#Supplementary Material (ESI) for Dalton Transactions #This journal is (c) The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Bim Graham' 'Leone Spiccia' 'Alan M. Bond' 'Milton T. W. Hearn' 'Christopher M. Kepert' _publ_contact_author_name 'Dr Leone Spiccia' _publ_contact_author_address ; Dr Leone Spiccia School of Chemistry Monash University PO Box 23 3800 Victoria AUSTRALIA ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation (1985, 1992). teXsan. Crystal Structure Analysis Package, The Woodlands, TX, USA 77381 ; data_A_TEXRAY.INF_file1 _database_code_CSD 159103 #------------------------------------------------------------------------------ _audit_creation_date 'Thu Sep 23 15:54:44 1999' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution ? _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #------------------------------------------------------------------------------ _cell_length_a 14.1402(2) _cell_length_b 9.6023(1) _cell_length_c 16.4655(2) _cell_angle_alpha 89 _cell_angle_beta 89 _cell_angle_gamma 90 _cell_volume 2235.66(9) _cell_formula_units_Z 4 _cell_measurement_temperature 273.2 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0.0 _cell_measurement_theta_max 0.0 #------------------------------------------------------------------------------ _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c n ' _symmetry_Int_Tables_number 60 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2-x,1/2-y,1/2+z' '1/2+x,1/2-y, -z' ' -x, +y,1/2-z' ' -x, -y, -z' '1/2+x,1/2+y,1/2-z' '1/2-x,1/2+y, +z' ' +x, -y,1/2+z' #------------------------------------------------------------------------------ _exptl_crystal_description 'unknown' _exptl_crystal_colour 'unknown' _exptl_crystal_size_max 0.000 _exptl_crystal_size_mid 0.000 _exptl_crystal_size_min 0.000 _exptl_crystal_density_diffrn 1.610 _exptl_crystal_density_meas ? _chemical_formula_weight 542.05 _chemical_formula_analytical ? _chemical_formula_sum 'C14 H32 Cl2 N6 O8 Ni ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 1136.00 _exptl_absorpt_coefficient_mu 1.160 _exptl_absorpt_correction_type none #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 273.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoKalpha _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector ? _diffrn_measurement_device 'unknown' _diffrn_measurement_method 'omega scans with profile analysis' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 3679 _reflns_number_total 3679 _reflns_number_observed 2518 _reflns_observed_criterion 3.00 _diffrn_reflns_av_R_equivalents 0.00 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 30.02 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ni 0 4 0.339 1.112 'International Tables' C 0 56 0.003 0.002 'International Tables' N 0 24 0.006 0.003 'International Tables' O 0 32 0.011 0.006 'International Tables' H 0 128 0.000 0.000 'International Tables' Cl 0 8 0.148 0.159 'International Tables' #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom Ni(1) 0.0000 0.23938(4) 0.2500 0.0135(1) Uij ? ? Cl(1) 0.16425(4) 0.21694(6) -0.38300(3) 0.0219(2) Uij ? ? O(1) 0.0729(1) 0.2725(2) -0.4034(1) 0.0323(5) Uij ? ? O(2) 0.2243(1) 0.3243(2) -0.3516(1) 0.0335(5) Uij ? ? O(3) 0.2054(1) 0.1560(3) -0.4530(1) 0.0665(8) Uij ? ? O(4) 0.1529(1) 0.1128(2) -0.3223(1) 0.0542(7) Uij ? ? N(1) -0.0704(1) 0.4032(2) 0.1881(1) 0.0162(5) Uij ? ? N(2) -0.1081(1) 0.1165(2) 0.1990(1) 0.0171(5) Uij ? ? N(3) 0.0617(1) 0.2110(2) 0.1326(1) 0.0173(5) Uij ? ? C(1) -0.0515(2) 0.5318(2) 0.2354(1) 0.0206(6) Uij ? ? C(2) -0.1706(2) 0.3589(2) 0.1903(1) 0.0199(6) Uij ? ? C(3) -0.1809(2) 0.2091(2) 0.1624(1) 0.0207(6) Uij ? ? C(4) -0.0598(2) 0.0231(2) 0.1410(1) 0.0212(6) Uij ? ? C(5) 0.0063(2) 0.1049(2) 0.0864(1) 0.0207(6) Uij ? ? C(6) 0.0609(2) 0.3483(2) 0.0918(1) 0.0209(6) Uij ? ? C(7) -0.0347(2) 0.4158(2) 0.1027(1) 0.0202(6) Uij ? ? H(1) -0.0632 0.6122 0.2021 0.0258 Uij ? ? H(2) -0.0930 0.5364 0.2813 0.0258 Uij ? ? H(3) -0.2064 0.4175 0.1555 0.0240 Uij ? ? H(4) -0.1935 0.3667 0.2443 0.0240 Uij ? ? H(5) -0.1744 0.2059 0.1048 0.0251 Uij ? ? H(6) -0.2416 0.1761 0.1771 0.0251 Uij ? ? H(7) -0.1366 0.0621 0.2405 0.0204 Uij ? ? H(8) -0.0242 -0.0441 0.1701 0.0258 Uij ? ? H(9) -0.1057 -0.0227 0.1084 0.0258 Uij ? ? H(10) 0.0489 0.0426 0.0607 0.0246 Uij ? ? H(11) -0.0302 0.1516 0.0460 0.0246 Uij ? ? H(12) 0.1250 0.1796 0.1385 0.0209 Uij ? ? H(13) 0.0731 0.3360 0.0356 0.0251 Uij ? ? H(14) 0.1084 0.4057 0.1149 0.0251 Uij ? ? H(15) -0.0786 0.3725 0.0674 0.0242 Uij ? ? H(16) -0.0296 0.5118 0.0897 0.0242 Uij ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ni(1) 0.0152(2) 0.0142(2) 0.0110(2) 0.0000 -0.0011(2) 0.0000 Cl(1) 0.0228(3) 0.0225(3) 0.0204(3) 0.0044(2) -0.0038(3) -0.0008(2) O(1) 0.0256(10) 0.031(1) 0.041(1) 0.0100(8) -0.0117(8) -0.0044(8) O(2) 0.0253(10) 0.023(1) 0.053(1) -0.0042(8) -0.0048(8) -0.0019(8) O(3) 0.046(1) 0.113(2) 0.041(1) 0.028(1) -0.001(1) -0.039(1) O(4) 0.055(1) 0.045(1) 0.063(1) -0.025(1) -0.035(1) 0.035(1) N(1) 0.0179(10) 0.016(1) 0.0151(9) -0.0004(8) -0.0002(8) 0.0000(7) N(2) 0.020(1) 0.016(1) 0.0158(9) -0.0013(8) -0.0018(8) 0.0014(7) N(3) 0.018(1) 0.021(1) 0.0133(9) 0.0020(8) -0.0020(8) -0.0005(8) C(1) 0.025(1) 0.015(1) 0.021(1) 0.0023(10) -0.0010(10) 0.0002(9) C(2) 0.017(1) 0.022(1) 0.021(1) 0.0033(9) 0.000(1) 0.0026(9) C(3) 0.017(1) 0.024(1) 0.021(1) -0.0016(10) -0.0027(10) 0.0018(10) C(4) 0.026(1) 0.019(1) 0.019(1) 0.000(1) -0.0067(10) -0.0046(10) C(5) 0.025(1) 0.022(1) 0.016(1) 0.004(1) -0.0036(10) -0.0047(9) C(6) 0.024(1) 0.024(1) 0.015(1) -0.003(1) 0.0027(10) 0.0021(10) C(7) 0.025(1) 0.020(1) 0.016(1) -0.002(1) -0.0008(10) 0.0041(9) #------------------------------------------------------------------------------ _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 2518 _refine_ls_number_parameters 141 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0368 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0424 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 4.091 _refine_ls_shift/esd_max 0.0100 _refine_ls_shift/esd_mean ? _refine_diff_density_min -0.46 _refine_diff_density_max 1.36 #------------------------------------------------------------------------------ _geom_special_details ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni(1) N(1) 2.123(2) ? ? yes Ni(1) N(1) 2.123(2) ? ? yes Ni(1) N(2) 2.105(2) ? ? yes Ni(1) N(2) 2.105(2) ? ? yes Ni(1) N(3) 2.138(2) ? ? yes Ni(1) N(3) 2.138(2) ? ? yes Cl(1) O(1) 1.437(2) ? ? yes Cl(1) O(2) 1.432(2) ? ? yes Cl(1) O(3) 1.417(2) ? ? yes Cl(1) O(4) 1.423(2) ? ? yes N(1) C(1) 1.485(3) ? ? yes N(1) C(2) 1.479(3) ? ? yes N(1) C(7) 1.498(3) ? ? yes N(2) C(3) 1.488(3) ? ? yes N(2) C(4) 1.477(3) ? ? yes N(3) C(5) 1.493(3) ? ? yes N(3) C(6) 1.480(3) ? ? yes C(1) C(1) 1.535(4) ? ? yes C(2) C(3) 1.517(3) ? ? yes C(4) C(5) 1.516(3) ? ? yes C(6) C(7) 1.510(3) ? ? yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N(1) Ni(1) N(1) 84.37(9) ? ? ? yes N(1) Ni(1) N(2) 83.29(7) ? ? ? yes N(1) Ni(1) N(2) 161.33(7) ? ? ? yes N(1) Ni(1) N(3) 81.48(7) ? ? ? yes N(1) Ni(1) N(3) 109.72(7) ? ? ? yes N(1) Ni(1) N(2) 161.33(7) ? ? ? yes N(1) Ni(1) N(2) 83.29(7) ? ? ? yes N(1) Ni(1) N(3) 109.72(7) ? ? ? yes N(1) Ni(1) N(3) 81.48(7) ? ? ? yes N(2) Ni(1) N(2) 111.83(10) ? ? ? yes N(2) Ni(1) N(3) 82.20(7) ? ? ? yes N(2) Ni(1) N(3) 89.57(7) ? ? ? yes N(2) Ni(1) N(3) 89.57(7) ? ? ? yes N(2) Ni(1) N(3) 82.20(7) ? ? ? yes N(3) Ni(1) N(3) 165.3(1) ? ? ? yes O(1) Cl(1) O(2) 110.5(1) ? ? ? yes O(1) Cl(1) O(3) 109.4(1) ? ? ? yes O(1) Cl(1) O(4) 108.9(1) ? ? ? yes O(2) Cl(1) O(3) 110.3(1) ? ? ? yes O(2) Cl(1) O(4) 108.6(1) ? ? ? yes O(3) Cl(1) O(4) 109.1(2) ? ? ? yes Ni(1) N(1) C(1) 106.3(1) ? ? ? yes Ni(1) N(1) C(2) 103.0(1) ? ? ? yes Ni(1) N(1) C(7) 110.7(1) ? ? ? yes C(1) N(1) C(2) 113.5(2) ? ? ? yes C(1) N(1) C(7) 111.4(2) ? ? ? yes C(2) N(1) C(7) 111.7(2) ? ? ? yes Ni(1) N(2) C(3) 109.2(1) ? ? ? yes Ni(1) N(2) C(4) 105.2(1) ? ? ? yes C(3) N(2) C(4) 114.9(2) ? ? ? yes Ni(1) N(3) C(5) 109.5(1) ? ? ? yes Ni(1) N(3) C(6) 107.1(1) ? ? ? yes C(5) N(3) C(6) 111.8(2) ? ? ? yes N(1) C(1) C(1) 109.6(1) ? ? ? yes N(1) C(2) C(3) 110.9(2) ? ? ? yes N(2) C(3) C(2) 112.2(2) ? ? ? yes N(2) C(4) C(5) 110.7(2) ? ? ? yes N(3) C(5) C(4) 111.9(2) ? ? ? yes N(3) C(6) C(7) 109.6(2) ? ? ? yes N(1) C(7) C(6) 112.2(2) ? ? ? yes #------------------------------------------------------------------------------ data_A_TEXRAY.INF_file2 _database_code_CSD 159104 #------------------------------------------------------------------------------ _audit_creation_date 'Thu Sep 23 17:40:55 1999' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution ? _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #------------------------------------------------------------------------------ _cell_length_a 9.5317(3) _cell_length_b 15.6344(5) _cell_length_c 16.8035(4) _cell_angle_alpha 92.521(2) _cell_angle_beta 91.116(2) _cell_angle_gamma 105.705(1) _cell_volume 2407.0(1) _cell_formula_units_Z 2 _cell_measurement_temperature 273.2 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0.0 _cell_measurement_theta_max 0.0 #------------------------------------------------------------------------------ _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, -y, -z' #------------------------------------------------------------------------------ _exptl_crystal_description 'unknown' _exptl_crystal_colour 'unknown' _exptl_crystal_size_max 0.000 _exptl_crystal_size_mid 0.000 _exptl_crystal_size_min 0.000 _exptl_crystal_density_diffrn 1.652 _exptl_crystal_density_meas ? _chemical_formula_weight 1197.11 _chemical_formula_analytical ? _chemical_formula_sum 'C27 H71 Cl4 N9 O26 Ni2 ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 1256.00 _exptl_absorpt_coefficient_mu 1.099 _exptl_absorpt_correction_type none #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 273.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoKalpha _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector ? _diffrn_measurement_device 'unknown' _diffrn_measurement_method 'omega scans with profile analysis' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 12062 _reflns_number_total 12062 _reflns_number_observed 6366 _reflns_observed_criterion 3.00 _diffrn_reflns_av_R_equivalents 0.00 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 30.08 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ni 0 4 0.339 1.112 'International Tables' Cl 0 8 0.148 0.159 'International Tables' O 0 52 0.011 0.006 'International Tables' C 0 54 0.003 0.002 'International Tables' N 0 18 0.006 0.003 'International Tables' H 0 142 0.000 0.000 'International Tables' #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom Ni(1) 0.20196(10) 0.91097(6) 0.28108(5) 0.0224(3) Uij ? ? Ni(2) 0.1713(1) 1.40270(7) 0.22342(6) 0.0371(3) Uij ? ? Cl(1) -0.4345(2) 0.2025(2) 0.0190(1) 0.0415(7) Uij ? ? Cl(2) 0.2618(3) 0.4412(2) -0.1553(1) 0.0492(7) Uij ? ? Cl(3) 0.5068(3) 0.3208(2) 0.5721(2) 0.0629(9) Uij ? ? Cl(4) 0.8526(2) 0.1113(2) 0.4021(1) 0.0437(7) Uij ? ? O(1) -0.0013(8) 1.3696(5) 0.2979(4) 0.071(3) Uij ? ? O(2) 0.2956(6) 1.3501(4) 0.3009(3) 0.047(2) Uij ? ? O(3) 0.2378(7) 1.5253(4) 0.2912(4) 0.064(2) Uij ? ? O(4) -0.5722(7) 0.2037(5) -0.0128(4) 0.072(3) Uij ? ? O(5) -0.329(1) 0.2720(8) -0.0173(5) 0.134(4) Uij ? ? O(6) -0.4200(7) 0.2227(4) 0.1033(3) 0.051(2) Uij ? ? O(7) -0.404(1) 0.1243(8) -0.0023(7) 0.155(5) Uij ? ? O(8) 0.3255(7) 0.5257(4) -0.1141(5) 0.069(2) Uij ? ? O(9) 0.190(1) 0.3783(5) -0.1002(4) 0.095(3) Uij ? ? O(10) 0.3733(8) 0.4118(4) -0.1965(5) 0.070(3) Uij ? ? O(11) 0.1556(7) 0.4511(5) -0.2133(5) 0.076(3) Uij ? ? O(12) 0.3898(8) 0.2478(5) 0.5500(5) 0.087(3) Uij ? ? O(13) 0.523(1) 0.3824(6) 0.5118(5) 0.111(4) Uij ? ? O(14) 0.474(1) 0.3614(9) 0.6478(6) 0.155(5) Uij ? ? O(15) 0.6387(8) 0.2974(5) 0.5812(6) 0.095(3) Uij ? ? O(16) 0.7844(8) 0.1037(6) 0.3254(3) 0.081(3) Uij ? ? O(17) 0.9964(8) 0.1515(10) 0.3987(5) 0.163(5) Uij ? ? O(18) 0.792(1) 0.1606(7) 0.4559(4) 0.112(4) Uij ? ? O(19) 0.824(1) 0.0263(6) 0.4340(5) 0.109(4) Uij ? ? O(20) 0.4968(8) 0.2559(5) 0.8148(4) 0.064(2) Uij ? ? O(21) 0.948(1) 0.4765(8) 0.5895(8) 0.163(6) Uij ? ? O(22) 0.194(1) 0.4656(9) 0.5279(7) 0.139(5) Uij ? ? O(23) 0.1940(9) 0.3100(8) 0.4486(5) 0.123(4) Uij ? ? O(24) 0.614(1) 0.2557(7) 0.3845(6) 0.133(5) Uij ? ? O(25) 0.7088(9) 0.3301(6) 0.2476(5) 0.098(3) Uij ? ? O(26) 0.5850(9) 0.4580(7) 0.3277(6) 0.107(4) Uij ? ? N(1) 0.0763(6) 0.8458(4) 0.1796(4) 0.026(2) Uij ? ? N(2) 0.1454(7) 0.7805(4) 0.3196(4) 0.037(2) Uij ? ? N(3) -0.0082(7) 0.9071(5) 0.3248(4) 0.033(2) Uij ? ? N(4) 0.2946(7) 1.0444(4) 0.2413(4) 0.037(2) Uij ? ? N(5) 0.4149(6) 0.9000(4) 0.2569(3) 0.027(2) Uij ? ? N(6) 0.3050(7) 0.9728(4) 0.3885(4) 0.028(2) Uij ? ? N(7) 0.0951(6) 1.2855(4) 0.1470(4) 0.027(2) Uij ? ? N(8) 0.3386(8) 1.4346(4) 0.1458(4) 0.037(2) Uij ? ? N(9) 0.0675(9) 1.4617(6) 0.1389(5) 0.060(3) Uij ? ? C(1) 0.1316(9) 0.7648(5) 0.1690(5) 0.038(3) Uij ? ? C(2) 0.1373(9) 0.7191(6) 0.2475(6) 0.043(3) Uij ? ? C(3) 0.0107(10) 0.7614(6) 0.3670(5) 0.044(3) Uij ? ? C(4) -0.0306(9) 0.8434(7) 0.3889(5) 0.050(3) Uij ? ? C(5) -0.1194(8) 0.8811(5) 0.2598(4) 0.030(2) Uij ? ? C(6) -0.0820(8) 0.8164(5) 0.2006(5) 0.031(2) Uij ? ? C(7) 0.4575(10) 1.0569(7) 0.2351(7) 0.064(4) Uij ? ? C(8) 0.4843(9) 0.9723(8) 0.2045(6) 0.059(3) Uij ? ? C(9) 0.4955(9) 0.9059(6) 0.3324(5) 0.038(3) Uij ? ? C(10) 0.4432(10) 0.9487(7) 0.4011(5) 0.053(3) Uij ? ? C(11) 0.315(2) 1.0688(7) 0.3912(6) 0.088(4) Uij ? ? C(12) 0.266(1) 1.0982(6) 0.3111(5) 0.062(3) Uij ? ? C(13) 0.2108(9) 1.2869(5) 0.0890(5) 0.036(3) Uij ? ? C(14) 0.356(1) 1.3471(6) 0.1133(6) 0.047(3) Uij ? ? C(15) 0.313(1) 1.4917(6) 0.0827(6) 0.062(3) Uij ? ? C(16) 0.192(1) 1.5296(6) 0.1069(6) 0.059(3) Uij ? ? C(17) -0.012(1) 1.3924(7) 0.0799(7) 0.065(4) Uij ? ? C(18) -0.0357(8) 1.3000(6) 0.1066(5) 0.038(3) Uij ? ? C(19) 0.0935(8) 0.8924(6) 0.1042(5) 0.031(2) Uij ? ? C(20) 0.2465(8) 1.0770(5) 0.1658(5) 0.030(2) Uij ? ? C(21) 0.0596(9) 1.2052(6) 0.1954(4) 0.034(2) Uij ? ? C(22) 0.0224(8) 0.9688(5) 0.1067(4) 0.028(2) Uij ? ? C(23) 0.0855(8) 1.0514(5) 0.1436(4) 0.021(2) Uij ? ? C(24) 0.0036(8) 1.1142(5) 0.1511(4) 0.028(2) Uij ? ? C(25) -0.1416(9) 1.0894(6) 0.1219(5) 0.033(2) Uij ? ? C(26) -0.1991(8) 1.0113(6) 0.0806(5) 0.031(2) Uij ? ? C(27) -0.1212(8) 0.9493(5) 0.0722(4) 0.032(2) Uij ? ? H(1) 0.0678 0.7230 0.1322 0.0463 Uij ? ? H(2) 0.2265 0.7810 0.1485 0.0463 Uij ? ? H(3) 0.0523 0.6711 0.2495 0.0513 Uij ? ? H(4) 0.2212 0.6975 0.2479 0.0513 Uij ? ? H(5) -0.0672 0.7223 0.3366 0.0538 Uij ? ? H(6) 0.0277 0.7343 0.4145 0.0538 Uij ? ? H(7) 0.2230 0.7748 0.3532 0.0449 Uij ? ? H(8) -0.1307 0.8272 0.4017 0.0584 Uij ? ? H(9) 0.0267 0.8713 0.4346 0.0584 Uij ? ? H(10) -0.0076 0.9639 0.3472 0.0395 Uij ? ? H(11) -0.2112 0.8545 0.2813 0.0357 Uij ? ? H(12) -0.1240 0.9332 0.2336 0.0357 Uij ? ? H(13) -0.1009 0.7600 0.2226 0.0376 Uij ? ? H(14) -0.1409 0.8123 0.1534 0.0376 Uij ? ? H(15) 0.4959 1.1027 0.2000 0.0768 Uij ? ? H(16) 0.5036 1.0737 0.2867 0.0768 Uij ? ? H(17) 0.4431 0.9573 0.1523 0.0731 Uij ? ? H(18) 0.5857 0.9779 0.2042 0.0731 Uij ? ? H(19) 0.4079 0.8442 0.2301 0.0322 Uij ? ? H(20) 0.4907 0.8465 0.3461 0.0437 Uij ? ? H(21) 0.5936 0.9372 0.3247 0.0437 Uij ? ? H(22) 0.4321 0.9109 0.4437 0.0635 Uij ? ? H(23) 0.5168 1.0030 0.4149 0.0635 Uij ? ? H(24) 0.2437 0.9479 0.4306 0.0328 Uij ? ? H(25) 0.4126 1.1019 0.4025 0.1071 Uij ? ? H(26) 0.2539 1.0818 0.4314 0.1071 Uij ? ? H(27) 0.1634 1.0911 0.3125 0.0744 Uij ? ? H(28) 0.3155 1.1580 0.3055 0.0744 Uij ? ? H(29) 0.2199 1.2280 0.0821 0.0433 Uij ? ? H(30) 0.1816 1.3056 0.0401 0.0433 Uij ? ? H(31) 0.3993 1.3201 0.1542 0.0562 Uij ? ? H(32) 0.4172 1.3558 0.0692 0.0562 Uij ? ? H(33) 0.4252 1.4653 0.1752 0.0453 Uij ? ? H(34) 0.3985 1.5385 0.0763 0.0752 Uij ? ? H(35) 0.2862 1.4576 0.0342 0.0752 Uij ? ? H(36) 0.2277 1.5762 0.1472 0.0698 Uij ? ? H(37) 0.1581 1.5546 0.0619 0.0698 Uij ? ? H(38) 0.0024 1.4901 0.1638 0.0742 Uij ? ? H(39) 0.0427 1.3972 0.0324 0.0780 Uij ? ? H(40) -0.1040 1.4020 0.0682 0.0780 Uij ? ? H(41) -0.0622 1.2598 0.0617 0.0446 Uij ? ? H(42) -0.1128 1.2892 0.1431 0.0446 Uij ? ? H(43) 0.0493 0.8508 0.0621 0.0375 Uij ? ? H(44) 0.1945 0.9151 0.0953 0.0375 Uij ? ? H(45) 0.2944 1.0561 0.1231 0.0349 Uij ? ? H(46) 0.2781 1.1406 0.1698 0.0349 Uij ? ? H(47) 0.1454 1.2046 0.2246 0.0405 Uij ? ? H(48) -0.0135 1.2112 0.2312 0.0405 Uij ? ? H(49) -0.2007 1.1292 0.1312 0.0395 Uij ? ? H(50) -0.2946 0.9987 0.0570 0.0375 Uij ? ? H(51) -0.1621 0.8942 0.0438 0.0375 Uij ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ni(1) 0.0181(5) 0.0219(6) 0.0267(5) 0.0050(4) 0.0024(4) -0.0016(4) Ni(2) 0.0391(7) 0.0389(7) 0.0396(7) 0.0245(6) -0.0087(5) -0.0144(5) Cl(1) 0.034(1) 0.043(1) 0.051(1) 0.019(1) -0.002(1) -0.010(1) Cl(2) 0.047(1) 0.030(1) 0.063(2) 0.001(1) -0.013(1) -0.008(1) Cl(3) 0.060(2) 0.064(2) 0.064(2) 0.016(2) -0.013(1) 0.007(1) Cl(4) 0.036(1) 0.064(2) 0.028(1) 0.007(1) 0.0072(9) -0.001(1) O(1) 0.060(5) 0.090(6) 0.064(5) 0.029(4) 0.012(4) -0.026(4) O(2) 0.054(4) 0.058(4) 0.036(3) 0.029(3) -0.015(3) 0.003(3) O(3) 0.070(5) 0.056(5) 0.072(5) 0.034(4) -0.029(4) -0.029(4) O(4) 0.036(4) 0.105(6) 0.083(5) 0.039(4) -0.015(4) -0.045(5) O(5) 0.107(7) 0.18(1) 0.056(5) -0.057(7) 0.014(5) 0.011(6) O(6) 0.057(4) 0.057(4) 0.039(4) 0.014(4) 0.009(3) 0.006(3) O(7) 0.21(1) 0.154(10) 0.152(9) 0.157(10) -0.100(9) -0.093(8) O(8) 0.060(5) 0.033(4) 0.105(6) 0.003(3) -0.018(4) -0.023(4) O(9) 0.138(8) 0.056(5) 0.056(5) -0.034(5) 0.002(5) 0.004(4) O(10) 0.076(5) 0.044(4) 0.095(6) 0.027(4) -0.018(4) -0.015(4) O(11) 0.047(4) 0.084(6) 0.091(6) 0.011(4) -0.025(4) -0.005(5) O(12) 0.052(5) 0.068(6) 0.130(7) 0.001(4) -0.035(5) 0.001(5) O(13) 0.136(8) 0.098(7) 0.100(7) 0.022(6) -0.005(6) 0.059(6) O(14) 0.16(1) 0.25(2) 0.074(6) 0.10(1) -0.001(7) -0.059(8) O(15) 0.061(5) 0.075(6) 0.157(8) 0.030(5) -0.012(5) 0.015(6) O(16) 0.074(5) 0.114(7) 0.026(3) -0.023(5) -0.008(3) 0.007(4) O(17) 0.030(5) 0.35(2) 0.064(5) -0.029(7) -0.007(4) 0.057(8) O(18) 0.184(10) 0.139(8) 0.052(5) 0.116(8) -0.029(6) -0.022(5) O(19) 0.166(10) 0.098(8) 0.068(5) 0.045(7) -0.014(6) 0.000(5) O(20) 0.080(5) 0.063(5) 0.065(4) 0.047(4) 0.004(4) 0.002(4) O(21) 0.16(1) 0.116(10) 0.20(1) 0.011(8) -0.009(10) -0.033(9) O(22) 0.105(8) 0.18(1) 0.138(9) 0.042(8) 0.008(7) -0.001(8) O(23) 0.077(6) 0.22(1) 0.072(6) 0.037(7) 0.020(5) 0.055(7) O(24) 0.16(1) 0.111(9) 0.121(8) 0.025(8) -0.010(8) 0.001(7) O(25) 0.072(6) 0.119(8) 0.102(6) 0.025(5) 0.010(5) 0.005(6) O(26) 0.067(6) 0.140(9) 0.111(7) 0.021(6) -0.004(5) 0.048(6) N(1) 0.018(3) 0.026(4) 0.035(4) 0.009(3) 0.005(3) -0.003(3) N(2) 0.033(4) 0.027(4) 0.047(4) 0.004(3) -0.004(3) 0.007(3) N(3) 0.030(4) 0.041(4) 0.030(4) 0.012(3) 0.001(3) -0.008(3) N(4) 0.036(4) 0.034(4) 0.041(4) 0.007(3) -0.013(3) 0.005(3) N(5) 0.022(3) 0.031(4) 0.027(3) 0.006(3) 0.005(3) -0.003(3) N(6) 0.029(4) 0.028(4) 0.028(4) 0.013(3) -0.003(3) -0.002(3) N(7) 0.026(4) 0.029(4) 0.029(4) 0.014(3) -0.004(3) -0.001(3) N(8) 0.050(5) 0.023(4) 0.038(4) 0.008(3) -0.003(3) -0.003(3) N(9) 0.065(6) 0.050(5) 0.075(6) 0.045(5) -0.044(5) -0.036(5) C(1) 0.039(5) 0.022(5) 0.051(5) 0.009(4) 0.002(4) -0.022(4) C(2) 0.037(5) 0.027(5) 0.066(6) 0.010(4) -0.004(5) 0.006(5) C(3) 0.039(5) 0.037(6) 0.049(6) -0.006(4) 0.008(4) 0.014(5) C(4) 0.024(5) 0.082(8) 0.036(5) 0.001(5) 0.009(4) 0.012(5) C(5) 0.018(4) 0.041(5) 0.030(4) 0.006(4) 0.005(3) 0.003(4) C(6) 0.024(4) 0.026(5) 0.036(4) -0.003(4) 0.001(4) -0.004(4) C(7) 0.034(6) 0.055(7) 0.094(8) -0.012(5) -0.022(6) 0.053(6) C(8) 0.013(5) 0.107(10) 0.059(6) 0.016(5) 0.005(4) 0.035(7) C(9) 0.034(5) 0.037(5) 0.044(5) 0.014(4) 0.001(4) 0.001(4) C(10) 0.039(5) 0.096(8) 0.036(5) 0.040(6) -0.008(4) -0.012(5) C(11) 0.16(1) 0.039(7) 0.062(7) 0.037(8) -0.064(8) -0.010(5) C(12) 0.116(9) 0.028(6) 0.039(5) 0.017(6) -0.034(6) -0.007(4) C(13) 0.041(5) 0.027(5) 0.043(5) 0.013(4) 0.013(4) -0.008(4) C(14) 0.053(6) 0.030(5) 0.056(6) 0.009(5) 0.015(5) -0.013(4) C(15) 0.080(8) 0.036(6) 0.064(7) 0.006(6) -0.030(6) 0.003(5) C(16) 0.089(8) 0.024(6) 0.067(7) 0.021(6) -0.016(6) -0.004(5) C(17) 0.064(7) 0.052(7) 0.088(8) 0.036(6) -0.033(6) -0.006(6) C(18) 0.027(5) 0.043(6) 0.047(5) 0.014(4) -0.010(4) 0.006(4) C(19) 0.020(4) 0.042(5) 0.031(4) 0.008(4) 0.002(3) -0.001(4) C(20) 0.023(4) 0.026(5) 0.039(5) 0.006(4) -0.004(4) 0.003(4) C(21) 0.042(5) 0.038(5) 0.027(4) 0.019(4) 0.005(4) 0.004(4) C(22) 0.026(4) 0.041(5) 0.018(4) 0.013(4) 0.004(3) -0.002(4) C(23) 0.020(4) 0.025(4) 0.021(4) 0.009(3) -0.001(3) 0.001(3) C(24) 0.030(5) 0.035(5) 0.018(4) 0.008(4) 0.005(3) 0.003(3) C(25) 0.026(5) 0.041(6) 0.036(5) 0.016(4) 0.014(4) 0.007(4) C(26) 0.020(4) 0.045(6) 0.030(4) 0.010(4) 0.004(3) 0.011(4) C(27) 0.031(5) 0.037(5) 0.025(4) 0.005(4) 0.001(4) -0.004(4) #------------------------------------------------------------------------------ _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 6366 _refine_ls_number_parameters 613 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0919 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.1038 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 3.895 _refine_ls_shift/esd_max 0.0473 _refine_ls_shift/esd_mean ? _refine_diff_density_min -1.36 _refine_diff_density_max 1.39 #------------------------------------------------------------------------------ _geom_special_details ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni(1) N(1) 2.118(6) ? ? yes Ni(1) N(2) 2.099(7) ? ? yes Ni(1) N(3) 2.134(6) ? ? yes Ni(1) N(4) 2.174(7) ? ? yes Ni(1) N(5) 2.128(6) ? ? yes Ni(1) N(6) 2.103(6) ? ? yes Ni(2) O(1) 2.054(7) ? ? yes Ni(2) O(2) 2.083(5) ? ? yes Ni(2) O(3) 2.119(6) ? ? yes Ni(2) N(7) 2.138(6) ? ? yes Ni(2) N(8) 2.050(7) ? ? yes Ni(2) N(9) 2.099(7) ? ? yes Cl(1) O(4) 1.412(6) ? ? yes Cl(1) O(5) 1.434(9) ? ? yes Cl(1) O(6) 1.433(6) ? ? yes Cl(1) O(7) 1.367(8) ? ? yes Cl(2) O(8) 1.436(7) ? ? yes Cl(2) O(9) 1.428(8) ? ? yes Cl(2) O(10) 1.444(8) ? ? yes Cl(2) O(11) 1.434(7) ? ? yes Cl(3) O(12) 1.394(7) ? ? yes Cl(3) O(13) 1.410(8) ? ? yes Cl(3) O(14) 1.473(9) ? ? yes Cl(3) O(15) 1.408(7) ? ? yes Cl(4) O(16) 1.419(6) ? ? yes Cl(4) O(17) 1.347(8) ? ? yes Cl(4) O(18) 1.393(8) ? ? yes Cl(4) O(19) 1.414(9) ? ? yes N(1) C(1) 1.502(10) ? ? yes N(1) C(6) 1.507(10) ? ? yes N(1) C(19) 1.480(10) ? ? yes N(2) C(2) 1.50(1) ? ? yes N(2) C(3) 1.49(1) ? ? yes N(3) C(4) 1.48(1) ? ? yes N(3) C(5) 1.471(9) ? ? yes N(4) C(7) 1.52(1) ? ? yes N(4) C(12) 1.49(1) ? ? yes N(4) C(20) 1.497(10) ? ? yes N(5) C(8) 1.48(1) ? ? yes N(5) C(9) 1.456(10) ? ? yes N(6) C(10) 1.479(10) ? ? yes N(6) C(11) 1.48(1) ? ? yes N(7) C(13) 1.48(1) ? ? yes N(7) C(18) 1.483(8) ? ? yes N(7) C(21) 1.491(10) ? ? yes N(8) C(14) 1.50(1) ? ? yes N(8) C(15) 1.47(1) ? ? yes N(9) C(16) 1.49(1) ? ? yes N(9) C(17) 1.47(1) ? ? yes C(1) C(2) 1.54(1) ? ? yes C(3) C(4) 1.47(1) ? ? yes C(5) C(6) 1.50(1) ? ? yes C(7) C(8) 1.49(2) ? ? yes C(9) C(10) 1.47(1) ? ? yes C(11) C(12) 1.54(1) ? ? yes C(13) C(14) 1.49(1) ? ? yes C(15) C(16) 1.49(2) ? ? yes C(17) C(18) 1.49(1) ? ? yes C(19) C(22) 1.53(1) ? ? yes C(20) C(23) 1.512(10) ? ? yes C(21) C(24) 1.53(1) ? ? yes C(22) C(23) 1.38(1) ? ? yes C(22) C(27) 1.42(1) ? ? yes C(23) C(24) 1.41(1) ? ? yes C(24) C(25) 1.40(1) ? ? yes C(25) C(26) 1.35(1) ? ? yes C(26) C(27) 1.38(1) ? ? yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N(1) Ni(1) N(2) 81.2(2) ? ? ? yes N(1) Ni(1) N(3) 82.2(2) ? ? ? yes N(1) Ni(1) N(4) 102.4(2) ? ? ? yes N(1) Ni(1) N(5) 103.3(2) ? ? ? yes N(1) Ni(1) N(6) 173.7(2) ? ? ? yes N(2) Ni(1) N(3) 81.5(3) ? ? ? yes N(2) Ni(1) N(4) 171.2(3) ? ? ? yes N(2) Ni(1) N(5) 89.7(3) ? ? ? yes N(2) Ni(1) N(6) 96.6(3) ? ? ? yes N(3) Ni(1) N(4) 106.9(3) ? ? ? yes N(3) Ni(1) N(5) 168.8(2) ? ? ? yes N(3) Ni(1) N(6) 91.6(2) ? ? ? yes N(4) Ni(1) N(5) 81.7(3) ? ? ? yes N(4) Ni(1) N(6) 80.7(2) ? ? ? yes N(5) Ni(1) N(6) 82.6(2) ? ? ? yes O(1) Ni(2) O(2) 90.1(3) ? ? ? yes O(1) Ni(2) O(3) 86.4(3) ? ? ? yes O(1) Ni(2) N(7) 94.3(3) ? ? ? yes O(1) Ni(2) N(8) 178.0(3) ? ? ? yes O(1) Ni(2) N(9) 96.1(3) ? ? ? yes O(2) Ni(2) O(3) 89.0(2) ? ? ? yes O(2) Ni(2) N(7) 96.4(2) ? ? ? yes O(2) Ni(2) N(8) 91.5(2) ? ? ? yes O(2) Ni(2) N(9) 173.7(3) ? ? ? yes O(3) Ni(2) N(7) 174.5(2) ? ? ? yes O(3) Ni(2) N(8) 94.8(3) ? ? ? yes O(3) Ni(2) N(9) 90.1(3) ? ? ? yes N(7) Ni(2) N(8) 84.3(2) ? ? ? yes N(7) Ni(2) N(9) 84.4(3) ? ? ? yes N(8) Ni(2) N(9) 82.3(3) ? ? ? yes O(4) Cl(1) O(5) 106.4(6) ? ? ? yes O(4) Cl(1) O(6) 112.6(4) ? ? ? yes O(4) Cl(1) O(7) 110.9(5) ? ? ? yes O(5) Cl(1) O(6) 106.8(4) ? ? ? yes O(5) Cl(1) O(7) 106.9(8) ? ? ? yes O(6) Cl(1) O(7) 112.7(5) ? ? ? yes O(8) Cl(2) O(9) 109.8(5) ? ? ? yes O(8) Cl(2) O(10) 109.7(4) ? ? ? yes O(8) Cl(2) O(11) 109.0(4) ? ? ? yes O(9) Cl(2) O(10) 111.7(5) ? ? ? yes O(9) Cl(2) O(11) 108.3(5) ? ? ? yes O(10) Cl(2) O(11) 108.4(5) ? ? ? yes O(12) Cl(3) O(13) 108.2(5) ? ? ? yes O(12) Cl(3) O(14) 108.5(7) ? ? ? yes O(12) Cl(3) O(15) 112.4(5) ? ? ? yes O(13) Cl(3) O(14) 110.0(7) ? ? ? yes O(13) Cl(3) O(15) 108.4(6) ? ? ? yes O(14) Cl(3) O(15) 109.3(6) ? ? ? yes O(16) Cl(4) O(17) 110.5(5) ? ? ? yes O(16) Cl(4) O(18) 111.5(5) ? ? ? yes O(16) Cl(4) O(19) 109.5(5) ? ? ? yes O(17) Cl(4) O(18) 108.3(8) ? ? ? yes O(17) Cl(4) O(19) 112.6(8) ? ? ? yes O(18) Cl(4) O(19) 104.3(6) ? ? ? yes Ni(1) N(1) C(1) 101.1(4) ? ? ? yes Ni(1) N(1) C(6) 109.2(4) ? ? ? yes Ni(1) N(1) C(19) 118.1(5) ? ? ? yes C(1) N(1) C(6) 108.5(6) ? ? ? yes C(1) N(1) C(19) 108.5(6) ? ? ? yes C(6) N(1) C(19) 110.6(5) ? ? ? yes Ni(1) N(2) C(2) 107.4(5) ? ? ? yes Ni(1) N(2) C(3) 111.9(5) ? ? ? yes C(2) N(2) C(3) 114.5(6) ? ? ? yes Ni(1) N(3) C(4) 105.0(5) ? ? ? yes Ni(1) N(3) C(5) 110.3(5) ? ? ? yes C(4) N(3) C(5) 113.5(6) ? ? ? yes Ni(1) N(4) C(7) 107.0(5) ? ? ? yes Ni(1) N(4) C(12) 100.2(5) ? ? ? yes Ni(1) N(4) C(20) 123.4(5) ? ? ? yes C(7) N(4) C(12) 109.9(8) ? ? ? yes C(7) N(4) C(20) 105.8(6) ? ? ? yes C(12) N(4) C(20) 110.2(6) ? ? ? yes Ni(1) N(5) C(8) 107.9(5) ? ? ? yes Ni(1) N(5) C(9) 108.4(5) ? ? ? yes C(8) N(5) C(9) 112.3(6) ? ? ? yes Ni(1) N(6) C(10) 109.4(5) ? ? ? yes Ni(1) N(6) C(11) 110.3(5) ? ? ? yes C(10) N(6) C(11) 116.5(8) ? ? ? yes Ni(2) N(7) C(13) 106.4(5) ? ? ? yes Ni(2) N(7) C(18) 102.8(5) ? ? ? yes Ni(2) N(7) C(21) 109.9(4) ? ? ? yes C(13) N(7) C(18) 110.4(6) ? ? ? yes C(13) N(7) C(21) 113.9(6) ? ? ? yes C(18) N(7) C(21) 112.6(6) ? ? ? yes Ni(2) N(8) C(14) 105.5(5) ? ? ? yes Ni(2) N(8) C(15) 113.1(6) ? ? ? yes C(14) N(8) C(15) 112.8(7) ? ? ? yes Ni(2) N(9) C(16) 102.4(5) ? ? ? yes Ni(2) N(9) C(17) 108.6(6) ? ? ? yes C(16) N(9) C(17) 114.7(9) ? ? ? yes N(1) C(1) C(2) 112.2(7) ? ? ? yes N(2) C(2) C(1) 112.9(7) ? ? ? yes N(2) C(3) C(4) 111.5(7) ? ? ? yes N(3) C(4) C(3) 113.3(7) ? ? ? yes N(3) C(5) C(6) 110.9(6) ? ? ? yes N(1) C(6) C(5) 111.4(6) ? ? ? yes N(4) C(7) C(8) 109.4(7) ? ? ? yes N(5) C(8) C(7) 109.3(8) ? ? ? yes N(5) C(9) C(10) 116.9(7) ? ? ? yes N(6) C(10) C(9) 116.5(7) ? ? ? yes N(6) C(11) C(12) 112.0(8) ? ? ? yes N(4) C(12) C(11) 112.9(8) ? ? ? yes N(7) C(13) C(14) 114.6(7) ? ? ? yes N(8) C(14) C(13) 109.5(7) ? ? ? yes N(8) C(15) C(16) 108.4(9) ? ? ? yes N(9) C(16) C(15) 112.2(8) ? ? ? yes N(9) C(17) C(18) 114.0(8) ? ? ? yes N(7) C(18) C(17) 112.9(7) ? ? ? yes N(1) C(19) C(22) 111.7(6) ? ? ? yes N(4) C(20) C(23) 118.5(6) ? ? ? yes N(7) C(21) C(24) 117.7(6) ? ? ? yes C(19) C(22) C(23) 123.9(6) ? ? ? yes C(19) C(22) C(27) 116.0(7) ? ? ? yes C(23) C(22) C(27) 120.0(7) ? ? ? yes C(20) C(23) C(22) 119.1(6) ? ? ? yes C(20) C(23) C(24) 120.9(7) ? ? ? yes C(22) C(23) C(24) 119.5(6) ? ? ? yes C(21) C(24) C(23) 123.7(7) ? ? ? yes C(21) C(24) C(25) 117.7(7) ? ? ? yes C(23) C(24) C(25) 118.4(7) ? ? ? yes C(24) C(25) C(26) 121.7(7) ? ? ? yes C(25) C(26) C(27) 120.7(7) ? ? ? yes C(22) C(27) C(26) 119.3(7) ? ? ? yes #------------------------------------------------------------------------------ ###END