78.27(17) . . ? O58 Ni7 N51 79.38(19) . . ? O134 Ni7 N51 87.3(2) . . ? O48 Ni7 N51 163.6(2) . . ? O68 Ni7 N51 100.63(19) . . ? O58 Ni7 Cl4 169.33(13) . . ? O134 Ni7 Cl4 95.87(16) . . ? O48 Ni7 Cl4 87.76(13) . . ? O68 Ni7 Cl4 93.73(13) . . ? N51 Ni7 Cl4 108.67(16) . . ? O58 Ni7 Ni5 44.71(12) . . ? O134 Ni7 Ni5 78.07(14) . . ? O48 Ni7 Ni5 42.96(13) . . ? O68 Ni7 Ni5 86.82(11) . . ? N51 Ni7 Ni5 120.80(15) . . ? Cl4 Ni7 Ni5 129.55(5) . . ? O78 Ni8 O123 95.33(19) . . ? O78 Ni8 O48 80.43(18) . . ? O123 Ni8 O48 169.66(18) . . ? O78 Ni8 O68 85.52(17) . . ? O123 Ni8 O68 91.03(18) . . ? O48 Ni8 O68 79.29(17) . . ? O78 Ni8 O201 166.90(18) . . ? O123 Ni8 O201 96.60(19) . . ? O48 Ni8 O201 86.90(18) . . ? O68 Ni8 O201 88.87(17) . . ? O78 Ni8 N71 80.2(2) . . ? O123 Ni8 N71 85.92(18) . . ? O48 Ni8 N71 102.50(18) . . ? O68 Ni8 N71 165.0(2) . . ? O201 Ni8 N71 106.1(2) . . ? O78 Ni8 Ni6 44.57(12) . . ? O123 Ni8 Ni6 82.02(13) . . ? O48 Ni8 Ni6 88.43(13) . . ? O68 Ni8 Ni6 43.76(12) . . ? O201 Ni8 Ni6 132.32(13) . . ? N71 Ni8 Ni6 121.25(18) . . ? C202 O201 Ni8 126.4(4) . . ? C211 O211 Ni5 124.4(9) . . ? C222 O221 Ni4 128.5(5) . . ? C232 O231 Ni2 124.1(6) . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 27.92 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 1.638 _refine_diff_density_min -0.733 _refine_diff_density_rms 0.133 #END