# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_Compound1 _database_code_depnum_ccdc_archive 'CCDC 912356' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety 'C18 H26 Cl2 N2 Ni O2' _chemical_formula_sum 'C18 H26 Cl2 N2 Ni O2' _chemical_melting_point ? _exptl_crystal_description block _exptl_crystal_colour green _diffrn_ambient_temperature 173(2) _chemical_formula_weight 432.02 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_int_tables_number 14 _chemical_absolute_configuration ? 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 6.453(5) _cell_length_b 9.664(6) _cell_length_c 15.797(1) _cell_angle_alpha 90.00 _cell_angle_beta 101.634(5) _cell_angle_gamma 90.00 _cell_volume 964.9(10) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 2411 _cell_measurement_theta_min 0.407 _cell_measurement_theta_max 27.485 _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.487 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 452 _exptl_absorpt_coefficient_mu 1.296 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2392 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0542 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.48 _diffrn_reflns_theta_max 28.29 _reflns_number_total 2392 _reflns_number_gt 1741 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP-3 _computing_publication_material PLATON _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0409P)^2^+1.0212P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2392 _refine_ls_number_parameters 120 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0742 _refine_ls_R_factor_gt 0.0421 _refine_ls_wR_factor_ref 0.1029 _refine_ls_wR_factor_gt 0.0930 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.059 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_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 0.01709(15) Uani 1 2 d S . . Cl1 Cl 0.72449(11) 0.59754(7) 0.40573(5) 0.02607(19) Uani 1 1 d . . . O1 O 0.7736(3) 0.50497(19) 0.60029(13) 0.0208(4) Uani 1 1 d . . . N1 N 0.4229(3) 0.7023(2) 0.53135(14) 0.0181(5) Uani 1 1 d . . . C1 C 0.8241(4) 0.6188(3) 0.66174(17) 0.0203(6) Uani 1 1 d . . . C2 C 0.9413(5) 0.7296(3) 0.6221(2) 0.0304(7) Uani 1 1 d . . . H2A H 1.0753 0.6940 0.6147 0.046 Uiso 1 1 calc R . . H2B H 0.9636 0.8087 0.6595 0.046 Uiso 1 1 calc R . . H2C H 0.8589 0.7562 0.5669 0.046 Uiso 1 1 calc R . . C3 C 0.9595(5) 0.5612(4) 0.7437(2) 0.0403(9) Uani 1 1 d . . . H3A H 0.8808 0.4925 0.7678 0.060 Uiso 1 1 calc R . . H3B H 0.9987 0.6347 0.7847 0.060 Uiso 1 1 calc R . . H3C H 1.0847 0.5200 0.7306 0.060 Uiso 1 1 calc R . . C4 C 0.6144(4) 0.6698(3) 0.68024(17) 0.0222(6) Uani 1 1 d . . . H4A H 0.5306 0.5901 0.6897 0.027 Uiso 1 1 calc R . . H4B H 0.6429 0.7229 0.7335 0.027 Uiso 1 1 calc R . . C5 C 0.4858(4) 0.7572(3) 0.61088(18) 0.0192(6) Uani 1 1 d . . . C6 C 0.4347(4) 0.8934(3) 0.6280(2) 0.0245(6) Uani 1 1 d . . . H6 H 0.4840 0.9310 0.6825 0.029 Uiso 1 1 calc R . . C7 C 0.3112(5) 0.9723(3) 0.5643(2) 0.0283(7) Uani 1 1 d . . . H7 H 0.2739 1.0624 0.5756 0.034 Uiso 1 1 calc R . . C8 C 0.2448(4) 0.9146(3) 0.4840(2) 0.0255(7) Uani 1 1 d . . . H8 H 0.1599 0.9645 0.4398 0.031 Uiso 1 1 calc R . . C9 C 0.3067(4) 0.7806(3) 0.46993(19) 0.0228(6) Uani 1 1 d . . . H9 H 0.2652 0.7432 0.4149 0.027 Uiso 1 1 calc R . . H1O H 0.879(6) 0.489(3) 0.586(2) 0.034 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0190(3) 0.0154(2) 0.0169(3) -0.0002(2) 0.00348(19) -0.0008(2) Cl1 0.0271(4) 0.0274(4) 0.0257(4) 0.0010(3) 0.0101(3) -0.0035(3) O1 0.0173(9) 0.0220(10) 0.0232(10) -0.0051(9) 0.0044(8) 0.0008(9) N1 0.0163(11) 0.0175(11) 0.0211(12) -0.0001(10) 0.0053(9) -0.0021(9) C1 0.0208(14) 0.0224(14) 0.0164(14) -0.0040(11) 0.0009(11) 0.0004(11) C2 0.0233(15) 0.0265(16) 0.0436(19) -0.0034(14) 0.0121(14) -0.0051(13) C3 0.0368(19) 0.057(2) 0.0235(17) 0.0032(16) -0.0031(14) 0.0170(17) C4 0.0252(14) 0.0254(15) 0.0161(14) -0.0024(11) 0.0040(12) -0.0003(12) C5 0.0154(12) 0.0217(14) 0.0219(15) -0.0018(11) 0.0067(11) -0.0015(11) C6 0.0196(14) 0.0237(15) 0.0311(16) -0.0082(13) 0.0069(12) -0.0019(12) C7 0.0225(14) 0.0213(16) 0.044(2) -0.0033(13) 0.0132(14) 0.0011(12) C8 0.0193(14) 0.0243(15) 0.0331(17) 0.0059(13) 0.0054(12) 0.0003(12) C9 0.0197(14) 0.0213(14) 0.0265(16) 0.0022(12) 0.0024(12) -0.0010(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N1 2.101(2) . ? Ni1 N1 2.101(2) 3_666 ? Ni1 O1 2.1214(19) . ? Ni1 O1 2.1214(19) 3_666 ? Ni1 Cl1 2.465(2) 3_666 ? Ni1 Cl1 2.465(2) . ? O1 C1 1.460(3) . ? O1 H1O 0.78(4) . ? N1 C9 1.335(3) . ? N1 C5 1.349(3) . ? C1 C3 1.515(4) . ? C1 C2 1.517(4) . ? C1 C4 1.523(4) . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 C5 1.495(4) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.396(4) . ? C6 C7 1.381(4) . ? C6 H6 0.9300 . ? C7 C8 1.374(4) . ? C7 H7 0.9300 . ? C8 C9 1.387(4) . ? C8 H8 0.9300 . ? C9 H9 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ni1 N1 180.000(1) . 3_666 ? N1 Ni1 O1 90.22(8) . . ? N1 Ni1 O1 89.78(8) 3_666 . ? N1 Ni1 O1 89.78(8) . 3_666 ? N1 Ni1 O1 90.22(8) 3_666 3_666 ? O1 Ni1 O1 180.0 . 3_666 ? N1 Ni1 Cl1 90.99(6) . 3_666 ? N1 Ni1 Cl1 89.01(6) 3_666 3_666 ? O1 Ni1 Cl1 93.40(6) . 3_666 ? O1 Ni1 Cl1 86.60(6) 3_666 3_666 ? N1 Ni1 Cl1 89.01(6) . . ? N1 Ni1 Cl1 90.99(6) 3_666 . ? O1 Ni1 Cl1 86.60(6) . . ? O1 Ni1 Cl1 93.40(6) 3_666 . ? Cl1 Ni1 Cl1 180.0 3_666 . ? C1 O1 Ni1 123.68(15) . . ? C1 O1 H1O 105(3) . . ? Ni1 O1 H1O 115(3) . . ? C9 N1 C5 118.2(2) . . ? C9 N1 Ni1 118.75(19) . . ? C5 N1 Ni1 123.01(18) . . ? O1 C1 C3 107.8(2) . . ? O1 C1 C2 108.7(2) . . ? C3 C1 C2 111.3(3) . . ? O1 C1 C4 106.5(2) . . ? C3 C1 C4 109.7(2) . . ? C2 C1 C4 112.7(2) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C5 C4 C1 115.2(2) . . ? C5 C4 H4A 108.5 . . ? C1 C4 H4A 108.5 . . ? C5 C4 H4B 108.5 . . ? C1 C4 H4B 108.5 . . ? H4A C4 H4B 107.5 . . ? N1 C5 C6 120.9(3) . . ? N1 C5 C4 118.6(2) . . ? C6 C5 C4 120.5(3) . . ? C7 C6 C5 120.2(3) . . ? C7 C6 H6 119.9 . . ? C5 C6 H6 119.9 . . ? C8 C7 C6 118.4(3) . . ? C8 C7 H7 120.8 . . ? C6 C7 H7 120.8 . . ? C7 C8 C9 118.7(3) . . ? C7 C8 H8 120.6 . . ? C9 C8 H8 120.6 . . ? N1 C9 C8 123.4(3) . . ? N1 C9 H9 118.3 . . ? C8 C9 H9 118.3 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.405 _refine_diff_density_min -0.681 _refine_diff_density_rms 0.101 data_compound2 _database_code_depnum_ccdc_archive 'CCDC 912357' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety 'C28 H36 Cl2 N4 Ni2 O4, 2(C H2 Cl2), 2(Cl) ' _chemical_formula_sum 'C30 H40 Cl8 N4 Ni2 O4' _chemical_melting_point ? _exptl_crystal_description prism _exptl_crystal_colour green _diffrn_ambient_temperature 173(2) _chemical_formula_weight 921.68 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 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' 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' 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_int_tables_number 2 _chemical_absolute_configuration ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.3633(16) _cell_length_b 10.4885(8) _cell_length_c 10.5196(15) _cell_angle_alpha 91.769(8) _cell_angle_beta 116.368(6) _cell_angle_gamma 99.801(8) _cell_volume 1002.1(2) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 2290 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.103 _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.527 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 472 _exptl_absorpt_coefficient_mu 1.511 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3562 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0776 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.67 _diffrn_reflns_theta_max 25.10 _reflns_number_total 3562 _reflns_number_gt 2965 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP-3 _computing_publication_material PLATON _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. The crystals were of poor quality. However, the refinement resulted in a good quality model. N2 was refined applying an isotropic restrain, while the O2-H2O distance was refined with a restrained interatomic distance. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+14.4473P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3562 _refine_ls_number_parameters 223 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.1334 _refine_ls_R_factor_gt 0.1108 _refine_ls_wR_factor_ref 0.2001 _refine_ls_wR_factor_gt 0.1919 _refine_ls_goodness_of_fit_ref 1.254 _refine_ls_restrained_S_all 1.254 _refine_ls_shift/su_max 0.005 _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 0.99229(13) 0.37782(10) 0.37246(12) 0.0147(3) Uani 1 1 d . . . Cl1 Cl 0.9669(2) 0.6037(2) 0.3802(2) 0.0188(5) Uani 1 1 d . . . Cl2 Cl 0.6214(3) 0.2582(2) 0.5007(2) 0.0252(5) Uani 1 1 d . . . Cl3 Cl 0.5204(4) 0.0522(3) 0.8422(4) 0.0597(9) Uani 1 1 d . . . Cl4 Cl 0.7826(5) -0.0485(5) 0.8937(4) 0.0879(14) Uani 1 1 d . . . O1 O 1.2097(7) 0.4553(6) 0.4251(7) 0.0257(15) Uani 1 1 d . . . O2 O 0.7730(7) 0.3033(6) 0.3141(7) 0.0243(15) Uani 1 1 d D . . N1 N 1.0449(9) 0.1950(7) 0.3845(8) 0.0226(18) Uani 1 1 d . . . N2 N 0.9323(9) 0.3595(7) 0.1552(8) 0.0224(18) Uani 1 1 d U . . C1 C 1.3325(10) 0.3938(9) 0.4905(11) 0.029(2) Uani 1 1 d . . . H1A H 1.4187 0.4583 0.5610 0.035 Uiso 1 1 calc R . . H1B H 1.3579 0.3616 0.4168 0.035 Uiso 1 1 calc R . . C2 C 1.2986(11) 0.2816(9) 0.5644(10) 0.027(2) Uani 1 1 d . . . H2A H 1.3898 0.2486 0.6180 0.032 Uiso 1 1 calc R . . H2B H 1.2696 0.3147 0.6350 0.032 Uiso 1 1 calc R . . C3 C 1.1795(10) 0.1692(9) 0.4678(10) 0.022(2) Uani 1 1 d . . . C4 C 1.2075(12) 0.0437(9) 0.4667(11) 0.030(2) Uani 1 1 d . . . H4 H 1.3028 0.0282 0.5253 0.036 Uiso 1 1 calc R . . C5 C 1.0940(13) -0.0576(9) 0.3789(11) 0.034(3) Uani 1 1 d . . . H5 H 1.1111 -0.1437 0.3772 0.040 Uiso 1 1 calc R . . C6 C 0.9580(13) -0.0344(9) 0.2949(11) 0.032(3) Uani 1 1 d . . . H6 H 0.8788 -0.1035 0.2356 0.039 Uiso 1 1 calc R . . C7 C 0.9384(11) 0.0912(8) 0.2982(11) 0.026(2) Uani 1 1 d . . . H7 H 0.8443 0.1073 0.2363 0.031 Uiso 1 1 calc R . . C8 C 0.6476(11) 0.3033(11) 0.1784(11) 0.036(3) Uani 1 1 d . . . H8A H 0.5663 0.3252 0.1944 0.044 Uiso 1 1 calc R . . H8B H 0.6132 0.2153 0.1241 0.044 Uiso 1 1 calc R . . C9 C 0.6885(11) 0.4018(10) 0.0930(10) 0.033(2) Uani 1 1 d . . . H9A H 0.5983 0.4071 0.0055 0.040 Uiso 1 1 calc R . . H9B H 0.7265 0.4886 0.1504 0.040 Uiso 1 1 calc R . . C10 C 0.8006(11) 0.3719(9) 0.0507(10) 0.025(2) Uani 1 1 d . . . C11 C 0.7710(13) 0.3579(9) -0.0933(11) 0.034(3) Uani 1 1 d . . . H11 H 0.6778 0.3672 -0.1652 0.040 Uiso 1 1 calc R . . C12 C 0.8749(14) 0.3310(9) -0.1319(11) 0.038(3) Uani 1 1 d . . . H12 H 0.8549 0.3217 -0.2294 0.046 Uiso 1 1 calc R . . C13 C 1.0090(13) 0.3178(9) -0.0251(11) 0.033(3) Uani 1 1 d . . . H13 H 1.0837 0.2987 -0.0472 0.040 Uiso 1 1 calc R . . C14 C 1.0322(12) 0.3329(9) 0.1144(11) 0.028(2) Uani 1 1 d . . . H14 H 1.1251 0.3240 0.1872 0.033 Uiso 1 1 calc R . . C15 C 0.6289(13) 0.0054(11) 0.7653(11) 0.044(3) Uani 1 1 d . . . H15A H 0.5682 -0.0654 0.6860 0.053 Uiso 1 1 calc R . . H15B H 0.6631 0.0805 0.7254 0.053 Uiso 1 1 calc R . . H1O H 1.250(13) 0.537(12) 0.443(13) 0.053 Uiso 1 1 d . . . H2O H 0.732(12) 0.273(10) 0.370(10) 0.053 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0186(6) 0.0145(6) 0.0154(6) 0.0004(4) 0.0120(5) 0.0024(4) Cl1 0.0255(13) 0.0183(11) 0.0168(11) 0.0026(8) 0.0129(10) 0.0056(9) Cl2 0.0234(13) 0.0255(12) 0.0296(13) 0.0007(10) 0.0159(11) 0.0017(9) Cl3 0.084(3) 0.0497(19) 0.051(2) -0.0011(15) 0.0426(19) -0.0044(17) Cl4 0.081(3) 0.110(3) 0.060(2) 0.035(2) 0.015(2) 0.031(3) O1 0.021(4) 0.026(4) 0.033(4) -0.003(3) 0.015(3) 0.003(3) O2 0.021(4) 0.035(4) 0.020(4) 0.003(3) 0.014(3) 0.001(3) N1 0.035(5) 0.010(4) 0.027(4) -0.003(3) 0.020(4) -0.001(3) N2 0.029(4) 0.026(3) 0.016(3) 0.002(3) 0.017(3) -0.001(3) C1 0.019(5) 0.025(5) 0.045(7) 0.005(4) 0.015(5) 0.007(4) C2 0.027(6) 0.022(5) 0.030(6) 0.004(4) 0.010(5) 0.009(4) C3 0.028(6) 0.024(5) 0.029(5) 0.011(4) 0.024(5) 0.011(4) C4 0.036(6) 0.030(6) 0.029(6) 0.012(4) 0.016(5) 0.014(5) C5 0.059(8) 0.022(5) 0.038(6) 0.008(5) 0.031(6) 0.026(5) C6 0.055(8) 0.017(5) 0.029(6) -0.002(4) 0.026(6) -0.002(5) C7 0.033(6) 0.013(5) 0.037(6) -0.002(4) 0.022(5) -0.001(4) C8 0.016(5) 0.056(7) 0.028(6) -0.006(5) 0.006(5) -0.005(5) C9 0.028(6) 0.046(6) 0.020(5) 0.008(5) 0.005(5) 0.006(5) C10 0.032(6) 0.018(5) 0.024(5) -0.003(4) 0.017(5) -0.008(4) C11 0.049(7) 0.030(6) 0.020(5) 0.003(4) 0.019(5) -0.003(5) C12 0.068(9) 0.024(6) 0.027(6) 0.006(4) 0.028(6) 0.005(5) C13 0.059(8) 0.018(5) 0.041(7) 0.002(4) 0.040(6) 0.003(5) C14 0.040(6) 0.023(5) 0.031(6) -0.003(4) 0.026(5) 0.005(4) C15 0.059(8) 0.046(7) 0.018(6) 0.009(5) 0.013(6) 0.002(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 O2 2.069(6) . ? Ni1 O1 2.070(7) . ? Ni1 N1 2.073(7) . ? Ni1 N2 2.078(7) . ? Ni1 Cl1 2.431(2) . ? Ni1 Cl1 2.439(2) 2_766 ? Cl1 Ni1 2.439(2) 2_766 ? Cl3 C15 1.769(12) . ? Cl4 C15 1.768(12) . ? O1 C1 1.428(11) . ? O2 C8 1.441(12) . ? N1 C3 1.358(12) . ? N1 C7 1.367(11) . ? N2 C14 1.348(12) . ? N2 C10 1.351(12) . ? C1 C2 1.507(13) . ? C2 C3 1.504(13) . ? C3 C4 1.396(13) . ? C4 C5 1.384(14) . ? C5 C6 1.360(15) . ? C6 C7 1.368(13) . ? C8 C9 1.517(14) . ? C9 C10 1.491(14) . ? C10 C11 1.402(13) . ? C11 C12 1.374(15) . ? C12 C13 1.379(16) . ? C13 C14 1.377(13) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Ni1 O1 178.2(3) . . ? O2 Ni1 N1 93.3(3) . . ? O1 Ni1 N1 87.7(3) . . ? O2 Ni1 N2 86.4(3) . . ? O1 Ni1 N2 92.1(3) . . ? N1 Ni1 N2 89.9(3) . . ? O2 Ni1 Cl1 94.15(19) . . ? O1 Ni1 Cl1 84.92(19) . . ? N1 Ni1 Cl1 172.0(2) . . ? N2 Ni1 Cl1 93.6(2) . . ? O2 Ni1 Cl1 87.39(18) . 2_766 ? O1 Ni1 Cl1 94.1(2) . 2_766 ? N1 Ni1 Cl1 92.2(2) . 2_766 ? N2 Ni1 Cl1 173.5(2) . 2_766 ? Cl1 Ni1 Cl1 85.19(8) . 2_766 ? Ni1 Cl1 Ni1 94.81(8) . 2_766 ? C1 O1 Ni1 127.2(6) . . ? C8 O2 Ni1 127.8(6) . . ? C3 N1 C7 116.2(8) . . ? C3 N1 Ni1 125.4(6) . . ? C7 N1 Ni1 118.3(7) . . ? C14 N2 C10 117.0(8) . . ? C14 N2 Ni1 117.7(7) . . ? C10 N2 Ni1 125.2(6) . . ? O1 C1 C2 111.0(8) . . ? C3 C2 C1 115.4(8) . . ? N1 C3 C4 122.0(9) . . ? N1 C3 C2 117.3(8) . . ? C4 C3 C2 120.6(9) . . ? C5 C4 C3 118.9(9) . . ? C6 C5 C4 120.2(9) . . ? C5 C6 C7 118.2(10) . . ? N1 C7 C6 124.5(10) . . ? O2 C8 C9 110.2(8) . . ? C10 C9 C8 114.5(9) . . ? N2 C10 C11 120.8(9) . . ? N2 C10 C9 118.1(8) . . ? C11 C10 C9 121.1(9) . . ? C12 C11 C10 121.0(10) . . ? C11 C12 C13 118.1(10) . . ? C14 C13 C12 118.4(10) . . ? N2 C14 C13 124.7(10) . . ? Cl4 C15 Cl3 111.1(6) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.10 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.774 _refine_diff_density_min -0.740 _refine_diff_density_rms 0.150 data_compound3 _database_code_depnum_ccdc_archive 'CCDC 912358' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H52 Cl8 N4 Ni4 O4' _chemical_formula_sum 'C36 H52 Cl8 N4 Ni4 O4' _chemical_formula_weight 1123.26 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' 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' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'I 41/a' _symmetry_int_tables_number 88 _chemical_absolute_configuration ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y+1/2, z' '-y+3/4, x+1/4, z+1/4' 'y+1/4, -x+1/4, z+1/4' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1, z+1/2' '-y+5/4, x+3/4, z+3/4' 'y+3/4, -x+3/4, z+3/4' '-x, -y, -z' 'x, y-1/2, -z' 'y-3/4, -x-1/4, -z-1/4' '-y-1/4, x-1/4, -z-1/4' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y, -z+1/2' 'y-1/4, -x+1/4, -z+1/4' '-y+1/4, x+1/4, -z+1/4' _cell_length_a 17.4746(11) _cell_length_b 17.4746(11) _cell_length_c 19.6937(16) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6013.7(7) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 3056 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.103 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.241 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2304 _exptl_absorpt_coefficient_mu 1.620 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5497 _diffrn_reflns_av_R_equivalents 0.0383 _diffrn_reflns_av_sigmaI/netI 0.0803 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 27.07 _reflns_number_total 3312 _reflns_number_gt 1782 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP-3 _computing_publication_material PLATON _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. the solvent (probably dichloromethane, was disordered around a 4-fold rotoinversion. Attempts to locate the atomic position failed. A Platon-squeeze procedure was then applied (solvent accessible volume: 1980.1 A3, elecron count/cell: 1332) ; loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.012 -0.002 -0.003 1977 1332 ' ' _platon_squeeze_details ; solvent accessible volume: 1980.1 A3, elecron count/cell: 1332 ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0800P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3312 _refine_ls_number_parameters 133 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1021 _refine_ls_R_factor_gt 0.0555 _refine_ls_wR_factor_ref 0.1534 _refine_ls_wR_factor_gt 0.1402 _refine_ls_goodness_of_fit_ref 0.961 _refine_ls_restrained_S_all 0.961 _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 Ni1 Ni 0.96356(3) 0.15260(3) 0.68721(3) 0.0358(2) Uani 1 1 d . . . O1 O 0.85438(16) 0.10909(17) 0.67497(16) 0.0385(7) Uani 1 1 d . . . N1 N 0.95358(19) 0.1509(2) 0.79083(18) 0.0406(9) Uani 1 1 d . . . Cl1 Cl 1.02717(6) 0.03396(6) 0.68300(6) 0.0431(3) Uani 1 1 d . . . Cl2 Cl 0.96679(6) 0.16237(6) 0.56419(6) 0.0443(3) Uani 1 1 d . . . C1 C 0.8022(2) 0.0956(3) 0.7332(2) 0.0436(11) Uani 1 1 d . . . C2 C 0.7210(2) 0.0958(3) 0.7052(3) 0.0582(14) Uani 1 1 d . . . H2A H 0.7077 0.1467 0.6909 0.087 Uiso 1 1 calc R . . H2B H 0.6861 0.0794 0.7399 0.087 Uiso 1 1 calc R . . H2C H 0.7179 0.0616 0.6671 0.087 Uiso 1 1 calc R . . C3 C 0.8124(3) 0.1594(3) 0.7839(2) 0.0495(12) Uani 1 1 d . . . H3A H 0.8102 0.2078 0.7600 0.059 Uiso 1 1 calc R . . H3B H 0.7697 0.1581 0.8155 0.059 Uiso 1 1 calc R . . C4 C 0.8233(3) 0.0165(3) 0.7611(3) 0.0579(14) Uani 1 1 d . . . H4A H 0.8113 -0.0219 0.7278 0.087 Uiso 1 1 calc R . . H4B H 0.7946 0.0067 0.8018 0.087 Uiso 1 1 calc R . . H4C H 0.8770 0.0150 0.7711 0.087 Uiso 1 1 calc R . . C5 C 0.8857(3) 0.1566(3) 0.8241(2) 0.0455(12) Uani 1 1 d . . . C6 C 0.8841(3) 0.1578(3) 0.8946(3) 0.0611(14) Uani 1 1 d . . . H6 H 0.8377 0.1628 0.9172 0.073 Uiso 1 1 calc R . . C7 C 0.9522(4) 0.1513(4) 0.9317(3) 0.0824(19) Uani 1 1 d . . . H7 H 0.9514 0.1502 0.9789 0.099 Uiso 1 1 calc R . . C8 C 1.0193(3) 0.1469(3) 0.8972(3) 0.0746(17) Uani 1 1 d . . . H8 H 1.0656 0.1445 0.9204 0.089 Uiso 1 1 calc R . . C9 C 1.0174(3) 0.1459(3) 0.8271(3) 0.0551(13) Uani 1 1 d . . . H9 H 1.0636 0.1415 0.8040 0.066 Uiso 1 1 calc R . . H1O H 0.827(3) 0.134(3) 0.648(3) 0.09(2) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0313(3) 0.0392(3) 0.0370(4) -0.0015(3) 0.0007(2) 0.0023(2) O1 0.0297(15) 0.0404(17) 0.045(2) -0.0018(15) 0.0048(15) 0.0007(14) N1 0.037(2) 0.050(2) 0.035(2) -0.0028(17) 0.0050(17) 0.0090(17) Cl1 0.0442(6) 0.0400(6) 0.0452(7) 0.0038(5) 0.0032(5) 0.0052(5) Cl2 0.0421(6) 0.0409(6) 0.0497(7) 0.0035(5) 0.0024(5) 0.0001(5) C1 0.039(2) 0.041(3) 0.051(3) 0.003(2) 0.006(2) -0.002(2) C2 0.037(3) 0.059(3) 0.078(4) -0.001(3) 0.008(3) -0.003(2) C3 0.050(3) 0.043(3) 0.055(3) 0.004(2) 0.016(2) 0.005(2) C4 0.061(3) 0.051(3) 0.061(3) 0.011(3) 0.014(3) 0.003(3) C5 0.050(3) 0.039(2) 0.048(3) 0.000(2) 0.004(2) 0.008(2) C6 0.058(3) 0.070(4) 0.055(4) 0.001(3) 0.011(3) 0.005(3) C7 0.097(5) 0.101(5) 0.049(4) 0.001(3) 0.007(4) 0.009(4) C8 0.066(4) 0.108(5) 0.050(4) -0.002(3) -0.009(3) 0.006(3) C9 0.051(3) 0.065(3) 0.049(3) -0.002(3) -0.008(3) 0.010(2) _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 N1 2.048(4) . ? Ni1 O1 2.068(3) . ? Ni1 Cl1 2.3537(12) . ? Ni1 Cl2 2.4294(13) . ? Ni1 Cl2 2.4413(12) 16_646 ? Ni1 Cl2 2.4516(12) 15_666 ? O1 C1 1.484(5) . ? O1 H1O 0.83(5) . ? N1 C9 1.328(6) . ? N1 C5 1.358(5) . ? Cl2 Ni1 2.4413(12) 15_666 ? Cl2 Ni1 2.4516(12) 16_646 ? C1 C3 1.508(6) . ? C1 C2 1.522(6) . ? C1 C4 1.534(6) . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 C5 1.508(6) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 C6 1.388(6) . ? C6 C7 1.401(8) . ? C6 H6 0.9300 . ? C7 C8 1.356(8) . ? C7 H7 0.9300 . ? C8 C9 1.382(7) . ? C8 H8 0.9300 . ? C9 H9 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ni1 O1 91.84(13) . . ? N1 Ni1 Cl1 93.57(10) . . ? O1 Ni1 Cl1 96.19(9) . . ? N1 Ni1 Cl2 175.24(10) . . ? O1 Ni1 Cl2 86.04(9) . . ? Cl1 Ni1 Cl2 90.90(4) . . ? N1 Ni1 Cl2 95.38(11) . 16_646 ? O1 Ni1 Cl2 170.75(10) . 16_646 ? Cl1 Ni1 Cl2 89.14(4) . 16_646 ? Cl2 Ni1 Cl2 86.32(4) . 16_646 ? N1 Ni1 Cl2 89.66(10) . 15_666 ? O1 Ni1 Cl2 90.25(9) . 15_666 ? Cl1 Ni1 Cl2 172.70(4) . 15_666 ? Cl2 Ni1 Cl2 86.09(4) . 15_666 ? Cl2 Ni1 Cl2 84.04(4) 16_646 15_666 ? C1 O1 Ni1 122.4(3) . . ? C1 O1 H1O 103(4) . . ? Ni1 O1 H1O 115(4) . . ? C9 N1 C5 118.6(4) . . ? C9 N1 Ni1 117.8(3) . . ? C5 N1 Ni1 123.6(3) . . ? Ni1 Cl2 Ni1 93.62(4) . 15_666 ? Ni1 Cl2 Ni1 93.36(4) . 16_646 ? Ni1 Cl2 Ni1 95.95(4) 15_666 16_646 ? O1 C1 C3 108.8(3) . . ? O1 C1 C2 107.1(4) . . ? C3 C1 C2 110.4(4) . . ? O1 C1 C4 105.8(4) . . ? C3 C1 C4 113.6(4) . . ? C2 C1 C4 110.9(4) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C5 C3 C1 115.1(4) . . ? C5 C3 H3A 108.5 . . ? C1 C3 H3A 108.5 . . ? C5 C3 H3B 108.5 . . ? C1 C3 H3B 108.5 . . ? H3A C3 H3B 107.5 . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N1 C5 C6 120.1(4) . . ? N1 C5 C3 119.4(4) . . ? C6 C5 C3 120.4(4) . . ? C5 C6 C7 120.2(5) . . ? C5 C6 H6 119.9 . . ? C7 C6 H6 119.9 . . ? C8 C7 C6 118.6(6) . . ? C8 C7 H7 120.7 . . ? C6 C7 H7 120.7 . . ? C7 C8 C9 118.7(5) . . ? C7 C8 H8 120.7 . . ? C9 C8 H8 120.7 . . ? N1 C9 C8 123.9(5) . . ? N1 C9 H9 118.1 . . ? C8 C9 H9 118.1 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.07 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.493 _refine_diff_density_min -0.570 _refine_diff_density_rms 0.114 data_compound4 _database_code_depnum_ccdc_archive 'CCDC 912359' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety 'C28 H36 Cl8 N4 Ni4 O4, 2(C H Cl3)' _chemical_formula_sum 'C30 H38 Cl14 N4 Ni4 O4' _chemical_melting_point ? _exptl_crystal_description prism _exptl_crystal_colour yellow _diffrn_ambient_temperature 173(2) _chemical_formula_weight 1249.78 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 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' 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' 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' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'I 41/a' _symmetry_int_tables_number 88 _chemical_absolute_configuration ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y+1/2, z' '-y+3/4, x+1/4, z+1/4' 'y+1/4, -x+1/4, z+1/4' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1, z+1/2' '-y+5/4, x+3/4, z+3/4' 'y+3/4, -x+3/4, z+3/4' '-x, -y, -z' 'x, y-1/2, -z' 'y-3/4, -x-1/4, -z-1/4' '-y-1/4, x-1/4, -z-1/4' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y, -z+1/2' 'y-1/4, -x+1/4, -z+1/4' '-y+1/4, x+1/4, -z+1/4' _cell_length_a 15.037(4) _cell_length_b 15.037(4) _cell_length_c 40.887(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9246(5) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5594 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.878 _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.796 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5024 _exptl_absorpt_coefficient_mu 2.453 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10179 _diffrn_reflns_av_R_equivalents 0.0620 _diffrn_reflns_av_sigmaI/netI 0.0877 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_limit_l_max 53 _diffrn_reflns_theta_min 1.44 _diffrn_reflns_theta_max 27.86 _reflns_number_total 5517 _reflns_number_gt 2837 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP-3 _computing_publication_material PLATON _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. A chloroform molecule was found disordered over two positions with no atom in common. These were refined unrestrained and anisotropically. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0924P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5517 _refine_ls_number_parameters 292 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1354 _refine_ls_R_factor_gt 0.0528 _refine_ls_wR_factor_ref 0.1796 _refine_ls_wR_factor_gt 0.1287 _refine_ls_goodness_of_fit_ref 0.979 _refine_ls_restrained_S_all 0.979 _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 Ni1 Ni 0.47487(4) 0.37151(4) 0.707347(17) 0.0240(2) Uani 1 1 d . . . Ni2 Ni 0.37927(4) 0.22571(4) 0.647686(17) 0.0250(2) Uani 1 1 d . . . Cl1 Cl 0.60448(8) 0.27374(8) 0.70729(3) 0.0239(3) Uani 1 1 d . . . Cl2 Cl 0.56569(9) 0.49873(9) 0.70336(4) 0.0362(4) Uani 1 1 d . . . Cl3 Cl 0.47677(8) 0.35569(8) 0.64742(3) 0.0265(3) Uani 1 1 d . . . Cl4 Cl 0.25172(8) 0.31486(9) 0.65256(4) 0.0330(4) Uani 1 1 d . . . O1 O 0.3564(2) 0.4350(2) 0.70005(10) 0.0305(9) Uani 1 1 d . . . O2 O 0.3165(2) 0.1074(3) 0.65528(10) 0.0311(9) Uani 1 1 d . . . N1 N 0.4633(3) 0.3784(3) 0.75715(11) 0.0253(10) Uani 1 1 d . . . N2 N 0.3686(3) 0.2156(3) 0.59769(11) 0.0320(11) Uani 1 1 d . . . C1 C 0.3007(4) 0.4587(4) 0.72741(14) 0.0349(14) Uani 1 1 d . . . H1A H 0.2405 0.4678 0.7196 0.042 Uiso 1 1 calc R . . H1B H 0.3215 0.5145 0.7365 0.042 Uiso 1 1 calc R . . C2 C 0.2996(3) 0.3898(4) 0.75401(14) 0.0329(14) Uani 1 1 d . . . H2A H 0.2859 0.3326 0.7443 0.040 Uiso 1 1 calc R . . H2B H 0.2519 0.4041 0.7691 0.040 Uiso 1 1 calc R . . C3 C 0.3850(3) 0.3809(3) 0.77321(14) 0.0289(13) Uani 1 1 d . . . C4 C 0.3821(4) 0.3783(4) 0.80716(15) 0.0418(15) Uani 1 1 d . . . H4 H 0.3276 0.3799 0.8179 0.050 Uiso 1 1 calc R . . C5 C 0.4609(4) 0.3731(4) 0.82522(15) 0.0449(16) Uani 1 1 d . . . H5 H 0.4596 0.3709 0.8479 0.054 Uiso 1 1 calc R . . C6 C 0.5405(4) 0.3715(4) 0.80854(14) 0.0371(14) Uani 1 1 d . . . H6 H 0.5942 0.3683 0.8197 0.045 Uiso 1 1 calc R . . C7 C 0.5386(4) 0.3748(4) 0.77500(14) 0.0324(14) Uani 1 1 d . . . H7 H 0.5925 0.3746 0.7639 0.039 Uiso 1 1 calc R . . C8 C 0.2842(4) 0.0586(4) 0.62739(15) 0.0398(15) Uani 1 1 d . . . H8A H 0.2307 0.0871 0.6192 0.048 Uiso 1 1 calc R . . H8B H 0.2684 -0.0011 0.6342 0.048 Uiso 1 1 calc R . . C9 C 0.3517(4) 0.0532(4) 0.60006(16) 0.0457(17) Uani 1 1 d . . . H9A H 0.4088 0.0370 0.6093 0.055 Uiso 1 1 calc R . . H9B H 0.3341 0.0062 0.5852 0.055 Uiso 1 1 calc R . . C10 C 0.3625(4) 0.1384(4) 0.58085(16) 0.0387(15) Uani 1 1 d . . . C11 C 0.3641(4) 0.1380(6) 0.54694(17) 0.059(2) Uani 1 1 d . . . H11 H 0.3609 0.0843 0.5357 0.071 Uiso 1 1 calc R . . C12 C 0.3703(5) 0.2151(7) 0.53001(19) 0.070(3) Uani 1 1 d . . . H12 H 0.3725 0.2143 0.5073 0.085 Uiso 1 1 calc R . . C13 C 0.3735(5) 0.2945(5) 0.54657(17) 0.061(2) Uani 1 1 d . . . H13 H 0.3763 0.3484 0.5354 0.073 Uiso 1 1 calc R . . C14 C 0.3723(4) 0.2917(5) 0.58060(15) 0.0447(16) Uani 1 1 d . . . H14 H 0.3742 0.3451 0.5920 0.054 Uiso 1 1 calc R . . H1O H 0.318(4) 0.409(4) 0.6879(14) 0.034(17) Uiso 1 1 d . . . H2O H 0.349(4) 0.069(4) 0.6641(16) 0.06(2) Uiso 1 1 d . . . Cl1A Cl 0.4376(5) 0.5599(7) 0.5951(3) 0.134(5) Uani 0.50 1 d P A 1 Cl1B Cl 0.4526(7) 0.6038(8) 0.6108(3) 0.149(4) Uani 0.50 1 d P B 2 Cl2A Cl 0.5705(8) 0.6579(10) 0.5596(5) 0.118(5) Uani 0.50 1 d P A 1 Cl2B Cl 0.5650(8) 0.6476(9) 0.5543(4) 0.098(4) Uani 0.50 1 d P B 2 Cl3A Cl 0.4533(6) 0.5345(6) 0.5273(3) 0.139(3) Uani 0.50 1 d P A 1 Cl3B Cl 0.4373(6) 0.5144(5) 0.5524(3) 0.127(3) Uani 0.50 1 d P B 2 C15A C 0.463(2) 0.613(3) 0.5564(5) 0.059(5) Uani 0.50 1 d P A 1 H15A H 0.4201 0.6604 0.5523 0.071 Uiso 0.50 1 calc PR A 1 C15B C 0.466(2) 0.618(3) 0.5714(5) 0.059(5) Uani 0.50 1 d P B 2 H15B H 0.4214 0.6621 0.5643 0.071 Uiso 0.50 1 calc PR B 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 0.0226(4) 0.0232(4) 0.0263(4) -0.0015(3) 0.0025(3) 0.0004(3) Ni2 0.0229(4) 0.0265(4) 0.0254(4) -0.0004(3) -0.0027(3) 0.0016(3) Cl1 0.0207(6) 0.0250(6) 0.0260(7) -0.0004(6) 0.0002(5) -0.0005(5) Cl2 0.0404(8) 0.0261(7) 0.0421(9) -0.0045(7) 0.0091(7) -0.0075(6) Cl3 0.0248(7) 0.0264(7) 0.0282(8) 0.0027(6) 0.0009(6) 0.0010(5) Cl4 0.0261(7) 0.0367(8) 0.0363(9) -0.0003(7) -0.0042(6) 0.0072(6) O1 0.025(2) 0.033(2) 0.034(2) 0.0011(19) -0.0009(19) 0.0061(17) O2 0.028(2) 0.030(2) 0.035(2) 0.0003(19) -0.0069(19) -0.0023(17) N1 0.024(2) 0.029(2) 0.023(3) 0.001(2) 0.003(2) 0.0004(19) N2 0.027(3) 0.047(3) 0.023(3) 0.001(2) -0.007(2) 0.002(2) C1 0.028(3) 0.037(3) 0.039(4) -0.004(3) 0.004(3) 0.013(2) C2 0.025(3) 0.037(3) 0.037(4) -0.004(3) 0.011(3) -0.003(2) C3 0.030(3) 0.025(3) 0.032(3) -0.006(3) 0.008(3) 0.000(2) C4 0.037(4) 0.051(4) 0.038(4) 0.006(3) 0.013(3) 0.004(3) C5 0.059(4) 0.052(4) 0.024(3) -0.007(3) 0.005(3) 0.008(3) C6 0.043(4) 0.042(3) 0.026(3) -0.001(3) -0.002(3) 0.004(3) C7 0.025(3) 0.036(3) 0.036(4) -0.005(3) 0.004(3) 0.000(2) C8 0.044(4) 0.031(3) 0.044(4) -0.009(3) -0.012(3) -0.008(3) C9 0.039(4) 0.051(4) 0.048(4) -0.024(4) -0.011(3) 0.002(3) C10 0.023(3) 0.058(4) 0.035(4) -0.015(3) -0.006(3) 0.000(3) C11 0.036(4) 0.101(6) 0.040(4) -0.033(4) 0.005(3) -0.023(4) C12 0.051(5) 0.129(8) 0.031(4) 0.003(5) 0.000(4) -0.038(5) C13 0.060(5) 0.086(6) 0.037(4) 0.016(4) -0.015(4) -0.023(4) C14 0.040(4) 0.068(5) 0.026(3) 0.007(3) -0.012(3) -0.003(3) Cl1A 0.049(3) 0.164(9) 0.188(12) 0.100(8) 0.014(5) 0.023(5) Cl1B 0.100(7) 0.182(10) 0.164(10) -0.005(7) 0.028(6) 0.011(6) Cl2A 0.042(5) 0.074(6) 0.239(14) 0.041(7) -0.024(6) -0.012(4) Cl2B 0.074(7) 0.071(6) 0.150(8) 0.049(5) 0.060(6) 0.035(5) Cl3A 0.126(6) 0.107(6) 0.185(9) 0.004(6) -0.030(7) 0.035(4) Cl3B 0.118(5) 0.067(4) 0.197(10) -0.013(6) -0.037(7) 0.012(3) C15A 0.045(5) 0.075(7) 0.057(16) 0.027(17) -0.012(15) 0.001(5) C15B 0.045(5) 0.075(7) 0.057(16) 0.027(17) -0.012(15) 0.001(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 O1 2.043(4) . ? Ni1 N1 2.046(4) . ? Ni1 Cl2 2.3562(16) . ? Ni1 Cl1 2.4414(15) . ? Ni1 Cl3 2.4618(18) . ? Ni1 Cl1 2.4889(15) 2_655 ? Ni2 O2 2.037(4) . ? Ni2 N2 2.056(5) . ? Ni2 Cl4 2.3485(15) . ? Ni2 Cl3 2.4434(16) . ? Ni2 Cl1 2.4494(17) 2_655 ? Ni2 Cl3 2.4870(15) 2_655 ? Cl1 Ni2 2.4494(17) 2_655 ? Cl1 Ni1 2.4889(15) 2_655 ? Cl3 Ni2 2.4870(15) 2_655 ? O1 C1 1.442(6) . ? O1 H1O 0.86(6) . ? O2 C8 1.441(7) . ? O2 H2O 0.84(6) . ? N1 C7 1.348(7) . ? N1 C3 1.349(6) . ? N2 C14 1.341(8) . ? N2 C10 1.353(7) . ? C1 C2 1.502(8) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C3 1.511(7) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.389(8) . ? C4 C5 1.398(8) . ? C4 H4 0.9300 . ? C5 C6 1.378(8) . ? C5 H5 0.9300 . ? C6 C7 1.373(8) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C9 1.512(8) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.512(9) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.387(9) . ? C11 C12 1.353(10) . ? C11 H11 0.9300 . ? C12 C13 1.374(11) . ? C12 H12 0.9300 . ? C13 C14 1.392(9) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? Cl1A C15A 1.81(3) . ? Cl1B C15B 1.64(2) . ? Cl2A C15A 1.76(4) . ? Cl2B C15B 1.71(4) . ? Cl3A C15A 1.68(3) . ? Cl3B C15B 1.79(4) . ? C15A H15A 0.9800 . ? C15B H15B 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ni1 N1 92.71(16) . . ? O1 Ni1 Cl2 96.65(12) . . ? N1 Ni1 Cl2 94.44(12) . . ? O1 Ni1 Cl1 167.80(12) . . ? N1 Ni1 Cl1 95.71(12) . . ? Cl2 Ni1 Cl1 91.50(5) . . ? O1 Ni1 Cl3 84.84(12) . . ? N1 Ni1 Cl3 175.02(12) . . ? Cl2 Ni1 Cl3 90.16(5) . . ? Cl1 Ni1 Cl3 86.08(5) . . ? O1 Ni1 Cl1 89.55(12) . 2_655 ? N1 Ni1 Cl1 90.25(12) . 2_655 ? Cl2 Ni1 Cl1 172.04(5) . 2_655 ? Cl1 Ni1 Cl1 81.62(5) . 2_655 ? Cl3 Ni1 Cl1 85.40(5) . 2_655 ? O2 Ni2 N2 92.93(18) . . ? O2 Ni2 Cl4 96.16(12) . . ? N2 Ni2 Cl4 93.61(13) . . ? O2 Ni2 Cl3 167.68(12) . . ? N2 Ni2 Cl3 95.82(14) . . ? Cl4 Ni2 Cl3 91.94(5) . . ? O2 Ni2 Cl1 84.11(12) . 2_655 ? N2 Ni2 Cl1 175.77(14) . 2_655 ? Cl4 Ni2 Cl1 89.72(5) . 2_655 ? Cl3 Ni2 Cl1 86.66(5) . 2_655 ? O2 Ni2 Cl3 88.51(12) . 2_655 ? N2 Ni2 Cl3 91.55(13) . 2_655 ? Cl4 Ni2 Cl3 172.85(6) . 2_655 ? Cl3 Ni2 Cl3 82.61(5) . 2_655 ? Cl1 Ni2 Cl3 85.36(5) 2_655 2_655 ? Ni1 Cl1 Ni2 94.50(5) . 2_655 ? Ni1 Cl1 Ni1 98.38(5) . 2_655 ? Ni2 Cl1 Ni1 92.96(5) 2_655 2_655 ? Ni2 Cl3 Ni1 93.78(5) . . ? Ni2 Cl3 Ni2 97.39(5) . 2_655 ? Ni1 Cl3 Ni2 93.06(5) . 2_655 ? C1 O1 Ni1 120.6(3) . . ? C1 O1 H1O 99(4) . . ? Ni1 O1 H1O 118(4) . . ? C8 O2 Ni2 118.7(3) . . ? C8 O2 H2O 101(5) . . ? Ni2 O2 H2O 113(5) . . ? C7 N1 C3 118.1(5) . . ? C7 N1 Ni1 117.7(4) . . ? C3 N1 Ni1 124.1(4) . . ? C14 N2 C10 118.0(5) . . ? C14 N2 Ni2 116.9(4) . . ? C10 N2 Ni2 125.1(4) . . ? O1 C1 C2 113.4(4) . . ? O1 C1 H1A 108.9 . . ? C2 C1 H1A 108.9 . . ? O1 C1 H1B 108.9 . . ? C2 C1 H1B 108.9 . . ? H1A C1 H1B 107.7 . . ? C1 C2 C3 115.3(5) . . ? C1 C2 H2A 108.4 . . ? C3 C2 H2A 108.4 . . ? C1 C2 H2B 108.4 . . ? C3 C2 H2B 108.4 . . ? H2A C2 H2B 107.5 . . ? N1 C3 C4 120.9(5) . . ? N1 C3 C2 119.4(5) . . ? C4 C3 C2 119.7(5) . . ? C3 C4 C5 120.2(6) . . ? C3 C4 H4 119.9 . . ? C5 C4 H4 119.9 . . ? C6 C5 C4 118.4(6) . . ? C6 C5 H5 120.8 . . ? C4 C5 H5 120.8 . . ? C7 C6 C5 118.4(6) . . ? C7 C6 H6 120.8 . . ? C5 C6 H6 120.8 . . ? N1 C7 C6 124.1(5) . . ? N1 C7 H7 118.0 . . ? C6 C7 H7 118.0 . . ? O2 C8 C9 112.7(5) . . ? O2 C8 H8A 109.1 . . ? C9 C8 H8A 109.1 . . ? O2 C8 H8B 109.1 . . ? C9 C8 H8B 109.1 . . ? H8A C8 H8B 107.8 . . ? C10 C9 C8 114.2(5) . . ? C10 C9 H9A 108.7 . . ? C8 C9 H9A 108.7 . . ? C10 C9 H9B 108.7 . . ? C8 C9 H9B 108.7 . . ? H9A C9 H9B 107.6 . . ? N2 C10 C11 120.7(6) . . ? N2 C10 C9 118.1(6) . . ? C11 C10 C9 121.2(6) . . ? C12 C11 C10 120.6(7) . . ? C12 C11 H11 119.7 . . ? C10 C11 H11 119.7 . . ? C11 C12 C13 119.7(7) . . ? C11 C12 H12 120.2 . . ? C13 C12 H12 120.2 . . ? C12 C13 C14 117.7(7) . . ? C12 C13 H13 121.1 . . ? C14 C13 H13 121.1 . . ? N2 C14 C13 123.2(7) . . ? N2 C14 H14 118.4 . . ? C13 C14 H14 118.4 . . ? Cl3A C15A Cl2A 114(2) . . ? Cl3A C15A Cl1A 107(2) . . ? Cl2A C15A Cl1A 107.4(14) . . ? Cl3A C15A H15A 109.5 . . ? Cl2A C15A H15A 109.5 . . ? Cl1A C15A H15A 109.5 . . ? Cl1B C15B Cl2B 122.7(19) . . ? Cl1B C15B Cl3B 106(2) . . ? Cl2B C15B Cl3B 104.8(19) . . ? Cl1B C15B H15B 107.4 . . ? Cl2B C15B H15B 107.4 . . ? Cl3B C15B H15B 107.4 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.86 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.919 _refine_diff_density_min -1.291 _refine_diff_density_rms 0.271 data_compound5 _database_code_depnum_ccdc_archive 'CCDC 912360' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety 'C36 H56 Cl4 N4 Ni4 O8, 3(C H2 Cl2) ' _chemical_formula_sum 'C39 H62 Cl10 N4 Ni4 O8' _chemical_melting_point ? _exptl_crystal_description prism _exptl_crystal_colour green _diffrn_ambient_temperature 173(2) _chemical_formula_weight 1304.27 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 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' 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' 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_int_tables_number 2 _chemical_absolute_configuration ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.8999(4) _cell_length_b 13.8702(4) _cell_length_c 16.8384(6) _cell_angle_alpha 80.868(2) _cell_angle_beta 72.476(2) _cell_angle_gamma 72.690(2) _cell_volume 2734.94(15) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 7198 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.485 _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.584 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1340 _exptl_absorpt_coefficient_mu 1.893 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18588 _diffrn_reflns_av_R_equivalents 0.0342 _diffrn_reflns_av_sigmaI/netI 0.0824 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.27 _diffrn_reflns_theta_max 27.47 _reflns_number_total 12454 _reflns_number_gt 8232 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP-3 _computing_publication_material PLATON _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0740P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12454 _refine_ls_number_parameters 606 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0956 _refine_ls_R_factor_gt 0.0493 _refine_ls_wR_factor_ref 0.1501 _refine_ls_wR_factor_gt 0.1104 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.062 _refine_ls_shift/su_max 0.005 _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 0.19549(4) 0.41361(4) 0.20463(3) 0.01743(13) Uani 1 1 d . . . Ni2 Ni 0.07080(4) 0.27276(4) 0.16307(3) 0.01930(14) Uani 1 1 d . . . Ni3 Ni -0.05144(4) 0.41240(4) 0.31475(3) 0.01859(14) Uani 1 1 d . . . Ni4 Ni 0.15286(4) 0.22301(4) 0.32749(3) 0.01856(13) Uani 1 1 d . . . Cl1 Cl 0.36503(8) 0.39755(8) 0.24429(7) 0.0265(2) Uani 1 1 d . . . Cl2 Cl -0.10949(9) 0.29970(9) 0.13665(7) 0.0289(3) Uani 1 1 d . . . Cl4 Cl 0.20266(9) 0.04498(8) 0.30572(7) 0.0279(3) Uani 1 1 d . . . Cl3 Cl -0.09298(9) 0.59099(8) 0.32844(7) 0.0284(3) Uani 1 1 d . . . N1 N 0.2824(3) 0.4381(3) 0.0805(2) 0.0206(8) Uani 1 1 d . . . N2 N 0.1493(3) 0.2873(3) 0.0346(2) 0.0222(8) Uani 1 1 d . . . N3 N -0.1391(3) 0.3935(3) 0.4408(2) 0.0210(8) Uani 1 1 d . . . N4 N 0.0844(3) 0.1909(3) 0.4541(2) 0.0223(8) Uani 1 1 d . . . O1 O 0.1406(2) 0.5711(2) 0.21733(17) 0.0202(6) Uani 1 1 d D . . O2 O 0.1048(3) 0.1158(2) 0.15914(18) 0.0260(7) Uani 1 1 d D . . O3 O -0.1998(2) 0.4376(2) 0.27924(17) 0.0247(7) Uani 1 1 d D . . O4 O 0.3097(2) 0.2105(2) 0.34973(18) 0.0230(6) Uani 1 1 d D . . O5 O 0.0406(2) 0.4197(2) 0.19001(16) 0.0180(6) Uani 1 1 d . . . H5O H 0.0092 0.4741 0.1522 0.022 Uiso 1 1 calc R . . O6 O 0.2131(2) 0.2607(2) 0.20235(16) 0.0185(6) Uani 1 1 d . . . H6O H 0.2858 0.2189 0.1718 0.022 Uiso 1 1 calc R . . O7 O 0.1093(2) 0.3800(2) 0.32719(16) 0.0183(6) Uani 1 1 d . . . H7O H 0.1207 0.4095 0.3720 0.022 Uiso 1 1 calc R . . O8 O 0.0046(2) 0.2599(2) 0.29160(16) 0.0189(6) Uani 1 1 d . . . H8O H -0.0477 0.2175 0.3151 0.023 Uiso 1 1 calc R . . C1 C 0.1550(3) 0.6489(3) 0.1492(3) 0.0206(9) Uani 1 1 d . . . C2 C 0.2624(4) 0.6744(3) 0.1448(3) 0.0306(11) Uani 1 1 d . . . H2A H 0.2511 0.7105 0.1922 0.046 Uiso 1 1 calc R . . H2B H 0.2828 0.7160 0.0945 0.046 Uiso 1 1 calc R . . H2C H 0.3217 0.6131 0.1450 0.046 Uiso 1 1 calc R . . C3 C 0.0532(4) 0.7412(3) 0.1678(3) 0.0294(10) Uani 1 1 d . . . H3A H -0.0142 0.7223 0.1720 0.044 Uiso 1 1 calc R . . H3B H 0.0625 0.7935 0.1235 0.044 Uiso 1 1 calc R . . H3C H 0.0473 0.7659 0.2196 0.044 Uiso 1 1 calc R . . C4 C 0.1600(3) 0.6098(3) 0.0671(3) 0.0239(9) Uani 1 1 d . . . H4A H 0.0939 0.5855 0.0759 0.029 Uiso 1 1 calc R . . H4B H 0.1559 0.6663 0.0250 0.029 Uiso 1 1 calc R . . C5 C 0.2638(3) 0.5259(3) 0.0331(3) 0.0205(9) Uani 1 1 d . . . C6 C 0.3359(3) 0.5409(3) -0.0451(3) 0.0272(10) Uani 1 1 d . . . H6 H 0.3217 0.6028 -0.0762 0.033 Uiso 1 1 calc R . . C7 C 0.4284(4) 0.4636(4) -0.0761(3) 0.0306(11) Uani 1 1 d . . . H7 H 0.4778 0.4725 -0.1281 0.037 Uiso 1 1 calc R . . C8 C 0.4468(4) 0.3724(4) -0.0290(3) 0.0319(11) Uani 1 1 d . . . H8 H 0.5077 0.3183 -0.0492 0.038 Uiso 1 1 calc R . . C9 C 0.3731(3) 0.3628(3) 0.0489(3) 0.0267(10) Uani 1 1 d . . . H9 H 0.3868 0.3017 0.0809 0.032 Uiso 1 1 calc R . . C10 C 0.1653(4) 0.0609(3) 0.0841(3) 0.0335(11) Uani 1 1 d . . . C11 C 0.2178(5) -0.0489(4) 0.1127(3) 0.0517(16) Uani 1 1 d . . . H11A H 0.2750 -0.0504 0.1387 0.078 Uiso 1 1 calc R . . H11B H 0.2508 -0.0888 0.0652 0.078 Uiso 1 1 calc R . . H11C H 0.1604 -0.0763 0.1519 0.078 Uiso 1 1 calc R . . C12 C 0.0809(5) 0.0654(4) 0.0382(3) 0.0474(14) Uani 1 1 d . . . H12A H 0.0309 0.0250 0.0695 0.071 Uiso 1 1 calc R . . H12B H 0.1194 0.0397 -0.0157 0.071 Uiso 1 1 calc R . . H12C H 0.0381 0.1343 0.0312 0.071 Uiso 1 1 calc R . . C13 C 0.2598(4) 0.1093(3) 0.0327(3) 0.0310(11) Uani 1 1 d . . . H13A H 0.3017 0.1164 0.0697 0.037 Uiso 1 1 calc R . . H13B H 0.3113 0.0634 -0.0086 0.037 Uiso 1 1 calc R . . C14 C 0.2217(4) 0.2114(3) -0.0116(3) 0.0264(10) Uani 1 1 d . . . C15 C 0.2618(4) 0.2264(4) -0.0979(3) 0.0398(13) Uani 1 1 d . . . H15 H 0.3092 0.1725 -0.1288 0.048 Uiso 1 1 calc R . . C16 C 0.2313(4) 0.3212(4) -0.1375(3) 0.0408(13) Uani 1 1 d . . . H16 H 0.2567 0.3317 -0.1952 0.049 Uiso 1 1 calc R . . C17 C 0.1623(4) 0.3997(4) -0.0899(3) 0.0324(11) Uani 1 1 d . . . H17 H 0.1442 0.4654 -0.1141 0.039 Uiso 1 1 calc R . . C18 C 0.1209(3) 0.3788(3) -0.0056(3) 0.0247(10) Uani 1 1 d . . . H18 H 0.0700 0.4313 0.0255 0.030 Uiso 1 1 calc R . . C19 C -0.3810(4) 0.4118(5) 0.2888(3) 0.0524(16) Uani 1 1 d . . . H19A H -0.3891 0.4623 0.2434 0.079 Uiso 1 1 calc R . . H19B H -0.4541 0.4118 0.3257 0.079 Uiso 1 1 calc R . . H19C H -0.3451 0.3464 0.2673 0.079 Uiso 1 1 calc R . . C20 C -0.3093(3) 0.4353(4) 0.3364(3) 0.0288(10) Uani 1 1 d . . . C21 C -0.3615(4) 0.5383(4) 0.3709(3) 0.0415(13) Uani 1 1 d . . . H21A H -0.3077 0.5568 0.3902 0.062 Uiso 1 1 calc R . . H21B H -0.4269 0.5360 0.4166 0.062 Uiso 1 1 calc R . . H21C H -0.3830 0.5876 0.3278 0.062 Uiso 1 1 calc R . . C22 C -0.2907(4) 0.3510(4) 0.4064(3) 0.0293(10) Uani 1 1 d . . . H22A H -0.3625 0.3370 0.4358 0.035 Uiso 1 1 calc R . . H22B H -0.2409 0.2898 0.3809 0.035 Uiso 1 1 calc R . . C23 C -0.2417(3) 0.3746(3) 0.4685(3) 0.0242(10) Uani 1 1 d . . . C24 C -0.2991(4) 0.3771(4) 0.5527(3) 0.0334(11) Uani 1 1 d . . . H24 H -0.3699 0.3647 0.5709 0.040 Uiso 1 1 calc R . . C25 C -0.2528(4) 0.3976(4) 0.6096(3) 0.0377(12) Uani 1 1 d . . . H25 H -0.2917 0.3998 0.6659 0.045 Uiso 1 1 calc R . . C26 C -0.1469(4) 0.4148(3) 0.5812(3) 0.0309(11) Uani 1 1 d . . . H26 H -0.1123 0.4274 0.6182 0.037 Uiso 1 1 calc R . . C27 C -0.0945(4) 0.4130(3) 0.4976(3) 0.0248(10) Uani 1 1 d . . . H27 H -0.0240 0.4259 0.4786 0.030 Uiso 1 1 calc R . . C28 C 0.3274(4) 0.1962(3) 0.4329(3) 0.0269(10) Uani 1 1 d . . . C29 C 0.3562(4) 0.0829(4) 0.4552(3) 0.0372(12) Uani 1 1 d . . . H29A H 0.2995 0.0558 0.4480 0.056 Uiso 1 1 calc R . . H29B H 0.3592 0.0697 0.5123 0.056 Uiso 1 1 calc R . . H29C H 0.4281 0.0514 0.4193 0.056 Uiso 1 1 calc R . . C30 C 0.4245(4) 0.2390(4) 0.4293(3) 0.0409(13) Uani 1 1 d . . . H30A H 0.4896 0.2087 0.3867 0.061 Uiso 1 1 calc R . . H30B H 0.4417 0.2245 0.4823 0.061 Uiso 1 1 calc R . . H30C H 0.4035 0.3110 0.4168 0.061 Uiso 1 1 calc R . . C31 C 0.2199(4) 0.2522(3) 0.4944(3) 0.0265(10) Uani 1 1 d . . . H31A H 0.2379 0.2553 0.5457 0.032 Uiso 1 1 calc R . . H31B H 0.1969 0.3212 0.4710 0.032 Uiso 1 1 calc R . . C32 C 0.1214(3) 0.2074(3) 0.5159(3) 0.0227(9) Uani 1 1 d . . . C33 C 0.0708(4) 0.1821(3) 0.5985(3) 0.0306(11) Uani 1 1 d . . . H33 H 0.0974 0.1935 0.6408 0.037 Uiso 1 1 calc R . . C34 C -0.0190(4) 0.1401(4) 0.6181(3) 0.0366(12) Uani 1 1 d . . . H34 H -0.0541 0.1239 0.6735 0.044 Uiso 1 1 calc R . . C35 C -0.0562(4) 0.1223(3) 0.5544(3) 0.0334(11) Uani 1 1 d . . . H35 H -0.1163 0.0937 0.5657 0.040 Uiso 1 1 calc R . . C36 C -0.0016(4) 0.1480(3) 0.4740(3) 0.0265(10) Uani 1 1 d . . . H36 H -0.0254 0.1351 0.4308 0.032 Uiso 1 1 calc R . . C37 C 0.5574(4) 0.1463(5) 0.1848(4) 0.0549(16) Uani 1 1 d . . . H37A H 0.5014 0.2061 0.2083 0.066 Uiso 1 1 calc R . . H37B H 0.5858 0.1043 0.2296 0.066 Uiso 1 1 calc R . . C38 C 0.4431(5) 0.8550(6) 0.3180(5) 0.081(2) Uani 1 1 d . . . H38A H 0.4057 0.9241 0.3024 0.097 Uiso 1 1 calc R . . H38B H 0.4000 0.8359 0.3732 0.097 Uiso 1 1 calc R . . C39 C 0.8576(5) 0.0587(5) 0.2482(4) 0.0666(19) Uani 1 1 d . . . H39A H 0.9360 0.0391 0.2491 0.080 Uiso 1 1 calc R . . H39B H 0.8467 0.1175 0.2089 0.080 Uiso 1 1 calc R . . Cl5 Cl 0.49439(14) 0.07881(14) 0.14159(13) 0.0773(5) Uani 1 1 d . . . Cl6 Cl 0.66826(15) 0.18262(13) 0.10891(13) 0.0806(6) Uani 1 1 d . . . Cl7 Cl 0.44533(16) 0.77314(16) 0.24515(14) 0.0862(6) Uani 1 1 d . . . Cl8 Cl 0.57660(16) 0.84922(17) 0.32117(13) 0.0902(7) Uani 1 1 d . . . Cl9 Cl 0.82819(15) -0.04068(12) 0.21433(11) 0.0678(5) Uani 1 1 d . . . Cl10 Cl 0.7734(2) 0.09071(14) 0.34631(13) 0.1065(8) Uani 1 1 d . . . H2O H 0.127(5) 0.086(5) 0.205(2) 0.100 Uiso 1 1 d D . . H1O H 0.072(3) 0.581(5) 0.254(3) 0.100 Uiso 1 1 d D . . H3O H -0.187(6) 0.387(4) 0.247(4) 0.100 Uiso 1 1 d D . . H4O H 0.325(6) 0.269(3) 0.324(4) 0.100 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0166(3) 0.0181(3) 0.0172(3) -0.0007(2) -0.0029(2) -0.0060(2) Ni2 0.0221(3) 0.0208(3) 0.0168(3) -0.0015(2) -0.0051(2) -0.0084(2) Ni3 0.0163(3) 0.0220(3) 0.0169(3) -0.0024(2) -0.0026(2) -0.0058(2) Ni4 0.0199(3) 0.0193(3) 0.0163(3) 0.0001(2) -0.0037(2) -0.0069(2) Cl1 0.0223(5) 0.0302(6) 0.0299(6) 0.0022(5) -0.0094(4) -0.0110(4) Cl2 0.0281(6) 0.0367(6) 0.0274(6) -0.0015(5) -0.0124(5) -0.0121(5) Cl4 0.0358(6) 0.0210(5) 0.0255(6) -0.0003(4) -0.0075(5) -0.0070(5) Cl3 0.0246(5) 0.0240(6) 0.0320(6) -0.0068(5) 0.0009(5) -0.0060(4) N1 0.0194(17) 0.0229(19) 0.0197(18) -0.0024(15) -0.0031(14) -0.0077(15) N2 0.0246(18) 0.0244(19) 0.0200(19) -0.0024(16) -0.0069(15) -0.0085(15) N3 0.0198(17) 0.0232(19) 0.0182(18) -0.0027(15) -0.0020(14) -0.0058(15) N4 0.0241(18) 0.0205(18) 0.0204(19) 0.0006(15) -0.0034(15) -0.0070(15) O1 0.0214(14) 0.0173(14) 0.0200(15) -0.0004(12) -0.0030(12) -0.0055(12) O2 0.0353(17) 0.0235(16) 0.0217(16) -0.0022(13) -0.0066(14) -0.0122(14) O3 0.0178(14) 0.0353(18) 0.0203(16) -0.0005(13) -0.0035(12) -0.0087(13) O4 0.0211(14) 0.0264(16) 0.0212(16) 0.0000(13) -0.0054(12) -0.0071(13) O5 0.0186(14) 0.0198(14) 0.0156(14) -0.0008(12) -0.0033(11) -0.0065(11) O6 0.0216(14) 0.0187(14) 0.0151(14) -0.0012(12) -0.0032(11) -0.0070(12) O7 0.0198(14) 0.0199(14) 0.0145(14) -0.0026(12) -0.0031(11) -0.0051(12) O8 0.0211(14) 0.0199(14) 0.0165(14) 0.0013(12) -0.0051(11) -0.0080(12) C1 0.023(2) 0.016(2) 0.023(2) -0.0008(17) -0.0053(18) -0.0071(17) C2 0.033(2) 0.030(3) 0.033(3) 0.000(2) -0.009(2) -0.015(2) C3 0.030(2) 0.020(2) 0.035(3) 0.002(2) -0.008(2) -0.0051(19) C4 0.026(2) 0.024(2) 0.022(2) 0.0024(18) -0.0085(18) -0.0075(19) C5 0.019(2) 0.025(2) 0.020(2) -0.0005(18) -0.0076(17) -0.0071(17) C6 0.025(2) 0.030(2) 0.025(2) 0.007(2) -0.0087(19) -0.0081(19) C7 0.027(2) 0.040(3) 0.022(2) 0.006(2) -0.0032(19) -0.013(2) C8 0.022(2) 0.038(3) 0.030(3) -0.009(2) 0.003(2) -0.007(2) C9 0.023(2) 0.023(2) 0.031(3) -0.005(2) -0.0032(19) -0.0046(18) C10 0.051(3) 0.027(2) 0.024(2) -0.009(2) -0.005(2) -0.014(2) C11 0.087(4) 0.023(3) 0.038(3) -0.009(2) -0.003(3) -0.014(3) C12 0.062(4) 0.058(4) 0.037(3) -0.011(3) -0.013(3) -0.033(3) C13 0.033(3) 0.026(2) 0.032(3) -0.011(2) -0.004(2) -0.006(2) C14 0.025(2) 0.031(2) 0.025(2) -0.008(2) -0.0011(19) -0.0117(19) C15 0.045(3) 0.043(3) 0.026(3) -0.007(2) 0.002(2) -0.013(2) C16 0.044(3) 0.058(4) 0.016(2) 0.002(2) 0.001(2) -0.019(3) C17 0.030(2) 0.040(3) 0.030(3) 0.010(2) -0.011(2) -0.017(2) C18 0.025(2) 0.030(2) 0.022(2) -0.0012(19) -0.0099(18) -0.0076(19) C19 0.029(3) 0.100(5) 0.039(3) 0.004(3) -0.014(2) -0.033(3) C20 0.017(2) 0.047(3) 0.022(2) 0.006(2) -0.0031(18) -0.014(2) C21 0.022(2) 0.045(3) 0.042(3) 0.003(2) -0.001(2) 0.003(2) C22 0.020(2) 0.042(3) 0.029(3) 0.002(2) -0.0064(19) -0.016(2) C23 0.024(2) 0.024(2) 0.023(2) 0.0021(19) -0.0045(18) -0.0069(18) C24 0.023(2) 0.046(3) 0.023(2) 0.000(2) 0.0012(19) -0.007(2) C25 0.041(3) 0.045(3) 0.015(2) -0.002(2) 0.000(2) -0.002(2) C26 0.039(3) 0.032(3) 0.023(2) -0.004(2) -0.015(2) -0.005(2) C27 0.028(2) 0.027(2) 0.020(2) -0.0015(19) -0.0078(18) -0.0068(19) C28 0.028(2) 0.030(2) 0.024(2) 0.0013(19) -0.0098(19) -0.009(2) C29 0.033(3) 0.041(3) 0.030(3) 0.004(2) -0.009(2) -0.001(2) C30 0.033(3) 0.068(4) 0.029(3) 0.001(3) -0.014(2) -0.021(3) C31 0.031(2) 0.030(2) 0.022(2) -0.0020(19) -0.0130(19) -0.009(2) C32 0.028(2) 0.020(2) 0.018(2) -0.0016(17) -0.0051(18) -0.0048(18) C33 0.035(3) 0.032(3) 0.022(2) -0.003(2) -0.005(2) -0.006(2) C34 0.048(3) 0.035(3) 0.019(2) 0.003(2) 0.006(2) -0.017(2) C35 0.033(3) 0.029(3) 0.033(3) 0.003(2) -0.001(2) -0.012(2) C36 0.031(2) 0.023(2) 0.024(2) 0.0004(19) -0.0024(19) -0.0106(19) C37 0.042(3) 0.066(4) 0.050(4) -0.018(3) -0.011(3) 0.002(3) C38 0.051(4) 0.078(5) 0.094(6) -0.023(4) -0.001(4) 0.000(4) C39 0.056(4) 0.064(4) 0.079(5) 0.006(4) -0.011(3) -0.027(3) Cl5 0.0541(9) 0.0682(11) 0.1166(16) -0.0226(11) -0.0324(10) -0.0090(8) Cl6 0.0716(11) 0.0569(10) 0.1059(15) 0.0097(10) -0.0150(10) -0.0233(9) Cl7 0.0743(12) 0.0893(14) 0.1026(15) -0.0047(12) -0.0338(11) -0.0244(11) Cl8 0.0694(11) 0.1157(16) 0.0796(13) -0.0387(12) -0.0266(10) 0.0069(11) Cl9 0.0845(12) 0.0427(8) 0.0703(11) -0.0042(8) -0.0253(9) -0.0036(8) Cl10 0.164(2) 0.0526(11) 0.0814(14) -0.0188(10) 0.0016(14) -0.0259(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 O5 2.062(3) . ? Ni1 O6 2.070(3) . ? Ni1 N1 2.081(3) . ? Ni1 O7 2.082(3) . ? Ni1 O1 2.110(3) . ? Ni1 Cl1 2.4128(12) . ? Ni2 O5 2.055(3) . ? Ni2 O8 2.074(3) . ? Ni2 O6 2.086(3) . ? Ni2 O2 2.097(3) . ? Ni2 N2 2.100(3) . ? Ni2 Cl2 2.4082(12) . ? Ni3 O7 2.055(3) . ? Ni3 O8 2.081(3) . ? Ni3 O5 2.082(3) . ? Ni3 O3 2.090(3) . ? Ni3 N3 2.100(3) . ? Ni3 Cl3 2.4068(11) . ? Ni4 O6 2.055(3) . ? Ni4 O8 2.074(3) . ? Ni4 O7 2.080(3) . ? Ni4 N4 2.080(3) . ? Ni4 O4 2.120(3) . ? Ni4 Cl4 2.4178(11) . ? N1 C5 1.345(5) . ? N1 C9 1.348(5) . ? N2 C18 1.343(5) . ? N2 C14 1.350(5) . ? N3 C27 1.350(5) . ? N3 C23 1.355(5) . ? N4 C36 1.342(5) . ? N4 C32 1.343(5) . ? O1 C1 1.454(5) . ? O1 H1O 0.90(5) . ? O2 C10 1.464(5) . ? O2 H2O 0.90(5) . ? O3 C20 1.457(5) . ? O3 H3O 0.90(6) . ? O4 C28 1.460(5) . ? O4 H4O 0.90(5) . ? O5 H5O 0.9800 . ? O6 H6O 0.9800 . ? O7 H7O 0.9800 . ? O8 H8O 0.9800 . ? C1 C2 1.507(6) . ? C1 C3 1.530(5) . ? C1 C4 1.542(6) . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 C5 1.515(5) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.391(6) . ? C6 C7 1.374(6) . ? C6 H6 0.9300 . ? C7 C8 1.379(7) . ? C7 H7 0.9300 . ? C8 C9 1.381(6) . ? C8 H8 0.9300 . ? C9 H9 0.9300 . ? C10 C12 1.497(7) . ? C10 C13 1.534(6) . ? C10 C11 1.536(7) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 C14 1.509(6) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.392(6) . ? C15 C16 1.378(7) . ? C15 H15 0.9300 . ? C16 C17 1.376(6) . ? C16 H16 0.9300 . ? C17 C18 1.374(6) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 C20 1.521(7) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 C21 1.513(6) . ? C20 C22 1.542(6) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 C23 1.493(6) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.389(6) . ? C24 C25 1.374(7) . ? C24 H24 0.9300 . ? C25 C26 1.384(7) . ? C25 H25 0.9300 . ? C26 C27 1.368(6) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C28 C29 1.515(6) . ? C28 C30 1.521(6) . ? C28 C31 1.532(6) . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 C32 1.501(6) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 C33 1.385(6) . ? C33 C34 1.379(7) . ? C33 H33 0.9300 . ? C34 C35 1.380(7) . ? C34 H34 0.9300 . ? C35 C36 1.370(6) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? C37 Cl6 1.748(6) . ? C37 Cl5 1.759(6) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 Cl8 1.717(7) . ? C38 Cl7 1.788(7) . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C39 Cl10 1.723(6) . ? C39 Cl9 1.750(6) . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? 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 O5 Ni1 O6 80.13(11) . . ? O5 Ni1 N1 99.90(12) . . ? O6 Ni1 N1 97.00(11) . . ? O5 Ni1 O7 79.11(11) . . ? O6 Ni1 O7 79.44(10) . . ? N1 Ni1 O7 176.41(11) . . ? O5 Ni1 O1 89.06(11) . . ? O6 Ni1 O1 167.75(10) . . ? N1 Ni1 O1 90.48(12) . . ? O7 Ni1 O1 92.95(10) . . ? O5 Ni1 Cl1 170.97(8) . . ? O6 Ni1 Cl1 97.52(8) . . ? N1 Ni1 Cl1 89.02(10) . . ? O7 Ni1 Cl1 91.90(8) . . ? O1 Ni1 Cl1 92.27(8) . . ? O5 Ni2 O8 79.57(10) . . ? O5 Ni2 O6 79.92(10) . . ? O8 Ni2 O6 79.48(10) . . ? O5 Ni2 O2 168.94(11) . . ? O8 Ni2 O2 90.57(11) . . ? O6 Ni2 O2 93.44(11) . . ? O5 Ni2 N2 98.89(12) . . ? O8 Ni2 N2 175.44(12) . . ? O6 Ni2 N2 96.04(12) . . ? O2 Ni2 N2 90.56(12) . . ? O5 Ni2 Cl2 94.27(8) . . ? O8 Ni2 Cl2 93.16(8) . . ? O6 Ni2 Cl2 171.31(7) . . ? O2 Ni2 Cl2 91.25(9) . . ? N2 Ni2 Cl2 91.23(10) . . ? O7 Ni3 O8 80.21(10) . . ? O7 Ni3 O5 79.28(10) . . ? O8 Ni3 O5 78.81(10) . . ? O7 Ni3 O3 169.26(10) . . ? O8 Ni3 O3 94.45(11) . . ? O5 Ni3 O3 90.58(11) . . ? O7 Ni3 N3 99.31(12) . . ? O8 Ni3 N3 97.04(12) . . ? O5 Ni3 N3 175.78(12) . . ? O3 Ni3 N3 90.56(12) . . ? O7 Ni3 Cl3 94.65(8) . . ? O8 Ni3 Cl3 172.34(8) . . ? O5 Ni3 Cl3 94.72(8) . . ? O3 Ni3 Cl3 89.67(9) . . ? N3 Ni3 Cl3 89.35(10) . . ? O6 Ni4 O8 80.19(11) . . ? O6 Ni4 O7 79.83(10) . . ? O8 Ni4 O7 79.79(11) . . ? O6 Ni4 N4 177.04(12) . . ? O8 Ni4 N4 97.46(12) . . ? O7 Ni4 N4 98.03(12) . . ? O6 Ni4 O4 91.83(11) . . ? O8 Ni4 O4 169.03(11) . . ? O7 Ni4 O4 91.46(11) . . ? N4 Ni4 O4 90.26(13) . . ? O6 Ni4 Cl4 92.17(8) . . ? O8 Ni4 Cl4 95.35(8) . . ? O7 Ni4 Cl4 171.21(8) . . ? N4 Ni4 Cl4 89.83(10) . . ? O4 Ni4 Cl4 92.44(8) . . ? C5 N1 C9 117.7(3) . . ? C5 N1 Ni1 125.6(3) . . ? C9 N1 Ni1 116.3(3) . . ? C18 N2 C14 117.3(4) . . ? C18 N2 Ni2 117.1(3) . . ? C14 N2 Ni2 125.5(3) . . ? C27 N3 C23 118.0(4) . . ? C27 N3 Ni3 116.5(3) . . ? C23 N3 Ni3 125.1(3) . . ? C36 N4 C32 118.6(4) . . ? C36 N4 Ni4 116.3(3) . . ? C32 N4 Ni4 125.1(3) . . ? C1 O1 Ni1 125.3(2) . . ? C1 O1 H1O 117(5) . . ? Ni1 O1 H1O 105(4) . . ? C10 O2 Ni2 124.6(3) . . ? C10 O2 H2O 114(4) . . ? Ni2 O2 H2O 107(4) . . ? C20 O3 Ni3 124.9(3) . . ? C20 O3 H3O 102(4) . . ? Ni3 O3 H3O 105(5) . . ? C28 O4 Ni4 123.7(2) . . ? C28 O4 H4O 109(5) . . ? Ni4 O4 H4O 102(5) . . ? Ni2 O5 Ni1 99.50(11) . . ? Ni2 O5 Ni3 100.31(12) . . ? Ni1 O5 Ni3 99.83(12) . . ? Ni2 O5 H5O 117.9 . . ? Ni1 O5 H5O 117.9 . . ? Ni3 O5 H5O 117.9 . . ? Ni4 O6 Ni1 100.20(11) . . ? Ni4 O6 Ni2 99.49(11) . . ? Ni1 O6 Ni2 98.26(11) . . ? Ni4 O6 H6O 118.3 . . ? Ni1 O6 H6O 118.3 . . ? Ni2 O6 H6O 118.3 . . ? Ni3 O7 Ni4 99.33(11) . . ? Ni3 O7 Ni1 100.06(12) . . ? Ni4 O7 Ni1 99.00(10) . . ? Ni3 O7 H7O 118.2 . . ? Ni4 O7 H7O 118.2 . . ? Ni1 O7 H7O 118.2 . . ? Ni2 O8 Ni4 99.28(11) . . ? Ni2 O8 Ni3 99.73(12) . . ? Ni4 O8 Ni3 98.70(11) . . ? Ni2 O8 H8O 118.4 . . ? Ni4 O8 H8O 118.4 . . ? Ni3 O8 H8O 118.4 . . ? O1 C1 C2 106.7(3) . . ? O1 C1 C3 108.9(3) . . ? C2 C1 C3 111.3(3) . . ? O1 C1 C4 109.9(3) . . ? C2 C1 C4 111.9(3) . . ? C3 C1 C4 108.0(4) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C5 C4 C1 115.5(4) . . ? C5 C4 H4A 108.4 . . ? C1 C4 H4A 108.4 . . ? C5 C4 H4B 108.4 . . ? C1 C4 H4B 108.4 . . ? H4A C4 H4B 107.5 . . ? N1 C5 C6 122.1(4) . . ? N1 C5 C4 118.0(3) . . ? C6 C5 C4 119.9(4) . . ? C7 C6 C5 119.4(4) . . ? C7 C6 H6 120.3 . . ? C5 C6 H6 120.3 . . ? C6 C7 C8 119.0(4) . . ? C6 C7 H7 120.5 . . ? C8 C7 H7 120.5 . . ? C7 C8 C9 118.8(4) . . ? C7 C8 H8 120.6 . . ? C9 C8 H8 120.6 . . ? N1 C9 C8 123.0(4) . . ? N1 C9 H9 118.5 . . ? C8 C9 H9 118.5 . . ? O2 C10 C12 107.4(4) . . ? O2 C10 C13 108.6(3) . . ? C12 C10 C13 113.2(4) . . ? O2 C10 C11 107.5(4) . . ? C12 C10 C11 111.0(4) . . ? C13 C10 C11 109.0(4) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 C10 115.4(4) . . ? C14 C13 H13A 108.4 . . ? C10 C13 H13A 108.4 . . ? C14 C13 H13B 108.4 . . ? C10 C13 H13B 108.4 . . ? H13A C13 H13B 107.5 . . ? N2 C14 C15 121.3(4) . . ? N2 C14 C13 118.3(4) . . ? C15 C14 C13 120.3(4) . . ? C16 C15 C14 120.1(4) . . ? C16 C15 H15 120.0 . . ? C14 C15 H15 120.0 . . ? C17 C16 C15 118.6(4) . . ? C17 C16 H16 120.7 . . ? C15 C16 H16 120.7 . . ? C18 C17 C16 118.5(5) . . ? C18 C17 H17 120.8 . . ? C16 C17 H17 120.8 . . ? N2 C18 C17 124.1(4) . . ? N2 C18 H18 118.0 . . ? C17 C18 H18 118.0 . . ? C20 C19 H19A 109.5 . . ? C20 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C20 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? O3 C20 C21 106.9(4) . . ? O3 C20 C19 108.9(4) . . ? C21 C20 C19 111.6(4) . . ? O3 C20 C22 108.3(3) . . ? C21 C20 C22 111.4(4) . . ? C19 C20 C22 109.6(4) . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C23 C22 C20 115.0(4) . . ? C23 C22 H22A 108.5 . . ? C20 C22 H22A 108.5 . . ? C23 C22 H22B 108.5 . . ? C20 C22 H22B 108.5 . . ? H22A C22 H22B 107.5 . . ? N3 C23 C24 120.3(4) . . ? N3 C23 C22 118.3(4) . . ? C24 C23 C22 121.3(4) . . ? C25 C24 C23 120.9(4) . . ? C25 C24 H24 119.6 . . ? C23 C24 H24 119.6 . . ? C24 C25 C26 118.5(4) . . ? C24 C25 H25 120.7 . . ? C26 C25 H25 120.7 . . ? C27 C26 C25 118.4(4) . . ? C27 C26 H26 120.8 . . ? C25 C26 H26 120.8 . . ? N3 C27 C26 123.8(4) . . ? N3 C27 H27 118.1 . . ? C26 C27 H27 118.1 . . ? O4 C28 C29 106.1(4) . . ? O4 C28 C30 108.6(4) . . ? C29 C28 C30 111.0(4) . . ? O4 C28 C31 109.3(3) . . ? C29 C28 C31 111.9(4) . . ? C30 C28 C31 109.8(4) . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C32 C31 C28 116.2(3) . . ? C32 C31 H31A 108.2 . . ? C28 C31 H31A 108.2 . . ? C32 C31 H31B 108.2 . . ? C28 C31 H31B 108.2 . . ? H31A C31 H31B 107.4 . . ? N4 C32 C33 120.7(4) . . ? N4 C32 C31 119.1(4) . . ? C33 C32 C31 120.2(4) . . ? C34 C33 C32 120.0(4) . . ? C34 C33 H33 120.0 . . ? C32 C33 H33 120.0 . . ? C33 C34 C35 119.2(4) . . ? C33 C34 H34 120.4 . . ? C35 C34 H34 120.4 . . ? C36 C35 C34 117.8(4) . . ? C36 C35 H35 121.1 . . ? C34 C35 H35 121.1 . . ? N4 C36 C35 123.7(4) . . ? N4 C36 H36 118.2 . . ? C35 C36 H36 118.2 . . ? Cl6 C37 Cl5 110.8(3) . . ? Cl6 C37 H37A 109.5 . . ? Cl5 C37 H37A 109.5 . . ? Cl6 C37 H37B 109.5 . . ? Cl5 C37 H37B 109.5 . . ? H37A C37 H37B 108.1 . . ? Cl8 C38 Cl7 111.7(3) . . ? Cl8 C38 H38A 109.3 . . ? Cl7 C38 H38A 109.3 . . ? Cl8 C38 H38B 109.3 . . ? Cl7 C38 H38B 109.3 . . ? H38A C38 H38B 107.9 . . ? Cl10 C39 Cl9 112.4(3) . . ? Cl10 C39 H39A 109.1 . . ? Cl9 C39 H39A 109.1 . . ? Cl10 C39 H39B 109.1 . . ? Cl9 C39 H39B 109.1 . . ? H39A C39 H39B 107.9 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.832 _refine_diff_density_min -1.133 _refine_diff_density_rms 0.252