# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Ghosh, Ashutosh' _publ_contact_author_email 'ghosh 59@yahoo.com' _publ_section_title ; Structural and magnetic studies of Schiff base complexes of nickel(II) nitrite: solvent-assisted single-crystal-to-single-crystal transformation, ligand rearrangement and a very rare bridging mode ; loop_ _publ_author_name S.Naiya Y.Song A.Ghosh D.Hui-Sheng M.G.B.Drew # Attachment '- (1-4) revised.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 786102' #TrackingRef '- (1-4) revised.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H38 Cl2 N6 Ni2 O9' _chemical_formula_weight 730.92 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' O O 0.0106 0.0060 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/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 19.404(4) _cell_length_b 16.111(3) _cell_length_c 7.3647(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.17(2) _cell_angle_gamma 90.00 _cell_volume 2302.3(7) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 15183 _cell_measurement_theta_min 2.45 _cell_measurement_theta_max 30.00 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.054 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 760 _exptl_absorpt_coefficient_mu 0.972 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'ABSPACK, Oxford Diffraction Ltd' _exptl_absorpt_correction_T_min 0.889 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_standards_number n/a _diffrn_measurement_device 'Oxford Diffaction X-Calibur System' _diffrn_measurement_method '321 frames, counting time 10 s.' _diffrn_standards_interval_count n/a _diffrn_standards_interval_time n/a _diffrn_standards_decay_% n/a _diffrn_reflns_number 15183 _diffrn_reflns_av_R_equivalents 0.1122 _diffrn_reflns_av_sigmaI/netI 0.3506 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 5 _diffrn_reflns_theta_min 2.45 _diffrn_reflns_theta_max 30.00 _reflns_number_total 6639 _reflns_number_gt 2259 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Crysalis, Oxford Diffraction' _computing_cell_refinement 'Crysalis, Oxford Diffraction' _computing_data_reduction 'Crysalis, Oxford Diffraction' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics PLATON(Spek,2004) _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. Distance constraints were imposed on the solvent molecules The crystal suffered from merohedral twinning (the beta angle being close to 90) and the basf factor was refined to 0.50(2) ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc #_refine_ls_weighting_details _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0944P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6639 _refine_ls_number_parameters 188 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.1878 _refine_ls_R_factor_gt 0.0870 _refine_ls_wR_factor_ref 0.2305 _refine_ls_wR_factor_gt 0.2072 _refine_ls_goodness_of_fit_ref 0.804 _refine_ls_restrained_S_all 0.835 _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 Ni1 Ni 0.05846(7) -0.04904(6) 0.41257(15) 0.0336(3) Uani 1 1 d . . . O11 O -0.0411(2) -0.0369(3) 0.3817(6) 0.0266(13) Uani 1 1 d U . . C12 C -0.0850(3) -0.0938(4) 0.3132(8) 0.0112(14) Uani 1 1 d U . . C13 C -0.1499(4) -0.0948(5) 0.3471(9) 0.0251(19) Uani 1 1 d . . . H23 H -0.1661 -0.0518 0.4196 0.030 Uiso 1 1 calc R . . C14 C -0.2004(5) -0.1535(6) 0.2880(10) 0.037(2) Uani 1 1 d . . . H24 H -0.2462 -0.1505 0.3244 0.044 Uiso 1 1 calc R . . C15 C -0.1766(5) -0.2153(6) 0.1727(11) 0.043(3) Uani 1 1 d . . . H25 H -0.2064 -0.2548 0.1243 0.052 Uiso 1 1 calc R . . C16 C -0.1047(4) -0.2159(5) 0.1312(9) 0.0188(17) Uani 1 1 d . . . H26 H -0.0882 -0.2580 0.0566 0.023 Uiso 1 1 calc R . . C17 C -0.0567(4) -0.1558(4) 0.1975(8) 0.0136(14) Uani 1 1 d U . . C18 C 0.0113(4) -0.1599(5) 0.1419(10) 0.0168(18) Uani 1 1 d . . . H28 H 0.0197 -0.1953 0.0447 0.020 Uiso 1 1 calc R . . N19 N 0.0583(3) -0.1262(3) 0.1976(7) 0.0134(12) Uani 1 1 d . . . C20 C 0.1281(4) -0.1328(5) 0.1057(12) 0.034(2) Uani 1 1 d . . . H30A H 0.1260 -0.1773 0.0170 0.041 Uiso 1 1 calc R . . H30B H 0.1621 -0.1483 0.1963 0.041 Uiso 1 1 calc R . . C21 C 0.1541(6) -0.0497(6) 0.0052(12) 0.055(3) Uani 1 1 d . . . H31A H 0.1987 -0.0599 -0.0496 0.065 Uiso 1 1 calc R . . H31B H 0.1219 -0.0354 -0.0909 0.065 Uiso 1 1 calc R . . C22 C 0.1600(6) 0.0243(6) 0.1406(13) 0.056(3) Uani 1 1 d . . . H32A H 0.1960 0.0121 0.2282 0.068 Uiso 1 1 calc R . . H32B H 0.1737 0.0735 0.0741 0.068 Uiso 1 1 calc R . . N23 N 0.0958(4) 0.0421(4) 0.2389(8) 0.0317(17) Uani 1 1 d . . . H33A H 0.0628 0.0532 0.1562 0.038 Uiso 1 1 calc R . . H33B H 0.1023 0.0887 0.3043 0.038 Uiso 1 1 calc R . . O1 O 0.1507(3) -0.0997(4) 0.5209(9) 0.0529(18) Uani 1 1 d . . . N2 N 0.1206(5) -0.1507(5) 0.6215(11) 0.043(2) Uani 1 1 d . . . O3 O 0.0539(4) -0.1483(4) 0.6098(8) 0.0574(19) Uani 1 1 d . . . C1 C 0.4489(8) -0.0852(11) 0.625(2) 0.049(5) Uiso 0.50 1 d PD A 1 H1A H 0.4417 -0.0549 0.7369 0.059 Uiso 0.50 1 calc PR A 1 H1B H 0.4208 -0.1350 0.6247 0.059 Uiso 0.50 1 calc PR A 1 Cl11 Cl 0.5482(2) -0.1111(2) 0.5853(6) 0.0330(9) Uiso 0.50 1 d PD . 1 Cl12 Cl 0.4300(2) -0.0141(2) 0.4062(6) 0.0341(9) Uiso 0.50 1 d PD . 1 O71 O 0.3442(9) 0.0479(13) 0.568(3) 0.147(8) Uiso 0.50 1 d PD B 2 H71 H 0.3357 0.0518 0.4591 0.177 Uiso 0.50 1 calc PR B 2 C72 C 0.4158(9) 0.0835(12) 0.607(3) 0.064(6) Uiso 0.50 1 d PD B 2 H72A H 0.4354 0.1063 0.4963 0.077 Uiso 0.50 1 calc PR B 2 H72B H 0.4128 0.1275 0.6961 0.077 Uiso 0.50 1 calc PR B 2 C73 C 0.4596(11) 0.0145(15) 0.676(3) 0.093(9) Uiso 0.50 1 d PD B 2 H73A H 0.4309 -0.0268 0.7322 0.111 Uiso 0.50 1 calc PR B 2 H73B H 0.4916 0.0358 0.7645 0.111 Uiso 0.50 1 calc PR B 2 H73C H 0.4845 -0.0100 0.5776 0.111 Uiso 0.50 1 calc PR B 2 O100 O 0.3553(11) 0.0406(14) 0.108(4) 0.144(8) Uiso 0.50 1 d P C 2 O101 O 0.3270(12) -0.1437(16) 0.626(4) 0.159(9) Uiso 0.50 1 d P D 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0402(6) 0.0328(5) 0.0279(5) -0.0011(6) 0.0013(7) 0.0023(7) O11 0.0287(16) 0.0247(16) 0.0264(15) -0.0017(10) 0.0004(10) 0.0003(10) C12 0.0114(17) 0.0110(17) 0.0111(16) 0.0009(10) -0.0001(10) -0.0004(10) C13 0.037(5) 0.022(5) 0.017(4) 0.002(3) -0.009(4) 0.002(4) C14 0.054(6) 0.040(6) 0.016(4) 0.006(4) 0.013(4) -0.004(5) C15 0.063(7) 0.037(6) 0.030(4) 0.003(4) -0.012(5) -0.009(5) C16 0.019(4) 0.021(4) 0.016(4) -0.005(3) 0.002(3) 0.001(3) C17 0.0137(16) 0.0141(16) 0.0129(16) -0.0001(10) -0.0007(10) -0.0002(10) C18 0.005(4) 0.023(4) 0.023(4) 0.003(3) -0.004(3) 0.002(3) N19 0.009(3) 0.015(3) 0.016(3) 0.002(2) -0.004(3) 0.005(3) C20 0.041(5) 0.034(5) 0.027(4) -0.003(4) 0.000(4) 0.007(4) C21 0.062(7) 0.060(7) 0.041(5) 0.013(6) -0.012(5) -0.019(6) C22 0.073(8) 0.053(7) 0.043(6) -0.007(5) -0.008(5) -0.014(6) N23 0.050(5) 0.021(4) 0.024(3) 0.008(3) 0.001(3) -0.005(4) O1 0.054(5) 0.060(5) 0.045(4) -0.006(4) -0.005(3) 0.005(4) N2 0.051(6) 0.036(5) 0.043(5) 0.008(4) -0.006(4) 0.005(4) O3 0.086(6) 0.038(4) 0.048(4) -0.011(3) -0.017(5) 0.010(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 O11 1.955(5) . ? Ni1 N19 2.013(5) . ? Ni1 N23 2.079(6) . ? Ni1 O11 2.081(5) 3_556 ? Ni1 O1 2.121(7) . ? Ni1 O3 2.162(7) . ? O11 C12 1.348(8) . ? O11 Ni1 2.081(5) 3_556 ? C12 C13 1.285(10) . ? C12 C17 1.424(9) . ? C13 C14 1.429(11) . ? C14 C15 1.388(12) . ? C15 C16 1.430(11) . ? C16 C17 1.429(9) . ? C17 C18 1.383(10) . ? C18 N19 1.137(8) . ? N19 C20 1.518(10) . ? C20 C21 1.611(12) . ? C21 C22 1.559(12) . ? C22 N23 1.471(12) . ? O1 N2 1.252(9) . ? N2 O3 1.297(9) . ? C1 Cl11 1.994(15) . ? C1 Cl12 2.008(13) . ? Cl11 Cl12 2.062(5) 3_656 ? Cl12 Cl11 2.062(5) 3_656 ? O71 C72 1.528(16) . ? C72 C73 1.491(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 O11 Ni1 N19 88.4(2) . . ? O11 Ni1 N23 101.7(2) . . ? N19 Ni1 N23 87.3(2) . . ? O11 Ni1 O11 81.7(2) . 3_556 ? N19 Ni1 O11 169.7(2) . 3_556 ? N23 Ni1 O11 92.0(2) . 3_556 ? O11 Ni1 O1 156.2(3) . . ? N19 Ni1 O1 93.3(2) . . ? N23 Ni1 O1 102.0(3) . . ? O11 Ni1 O1 96.9(2) 3_556 . ? O11 Ni1 O3 96.3(3) . . ? N19 Ni1 O3 94.1(2) . . ? N23 Ni1 O3 161.9(3) . . ? O11 Ni1 O3 89.8(2) 3_556 . ? O1 Ni1 O3 59.9(3) . . ? C12 O11 Ni1 126.8(4) . . ? C12 O11 Ni1 128.4(4) . 3_556 ? Ni1 O11 Ni1 98.3(2) . 3_556 ? C13 C12 O11 123.7(7) . . ? C13 C12 C17 119.2(7) . . ? O11 C12 C17 117.1(6) . . ? C12 C13 C14 128.4(8) . . ? C15 C14 C13 115.6(8) . . ? C14 C15 C16 117.5(8) . . ? C17 C16 C15 123.9(7) . . ? C18 C17 C12 125.5(6) . . ? C18 C17 C16 119.2(6) . . ? C12 C17 C16 115.3(7) . . ? N19 C18 C17 129.5(8) . . ? C18 N19 C20 121.4(6) . . ? C18 N19 Ni1 125.2(6) . . ? C20 N19 Ni1 113.2(5) . . ? N19 C20 C21 115.3(7) . . ? C22 C21 C20 111.4(7) . . ? N23 C22 C21 113.8(8) . . ? C22 N23 Ni1 117.5(6) . . ? N2 O1 Ni1 94.7(5) . . ? O1 N2 O3 114.0(7) . . ? N2 O3 Ni1 91.4(5) . . ? Cl11 C1 Cl12 100.2(7) . . ? C1 Cl11 Cl12 89.4(5) . 3_656 ? C1 Cl12 Cl11 119.8(6) . 3_656 ? C73 C72 O71 107.5(14) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.121 _refine_diff_density_min -0.677 _refine_diff_density_rms 0.123 _publ_section_references ; Oxford Diffraction Ltd, Crysalis Program (2005) Oxford Diffraction Ltd, Abspack Program (2005) Sheldrick, G.M. (1997) SHELXL program for crystallography refinement. University of Gottingen, Germany. Spek, A.L., (2004) PLATON program, Utrecht University, The Netherlands ; #===END data_2 _database_code_depnum_ccdc_archive 'CCDC 786103' #TrackingRef '- (1-4) revised.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H47 Cl N8 Ni2 O11' _chemical_formula_weight 836.62 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.632(5) _cell_length_b 12.447(7) _cell_length_c 15.370(9) _cell_angle_alpha 87.403(17) _cell_angle_beta 85.004(19) _cell_angle_gamma 81.392(18) _cell_volume 1813.9(17) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 16871 _cell_measurement_theta_min 1.33 _cell_measurement_theta_max 22.53 _exptl_crystal_description needle _exptl_crystal_colour blue _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.532 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 876 _exptl_absorpt_coefficient_mu 1.179 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details SADABS _exptl_absorpt_correction_T_min 0.821 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_standards_number n/a _diffrn_measurement_device ? _diffrn_measurement_method ? _diffrn_standards_interval_count n/a _diffrn_standards_interval_time n/a _diffrn_standards_decay_% n/a _diffrn_reflns_number 16817 _diffrn_reflns_av_R_equivalents 0.1003 _diffrn_reflns_av_sigmaI/netI 0.0932 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.33 _diffrn_reflns_theta_max 22.53 _reflns_number_total 4729 _reflns_number_gt 3241 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics PLATON(Spek,2004) _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 _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.0378P)^2^+2.1536P] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4729 _refine_ls_number_parameters 466 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0896 _refine_ls_R_factor_gt 0.0498 _refine_ls_wR_factor_ref 0.1159 _refine_ls_wR_factor_gt 0.1009 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.011 _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 O1 O 0.2834(4) 0.4998(3) 0.0441(2) 0.0260(10) Uani 1 1 d . . . O3 O 0.1543(4) 0.4834(3) -0.0609(3) 0.0339(11) Uani 1 1 d . . . N2 N 0.2080(5) 0.4428(4) 0.0055(3) 0.0213(11) Uani 1 1 d . . . C12 C 0.5015(6) 0.2156(5) 0.0720(4) 0.0220(14) Uani 1 1 d . . . C13 C 0.6119(6) 0.1944(5) 0.1270(4) 0.0279(15) Uani 1 1 d . . . H13 H 0.6049 0.2300 0.1795 0.033 Uiso 1 1 calc R . . C14 C 0.7313(6) 0.1212(5) 0.1041(4) 0.0301(16) Uani 1 1 d . . . H14 H 0.8028 0.1073 0.1419 0.036 Uiso 1 1 calc R . . C15 C 0.7455(6) 0.0690(5) 0.0266(4) 0.0315(16) Uani 1 1 d . . . H15 H 0.8271 0.0218 0.0105 0.038 Uiso 1 1 calc R . . C16 C 0.6373(6) 0.0874(5) -0.0269(4) 0.0294(16) Uani 1 1 d . . . H16 H 0.6475 0.0522 -0.0796 0.035 Uiso 1 1 calc R . . C17 C 0.5125(6) 0.1568(4) -0.0055(4) 0.0208(14) Uani 1 1 d . . . C18 C 0.4029(6) 0.1661(5) -0.0659(4) 0.0267(15) Uani 1 1 d . . . H18 H 0.4284 0.1322 -0.1188 0.032 Uiso 1 1 calc R . . C20 C 0.1922(6) 0.2164(5) -0.1320(4) 0.0312(16) Uani 1 1 d . . . H20A H 0.2376 0.1603 -0.1710 0.037 Uiso 1 1 calc R . . H20B H 0.1928 0.2859 -0.1632 0.037 Uiso 1 1 calc R . . C21 C 0.0393(6) 0.1988(5) -0.1092(4) 0.0285(15) Uani 1 1 d . . . H21A H -0.0033 0.1907 -0.1629 0.034 Uiso 1 1 calc R . . H21B H 0.0388 0.1314 -0.0751 0.034 Uiso 1 1 calc R . . C22 C -0.0498(6) 0.2884(5) -0.0591(4) 0.0293(15) Uani 1 1 d . . . H22A H -0.0372 0.3577 -0.0878 0.035 Uiso 1 1 calc R . . H22B H -0.1482 0.2800 -0.0597 0.035 Uiso 1 1 calc R . . C32 C 0.0368(6) 0.3931(5) 0.2254(4) 0.0211(14) Uani 1 1 d . . . C33 C -0.0654(6) 0.3231(5) 0.2394(4) 0.0281(15) Uani 1 1 d . . . H33 H -0.0484 0.2547 0.2152 0.034 Uiso 1 1 calc R . . C34 C -0.1910(6) 0.3547(6) 0.2887(4) 0.0326(17) Uani 1 1 d . . . H34 H -0.2565 0.3067 0.2974 0.039 Uiso 1 1 calc R . . C35 C -0.2211(6) 0.4549(6) 0.3250(4) 0.0379(17) Uani 1 1 d . . . H35 H -0.3069 0.4756 0.3568 0.045 Uiso 1 1 calc R . . C36 C -0.1214(6) 0.5249(5) 0.3136(4) 0.0330(16) Uani 1 1 d . . . H36 H -0.1413 0.5931 0.3380 0.040 Uiso 1 1 calc R . . C37 C 0.0090(5) 0.4953(5) 0.2661(4) 0.0228(14) Uani 1 1 d . . . C38 C 0.1062(6) 0.5739(5) 0.2608(4) 0.0265(15) Uani 1 1 d . . . H38 H 0.0717 0.6411 0.2843 0.032 Uiso 1 1 calc R . . C40 C 0.3057(6) 0.6598(5) 0.2292(4) 0.0299(16) Uani 1 1 d . . . H40A H 0.2618 0.7036 0.2775 0.036 Uiso 1 1 calc R . . H40B H 0.2908 0.7027 0.1756 0.036 Uiso 1 1 calc R . . C41 C 0.4621(6) 0.6345(5) 0.2387(4) 0.0314(16) Uani 1 1 d . . . H41A H 0.4775 0.5838 0.2879 0.038 Uiso 1 1 calc R . . H41B H 0.4963 0.7009 0.2519 0.038 Uiso 1 1 calc R . . C42 C 0.5478(6) 0.5866(5) 0.1586(4) 0.0347(17) Uani 1 1 d . . . H42A H 0.5180 0.6289 0.1071 0.042 Uiso 1 1 calc R . . H42B H 0.6463 0.5919 0.1631 0.042 Uiso 1 1 calc R . . C82 C 0.3833(6) 0.3700(5) 0.3571(4) 0.0279(15) Uani 1 1 d . . . H82 H 0.3272 0.4365 0.3674 0.033 Uiso 1 1 calc R . . N83 N 0.4381(5) 0.3161(4) 0.4245(3) 0.0323(13) Uani 1 1 d . . . C84 C 0.4132(8) 0.3607(6) 0.5115(4) 0.061(2) Uani 1 1 d . . . H84A H 0.3578 0.4314 0.5084 0.092 Uiso 1 1 calc R . . H84B H 0.5018 0.3665 0.5338 0.092 Uiso 1 1 calc R . . H84C H 0.3637 0.3134 0.5497 0.092 Uiso 1 1 calc R . . C85 C 0.5238(6) 0.2109(5) 0.4173(4) 0.0387(17) Uani 1 1 d . . . H85A H 0.5331 0.1896 0.3575 0.058 Uiso 1 1 calc R . . H85B H 0.4800 0.1584 0.4534 0.058 Uiso 1 1 calc R . . H85C H 0.6154 0.2147 0.4361 0.058 Uiso 1 1 calc R . . C92 C 0.2389(6) 0.1208(5) 0.1963(4) 0.0256(15) Uani 1 1 d . . . H92 H 0.3033 0.1665 0.2067 0.031 Uiso 1 1 calc R . . N93 N 0.2186(5) 0.0431(4) 0.2555(3) 0.0285(13) Uani 1 1 d . . . C94 C 0.1181(8) -0.0293(6) 0.2443(5) 0.059(2) Uani 1 1 d . . . H94A H 0.0863 -0.0183 0.1866 0.088 Uiso 1 1 calc R . . H94B H 0.0392 -0.0144 0.2868 0.088 Uiso 1 1 calc R . . H94C H 0.1620 -0.1032 0.2520 0.088 Uiso 1 1 calc R . . C95 C 0.2979(8) 0.0255(6) 0.3322(5) 0.063(2) Uani 1 1 d . . . H95A H 0.3589 0.0797 0.3327 0.095 Uiso 1 1 calc R . . H95B H 0.3532 -0.0454 0.3309 0.095 Uiso 1 1 calc R . . H95C H 0.2339 0.0305 0.3839 0.095 Uiso 1 1 calc R . . O71 O 0.7640(8) 0.3838(6) 0.5566(4) 0.097(2) Uani 1 1 d . . . C72 C 0.8576(17) 0.3521(14) 0.5248(9) 0.184(9) Uani 1 1 d . . . H72 H 0.9052 0.4112 0.5116 0.220 Uiso 1 1 calc R . . N73 N 0.9423(6) 0.2688(6) 0.4939(4) 0.0571(18) Uani 1 1 d . . . C74 C 0.9101(10) 0.1631(8) 0.5001(7) 0.112(4) Uani 1 1 d . . . H74A H 0.9109 0.1360 0.4426 0.168 Uiso 1 1 calc R . . H74B H 0.8183 0.1631 0.5300 0.168 Uiso 1 1 calc R . . H74C H 0.9788 0.1175 0.5321 0.168 Uiso 1 1 calc R . . C75 C 1.0773(10) 0.2867(10) 0.4537(7) 0.119(5) Uani 1 1 d . . . H75A H 1.1487 0.2609 0.4927 0.179 Uiso 1 1 calc R . . H75B H 1.0769 0.3631 0.4414 0.179 Uiso 1 1 calc R . . H75C H 1.0968 0.2482 0.4003 0.179 Uiso 1 1 calc R . . N19 N 0.2752(5) 0.2149(4) -0.0559(3) 0.0230(12) Uani 1 1 d . . . N23 N -0.0138(4) 0.2891(4) 0.0330(3) 0.0260(12) Uani 1 1 d . . . H23A H -0.0447 0.2313 0.0615 0.031 Uiso 1 1 calc R . . H23B H -0.0634 0.3490 0.0572 0.031 Uiso 1 1 calc R . . N39 N 0.2353(5) 0.5622(4) 0.2272(3) 0.0226(12) Uani 1 1 d . . . N43 N 0.5328(4) 0.4721(4) 0.1476(3) 0.0266(12) Uani 1 1 d . . . H43A H 0.5880 0.4313 0.1846 0.032 Uiso 1 1 calc R . . H43B H 0.5679 0.4543 0.0931 0.032 Uiso 1 1 calc R . . O81 O 0.4005(4) 0.3392(3) 0.2805(3) 0.0252(10) Uani 1 1 d . . . O91 O 0.1781(4) 0.1372(3) 0.1278(3) 0.0250(10) Uani 1 1 d . . . O11 O 0.3885(4) 0.2868(3) 0.0943(2) 0.0215(9) Uani 1 1 d . . . O31 O 0.1537(4) 0.3640(3) 0.1762(2) 0.0223(9) Uani 1 1 d . . . O44 O 0.2468(8) -0.0046(5) 0.6921(4) 0.123(3) Uani 1 1 d . . . O41 O 0.2822(6) 0.0598(4) 0.5512(3) 0.0677(16) Uani 1 1 d . . . O42 O 0.1416(5) 0.1674(4) 0.6566(3) 0.0517(13) Uani 1 1 d . . . O43 O 0.3848(6) 0.1306(7) 0.6631(5) 0.132(3) Uani 1 1 d . . . Ni2 Ni 0.19333(7) 0.28573(6) 0.05705(5) 0.0201(2) Uani 1 1 d . . . Ni1 Ni 0.33549(7) 0.42655(6) 0.16643(5) 0.0206(2) Uani 1 1 d . . . Cl4 Cl 0.26237(18) 0.08617(17) 0.64109(11) 0.0479(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 O1 0.019(2) 0.032(3) 0.029(2) -0.002(2) -0.0067(18) -0.006(2) O3 0.034(2) 0.034(3) 0.035(3) 0.002(2) -0.007(2) -0.008(2) N2 0.017(3) 0.026(3) 0.021(3) -0.001(2) -0.004(2) -0.002(2) C12 0.016(3) 0.020(4) 0.032(4) 0.004(3) -0.002(3) -0.009(3) C13 0.022(3) 0.027(4) 0.037(4) 0.002(3) -0.004(3) -0.011(3) C14 0.023(4) 0.029(4) 0.040(4) 0.009(3) -0.007(3) -0.009(3) C15 0.018(3) 0.021(4) 0.054(5) 0.003(3) -0.003(3) 0.001(3) C16 0.026(4) 0.020(4) 0.043(4) -0.004(3) 0.010(3) -0.012(3) C17 0.016(3) 0.016(3) 0.031(4) 0.001(3) -0.002(3) -0.005(3) C18 0.032(4) 0.016(4) 0.034(4) -0.002(3) 0.003(3) -0.013(3) C20 0.035(4) 0.035(4) 0.028(4) -0.001(3) -0.011(3) -0.012(3) C21 0.031(4) 0.026(4) 0.034(4) 0.001(3) -0.017(3) -0.014(3) C22 0.026(3) 0.028(4) 0.035(4) 0.003(3) -0.015(3) -0.003(3) C32 0.020(3) 0.027(4) 0.018(3) -0.001(3) -0.005(3) -0.005(3) C33 0.025(4) 0.035(4) 0.026(4) -0.001(3) -0.009(3) -0.009(3) C34 0.020(3) 0.057(5) 0.023(4) 0.001(3) 0.000(3) -0.014(3) C35 0.021(4) 0.063(5) 0.029(4) -0.013(4) 0.001(3) -0.001(4) C36 0.020(3) 0.039(4) 0.037(4) -0.012(3) -0.005(3) 0.006(3) C37 0.013(3) 0.032(4) 0.024(3) 0.002(3) -0.003(3) -0.005(3) C38 0.030(4) 0.024(4) 0.024(4) 0.001(3) -0.009(3) 0.003(3) C40 0.038(4) 0.018(4) 0.037(4) -0.001(3) -0.005(3) -0.013(3) C41 0.036(4) 0.023(4) 0.041(4) -0.004(3) -0.012(3) -0.018(3) C42 0.029(4) 0.031(4) 0.048(4) -0.012(3) 0.004(3) -0.020(3) C82 0.021(3) 0.027(4) 0.036(4) -0.003(3) -0.003(3) -0.003(3) N83 0.033(3) 0.033(3) 0.030(3) -0.005(3) -0.006(3) 0.001(3) C84 0.087(6) 0.060(5) 0.030(4) -0.016(4) -0.001(4) 0.014(5) C85 0.038(4) 0.034(4) 0.044(4) 0.004(3) -0.010(3) -0.002(3) C92 0.024(3) 0.020(4) 0.034(4) 0.000(3) -0.003(3) -0.008(3) N93 0.032(3) 0.026(3) 0.032(3) 0.009(3) -0.014(2) -0.012(3) C94 0.068(5) 0.044(5) 0.077(6) 0.021(4) -0.035(4) -0.038(4) C95 0.077(6) 0.067(6) 0.058(5) 0.024(4) -0.037(5) -0.042(5) O71 0.116(6) 0.097(6) 0.058(4) -0.012(4) -0.019(4) 0.058(5) C72 0.190(16) 0.232(18) 0.096(11) -0.069(11) -0.106(11) 0.150(15) N73 0.041(4) 0.084(6) 0.038(4) 0.004(4) -0.010(3) 0.021(4) C74 0.085(7) 0.093(8) 0.171(12) 0.062(8) -0.077(7) -0.039(6) C75 0.079(7) 0.173(12) 0.107(9) 0.084(8) -0.033(7) -0.034(8) N19 0.019(3) 0.019(3) 0.032(3) 0.003(2) -0.002(2) -0.007(2) N23 0.026(3) 0.022(3) 0.032(3) -0.001(2) -0.009(2) -0.006(2) N39 0.020(3) 0.024(3) 0.026(3) -0.004(2) -0.007(2) -0.003(2) N43 0.021(3) 0.028(3) 0.032(3) -0.001(2) -0.001(2) -0.009(2) O81 0.028(2) 0.028(3) 0.019(2) -0.001(2) -0.0035(19) -0.0018(19) O91 0.025(2) 0.022(2) 0.030(3) -0.0034(19) -0.007(2) -0.0060(19) O11 0.016(2) 0.020(2) 0.030(2) -0.0044(19) -0.0036(18) -0.0031(19) O31 0.014(2) 0.027(2) 0.027(2) -0.0043(19) 0.0002(18) -0.0055(18) O44 0.162(7) 0.080(5) 0.088(5) 0.049(4) 0.053(5) 0.054(5) O41 0.086(4) 0.081(4) 0.033(3) -0.013(3) -0.001(3) -0.003(3) O42 0.045(3) 0.060(3) 0.047(3) -0.010(3) -0.011(2) 0.008(3) O43 0.041(4) 0.219(9) 0.148(7) -0.092(6) -0.013(4) -0.028(5) Ni2 0.0165(4) 0.0203(5) 0.0247(5) -0.0017(3) -0.0044(3) -0.0048(3) Ni1 0.0163(4) 0.0215(5) 0.0255(5) -0.0025(4) -0.0027(3) -0.0063(3) Cl4 0.0387(11) 0.0697(14) 0.0331(11) -0.0017(10) -0.0043(8) 0.0001(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 O1 N2 1.285(6) . ? O1 Ni1 2.119(4) . ? O3 N2 1.238(6) . ? N2 Ni2 2.095(5) . ? C12 O11 1.328(6) . ? C12 C13 1.403(8) . ? C12 C17 1.414(8) . ? C13 C14 1.387(8) . ? C14 C15 1.370(8) . ? C15 C16 1.368(8) . ? C16 C17 1.395(8) . ? C17 C18 1.454(8) . ? C18 N19 1.287(7) . ? C20 N19 1.470(7) . ? C20 C21 1.530(7) . ? C21 C22 1.500(8) . ? C22 N23 1.487(7) . ? C32 O31 1.313(6) . ? C32 C33 1.406(7) . ? C32 C37 1.422(8) . ? C33 C34 1.384(8) . ? C34 C35 1.371(9) . ? C35 C36 1.385(8) . ? C36 C37 1.405(8) . ? C37 C38 1.448(8) . ? C38 N39 1.293(7) . ? C40 N39 1.480(7) . ? C40 C41 1.511(8) . ? C41 C42 1.515(8) . ? C42 N43 1.473(7) . ? C82 O81 1.244(7) . ? C82 N83 1.315(7) . ? N83 C85 1.443(7) . ? N83 C84 1.458(8) . ? C92 O91 1.242(7) . ? C92 N93 1.322(7) . ? N93 C94 1.442(7) . ? N93 C95 1.452(8) . ? O71 C72 1.020(14) . ? C72 N73 1.301(14) . ? N73 C74 1.393(10) . ? N73 C75 1.434(10) . ? N19 Ni2 2.027(5) . ? N23 Ni2 2.055(4) . ? N39 Ni1 2.038(5) . ? N43 Ni1 2.056(4) . ? O81 Ni1 2.112(4) . ? O91 Ni2 2.119(4) . ? O11 Ni2 2.014(4) . ? O11 Ni1 2.079(4) . ? O31 Ni1 2.011(3) . ? O31 Ni2 2.092(4) . ? O44 Cl4 1.364(6) . ? O41 Cl4 1.424(5) . ? O42 Cl4 1.433(5) . ? O43 Cl4 1.446(6) . ? 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 N2 O1 Ni1 110.8(3) . . ? O3 N2 O1 117.4(4) . . ? O3 N2 Ni2 125.3(4) . . ? O1 N2 Ni2 117.2(4) . . ? O11 C12 C13 120.1(5) . . ? O11 C12 C17 121.6(5) . . ? C13 C12 C17 118.3(5) . . ? C14 C13 C12 120.8(6) . . ? C15 C14 C13 120.8(6) . . ? C16 C15 C14 118.8(6) . . ? C15 C16 C17 122.8(6) . . ? C16 C17 C12 118.3(5) . . ? C16 C17 C18 117.6(5) . . ? C12 C17 C18 124.1(5) . . ? N19 C18 C17 128.6(6) . . ? N19 C20 C21 114.3(5) . . ? C22 C21 C20 114.6(5) . . ? N23 C22 C21 112.3(5) . . ? O31 C32 C33 120.5(5) . . ? O31 C32 C37 121.7(5) . . ? C33 C32 C37 117.8(5) . . ? C34 C33 C32 120.8(6) . . ? C35 C34 C33 121.7(6) . . ? C34 C35 C36 118.8(6) . . ? C35 C36 C37 121.5(6) . . ? C36 C37 C32 119.3(5) . . ? C36 C37 C38 116.5(6) . . ? C32 C37 C38 124.2(5) . . ? N39 C38 C37 127.9(6) . . ? N39 C40 C41 113.9(5) . . ? C40 C41 C42 114.2(5) . . ? N43 C42 C41 112.8(5) . . ? O81 C82 N83 125.2(6) . . ? C82 N83 C85 122.7(5) . . ? C82 N83 C84 120.8(6) . . ? C85 N83 C84 116.6(5) . . ? O91 C92 N93 124.8(5) . . ? C92 N93 C94 120.5(5) . . ? C92 N93 C95 121.8(5) . . ? C94 N93 C95 117.7(5) . . ? O71 C72 N73 150(2) . . ? C72 N73 C74 123.3(12) . . ? C72 N73 C75 118.0(12) . . ? C74 N73 C75 118.7(8) . . ? C18 N19 C20 115.7(5) . . ? C18 N19 Ni2 122.4(4) . . ? C20 N19 Ni2 121.9(4) . . ? C22 N23 Ni2 118.7(3) . . ? C38 N39 C40 114.9(5) . . ? C38 N39 Ni1 124.6(4) . . ? C40 N39 Ni1 120.4(4) . . ? C42 N43 Ni1 118.8(4) . . ? C82 O81 Ni1 127.9(4) . . ? C92 O91 Ni2 117.7(4) . . ? C12 O11 Ni2 125.8(3) . . ? C12 O11 Ni1 138.8(3) . . ? Ni2 O11 Ni1 95.34(15) . . ? C32 O31 Ni1 129.6(3) . . ? C32 O31 Ni2 132.1(3) . . ? Ni1 O31 Ni2 95.04(14) . . ? O11 Ni2 N19 90.54(17) . . ? O11 Ni2 N23 173.64(17) . . ? N19 Ni2 N23 95.69(19) . . ? O11 Ni2 O31 77.31(14) . . ? N19 Ni2 O31 167.59(15) . . ? N23 Ni2 O31 96.51(16) . . ? O11 Ni2 N2 85.70(16) . . ? N19 Ni2 N2 92.98(18) . . ? N23 Ni2 N2 95.22(18) . . ? O31 Ni2 N2 83.65(17) . . ? O11 Ni2 O91 91.00(15) . . ? N19 Ni2 O91 95.01(17) . . ? N23 Ni2 O91 87.20(17) . . ? O31 Ni2 O91 87.86(15) . . ? N2 Ni2 O91 171.38(17) . . ? O31 Ni1 N39 89.87(16) . . ? O31 Ni1 N43 172.29(17) . . ? N39 Ni1 N43 97.83(18) . . ? O31 Ni1 O11 77.65(14) . . ? N39 Ni1 O11 165.77(16) . . ? N43 Ni1 O11 94.66(16) . . ? O31 Ni1 O81 91.37(15) . . ? N39 Ni1 O81 96.61(17) . . ? N43 Ni1 O81 88.12(17) . . ? O11 Ni1 O81 90.57(15) . . ? O31 Ni1 O1 89.21(14) . . ? N39 Ni1 O1 89.73(17) . . ? N43 Ni1 O1 90.45(17) . . ? O11 Ni1 O1 83.36(15) . . ? O81 Ni1 O1 173.63(15) . . ? O44 Cl4 O41 110.3(4) . . ? O44 Cl4 O42 109.9(3) . . ? O41 Cl4 O42 110.7(3) . . ? O44 Cl4 O43 109.8(5) . . ? O41 Cl4 O43 108.1(4) . . ? O42 Cl4 O43 107.9(4) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 22.53 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.653 _refine_diff_density_min -0.721 _refine_diff_density_rms 0.086 _publ_section_references ; Sheldrick, G.M. (1997) SHELXL program for crystallography refinement. University of Gottingen, Germany. Spek, A.L., (2004) PLATON program, Utrecht University, The Netherlands ; #===END data_3 _database_code_depnum_ccdc_archive 'CCDC 786104' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H40 Cl N7 Ni2 O10' _chemical_formula_weight 763.52 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' 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.6826(17) _cell_length_b 33.861(10) _cell_length_c 10.8615(8) _cell_angle_alpha 90.00 _cell_angle_beta 110.332(13) _cell_angle_gamma 90.00 _cell_volume 3339.2(11) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 20176 _cell_measurement_theta_min 2.51 _cell_measurement_theta_max 30.00 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.519 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1592 _exptl_absorpt_coefficient_mu 1.270 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'ABSPACK, Oxford Diffraction Ltd' _exptl_absorpt_correction_T_min 0.824 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_standards_number n/a _diffrn_measurement_device 'Oxford Diffaction X-Calibur System' _diffrn_measurement_method '321 frames, counting time 10 s.' _diffrn_standards_interval_count n/a _diffrn_standards_interval_time n/a _diffrn_standards_decay_% n/a _diffrn_reflns_number 20176 _diffrn_reflns_av_R_equivalents 0.0508 _diffrn_reflns_av_sigmaI/netI 0.0780 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -46 _diffrn_reflns_limit_k_max 47 _diffrn_reflns_limit_l_min -6 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.51 _diffrn_reflns_theta_max 30.00 _reflns_number_total 9335 _reflns_number_gt 6740 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Crysalis, Oxford Diffraction' _computing_cell_refinement 'Crysalis, Oxford Diffraction' _computing_data_reduction 'Crysalis, Oxford Diffraction' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics PLATON(Spek,2004) _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 _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.0358P)^2^+12.6684P] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9335 _refine_ls_number_parameters 419 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1118 _refine_ls_R_factor_gt 0.0778 _refine_ls_wR_factor_ref 0.1491 _refine_ls_wR_factor_gt 0.1400 _refine_ls_goodness_of_fit_ref 1.101 _refine_ls_restrained_S_all 1.101 _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 C12 C 0.6717(4) 0.59518(12) 0.3112(4) 0.0147(8) Uani 1 1 d . . . C13 C 0.7284(5) 0.57148(13) 0.4243(4) 0.0199(9) Uani 1 1 d . . . H13 H 0.7058 0.5776 0.4987 0.024 Uiso 1 1 calc R . . C14 C 0.8169(5) 0.53944(15) 0.4263(5) 0.0264(10) Uani 1 1 d . . . H14 H 0.8536 0.5244 0.5024 0.032 Uiso 1 1 calc R . . C15 C 0.8526(5) 0.52912(14) 0.3169(5) 0.0290(10) Uani 1 1 d . . . H15 H 0.9112 0.5072 0.3187 0.035 Uiso 1 1 calc R . . C16 C 0.7993(5) 0.55199(14) 0.2068(4) 0.0257(10) Uani 1 1 d . . . H16 H 0.8252 0.5457 0.1344 0.031 Uiso 1 1 calc R . . C21 C 0.3853(6) 0.66179(17) -0.1651(4) 0.0334(12) Uani 1 1 d . . . H21A H 0.3341 0.6367 -0.1753 0.040 Uiso 1 1 calc R . . H21B H 0.3811 0.6703 -0.2517 0.040 Uiso 1 1 calc R . . C17 C 0.7075(4) 0.58445(13) 0.1988(4) 0.0185(8) Uani 1 1 d . . . C18 C 0.6600(5) 0.60677(13) 0.0772(4) 0.0198(9) Uani 1 1 d . . . H18 H 0.7030 0.5999 0.0159 0.024 Uiso 1 1 calc R . . C20 C 0.5455(5) 0.65538(15) -0.0806(4) 0.0285(11) Uani 1 1 d . . . H20A H 0.5930 0.6401 -0.1301 0.034 Uiso 1 1 calc R . . H20B H 0.5943 0.6808 -0.0614 0.034 Uiso 1 1 calc R . . C22 C 0.3040(6) 0.69193(15) -0.1116(4) 0.0308(11) Uani 1 1 d . . . H22A H 0.3641 0.7154 -0.0839 0.037 Uiso 1 1 calc R . . H22B H 0.2129 0.6994 -0.1802 0.037 Uiso 1 1 calc R . . C32 C 0.2278(4) 0.67402(13) 0.3123(4) 0.0174(8) Uani 1 1 d . . . C33 C 0.0938(5) 0.66109(14) 0.2193(5) 0.0253(9) Uani 1 1 d . . . H33 H 0.0949 0.6452 0.1497 0.030 Uiso 1 1 calc R . . C34 C -0.0387(5) 0.67160(16) 0.2301(5) 0.0324(12) Uani 1 1 d . . . H34 H -0.1258 0.6629 0.1672 0.039 Uiso 1 1 calc R . . C35 C -0.0451(5) 0.69499(17) 0.3329(5) 0.0362(12) Uani 1 1 d . . . H35 H -0.1353 0.7015 0.3401 0.043 Uiso 1 1 calc R . . C36 C 0.0844(5) 0.70842(15) 0.4239(5) 0.0294(11) Uani 1 1 d . . . H36 H 0.0805 0.7247 0.4916 0.035 Uiso 1 1 calc R . . C37 C 0.2221(4) 0.69820(13) 0.4172(4) 0.0197(9) Uani 1 1 d . . . C38 C 0.3493(5) 0.71518(13) 0.5170(4) 0.0206(9) Uani 1 1 d . . . H38 H 0.3302 0.7346 0.5693 0.025 Uiso 1 1 calc R . . C40 C 0.5943(6) 0.73189(16) 0.6370(5) 0.0336(12) Uani 1 1 d . . . H40A H 0.5489 0.7433 0.6955 0.040 Uiso 1 1 calc R . . H40B H 0.6191 0.7534 0.5896 0.040 Uiso 1 1 calc R . . C41 C 0.7356(6) 0.71165(17) 0.7195(5) 0.0347(12) Uani 1 1 d . . . H41A H 0.7930 0.7301 0.7859 0.042 Uiso 1 1 calc R . . H41B H 0.7105 0.6896 0.7648 0.042 Uiso 1 1 calc R . . C42 C 0.8311(5) 0.69648(15) 0.6458(5) 0.0277(10) Uani 1 1 d . . . H42A H 0.8402 0.7166 0.5857 0.033 Uiso 1 1 calc R . . H42B H 0.9288 0.6907 0.7074 0.033 Uiso 1 1 calc R . . C82 C 0.3747(6) 0.60966(16) 0.5469(5) 0.0357(12) Uani 1 1 d . . . H82 H 0.2985 0.6236 0.4861 0.043 Uiso 1 1 calc R . . N83 N 0.3344(4) 0.58252(12) 0.6181(4) 0.0287(9) Uani 1 1 d . . . C84 C 0.1769(6) 0.5781(2) 0.5902(7) 0.0537(17) Uani 1 1 d . . . H84A H 0.1248 0.5983 0.5296 0.080 Uiso 1 1 calc R . . H84B H 0.1565 0.5806 0.6702 0.080 Uiso 1 1 calc R . . H84C H 0.1456 0.5526 0.5523 0.080 Uiso 1 1 calc R . . C85 C 0.4339(8) 0.5583(2) 0.7128(8) 0.071(2) Uani 1 1 d . . . H85A H 0.4307 0.5321 0.6783 0.107 Uiso 1 1 calc R . . H85B H 0.4074 0.5575 0.7901 0.107 Uiso 1 1 calc R . . H85C H 0.5317 0.5688 0.7347 0.107 Uiso 1 1 calc R . . C92 C 0.3172(5) 0.57567(15) 0.1956(5) 0.0279(10) Uani 1 1 d . . . H92 H 0.3264 0.5889 0.2731 0.033 Uiso 1 1 calc R . . N93 N 0.2855(5) 0.53805(13) 0.1908(4) 0.0311(9) Uani 1 1 d . . . C94 C 0.2669(8) 0.51548(18) 0.0736(6) 0.0569(19) Uani 1 1 d . . . H94A H 0.2628 0.5331 0.0031 0.085 Uiso 1 1 calc R . . H94B H 0.1770 0.5006 0.0504 0.085 Uiso 1 1 calc R . . H94C H 0.3485 0.4977 0.0892 0.085 Uiso 1 1 calc R . . C95 C 0.2594(10) 0.51820(19) 0.2995(7) 0.066(2) Uani 1 1 d . . . H95A H 0.2764 0.5363 0.3712 0.099 Uiso 1 1 calc R . . H95B H 0.3252 0.4961 0.3274 0.099 Uiso 1 1 calc R . . H95C H 0.1594 0.5090 0.2715 0.099 Uiso 1 1 calc R . . O1 O 0.6115(3) 0.70943(10) 0.3408(3) 0.0243(7) Uani 1 1 d . . . O3 O 0.5857(4) 0.72897(11) 0.1497(3) 0.0417(10) Uani 1 1 d . . . O11 O 0.5900(3) 0.62631(9) 0.3120(3) 0.0179(6) Uani 1 1 d . . . O31 O 0.3541(3) 0.66310(9) 0.3022(3) 0.0202(6) Uani 1 1 d . . . O71 O 0.0011(5) 0.55380(13) 0.8023(4) 0.0535(12) Uani 1 1 d . . . O72 O 0.0239(5) 0.62191(13) 0.8338(4) 0.0551(12) Uani 1 1 d . . . O73 O -0.0282(4) 0.58136(14) 0.9881(3) 0.0480(11) Uani 1 1 d . . . O74 O -0.2070(4) 0.59167(14) 0.7804(4) 0.0490(11) Uani 1 1 d . . . O91 O 0.3363(3) 0.59546(9) 0.1068(3) 0.0231(7) Uani 1 1 d . . . O81 O 0.4950(4) 0.61798(11) 0.5519(3) 0.0352(8) Uani 1 1 d . . . N2 N 0.5547(4) 0.70365(11) 0.2162(3) 0.0218(8) Uani 1 1 d . . . N19 N 0.5658(4) 0.63485(11) 0.0445(3) 0.0212(8) Uani 1 1 d . . . N23 N 0.2710(4) 0.67528(12) 0.0010(3) 0.0261(8) Uani 1 1 d . . . H23A H 0.2008 0.6568 -0.0304 0.031 Uiso 1 1 calc R . . H23B H 0.2318 0.6947 0.0350 0.031 Uiso 1 1 calc R . . N39 N 0.4854(4) 0.70656(11) 0.5419(3) 0.0199(7) Uani 1 1 d . . . N43 N 0.7676(4) 0.66053(12) 0.5718(3) 0.0219(8) Uani 1 1 d . . . H43A H 0.7733 0.6411 0.6299 0.026 Uiso 1 1 calc R . . H43B H 0.8243 0.6534 0.5252 0.026 Uiso 1 1 calc R . . Ni1 Ni 0.55311(6) 0.663750(16) 0.44516(5) 0.01486(12) Uani 1 1 d . . . Ni2 Ni 0.44026(6) 0.650293(16) 0.15272(5) 0.01630(12) Uani 1 1 d . . . Cl7 Cl -0.05213(12) 0.58744(4) 0.85263(10) 0.0248(2) 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 C12 0.0180(18) 0.0064(19) 0.0194(18) -0.0024(14) 0.0060(15) -0.0033(14) C13 0.021(2) 0.018(2) 0.0216(19) 0.0016(16) 0.0091(17) 0.0011(16) C14 0.026(2) 0.025(3) 0.027(2) 0.0042(19) 0.0086(19) 0.0059(19) C15 0.029(2) 0.018(3) 0.041(3) 0.004(2) 0.013(2) 0.0101(19) C16 0.028(2) 0.026(3) 0.027(2) -0.0059(19) 0.0149(19) 0.0031(19) C21 0.041(3) 0.045(3) 0.0123(18) 0.002(2) 0.0077(19) -0.001(2) C17 0.0194(19) 0.019(2) 0.0209(19) -0.0008(16) 0.0113(16) -0.0014(16) C18 0.025(2) 0.021(2) 0.0166(18) -0.0037(16) 0.0120(17) -0.0014(17) C20 0.042(3) 0.029(3) 0.019(2) 0.0056(18) 0.016(2) 0.002(2) C22 0.036(3) 0.025(3) 0.025(2) 0.0081(19) 0.002(2) 0.003(2) C32 0.0173(19) 0.015(2) 0.0224(19) 0.0025(16) 0.0100(16) 0.0002(15) C33 0.020(2) 0.024(3) 0.029(2) -0.0014(19) 0.0061(18) -0.0013(18) C34 0.017(2) 0.039(3) 0.040(3) 0.000(2) 0.009(2) -0.006(2) C35 0.019(2) 0.048(4) 0.049(3) 0.007(3) 0.021(2) 0.005(2) C36 0.029(2) 0.033(3) 0.032(2) 0.001(2) 0.019(2) 0.008(2) C37 0.020(2) 0.022(2) 0.0217(19) 0.0026(17) 0.0124(17) 0.0038(17) C38 0.030(2) 0.018(2) 0.0187(19) -0.0006(16) 0.0145(18) 0.0059(18) C40 0.039(3) 0.025(3) 0.035(3) -0.012(2) 0.011(2) -0.008(2) C41 0.035(3) 0.043(3) 0.025(2) -0.014(2) 0.010(2) -0.012(2) C42 0.024(2) 0.030(3) 0.028(2) -0.007(2) 0.0063(19) -0.0101(19) C82 0.042(3) 0.029(3) 0.039(3) -0.006(2) 0.018(2) -0.006(2) N83 0.032(2) 0.019(2) 0.042(2) 0.0034(18) 0.0209(19) -0.0053(16) C84 0.036(3) 0.062(5) 0.065(4) -0.006(3) 0.021(3) 0.001(3) C85 0.061(5) 0.055(5) 0.079(5) 0.028(4) 0.000(4) -0.004(4) C92 0.033(2) 0.022(3) 0.035(2) -0.009(2) 0.020(2) -0.0057(19) N93 0.036(2) 0.024(2) 0.035(2) -0.0066(18) 0.0151(19) -0.0042(18) C94 0.097(5) 0.024(3) 0.035(3) -0.006(2) 0.005(3) 0.005(3) C95 0.119(7) 0.030(4) 0.075(5) -0.008(3) 0.065(5) -0.021(4) O1 0.0259(16) 0.0291(19) 0.0201(14) -0.0020(13) 0.0110(13) -0.0036(14) O3 0.059(3) 0.036(2) 0.0282(18) 0.0080(16) 0.0121(18) -0.0126(19) O11 0.0211(14) 0.0202(17) 0.0126(12) -0.0004(11) 0.0062(11) 0.0056(12) O31 0.0157(13) 0.0269(18) 0.0200(14) -0.0074(13) 0.0086(11) -0.0007(12) O71 0.072(3) 0.044(3) 0.051(2) -0.014(2) 0.030(2) 0.007(2) O72 0.048(3) 0.044(3) 0.057(3) 0.015(2) -0.002(2) -0.019(2) O73 0.043(2) 0.083(3) 0.0200(16) 0.0048(19) 0.0131(16) 0.004(2) O74 0.0204(17) 0.072(3) 0.045(2) 0.012(2) -0.0013(16) -0.0013(18) O91 0.0289(16) 0.0171(17) 0.0218(14) -0.0048(12) 0.0070(13) -0.0030(13) O81 0.049(2) 0.027(2) 0.043(2) -0.0003(16) 0.0330(18) -0.0048(16) N2 0.0252(18) 0.021(2) 0.0236(18) 0.0036(15) 0.0135(16) 0.0019(15) N19 0.0278(19) 0.021(2) 0.0176(16) -0.0012(14) 0.0110(15) -0.0027(15) N23 0.0250(19) 0.030(2) 0.0208(18) -0.0007(16) 0.0050(16) 0.0040(16) N39 0.0289(19) 0.016(2) 0.0171(16) -0.0036(14) 0.0108(15) -0.0028(15) N43 0.0180(17) 0.028(2) 0.0185(16) -0.0038(15) 0.0047(14) -0.0032(15) Ni1 0.0154(2) 0.0165(3) 0.0142(2) -0.0032(2) 0.00708(19) -0.0022(2) Ni2 0.0185(2) 0.0172(3) 0.0132(2) -0.0012(2) 0.00556(19) 0.0010(2) Cl7 0.0218(5) 0.0296(6) 0.0213(5) 0.0006(4) 0.0055(4) -0.0023(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C12 O11 1.320(5) . ? C12 C13 1.409(6) . ? C12 C17 1.427(5) . ? C13 C14 1.378(6) . ? C14 C15 1.393(6) . ? C15 C16 1.366(7) . ? C16 C17 1.397(6) . ? C21 C20 1.519(7) . ? C21 C22 1.522(7) . ? C17 C18 1.451(6) . ? C18 N19 1.279(6) . ? C20 N19 1.477(5) . ? C22 N23 1.479(6) . ? C32 O31 1.319(5) . ? C32 C33 1.409(6) . ? C32 C37 1.419(6) . ? C33 C34 1.374(6) . ? C34 C35 1.388(7) . ? C35 C36 1.376(7) . ? C36 C37 1.404(6) . ? C37 C38 1.448(6) . ? C38 N39 1.283(5) . ? C40 N39 1.469(6) . ? C40 C41 1.514(7) . ? C41 C42 1.508(7) . ? C42 N43 1.471(6) . ? C82 O81 1.181(6) . ? C82 N83 1.343(6) . ? N83 C85 1.403(7) . ? N83 C84 1.456(7) . ? C92 O91 1.240(5) . ? C92 N93 1.307(6) . ? N93 C94 1.441(7) . ? N93 C95 1.455(7) . ? O1 N2 1.287(4) . ? O1 Ni1 2.108(3) . ? O3 N2 1.223(5) . ? O11 Ni2 2.003(3) . ? O11 Ni1 2.046(3) . ? O31 Ni1 2.011(3) . ? O31 Ni2 2.112(3) . ? O71 Cl7 1.435(4) . ? O72 Cl7 1.432(4) . ? O73 Cl7 1.423(3) . ? O74 Cl7 1.438(4) . ? O91 Ni2 2.088(3) . ? O81 Ni1 2.125(3) . ? N2 Ni2 2.106(4) . ? N19 Ni2 2.031(3) . ? N23 Ni2 2.059(4) . ? N39 Ni1 2.028(4) . ? N43 Ni1 2.057(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O11 C12 C13 120.2(3) . . ? O11 C12 C17 122.2(4) . . ? C13 C12 C17 117.6(4) . . ? C14 C13 C12 120.9(4) . . ? C13 C14 C15 121.4(4) . . ? C16 C15 C14 118.3(4) . . ? C15 C16 C17 122.6(4) . . ? C20 C21 C22 114.8(4) . . ? C16 C17 C12 119.1(4) . . ? C16 C17 C18 117.4(4) . . ? C12 C17 C18 123.5(4) . . ? N19 C18 C17 127.6(4) . . ? N19 C20 C21 113.9(4) . . ? N23 C22 C21 110.5(4) . . ? O31 C32 C33 120.2(4) . . ? O31 C32 C37 121.6(4) . . ? C33 C32 C37 118.2(4) . . ? C34 C33 C32 120.8(4) . . ? C33 C34 C35 121.3(5) . . ? C36 C35 C34 118.8(4) . . ? C35 C36 C37 121.7(4) . . ? C36 C37 C32 119.1(4) . . ? C36 C37 C38 116.1(4) . . ? C32 C37 C38 124.8(4) . . ? N39 C38 C37 127.7(4) . . ? N39 C40 C41 115.6(4) . . ? C42 C41 C40 115.7(4) . . ? N43 C42 C41 110.8(4) . . ? O81 C82 N83 128.0(6) . . ? C82 N83 C85 124.0(5) . . ? C82 N83 C84 116.3(5) . . ? C85 N83 C84 119.7(5) . . ? O91 C92 N93 126.3(4) . . ? C92 N93 C94 120.5(5) . . ? C92 N93 C95 121.5(4) . . ? C94 N93 C95 117.9(5) . . ? N2 O1 Ni1 111.0(3) . . ? C12 O11 Ni2 125.1(2) . . ? C12 O11 Ni1 138.7(2) . . ? Ni2 O11 Ni1 96.17(12) . . ? C32 O31 Ni1 126.9(3) . . ? C32 O31 Ni2 138.3(3) . . ? Ni1 O31 Ni2 93.88(11) . . ? C92 O91 Ni2 119.0(3) . . ? C82 O81 Ni1 126.4(4) . . ? O3 N2 O1 114.3(4) . . ? O3 N2 Ni2 128.1(3) . . ? O1 N2 Ni2 117.3(3) . . ? C18 N19 C20 117.4(4) . . ? C18 N19 Ni2 122.9(3) . . ? C20 N19 Ni2 119.7(3) . . ? C22 N23 Ni2 118.5(3) . . ? C38 N39 C40 116.7(4) . . ? C38 N39 Ni1 123.1(3) . . ? C40 N39 Ni1 120.0(3) . . ? C42 N43 Ni1 117.1(3) . . ? O31 Ni1 N39 90.72(13) . . ? O31 Ni1 O11 78.64(11) . . ? N39 Ni1 O11 167.51(13) . . ? O31 Ni1 N43 171.66(13) . . ? N39 Ni1 N43 97.14(15) . . ? O11 Ni1 N43 93.23(13) . . ? O31 Ni1 O1 87.52(12) . . ? N39 Ni1 O1 87.11(13) . . ? O11 Ni1 O1 85.92(12) . . ? N43 Ni1 O1 90.08(14) . . ? O31 Ni1 O81 92.81(14) . . ? N39 Ni1 O81 92.52(14) . . ? O11 Ni1 O81 94.50(13) . . ? N43 Ni1 O81 89.64(15) . . ? O1 Ni1 O81 179.51(14) . . ? O11 Ni2 N19 89.77(13) . . ? O11 Ni2 N23 173.62(13) . . ? N19 Ni2 N23 96.48(15) . . ? O11 Ni2 O91 89.44(12) . . ? N19 Ni2 O91 88.20(14) . . ? N23 Ni2 O91 89.45(15) . . ? O11 Ni2 N2 85.67(13) . . ? N19 Ni2 N2 93.29(14) . . ? N23 Ni2 N2 95.24(16) . . ? O91 Ni2 N2 174.88(13) . . ? O11 Ni2 O31 77.30(11) . . ? N19 Ni2 O31 166.72(13) . . ? N23 Ni2 O31 96.53(13) . . ? O91 Ni2 O31 94.59(12) . . ? N2 Ni2 O31 82.87(13) . . ? O73 Cl7 O72 111.0(3) . . ? O73 Cl7 O71 109.2(3) . . ? O72 Cl7 O71 108.8(3) . . ? O73 Cl7 O74 110.0(2) . . ? O72 Cl7 O74 109.4(3) . . ? O71 Cl7 O74 108.4(3) . . ? _diffrn_measured_fraction_theta_max 0.957 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.957 _refine_diff_density_max 1.482 _refine_diff_density_min -1.663 _refine_diff_density_rms 0.114 _publ_section_references ; Oxford Diffraction Ltd, Crysalis Program (2005) Oxford Diffraction Ltd, Abspack Program (2005) Sheldrick, G.M. (1997) SHELXL program for crystallography refinement. University of Gottingen, Germany. Spek, A.L., (2004) PLATON program, Utrecht University, The Netherlands ; #===END data_4 _database_code_depnum_ccdc_archive 'CCDC 786105' #TrackingRef '- (1-4) revised.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H37 Cl2 N6 Ni3 O9.50' _chemical_formula_weight 940.74 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pnnm loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y+1/2, -z+1/2' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, y, -z' '-x-1/2, y-1/2, z-1/2' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 16.004(3) _cell_length_b 15.268(3) _cell_length_c 15.745(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3847.4(13) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 29489 _cell_measurement_theta_min 1.81 _cell_measurement_theta_max 22.97 _exptl_crystal_description needle _exptl_crystal_colour black _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.619 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1920 _exptl_absorpt_coefficient_mu 1.655 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details SADABS _exptl_absorpt_correction_T_min 0.827 _exptl_absorpt_correction_T_max 0.987 _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_standards_number n/a _diffrn_measurement_device ? _diffrn_measurement_method ? _diffrn_standards_interval_count n/a _diffrn_standards_interval_time n/a _diffrn_standards_decay_% n/a _diffrn_reflns_number 29489 _diffrn_reflns_av_R_equivalents 0.1105 _diffrn_reflns_av_sigmaI/netI 0.0491 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 22.97 _reflns_number_total 2792 _reflns_number_gt 2121 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics PLATON(Spek,2004) _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 _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.1099P)^2^+45.3665P] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2792 _refine_ls_number_parameters 265 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0975 _refine_ls_R_factor_gt 0.0721 _refine_ls_wR_factor_ref 0.2122 _refine_ls_wR_factor_gt 0.1995 _refine_ls_goodness_of_fit_ref 0.997 _refine_ls_restrained_S_all 0.997 _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 Ni1 Ni 0.5000 0.5000 0.5000 0.0234(6) Uani 1 4 d S . . Ni2 Ni 0.0000 0.5000 0.5000 0.0248(6) Uani 1 4 d S . . Ni3 Ni 0.16426(9) 0.58921(10) 0.5000 0.0232(4) Uani 1 2 d S . . Ni4 Ni 0.38160(10) 0.35121(10) 0.5000 0.0303(5) Uani 1 2 d S . . C12 C 0.4811(5) 0.3765(6) 0.6583(6) 0.036(2) Uani 1 1 d . . . C13 C 0.5528(5) 0.4052(7) 0.7001(7) 0.040(3) Uani 1 1 d . . . H13 H 0.5903 0.4419 0.6723 0.048 Uiso 1 1 calc R . . C14 C 0.5688(6) 0.3788(8) 0.7852(7) 0.051(3) Uani 1 1 d . . . H14 H 0.6160 0.3999 0.8130 0.061 Uiso 1 1 calc R . . C15 C 0.5169(7) 0.3238(9) 0.8262(8) 0.068(4) Uani 1 1 d . . . H15 H 0.5299 0.3039 0.8805 0.082 Uiso 1 1 calc R . . C16 C 0.4438(7) 0.2971(9) 0.7867(9) 0.073(4) Uani 1 1 d . . . H16 H 0.4064 0.2622 0.8166 0.088 Uiso 1 1 calc R . . C17 C 0.4247(6) 0.3210(8) 0.7034(8) 0.058(3) Uani 1 1 d . . . C18 C 0.3443(6) 0.2930(8) 0.6702(9) 0.060(4) Uani 1 1 d . . . H18 H 0.3094 0.2656 0.7092 0.072 Uiso 1 1 calc R . . C20 C 0.2275(6) 0.2734(7) 0.5798(8) 0.053(3) Uani 1 1 d . . . H20A H 0.1926 0.3252 0.5758 0.064 Uiso 1 1 calc R . . H20B H 0.2079 0.2391 0.6277 0.064 Uiso 1 1 calc R . . C21 C 0.2175(10) 0.2202(10) 0.5000 0.069(6) Uani 1 2 d S . . H21A H 0.1626 0.1934 0.5000 0.082 Uiso 1 2 calc SR . . H21B H 0.2587 0.1736 0.5000 0.082 Uiso 1 2 calc SR . . C32 C 0.1193(5) 0.4937(5) 0.6578(6) 0.029(2) Uani 1 1 d . . . C33 C 0.0793(5) 0.4222(6) 0.6989(7) 0.038(2) Uani 1 1 d . . . H33 H 0.0356 0.3942 0.6710 0.046 Uiso 1 1 calc R . . C34 C 0.1017(7) 0.3932(7) 0.7759(7) 0.051(3) Uani 1 1 d . . . H34 H 0.0755 0.3445 0.7994 0.062 Uiso 1 1 calc R . . C35 C 0.1648(7) 0.4367(8) 0.8211(8) 0.059(3) Uani 1 1 d . . . H35 H 0.1798 0.4185 0.8754 0.070 Uiso 1 1 calc R . . C36 C 0.2043(7) 0.5070(7) 0.7833(6) 0.046(3) Uani 1 1 d . . . H36 H 0.2467 0.5354 0.8129 0.055 Uiso 1 1 calc R . . C37 C 0.1831(5) 0.5371(6) 0.7028(6) 0.030(2) Uani 1 1 d . . . C38 C 0.2272(5) 0.6130(6) 0.6721(6) 0.026(2) Uani 1 1 d . . . H38 H 0.2607 0.6421 0.7114 0.031 Uiso 1 1 calc R . . C40 C 0.2774(8) 0.7227(8) 0.5823(7) 0.064(4) Uani 1 1 d . . . H40A H 0.2542 0.7702 0.6157 0.077 Uiso 1 1 calc R . . H40B H 0.3326 0.7105 0.6050 0.077 Uiso 1 1 calc R . . C41 C 0.2874(15) 0.7529(12) 0.5000 0.088(8) Uani 1 2 d S . . H41A H 0.3449 0.7729 0.5000 0.105 Uiso 1 2 calc SR . . H41B H 0.2542 0.8060 0.5000 0.105 Uiso 1 2 calc SR . . N19 N 0.3149(5) 0.3006(5) 0.5958(7) 0.046(2) Uani 1 1 d . . . N39 N 0.2256(4) 0.6452(4) 0.5967(5) 0.0294(18) Uani 1 1 d . . . N5 N 0.0617(7) 0.6737(6) 0.5000 0.034(3) Uani 1 2 d S . . N2 N 0.3247(6) 0.4680(6) 0.5000 0.025(2) Uani 1 2 d S . . O11 O 0.4649(3) 0.4016(4) 0.5800(4) 0.0343(16) Uani 1 1 d . . . O3 O 0.3717(5) 0.5365(5) 0.5000 0.0248(19) Uani 1 2 d S . . O31 O 0.0955(3) 0.5190(4) 0.5824(4) 0.0272(14) Uani 1 1 d . . . O4 O -0.0126(6) 0.6362(6) 0.5000 0.038(2) Uani 1 2 d S . . O6 O 0.0581(7) 0.7531(8) 0.5000 0.058(3) Uani 1 2 d S . . O1 O 0.2483(5) 0.4790(5) 0.5000 0.029(2) Uani 1 2 d S . . OW1 O 0.0000 0.0000 0.5000 0.104(7) Uiso 1 4 d S . . OW2 O -0.1588(9) 0.0111(10) 0.5000 0.093(4) Uiso 1 2 d S . . C81 C 0.4401(13) 0.1076(14) 0.4394(13) 0.046(5) Uiso 0.50 1 d P . . H81A H 0.3955 0.1223 0.4002 0.055 Uiso 0.50 1 calc PR . . H81B H 0.4791 0.0691 0.4106 0.055 Uiso 0.50 1 calc PR . . Cl82 Cl 0.4939(3) 0.2080(3) 0.4752(3) 0.0441(14) Uiso 0.50 1 d P . . Cl83 Cl 0.3984(4) 0.0547(4) 0.5310(3) 0.0562(16) Uiso 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0165(11) 0.0212(12) 0.0325(13) 0.000 0.000 -0.0036(9) Ni2 0.0159(11) 0.0216(12) 0.0368(14) 0.000 0.000 -0.0008(9) Ni3 0.0208(8) 0.0209(8) 0.0280(9) 0.000 0.000 -0.0034(7) Ni4 0.0170(8) 0.0186(8) 0.0551(12) 0.000 0.000 -0.0032(7) C12 0.019(5) 0.044(6) 0.045(6) 0.020(5) 0.008(4) 0.005(4) C13 0.021(5) 0.053(6) 0.047(6) 0.013(5) 0.000(5) 0.008(4) C14 0.026(5) 0.071(8) 0.057(8) 0.017(6) 0.000(5) 0.008(5) C15 0.043(7) 0.103(10) 0.059(8) 0.046(8) 0.004(6) 0.015(7) C16 0.042(7) 0.099(11) 0.079(10) 0.060(8) 0.006(7) 0.002(7) C17 0.030(6) 0.067(8) 0.076(9) 0.041(7) 0.005(6) 0.006(5) C18 0.024(6) 0.068(8) 0.087(10) 0.049(7) 0.002(6) -0.007(5) C20 0.022(5) 0.053(7) 0.086(9) 0.034(7) -0.008(6) -0.012(5) C21 0.024(8) 0.025(8) 0.16(2) 0.000 0.000 -0.009(7) C32 0.017(4) 0.023(5) 0.046(6) 0.000(4) 0.007(4) 0.009(4) C33 0.019(5) 0.039(6) 0.057(7) 0.013(5) -0.002(5) 0.001(4) C34 0.043(6) 0.057(7) 0.054(7) 0.035(6) -0.001(6) -0.009(6) C35 0.068(8) 0.064(8) 0.044(7) 0.018(6) -0.005(6) -0.007(7) C36 0.050(7) 0.050(6) 0.037(6) 0.000(5) -0.013(5) -0.003(5) C37 0.025(5) 0.028(5) 0.036(6) 0.005(4) 0.004(4) 0.005(4) C38 0.019(4) 0.030(5) 0.029(6) -0.003(4) -0.002(4) 0.001(4) C40 0.090(10) 0.058(7) 0.044(7) 0.005(6) -0.008(7) -0.045(7) C41 0.16(2) 0.060(12) 0.047(11) 0.000 0.000 -0.086(14) N19 0.018(4) 0.032(5) 0.089(8) 0.014(5) 0.001(5) -0.011(3) N39 0.027(4) 0.022(4) 0.040(5) -0.003(4) 0.004(4) -0.005(3) N5 0.050(8) 0.008(5) 0.045(7) 0.000 0.000 0.012(5) N2 0.017(6) 0.025(6) 0.034(6) 0.000 0.000 -0.005(5) O11 0.019(3) 0.032(3) 0.053(4) 0.013(3) -0.005(3) -0.006(3) O3 0.018(4) 0.017(4) 0.039(5) 0.000 0.000 -0.002(4) O31 0.023(3) 0.029(3) 0.030(4) 0.007(3) -0.004(3) 0.000(3) O4 0.040(6) 0.035(5) 0.039(6) 0.000 0.000 -0.016(5) O6 0.048(7) 0.060(8) 0.066(8) 0.000 0.000 -0.006(6) O1 0.014(5) 0.020(4) 0.053(6) 0.000 0.000 0.001(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 O11 2.039(6) . ? Ni1 O11 2.039(6) 2_665 ? Ni1 O11 2.039(6) 5_666 ? Ni1 O11 2.039(6) 6_556 ? Ni1 O3 2.128(8) 5_666 ? Ni1 O3 2.128(8) . ? Ni1 Ni4 2.9584(16) 5_666 ? Ni1 Ni4 2.9584(16) . ? Ni2 O31 2.026(6) 2_565 ? Ni2 O31 2.026(6) . ? Ni2 O31 2.026(6) 5_566 ? Ni2 O31 2.026(6) 6_556 ? Ni2 O4 2.090(9) . ? Ni2 O4 2.090(9) 5_566 ? Ni2 Ni3 2.9608(15) 5_566 ? Ni2 Ni3 2.9609(15) . ? Ni3 N39 2.003(8) 6_556 ? Ni3 N39 2.003(8) . ? Ni3 O31 2.011(6) 6_556 ? Ni3 O31 2.011(6) . ? Ni3 N5 2.087(10) . ? Ni3 O1 2.154(8) . ? Ni4 O11 1.989(6) 6_556 ? Ni4 O11 1.989(6) . ? Ni4 N2 2.001(10) . ? Ni4 N19 2.003(9) 6_556 ? Ni4 N19 2.003(9) . ? C12 O11 1.318(11) . ? C12 C13 1.394(13) . ? C12 C17 1.427(13) . ? C13 C14 1.423(15) . ? C14 C15 1.346(15) . ? C15 C16 1.386(17) . ? C16 C17 1.394(17) . ? C17 C18 1.453(16) . ? C18 N19 1.269(15) . ? C20 N19 1.481(12) . ? C20 C21 1.504(14) . ? C21 C20 1.505(14) 6_556 ? C32 O31 1.305(11) . ? C32 C37 1.409(13) . ? C32 C33 1.422(12) . ? C33 C34 1.340(14) . ? C34 C35 1.402(15) . ? C35 C36 1.381(15) . ? C36 C37 1.390(13) . ? C37 C38 1.440(12) . ? C38 N39 1.286(11) . ? C40 C41 1.385(12) . ? C40 N39 1.463(12) . ? C41 C40 1.385(12) 6_556 ? N5 O6 1.214(14) . ? N5 O4 1.321(14) . ? N2 O1 1.236(12) . ? N2 O3 1.289(12) . ? C81 Cl83 1.78(2) . ? C81 Cl82 1.85(2) . ? C81 Cl82 2.21(2) 6_556 ? Cl82 Cl82 0.782(8) 6_556 ? Cl82 C81 2.21(2) 6_556 ? Cl83 Cl83 0.977(10) 6_556 ? Cl83 C81 1.15(2) 6_556 ? 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 O11 Ni1 O11 103.7(4) . 2_665 ? O11 Ni1 O11 179.998(2) . 5_666 ? O11 Ni1 O11 76.3(4) 2_665 5_666 ? O11 Ni1 O11 76.3(4) . 6_556 ? O11 Ni1 O11 179.998(1) 2_665 6_556 ? O11 Ni1 O11 103.7(4) 5_666 6_556 ? O11 Ni1 O3 94.2(2) . 5_666 ? O11 Ni1 O3 85.8(2) 2_665 5_666 ? O11 Ni1 O3 85.8(2) 5_666 5_666 ? O11 Ni1 O3 94.2(2) 6_556 5_666 ? O11 Ni1 O3 85.8(2) . . ? O11 Ni1 O3 94.2(2) 2_665 . ? O11 Ni1 O3 94.2(2) 5_666 . ? O11 Ni1 O3 85.8(2) 6_556 . ? O3 Ni1 O3 180.0(4) 5_666 . ? O11 Ni1 Ni4 137.92(17) . 5_666 ? O11 Ni1 Ni4 42.08(17) 2_665 5_666 ? O11 Ni1 Ni4 42.09(17) 5_666 5_666 ? O11 Ni1 Ni4 137.92(17) 6_556 5_666 ? O3 Ni1 Ni4 65.4(2) 5_666 5_666 ? O3 Ni1 Ni4 114.6(2) . 5_666 ? O11 Ni1 Ni4 42.08(17) . . ? O11 Ni1 Ni4 137.92(17) 2_665 . ? O11 Ni1 Ni4 137.92(17) 5_666 . ? O11 Ni1 Ni4 42.08(17) 6_556 . ? O3 Ni1 Ni4 114.6(2) 5_666 . ? O3 Ni1 Ni4 65.4(2) . . ? Ni4 Ni1 Ni4 180.0 5_666 . ? O31 Ni2 O31 100.3(3) 2_565 . ? O31 Ni2 O31 79.7(3) 2_565 5_566 ? O31 Ni2 O31 179.998(1) . 5_566 ? O31 Ni2 O31 180.0(3) 2_565 6_556 ? O31 Ni2 O31 79.7(3) . 6_556 ? O31 Ni2 O31 100.3(3) 5_566 6_556 ? O31 Ni2 O4 94.0(2) 2_565 . ? O31 Ni2 O4 86.0(3) . . ? O31 Ni2 O4 94.0(2) 5_566 . ? O31 Ni2 O4 86.0(3) 6_556 . ? O31 Ni2 O4 86.0(3) 2_565 5_566 ? O31 Ni2 O4 94.0(2) . 5_566 ? O31 Ni2 O4 86.0(3) 5_566 5_566 ? O31 Ni2 O4 94.0(2) 6_556 5_566 ? O4 Ni2 O4 179.998(1) . 5_566 ? O31 Ni2 Ni3 42.64(16) 2_565 5_566 ? O31 Ni2 Ni3 137.36(16) . 5_566 ? O31 Ni2 Ni3 42.64(16) 5_566 5_566 ? O31 Ni2 Ni3 137.36(16) 6_556 5_566 ? O4 Ni2 Ni3 111.8(3) . 5_566 ? O4 Ni2 Ni3 68.2(3) 5_566 5_566 ? O31 Ni2 Ni3 137.36(16) 2_565 . ? O31 Ni2 Ni3 42.64(16) . . ? O31 Ni2 Ni3 137.36(16) 5_566 . ? O31 Ni2 Ni3 42.64(16) 6_556 . ? O4 Ni2 Ni3 68.2(3) . . ? O4 Ni2 Ni3 111.8(3) 5_566 . ? Ni3 Ni2 Ni3 180.0 5_566 . ? N39 Ni3 N39 98.9(4) 6_556 . ? N39 Ni3 O31 90.3(3) 6_556 6_556 ? N39 Ni3 O31 170.4(3) . 6_556 ? N39 Ni3 O31 170.4(3) 6_556 . ? N39 Ni3 O31 90.3(3) . . ? O31 Ni3 O31 80.4(3) 6_556 . ? N39 Ni3 N5 97.0(3) 6_556 . ? N39 Ni3 N5 97.0(3) . . ? O31 Ni3 N5 84.2(3) 6_556 . ? O31 Ni3 N5 84.2(3) . . ? N39 Ni3 O1 91.6(2) 6_556 . ? N39 Ni3 O1 91.6(2) . . ? O31 Ni3 O1 85.7(2) 6_556 . ? O31 Ni3 O1 85.7(2) . . ? N5 Ni3 O1 166.8(4) . . ? N39 Ni3 Ni2 129.2(2) 6_556 . ? N39 Ni3 Ni2 129.2(2) . . ? O31 Ni3 Ni2 43.03(16) 6_556 . ? O31 Ni3 Ni2 43.03(16) . . ? N5 Ni3 Ni2 65.6(3) . . ? O1 Ni3 Ni2 101.2(2) . . ? O11 Ni4 O11 78.5(4) 6_556 . ? O11 Ni4 N2 87.7(3) 6_556 . ? O11 Ni4 N2 87.7(3) . . ? O11 Ni4 N19 91.7(3) 6_556 6_556 ? O11 Ni4 N19 169.5(3) . 6_556 ? N2 Ni4 N19 95.8(3) . 6_556 ? O11 Ni4 N19 169.5(3) 6_556 . ? O11 Ni4 N19 91.7(3) . . ? N2 Ni4 N19 95.8(3) . . ? N19 Ni4 N19 97.7(5) 6_556 . ? O11 Ni4 Ni1 43.39(17) 6_556 . ? O11 Ni4 Ni1 43.39(17) . . ? N2 Ni4 Ni1 66.9(3) . . ? N19 Ni4 Ni1 129.6(3) 6_556 . ? N19 Ni4 Ni1 129.6(3) . . ? O11 C12 C13 120.8(8) . . ? O11 C12 C17 121.0(9) . . ? C13 C12 C17 118.2(10) . . ? C12 C13 C14 120.2(9) . . ? C15 C14 C13 121.1(11) . . ? C14 C15 C16 119.3(11) . . ? C17 C16 C15 122.0(11) . . ? C16 C17 C12 119.0(11) . . ? C16 C17 C18 117.1(10) . . ? C12 C17 C18 123.7(10) . . ? N19 C18 C17 129.4(10) . . ? N19 C20 C21 113.1(11) . . ? C20 C21 C20 113.4(12) . 6_556 ? O31 C32 C37 122.0(8) . . ? O31 C32 C33 120.6(8) . . ? C37 C32 C33 117.3(9) . . ? C34 C33 C32 123.0(10) . . ? C33 C34 C35 119.7(10) . . ? C36 C35 C34 118.6(10) . . ? C35 C36 C37 122.6(10) . . ? C36 C37 C32 118.7(9) . . ? C36 C37 C38 116.9(9) . . ? C32 C37 C38 124.4(8) . . ? N39 C38 C37 127.4(8) . . ? C41 C40 N39 118.7(10) . . ? C40 C41 C40 138.7(15) . 6_556 ? C18 N19 C20 118.8(9) . . ? C18 N19 Ni4 122.1(7) . . ? C20 N19 Ni4 119.0(8) . . ? C38 N39 C40 116.1(8) . . ? C38 N39 Ni3 123.3(6) . . ? C40 N39 Ni3 120.4(7) . . ? O6 N5 O4 112.9(11) . . ? O6 N5 Ni3 130.9(10) . . ? O4 N5 Ni3 116.2(7) . . ? O1 N2 O3 117.8(9) . . ? O1 N2 Ni4 124.9(8) . . ? O3 N2 Ni4 117.3(7) . . ? C12 O11 Ni4 127.7(6) . . ? C12 O11 Ni1 137.6(6) . . ? Ni4 O11 Ni1 94.5(3) . . ? N2 O3 Ni1 110.5(6) . . ? C32 O31 Ni3 125.8(5) . . ? C32 O31 Ni2 139.5(5) . . ? Ni3 O31 Ni2 94.3(2) . . ? N5 O4 Ni2 110.1(7) . . ? N2 O1 Ni3 136.5(7) . . ? Cl83 C81 Cl82 107.7(11) . . ? Cl83 C81 Cl82 88.1(9) . 6_556 ? Cl82 C81 Cl82 19.7(3) . 6_556 ? Cl82 Cl82 C81 107.7(7) 6_556 . ? Cl82 Cl82 C81 52.6(6) 6_556 6_556 ? C81 Cl82 C81 55.2(12) . 6_556 ? Cl83 Cl83 C81 114.0(11) 6_556 6_556 ? Cl83 Cl83 C81 36.0(7) 6_556 . ? C81 Cl83 C81 78.0(17) 6_556 . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 22.97 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.003 _refine_diff_density_min -0.785 _refine_diff_density_rms 0.140 _publ_section_references ; Sheldrick, G.M. (1997) SHELXL program for crystallography refinement. University of Gottingen, Germany. Spek, A.L., (2004) PLATON program, Utrecht University, The Netherlands ; #===END