# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _publ_contact_author_name 'Prof T. S. Andy Hor' _publ_contact_author_address ; Prof T. S. Andy Hor Department of Chemistry National University of Singapore 3 Science Drive 3 117543 Singapore ; loop_ _publ_author_name W.-H.Zhang 'Norlela Binte Sulaiman' P.X.S.Tio T.S.A.Hor data_[Ni(hmpH)2(H2O)2]Br2 _database_code_depnum_ccdc_archive 'CCDC 798244' #TrackingRef 'CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H18 Br2 N2 Ni O4' _chemical_formula_weight 472.81 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 20.5097(16) _cell_length_b 7.9119(6) _cell_length_c 12.3903(10) _cell_angle_alpha 90.00 _cell_angle_beta 123.3340(10) _cell_angle_gamma 90.00 _cell_volume 1679.8(2) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 2205 _cell_measurement_theta_min 2.84 _cell_measurement_theta_max 27.38 _exptl_crystal_description BLOCK _exptl_crystal_colour GREEN _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'Not Measured' _exptl_crystal_density_diffrn 1.870 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 936 _exptl_absorpt_coefficient_mu 5.927 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.1713 _exptl_absorpt_correction_T_max 0.5887 _exptl_absorpt_process_details 'Sadabs, (Sheldrick 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5721 _diffrn_reflns_av_R_equivalents 0.0289 _diffrn_reflns_av_sigmaI/netI 0.0327 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.38 _diffrn_reflns_theta_max 27.49 _reflns_number_total 1929 _reflns_number_gt 1742 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0557P)^2^+1.3419P] 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 1929 _refine_ls_number_parameters 105 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0427 _refine_ls_R_factor_gt 0.0357 _refine_ls_wR_factor_ref 0.1132 _refine_ls_wR_factor_gt 0.0898 _refine_ls_goodness_of_fit_ref 1.227 _refine_ls_restrained_S_all 1.227 _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 0.17487(7) 0.2500 0.02101(19) Uani 1 2 d S . . Br1 Br 0.58708(2) 0.69285(5) 0.18410(4) 0.03150(17) Uani 1 1 d . . . O1 O 0.47042(15) 0.0022(3) 0.1059(3) 0.0307(6) Uani 1 1 d D . . H1O H 0.500(2) -0.076(4) 0.124(4) 0.037 Uiso 1 1 d D . . N1 N 0.38297(17) 0.1385(4) 0.1757(3) 0.0266(7) Uani 1 1 d . . . C1 C 0.3442(2) 0.2125(5) 0.2218(5) 0.0361(9) Uani 1 1 d . . . H1 H 0.3705 0.2915 0.2891 0.043 Uiso 1 1 calc R . . C2 C 0.2673(3) 0.1765(6) 0.1737(6) 0.0469(12) Uani 1 1 d . . . H2 H 0.2419 0.2285 0.2090 0.056 Uiso 1 1 calc R . . C3 C 0.2280(2) 0.0632(7) 0.0732(6) 0.0536(14) Uani 1 1 d . . . H3 H 0.1752 0.0379 0.0377 0.064 Uiso 1 1 calc R . . C4 C 0.2681(2) -0.0120(6) 0.0260(5) 0.0450(11) Uani 1 1 d . . . H4 H 0.2426 -0.0890 -0.0430 0.054 Uiso 1 1 calc R . . C5 C 0.3466(2) 0.0263(5) 0.0808(4) 0.0320(9) Uani 1 1 d . . . C6 C 0.3920(2) -0.0561(6) 0.0345(4) 0.0393(10) Uani 1 1 d . . . H6A H 0.3912 -0.1789 0.0440 0.047 Uiso 1 1 calc R . . H6B H 0.3678 -0.0308 -0.0573 0.047 Uiso 1 1 calc R . . O2 O 0.47664(17) 0.3636(4) 0.1198(3) 0.0331(6) Uani 1 1 d D . . H1W H 0.444(2) 0.338(6) 0.042(2) 0.040 Uiso 1 1 d D . . H2W H 0.511(2) 0.434(4) 0.147(4) 0.040 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 0.0164(3) 0.0244(3) 0.0198(3) 0.000 0.0084(3) 0.000 Br1 0.0300(3) 0.0305(2) 0.0314(3) -0.00200(15) 0.0152(2) -0.00103(14) O1 0.0278(15) 0.0305(14) 0.0297(15) -0.0052(12) 0.0133(13) 0.0002(11) N1 0.0177(15) 0.0302(15) 0.0275(17) 0.0083(14) 0.0097(13) 0.0018(12) C1 0.027(2) 0.042(2) 0.041(2) 0.0117(19) 0.020(2) 0.0071(17) C2 0.034(2) 0.055(3) 0.059(3) 0.022(3) 0.030(3) 0.010(2) C3 0.019(2) 0.061(3) 0.071(3) 0.036(3) 0.018(2) 0.009(2) C4 0.025(2) 0.042(2) 0.042(3) 0.014(2) 0.0023(19) -0.0065(18) C5 0.0208(19) 0.034(2) 0.028(2) 0.0092(17) 0.0046(16) -0.0015(15) C6 0.030(2) 0.044(2) 0.029(2) -0.0084(19) 0.0069(18) -0.0069(19) O2 0.0370(17) 0.0328(14) 0.0236(14) 0.0003(12) 0.0129(14) -0.0103(12) _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 2.052(3) 2_655 ? Ni1 O2 2.052(3) . ? Ni1 O1 2.057(3) . ? Ni1 O1 2.057(3) 2_655 ? Ni1 N1 2.065(3) . ? Ni1 N1 2.065(3) 2_655 ? O1 C6 1.421(5) . ? O1 H1O 0.803(19) . ? N1 C5 1.327(5) . ? N1 C1 1.341(5) . ? C1 C2 1.375(6) . ? C1 H1 0.9400 . ? C2 C3 1.379(7) . ? C2 H2 0.9400 . ? C3 C4 1.379(7) . ? C3 H3 0.9400 . ? C4 C5 1.393(5) . ? C4 H4 0.9400 . ? C5 C6 1.486(6) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? O2 H1W 0.843(19) . ? O2 H2W 0.816(19) . ? 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 O2 86.64(17) 2_655 . ? O2 Ni1 O1 174.57(11) 2_655 . ? O2 Ni1 O1 88.33(12) . . ? O2 Ni1 O1 88.33(12) 2_655 2_655 ? O2 Ni1 O1 174.57(11) . 2_655 ? O1 Ni1 O1 96.76(16) . 2_655 ? O2 Ni1 N1 99.45(13) 2_655 . ? O2 Ni1 N1 92.22(12) . . ? O1 Ni1 N1 78.70(12) . . ? O1 Ni1 N1 90.61(11) 2_655 . ? O2 Ni1 N1 92.22(12) 2_655 2_655 ? O2 Ni1 N1 99.45(13) . 2_655 ? O1 Ni1 N1 90.61(11) . 2_655 ? O1 Ni1 N1 78.70(12) 2_655 2_655 ? N1 Ni1 N1 163.96(18) . 2_655 ? C6 O1 Ni1 116.7(2) . . ? C6 O1 H1O 110(3) . . ? Ni1 O1 H1O 117(3) . . ? C5 N1 C1 119.5(3) . . ? C5 N1 Ni1 116.0(3) . . ? C1 N1 Ni1 124.4(3) . . ? N1 C1 C2 122.1(5) . . ? N1 C1 H1 118.9 . . ? C2 C1 H1 118.9 . . ? C3 C2 C1 119.2(5) . . ? C3 C2 H2 120.4 . . ? C1 C2 H2 120.4 . . ? C2 C3 C4 118.3(4) . . ? C2 C3 H3 120.9 . . ? C4 C3 H3 120.9 . . ? C3 C4 C5 119.9(5) . . ? C3 C4 H4 120.1 . . ? C5 C4 H4 120.1 . . ? N1 C5 C4 120.9(4) . . ? N1 C5 C6 117.9(3) . . ? C4 C5 C6 121.1(4) . . ? O1 C6 C5 110.6(3) . . ? O1 C6 H6A 109.5 . . ? C5 C6 H6A 109.5 . . ? O1 C6 H6B 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 108.1 . . ? Ni1 O2 H1W 115(3) . . ? Ni1 O2 H2W 114(3) . . ? H1W O2 H2W 126(5) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O2 H2W Br1 0.816(19) 2.46(2) 3.251(3) 165(4) . O2 H1W Br1 0.843(19) 2.51(3) 3.268(3) 149(4) 5_665 O1 H1O Br1 0.803(19) 2.376(19) 3.179(3) 178(4) 1_545 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.690 _refine_diff_density_min -0.671 _refine_diff_density_rms 0.199 data_Ni4(hmp)4(OAc)4 _database_code_depnum_ccdc_archive 'CCDC 798245' #TrackingRef 'CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H36 N4 Ni4 O12' _chemical_formula_weight 903.49 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 17.2034(8) _cell_length_b 12.6231(7) _cell_length_c 16.8913(9) _cell_angle_alpha 90.00 _cell_angle_beta 105.2340(10) _cell_angle_gamma 90.00 _cell_volume 3539.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5210 _cell_measurement_theta_min 2.50 _cell_measurement_theta_max 27.52 _exptl_crystal_description Block _exptl_crystal_colour Green _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas 'Not Measured' _exptl_crystal_density_diffrn 1.696 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1856 _exptl_absorpt_coefficient_mu 2.163 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6716 _exptl_absorpt_correction_T_max 0.7235 _exptl_absorpt_process_details 'Sadabs, (Sheldrick 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12360 _diffrn_reflns_av_R_equivalents 0.0281 _diffrn_reflns_av_sigmaI/netI 0.0310 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 27.50 _reflns_number_total 4067 _reflns_number_gt 3617 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0494P)^2^+1.6260P] 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 4067 _refine_ls_number_parameters 237 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0362 _refine_ls_R_factor_gt 0.0314 _refine_ls_wR_factor_ref 0.0827 _refine_ls_wR_factor_gt 0.0803 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.060 _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 0.518967(15) 0.72917(2) 0.349036(15) 0.01496(9) Uani 1 1 d . . . Ni2 Ni 0.403826(14) 0.58368(2) 0.241909(15) 0.01508(9) Uani 1 1 d . . . O1 O 0.57586(9) 0.74089(11) 0.25879(8) 0.0157(3) Uani 1 1 d . . . O2 O 0.51020(8) 0.57093(11) 0.32744(8) 0.0157(3) Uani 1 1 d . . . O3 O 0.43889(9) 0.72468(12) 0.41771(9) 0.0195(3) Uani 1 1 d . . . O4 O 0.34432(8) 0.62187(12) 0.33354(9) 0.0196(3) Uani 1 1 d . . . O5 O 0.62512(9) 0.69179(12) 0.43636(8) 0.0205(3) Uani 1 1 d . . . O6 O 0.68597(9) 0.58625(12) 0.36207(9) 0.0219(3) Uani 1 1 d . . . N1 N 0.54563(10) 0.88763(14) 0.35793(10) 0.0179(3) Uani 1 1 d . . . N2 N 0.39670(10) 0.42887(14) 0.27318(10) 0.0177(4) Uani 1 1 d . . . C1 C 0.51751(13) 0.96233(18) 0.39978(13) 0.0223(4) Uani 1 1 d . . . H1 H 0.4801 0.9424 0.4296 0.027 Uiso 1 1 calc R . . C2 C 0.54105(15) 1.06726(18) 0.40102(14) 0.0278(5) Uani 1 1 d . . . H2 H 0.5206 1.1185 0.4315 0.033 Uiso 1 1 calc R . . C3 C 0.59503(15) 1.09597(18) 0.35689(15) 0.0281(5) Uani 1 1 d . . . H3 H 0.6116 1.1677 0.3559 0.034 Uiso 1 1 calc R . . C4 C 0.62463(14) 1.01926(19) 0.31421(13) 0.0249(5) Uani 1 1 d . . . H4 H 0.6619 1.0375 0.2837 0.030 Uiso 1 1 calc R . . C5 C 0.59925(12) 0.91502(17) 0.31646(12) 0.0185(4) Uani 1 1 d . . . C6 C 0.63055(12) 0.82548(17) 0.27398(12) 0.0184(4) Uani 1 1 d . . . H6A H 0.6390 0.8512 0.2215 0.022 Uiso 1 1 calc R . . H6B H 0.6831 0.8009 0.3089 0.022 Uiso 1 1 calc R . . C7 C 0.33887(12) 0.35881(17) 0.23796(13) 0.0206(4) Uani 1 1 d . . . H7 H 0.3051 0.3739 0.1849 0.025 Uiso 1 1 calc R . . C8 C 0.32695(13) 0.26592(18) 0.27626(14) 0.0231(5) Uani 1 1 d . . . H8 H 0.2863 0.2172 0.2498 0.028 Uiso 1 1 calc R . . C9 C 0.37537(14) 0.24533(18) 0.35393(15) 0.0262(5) Uani 1 1 d . . . H9 H 0.3673 0.1830 0.3823 0.031 Uiso 1 1 calc R . . C10 C 0.43601(13) 0.31655(18) 0.39026(13) 0.0226(4) Uani 1 1 d . . . H10 H 0.4703 0.3033 0.4433 0.027 Uiso 1 1 calc R . . C11 C 0.44529(12) 0.40737(16) 0.34734(12) 0.0178(4) Uani 1 1 d . . . C12 C 0.50864(13) 0.49053(17) 0.38385(12) 0.0198(4) Uani 1 1 d . . . H12A H 0.4968 0.5216 0.4332 0.024 Uiso 1 1 calc R . . H12B H 0.5623 0.4564 0.4009 0.024 Uiso 1 1 calc R . . C13 C 0.37074(12) 0.67888(17) 0.39588(12) 0.0194(4) Uani 1 1 d . . . C14 C 0.31619(14) 0.6963(2) 0.45136(14) 0.0286(5) Uani 1 1 d . . . H14A H 0.2649 0.6598 0.4287 0.043 Uiso 1 1 calc R . . H14B H 0.3064 0.7724 0.4554 0.043 Uiso 1 1 calc R . . H14C H 0.3419 0.6681 0.5060 0.043 Uiso 1 1 calc R . . C15 C 0.67926(12) 0.62817(17) 0.42850(12) 0.0202(4) Uani 1 1 d . . . C16 C 0.74352(14) 0.5994(2) 0.50524(14) 0.0301(5) Uani 1 1 d . . . H16A H 0.7827 0.6572 0.5196 0.045 Uiso 1 1 calc R . . H16B H 0.7710 0.5346 0.4955 0.045 Uiso 1 1 calc R . . H16C H 0.7186 0.5876 0.5504 0.045 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.01430(14) 0.01676(15) 0.01364(14) -0.00058(9) 0.00337(10) -0.00116(9) Ni2 0.01283(14) 0.01666(15) 0.01463(14) 0.00092(9) 0.00162(10) -0.00055(9) O1 0.0147(6) 0.0166(7) 0.0158(7) -0.0015(5) 0.0040(5) -0.0022(5) O2 0.0153(7) 0.0166(7) 0.0141(6) 0.0013(5) 0.0017(5) 0.0001(5) O3 0.0183(7) 0.0239(8) 0.0173(7) -0.0005(6) 0.0063(6) -0.0014(6) O4 0.0171(7) 0.0215(8) 0.0208(7) 0.0008(6) 0.0059(6) -0.0001(6) O5 0.0207(7) 0.0208(8) 0.0176(7) -0.0004(6) 0.0008(6) -0.0022(6) O6 0.0170(7) 0.0231(8) 0.0219(7) -0.0018(6) -0.0016(6) 0.0002(6) N1 0.0168(8) 0.0197(9) 0.0162(8) 0.0004(7) 0.0025(6) 0.0003(7) N2 0.0157(8) 0.0194(9) 0.0183(8) 0.0000(7) 0.0048(7) 0.0000(7) C1 0.0237(11) 0.0237(11) 0.0197(10) -0.0003(8) 0.0062(8) 0.0011(9) C2 0.0353(13) 0.0204(11) 0.0271(12) -0.0033(9) 0.0071(10) 0.0053(10) C3 0.0367(13) 0.0170(11) 0.0299(12) -0.0009(9) 0.0075(10) -0.0047(9) C4 0.0274(11) 0.0221(11) 0.0250(11) 0.0009(9) 0.0066(9) -0.0058(9) C5 0.0165(9) 0.0198(11) 0.0172(9) 0.0004(8) 0.0010(8) -0.0010(8) C6 0.0155(9) 0.0188(10) 0.0215(10) -0.0005(8) 0.0062(8) -0.0038(8) C7 0.0160(10) 0.0227(11) 0.0224(10) -0.0042(8) 0.0040(8) -0.0008(8) C8 0.0180(10) 0.0189(11) 0.0329(12) -0.0062(9) 0.0076(9) -0.0012(8) C9 0.0272(12) 0.0197(11) 0.0339(12) 0.0045(9) 0.0115(10) -0.0003(9) C10 0.0241(11) 0.0208(11) 0.0222(10) 0.0028(8) 0.0049(8) 0.0017(9) C11 0.0165(9) 0.0183(10) 0.0194(10) -0.0014(8) 0.0061(8) 0.0014(8) C12 0.0202(10) 0.0197(11) 0.0173(9) 0.0026(8) 0.0006(8) -0.0014(8) C13 0.0195(10) 0.0201(11) 0.0186(10) 0.0043(8) 0.0050(8) 0.0035(8) C14 0.0225(11) 0.0372(14) 0.0282(12) -0.0025(10) 0.0105(9) -0.0012(10) C15 0.0179(10) 0.0185(10) 0.0208(10) 0.0011(8) -0.0011(8) -0.0050(8) C16 0.0281(12) 0.0296(13) 0.0247(11) -0.0007(9) -0.0068(9) 0.0023(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 O3 2.0214(14) . ? Ni1 O1 2.0218(14) . ? Ni1 O2 2.0290(14) . ? Ni1 N1 2.0488(18) . ? Ni1 O5 2.0780(14) . ? Ni1 O1 2.1068(14) 2_655 ? Ni1 Ni2 2.9273(4) 2_655 ? Ni1 Ni2 2.9474(4) . ? Ni2 O6 2.0116(15) 2_655 ? Ni2 O1 2.0156(14) 2_655 ? Ni2 O2 2.0181(14) . ? Ni2 N2 2.0363(18) . ? Ni2 O2 2.1204(14) 2_655 ? Ni2 O4 2.1234(14) . ? Ni2 Ni1 2.9273(4) 2_655 ? O1 C6 1.402(2) . ? O1 Ni2 2.0156(14) 2_655 ? O1 Ni1 2.1068(14) 2_655 ? O2 C12 1.397(2) . ? O2 Ni2 2.1204(14) 2_655 ? O3 C13 1.272(3) . ? O4 C13 1.258(3) . ? O5 C15 1.263(3) . ? O6 C15 1.273(3) . ? O6 Ni2 2.0116(15) 2_655 ? N1 C5 1.342(3) . ? N1 C1 1.343(3) . ? N2 C11 1.338(3) . ? N2 C7 1.347(3) . ? C1 C2 1.384(3) . ? C1 H1 0.9500 . ? C2 C3 1.383(3) . ? C2 H2 0.9500 . ? C3 C4 1.382(3) . ? C3 H3 0.9500 . ? C4 C5 1.390(3) . ? C4 H4 0.9500 . ? C5 C6 1.512(3) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.380(3) . ? C7 H7 0.9500 . ? C8 C9 1.381(3) . ? C8 H8 0.9500 . ? C9 C10 1.392(3) . ? C9 H9 0.9500 . ? C10 C11 1.388(3) . ? C10 H10 0.9500 . ? C11 C12 1.522(3) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.506(3) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.510(3) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 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 O3 Ni1 O1 166.56(6) . . ? O3 Ni1 O2 92.63(6) . . ? O1 Ni1 O2 87.95(6) . . ? O3 Ni1 N1 99.12(6) . . ? O1 Ni1 N1 80.82(6) . . ? O2 Ni1 N1 168.22(6) . . ? O3 Ni1 O5 100.99(6) . . ? O1 Ni1 O5 92.44(6) . . ? O2 Ni1 O5 85.07(6) . . ? N1 Ni1 O5 91.81(6) . . ? O3 Ni1 O1 90.48(6) . 2_655 ? O1 Ni1 O1 76.19(6) . 2_655 ? O2 Ni1 O1 84.81(5) . 2_655 ? N1 Ni1 O1 95.88(6) . 2_655 ? O5 Ni1 O1 165.02(6) . 2_655 ? O3 Ni1 Ni2 139.04(4) . 2_655 ? O1 Ni1 Ni2 43.44(4) . 2_655 ? O2 Ni1 Ni2 46.41(4) . 2_655 ? N1 Ni1 Ni2 121.82(5) . 2_655 ? O5 Ni1 Ni2 78.15(4) . 2_655 ? O1 Ni1 Ni2 86.87(4) 2_655 2_655 ? O3 Ni1 Ni2 83.42(4) . . ? O1 Ni1 Ni2 87.88(4) . . ? O2 Ni1 Ni2 43.11(4) . . ? N1 Ni1 Ni2 139.00(5) . . ? O5 Ni1 Ni2 128.16(4) . . ? O1 Ni1 Ni2 43.13(4) 2_655 . ? Ni2 Ni1 Ni2 67.126(11) 2_655 . ? O6 Ni2 O1 94.22(6) 2_655 2_655 ? O6 Ni2 O2 165.99(6) 2_655 . ? O1 Ni2 O2 87.52(6) 2_655 . ? O6 Ni2 N2 99.05(6) 2_655 . ? O1 Ni2 N2 165.62(6) 2_655 . ? O2 Ni2 N2 80.96(6) . . ? O6 Ni2 O2 90.34(6) 2_655 2_655 ? O1 Ni2 O2 85.66(5) 2_655 2_655 ? O2 Ni2 O2 75.91(6) . 2_655 ? N2 Ni2 O2 99.72(6) . 2_655 ? O6 Ni2 O4 103.06(6) 2_655 . ? O1 Ni2 O4 84.16(6) 2_655 . ? O2 Ni2 O4 90.94(6) . . ? N2 Ni2 O4 87.44(6) . . ? O2 Ni2 O4 163.70(6) 2_655 . ? O6 Ni2 Ni1 83.22(4) 2_655 2_655 ? O1 Ni2 Ni1 43.61(4) 2_655 2_655 ? O2 Ni2 Ni1 88.54(4) . 2_655 ? N2 Ni2 Ni1 143.59(5) . 2_655 ? O2 Ni2 Ni1 43.88(4) 2_655 2_655 ? O4 Ni2 Ni1 127.75(4) . 2_655 ? O6 Ni2 Ni1 139.82(4) 2_655 . ? O1 Ni2 Ni1 45.61(4) 2_655 . ? O2 Ni2 Ni1 43.40(4) . . ? N2 Ni2 Ni1 121.01(5) . . ? O2 Ni2 Ni1 86.14(4) 2_655 . ? O4 Ni2 Ni1 77.64(4) . . ? Ni1 Ni2 Ni1 66.849(11) 2_655 . ? C6 O1 Ni2 129.95(13) . 2_655 ? C6 O1 Ni1 110.63(11) . . ? Ni2 O1 Ni1 92.95(6) 2_655 . ? C6 O1 Ni1 122.81(12) . 2_655 ? Ni2 O1 Ni1 91.26(6) 2_655 2_655 ? Ni1 O1 Ni1 103.20(6) . 2_655 ? C12 O2 Ni2 111.71(12) . . ? C12 O2 Ni1 127.32(13) . . ? Ni2 O2 Ni1 93.49(6) . . ? C12 O2 Ni2 124.96(13) . 2_655 ? Ni2 O2 Ni2 103.38(6) . 2_655 ? Ni1 O2 Ni2 89.71(6) . 2_655 ? C13 O3 Ni1 124.17(13) . . ? C13 O4 Ni2 127.08(13) . . ? C15 O5 Ni1 127.20(13) . . ? C15 O6 Ni2 123.34(13) . 2_655 ? C5 N1 C1 119.08(19) . . ? C5 N1 Ni1 112.62(14) . . ? C1 N1 Ni1 128.29(15) . . ? C11 N2 C7 119.17(19) . . ? C11 N2 Ni2 111.84(14) . . ? C7 N2 Ni2 127.10(14) . . ? N1 C1 C2 122.4(2) . . ? N1 C1 H1 118.8 . . ? C2 C1 H1 118.8 . . ? C3 C2 C1 118.5(2) . . ? C3 C2 H2 120.7 . . ? C1 C2 H2 120.7 . . ? C4 C3 C2 119.3(2) . . ? C4 C3 H3 120.4 . . ? C2 C3 H3 120.4 . . ? C3 C4 C5 119.2(2) . . ? C3 C4 H4 120.4 . . ? C5 C4 H4 120.4 . . ? N1 C5 C4 121.5(2) . . ? N1 C5 C6 115.75(18) . . ? C4 C5 C6 122.77(19) . . ? O1 C6 C5 110.54(16) . . ? O1 C6 H6A 109.5 . . ? C5 C6 H6A 109.5 . . ? O1 C6 H6B 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 108.1 . . ? N2 C7 C8 122.3(2) . . ? N2 C7 H7 118.9 . . ? C8 C7 H7 118.9 . . ? C7 C8 C9 118.6(2) . . ? C7 C8 H8 120.7 . . ? C9 C8 H8 120.7 . . ? C8 C9 C10 119.5(2) . . ? C8 C9 H9 120.3 . . ? C10 C9 H9 120.3 . . ? C11 C10 C9 118.6(2) . . ? C11 C10 H10 120.7 . . ? C9 C10 H10 120.7 . . ? N2 C11 C10 121.81(19) . . ? N2 C11 C12 116.37(18) . . ? C10 C11 C12 121.76(18) . . ? O2 C12 C11 111.38(16) . . ? O2 C12 H12A 109.4 . . ? C11 C12 H12A 109.4 . . ? O2 C12 H12B 109.4 . . ? C11 C12 H12B 109.4 . . ? H12A C12 H12B 108.0 . . ? O4 C13 O3 127.27(19) . . ? O4 C13 C14 117.22(19) . . ? O3 C13 C14 115.51(19) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O5 C15 O6 126.67(18) . . ? O5 C15 C16 117.16(19) . . ? O6 C15 C16 116.16(19) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.761 _refine_diff_density_min -0.285 _refine_diff_density_rms 0.102 data_[Ni2(mu-Br)2(ehmpH)4]Br2 _database_code_depnum_ccdc_archive 'CCDC 798246' #TrackingRef 'CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C110 H139 Br12 N13 Ni6 O38' _chemical_formula_weight 3562.52 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' 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.7506(5) _cell_length_b 22.6852(8) _cell_length_c 25.2982(8) _cell_angle_alpha 110.5250(10) _cell_angle_beta 93.0870(10) _cell_angle_gamma 105.9330(10) _cell_volume 7007.1(4) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 5942 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 20.24 _exptl_crystal_description Block _exptl_crystal_colour Green _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas 'Not Measured' _exptl_crystal_density_diffrn 1.709 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3608 _exptl_absorpt_coefficient_mu 4.291 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.4807 _exptl_absorpt_correction_T_max 0.5654 _exptl_absorpt_process_details 'Sadabs, (Sheldrick 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 76088 _diffrn_reflns_av_R_equivalents 0.0826 _diffrn_reflns_av_sigmaI/netI 0.0946 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 25.00 _reflns_number_total 24684 _reflns_number_gt 15765 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1125P)^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 24684 _refine_ls_number_parameters 1522 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1121 _refine_ls_R_factor_gt 0.0693 _refine_ls_wR_factor_ref 0.2088 _refine_ls_wR_factor_gt 0.1866 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.062 _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 1.01973(8) -0.06735(5) 0.16848(5) 0.0332(3) Uani 1 1 d . . . Ni2 Ni 1.29112(8) -0.06477(5) 0.19669(5) 0.0308(3) Uani 1 1 d . . . Ni3 Ni 0.22610(8) -0.30138(5) 0.48956(4) 0.0289(3) Uani 1 1 d . . . Ni4 Ni 0.32289(8) -0.27094(5) 0.36545(4) 0.0241(2) Uani 1 1 d . . . Ni5 Ni 0.54202(8) 0.41276(5) 0.10102(4) 0.0266(3) Uani 1 1 d . . . Ni6 Ni 0.63686(8) 0.35873(5) 0.21069(4) 0.0249(2) Uani 1 1 d . . . Br1 Br 1.19014(7) -0.01588(4) 0.14279(4) 0.0366(2) Uani 1 1 d . . . Br2 Br 1.12191(7) -0.10624(4) 0.22922(4) 0.0333(2) Uani 1 1 d . . . Br3 Br 0.14645(6) -0.30345(4) 0.39481(3) 0.0271(2) Uani 1 1 d . . . Br4 Br 0.40328(6) -0.25789(4) 0.46387(4) 0.0291(2) Uani 1 1 d . . . Br5 Br 0.68529(6) 0.36516(4) 0.11630(3) 0.0282(2) Uani 1 1 d . . . Br6 Br 0.48339(6) 0.39468(4) 0.18991(3) 0.0281(2) Uani 1 1 d . . . Br7 Br 0.67545(8) 0.56355(5) 0.02173(4) 0.0458(3) Uani 1 1 d . . . Br8 Br 0.24594(9) -0.41684(5) 0.60211(4) 0.0547(3) Uani 1 1 d . . . Br9 Br 0.05349(10) -0.29753(6) 0.63459(5) 0.0627(3) Uani 1 1 d . . . Br10 Br 0.35297(11) -0.32715(8) 0.17860(5) 0.0804(4) Uani 1 1 d . . . Br11 Br 0.64037(15) -0.18179(10) 0.27912(9) 0.0653(8) Uani 0.602(3) 1 d P A 1 Br12 Br 0.7538(4) -0.1115(4) 0.2786(2) 0.182(4) Uani 0.398(3) 1 d P A 2 Br13 Br 1.64171(14) 0.06635(12) 0.19436(9) 0.1057(12) Uani 0.768(5) 1 d P B 1 Br14 Br 1.6423(5) -0.0057(6) 0.2055(4) 0.141(5) Uani 0.232(5) 1 d P B 2 O1 O 0.8829(5) -0.1153(4) 0.1867(3) 0.059(2) Uani 1 1 d . . . HO1 H 0.8309 -0.1055 0.1992 0.071 Uiso 1 1 d R . . O2 O 1.0432(7) -0.3232(4) -0.0587(4) 0.101(3) Uani 1 1 d . . . O3 O 1.1133(8) -0.2161(5) -0.0385(4) 0.083(3) Uani 1 1 d . . . O4 O 0.9406(5) -0.0319(3) 0.1212(3) 0.0482(17) Uani 1 1 d . . . HO4 H 0.9343 -0.0347 0.0868 0.058 Uiso 1 1 d R . . O5 O 1.1721(6) 0.1046(4) 0.3984(3) 0.059(2) Uani 1 1 d . . . O6 O 1.0940(6) 0.1833(4) 0.4179(3) 0.072(2) Uani 1 1 d . . . O7 O 1.4166(5) -0.0313(3) 0.1618(3) 0.0497(18) Uani 1 1 d . . . HO7 H 1.4604 0.0067 0.1699 0.060 Uiso 1 1 d R . . O8 O 1.0893(6) -0.3447(3) 0.0890(3) 0.059(2) Uani 1 1 d . . . O9 O 1.2019(6) -0.3782(3) 0.0321(3) 0.062(2) Uani 1 1 d . . . O10 O 1.3717(5) -0.1019(3) 0.2425(3) 0.0402(15) Uani 1 1 d . . . HO10 H 1.3698 -0.1407 0.2398 0.048 Uiso 1 1 d R . . O11 O 1.2879(5) 0.1952(3) 0.3166(3) 0.0519(18) Uani 1 1 d . . . O12 O 1.3920(6) 0.2328(3) 0.4013(3) 0.070(2) Uani 1 1 d . . . O13 O 0.2971(5) -0.2963(3) 0.5643(3) 0.0424(16) Uani 1 1 d . . . HO13 H 0.3145 -0.3234 0.5760 0.051 Uiso 1 1 d R . . O14 O 0.0806(8) -0.0884(4) 0.5014(4) 0.082(3) Uani 1 1 d . . . O15 O 0.1213(9) -0.0186(4) 0.5933(4) 0.101(3) Uani 1 1 d D . . O16 O 0.0793(5) -0.3378(3) 0.5045(3) 0.0424(16) Uani 1 1 d . . . HO16 H 0.0458 -0.3267 0.5315 0.051 Uiso 1 1 d R . . O17 O 0.3282(8) -0.5864(4) 0.4052(5) 0.117(4) Uani 1 1 d . . . O18 O 0.4323(6) -0.4853(4) 0.4140(3) 0.060(2) Uani 1 1 d . . . O19 O 0.2553(4) -0.2782(3) 0.2883(2) 0.0299(13) Uani 1 1 d . . . HO19 H 0.2590 -0.3005 0.2540 0.036 Uiso 1 1 d R . . O20 O 0.4186(6) -0.0166(3) 0.5471(3) 0.0550(19) Uani 1 1 d . . . O21 O 0.3354(6) 0.0386(3) 0.5133(3) 0.057(2) Uani 1 1 d . . . O22 O 0.4677(4) -0.2496(3) 0.3439(3) 0.0349(14) Uani 1 1 d . . . HO22 H 0.4986 -0.2236 0.3285 0.042 Uiso 1 1 d R . . O23 O 0.0993(5) -0.5487(3) 0.2749(4) 0.061(2) Uani 1 1 d . . . O24 O 0.2193(5) -0.5965(3) 0.2756(3) 0.0540(19) Uani 1 1 d . . . O25 O 0.5912(5) 0.4225(3) 0.0282(2) 0.0393(15) Uani 1 1 d . . . HO25 H 0.6373 0.4526 0.0227 0.047 Uiso 1 1 d R . . O26 O 0.1951(6) 0.1124(4) -0.0272(4) 0.077(3) Uani 1 1 d . . . O27 O 0.2466(6) 0.1727(3) 0.0656(4) 0.067(2) Uani 1 1 d D . . O28 O 0.4252(5) 0.4519(3) 0.0963(2) 0.0359(15) Uani 1 1 d . . . HO28 H 0.3626 0.4362 0.0803 0.043 Uiso 1 1 d R . . O29 O 0.9240(6) 0.6974(4) 0.2153(4) 0.075(2) Uani 1 1 d . . . O30 O 0.9266(5) 0.5936(3) 0.1917(3) 0.0438(16) Uani 1 1 d . . . O31 O 0.5902(5) 0.3539(3) 0.2859(2) 0.0383(15) Uani 1 1 d . . . HO31 H 0.5901 0.3836 0.3177 0.046 Uiso 1 1 d R . . O32 O 0.4970(8) 0.1177(4) 0.0177(4) 0.115(4) Uani 1 1 d . . . O33 O 0.3709(6) 0.0506(3) 0.0388(3) 0.069(2) Uani 1 1 d . . . O34 O 0.7633(4) 0.3308(3) 0.2248(3) 0.0380(15) Uani 1 1 d . . . HO34 H 0.7696 0.2948 0.2253 0.046 Uiso 1 1 d R . . O35 O 0.6901(5) 0.6335(3) 0.3176(3) 0.056(2) Uani 1 1 d . . . O36 O 0.8576(5) 0.6820(3) 0.3368(3) 0.055(2) Uani 1 1 d . . . O37 O 0.2267(6) -0.2334(4) 0.7337(3) 0.066(2) Uiso 1 1 d . . . H137 H 0.1687 -0.2405 0.7150 0.099 Uiso 1 1 d R . . H237 H 0.2616 -0.1932 0.7416 0.099 Uiso 1 1 d R . . O38 O 1.4630(8) -0.1831(5) 0.1835(4) 0.108(3) Uiso 1 1 d . . . H138 H 1.4466 -0.1828 0.1507 0.162 Uiso 1 1 d R . . H238 H 1.5275 -0.1646 0.1935 0.162 Uiso 1 1 d R . . N1 N 0.9799(6) -0.1617(4) 0.1043(3) 0.042(2) Uani 1 1 d . . . N2 N 1.0175(6) 0.0203(4) 0.2303(3) 0.0370(18) Uani 1 1 d . . . N3 N 1.2770(6) -0.1481(4) 0.1251(3) 0.0373(18) Uani 1 1 d . . . N4 N 1.3500(5) 0.0162(3) 0.2734(3) 0.0318(17) Uani 1 1 d . . . N5 N 0.2281(5) -0.2081(3) 0.5432(3) 0.0321(17) Uani 1 1 d . . . N6 N 0.2054(6) -0.4016(3) 0.4560(3) 0.0329(17) Uani 1 1 d . . . N7 N 0.3158(5) -0.1758(3) 0.3867(3) 0.0268(16) Uani 1 1 d . . . N8 N 0.3343(5) -0.3651(3) 0.3276(3) 0.0252(15) Uani 1 1 d . . . N9 N 0.4546(5) 0.3233(3) 0.0372(3) 0.0281(16) Uani 1 1 d . . . N10 N 0.6179(6) 0.5135(3) 0.1440(3) 0.0294(16) Uani 1 1 d . . . N11 N 0.5462(5) 0.2607(3) 0.1821(3) 0.0274(16) Uani 1 1 d . . . N12 N 0.7417(5) 0.4490(3) 0.2574(3) 0.0244(15) Uani 1 1 d . . . N13 N 0.8231(12) -0.3063(8) -0.1077(7) 0.133(4) Uiso 1 1 d D . . C1 C 0.8630(8) -0.1824(5) 0.1686(5) 0.060(3) Uani 1 1 d . . . H1A H 0.7887 -0.2044 0.1604 0.072 Uiso 1 1 calc R . . H1B H 0.8923 -0.1931 0.1989 0.072 Uiso 1 1 calc R . . C2 C 0.9090(8) -0.2075(5) 0.1150(5) 0.049(3) Uani 1 1 d . . . C3 C 0.8786(9) -0.2740(6) 0.0798(6) 0.066(3) Uani 1 1 d . . . H3A H 0.8263 -0.3054 0.0871 0.079 Uiso 1 1 calc R . . C4 C 0.9280(10) -0.2922(5) 0.0339(6) 0.075(4) Uani 1 1 d . . . H4A H 0.9120 -0.3375 0.0110 0.090 Uiso 1 1 calc R . . C5 C 1.0014(9) -0.2462(5) 0.0196(5) 0.062(3) Uani 1 1 d . . . C6 C 1.0249(8) -0.1796(5) 0.0584(4) 0.047(3) Uani 1 1 d . . . H6A H 1.0745 -0.1465 0.0515 0.057 Uiso 1 1 calc R . . C7 C 1.0530(11) -0.2665(7) -0.0289(5) 0.074(4) Uani 1 1 d . . . C8 C 1.1674(11) -0.2295(7) -0.0882(5) 0.0922(19) Uani 1 1 d . . . H8A H 1.2345 -0.1954 -0.0788 0.111 Uiso 1 1 calc R . . H8B H 1.1784 -0.2727 -0.0978 0.111 Uiso 1 1 calc R . . C9 C 1.1060(11) -0.2292(7) -0.1369(5) 0.0922(19) Uani 1 1 d . . . H9A H 1.1411 -0.2383 -0.1697 0.138 Uiso 1 1 calc R . . H9B H 1.0962 -0.1862 -0.1274 0.138 Uiso 1 1 calc R . . H9C H 1.0398 -0.2631 -0.1461 0.138 Uiso 1 1 calc R . . C10 C 0.8990(8) 0.0162(6) 0.1529(4) 0.057(3) Uani 1 1 d . . . H10A H 0.8262 -0.0045 0.1525 0.068 Uiso 1 1 calc R . . H10B H 0.9043 0.0492 0.1356 0.068 Uiso 1 1 calc R . . C11 C 0.9559(8) 0.0501(5) 0.2144(4) 0.047(3) Uani 1 1 d . . . C12 C 0.9427(8) 0.1065(5) 0.2517(5) 0.054(3) Uani 1 1 d . . . H12A H 0.8983 0.1258 0.2395 0.065 Uiso 1 1 calc R . . C13 C 0.9945(8) 0.1354(5) 0.3074(5) 0.055(3) Uani 1 1 d . . . H13A H 0.9885 0.1755 0.3329 0.066 Uiso 1 1 calc R . . C14 C 1.0551(7) 0.1041(5) 0.3247(4) 0.043(2) Uani 1 1 d . . . C15 C 1.0654(6) 0.0473(4) 0.2848(4) 0.037(2) Uani 1 1 d . . . H15A H 1.1080 0.0264 0.2964 0.045 Uiso 1 1 calc R . . C16 C 1.1136(8) 0.1288(5) 0.3839(4) 0.044(2) Uani 1 1 d . . . C17 C 1.1477(11) 0.2134(7) 0.4767(6) 0.0922(19) Uani 1 1 d . . . H17A H 1.2210 0.2187 0.4778 0.111 Uiso 1 1 calc R . . H17B H 1.1197 0.1860 0.4982 0.111 Uiso 1 1 calc R . . C18 C 1.1303(11) 0.2810(7) 0.5017(6) 0.0922(19) Uani 1 1 d . . . H18A H 1.1644 0.3039 0.5412 0.138 Uiso 1 1 calc R . . H18B H 1.0573 0.2748 0.5000 0.138 Uiso 1 1 calc R . . H18C H 1.1581 0.3073 0.4797 0.138 Uiso 1 1 calc R . . C19 C 1.4093(8) -0.0693(5) 0.1033(4) 0.047(3) Uani 1 1 d . . . H19A H 1.4780 -0.0686 0.0943 0.056 Uiso 1 1 calc R . . H19B H 1.3792 -0.0501 0.0800 0.056 Uiso 1 1 calc R . . C20 C 1.3435(7) -0.1400(5) 0.0891(4) 0.037(2) Uani 1 1 d . . . C21 C 1.3498(8) -0.1929(5) 0.0436(4) 0.049(3) Uani 1 1 d . . . H21A H 1.3942 -0.1856 0.0180 0.059 Uiso 1 1 calc R . . C22 C 1.2922(8) -0.2571(5) 0.0347(4) 0.046(3) Uani 1 1 d . . . H22A H 1.2978 -0.2935 0.0040 0.055 Uiso 1 1 calc R . . C23 C 1.2264(7) -0.2656(4) 0.0723(4) 0.037(2) Uani 1 1 d . . . C24 C 1.2183(6) -0.2119(4) 0.1162(4) 0.032(2) Uani 1 1 d . . . H24A H 1.1715 -0.2186 0.1409 0.039 Uiso 1 1 calc R . . C25 C 1.1634(9) -0.3327(5) 0.0669(4) 0.046(3) Uani 1 1 d . . . C26 C 1.1511(11) -0.4476(7) 0.0206(5) 0.0922(19) Uani 1 1 d . . . H26A H 1.0932 -0.4523 0.0414 0.111 Uiso 1 1 calc R . . H26B H 1.1991 -0.4671 0.0328 0.111 Uiso 1 1 calc R . . C27 C 1.1148(11) -0.4810(7) -0.0418(5) 0.0922(19) Uani 1 1 d . . . H27A H 1.0808 -0.5278 -0.0514 0.138 Uiso 1 1 calc R . . H27B H 1.1728 -0.4755 -0.0618 0.138 Uiso 1 1 calc R . . H27C H 1.0669 -0.4614 -0.0532 0.138 Uiso 1 1 calc R . . C28 C 1.4398(8) -0.0550(5) 0.2924(5) 0.048(3) Uani 1 1 d . . . H28A H 1.5103 -0.0461 0.2845 0.058 Uiso 1 1 calc R . . H28B H 1.4359 -0.0727 0.3227 0.058 Uiso 1 1 calc R . . C29 C 1.4129(7) 0.0077(4) 0.3118(4) 0.035(2) Uani 1 1 d . . . C30 C 1.4494(7) 0.0547(4) 0.3646(4) 0.038(2) Uani 1 1 d . . . H30A H 1.4912 0.0473 0.3907 0.046 Uiso 1 1 calc R . . C31 C 1.4271(7) 0.1131(5) 0.3811(4) 0.042(2) Uani 1 1 d . . . H31A H 1.4518 0.1457 0.4182 0.051 Uiso 1 1 calc R . . C32 C 1.3657(7) 0.1224(4) 0.3403(4) 0.035(2) Uani 1 1 d . . . C33 C 1.3274(6) 0.0723(4) 0.2875(4) 0.030(2) Uani 1 1 d . . . H33A H 1.2841 0.0779 0.2608 0.036 Uiso 1 1 calc R . . C34 C 1.3425(7) 0.1869(4) 0.3515(4) 0.040(2) Uani 1 1 d . . . C35 C 1.3799(9) 0.2984(5) 0.4145(5) 0.067(3) Uani 1 1 d . . . H35A H 1.3863 0.3109 0.3812 0.080 Uiso 1 1 calc R . . H35B H 1.3125 0.2985 0.4252 0.080 Uiso 1 1 calc R . . C36 C 1.4612(12) 0.3442(5) 0.4620(6) 0.107(6) Uani 1 1 d . . . H36A H 1.4566 0.3887 0.4724 0.160 Uiso 1 1 calc R . . H36B H 1.5273 0.3434 0.4507 0.160 Uiso 1 1 calc R . . H36C H 1.4538 0.3311 0.4945 0.160 Uiso 1 1 calc R . . C37 C 0.3246(8) -0.2342(5) 0.6094(4) 0.044(2) Uani 1 1 d . . . H37A H 0.3993 -0.2143 0.6164 0.053 Uiso 1 1 calc R . . H37B H 0.3044 -0.2402 0.6442 0.053 Uiso 1 1 calc R . . C38 C 0.2757(7) -0.1884(4) 0.5973(4) 0.036(2) Uani 1 1 d . . . C39 C 0.2765(8) -0.1295(5) 0.6386(4) 0.050(3) Uani 1 1 d . . . H39A H 0.3098 -0.1164 0.6762 0.059 Uiso 1 1 calc R . . C40 C 0.2281(8) -0.0892(5) 0.6245(4) 0.048(3) Uani 1 1 d . . . H40A H 0.2289 -0.0485 0.6522 0.058 Uiso 1 1 calc R . . C41 C 0.1785(8) -0.1104(5) 0.5688(4) 0.043(2) Uani 1 1 d . . . C42 C 0.1821(7) -0.1699(4) 0.5293(4) 0.033(2) Uani 1 1 d . . . H42A H 0.1506 -0.1839 0.4912 0.040 Uiso 1 1 calc R . . C43 C 0.1191(10) -0.0741(5) 0.5497(6) 0.062(3) Uani 1 1 d . . . C44 C 0.0924(11) 0.0298(6) 0.5769(7) 0.105(3) Uani 1 1 d D . . H44A H 0.1359 0.0751 0.6001 0.126 Uiso 1 1 calc R . . H44B H 0.0934 0.0212 0.5362 0.126 Uiso 1 1 calc R . . C45 C -0.0091(10) 0.0173(7) 0.5894(7) 0.105(3) Uani 1 1 d D . . H45A H -0.0410 0.0464 0.5799 0.157 Uiso 1 1 calc R . . H45B H -0.0069 0.0257 0.6299 0.157 Uiso 1 1 calc R . . H45C H -0.0487 -0.0285 0.5670 0.157 Uiso 1 1 calc R . . C46 C 0.0318(7) -0.4061(5) 0.4694(5) 0.051(3) Uani 1 1 d . . . H46A H -0.0108 -0.4098 0.4354 0.061 Uiso 1 1 calc R . . H46B H -0.0130 -0.4275 0.4907 0.061 Uiso 1 1 calc R . . C47 C 0.1089(8) -0.4411(4) 0.4512(4) 0.040(2) Uani 1 1 d . . . C48 C 0.0852(9) -0.5087(5) 0.4307(4) 0.054(3) Uani 1 1 d . . . H48A H 0.0167 -0.5352 0.4251 0.065 Uiso 1 1 calc R . . C49 C 0.1575(9) -0.5372(5) 0.4186(5) 0.057(3) Uani 1 1 d . . . H49A H 0.1407 -0.5835 0.4056 0.069 Uiso 1 1 calc R . . C50 C 0.2583(9) -0.4984(4) 0.4252(4) 0.047(3) Uani 1 1 d . . . C51 C 0.2767(8) -0.4302(4) 0.4424(4) 0.037(2) Uani 1 1 d . . . H51A H 0.3435 -0.4034 0.4443 0.045 Uiso 1 1 calc R . . C52 C 0.3428(10) -0.5282(6) 0.4134(5) 0.066(3) Uani 1 1 d . . . C53 C 0.5179(13) -0.5095(7) 0.4008(7) 0.103(5) Uani 1 1 d . . . H53A H 0.5291 -0.5323 0.4259 0.124 Uiso 1 1 calc R . . H53B H 0.5022 -0.5417 0.3612 0.124 Uiso 1 1 calc R . . C54 C 0.6092(12) -0.4568(8) 0.4078(7) 0.104(6) Uani 1 1 d . . . H54A H 0.6654 -0.4747 0.3986 0.156 Uiso 1 1 calc R . . H54B H 0.6255 -0.4253 0.4471 0.156 Uiso 1 1 calc R . . H54C H 0.5987 -0.4348 0.3823 0.156 Uiso 1 1 calc R . . C55 C 0.2225(7) -0.2231(4) 0.2895(4) 0.040(2) Uani 1 1 d . . . H55A H 0.1475 -0.2372 0.2805 0.048 Uiso 1 1 calc R . . H55B H 0.2503 -0.2072 0.2603 0.048 Uiso 1 1 calc R . . C56 C 0.2581(6) -0.1681(4) 0.3471(4) 0.031(2) Uani 1 1 d . . . C57 C 0.2297(8) -0.1111(4) 0.3573(4) 0.041(2) Uani 1 1 d . . . H57A H 0.1875 -0.1077 0.3288 0.049 Uiso 1 1 calc R . . C58 C 0.2647(8) -0.0602(5) 0.4098(4) 0.043(2) Uani 1 1 d . . . H58A H 0.2464 -0.0213 0.4177 0.051 Uiso 1 1 calc R . . C59 C 0.3274(6) -0.0661(4) 0.4515(4) 0.0276(19) Uani 1 1 d . . . C60 C 0.3495(6) -0.1249(4) 0.4383(4) 0.031(2) Uani 1 1 d . . . H60A H 0.3902 -0.1299 0.4665 0.037 Uiso 1 1 calc R . . C61 C 0.3688(7) -0.0129(4) 0.5088(4) 0.039(2) Uani 1 1 d . . . C62 C 0.3599(12) 0.0933(6) 0.5682(7) 0.105(3) Uani 1 1 d . . . H62A H 0.4342 0.1121 0.5810 0.126 Uiso 1 1 calc R . . H62B H 0.3279 0.0790 0.5972 0.126 Uiso 1 1 calc R . . C63 C 0.3169(11) 0.1427(6) 0.5574(7) 0.105(3) Uani 1 1 d . . . H63A H 0.3296 0.1812 0.5926 0.157 Uiso 1 1 calc R . . H63B H 0.2436 0.1228 0.5439 0.157 Uiso 1 1 calc R . . H63C H 0.3496 0.1562 0.5286 0.157 Uiso 1 1 calc R . . C64 C 0.5094(6) -0.3024(4) 0.3327(4) 0.041(2) Uani 1 1 d . . . H64A H 0.5553 -0.2951 0.3669 0.050 Uiso 1 1 calc R . . H64B H 0.5499 -0.3035 0.3018 0.050 Uiso 1 1 calc R . . C65 C 0.4268(6) -0.3670(4) 0.3158(3) 0.0279(19) Uani 1 1 d . . . C66 C 0.4487(7) -0.4262(4) 0.2923(4) 0.036(2) Uani 1 1 d . . . H66A H 0.5146 -0.4264 0.2842 0.043 Uiso 1 1 calc R . . C67 C 0.3702(7) -0.4857(4) 0.2812(4) 0.038(2) Uani 1 1 d . . . H67A H 0.3834 -0.5264 0.2666 0.046 Uiso 1 1 calc R . . C68 C 0.2744(6) -0.4840(4) 0.2915(4) 0.029(2) Uani 1 1 d . . . C69 C 0.2577(6) -0.4232(4) 0.3148(3) 0.0281(19) Uani 1 1 d . . . H69A H 0.1917 -0.4220 0.3219 0.034 Uiso 1 1 calc R . . C70 C 0.1871(7) -0.5460(4) 0.2804(4) 0.039(2) Uani 1 1 d . . . C71 C 0.1434(8) -0.6603(5) 0.2638(6) 0.064(3) Uani 1 1 d . . . H71A H 0.1045 -0.6770 0.2251 0.077 Uiso 1 1 calc R . . H71B H 0.0952 -0.6552 0.2910 0.077 Uiso 1 1 calc R . . C72 C 0.1944(11) -0.7089(6) 0.2687(8) 0.108(6) Uani 1 1 d . . . H72A H 0.1428 -0.7513 0.2606 0.162 Uiso 1 1 calc R . . H72B H 0.2319 -0.6927 0.3072 0.162 Uiso 1 1 calc R . . H72C H 0.2415 -0.7142 0.2415 0.162 Uiso 1 1 calc R . . C73 C 0.5435(8) 0.3715(4) -0.0245(4) 0.041(2) Uani 1 1 d . . . H73A H 0.5955 0.3564 -0.0455 0.049 Uiso 1 1 calc R . . H73B H 0.5066 0.3882 -0.0473 0.049 Uiso 1 1 calc R . . C74 C 0.4708(6) 0.3153(4) -0.0161(4) 0.031(2) Uani 1 1 d . . . C75 C 0.4189(8) 0.2566(5) -0.0622(4) 0.049(3) Uani 1 1 d . . . H75A H 0.4318 0.2516 -0.0994 0.058 Uiso 1 1 calc R . . C76 C 0.3491(8) 0.2061(5) -0.0535(5) 0.053(3) Uani 1 1 d . . . H76A H 0.3161 0.1657 -0.0842 0.064 Uiso 1 1 calc R . . C77 C 0.3276(7) 0.2155(5) 0.0020(4) 0.041(2) Uani 1 1 d . . . C78 C 0.3837(7) 0.2737(4) 0.0459(4) 0.037(2) Uani 1 1 d . . . H78A H 0.3726 0.2795 0.0835 0.044 Uiso 1 1 calc R . . C79 C 0.2518(8) 0.1621(5) 0.0109(5) 0.048(3) Uani 1 1 d . . . C80 C 0.1669(11) 0.1248(7) 0.0782(6) 0.096(2) Uani 1 1 d D . . H80A H 0.1869 0.0851 0.0732 0.116 Uiso 1 1 calc R . . H80B H 0.1026 0.1116 0.0522 0.116 Uiso 1 1 calc R . . C81 C 0.1533(11) 0.1557(7) 0.1374(6) 0.096(2) Uani 1 1 d D . . H81A H 0.1058 0.1231 0.1481 0.145 Uiso 1 1 calc R . . H81B H 0.1261 0.1919 0.1409 0.145 Uiso 1 1 calc R . . H81C H 0.2189 0.1727 0.1625 0.145 Uiso 1 1 calc R . . C82 C 0.4464(7) 0.5203(4) 0.1333(4) 0.039(2) Uani 1 1 d . . . H82A H 0.4137 0.5230 0.1672 0.047 Uiso 1 1 calc R . . H82B H 0.4180 0.5432 0.1131 0.047 Uiso 1 1 calc R . . C83 C 0.5593(7) 0.5528(4) 0.1511(3) 0.033(2) Uani 1 1 d . . . C84 C 0.6005(8) 0.6210(5) 0.1747(4) 0.045(2) Uani 1 1 d . . . H84A H 0.5573 0.6476 0.1802 0.054 Uiso 1 1 calc R . . C85 C 0.7064(8) 0.6503(4) 0.1904(4) 0.046(3) Uani 1 1 d . . . H85A H 0.7359 0.6967 0.2061 0.056 Uiso 1 1 calc R . . C86 C 0.7668(7) 0.6090(4) 0.1821(4) 0.035(2) Uani 1 1 d . . . C87 C 0.7207(7) 0.5410(4) 0.1589(4) 0.033(2) Uani 1 1 d . . . H87A H 0.7620 0.5132 0.1535 0.039 Uiso 1 1 calc R . . C88 C 0.8808(8) 0.6393(5) 0.1978(4) 0.048(3) Uani 1 1 d . . . C89 C 1.0389(11) 0.6184(7) 0.2068(7) 0.096(2) Uani 1 1 d . . . H89A H 1.0685 0.6467 0.1863 0.116 Uiso 1 1 calc R . . H89B H 1.0601 0.6440 0.2481 0.116 Uiso 1 1 calc R . . C90 C 1.0716(11) 0.5590(7) 0.1895(6) 0.096(2) Uani 1 1 d . . . H90A H 1.1458 0.5720 0.1981 0.145 Uiso 1 1 calc R . . H90B H 1.0490 0.5340 0.1487 0.145 Uiso 1 1 calc R . . H90C H 1.0416 0.5316 0.2102 0.145 Uiso 1 1 calc R . . C91 C 0.5193(9) 0.2939(5) 0.2804(4) 0.055(3) Uani 1 1 d . . . H91A H 0.4546 0.3014 0.2903 0.066 Uiso 1 1 calc R . . H91B H 0.5450 0.2774 0.3075 0.066 Uiso 1 1 calc R . . C92 C 0.4995(7) 0.2426(5) 0.2213(4) 0.041(2) Uani 1 1 d . . . C93 C 0.4331(10) 0.1801(6) 0.2076(4) 0.076(4) Uani 1 1 d . . . H93A H 0.3993 0.1689 0.2357 0.091 Uiso 1 1 calc R . . C94 C 0.4162(9) 0.1341(5) 0.1534(5) 0.067(4) Uani 1 1 d . . . H94A H 0.3716 0.0909 0.1442 0.080 Uiso 1 1 calc R . . C95 C 0.4645(7) 0.1509(4) 0.1121(4) 0.040(2) Uani 1 1 d . . . C96 C 0.5294(6) 0.2159(4) 0.1294(4) 0.035(2) Uani 1 1 d . . . H96A H 0.5632 0.2287 0.1020 0.042 Uiso 1 1 calc R . . C97 C 0.4477(8) 0.1049(5) 0.0518(4) 0.047(3) Uani 1 1 d . . . C98 C 0.3460(11) 0.0044(6) -0.0202(6) 0.100(3) Uani 1 1 d . . . H98A H 0.3941 -0.0212 -0.0283 0.120 Uiso 1 1 calc R . . H98B H 0.3496 0.0282 -0.0462 0.120 Uiso 1 1 calc R . . C99 C 0.2390(11) -0.0405(6) -0.0279(6) 0.100(3) Uani 1 1 d . . . H99A H 0.2192 -0.0730 -0.0669 0.149 Uiso 1 1 calc R . . H99B H 0.1922 -0.0146 -0.0202 0.149 Uiso 1 1 calc R . . H99C H 0.2365 -0.0632 -0.0015 0.149 Uiso 1 1 calc R . . C100 C 0.8562(7) 0.3835(5) 0.2534(5) 0.054(3) Uani 1 1 d . . . H10C H 0.9069 0.3824 0.2276 0.065 Uiso 1 1 calc R . . H10D H 0.8839 0.3773 0.2869 0.065 Uiso 1 1 calc R . . C101 C 0.8381(6) 0.4501(4) 0.2724(3) 0.032(2) Uani 1 1 d . . . C102 C 0.9164(7) 0.5060(4) 0.3021(4) 0.039(2) Uani 1 1 d . . . H10E H 0.9818 0.5037 0.3118 0.046 Uiso 1 1 calc R . . C103 C 0.8996(7) 0.5663(4) 0.3179(4) 0.037(2) Uani 1 1 d . . . H10F H 0.9538 0.6057 0.3374 0.044 Uiso 1 1 calc R . . C104 C 0.7995(6) 0.5684(4) 0.3046(3) 0.0251(18) Uani 1 1 d . . . C105 C 0.7248(6) 0.5086(4) 0.2752(3) 0.0264(19) Uani 1 1 d . . . H10G H 0.6576 0.5091 0.2670 0.032 Uiso 1 1 calc R . . C106 C 0.7746(7) 0.6304(4) 0.3202(4) 0.039(2) Uani 1 1 d . . . C107 C 0.8459(11) 0.7459(6) 0.3519(7) 0.100(3) Uani 1 1 d . . . H10H H 0.8090 0.7551 0.3844 0.120 Uiso 1 1 calc R . . H10I H 0.8066 0.7483 0.3196 0.120 Uiso 1 1 calc R . . C108 C 0.9495(11) 0.7949(6) 0.3673(7) 0.100(3) Uani 1 1 d . . . H10J H 0.9437 0.8391 0.3780 0.149 Uiso 1 1 calc R . . H10L H 0.9850 0.7856 0.3347 0.149 Uiso 1 1 calc R . . H10M H 0.9876 0.7921 0.3992 0.149 Uiso 1 1 calc R . . C109 C 0.8203(14) -0.4268(8) -0.1216(8) 0.133(4) Uiso 1 1 d D . . H10K H 0.8896 -0.4286 -0.1242 0.199 Uiso 1 1 calc R . . H10N H 0.7739 -0.4610 -0.1553 0.199 Uiso 1 1 calc R . . H10O H 0.7999 -0.4340 -0.0877 0.199 Uiso 1 1 calc R . . C110 C 0.8166(15) -0.3633(9) -0.1182(8) 0.133(4) 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 0.0301(6) 0.0298(6) 0.0365(7) 0.0135(5) 0.0006(5) 0.0040(5) Ni2 0.0312(6) 0.0270(6) 0.0289(6) 0.0075(5) 0.0057(5) 0.0048(5) Ni3 0.0336(6) 0.0260(6) 0.0289(6) 0.0114(5) 0.0084(5) 0.0103(5) Ni4 0.0253(6) 0.0196(5) 0.0268(6) 0.0071(5) 0.0051(4) 0.0080(4) Ni5 0.0300(6) 0.0217(6) 0.0254(6) 0.0069(5) 0.0026(5) 0.0071(5) Ni6 0.0250(6) 0.0219(6) 0.0257(6) 0.0077(5) 0.0031(4) 0.0062(4) Br1 0.0401(5) 0.0326(5) 0.0344(5) 0.0171(4) 0.0039(4) 0.0021(4) Br2 0.0356(5) 0.0368(5) 0.0320(5) 0.0182(4) 0.0072(4) 0.0112(4) Br3 0.0244(4) 0.0271(4) 0.0289(5) 0.0097(4) 0.0054(3) 0.0076(3) Br4 0.0280(5) 0.0282(5) 0.0322(5) 0.0121(4) 0.0028(4) 0.0101(4) Br5 0.0315(5) 0.0253(4) 0.0292(5) 0.0099(4) 0.0104(4) 0.0108(4) Br6 0.0274(4) 0.0299(5) 0.0274(5) 0.0091(4) 0.0062(4) 0.0115(4) Br7 0.0564(6) 0.0348(5) 0.0406(6) 0.0176(4) -0.0080(5) 0.0042(5) Br8 0.0767(8) 0.0426(6) 0.0429(6) 0.0208(5) -0.0071(5) 0.0130(5) Br9 0.0690(8) 0.0563(7) 0.0619(8) 0.0212(6) 0.0211(6) 0.0180(6) Br10 0.1029(11) 0.1166(12) 0.0491(7) 0.0268(7) 0.0331(7) 0.0785(10) Br11 0.0543(13) 0.0645(14) 0.0778(15) 0.0372(11) 0.0148(10) 0.0059(10) Br12 0.116(4) 0.249(8) 0.093(4) -0.003(4) 0.060(3) 0.002(4) Br13 0.0537(11) 0.106(2) 0.0850(15) -0.0129(12) -0.0001(10) -0.0201(10) Br14 0.049(4) 0.205(13) 0.136(7) 0.065(7) -0.005(4) -0.007(5) O1 0.030(4) 0.055(5) 0.099(6) 0.035(4) 0.025(4) 0.010(3) O2 0.086(7) 0.057(6) 0.124(8) -0.014(6) -0.003(6) 0.030(5) O3 0.117(8) 0.068(6) 0.063(6) 0.010(5) 0.025(5) 0.045(6) O4 0.050(4) 0.051(4) 0.044(4) 0.017(3) -0.007(3) 0.020(3) O5 0.065(5) 0.056(5) 0.047(5) 0.007(4) 0.000(4) 0.023(4) O6 0.086(6) 0.073(6) 0.043(5) -0.008(4) 0.004(4) 0.043(5) O7 0.043(4) 0.040(4) 0.044(4) 0.004(3) 0.015(3) -0.007(3) O8 0.055(5) 0.043(4) 0.074(5) 0.017(4) 0.029(4) 0.011(4) O9 0.080(5) 0.035(4) 0.055(5) 0.003(4) 0.036(4) 0.009(4) O10 0.043(4) 0.031(3) 0.045(4) 0.009(3) 0.001(3) 0.015(3) O11 0.065(5) 0.042(4) 0.057(5) 0.022(4) 0.000(4) 0.026(4) O12 0.084(6) 0.033(4) 0.068(5) -0.006(4) -0.027(4) 0.021(4) O13 0.052(4) 0.038(4) 0.042(4) 0.019(3) 0.003(3) 0.017(3) O14 0.126(8) 0.061(6) 0.067(6) 0.012(5) 0.003(6) 0.059(6) O15 0.180(10) 0.070(6) 0.078(6) 0.013(5) 0.027(6) 0.097(7) O16 0.041(4) 0.045(4) 0.043(4) 0.018(3) 0.020(3) 0.012(3) O17 0.106(8) 0.038(5) 0.193(12) 0.024(6) -0.015(7) 0.034(5) O18 0.079(6) 0.048(5) 0.070(5) 0.024(4) 0.026(4) 0.042(4) O19 0.045(4) 0.028(3) 0.015(3) 0.005(2) 0.002(3) 0.014(3) O20 0.071(5) 0.050(4) 0.034(4) -0.002(3) -0.012(4) 0.031(4) O21 0.072(5) 0.030(4) 0.055(5) -0.003(3) -0.015(4) 0.027(4) O22 0.033(3) 0.027(3) 0.050(4) 0.017(3) 0.019(3) 0.012(3) O23 0.024(4) 0.033(4) 0.122(7) 0.022(4) 0.017(4) 0.012(3) O24 0.038(4) 0.028(4) 0.093(6) 0.020(4) 0.007(4) 0.011(3) O25 0.049(4) 0.038(4) 0.028(3) 0.016(3) 0.006(3) 0.004(3) O26 0.071(5) 0.042(5) 0.080(6) 0.011(4) -0.033(5) -0.018(4) O27 0.067(5) 0.045(5) 0.072(6) 0.023(4) 0.019(4) -0.009(4) O28 0.042(4) 0.030(3) 0.035(3) 0.008(3) -0.004(3) 0.018(3) O29 0.059(5) 0.035(5) 0.102(7) 0.007(4) 0.012(5) -0.004(4) O30 0.034(4) 0.035(4) 0.050(4) 0.016(3) 0.000(3) -0.006(3) O31 0.046(4) 0.030(3) 0.027(3) 0.004(3) 0.006(3) 0.002(3) O32 0.160(10) 0.056(5) 0.059(6) -0.014(4) 0.070(6) -0.036(6) O33 0.088(6) 0.036(4) 0.050(5) 0.002(4) 0.015(4) -0.014(4) O34 0.036(4) 0.020(3) 0.055(4) 0.011(3) 0.001(3) 0.011(3) O35 0.027(4) 0.044(4) 0.085(6) 0.011(4) 0.000(4) 0.013(3) O36 0.037(4) 0.020(3) 0.088(6) 0.003(3) -0.004(4) 0.006(3) N1 0.044(5) 0.036(5) 0.046(5) 0.019(4) -0.011(4) 0.008(4) N2 0.032(4) 0.043(5) 0.043(5) 0.019(4) 0.010(4) 0.017(4) N3 0.040(5) 0.037(5) 0.031(4) 0.009(4) 0.010(4) 0.012(4) N4 0.028(4) 0.033(4) 0.031(4) 0.011(3) 0.006(3) 0.007(3) N5 0.036(4) 0.034(4) 0.027(4) 0.010(3) 0.007(3) 0.013(3) N6 0.040(5) 0.027(4) 0.036(4) 0.015(3) 0.011(3) 0.012(4) N7 0.029(4) 0.025(4) 0.025(4) 0.008(3) 0.005(3) 0.008(3) N8 0.028(4) 0.021(4) 0.026(4) 0.007(3) 0.008(3) 0.010(3) N9 0.027(4) 0.022(4) 0.032(4) 0.010(3) 0.003(3) 0.006(3) N10 0.045(5) 0.023(4) 0.021(4) 0.011(3) 0.004(3) 0.009(3) N11 0.029(4) 0.023(4) 0.029(4) 0.007(3) 0.008(3) 0.008(3) N12 0.027(4) 0.022(4) 0.025(4) 0.008(3) 0.004(3) 0.011(3) C1 0.032(6) 0.064(8) 0.098(10) 0.060(7) 0.005(6) -0.001(5) C2 0.039(6) 0.037(6) 0.066(7) 0.027(6) -0.014(5) -0.001(5) C3 0.062(8) 0.043(7) 0.073(9) 0.023(7) -0.016(7) -0.010(6) C4 0.077(9) 0.024(6) 0.087(10) -0.003(6) -0.033(8) -0.001(6) C5 0.062(8) 0.041(7) 0.063(8) 0.002(6) -0.013(6) 0.011(6) C6 0.054(7) 0.038(6) 0.043(6) 0.013(5) 0.004(5) 0.010(5) C7 0.080(10) 0.057(9) 0.057(8) -0.008(7) -0.003(7) 0.022(7) C8 0.100(5) 0.084(4) 0.065(4) -0.006(3) 0.011(3) 0.033(4) C9 0.100(5) 0.084(4) 0.065(4) -0.006(3) 0.011(3) 0.033(4) C10 0.046(6) 0.077(8) 0.052(7) 0.022(6) 0.007(5) 0.028(6) C11 0.048(6) 0.048(6) 0.043(6) 0.016(5) 0.011(5) 0.013(5) C12 0.056(7) 0.065(7) 0.054(7) 0.024(6) 0.005(6) 0.039(6) C13 0.065(8) 0.044(6) 0.059(7) 0.017(6) 0.018(6) 0.026(6) C14 0.037(6) 0.037(6) 0.049(6) 0.012(5) 0.006(5) 0.008(5) C15 0.024(5) 0.041(6) 0.049(6) 0.018(5) 0.005(4) 0.012(4) C16 0.049(6) 0.033(6) 0.044(6) 0.008(5) 0.019(5) 0.012(5) C17 0.100(5) 0.084(4) 0.065(4) -0.006(3) 0.011(3) 0.033(4) C18 0.100(5) 0.084(4) 0.065(4) -0.006(3) 0.011(3) 0.033(4) C19 0.052(6) 0.048(6) 0.037(6) 0.011(5) 0.020(5) 0.013(5) C20 0.037(5) 0.039(5) 0.035(5) 0.016(4) 0.014(4) 0.010(4) C21 0.052(7) 0.056(7) 0.038(6) 0.015(5) 0.012(5) 0.015(5) C22 0.059(7) 0.037(6) 0.033(6) 0.007(5) 0.015(5) 0.008(5) C23 0.042(6) 0.029(5) 0.032(5) 0.003(4) 0.010(4) 0.009(4) C24 0.025(5) 0.033(5) 0.032(5) 0.011(4) 0.010(4) -0.001(4) C25 0.064(7) 0.037(6) 0.029(5) 0.006(5) 0.008(5) 0.011(5) C26 0.100(5) 0.084(4) 0.065(4) -0.006(3) 0.011(3) 0.033(4) C27 0.100(5) 0.084(4) 0.065(4) -0.006(3) 0.011(3) 0.033(4) C28 0.041(6) 0.040(6) 0.067(7) 0.021(5) 0.006(5) 0.018(5) C29 0.027(5) 0.039(5) 0.037(5) 0.016(5) 0.003(4) 0.005(4) C30 0.040(6) 0.028(5) 0.044(6) 0.017(5) -0.008(4) 0.006(4) C31 0.040(6) 0.042(6) 0.033(5) 0.010(5) -0.006(4) 0.002(5) C32 0.040(5) 0.031(5) 0.030(5) 0.008(4) 0.010(4) 0.011(4) C33 0.028(5) 0.025(5) 0.034(5) 0.012(4) 0.006(4) 0.003(4) C34 0.036(5) 0.030(5) 0.052(6) 0.017(5) 0.016(5) 0.005(4) C35 0.079(9) 0.031(6) 0.078(9) 0.003(6) 0.000(7) 0.023(6) C36 0.142(14) 0.028(7) 0.108(12) -0.008(7) -0.058(10) 0.021(8) C37 0.046(6) 0.045(6) 0.041(6) 0.017(5) 0.002(5) 0.015(5) C38 0.036(5) 0.033(5) 0.038(6) 0.012(4) 0.013(4) 0.009(4) C39 0.051(7) 0.046(6) 0.036(6) 0.003(5) 0.005(5) 0.007(5) C40 0.061(7) 0.032(6) 0.041(6) 0.001(5) 0.016(5) 0.014(5) C41 0.048(6) 0.035(6) 0.047(6) 0.012(5) 0.022(5) 0.017(5) C42 0.042(5) 0.029(5) 0.028(5) 0.008(4) 0.007(4) 0.013(4) C43 0.082(9) 0.035(6) 0.066(8) 0.011(6) 0.026(7) 0.024(6) C44 0.099(6) 0.060(5) 0.129(7) 0.003(4) -0.014(5) 0.034(4) C45 0.099(6) 0.060(5) 0.129(7) 0.003(4) -0.014(5) 0.034(4) C46 0.032(6) 0.054(7) 0.064(7) 0.029(6) 0.019(5) -0.001(5) C47 0.052(6) 0.034(5) 0.027(5) 0.013(4) 0.000(4) 0.001(5) C48 0.057(7) 0.042(6) 0.055(7) 0.021(5) -0.003(6) -0.001(6) C49 0.077(9) 0.032(6) 0.056(7) 0.021(5) -0.005(6) 0.006(6) C50 0.078(8) 0.021(5) 0.040(6) 0.012(4) -0.002(5) 0.016(5) C51 0.059(6) 0.026(5) 0.027(5) 0.011(4) 0.004(4) 0.013(5) C52 0.080(9) 0.033(6) 0.073(9) 0.006(6) -0.012(7) 0.022(6) C53 0.130(14) 0.084(11) 0.139(14) 0.051(10) 0.045(12) 0.086(11) C54 0.117(13) 0.126(14) 0.148(15) 0.099(13) 0.087(12) 0.084(12) C55 0.048(6) 0.043(6) 0.034(5) 0.017(5) 0.003(4) 0.020(5) C56 0.031(5) 0.027(5) 0.034(5) 0.012(4) 0.002(4) 0.008(4) C57 0.064(7) 0.032(5) 0.029(5) 0.007(4) 0.003(5) 0.026(5) C58 0.066(7) 0.033(5) 0.039(6) 0.011(5) 0.020(5) 0.031(5) C59 0.027(5) 0.020(4) 0.037(5) 0.011(4) 0.004(4) 0.007(4) C60 0.036(5) 0.028(5) 0.034(5) 0.017(4) 0.000(4) 0.011(4) C61 0.039(6) 0.030(5) 0.044(6) 0.012(5) 0.008(5) 0.007(4) C62 0.099(6) 0.060(5) 0.129(7) 0.003(4) -0.014(5) 0.034(4) C63 0.099(6) 0.060(5) 0.129(7) 0.003(4) -0.014(5) 0.034(4) C64 0.023(5) 0.040(6) 0.054(6) 0.012(5) 0.010(4) 0.006(4) C65 0.025(5) 0.028(5) 0.025(5) 0.004(4) 0.008(4) 0.006(4) C66 0.025(5) 0.034(5) 0.044(6) 0.004(4) 0.010(4) 0.016(4) C67 0.041(6) 0.027(5) 0.045(6) 0.004(4) 0.007(4) 0.021(4) C68 0.021(4) 0.025(5) 0.037(5) 0.006(4) 0.003(4) 0.007(4) C69 0.026(5) 0.024(5) 0.029(5) 0.004(4) 0.002(4) 0.009(4) C70 0.040(6) 0.022(5) 0.052(6) 0.005(4) 0.008(5) 0.015(4) C71 0.053(7) 0.038(6) 0.105(10) 0.033(7) 0.021(7) 0.010(5) C72 0.080(10) 0.049(8) 0.191(17) 0.043(10) -0.006(11) 0.023(7) C73 0.061(7) 0.039(6) 0.020(5) 0.006(4) 0.009(4) 0.018(5) C74 0.027(5) 0.033(5) 0.034(5) 0.012(4) 0.009(4) 0.015(4) C75 0.059(7) 0.048(6) 0.024(5) -0.001(5) -0.005(5) 0.015(5) C76 0.051(7) 0.028(6) 0.058(7) 0.000(5) -0.013(5) 0.005(5) C77 0.040(6) 0.034(5) 0.034(6) 0.000(4) -0.011(4) 0.010(4) C78 0.033(5) 0.035(5) 0.036(5) 0.009(4) -0.001(4) 0.009(4) C79 0.040(6) 0.036(6) 0.055(7) 0.016(5) -0.009(5) -0.001(5) C80 0.090(5) 0.084(5) 0.097(5) 0.043(5) 0.020(4) -0.011(4) C81 0.090(5) 0.084(5) 0.097(5) 0.043(5) 0.020(4) -0.011(4) C82 0.044(6) 0.037(5) 0.037(5) 0.010(4) 0.003(4) 0.019(5) C83 0.054(6) 0.024(5) 0.019(4) 0.004(4) 0.000(4) 0.016(4) C84 0.059(7) 0.035(6) 0.042(6) 0.012(5) 0.008(5) 0.020(5) C85 0.067(7) 0.020(5) 0.044(6) 0.010(4) 0.012(5) 0.004(5) C86 0.046(6) 0.025(5) 0.028(5) 0.005(4) 0.003(4) 0.007(4) C87 0.034(5) 0.023(5) 0.031(5) 0.008(4) -0.005(4) 0.001(4) C88 0.058(7) 0.029(6) 0.041(6) 0.012(5) -0.001(5) -0.007(5) C89 0.090(5) 0.084(5) 0.097(5) 0.043(5) 0.020(4) -0.011(4) C90 0.090(5) 0.084(5) 0.097(5) 0.043(5) 0.020(4) -0.011(4) C91 0.068(8) 0.051(7) 0.034(6) 0.016(5) 0.018(5) 0.000(6) C92 0.041(6) 0.039(6) 0.028(5) 0.011(4) 0.002(4) -0.007(4) C93 0.094(10) 0.071(8) 0.027(6) 0.018(6) 0.016(6) -0.027(7) C94 0.085(9) 0.044(7) 0.046(7) 0.016(6) 0.017(6) -0.017(6) C95 0.041(6) 0.023(5) 0.049(6) 0.013(4) 0.014(5) 0.000(4) C96 0.032(5) 0.035(5) 0.041(6) 0.020(5) 0.011(4) 0.008(4) C97 0.061(7) 0.025(5) 0.046(6) 0.008(5) 0.015(5) 0.006(5) C98 0.106(6) 0.039(4) 0.113(6) 0.001(4) -0.007(5) 0.002(3) C99 0.106(6) 0.039(4) 0.113(6) 0.001(4) -0.007(5) 0.002(3) C100 0.031(6) 0.033(6) 0.089(9) 0.014(6) -0.002(5) 0.008(4) C101 0.029(5) 0.035(5) 0.026(5) 0.003(4) 0.000(4) 0.014(4) C102 0.021(5) 0.035(5) 0.056(6) 0.012(5) 0.003(4) 0.011(4) C103 0.026(5) 0.031(5) 0.043(6) 0.007(4) 0.001(4) 0.004(4) C104 0.027(5) 0.022(4) 0.021(4) 0.004(4) -0.002(3) 0.007(4) C105 0.025(5) 0.026(5) 0.028(5) 0.009(4) 0.000(4) 0.011(4) C106 0.030(5) 0.036(6) 0.037(5) -0.002(4) 0.001(4) 0.013(4) C107 0.106(6) 0.039(4) 0.113(6) 0.001(4) -0.007(5) 0.002(3) C108 0.106(6) 0.039(4) 0.113(6) 0.001(4) -0.007(5) 0.002(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 O1 2.063(6) . ? Ni1 N2 2.064(7) . ? Ni1 O4 2.069(6) . ? Ni1 N1 2.083(8) . ? Ni1 Br1 2.5437(14) . ? Ni1 Br2 2.5520(14) . ? Ni2 N3 2.061(7) . ? Ni2 O7 2.062(6) . ? Ni2 N4 2.076(7) . ? Ni2 O10 2.083(6) . ? Ni2 Br2 2.5540(14) . ? Ni2 Br1 2.5923(14) . ? Ni3 O13 2.032(6) . ? Ni3 N6 2.058(7) . ? Ni3 N5 2.067(7) . ? Ni3 O16 2.070(6) . ? Ni3 Br3 2.5609(13) . ? Ni3 Br4 2.5753(13) . ? Ni4 O19 2.049(5) . ? Ni4 N7 2.066(7) . ? Ni4 O22 2.066(6) . ? Ni4 N8 2.067(6) . ? Ni4 Br4 2.5525(13) . ? Ni4 Br3 2.5648(13) . ? Ni5 O28 2.054(6) . ? Ni5 O25 2.058(6) . ? Ni5 N10 2.079(7) . ? Ni5 N9 2.079(7) . ? Ni5 Br6 2.5565(13) . ? Ni5 Br5 2.5641(13) . ? Ni6 N12 2.041(6) . ? Ni6 O34 2.060(6) . ? Ni6 N11 2.068(7) . ? Ni6 O31 2.070(6) . ? Ni6 Br6 2.5536(13) . ? Ni6 Br5 2.5551(13) . ? O1 C1 1.368(12) . ? O1 HO1 0.8496 . ? O2 C7 1.206(13) . ? O3 C7 1.322(16) . ? O3 C8 1.478(15) . ? O4 C10 1.392(11) . ? O4 HO4 0.8473 . ? O5 C16 1.197(12) . ? O6 C16 1.343(11) . ? O6 C17 1.454(14) . ? O7 C19 1.409(10) . ? O7 HO7 0.8501 . ? O8 C25 1.200(11) . ? O9 C25 1.354(11) . ? O9 C26 1.451(15) . ? O10 C28 1.410(11) . ? O10 HO10 0.8513 . ? O11 C34 1.225(11) . ? O12 C34 1.316(11) . ? O12 C35 1.466(12) . ? O13 C37 1.400(11) . ? O13 HO13 0.8508 . ? O14 C43 1.198(14) . ? O15 C43 1.343(13) . ? O15 C44 1.442(13) . ? O16 C46 1.425(11) . ? O16 HO16 0.8494 . ? O17 C52 1.218(13) . ? O18 C52 1.339(14) . ? O18 C53 1.438(14) . ? O19 C55 1.432(10) . ? O19 HO19 0.8501 . ? O20 C61 1.197(11) . ? O21 C61 1.341(11) . ? O21 C62 1.445(15) . ? O22 C64 1.413(10) . ? O22 HO22 0.8503 . ? O23 C70 1.190(10) . ? O24 C70 1.309(10) . ? O24 C71 1.452(11) . ? O25 C73 1.398(10) . ? O25 HO25 0.8529 . ? O26 C79 1.218(11) . ? O27 C79 1.329(12) . ? O27 C80 1.452(11) . ? O28 C82 1.440(10) . ? O28 HO28 0.8507 . ? O29 C88 1.191(11) . ? O30 C88 1.324(12) . ? O30 C89 1.468(15) . ? O31 C91 1.395(11) . ? O31 HO31 0.8493 . ? O32 C97 1.193(11) . ? O33 C97 1.304(11) . ? O33 C98 1.447(14) . ? O34 C100 1.429(11) . ? O34 HO34 0.8507 . ? O35 C106 1.182(10) . ? O36 C106 1.311(11) . ? O36 C107 1.421(14) . ? O37 H137 0.8499 . ? O37 H237 0.8499 . ? O38 H138 0.8500 . ? O38 H238 0.8499 . ? N1 C6 1.333(12) . ? N1 C2 1.333(12) . ? N2 C11 1.342(12) . ? N2 C15 1.342(11) . ? N3 C20 1.348(11) . ? N3 C24 1.381(11) . ? N4 C33 1.325(10) . ? N4 C29 1.364(11) . ? N5 C42 1.328(11) . ? N5 C38 1.347(11) . ? N6 C51 1.316(11) . ? N6 C47 1.353(11) . ? N7 C56 1.332(10) . ? N7 C60 1.354(10) . ? N8 C65 1.330(10) . ? N8 C69 1.361(10) . ? N9 C74 1.336(10) . ? N9 C78 1.363(11) . ? N10 C83 1.332(10) . ? N10 C87 1.350(11) . ? N11 C96 1.323(10) . ? N11 C92 1.331(11) . ? N12 C101 1.349(10) . ? N12 C105 1.358(10) . ? N13 C110 1.202(14) . ? C1 C2 1.519(15) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C2 C3 1.384(15) . ? C3 C4 1.374(17) . ? C3 H3A 0.9400 . ? C4 C5 1.401(17) . ? C4 H4A 0.9400 . ? C5 C6 1.419(14) . ? C5 C7 1.448(17) . ? C6 H6A 0.9400 . ? C8 C9 1.458(18) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C9 H9C 0.9700 . ? C10 C11 1.525(14) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C11 C12 1.365(14) . ? C12 C13 1.382(14) . ? C12 H12A 0.9400 . ? C13 C14 1.376(14) . ? C13 H13A 0.9400 . ? C14 C15 1.381(13) . ? C14 C16 1.496(14) . ? C15 H15A 0.9400 . ? C17 C18 1.533(17) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C18 H18C 0.9700 . ? C19 C20 1.512(13) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C20 C21 1.368(13) . ? C21 C22 1.384(13) . ? C21 H21A 0.9400 . ? C22 C23 1.374(12) . ? C22 H22A 0.9400 . ? C23 C24 1.366(11) . ? C23 C25 1.484(13) . ? C24 H24A 0.9400 . ? C26 C27 1.480(16) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C27 H27C 0.9700 . ? C28 C29 1.490(12) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C29 C30 1.345(12) . ? C30 C31 1.368(12) . ? C30 H30A 0.9400 . ? C31 C32 1.407(13) . ? C31 H31A 0.9400 . ? C32 C33 1.372(11) . ? C32 C34 1.515(13) . ? C33 H33A 0.9400 . ? C35 C36 1.454(15) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C36 H36C 0.9700 . ? C37 C38 1.486(13) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C38 C39 1.373(12) . ? C39 C40 1.394(14) . ? C39 H39A 0.9400 . ? C40 C41 1.387(14) . ? C40 H40A 0.9400 . ? C41 C42 1.385(12) . ? C41 C43 1.479(16) . ? C42 H42A 0.9400 . ? C44 C45 1.422(14) . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? C45 H45C 0.9700 . ? C46 C47 1.491(14) . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C47 C48 1.371(13) . ? C48 C49 1.321(15) . ? C48 H48A 0.9400 . ? C49 C50 1.387(15) . ? C49 H49A 0.9400 . ? C50 C51 1.395(12) . ? C50 C52 1.493(15) . ? C51 H51A 0.9400 . ? C53 C54 1.429(19) . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C54 H54A 0.9700 . ? C54 H54B 0.9700 . ? C54 H54C 0.9700 . ? C55 C56 1.495(12) . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C56 C57 1.395(11) . ? C57 C58 1.372(12) . ? C57 H57A 0.9400 . ? C58 C59 1.393(12) . ? C58 H58A 0.9400 . ? C59 C60 1.379(11) . ? C59 C61 1.479(12) . ? C60 H60A 0.9400 . ? C62 C63 1.497(18) . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C63 H63A 0.9700 . ? C63 H63B 0.9700 . ? C63 H63C 0.9700 . ? C64 C65 1.488(11) . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C65 C66 1.391(11) . ? C66 C67 1.402(12) . ? C66 H66A 0.9400 . ? C67 C68 1.364(11) . ? C67 H67A 0.9400 . ? C68 C69 1.387(11) . ? C68 C70 1.501(12) . ? C69 H69A 0.9400 . ? C71 C72 1.493(15) . ? C71 H71A 0.9800 . ? C71 H71B 0.9800 . ? C72 H72A 0.9700 . ? C72 H72B 0.9700 . ? C72 H72C 0.9700 . ? C73 C74 1.477(12) . ? C73 H73A 0.9800 . ? C73 H73B 0.9800 . ? C74 C75 1.394(12) . ? C75 C76 1.370(14) . ? C75 H75A 0.9400 . ? C76 C77 1.403(14) . ? C76 H76A 0.9400 . ? C77 C78 1.375(12) . ? C77 C79 1.461(14) . ? C78 H78A 0.9400 . ? C80 C81 1.461(13) . ? C80 H80A 0.9800 . ? C80 H80B 0.9800 . ? C81 H81A 0.9700 . ? C81 H81B 0.9700 . ? C81 H81C 0.9700 . ? C82 C83 1.490(13) . ? C82 H82A 0.9800 . ? C82 H82B 0.9800 . ? C83 C84 1.381(12) . ? C84 C85 1.393(14) . ? C84 H84A 0.9400 . ? C85 C86 1.385(13) . ? C85 H85A 0.9400 . ? C86 C87 1.385(11) . ? C86 C88 1.497(13) . ? C87 H87A 0.9400 . ? C89 C90 1.467(19) . ? C89 H89A 0.9800 . ? C89 H89B 0.9800 . ? C90 H90A 0.9700 . ? C90 H90B 0.9700 . ? C90 H90C 0.9700 . ? C91 C92 1.492(13) . ? C91 H91A 0.9800 . ? C91 H91B 0.9800 . ? C92 C93 1.370(13) . ? C93 C94 1.361(14) . ? C93 H93A 0.9400 . ? C94 C95 1.377(13) . ? C94 H94A 0.9400 . ? C95 C96 1.394(12) . ? C95 C97 1.477(13) . ? C96 H96A 0.9400 . ? C98 C99 1.500(18) . ? C98 H98A 0.9800 . ? C98 H98B 0.9800 . ? C99 H99A 0.9700 . ? C99 H99B 0.9700 . ? C99 H99C 0.9700 . ? C100 C101 1.512(12) . ? C100 H10C 0.9800 . ? C100 H10D 0.9800 . ? C101 C102 1.352(12) . ? C102 C103 1.372(12) . ? C102 H10E 0.9400 . ? C103 C104 1.416(12) . ? C103 H10F 0.9400 . ? C104 C105 1.375(11) . ? C104 C106 1.464(12) . ? C105 H10G 0.9400 . ? C107 C108 1.477(18) . ? C107 H10H 0.9800 . ? C107 H10I 0.9800 . ? C108 H10J 0.9700 . ? C108 H10L 0.9700 . ? C108 H10M 0.9700 . ? C109 C110 1.428(15) . ? C109 H10K 0.9700 . ? C109 H10N 0.9700 . ? C109 H10O 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 O1 Ni1 N2 89.1(3) . . ? O1 Ni1 O4 89.5(3) . . ? N2 Ni1 O4 78.6(3) . . ? O1 Ni1 N1 77.7(3) . . ? N2 Ni1 N1 164.8(3) . . ? O4 Ni1 N1 93.6(3) . . ? O1 Ni1 Br1 176.1(2) . . ? N2 Ni1 Br1 94.6(2) . . ? O4 Ni1 Br1 92.36(19) . . ? N1 Ni1 Br1 98.8(2) . . ? O1 Ni1 Br2 91.8(2) . . ? N2 Ni1 Br2 99.5(2) . . ? O4 Ni1 Br2 177.68(19) . . ? N1 Ni1 Br2 88.6(2) . . ? Br1 Ni1 Br2 86.41(4) . . ? N3 Ni2 O7 78.9(3) . . ? N3 Ni2 N4 162.1(3) . . ? O7 Ni2 N4 90.7(3) . . ? N3 Ni2 O10 87.8(3) . . ? O7 Ni2 O10 92.8(3) . . ? N4 Ni2 O10 78.2(3) . . ? N3 Ni2 Br2 98.6(2) . . ? O7 Ni2 Br2 172.8(2) . . ? N4 Ni2 Br2 93.40(19) . . ? O10 Ni2 Br2 93.89(17) . . ? N3 Ni2 Br1 94.0(2) . . ? O7 Ni2 Br1 88.0(2) . . ? N4 Ni2 Br1 100.2(2) . . ? O10 Ni2 Br1 178.14(17) . . ? Br2 Ni2 Br1 85.35(4) . . ? O13 Ni3 N6 88.8(3) . . ? O13 Ni3 N5 79.9(3) . . ? N6 Ni3 N5 162.4(3) . . ? O13 Ni3 O16 94.8(3) . . ? N6 Ni3 O16 79.5(3) . . ? N5 Ni3 O16 88.0(3) . . ? O13 Ni3 Br3 176.69(19) . . ? N6 Ni3 Br3 92.7(2) . . ? N5 Ni3 Br3 99.4(2) . . ? O16 Ni3 Br3 88.42(18) . . ? O13 Ni3 Br4 89.14(18) . . ? N6 Ni3 Br4 99.9(2) . . ? N5 Ni3 Br4 93.4(2) . . ? O16 Ni3 Br4 176.03(18) . . ? Br3 Ni3 Br4 87.69(4) . . ? O19 Ni4 N7 79.7(2) . . ? O19 Ni4 O22 92.3(2) . . ? N7 Ni4 O22 94.7(2) . . ? O19 Ni4 N8 90.2(2) . . ? N7 Ni4 N8 167.9(3) . . ? O22 Ni4 N8 79.1(2) . . ? O19 Ni4 Br4 177.36(16) . . ? N7 Ni4 Br4 98.02(19) . . ? O22 Ni4 Br4 89.13(17) . . ? N8 Ni4 Br4 92.25(18) . . ? O19 Ni4 Br3 90.56(16) . . ? N7 Ni4 Br3 88.77(18) . . ? O22 Ni4 Br3 175.81(17) . . ? N8 Ni4 Br3 97.92(18) . . ? Br4 Ni4 Br3 88.09(4) . . ? O28 Ni5 O25 94.2(2) . . ? O28 Ni5 N10 78.7(3) . . ? O25 Ni5 N10 87.7(2) . . ? O28 Ni5 N9 90.1(2) . . ? O25 Ni5 N9 77.7(3) . . ? N10 Ni5 N9 160.9(3) . . ? O28 Ni5 Br6 88.37(17) . . ? O25 Ni5 Br6 176.84(18) . . ? N10 Ni5 Br6 94.67(18) . . ? N9 Ni5 Br6 100.49(19) . . ? O28 Ni5 Br5 174.77(17) . . ? O25 Ni5 Br5 90.92(18) . . ? N10 Ni5 Br5 100.3(2) . . ? N9 Ni5 Br5 92.13(18) . . ? Br6 Ni5 Br5 86.57(4) . . ? N12 Ni6 O34 79.4(2) . . ? N12 Ni6 N11 163.6(3) . . ? O34 Ni6 N11 89.5(2) . . ? N12 Ni6 O31 89.0(2) . . ? O34 Ni6 O31 92.1(2) . . ? N11 Ni6 O31 79.3(2) . . ? N12 Ni6 Br6 100.13(18) . . ? O34 Ni6 Br6 177.58(18) . . ? N11 Ni6 Br6 91.45(19) . . ? O31 Ni6 Br6 90.23(17) . . ? N12 Ni6 Br5 92.14(18) . . ? O34 Ni6 Br5 90.82(18) . . ? N11 Ni6 Br5 100.15(19) . . ? O31 Ni6 Br5 176.98(18) . . ? Br6 Ni6 Br5 86.83(4) . . ? Ni1 Br1 Ni2 93.54(4) . . ? Ni1 Br2 Ni2 94.26(4) . . ? Ni3 Br3 Ni4 91.91(4) . . ? Ni4 Br4 Ni3 91.86(4) . . ? Ni6 Br5 Ni5 92.93(4) . . ? Ni6 Br6 Ni5 93.14(4) . . ? C1 O1 Ni1 113.4(6) . . ? C1 O1 HO1 108.9 . . ? Ni1 O1 HO1 137.2 . . ? C7 O3 C8 119.2(10) . . ? C10 O4 Ni1 115.3(6) . . ? C10 O4 HO4 108.5 . . ? Ni1 O4 HO4 135.3 . . ? C16 O6 C17 116.1(9) . . ? C19 O7 Ni2 113.7(5) . . ? C19 O7 HO7 108.6 . . ? Ni2 O7 HO7 133.2 . . ? C25 O9 C26 118.1(9) . . ? C28 O10 Ni2 116.4(5) . . ? C28 O10 HO10 109.0 . . ? Ni2 O10 HO10 134.4 . . ? C34 O12 C35 116.0(8) . . ? C37 O13 Ni3 115.4(5) . . ? C37 O13 HO13 109.1 . . ? Ni3 O13 HO13 135.5 . . ? C43 O15 C44 115.1(11) . . ? C46 O16 Ni3 112.3(5) . . ? C46 O16 HO16 109.1 . . ? Ni3 O16 HO16 136.0 . . ? C52 O18 C53 118.4(10) . . ? C55 O19 Ni4 115.6(5) . . ? C55 O19 HO19 109.0 . . ? Ni4 O19 HO19 132.2 . . ? C61 O21 C62 118.3(9) . . ? C64 O22 Ni4 113.5(5) . . ? C64 O22 HO22 109.0 . . ? Ni4 O22 HO22 133.0 . . ? C70 O24 C71 118.3(8) . . ? C73 O25 Ni5 118.0(5) . . ? C73 O25 HO25 109.2 . . ? Ni5 O25 HO25 132.8 . . ? C79 O27 C80 117.5(9) . . ? C82 O28 Ni5 115.4(5) . . ? C82 O28 HO28 109.0 . . ? Ni5 O28 HO28 135.1 . . ? C88 O30 C89 115.6(8) . . ? C91 O31 Ni6 115.4(5) . . ? C91 O31 HO31 109.2 . . ? Ni6 O31 HO31 132.4 . . ? C97 O33 C98 117.4(9) . . ? C100 O34 Ni6 116.1(5) . . ? C100 O34 HO34 109.3 . . ? Ni6 O34 HO34 132.4 . . ? C106 O36 C107 118.3(8) . . ? H137 O37 H237 107.7 . . ? H138 O38 H238 107.7 . . ? C6 N1 C2 119.8(9) . . ? C6 N1 Ni1 126.1(7) . . ? C2 N1 Ni1 113.8(7) . . ? C11 N2 C15 117.9(8) . . ? C11 N2 Ni1 115.4(6) . . ? C15 N2 Ni1 126.5(6) . . ? C20 N3 C24 117.9(7) . . ? C20 N3 Ni2 115.7(6) . . ? C24 N3 Ni2 125.6(6) . . ? C33 N4 C29 119.7(7) . . ? C33 N4 Ni2 124.9(6) . . ? C29 N4 Ni2 115.3(6) . . ? C42 N5 C38 119.8(7) . . ? C42 N5 Ni3 125.5(6) . . ? C38 N5 Ni3 114.6(6) . . ? C51 N6 C47 117.7(8) . . ? C51 N6 Ni3 126.8(6) . . ? C47 N6 Ni3 115.3(6) . . ? C56 N7 C60 117.7(7) . . ? C56 N7 Ni4 114.3(5) . . ? C60 N7 Ni4 127.2(5) . . ? C65 N8 C69 119.0(7) . . ? C65 N8 Ni4 114.8(5) . . ? C69 N8 Ni4 126.2(5) . . ? C74 N9 C78 118.9(7) . . ? C74 N9 Ni5 115.8(5) . . ? C78 N9 Ni5 125.3(6) . . ? C83 N10 C87 119.2(7) . . ? C83 N10 Ni5 115.6(6) . . ? C87 N10 Ni5 124.8(6) . . ? C96 N11 C92 118.2(7) . . ? C96 N11 Ni6 126.5(6) . . ? C92 N11 Ni6 115.2(6) . . ? C101 N12 C105 116.0(7) . . ? C101 N12 Ni6 117.2(5) . . ? C105 N12 Ni6 126.8(5) . . ? O1 C1 C2 110.1(8) . . ? O1 C1 H1A 109.6 . . ? C2 C1 H1A 109.6 . . ? O1 C1 H1B 109.6 . . ? C2 C1 H1B 109.6 . . ? H1A C1 H1B 108.1 . . ? N1 C2 C3 122.4(11) . . ? N1 C2 C1 116.0(9) . . ? C3 C2 C1 121.6(10) . . ? C4 C3 C2 117.3(11) . . ? C4 C3 H3A 121.4 . . ? C2 C3 H3A 121.4 . . ? C3 C4 C5 122.8(11) . . ? C3 C4 H4A 118.6 . . ? C5 C4 H4A 118.6 . . ? C4 C5 C6 114.4(11) . . ? C4 C5 C7 122.0(11) . . ? C6 C5 C7 123.4(12) . . ? N1 C6 C5 123.1(10) . . ? N1 C6 H6A 118.5 . . ? C5 C6 H6A 118.5 . . ? O2 C7 O3 121.8(13) . . ? O2 C7 C5 124.8(15) . . ? O3 C7 C5 113.3(11) . . ? C9 C8 O3 109.3(11) . . ? C9 C8 H8A 109.8 . . ? O3 C8 H8A 109.8 . . ? C9 C8 H8B 109.8 . . ? O3 C8 H8B 109.8 . . ? H8A C8 H8B 108.3 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? O4 C10 C11 110.1(8) . . ? O4 C10 H10A 109.6 . . ? C11 C10 H10A 109.6 . . ? O4 C10 H10B 109.6 . . ? C11 C10 H10B 109.6 . . ? H10A C10 H10B 108.2 . . ? N2 C11 C12 121.8(9) . . ? N2 C11 C10 116.4(9) . . ? C12 C11 C10 121.8(10) . . ? C11 C12 C13 120.3(10) . . ? C11 C12 H12A 119.9 . . ? C13 C12 H12A 119.9 . . ? C14 C13 C12 118.4(10) . . ? C14 C13 H13A 120.8 . . ? C12 C13 H13A 120.8 . . ? C13 C14 C15 118.4(9) . . ? C13 C14 C16 124.2(9) . . ? C15 C14 C16 117.3(9) . . ? N2 C15 C14 123.1(9) . . ? N2 C15 H15A 118.4 . . ? C14 C15 H15A 118.4 . . ? O5 C16 O6 124.9(10) . . ? O5 C16 C14 124.8(9) . . ? O6 C16 C14 110.3(9) . . ? O6 C17 C18 105.3(11) . . ? O6 C17 H17A 110.7 . . ? C18 C17 H17A 110.7 . . ? O6 C17 H17B 110.7 . . ? C18 C17 H17B 110.7 . . ? H17A C17 H17B 108.8 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O7 C19 C20 110.2(8) . . ? O7 C19 H19A 109.6 . . ? C20 C19 H19A 109.6 . . ? O7 C19 H19B 109.6 . . ? C20 C19 H19B 109.6 . . ? H19A C19 H19B 108.1 . . ? N3 C20 C21 121.2(9) . . ? N3 C20 C19 115.0(8) . . ? C21 C20 C19 123.8(8) . . ? C20 C21 C22 121.3(9) . . ? C20 C21 H21A 119.4 . . ? C22 C21 H21A 119.4 . . ? C23 C22 C21 117.6(9) . . ? C23 C22 H22A 121.2 . . ? C21 C22 H22A 121.2 . . ? C24 C23 C22 120.3(8) . . ? C24 C23 C25 118.4(8) . . ? C22 C23 C25 121.3(8) . . ? C23 C24 N3 121.7(8) . . ? C23 C24 H24A 119.1 . . ? N3 C24 H24A 119.1 . . ? O8 C25 O9 125.6(9) . . ? O8 C25 C23 125.5(9) . . ? O9 C25 C23 108.9(9) . . ? O9 C26 C27 106.8(12) . . ? O9 C26 H26A 110.4 . . ? C27 C26 H26A 110.4 . . ? O9 C26 H26B 110.4 . . ? C27 C26 H26B 110.4 . . ? H26A C26 H26B 108.6 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? O10 C28 C29 109.9(8) . . ? O10 C28 H28A 109.7 . . ? C29 C28 H28A 109.7 . . ? O10 C28 H28B 109.7 . . ? C29 C28 H28B 109.7 . . ? H28A C28 H28B 108.2 . . ? C30 C29 N4 120.8(8) . . ? C30 C29 C28 122.0(8) . . ? N4 C29 C28 117.2(8) . . ? C29 C30 C31 121.3(9) . . ? C29 C30 H30A 119.3 . . ? C31 C30 H30A 119.3 . . ? C30 C31 C32 117.3(8) . . ? C30 C31 H31A 121.3 . . ? C32 C31 H31A 121.3 . . ? C33 C32 C31 119.4(8) . . ? C33 C32 C34 118.1(8) . . ? C31 C32 C34 122.5(8) . . ? N4 C33 C32 121.4(8) . . ? N4 C33 H33A 119.3 . . ? C32 C33 H33A 119.3 . . ? O11 C34 O12 125.1(9) . . ? O11 C34 C32 123.0(9) . . ? O12 C34 C32 111.8(9) . . ? C36 C35 O12 106.2(9) . . ? C36 C35 H35A 110.5 . . ? O12 C35 H35A 110.5 . . ? C36 C35 H35B 110.5 . . ? O12 C35 H35B 110.5 . . ? H35A C35 H35B 108.7 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? O13 C37 C38 112.5(8) . . ? O13 C37 H37A 109.1 . . ? C38 C37 H37A 109.1 . . ? O13 C37 H37B 109.1 . . ? C38 C37 H37B 109.1 . . ? H37A C37 H37B 107.8 . . ? N5 C38 C39 120.8(9) . . ? N5 C38 C37 116.3(8) . . ? C39 C38 C37 122.8(9) . . ? C38 C39 C40 119.9(9) . . ? C38 C39 H39A 120.0 . . ? C40 C39 H39A 120.0 . . ? C41 C40 C39 118.6(9) . . ? C41 C40 H40A 120.7 . . ? C39 C40 H40A 120.7 . . ? C42 C41 C40 118.3(9) . . ? C42 C41 C43 118.2(9) . . ? C40 C41 C43 123.5(9) . . ? N5 C42 C41 122.5(9) . . ? N5 C42 H42A 118.7 . . ? C41 C42 H42A 118.7 . . ? O14 C43 O15 123.5(11) . . ? O14 C43 C41 125.6(10) . . ? O15 C43 C41 110.6(11) . . ? C45 C44 O15 98.8(12) . . ? C45 C44 H44A 112.0 . . ? O15 C44 H44A 112.0 . . ? C45 C44 H44B 112.0 . . ? O15 C44 H44B 112.0 . . ? H44A C44 H44B 109.7 . . ? C44 C45 H45A 109.5 . . ? C44 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C44 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? O16 C46 C47 111.9(8) . . ? O16 C46 H46A 109.2 . . ? C47 C46 H46A 109.2 . . ? O16 C46 H46B 109.2 . . ? C47 C46 H46B 109.2 . . ? H46A C46 H46B 107.9 . . ? N6 C47 C48 121.2(10) . . ? N6 C47 C46 115.6(8) . . ? C48 C47 C46 123.2(9) . . ? C49 C48 C47 120.8(11) . . ? C49 C48 H48A 119.6 . . ? C47 C48 H48A 119.6 . . ? C48 C49 C50 119.8(10) . . ? C48 C49 H49A 120.1 . . ? C50 C49 H49A 120.1 . . ? C49 C50 C51 116.9(10) . . ? C49 C50 C52 121.6(9) . . ? C51 C50 C52 121.4(10) . . ? N6 C51 C50 123.3(9) . . ? N6 C51 H51A 118.3 . . ? C50 C51 H51A 118.3 . . ? O17 C52 O18 125.4(12) . . ? O17 C52 C50 120.7(12) . . ? O18 C52 C50 113.9(9) . . ? C54 C53 O18 111.4(11) . . ? C54 C53 H53A 109.3 . . ? O18 C53 H53A 109.3 . . ? C54 C53 H53B 109.3 . . ? O18 C53 H53B 109.3 . . ? H53A C53 H53B 108.0 . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? O19 C55 C56 110.5(7) . . ? O19 C55 H55A 109.6 . . ? C56 C55 H55A 109.6 . . ? O19 C55 H55B 109.6 . . ? C56 C55 H55B 109.6 . . ? H55A C55 H55B 108.1 . . ? N7 C56 C57 122.7(8) . . ? N7 C56 C55 118.4(7) . . ? C57 C56 C55 118.9(8) . . ? C58 C57 C56 118.6(8) . . ? C58 C57 H57A 120.7 . . ? C56 C57 H57A 120.7 . . ? C57 C58 C59 119.8(8) . . ? C57 C58 H58A 120.1 . . ? C59 C58 H58A 120.1 . . ? C60 C59 C58 117.7(8) . . ? C60 C59 C61 119.6(8) . . ? C58 C59 C61 122.7(8) . . ? N7 C60 C59 123.4(8) . . ? N7 C60 H60A 118.3 . . ? C59 C60 H60A 118.3 . . ? O20 C61 O21 124.3(9) . . ? O20 C61 C59 125.6(9) . . ? O21 C61 C59 109.9(8) . . ? O21 C62 C63 104.3(12) . . ? O21 C62 H62A 110.9 . . ? C63 C62 H62A 110.9 . . ? O21 C62 H62B 110.9 . . ? C63 C62 H62B 110.9 . . ? H62A C62 H62B 108.9 . . ? C62 C63 H63A 109.5 . . ? C62 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C62 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? O22 C64 C65 110.9(7) . . ? O22 C64 H64A 109.5 . . ? C65 C64 H64A 109.5 . . ? O22 C64 H64B 109.5 . . ? C65 C64 H64B 109.5 . . ? H64A C64 H64B 108.0 . . ? N8 C65 C66 122.2(8) . . ? N8 C65 C64 117.3(7) . . ? C66 C65 C64 120.4(7) . . ? C65 C66 C67 118.3(8) . . ? C65 C66 H66A 120.8 . . ? C67 C66 H66A 120.8 . . ? C68 C67 C66 119.6(8) . . ? C68 C67 H67A 120.2 . . ? C66 C67 H67A 120.2 . . ? C67 C68 C69 119.1(8) . . ? C67 C68 C70 122.1(8) . . ? C69 C68 C70 118.7(7) . . ? N8 C69 C68 121.7(7) . . ? N8 C69 H69A 119.1 . . ? C68 C69 H69A 119.1 . . ? O23 C70 O24 124.5(9) . . ? O23 C70 C68 123.5(8) . . ? O24 C70 C68 111.9(8) . . ? O24 C71 C72 110.3(9) . . ? O24 C71 H71A 109.6 . . ? C72 C71 H71A 109.6 . . ? O24 C71 H71B 109.6 . . ? C72 C71 H71B 109.6 . . ? H71A C71 H71B 108.1 . . ? C71 C72 H72A 109.5 . . ? C71 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? C71 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? O25 C73 C74 110.6(7) . . ? O25 C73 H73A 109.5 . . ? C74 C73 H73A 109.5 . . ? O25 C73 H73B 109.5 . . ? C74 C73 H73B 109.5 . . ? H73A C73 H73B 108.1 . . ? N9 C74 C75 121.0(8) . . ? N9 C74 C73 117.6(7) . . ? C75 C74 C73 121.4(8) . . ? C76 C75 C74 120.2(9) . . ? C76 C75 H75A 119.9 . . ? C74 C75 H75A 119.9 . . ? C75 C76 C77 119.0(9) . . ? C75 C76 H76A 120.5 . . ? C77 C76 H76A 120.5 . . ? C78 C77 C76 117.9(9) . . ? C78 C77 C79 123.1(9) . . ? C76 C77 C79 118.9(9) . . ? N9 C78 C77 122.8(9) . . ? N9 C78 H78A 118.6 . . ? C77 C78 H78A 118.6 . . ? O26 C79 O27 121.3(10) . . ? O26 C79 C77 124.7(10) . . ? O27 C79 C77 114.0(8) . . ? O27 C80 C81 108.1(10) . . ? O27 C80 H80A 110.1 . . ? C81 C80 H80A 110.1 . . ? O27 C80 H80B 110.1 . . ? C81 C80 H80B 110.1 . . ? H80A C80 H80B 108.4 . . ? C80 C81 H81A 109.5 . . ? C80 C81 H81B 109.5 . . ? H81A C81 H81B 109.5 . . ? C80 C81 H81C 109.5 . . ? H81A C81 H81C 109.5 . . ? H81B C81 H81C 109.5 . . ? O28 C82 C83 109.8(7) . . ? O28 C82 H82A 109.7 . . ? C83 C82 H82A 109.7 . . ? O28 C82 H82B 109.7 . . ? C83 C82 H82B 109.7 . . ? H82A C82 H82B 108.2 . . ? N10 C83 C84 121.8(9) . . ? N10 C83 C82 117.3(7) . . ? C84 C83 C82 120.8(8) . . ? C83 C84 C85 119.8(9) . . ? C83 C84 H84A 120.1 . . ? C85 C84 H84A 120.1 . . ? C86 C85 C84 118.0(8) . . ? C86 C85 H85A 121.0 . . ? C84 C85 H85A 121.0 . . ? C87 C86 C85 119.5(9) . . ? C87 C86 C88 121.6(8) . . ? C85 C86 C88 118.9(8) . . ? N10 C87 C86 121.7(8) . . ? N10 C87 H87A 119.1 . . ? C86 C87 H87A 119.1 . . ? O29 C88 O30 124.8(10) . . ? O29 C88 C86 123.8(10) . . ? O30 C88 C86 111.3(8) . . ? C90 C89 O30 105.2(11) . . ? C90 C89 H89A 110.7 . . ? O30 C89 H89A 110.7 . . ? C90 C89 H89B 110.7 . . ? O30 C89 H89B 110.7 . . ? H89A C89 H89B 108.8 . . ? C89 C90 H90A 109.5 . . ? C89 C90 H90B 109.5 . . ? H90A C90 H90B 109.5 . . ? C89 C90 H90C 109.5 . . ? H90A C90 H90C 109.5 . . ? H90B C90 H90C 109.5 . . ? O31 C91 C92 112.4(7) . . ? O31 C91 H91A 109.1 . . ? C92 C91 H91A 109.1 . . ? O31 C91 H91B 109.1 . . ? C92 C91 H91B 109.1 . . ? H91A C91 H91B 107.9 . . ? N11 C92 C93 121.5(8) . . ? N11 C92 C91 117.4(8) . . ? C93 C92 C91 121.1(8) . . ? C94 C93 C92 120.1(9) . . ? C94 C93 H93A 119.9 . . ? C92 C93 H93A 119.9 . . ? C93 C94 C95 119.8(10) . . ? C93 C94 H94A 120.1 . . ? C95 C94 H94A 120.1 . . ? C94 C95 C96 116.3(9) . . ? C94 C95 C97 123.4(9) . . ? C96 C95 C97 120.3(8) . . ? N11 C96 C95 124.0(8) . . ? N11 C96 H96A 118.0 . . ? C95 C96 H96A 118.0 . . ? O32 C97 O33 123.1(10) . . ? O32 C97 C95 122.8(9) . . ? O33 C97 C95 114.0(9) . . ? O33 C98 C99 106.5(12) . . ? O33 C98 H98A 110.4 . . ? C99 C98 H98A 110.4 . . ? O33 C98 H98B 110.4 . . ? C99 C98 H98B 110.4 . . ? H98A C98 H98B 108.6 . . ? C98 C99 H99A 109.5 . . ? C98 C99 H99B 109.5 . . ? H99A C99 H99B 109.5 . . ? C98 C99 H99C 109.5 . . ? H99A C99 H99C 109.5 . . ? H99B C99 H99C 109.5 . . ? O34 C100 C101 111.1(7) . . ? O34 C100 H10C 109.4 . . ? C101 C100 H10C 109.4 . . ? O34 C100 H10D 109.4 . . ? C101 C100 H10D 109.4 . . ? H10C C100 H10D 108.0 . . ? N12 C101 C102 124.1(8) . . ? N12 C101 C100 115.9(7) . . ? C102 C101 C100 119.9(8) . . ? C101 C102 C103 119.4(8) . . ? C101 C102 H10E 120.3 . . ? C103 C102 H10E 120.3 . . ? C102 C103 C104 119.2(8) . . ? C102 C103 H10F 120.4 . . ? C104 C103 H10F 120.4 . . ? C105 C104 C103 116.8(7) . . ? C105 C104 C106 120.4(7) . . ? C103 C104 C106 122.8(7) . . ? N12 C105 C104 124.3(7) . . ? N12 C105 H10G 117.8 . . ? C104 C105 H10G 117.8 . . ? O35 C106 O36 124.3(9) . . ? O35 C106 C104 124.1(8) . . ? O36 C106 C104 111.6(8) . . ? O36 C107 C108 107.7(12) . . ? O36 C107 H10H 110.2 . . ? C108 C107 H10H 110.2 . . ? O36 C107 H10I 110.2 . . ? C108 C107 H10I 110.2 . . ? H10H C107 H10I 108.5 . . ? C107 C108 H10J 109.5 . . ? C107 C108 H10L 109.5 . . ? H10J C108 H10L 109.5 . . ? C107 C108 H10M 109.5 . . ? H10J C108 H10M 109.5 . . ? H10L C108 H10M 109.5 . . ? C110 C109 H10K 109.5 . . ? C110 C109 H10N 109.5 . . ? H10K C109 H10N 109.5 . . ? C110 C109 H10O 109.5 . . ? H10K C109 H10O 109.5 . . ? H10N C109 H10O 109.5 . . ? N13 C110 C109 170(2) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 3.549 _refine_diff_density_min -1.582 _refine_diff_density_rms 0.157 data_Ni(ehmpH)3Br2 _database_code_depnum_ccdc_archive 'CCDC 798247' #TrackingRef 'CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C82 H99 Br6 N9 Ni3 O28' _chemical_formula_weight 2314.29 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 28.336(6) _cell_length_b 8.9991(18) _cell_length_c 21.869(4) _cell_angle_alpha 90.00 _cell_angle_beta 110.33(3) _cell_angle_gamma 90.00 _cell_volume 5229.1(18) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 966 _cell_measurement_theta_min 2.48 _cell_measurement_theta_max 18.65 _exptl_crystal_description Block _exptl_crystal_colour Blue _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.470 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2344 _exptl_absorpt_coefficient_mu 2.899 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.3901 _exptl_absorpt_correction_T_max 0.8012 _exptl_absorpt_process_details 'Sadabs, (Sheldrick 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15506 _diffrn_reflns_av_R_equivalents 0.0518 _diffrn_reflns_av_sigmaI/netI 0.1124 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8943 _reflns_number_gt 6359 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1260P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.012(17) _refine_ls_number_reflns 11503 _refine_ls_number_parameters 541 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.1406 _refine_ls_R_factor_gt 0.0802 _refine_ls_wR_factor_ref 0.2377 _refine_ls_wR_factor_gt 0.1967 _refine_ls_goodness_of_fit_ref 0.992 _refine_ls_restrained_S_all 0.992 _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 0.63412(5) 2.79360(14) 0.96141(6) 0.0353(3) Uani 1 1 d . . . Ni2 Ni 1.0000 1.7171(2) 1.5000 0.0747(8) Uani 1 2 d S . . Br1 Br 0.77405(3) 0.66408(11) 0.92503(4) 0.0360(2) Uani 1 1 d . . . Br2 Br 0.49022(4) 0.98369(13) 0.83938(6) 0.0521(3) Uani 1 1 d . . . Br3A Br 0.86411(10) 2.4788(5) 1.42138(12) 0.0723(14) Uani 0.511(6) 1 d P A 1 Br3B Br 0.87068(13) 2.3504(4) 1.42463(13) 0.0715(13) Uani 0.489(6) 1 d P A 2 O1 O 0.5855(4) 2.9631(10) 0.9577(4) 0.0665(14) Uani 1 1 d . . . HO1 H 0.5618 2.9985 0.9265 0.080 Uiso 1 1 d R . . O2 O 0.7381(5) 2.7528(13) 1.2820(4) 0.093(4) Uani 1 1 d . . . O3 O 0.7632(4) 2.6386(13) 1.2109(4) 0.075(3) Uani 1 1 d . . . O4 O 0.6908(3) 2.9366(7) 0.9593(3) 0.0417(17) Uani 1 1 d . . . HO4 H 0.7154 2.9770 0.9889 0.050 Uiso 1 1 d R . . O5 O 0.5122(3) 2.5700(12) 0.7293(4) 0.068(3) Uani 1 1 d . . . O6 O 0.5236(4) 2.6782(17) 0.6430(4) 0.097(4) Uani 1 1 d . . . O7 O 0.6854(3) 2.6214(10) 0.9779(4) 0.0665(14) Uani 1 1 d . . . HO7 H 0.7173 2.6155 0.9927 0.080 Uiso 1 1 d R . . O8 O 0.4285(2) 2.3797(8) 0.9000(3) 0.0384(16) Uani 1 1 d . . . O9 O 0.4319(3) 2.6274(8) 0.9074(3) 0.0427(17) Uani 1 1 d . . . O10 O 1.0332(3) 1.5367(10) 1.4912(4) 0.0665(14) Uani 1 1 d . B . HO10 H 1.0617 1.4974 1.5161 0.080 Uiso 1 1 d R . . O11 O 0.8552(3) 1.9329(9) 1.2725(4) 0.054(2) Uani 1 1 d . . . O12 O 0.8679(3) 1.8316(10) 1.1852(4) 0.060(2) Uani 1 1 d . . . N1 N 0.6479(3) 2.8298(9) 1.0586(4) 0.037(2) Uani 1 1 d . . . N2 N 0.6216(3) 2.8088(10) 0.8618(4) 0.040(2) Uani 1 1 d . . . N3 N 0.5868(3) 2.6118(9) 0.9502(4) 0.0329(18) Uani 1 1 d . . . N4 N 0.9716(5) 1.6945(11) 1.3995(4) 0.065(3) Uani 1 1 d . B . C1 C 0.5774(5) 2.9927(15) 1.0165(5) 0.0607(19) Uani 1 1 d . . . H1A H 0.5450 2.9484 1.0147 0.073 Uiso 1 1 calc R . . H1B H 0.5753 3.1014 1.0219 0.073 Uiso 1 1 calc R . . C2 C 0.6191(4) 2.9305(12) 1.0740(5) 0.043(3) Uani 1 1 d . . . C3 C 0.6263(5) 2.9717(14) 1.1372(5) 0.048(3) Uani 1 1 d . . . H3 H 0.6059 3.0463 1.1462 0.058 Uiso 1 1 calc R . . C4 C 0.6627(5) 2.9046(16) 1.1858(6) 0.062(4) Uani 1 1 d . . . H4 H 0.6674 2.9287 1.2298 0.074 Uiso 1 1 calc R . . C5 C 0.6938(5) 2.7996(14) 1.1719(5) 0.052(3) Uani 1 1 d . . . C6 C 0.6853(4) 2.7689(13) 1.1080(5) 0.045(3) Uani 1 1 d . . . H6 H 0.7072 2.7007 1.0979 0.054 Uiso 1 1 calc R . . C7 C 0.7337(6) 2.7227(16) 1.2221(6) 0.060(4) Uani 1 1 d . . . C8 C 0.7767(8) 2.676(3) 1.3345(6) 0.115(7) Uani 1 1 d . . . H8A H 0.8111 2.7036 1.3366 0.139 Uiso 1 1 calc R . . H8B H 0.7728 2.5665 1.3307 0.139 Uiso 1 1 calc R . . C9 C 0.7640(12) 2.739(4) 1.3944(16) 0.224(16) Uiso 1 1 d . . . H9A H 0.7873 2.6960 1.4349 0.336 Uiso 1 1 calc R . . H9B H 0.7294 2.7121 1.3896 0.336 Uiso 1 1 calc R . . H9C H 0.7675 2.8471 1.3958 0.336 Uiso 1 1 calc R . . C10 C 0.6901(5) 2.9860(15) 0.8972(5) 0.0607(19) Uani 1 1 d . . . H10A H 0.7239 2.9726 0.8939 0.073 Uiso 1 1 calc R . . H10B H 0.6816 3.0930 0.8919 0.073 Uiso 1 1 calc R . . C11 C 0.6515(4) 2.8979(13) 0.8437(5) 0.043(3) Uani 1 1 d . . . C12 C 0.6468(5) 2.9098(16) 0.7786(5) 0.062(4) Uani 1 1 d . . . H12 H 0.6698 2.9703 0.7669 0.075 Uiso 1 1 calc R . . C13 C 0.6102(4) 2.8372(17) 0.7316(6) 0.061(4) Uani 1 1 d . . . H13 H 0.6062 2.8490 0.6869 0.073 Uiso 1 1 calc R . . C14 C 0.5785(5) 2.7447(16) 0.7506(5) 0.058(4) Uani 1 1 d . . . C15 C 0.5847(5) 2.7315(13) 0.8165(5) 0.050(3) Uani 1 1 d . . . H15 H 0.5631 2.6682 0.8296 0.059 Uiso 1 1 calc R . . C16 C 0.5349(5) 2.660(2) 0.7021(6) 0.073(4) Uani 1 1 d . . . C17 C 0.4684(4) 2.494(2) 0.6848(6) 0.073(4) Uani 1 1 d . . . H17A H 0.4788 2.4209 0.6583 0.087 Uiso 1 1 calc R . . H17B H 0.4453 2.5668 0.6552 0.087 Uiso 1 1 calc R . . C18 C 0.4423(7) 2.416(3) 0.7275(7) 0.129(9) Uani 1 1 d . . . H18A H 0.4678 2.3688 0.7649 0.194 Uiso 1 1 calc R . . H18B H 0.4192 2.3399 0.7015 0.194 Uiso 1 1 calc R . . H18C H 0.4235 2.4891 0.7430 0.194 Uiso 1 1 calc R . . C19 C 0.6648(3) 2.4782(12) 0.9576(5) 0.035(2) Uani 1 1 d . . . H19A H 0.6818 2.4038 0.9914 0.042 Uiso 1 1 calc R . . H19B H 0.6703 2.4499 0.9168 0.042 Uiso 1 1 calc R . . C20 C 0.6090(3) 2.4806(12) 0.9463(4) 0.035(2) Uani 1 1 d . . . C21 C 0.5809(4) 2.3480(11) 0.9309(5) 0.037(2) Uani 1 1 d . . . H21 H 0.5967 2.2562 0.9286 0.044 Uiso 1 1 calc R . . C22 C 0.5289(4) 2.3546(11) 0.9192(5) 0.037(2) Uani 1 1 d . . . H22 H 0.5089 2.2672 0.9095 0.044 Uiso 1 1 calc R . . C23 C 0.5073(3) 2.4938(12) 0.9222(4) 0.034(2) Uani 1 1 d . . . C24 C 0.5380(3) 2.6174(11) 0.9394(4) 0.032(2) Uani 1 1 d . . . H24 H 0.5234 2.7101 0.9437 0.039 Uiso 1 1 calc R . . C25 C 0.4519(4) 2.5097(11) 0.9085(4) 0.034(2) Uani 1 1 d . . . C26 C 0.3743(4) 2.3879(12) 0.8847(5) 0.041(2) Uani 1 1 d . . . H26A H 0.3662 2.4782 0.9049 0.050 Uiso 1 1 calc R . . H26B H 0.3631 2.3006 0.9037 0.050 Uiso 1 1 calc R . . C27 C 0.3463(4) 2.3919(15) 0.8136(6) 0.056(3) Uani 1 1 d . . . H27A H 0.3555 2.4816 0.7950 0.084 Uiso 1 1 calc R . . H27B H 0.3100 2.3929 0.8056 0.084 Uiso 1 1 calc R . . H27C H 0.3548 2.3038 0.7931 0.084 Uiso 1 1 calc R . . C28 C 1.0323(5) 1.5074(15) 1.4237(6) 0.0607(19) Uani 1 1 d . . . H28A H 1.0663 1.5253 1.4221 0.073 Uiso 1 1 calc R B . H28B H 1.0239 1.4016 1.4129 0.073 Uiso 1 1 calc R . . C29 C 0.9967(6) 1.5986(17) 1.3758(6) 0.077(4) Uani 1 1 d . B . C30 C 0.9873(5) 1.5827(14) 1.3096(6) 0.058(3) Uani 1 1 d . . . H30 H 1.0064 1.5155 1.2941 0.070 Uiso 1 1 calc R B . C31 C 0.9483(5) 1.6687(16) 1.2655(6) 0.067(4) Uani 1 1 d . B . H31 H 0.9416 1.6621 1.2199 0.081 Uiso 1 1 calc R . . C32 C 0.9216(5) 1.7579(13) 1.2885(6) 0.057(3) Uani 1 1 d . . . C33 C 0.9347(5) 1.7718(13) 1.3585(6) 0.054(3) Uani 1 1 d . B . H33 H 0.9162 1.8385 1.3752 0.065 Uiso 1 1 calc R . . C34 C 0.8793(4) 1.8411(13) 1.2417(6) 0.051(3) Uani 1 1 d . B . C35 C 0.8135(4) 2.0230(16) 1.2297(6) 0.065(4) Uani 1 1 d . . . H35A H 0.7888 1.9582 1.1978 0.078 Uiso 1 1 calc R . . H35B H 0.8265 2.0956 1.2054 0.078 Uiso 1 1 calc R . . C36 C 0.7893(5) 2.1015(17) 1.2698(7) 0.075(4) Uani 1 1 d . . . H36A H 0.7753 2.0290 1.2923 0.112 Uiso 1 1 calc R . . H36B H 0.7623 2.1647 1.2418 0.112 Uiso 1 1 calc R . . H36C H 0.8143 2.1633 1.3021 0.112 Uiso 1 1 calc R . . O13 O 1.0453(6) 1.8963(16) 1.5014(8) 0.040(4) Uiso 0.50 1 d P B -1 HO13 H 1.0756 1.9029 1.5028 0.048 Uiso 0.50 1 d PR B -1 O14 O 0.8232(12) 1.852(4) 1.5520(16) 0.147(8) Uiso 0.50 1 d PD B -1 O15 O 0.8084(13) 2.076(4) 1.5255(16) 0.147(8) Uiso 0.50 1 d P B -1 C37 C 1.0204(9) 2.044(3) 1.4949(12) 0.040(6) Uiso 0.50 1 d P B -1 H37A H 1.0176 2.0903 1.4528 0.048 Uiso 0.50 1 calc PR B -1 H37B H 1.0400 2.1106 1.5306 0.048 Uiso 0.50 1 calc PR B -1 C38 C 0.9667(6) 2.015(2) 1.4985(10) 0.047(7) Uiso 0.50 1 d PG B -1 C39 C 0.9367(6) 2.1398(17) 1.4944(9) 0.062(6) Uiso 0.50 1 d PG B -1 H39 H 0.9470 2.2338 1.4838 0.075 Uiso 0.50 1 calc PR B -1 C40 C 0.8916(6) 2.1267(17) 1.5058(10) 0.084(9) Uiso 0.50 1 d PGD B -1 H40 H 0.8711 2.2117 1.5030 0.100 Uiso 0.50 1 calc PR B -1 C41 C 0.8765(6) 1.9891(19) 1.5213(9) 0.067(7) Uiso 0.50 1 d PG B -1 C42 C 0.9065(7) 1.8646(16) 1.5254(10) 0.077(8) Uiso 0.50 1 d PGD B -1 H42 H 0.8961 1.7706 1.5360 0.092 Uiso 0.50 1 calc PR B -1 N5 N 0.9516(7) 1.8777(18) 1.5140(12) 0.17(2) Uiso 0.50 1 d PG B -1 C43 C 0.8370(13) 1.979(3) 1.5352(17) 0.090(9) Uiso 0.50 1 d PD B -1 C45 C 0.7936(16) 1.727(5) 1.6270(19) 0.129(11) Uiso 0.50 1 d PD B -1 H45A H 0.7967 1.6295 1.6091 0.193 Uiso 0.50 1 calc PR B -1 H45B H 0.7672 1.7240 1.6464 0.193 Uiso 0.50 1 calc PR B -1 H45C H 0.8256 1.7545 1.6605 0.193 Uiso 0.50 1 calc PR B -1 C44 C 0.7802(14) 1.840(5) 1.574(2) 0.129(11) Uiso 0.50 1 d PD B -1 H44A H 0.7499 1.8085 1.5372 0.155 Uiso 0.50 1 calc PR B -1 H44B H 0.7732 1.9374 1.5900 0.155 Uiso 0.50 1 calc PR B -1 C46 C 0.8967(14) 1.318(4) 1.6871(18) 0.094(10) Uiso 0.50 1 d P . . O16 O 0.8900(11) 1.469(3) 1.6965(14) 0.128(9) 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 0.0337(7) 0.0401(7) 0.0305(7) -0.0096(6) 0.0090(5) -0.0042(6) Ni2 0.128(3) 0.0394(12) 0.0413(13) 0.000 0.0100(14) 0.000 Br1 0.0305(5) 0.0435(5) 0.0336(5) 0.0019(5) 0.0106(4) 0.0006(5) Br2 0.0442(6) 0.0576(7) 0.0547(7) -0.0058(6) 0.0174(5) -0.0024(6) Br3A 0.0574(16) 0.100(3) 0.0498(16) 0.0045(16) 0.0063(11) 0.0180(17) Br3B 0.096(2) 0.064(3) 0.0400(15) -0.0123(13) 0.0051(14) -0.0050(17) O1 0.070(3) 0.066(3) 0.049(3) -0.002(2) 0.002(2) 0.015(3) O2 0.127(10) 0.119(9) 0.032(5) -0.016(5) 0.028(5) -0.013(7) O3 0.067(6) 0.122(9) 0.028(4) 0.003(5) 0.008(4) 0.002(6) O4 0.045(4) 0.042(4) 0.036(4) -0.001(3) 0.011(3) -0.012(3) O5 0.054(5) 0.108(8) 0.032(4) -0.030(5) 0.002(4) -0.005(5) O6 0.087(7) 0.161(11) 0.034(5) -0.023(7) 0.009(4) -0.015(8) O7 0.070(3) 0.066(3) 0.049(3) -0.002(2) 0.002(2) 0.015(3) O8 0.032(4) 0.042(4) 0.045(4) -0.009(3) 0.019(3) -0.002(3) O9 0.033(4) 0.044(4) 0.051(4) -0.001(3) 0.014(3) 0.004(3) O10 0.070(3) 0.066(3) 0.049(3) -0.002(2) 0.002(2) 0.015(3) O11 0.050(5) 0.059(5) 0.044(5) 0.005(4) 0.005(4) -0.001(4) O12 0.063(5) 0.077(6) 0.032(4) 0.008(4) 0.007(4) -0.004(5) N1 0.035(5) 0.042(5) 0.041(5) -0.013(4) 0.020(4) -0.015(4) N2 0.031(4) 0.053(5) 0.032(4) -0.003(4) 0.004(3) 0.009(4) N3 0.033(4) 0.036(4) 0.029(4) -0.005(3) 0.011(3) 0.001(4) N4 0.109(9) 0.041(6) 0.032(5) 0.005(4) 0.010(5) 0.016(6) C1 0.072(5) 0.059(4) 0.046(4) -0.009(4) 0.014(3) 0.011(4) C2 0.043(6) 0.046(6) 0.051(6) -0.019(5) 0.031(5) -0.018(5) C3 0.058(7) 0.057(7) 0.041(6) -0.019(6) 0.032(6) -0.010(6) C4 0.073(9) 0.087(10) 0.044(7) -0.035(7) 0.044(7) -0.037(8) C5 0.073(8) 0.058(7) 0.030(6) -0.025(5) 0.025(5) -0.034(7) C6 0.044(6) 0.061(7) 0.034(6) -0.009(5) 0.019(5) -0.002(5) C7 0.075(9) 0.078(9) 0.035(7) -0.019(6) 0.029(7) -0.031(8) C8 0.173(19) 0.133(16) 0.026(7) 0.008(10) 0.015(9) -0.003(16) C10 0.072(5) 0.059(4) 0.046(4) -0.009(4) 0.014(3) 0.011(4) C11 0.035(6) 0.061(7) 0.035(6) 0.004(5) 0.014(5) 0.008(5) C12 0.061(8) 0.091(10) 0.035(7) 0.010(7) 0.018(6) 0.010(7) C13 0.035(6) 0.113(12) 0.037(6) -0.003(7) 0.016(5) 0.010(7) C14 0.046(7) 0.096(10) 0.025(5) -0.010(6) 0.002(5) 0.020(7) C15 0.054(7) 0.056(7) 0.036(6) -0.014(5) 0.012(5) 0.006(6) C16 0.055(8) 0.123(13) 0.040(7) -0.020(9) 0.014(6) 0.027(10) C17 0.041(7) 0.114(12) 0.047(7) -0.031(8) -0.005(5) -0.008(8) C18 0.102(14) 0.24(3) 0.045(9) -0.044(12) 0.021(9) -0.047(16) C19 0.033(5) 0.041(5) 0.035(5) -0.014(5) 0.015(4) 0.002(5) C20 0.032(5) 0.045(6) 0.023(5) -0.004(4) 0.000(4) 0.000(5) C21 0.031(5) 0.024(5) 0.054(6) 0.012(4) 0.013(4) 0.001(4) C22 0.046(6) 0.029(5) 0.036(5) 0.000(4) 0.014(4) -0.006(4) C23 0.028(5) 0.044(6) 0.027(5) 0.001(4) 0.008(4) 0.012(5) C24 0.023(5) 0.041(5) 0.032(5) -0.008(4) 0.008(4) 0.004(4) C25 0.039(5) 0.032(6) 0.031(5) -0.002(4) 0.010(4) -0.004(4) C26 0.036(6) 0.040(6) 0.052(7) -0.009(5) 0.020(5) -0.008(5) C27 0.041(7) 0.070(8) 0.049(7) 0.008(6) 0.004(5) -0.009(6) C28 0.072(5) 0.059(4) 0.046(4) -0.009(4) 0.014(3) 0.011(4) C29 0.103(12) 0.067(9) 0.040(8) 0.016(7) 0.000(7) 0.023(9) C30 0.065(8) 0.054(7) 0.048(7) 0.004(6) 0.011(6) 0.016(6) C31 0.091(10) 0.058(8) 0.039(6) 0.013(7) 0.006(6) -0.004(9) C32 0.083(9) 0.047(7) 0.039(7) 0.013(5) 0.019(6) 0.004(7) C33 0.069(8) 0.039(6) 0.047(7) 0.004(5) 0.010(6) -0.001(6) C34 0.041(6) 0.049(7) 0.059(8) 0.011(6) 0.012(6) -0.010(5) C35 0.041(7) 0.084(10) 0.055(8) 0.014(7) 0.000(5) 0.003(6) C36 0.061(9) 0.088(11) 0.076(10) -0.004(8) 0.026(7) 0.000(8) _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 2.039(9) . ? Ni1 N1 2.048(8) . ? Ni1 O4 2.071(7) . ? Ni1 O7 2.069(9) . ? Ni1 N3 2.076(8) . ? Ni1 N2 2.086(8) . ? Ni2 O10 1.919(9) 2_758 ? Ni2 O10 1.919(9) . ? Ni2 O13 2.055(15) . ? Ni2 O13 2.055(14) 2_758 ? Ni2 N4 2.072(9) . ? Ni2 N4 2.072(9) 2_758 ? Ni2 N5 2.09(2) 2_758 ? Ni2 N5 2.087(14) . ? O1 C1 1.407(14) . ? O1 HO1 0.8347 . ? O2 C7 1.301(14) . ? O2 C8 1.46(2) . ? O3 C7 1.215(16) . ? O4 C10 1.423(14) . ? O4 HO4 0.8515 . ? O5 C16 1.300(19) . ? O5 C17 1.452(14) . ? O6 C16 1.230(15) . ? O7 C19 1.422(13) . ? O7 HO7 0.8474 . ? O8 C25 1.324(12) . ? O8 C26 1.458(12) . ? O9 C25 1.196(12) . ? O10 C28 1.492(14) . ? O10 HO10 0.8766 . ? O11 C34 1.387(15) . ? O11 C35 1.469(14) . ? O12 C34 1.166(14) . ? N1 C2 1.339(13) . ? N1 C6 1.341(14) . ? N2 C11 1.322(14) . ? N2 C15 1.356(14) . ? N3 C24 1.320(12) . ? N3 C20 1.355(13) . ? N4 C33 1.315(15) . ? N4 C29 1.333(18) . ? C1 C2 1.503(17) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.375(14) . ? C3 C4 1.340(18) . ? C3 H3 0.9500 . ? C4 C5 1.395(18) . ? C4 H4 0.9500 . ? C5 C6 1.363(13) . ? C5 C7 1.448(19) . ? C6 H6 0.9500 . ? C8 C9 1.58(3) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.519(16) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.388(15) . ? C12 C13 1.348(18) . ? C12 H12 0.9500 . ? C13 C14 1.389(19) . ? C13 H13 0.9500 . ? C14 C15 1.396(16) . ? C14 C16 1.52(2) . ? C15 H15 0.9500 . ? C17 C18 1.55(2) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.515(13) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.408(14) . ? C21 C22 1.407(14) . ? C21 H21 0.9500 . ? C22 C23 1.405(13) . ? C22 H22 0.9500 . ? C23 C24 1.381(14) . ? C23 C25 1.501(13) . ? C24 H24 0.9500 . ? C26 C27 1.480(15) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.433(18) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.385(18) . ? C30 C31 1.417(17) . ? C30 H30 0.9500 . ? C31 C32 1.318(19) . ? C31 H31 0.9500 . ? C32 C33 1.449(16) . ? C32 C34 1.481(17) . ? C33 H33 0.9500 . ? C35 C36 1.468(19) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? O13 C37 1.49(3) . ? O13 HO13 0.8509 . ? O14 C43 1.30(4) . ? O14 C44 1.458(19) . ? O15 C43 1.16(4) . ? C37 C38 1.57(3) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 C39 1.3900 . ? C38 N5 1.3900 . ? C39 C40 1.3900 . ? C39 H39 0.9500 . ? C40 C41 1.3900 . ? C40 H40 0.9500 . ? C41 C43 1.26(4) . ? C41 C42 1.3900 . ? C42 N5 1.3900 . ? C42 H42 0.9500 . ? C45 C44 1.492(19) . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C46 O16 1.39(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ni1 N1 78.8(3) . . ? O1 Ni1 O4 93.1(4) . . ? N1 Ni1 O4 93.2(3) . . ? O1 Ni1 O7 172.7(3) . . ? N1 Ni1 O7 93.9(3) . . ? O4 Ni1 O7 88.0(3) . . ? O1 Ni1 N3 100.6(3) . . ? N1 Ni1 N3 97.5(3) . . ? O4 Ni1 N3 164.0(3) . . ? O7 Ni1 N3 79.4(3) . . ? O1 Ni1 N2 92.4(3) . . ? N1 Ni1 N2 167.0(4) . . ? O4 Ni1 N2 77.7(3) . . ? O7 Ni1 N2 94.9(3) . . ? N3 Ni1 N2 93.4(3) . . ? O10 Ni2 O10 64.4(6) 2_758 . ? O10 Ni2 O13 171.0(5) 2_758 . ? O10 Ni2 O13 109.9(5) . . ? O10 Ni2 O13 109.9(5) 2_758 2_758 ? O10 Ni2 O13 171.0(5) . 2_758 ? O13 Ni2 O13 76.6(9) . 2_758 ? O10 Ni2 N4 90.0(4) 2_758 . ? O10 Ni2 N4 80.4(4) . . ? O13 Ni2 N4 95.9(6) . . ? O13 Ni2 N4 92.9(6) 2_758 . ? O10 Ni2 N4 80.4(4) 2_758 2_758 ? O10 Ni2 N4 90.0(4) . 2_758 ? O13 Ni2 N4 92.9(6) . 2_758 ? O13 Ni2 N4 95.9(6) 2_758 2_758 ? N4 Ni2 N4 168.7(6) . 2_758 ? O10 Ni2 N5 166.0(11) 2_758 2_758 ? O10 Ni2 N5 101.6(11) . 2_758 ? O13 Ni2 N5 11.4(13) . 2_758 ? O13 Ni2 N5 83.9(12) 2_758 2_758 ? N4 Ni2 N5 86.9(15) . 2_758 ? N4 Ni2 N5 101.0(15) 2_758 2_758 ? O10 Ni2 N5 101.6(6) 2_758 . ? O10 Ni2 N5 166.0(7) . . ? O13 Ni2 N5 83.9(7) . . ? O13 Ni2 N5 11.4(8) 2_758 . ? N4 Ni2 N5 101.0(7) . . ? N4 Ni2 N5 86.9(7) 2_758 . ? N5 Ni2 N5 92.4(16) 2_758 . ? C1 O1 Ni1 115.2(7) . . ? C1 O1 HO1 109.6 . . ? Ni1 O1 HO1 131.1 . . ? C7 O2 C8 118.4(14) . . ? C10 O4 Ni1 117.5(7) . . ? C10 O4 HO4 109.2 . . ? Ni1 O4 HO4 133.3 . . ? C16 O5 C17 115.5(10) . . ? C19 O7 Ni1 115.9(7) . . ? C19 O7 HO7 109.2 . . ? Ni1 O7 HO7 134.8 . . ? C25 O8 C26 115.0(8) . . ? C28 O10 Ni2 114.1(7) . . ? C28 O10 HO10 103.8 . . ? Ni2 O10 HO10 131.1 . . ? C34 O11 C35 116.3(9) . . ? C2 N1 C6 117.0(9) . . ? C2 N1 Ni1 117.1(7) . . ? C6 N1 Ni1 125.7(7) . . ? C11 N2 C15 120.2(9) . . ? C11 N2 Ni1 117.2(7) . . ? C15 N2 Ni1 122.6(8) . . ? C24 N3 C20 120.2(9) . . ? C24 N3 Ni1 125.8(7) . . ? C20 N3 Ni1 113.5(7) . . ? C33 N4 C29 118.9(11) . . ? C33 N4 Ni2 126.5(9) . . ? C29 N4 Ni2 114.4(9) . . ? O1 C1 C2 111.5(10) . . ? O1 C1 H1A 109.3 . . ? C2 C1 H1A 109.3 . . ? O1 C1 H1B 109.3 . . ? C2 C1 H1B 109.3 . . ? H1A C1 H1B 108.0 . . ? N1 C2 C3 123.0(11) . . ? N1 C2 C1 114.3(9) . . ? C3 C2 C1 122.7(10) . . ? C4 C3 C2 118.7(11) . . ? C4 C3 H3 120.6 . . ? C2 C3 H3 120.6 . . ? C3 C4 C5 120.2(10) . . ? C3 C4 H4 119.9 . . ? C5 C4 H4 119.9 . . ? C6 C5 C4 117.4(12) . . ? C6 C5 C7 119.6(11) . . ? C4 C5 C7 123.0(10) . . ? N1 C6 C5 123.5(11) . . ? N1 C6 H6 118.2 . . ? C5 C6 H6 118.2 . . ? O3 C7 O2 120.1(14) . . ? O3 C7 C5 123.8(10) . . ? O2 C7 C5 116.0(13) . . ? O2 C8 C9 99(2) . . ? O2 C8 H8A 112.0 . . ? C9 C8 H8A 112.0 . . ? O2 C8 H8B 112.0 . . ? C9 C8 H8B 112.0 . . ? H8A C8 H8B 109.6 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? O4 C10 C11 109.8(10) . . ? O4 C10 H10A 109.7 . . ? C11 C10 H10A 109.7 . . ? O4 C10 H10B 109.7 . . ? C11 C10 H10B 109.7 . . ? H10A C10 H10B 108.2 . . ? N2 C11 C12 120.8(11) . . ? N2 C11 C10 116.9(9) . . ? C12 C11 C10 122.3(11) . . ? C13 C12 C11 121.2(13) . . ? C13 C12 H12 119.4 . . ? C11 C12 H12 119.4 . . ? C12 C13 C14 117.9(11) . . ? C12 C13 H13 121.0 . . ? C14 C13 H13 121.0 . . ? C13 C14 C15 119.8(11) . . ? C13 C14 C16 123.0(11) . . ? C15 C14 C16 117.1(12) . . ? N2 C15 C14 120.0(12) . . ? N2 C15 H15 120.0 . . ? C14 C15 H15 120.0 . . ? O6 C16 O5 125.0(15) . . ? O6 C16 C14 121.1(16) . . ? O5 C16 C14 113.9(11) . . ? O5 C17 C18 106.7(11) . . ? O5 C17 H17A 110.4 . . ? C18 C17 H17A 110.4 . . ? O5 C17 H17B 110.4 . . ? C18 C17 H17B 110.4 . . ? H17A C17 H17B 108.6 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O7 C19 C20 109.3(8) . . ? O7 C19 H19A 109.8 . . ? C20 C19 H19A 109.8 . . ? O7 C19 H19B 109.8 . . ? C20 C19 H19B 109.8 . . ? H19A C19 H19B 108.3 . . ? N3 C20 C21 121.2(8) . . ? N3 C20 C19 118.9(9) . . ? C21 C20 C19 119.9(9) . . ? C22 C21 C20 118.4(9) . . ? C22 C21 H21 120.8 . . ? C20 C21 H21 120.8 . . ? C21 C22 C23 118.3(9) . . ? C21 C22 H22 120.8 . . ? C23 C22 H22 120.8 . . ? C24 C23 C22 119.2(8) . . ? C24 C23 C25 119.6(8) . . ? C22 C23 C25 121.2(9) . . ? N3 C24 C23 122.6(9) . . ? N3 C24 H24 118.7 . . ? C23 C24 H24 118.7 . . ? O9 C25 O8 124.8(9) . . ? O9 C25 C23 122.8(9) . . ? O8 C25 C23 112.4(8) . . ? O8 C26 C27 112.3(9) . . ? O8 C26 H26A 109.1 . . ? C27 C26 H26A 109.1 . . ? O8 C26 H26B 109.1 . . ? C27 C26 H26B 109.1 . . ? H26A C26 H26B 107.9 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C29 C28 O10 112.9(11) . . ? C29 C28 H28A 109.0 . . ? O10 C28 H28A 109.0 . . ? C29 C28 H28B 109.0 . . ? O10 C28 H28B 109.0 . . ? H28A C28 H28B 107.8 . . ? N4 C29 C30 122.5(12) . . ? N4 C29 C28 114.9(12) . . ? C30 C29 C28 122.5(13) . . ? C29 C30 C31 118.5(13) . . ? C29 C30 H30 120.7 . . ? C31 C30 H30 120.7 . . ? C32 C31 C30 119.1(12) . . ? C32 C31 H31 120.4 . . ? C30 C31 H31 120.4 . . ? C31 C32 C33 119.0(12) . . ? C31 C32 C34 118.5(11) . . ? C33 C32 C34 122.5(12) . . ? N4 C33 C32 121.7(12) . . ? N4 C33 H33 119.1 . . ? C32 C33 H33 119.1 . . ? O12 C34 O11 123.8(11) . . ? O12 C34 C32 123.8(12) . . ? O11 C34 C32 112.4(11) . . ? O11 C35 C36 109.0(11) . . ? O11 C35 H35A 109.9 . . ? C36 C35 H35A 109.9 . . ? O11 C35 H35B 109.9 . . ? C36 C35 H35B 109.9 . . ? H35A C35 H35B 108.3 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C37 O13 Ni2 115.1(12) . . ? C37 O13 HO13 112.4 . . ? Ni2 O13 HO13 132.3 . . ? C43 O14 C44 121(4) . . ? O13 C37 C38 106.6(17) . . ? O13 C37 H37A 110.4 . . ? C38 C37 H37A 110.4 . . ? O13 C37 H37B 110.4 . . ? C38 C37 H37B 110.4 . . ? H37A C37 H37B 108.6 . . ? C39 C38 N5 120.0 . . ? C39 C38 C37 116.5(15) . . ? N5 C38 C37 122.9(15) . . ? C40 C39 C38 120.0 . . ? C40 C39 H39 120.0 . . ? C38 C39 H39 120.0 . . ? C41 C40 C39 120.0 . . ? C41 C40 H40 120.0 . . ? C39 C40 H40 120.0 . . ? C43 C41 C40 119.9(8) . . ? C43 C41 C42 120.0(8) . . ? C40 C41 C42 120.0 . . ? C41 C42 N5 120.0 . . ? C41 C42 H42 120.0 . . ? N5 C42 H42 120.0 . . ? C42 N5 C38 120.0 . . ? C42 N5 Ni2 131.3(10) . . ? C38 N5 Ni2 107.9(10) . . ? O15 C43 C41 121(3) . . ? O15 C43 O14 117(4) . . ? C41 C43 O14 121(2) . . ? O14 C44 C45 107(3) . . ? O14 C44 H44A 110.4 . . ? C45 C44 H44A 110.4 . . ? O14 C44 H44B 110.4 . . ? C45 C44 H44B 110.4 . . ? H44A C44 H44B 108.6 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.775 _refine_diff_density_min -1.726 _refine_diff_density_rms 0.169 data_Ni4(ehmp)4Br4(H2O)4 _database_code_depnum_ccdc_archive 'CCDC 798248' #TrackingRef 'CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H48 Br4 N4 Ni4 O16' _chemical_formula_weight 1347.26 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M I4(1)/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+3/4, x+1/4, z+1/4' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+5/4, x+3/4, z+3/4' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-3/4, -x-1/4, -z-1/4' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y-1/4, -x+1/4, -z+1/4' '-y-1/4, x-1/4, -z-1/4' _cell_length_a 17.1496(4) _cell_length_b 17.1496(4) _cell_length_c 16.3976(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4822.7(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7735 _cell_measurement_theta_min 2.38 _cell_measurement_theta_max 27.48 _exptl_crystal_description Block _exptl_crystal_colour Green _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas 'Not Measured' _exptl_crystal_density_diffrn 1.856 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2688 _exptl_absorpt_coefficient_mu 4.920 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.3020 _exptl_absorpt_correction_T_max 0.5065 _exptl_absorpt_process_details 'Sadabs, (Sheldrick 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16743 _diffrn_reflns_av_R_equivalents 0.0286 _diffrn_reflns_av_sigmaI/netI 0.0198 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 27.48 _reflns_number_total 2765 _reflns_number_gt 2485 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0429P)^2^+4.4986P] 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 2765 _refine_ls_number_parameters 154 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0300 _refine_ls_R_factor_gt 0.0264 _refine_ls_wR_factor_ref 0.0696 _refine_ls_wR_factor_gt 0.0679 _refine_ls_goodness_of_fit_ref 1.080 _refine_ls_restrained_S_all 1.080 _refine_ls_shift/su_max 0.002 _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 0.508969(15) 0.657389(15) 0.560398(15) 0.01528(9) Uani 1 1 d . . . Br1 Br 0.622315(13) 0.564329(13) 0.547394(14) 0.02445(9) Uani 1 1 d . . . O1 O 0.42336(8) 0.74018(8) 0.56567(8) 0.0160(3) Uani 1 1 d . . . O2 O 0.60081(9) 0.59144(10) 0.24459(9) 0.0250(3) Uani 1 1 d . . . O3 O 0.49897(10) 0.59432(12) 0.15823(10) 0.0358(4) Uani 1 1 d . . . O4 O 0.43866(10) 0.56191(10) 0.58036(11) 0.0235(3) Uani 1 1 d . . . H41 H 0.4238(17) 0.5339(17) 0.5478(18) 0.022(7) Uiso 1 1 d . . . H42 H 0.396(2) 0.5702(17) 0.6079(19) 0.036(8) Uiso 1 1 d . . . N1 N 0.47477(10) 0.65984(10) 0.43972(10) 0.0174(3) Uani 1 1 d . . . C1 C 0.51245(12) 0.63117(12) 0.37452(13) 0.0186(4) Uani 1 1 d . . . H1 H 0.5613 0.6061 0.3823 0.022 Uiso 1 1 calc R . . C2 C 0.48249(13) 0.63692(13) 0.29600(13) 0.0205(4) Uani 1 1 d . . . C3 C 0.41146(13) 0.67368(14) 0.28446(13) 0.0233(5) Uani 1 1 d . . . H3 H 0.3900 0.6789 0.2313 0.028 Uiso 1 1 calc R . . C4 C 0.37215(13) 0.70280(13) 0.35198(13) 0.0218(4) Uani 1 1 d . . . H4A H 0.3230 0.7277 0.3457 0.026 Uiso 1 1 calc R . . C5 C 0.40544(12) 0.69503(12) 0.42879(12) 0.0176(4) Uani 1 1 d . . . C6 C 0.36628(12) 0.72575(13) 0.50524(12) 0.0189(4) Uani 1 1 d . . . H6A H 0.3379 0.7746 0.4926 0.023 Uiso 1 1 calc R . . H6B H 0.3281 0.6870 0.5256 0.023 Uiso 1 1 calc R . . C7 C 0.52713(13) 0.60562(14) 0.22477(13) 0.0233(4) Uani 1 1 d . . . C8 C 0.65170(14) 0.56220(15) 0.17997(14) 0.0276(5) Uani 1 1 d . . . H8A H 0.6471 0.5952 0.1307 0.033 Uiso 1 1 calc R . . H8B H 0.6373 0.5081 0.1654 0.033 Uiso 1 1 calc R . . C9 C 0.73288(15) 0.56496(16) 0.21261(16) 0.0319(5) Uani 1 1 d . . . H9A H 0.7456 0.6185 0.2285 0.048 Uiso 1 1 calc R . . H9B H 0.7694 0.5474 0.1704 0.048 Uiso 1 1 calc R . . H9C H 0.7369 0.5307 0.2603 0.048 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.01787(14) 0.01726(14) 0.01072(14) -0.00112(9) -0.00093(9) 0.00090(9) Br1 0.02584(13) 0.02565(13) 0.02185(13) -0.00697(8) -0.00456(8) 0.00677(8) O1 0.0171(7) 0.0206(7) 0.0102(7) -0.0014(5) -0.0020(5) 0.0001(5) O2 0.0260(8) 0.0356(9) 0.0133(7) -0.0032(6) 0.0025(6) 0.0042(7) O3 0.0319(9) 0.0596(12) 0.0160(8) -0.0115(8) -0.0028(7) 0.0035(8) O4 0.0287(9) 0.0210(8) 0.0210(8) -0.0050(7) 0.0031(7) -0.0041(6) N1 0.0200(8) 0.0189(8) 0.0133(8) -0.0011(6) -0.0004(7) -0.0020(7) C1 0.0210(10) 0.0203(10) 0.0144(10) -0.0016(8) 0.0001(8) -0.0012(8) C2 0.0238(11) 0.0239(11) 0.0137(10) -0.0025(8) 0.0008(8) -0.0029(8) C3 0.0243(11) 0.0323(12) 0.0132(10) -0.0030(8) -0.0045(8) -0.0035(9) C4 0.0195(10) 0.0286(11) 0.0174(10) -0.0031(9) -0.0038(8) -0.0010(8) C5 0.0185(10) 0.0198(10) 0.0146(10) -0.0019(8) -0.0008(8) -0.0028(8) C6 0.0184(10) 0.0257(11) 0.0126(9) -0.0034(8) -0.0018(8) 0.0011(8) C7 0.0271(11) 0.0275(11) 0.0154(10) -0.0039(8) -0.0002(8) -0.0002(9) C8 0.0314(13) 0.0359(13) 0.0155(10) -0.0018(9) 0.0070(9) 0.0046(10) C9 0.0283(12) 0.0326(13) 0.0349(13) -0.0038(11) 0.0071(10) -0.0032(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 Ni1 O1 2.0442(15) . ? Ni1 O1 2.0507(14) 12_767 ? Ni1 O4 2.0596(17) . ? Ni1 N1 2.0644(17) . ? Ni1 O1 2.1072(15) 6_564 ? Ni1 Br1 2.5241(3) . ? O1 C6 1.415(2) . ? O1 Ni1 2.0507(14) 15_566 ? O1 Ni1 2.1072(15) 6_564 ? O2 C7 1.327(3) . ? O2 C8 1.461(3) . ? O3 C7 1.209(3) . ? O4 H41 0.76(3) . ? O4 H42 0.87(3) . ? N1 C1 1.342(3) . ? N1 C5 1.345(3) . ? C1 C2 1.390(3) . ? C1 H1 0.9500 . ? C2 C3 1.385(3) . ? C2 C7 1.496(3) . ? C3 C4 1.389(3) . ? C3 H3 0.9500 . ? C4 C5 1.389(3) . ? C4 H4A 0.9500 . ? C5 C6 1.517(3) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C8 C9 1.492(4) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 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 O1 82.56(6) . 12_767 ? O1 Ni1 O4 97.18(6) . . ? O1 Ni1 O4 87.30(6) 12_767 . ? O1 Ni1 N1 79.76(6) . . ? O1 Ni1 N1 161.67(7) 12_767 . ? O4 Ni1 N1 90.13(7) . . ? O1 Ni1 O1 79.33(6) . 6_564 ? O1 Ni1 O1 81.03(6) 12_767 6_564 ? O4 Ni1 O1 168.14(6) . 6_564 ? N1 Ni1 O1 100.30(6) . 6_564 ? O1 Ni1 Br1 174.76(4) . . ? O1 Ni1 Br1 99.36(4) 12_767 . ? O4 Ni1 Br1 87.80(5) . . ? N1 Ni1 Br1 98.67(5) . . ? O1 Ni1 Br1 96.11(4) 6_564 . ? C6 O1 Ni1 110.24(11) . . ? C6 O1 Ni1 127.08(12) . 15_566 ? Ni1 O1 Ni1 98.21(6) . 15_566 ? C6 O1 Ni1 119.88(12) . 6_564 ? Ni1 O1 Ni1 100.47(6) . 6_564 ? Ni1 O1 Ni1 96.21(6) 15_566 6_564 ? C7 O2 C8 116.99(18) . . ? Ni1 O4 H41 126(2) . . ? Ni1 O4 H42 116(2) . . ? H41 O4 H42 101(3) . . ? C1 N1 C5 118.93(18) . . ? C1 N1 Ni1 128.25(15) . . ? C5 N1 Ni1 112.82(13) . . ? N1 C1 C2 122.3(2) . . ? N1 C1 H1 118.9 . . ? C2 C1 H1 118.9 . . ? C3 C2 C1 119.0(2) . . ? C3 C2 C7 120.45(19) . . ? C1 C2 C7 120.6(2) . . ? C2 C3 C4 118.8(2) . . ? C2 C3 H3 120.6 . . ? C4 C3 H3 120.6 . . ? C3 C4 C5 119.3(2) . . ? C3 C4 H4A 120.4 . . ? C5 C4 H4A 120.4 . . ? N1 C5 C4 121.80(19) . . ? N1 C5 C6 115.92(17) . . ? C4 C5 C6 122.28(19) . . ? O1 C6 C5 109.47(16) . . ? O1 C6 H6A 109.8 . . ? C5 C6 H6A 109.8 . . ? O1 C6 H6B 109.8 . . ? C5 C6 H6B 109.8 . . ? H6A C6 H6B 108.2 . . ? O3 C7 O2 124.9(2) . . ? O3 C7 C2 123.9(2) . . ? O2 C7 C2 111.21(18) . . ? O2 C8 C9 106.63(19) . . ? O2 C8 H8A 110.4 . . ? C9 C8 H8A 110.4 . . ? O2 C8 H8B 110.4 . . ? C9 C8 H8B 110.4 . . ? H8A C8 H8B 108.6 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O4 H42 Br1 0.87(3) 2.31(3) 3.1363(18) 158(3) 15_566 O4 H41 Br1 0.76(3) 2.43(3) 3.1889(17) 175(3) 9_666 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.802 _refine_diff_density_min -0.254 _refine_diff_density_rms 0.097 data_Ni4(ehmp)4(OAc)4(H2O)2 _database_code_depnum_ccdc_archive 'CCDC 798249' #TrackingRef 'CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H56 N4 Ni4 O22' _chemical_formula_weight 1227.77 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 18.0337(19) _cell_length_b 20.674(2) _cell_length_c 14.8310(16) _cell_angle_alpha 90.00 _cell_angle_beta 109.676(2) _cell_angle_gamma 90.00 _cell_volume 5206.6(9) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 994 _cell_measurement_theta_min 2.39 _cell_measurement_theta_max 25.48 _exptl_crystal_description Block _exptl_crystal_colour Green _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas 'Not Measured' _exptl_crystal_density_diffrn 1.566 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2544 _exptl_absorpt_coefficient_mu 1.507 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6130 _exptl_absorpt_correction_T_max 0.7945 _exptl_absorpt_process_details 'Sadabs, (Sheldrick 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18401 _diffrn_reflns_av_R_equivalents 0.0527 _diffrn_reflns_av_sigmaI/netI 0.0609 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 27.50 _reflns_number_total 5972 _reflns_number_gt 4718 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0555P)^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 5972 _refine_ls_number_parameters 344 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0628 _refine_ls_R_factor_gt 0.0452 _refine_ls_wR_factor_ref 0.1130 _refine_ls_wR_factor_gt 0.1049 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.057 _refine_ls_shift/su_max 0.002 _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 0.43011(2) 0.320704(16) 0.29516(3) 0.01185(11) Uani 1 1 d . . . Ni2 Ni 0.54964(2) 0.220483(16) 0.35967(3) 0.01147(11) Uani 1 1 d . . . N1 N 0.45740(14) 0.41665(11) 0.33095(17) 0.0139(5) Uani 1 1 d . . . N2 N 0.52076(14) 0.12454(11) 0.36470(17) 0.0140(5) Uani 1 1 d . . . O1 O 0.55371(11) 0.31861(9) 0.33629(14) 0.0130(4) Uani 1 1 d . . . O2 O 0.39604(12) 0.63788(9) 0.34755(15) 0.0191(5) Uani 1 1 d . . . O3 O 0.29846(13) 0.56782(10) 0.27587(18) 0.0276(6) Uani 1 1 d . . . O4 O 0.43287(11) 0.22275(9) 0.27230(14) 0.0130(4) Uani 1 1 d . . . O5 O 0.67272(13) -0.02355(10) 0.48324(16) 0.0224(5) Uani 1 1 d . . . O6 O 0.57715(15) -0.09857(11) 0.4329(2) 0.0399(7) Uani 1 1 d . . . O7 O 0.42806(12) 0.30587(9) 0.43079(15) 0.0180(5) Uani 1 1 d . . . O8 O 0.52598(12) 0.23335(9) 0.48325(14) 0.0164(4) Uani 1 1 d . . . O9 O 0.31384(12) 0.34534(9) 0.25167(14) 0.0167(4) Uani 1 1 d . . . O10 O 0.25080(12) 0.29914(10) 0.11068(15) 0.0184(5) Uani 1 1 d . . . C1 C 0.40726(17) 0.46646(13) 0.3120(2) 0.0143(6) Uani 1 1 d . . . H1 H 0.3536 0.4587 0.2756 0.017 Uiso 1 1 calc R . . C2 C 0.42995(18) 0.52880(13) 0.3432(2) 0.0165(6) Uani 1 1 d . . . C3 C 0.50861(17) 0.54009(14) 0.3975(2) 0.0173(6) Uani 1 1 d . . . H3 H 0.5262 0.5824 0.4197 0.021 Uiso 1 1 calc R . . C4 C 0.56072(18) 0.48831(14) 0.4185(2) 0.0169(6) Uani 1 1 d . . . H4 H 0.6145 0.4945 0.4560 0.020 Uiso 1 1 calc R . . C5 C 0.53289(17) 0.42691(13) 0.3836(2) 0.0131(6) Uani 1 1 d . . . C6 C 0.58548(17) 0.36763(13) 0.4050(2) 0.0144(6) Uani 1 1 d . . . H6A H 0.6385 0.3796 0.4046 0.017 Uiso 1 1 calc R . . H6B H 0.5910 0.3511 0.4695 0.017 Uiso 1 1 calc R . . C7 C 0.36706(19) 0.57903(14) 0.3176(2) 0.0181(6) Uani 1 1 d . . . C8 C 0.33805(19) 0.69041(14) 0.3285(2) 0.0197(7) Uani 1 1 d . . . H8A H 0.3591 0.7262 0.3744 0.024 Uiso 1 1 calc R . . H8B H 0.2892 0.6744 0.3372 0.024 Uiso 1 1 calc R . . C9 C 0.3199(2) 0.71492(16) 0.2275(2) 0.0271(8) Uani 1 1 d . . . H9A H 0.3672 0.7346 0.2209 0.041 Uiso 1 1 calc R . . H9B H 0.2778 0.7473 0.2135 0.041 Uiso 1 1 calc R . . H9C H 0.3028 0.6788 0.1825 0.041 Uiso 1 1 calc R . . C10 C 0.57047(17) 0.07516(14) 0.3987(2) 0.0154(6) Uani 1 1 d . . . H10 H 0.6255 0.0832 0.4215 0.019 Uiso 1 1 calc R . . C11 C 0.54358(18) 0.01239(14) 0.4016(2) 0.0172(6) Uani 1 1 d . . . C12 C 0.46319(19) 0.00112(14) 0.3674(2) 0.0221(7) Uani 1 1 d . . . H12 H 0.4434 -0.0414 0.3678 0.027 Uiso 1 1 calc R . . C13 C 0.41160(18) 0.05224(14) 0.3327(2) 0.0194(7) Uani 1 1 d . . . H13 H 0.3563 0.0454 0.3091 0.023 Uiso 1 1 calc R . . C14 C 0.44285(17) 0.11385(14) 0.3331(2) 0.0147(6) Uani 1 1 d . . . C15 C 0.39126(17) 0.17264(13) 0.2986(2) 0.0159(6) Uani 1 1 d . . . H15A H 0.3449 0.1606 0.2428 0.019 Uiso 1 1 calc R . . H15B H 0.3721 0.1881 0.3500 0.019 Uiso 1 1 calc R . . C16 C 0.59861(19) -0.04294(15) 0.4400(2) 0.0226(7) Uani 1 1 d . . . C17 C 0.73052(19) -0.07467(16) 0.5224(2) 0.0273(8) Uani 1 1 d . . . H17A H 0.7058 -0.1103 0.5467 0.033 Uiso 1 1 calc R . . H17B H 0.7748 -0.0574 0.5767 0.033 Uiso 1 1 calc R . . C18 C 0.7611(2) -0.1001(2) 0.4468(3) 0.0421(10) Uani 1 1 d . . . H18A H 0.7197 -0.1250 0.3996 0.063 Uiso 1 1 calc R . . H18B H 0.8067 -0.1281 0.4766 0.063 Uiso 1 1 calc R . . H18C H 0.7769 -0.0638 0.4148 0.063 Uiso 1 1 calc R . . C19 C 0.47054(18) 0.26673(14) 0.4920(2) 0.0178(6) Uani 1 1 d . . . C20 C 0.4522(2) 0.25886(16) 0.5837(2) 0.0235(7) Uani 1 1 d . . . H20A H 0.4796 0.2925 0.6294 0.035 Uiso 1 1 calc R . . H20B H 0.4698 0.2161 0.6113 0.035 Uiso 1 1 calc R . . H20C H 0.3953 0.2629 0.5699 0.035 Uiso 1 1 calc R . . C21 C 0.25621(17) 0.33876(13) 0.1767(2) 0.0142(6) Uani 1 1 d . . . C22 C 0.18612(19) 0.38299(15) 0.1635(2) 0.0253(7) Uani 1 1 d . . . H22A H 0.1861 0.3979 0.2262 0.038 Uiso 1 1 calc R . . H22B H 0.1373 0.3593 0.1312 0.038 Uiso 1 1 calc R . . H22C H 0.1897 0.4204 0.1245 0.038 Uiso 1 1 calc R . . O1W O 0.66571(12) 0.20485(10) 0.42491(15) 0.0156(4) Uani 1 1 d D . . H1W H 0.6865(19) 0.2022(15) 0.4852(8) 0.019 Uiso 1 1 d D . . H2W H 0.6891(18) 0.2357(11) 0.409(2) 0.019 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 0.01053(19) 0.00986(18) 0.0140(2) -0.00069(13) 0.00258(15) 0.00013(13) Ni2 0.01008(19) 0.00910(18) 0.01335(19) 0.00068(13) 0.00148(14) -0.00035(13) N1 0.0139(13) 0.0137(12) 0.0142(12) -0.0012(9) 0.0049(10) -0.0006(10) N2 0.0127(12) 0.0116(11) 0.0174(13) 0.0008(9) 0.0045(10) -0.0008(9) O1 0.0123(10) 0.0108(10) 0.0142(10) -0.0021(7) 0.0022(8) -0.0006(8) O2 0.0172(11) 0.0104(10) 0.0261(12) -0.0026(8) 0.0028(9) 0.0028(8) O3 0.0169(12) 0.0172(11) 0.0406(14) -0.0058(10) -0.0011(10) 0.0005(9) O4 0.0130(10) 0.0095(9) 0.0158(10) 0.0007(7) 0.0038(8) 0.0006(8) O5 0.0175(12) 0.0164(11) 0.0305(13) 0.0053(9) 0.0043(10) 0.0030(9) O6 0.0316(15) 0.0126(11) 0.0656(19) 0.0075(12) 0.0032(13) -0.0014(10) O7 0.0179(11) 0.0157(10) 0.0197(11) 0.0015(8) 0.0052(9) 0.0038(8) O8 0.0160(11) 0.0184(10) 0.0137(10) 0.0005(8) 0.0036(9) 0.0007(8) O9 0.0149(11) 0.0154(10) 0.0174(11) -0.0022(8) 0.0025(9) 0.0018(8) O10 0.0146(11) 0.0195(10) 0.0170(11) -0.0052(8) 0.0001(9) 0.0019(9) C1 0.0132(15) 0.0144(14) 0.0135(14) -0.0016(11) 0.0020(11) 0.0020(11) C2 0.0184(16) 0.0126(14) 0.0183(15) -0.0010(11) 0.0058(12) 0.0014(11) C3 0.0193(16) 0.0123(14) 0.0201(15) -0.0026(11) 0.0062(13) -0.0036(12) C4 0.0144(15) 0.0172(14) 0.0187(15) -0.0014(12) 0.0050(12) -0.0020(12) C5 0.0144(14) 0.0162(14) 0.0105(13) -0.0018(11) 0.0065(11) 0.0009(11) C6 0.0124(14) 0.0126(13) 0.0162(14) -0.0016(11) 0.0022(12) -0.0017(11) C7 0.0246(17) 0.0139(14) 0.0153(15) -0.0038(11) 0.0061(13) -0.0007(12) C8 0.0187(16) 0.0128(14) 0.0243(17) -0.0031(12) 0.0028(13) 0.0056(12) C9 0.0309(19) 0.0222(17) 0.0273(18) -0.0016(13) 0.0087(15) 0.0055(14) C10 0.0135(15) 0.0167(14) 0.0136(14) 0.0021(11) 0.0012(12) -0.0012(11) C11 0.0185(16) 0.0135(14) 0.0185(15) 0.0029(11) 0.0047(13) -0.0003(12) C12 0.0225(17) 0.0127(14) 0.0282(18) 0.0034(12) 0.0046(14) -0.0047(12) C13 0.0161(16) 0.0174(15) 0.0219(16) 0.0028(12) 0.0028(13) -0.0047(12) C14 0.0167(15) 0.0162(14) 0.0099(13) 0.0018(11) 0.0028(11) -0.0003(12) C15 0.0110(14) 0.0155(14) 0.0209(15) 0.0018(11) 0.0049(12) -0.0017(11) C16 0.0217(17) 0.0186(16) 0.0261(17) 0.0056(13) 0.0060(14) 0.0006(13) C17 0.0204(17) 0.0244(17) 0.0309(19) 0.0091(14) 0.0006(15) 0.0053(14) C18 0.033(2) 0.048(2) 0.042(2) -0.0079(19) 0.0078(18) 0.0103(18) C19 0.0181(16) 0.0131(14) 0.0212(16) -0.0053(12) 0.0051(13) -0.0071(12) C20 0.0264(18) 0.0252(16) 0.0225(17) 0.0009(13) 0.0131(14) -0.0004(14) C21 0.0148(15) 0.0103(13) 0.0181(15) 0.0013(11) 0.0064(12) -0.0020(11) C22 0.0184(17) 0.0252(17) 0.0268(18) -0.0043(14) 0.0003(14) 0.0089(14) O1W 0.0135(11) 0.0133(10) 0.0170(11) 0.0030(8) 0.0014(9) -0.0027(8) _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 O9 2.040(2) . ? Ni1 O7 2.047(2) . ? Ni1 O4 2.0566(18) . ? Ni1 O1 2.066(2) 2_655 ? Ni1 N1 2.070(2) . ? Ni1 O1 2.104(2) . ? Ni2 O1W 2.015(2) . ? Ni2 O8 2.034(2) . ? Ni2 N2 2.058(2) . ? Ni2 O1 2.0637(19) . ? Ni2 O4 2.068(2) . ? Ni2 O4 2.085(2) 2_655 ? N1 C1 1.336(4) . ? N1 C5 1.339(4) . ? N2 C10 1.340(4) . ? N2 C14 1.341(4) . ? O1 C6 1.414(3) . ? O1 Ni1 2.066(2) 2_655 ? O2 C7 1.339(3) . ? O2 C8 1.468(3) . ? O3 C7 1.205(4) . ? O4 C15 1.409(3) . ? O4 Ni2 2.085(2) 2_655 ? O5 C16 1.334(4) . ? O5 C17 1.460(4) . ? O6 C16 1.207(4) . ? O7 C19 1.264(4) . ? O8 C19 1.257(4) . ? O9 C21 1.248(3) . ? O10 C21 1.255(3) . ? C1 C2 1.384(4) . ? C1 H1 0.9500 . ? C2 C3 1.395(4) . ? C2 C7 1.490(4) . ? C3 C4 1.389(4) . ? C3 H3 0.9500 . ? C4 C5 1.399(4) . ? C4 H4 0.9500 . ? C5 C6 1.516(4) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C8 C9 1.510(5) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.391(4) . ? C10 H10 0.9500 . ? C11 C12 1.385(4) . ? C11 C16 1.496(4) . ? C12 C13 1.387(4) . ? C12 H12 0.9500 . ? C13 C14 1.392(4) . ? C13 H13 0.9500 . ? C14 C15 1.512(4) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C17 C18 1.502(5) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.514(4) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.518(4) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? O1W H1W 0.847(10) . ? O1W H2W 0.843(10) . ? 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 O9 Ni1 O7 89.50(8) . . ? O9 Ni1 O4 105.85(8) . . ? O7 Ni1 O4 91.37(8) . . ? O9 Ni1 O1 99.41(8) . 2_655 ? O7 Ni1 O1 168.16(8) . 2_655 ? O4 Ni1 O1 78.75(8) . 2_655 ? O9 Ni1 N1 88.40(9) . . ? O7 Ni1 N1 88.45(9) . . ? O4 Ni1 N1 165.75(9) . . ? O1 Ni1 N1 99.50(9) 2_655 . ? O9 Ni1 O1 166.56(8) . . ? O7 Ni1 O1 94.58(8) . . ? O4 Ni1 O1 86.88(7) . . ? O1 Ni1 O1 78.51(8) 2_655 . ? N1 Ni1 O1 78.94(8) . . ? O1W Ni2 O8 95.01(9) . . ? O1W Ni2 N2 93.59(9) . . ? O8 Ni2 N2 87.77(9) . . ? O1W Ni2 O1 98.53(8) . . ? O8 Ni2 O1 93.04(8) . . ? N2 Ni2 O1 167.73(9) . . ? O1W Ni2 O4 168.12(8) . . ? O8 Ni2 O4 94.78(8) . . ? N2 Ni2 O4 80.09(8) . . ? O1 Ni2 O4 87.64(7) . . ? O1W Ni2 O4 89.62(8) . 2_655 ? O8 Ni2 O4 170.60(8) . 2_655 ? N2 Ni2 O4 100.12(8) . 2_655 ? O1 Ni2 O4 78.17(8) . 2_655 ? O4 Ni2 O4 81.68(9) . 2_655 ? C1 N1 C5 118.9(2) . . ? C1 N1 Ni1 126.80(19) . . ? C5 N1 Ni1 114.12(18) . . ? C10 N2 C14 119.7(2) . . ? C10 N2 Ni2 127.05(19) . . ? C14 N2 Ni2 113.22(18) . . ? C6 O1 Ni2 127.75(17) . . ? C6 O1 Ni1 120.85(17) . 2_655 ? Ni2 O1 Ni1 101.74(8) . 2_655 ? C6 O1 Ni1 109.08(16) . . ? Ni2 O1 Ni1 88.55(7) . . ? Ni1 O1 Ni1 101.44(8) 2_655 . ? C7 O2 C8 115.8(2) . . ? C15 O4 Ni1 129.33(18) . . ? C15 O4 Ni2 109.56(16) . . ? Ni1 O4 Ni2 89.72(7) . . ? C15 O4 Ni2 120.39(17) . 2_655 ? Ni1 O4 Ni2 101.34(8) . 2_655 ? Ni2 O4 Ni2 98.26(9) . 2_655 ? C16 O5 C17 116.0(2) . . ? C19 O7 Ni1 126.5(2) . . ? C19 O8 Ni2 125.46(19) . . ? C21 O9 Ni1 135.5(2) . . ? N1 C1 C2 123.0(3) . . ? N1 C1 H1 118.5 . . ? C2 C1 H1 118.5 . . ? C1 C2 C3 118.5(3) . . ? C1 C2 C7 116.8(3) . . ? C3 C2 C7 124.7(3) . . ? C4 C3 C2 118.7(3) . . ? C4 C3 H3 120.7 . . ? C2 C3 H3 120.7 . . ? C3 C4 C5 119.0(3) . . ? C3 C4 H4 120.5 . . ? C5 C4 H4 120.5 . . ? N1 C5 C4 121.8(3) . . ? N1 C5 C6 115.8(2) . . ? C4 C5 C6 122.3(3) . . ? O1 C6 C5 110.8(2) . . ? O1 C6 H6A 109.5 . . ? C5 C6 H6A 109.5 . . ? O1 C6 H6B 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 108.1 . . ? O3 C7 O2 124.3(3) . . ? O3 C7 C2 124.0(3) . . ? O2 C7 C2 111.7(3) . . ? O2 C8 C9 110.0(3) . . ? O2 C8 H8A 109.7 . . ? C9 C8 H8A 109.7 . . ? O2 C8 H8B 109.7 . . ? C9 C8 H8B 109.7 . . ? H8A C8 H8B 108.2 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N2 C10 C11 121.8(3) . . ? N2 C10 H10 119.1 . . ? C11 C10 H10 119.1 . . ? C12 C11 C10 118.6(3) . . ? C12 C11 C16 119.3(3) . . ? C10 C11 C16 122.1(3) . . ? C11 C12 C13 119.7(3) . . ? C11 C12 H12 120.1 . . ? C13 C12 H12 120.1 . . ? C12 C13 C14 118.4(3) . . ? C12 C13 H13 120.8 . . ? C14 C13 H13 120.8 . . ? N2 C14 C13 121.8(3) . . ? N2 C14 C15 116.0(2) . . ? C13 C14 C15 122.2(3) . . ? O4 C15 C14 111.1(2) . . ? O4 C15 H15A 109.4 . . ? C14 C15 H15A 109.4 . . ? O4 C15 H15B 109.4 . . ? C14 C15 H15B 109.4 . . ? H15A C15 H15B 108.0 . . ? O6 C16 O5 124.6(3) . . ? O6 C16 C11 122.9(3) . . ? O5 C16 C11 112.5(3) . . ? O5 C17 C18 110.4(3) . . ? O5 C17 H17A 109.6 . . ? C18 C17 H17A 109.6 . . ? O5 C17 H17B 109.6 . . ? C18 C17 H17B 109.6 . . ? H17A C17 H17B 108.1 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O8 C19 O7 126.0(3) . . ? O8 C19 C20 117.1(3) . . ? O7 C19 C20 116.8(3) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? O9 C21 O10 126.1(3) . . ? O9 C21 C22 117.2(3) . . ? O10 C21 C22 116.7(3) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Ni2 O1W H1W 122(2) . . ? Ni2 O1W H2W 106(2) . . ? H1W O1W H2W 105(3) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H2W O10 0.843(10) 1.786(11) 2.623(3) 172(3) 2_655 O1W H1W O10 0.847(10) 1.832(13) 2.666(3) 168(3) 8_556 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.700 _refine_diff_density_min -0.493 _refine_diff_density_rms 0.115 data_[Ni4(hmp)4(OAc)4(MeOH)2] _database_code_depnum_ccdc_archive 'CCDC 806741' #TrackingRef 'CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H44 N4 Ni4 O15.38' _chemical_formula_weight 989.57 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 39.642(6) _cell_length_b 10.6741(15) _cell_length_c 19.194(3) _cell_angle_alpha 90.00 _cell_angle_beta 94.065(4) _cell_angle_gamma 90.00 _cell_volume 8102(2) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 879 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 25.45 _exptl_crystal_description BLOCK _exptl_crystal_colour BLUE _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'Not Measured' _exptl_crystal_density_diffrn 1.623 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4088 _exptl_absorpt_coefficient_mu 1.903 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.5990 _exptl_absorpt_correction_T_max 0.8325 _exptl_absorpt_process_details 'Sadabs, (Sheldrick 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22945 _diffrn_reflns_av_R_equivalents 0.0600 _diffrn_reflns_av_sigmaI/netI 0.0651 _diffrn_reflns_limit_h_min -46 _diffrn_reflns_limit_h_max 46 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7141 _reflns_number_gt 5427 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0693P)^2^+9.5065P] 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 7141 _refine_ls_number_parameters 541 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.0792 _refine_ls_R_factor_gt 0.0562 _refine_ls_wR_factor_ref 0.1402 _refine_ls_wR_factor_gt 0.1310 _refine_ls_goodness_of_fit_ref 1.087 _refine_ls_restrained_S_all 1.090 _refine_ls_shift/su_max 0.002 _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 0.358431(17) 0.63592(6) 0.38896(3) 0.01794(18) Uani 1 1 d . . . Ni2 Ni 0.415108(17) 0.74822(6) 0.32004(3) 0.01956(18) Uani 1 1 d . A . Ni3 Ni 0.342961(17) 0.75237(6) 0.23789(3) 0.01825(18) Uani 1 1 d . . . Ni4 Ni 0.354109(17) 0.92540(6) 0.35240(3) 0.01843(18) Uani 1 1 d . . . N1 N 0.35070(11) 0.6797(4) 0.4920(2) 0.0189(10) Uani 1 1 d . . . N2 N 0.43417(11) 0.6580(4) 0.2358(2) 0.0220(10) Uani 1 1 d . . . N3 N 0.36723(11) 0.7670(4) 0.1477(2) 0.0213(10) Uani 1 1 d . . . N4 N 0.32038(11) 0.9454(4) 0.4285(2) 0.0187(10) Uani 1 1 d . . . O1 O 0.38725(9) 0.7989(3) 0.40206(16) 0.0192(8) Uani 1 1 d . . . O2 O 0.37529(9) 0.6264(3) 0.29122(16) 0.0187(8) Uani 1 1 d . . . O3 O 0.38128(8) 0.8726(3) 0.27085(15) 0.0161(7) Uani 1 1 d . . . O4 O 0.32613(8) 0.7647(3) 0.33715(16) 0.0157(7) Uani 1 1 d . . . O5 O 0.39752(9) 0.5220(3) 0.42617(17) 0.0233(8) Uani 1 1 d . . . O6 O 0.44120(9) 0.6202(3) 0.38217(18) 0.0243(9) Uani 1 1 d . . . O7 O 0.32519(9) 0.4930(3) 0.39218(18) 0.0249(9) Uani 1 1 d . . . O8 O 0.30624(11) 0.4250(4) 0.28625(19) 0.0343(10) Uani 1 1 d . . . O9 O 0.31012(9) 0.8906(3) 0.20269(17) 0.0217(8) Uani 1 1 d . . . O10 O 0.32212(9) 1.0299(3) 0.28821(17) 0.0231(8) Uani 1 1 d . . . O11 O 0.38390(10) 1.0753(3) 0.38052(18) 0.0239(9) Uani 1 1 d D . . H11 H 0.4041(6) 1.050(6) 0.378(3) 0.04(2) Uiso 1 1 d D . . O12 O 0.31210(9) 0.6095(3) 0.20400(18) 0.0220(8) Uani 1 1 d D . . H12 H 0.3098(13) 0.548(3) 0.231(2) 0.016(14) Uiso 1 1 d D . . O13 O 0.45530(10) 0.8671(4) 0.3308(2) 0.0357(10) Uani 1 1 d D . . O14 O 0.44722(12) 1.0291(5) 0.4017(3) 0.0617(15) Uani 1 1 d D . . C1 C 0.32827(13) 0.6261(5) 0.5325(3) 0.0221(12) Uani 1 1 d . . . H1 H 0.3125 0.5673 0.5123 0.027 Uiso 1 1 calc R . . C2 C 0.32766(13) 0.6544(5) 0.6029(3) 0.0221(12) Uani 1 1 d . . . H2 H 0.3116 0.6163 0.6306 0.027 Uiso 1 1 calc R . . C3 C 0.35096(14) 0.7394(5) 0.6321(3) 0.0245(13) Uani 1 1 d . . . H3 H 0.3509 0.7615 0.6800 0.029 Uiso 1 1 calc R . . C4 C 0.37425(14) 0.7916(5) 0.5906(3) 0.0213(12) Uani 1 1 d . . . H4 H 0.3909 0.8482 0.6100 0.026 Uiso 1 1 calc R . . C5 C 0.37326(13) 0.7607(5) 0.5195(3) 0.0191(11) Uani 1 1 d . . . C6 C 0.39855(15) 0.8148(5) 0.4723(2) 0.0255(13) Uani 1 1 d . . . H6A H 0.4017 0.9052 0.4825 0.031 Uiso 1 1 calc R . . H6B H 0.4206 0.7726 0.4815 0.031 Uiso 1 1 calc R . . C7 C 0.46235(14) 0.6860(6) 0.2050(3) 0.0264(13) Uani 1 1 d . . . H7 H 0.4728 0.7649 0.2145 0.032 Uiso 1 1 calc R . . C8 C 0.47689(16) 0.6057(6) 0.1602(3) 0.0349(15) Uani 1 1 d . . . H8 H 0.4973 0.6277 0.1401 0.042 Uiso 1 1 calc R . . C9 C 0.46154(17) 0.4934(7) 0.1449(3) 0.0476(18) Uani 1 1 d . . . H9 H 0.4711 0.4362 0.1139 0.057 Uiso 1 1 calc R . . C10 C 0.43166(16) 0.4637(6) 0.1755(3) 0.0356(15) Uani 1 1 d . . . H10 H 0.4204 0.3868 0.1649 0.043 Uiso 1 1 calc R . . C11 C 0.41866(14) 0.5481(5) 0.2213(3) 0.0233(12) Uani 1 1 d . . . C12 C 0.38743(14) 0.5200(5) 0.2578(3) 0.0239(12) Uani 1 1 d . . . H12A H 0.3697 0.4883 0.2234 0.029 Uiso 1 1 calc R . . H12B H 0.3925 0.4534 0.2929 0.029 Uiso 1 1 calc R . . C13 C 0.36459(14) 0.6907(5) 0.0918(3) 0.0231(12) Uani 1 1 d . . . H13 H 0.3491 0.6226 0.0918 0.028 Uiso 1 1 calc R . . C14 C 0.38333(15) 0.7066(5) 0.0343(3) 0.0267(13) Uani 1 1 d . . . H14 H 0.3808 0.6515 -0.0046 0.032 Uiso 1 1 calc R . . C15 C 0.40590(14) 0.8052(5) 0.0353(3) 0.0253(13) Uani 1 1 d . . . H15 H 0.4193 0.8191 -0.0031 0.030 Uiso 1 1 calc R . . C16 C 0.40881(13) 0.8837(5) 0.0928(3) 0.0230(12) Uani 1 1 d . . . H16 H 0.4241 0.9523 0.0940 0.028 Uiso 1 1 calc R . . C17 C 0.38933(13) 0.8617(5) 0.1486(2) 0.0187(11) Uani 1 1 d . . . C18 C 0.39146(14) 0.9412(5) 0.2135(2) 0.0215(12) Uani 1 1 d . . . H18A H 0.4150 0.9706 0.2234 0.026 Uiso 1 1 calc R . . H18B H 0.3768 1.0157 0.2060 0.026 Uiso 1 1 calc R . . C19 C 0.32162(14) 1.0283(5) 0.4822(2) 0.0213(12) Uani 1 1 d . . . H19 H 0.3413 1.0783 0.4908 0.026 Uiso 1 1 calc R . . C20 C 0.29527(14) 1.0421(5) 0.5246(2) 0.0251(13) Uani 1 1 d . . . H20 H 0.2969 1.0994 0.5625 0.030 Uiso 1 1 calc R . . C21 C 0.26649(14) 0.9712(5) 0.5109(2) 0.0235(12) Uani 1 1 d . . . H21 H 0.2477 0.9807 0.5386 0.028 Uiso 1 1 calc R . . C22 C 0.26528(13) 0.8861(5) 0.4565(3) 0.0214(12) Uani 1 1 d . . . H22 H 0.2457 0.8363 0.4465 0.026 Uiso 1 1 calc R . . C23 C 0.29285(13) 0.8745(5) 0.4170(2) 0.0188(11) Uani 1 1 d . . . C24 C 0.29341(13) 0.7825(5) 0.3566(3) 0.0207(12) Uani 1 1 d . . . H24A H 0.2839 0.7012 0.3706 0.025 Uiso 1 1 calc R . . H24B H 0.2791 0.8148 0.3162 0.025 Uiso 1 1 calc R . . C25 C 0.42817(15) 0.5361(6) 0.4172(3) 0.0263(13) Uani 1 1 d . . . C26 C 0.45287(15) 0.4410(7) 0.4514(4) 0.0479(19) Uani 1 1 d . . . H26A H 0.4454 0.4170 0.4971 0.072 Uiso 1 1 calc R . . H26B H 0.4755 0.4784 0.4575 0.072 Uiso 1 1 calc R . . H26C H 0.4536 0.3666 0.4217 0.072 Uiso 1 1 calc R . . C27 C 0.30994(13) 0.4173(5) 0.3512(3) 0.0219(12) Uani 1 1 d . . . C28 C 0.29377(16) 0.3055(6) 0.3849(3) 0.0349(15) Uani 1 1 d . . . H28A H 0.2692 0.3169 0.3827 0.052 Uiso 1 1 calc R . . H28B H 0.3025 0.2987 0.4338 0.052 Uiso 1 1 calc R . . H28C H 0.2992 0.2289 0.3598 0.052 Uiso 1 1 calc R . . C29 C 0.30646(13) 0.9965(5) 0.2322(2) 0.0183(11) Uani 1 1 d . . . C30 C 0.28145(14) 1.0857(5) 0.1980(3) 0.0252(12) Uani 1 1 d . . . H30A H 0.2817 1.1641 0.2246 0.038 Uiso 1 1 calc R . . H30B H 0.2588 1.0487 0.1966 0.038 Uiso 1 1 calc R . . H30C H 0.2875 1.1030 0.1503 0.038 Uiso 1 1 calc R . . C31 C 0.38249(16) 1.1943(6) 0.3443(3) 0.0359(15) Uani 1 1 d . . . H31A H 0.3971 1.1912 0.3052 0.054 Uiso 1 1 calc R . . H31B H 0.3902 1.2610 0.3767 0.054 Uiso 1 1 calc R . . H31C H 0.3592 1.2113 0.3265 0.054 Uiso 1 1 calc R . . C32 C 0.27908(14) 0.6281(6) 0.1699(3) 0.0297(13) Uani 1 1 d . . . H32A H 0.2667 0.6901 0.1959 0.045 Uiso 1 1 calc R . . H32B H 0.2667 0.5486 0.1683 0.045 Uiso 1 1 calc R . . H32C H 0.2813 0.6584 0.1223 0.045 Uiso 1 1 calc R . . C33 C 0.4643(3) 0.9341(12) 0.3809(6) 0.056(3) Uani 0.584(9) 1 d PDU A 1 C34 C 0.4967(3) 0.8976(16) 0.4233(8) 0.088(5) Uani 0.584(9) 1 d PDU A 1 H34A H 0.4979 0.8062 0.4276 0.131 Uiso 0.584(9) 1 calc PR A 1 H34B H 0.4969 0.9352 0.4699 0.131 Uiso 0.584(9) 1 calc PR A 1 H34C H 0.5163 0.9280 0.3997 0.131 Uiso 0.584(9) 1 calc PR A 1 O1W O 0.5420(5) 0.166(2) 0.3475(10) 0.192(9) Uiso 0.584(9) 1 d P A 1 C33A C 0.4632(4) 0.9769(17) 0.3574(8) 0.054(4) Uiso 0.416(9) 1 d PDU A 2 C34A C 0.5002(4) 1.007(2) 0.3495(11) 0.078(6) Uiso 0.416(9) 1 d PDU A 2 H34D H 0.5125 1.0074 0.3956 0.116 Uiso 0.416(9) 1 calc PR A 2 H34E H 0.5021 1.0895 0.3277 0.116 Uiso 0.416(9) 1 calc PR A 2 H34F H 0.5100 0.9434 0.3200 0.116 Uiso 0.416(9) 1 calc PR A 2 O2W O 0.4942(6) 0.801(2) 0.4940(14) 0.150(9) Uiso 0.416(9) 1 d P A 2 O3W O 0.5022(8) 0.784(3) 0.5687(17) 0.199(13) Uiso 0.416(9) 1 d P A 3 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 0.0238(4) 0.0211(4) 0.0089(3) -0.0013(3) 0.0013(3) -0.0055(3) Ni2 0.0246(4) 0.0233(4) 0.0111(3) -0.0015(3) 0.0032(3) -0.0057(3) Ni3 0.0264(4) 0.0197(4) 0.0087(3) -0.0021(3) 0.0020(3) -0.0032(3) Ni4 0.0281(4) 0.0194(4) 0.0079(3) -0.0022(3) 0.0022(3) -0.0043(3) N1 0.023(2) 0.021(2) 0.013(2) -0.0024(19) -0.0005(18) -0.0005(19) N2 0.030(3) 0.025(3) 0.011(2) 0.0022(19) 0.0034(19) -0.001(2) N3 0.027(3) 0.024(3) 0.012(2) -0.0035(19) 0.0003(19) 0.002(2) N4 0.026(3) 0.018(2) 0.011(2) 0.0033(18) -0.0041(18) 0.0016(19) O1 0.025(2) 0.027(2) 0.0058(16) -0.0073(15) 0.0028(14) -0.0071(16) O2 0.026(2) 0.0202(19) 0.0101(16) -0.0065(15) 0.0049(15) -0.0029(15) O3 0.024(2) 0.0190(19) 0.0063(15) 0.0020(14) 0.0066(14) -0.0061(15) O4 0.0188(19) 0.0189(19) 0.0096(16) 0.0003(14) 0.0028(14) -0.0055(14) O5 0.024(2) 0.033(2) 0.0129(17) 0.0024(16) 0.0016(15) -0.0037(17) O6 0.025(2) 0.030(2) 0.0183(18) 0.0019(17) 0.0023(16) -0.0048(17) O7 0.032(2) 0.025(2) 0.0178(18) -0.0045(17) 0.0025(16) -0.0109(17) O8 0.054(3) 0.030(2) 0.018(2) 0.0007(18) -0.0057(18) -0.013(2) O9 0.031(2) 0.021(2) 0.0122(17) -0.0002(16) 0.0006(15) 0.0004(16) O10 0.035(2) 0.022(2) 0.0124(17) -0.0032(16) 0.0019(16) -0.0035(16) O11 0.037(3) 0.017(2) 0.0179(19) -0.0018(16) 0.0036(17) -0.0060(18) O12 0.027(2) 0.024(2) 0.0139(18) -0.0008(17) -0.0016(16) -0.0048(16) O13 0.031(2) 0.041(3) 0.036(2) -0.011(2) 0.0057(19) -0.0158(19) O14 0.041(3) 0.048(3) 0.096(4) -0.036(3) 0.005(3) -0.007(2) C1 0.024(3) 0.023(3) 0.020(3) 0.002(2) 0.002(2) -0.001(2) C2 0.025(3) 0.024(3) 0.018(3) 0.006(2) 0.003(2) 0.001(2) C3 0.040(4) 0.024(3) 0.010(2) 0.003(2) 0.001(2) 0.009(3) C4 0.034(3) 0.017(3) 0.012(2) 0.004(2) 0.000(2) -0.001(2) C5 0.024(3) 0.020(3) 0.014(2) 0.002(2) -0.001(2) 0.001(2) C6 0.040(4) 0.031(3) 0.006(2) -0.006(2) 0.001(2) -0.011(3) C7 0.033(3) 0.031(3) 0.016(3) 0.003(3) 0.005(2) 0.000(3) C8 0.034(4) 0.045(4) 0.027(3) -0.001(3) 0.012(3) -0.002(3) C9 0.048(4) 0.058(5) 0.040(4) -0.021(4) 0.019(3) 0.001(4) C10 0.042(4) 0.034(4) 0.032(3) -0.011(3) 0.011(3) -0.004(3) C11 0.027(3) 0.027(3) 0.016(3) 0.001(2) -0.001(2) -0.001(2) C12 0.030(3) 0.022(3) 0.020(3) -0.003(2) -0.002(2) -0.002(2) C13 0.032(3) 0.022(3) 0.016(3) -0.005(2) 0.002(2) 0.000(2) C14 0.041(4) 0.030(3) 0.009(2) -0.003(2) 0.001(2) 0.010(3) C15 0.032(3) 0.032(3) 0.013(3) 0.002(3) 0.008(2) 0.009(3) C16 0.024(3) 0.028(3) 0.018(3) 0.008(2) 0.004(2) 0.003(2) C17 0.027(3) 0.019(3) 0.009(2) 0.002(2) -0.003(2) 0.003(2) C18 0.031(3) 0.022(3) 0.011(2) 0.001(2) 0.004(2) -0.006(2) C19 0.034(3) 0.020(3) 0.010(2) -0.003(2) -0.003(2) 0.001(2) C20 0.041(4) 0.029(3) 0.007(2) -0.001(2) 0.005(2) 0.003(3) C21 0.031(3) 0.030(3) 0.009(2) 0.003(2) 0.004(2) 0.010(3) C22 0.025(3) 0.023(3) 0.016(3) 0.005(2) 0.000(2) 0.000(2) C23 0.030(3) 0.014(3) 0.012(2) 0.003(2) -0.001(2) 0.004(2) C24 0.025(3) 0.022(3) 0.016(3) 0.000(2) 0.001(2) -0.004(2) C25 0.031(4) 0.038(3) 0.009(2) -0.003(3) 0.001(2) -0.006(3) C26 0.026(4) 0.066(5) 0.050(4) 0.033(4) -0.005(3) -0.003(3) C27 0.017(3) 0.022(3) 0.026(3) 0.003(3) -0.001(2) 0.000(2) C28 0.049(4) 0.030(3) 0.027(3) -0.005(3) 0.002(3) -0.016(3) C29 0.025(3) 0.019(3) 0.011(2) 0.003(2) 0.009(2) -0.004(2) C30 0.031(3) 0.031(3) 0.013(2) -0.002(2) 0.001(2) 0.002(3) C31 0.048(4) 0.033(4) 0.026(3) 0.005(3) 0.001(3) -0.006(3) C32 0.029(3) 0.037(3) 0.022(3) -0.003(3) -0.006(2) -0.001(3) C33 0.037(5) 0.058(7) 0.074(7) -0.030(6) 0.005(5) 0.001(5) C34 0.069(8) 0.097(9) 0.095(9) -0.049(8) -0.006(7) 0.019(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 O7 2.020(4) . ? Ni1 O2 2.038(3) . ? Ni1 O5 2.057(4) . ? Ni1 N1 2.077(4) . ? Ni1 O4 2.083(3) . ? Ni1 O1 2.086(3) . ? Ni1 Ni2 2.9421(10) . ? Ni2 O13 2.036(4) . ? Ni2 O6 2.046(4) . ? Ni2 O1 2.058(3) . ? Ni2 O3 2.067(3) . ? Ni2 N2 2.071(4) . ? Ni2 O2 2.089(3) . ? Ni3 O12 2.033(4) . ? Ni3 N3 2.046(4) . ? Ni3 O9 2.051(4) . ? Ni3 O3 2.054(3) . ? Ni3 O4 2.067(3) . ? Ni3 O2 2.076(4) . ? Ni3 Ni4 2.8810(9) . ? Ni4 O10 2.037(4) . ? Ni4 O11 2.039(4) . ? Ni4 O3 2.041(3) . ? Ni4 O4 2.052(3) . ? Ni4 N4 2.060(4) . ? Ni4 O1 2.069(4) . ? N1 C5 1.326(7) . ? N1 C1 1.349(7) . ? N2 C7 1.334(7) . ? N2 C11 1.344(7) . ? N3 C17 1.336(7) . ? N3 C13 1.345(6) . ? N4 C23 1.334(7) . ? N4 C19 1.356(6) . ? O1 C6 1.401(6) . ? O2 C12 1.406(6) . ? O3 C18 1.405(6) . ? O4 C24 1.388(6) . ? O5 C25 1.248(6) . ? O6 C25 1.255(6) . ? O7 C27 1.253(6) . ? O8 C27 1.248(6) . ? O9 C29 1.277(6) . ? O10 C29 1.254(6) . ? O11 C31 1.447(7) . ? O12 C32 1.435(6) . ? O13 C33 1.232(2) . ? O13 C33A 1.308(16) . ? O14 C33A 1.231(2) . ? O14 C33 1.299(11) . ? C1 C2 1.387(7) . ? C2 C3 1.384(8) . ? C3 C4 1.380(8) . ? C4 C5 1.401(7) . ? C5 C6 1.513(7) . ? C7 C8 1.369(8) . ? C8 C9 1.367(9) . ? C9 C10 1.394(9) . ? C10 C11 1.384(8) . ? C11 C12 1.496(7) . ? C13 C14 1.385(7) . ? C14 C15 1.380(8) . ? C15 C16 1.384(7) . ? C16 C17 1.383(7) . ? C17 C18 1.505(7) . ? C19 C20 1.376(7) . ? C20 C21 1.379(8) . ? C21 C22 1.382(7) . ? C22 C23 1.379(7) . ? C23 C24 1.521(7) . ? C25 C26 1.526(8) . ? C27 C28 1.520(8) . ? C29 C30 1.493(7) . ? C33 C34 1.520(2) . ? C33A C34A 1.520(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O7 Ni1 O2 104.35(14) . . ? O7 Ni1 O5 91.15(15) . . ? O2 Ni1 O5 90.13(14) . . ? O7 Ni1 N1 90.01(15) . . ? O2 Ni1 N1 165.52(15) . . ? O5 Ni1 N1 87.75(15) . . ? O7 Ni1 O4 97.64(14) . . ? O2 Ni1 O4 79.85(13) . . ? O5 Ni1 O4 168.03(13) . . ? N1 Ni1 O4 100.31(15) . . ? O7 Ni1 O1 168.21(14) . . ? O2 Ni1 O1 86.55(13) . . ? O5 Ni1 O1 93.34(14) . . ? N1 Ni1 O1 79.28(15) . . ? O4 Ni1 O1 79.63(14) . . ? O7 Ni1 Ni2 147.37(11) . . ? O2 Ni1 Ni2 45.22(10) . . ? O5 Ni1 Ni2 79.42(10) . . ? N1 Ni1 Ni2 120.37(12) . . ? O4 Ni1 Ni2 88.83(9) . . ? O1 Ni1 Ni2 44.39(9) . . ? O13 Ni2 O6 89.86(16) . . ? O13 Ni2 O1 102.55(15) . . ? O6 Ni2 O1 90.35(14) . . ? O13 Ni2 O3 97.12(16) . . ? O6 Ni2 O3 168.57(13) . . ? O1 Ni2 O3 79.33(13) . . ? O13 Ni2 N2 92.45(17) . . ? O6 Ni2 N2 86.96(16) . . ? O1 Ni2 N2 164.76(16) . . ? O3 Ni2 N2 101.71(15) . . ? O13 Ni2 O2 170.38(14) . . ? O6 Ni2 O2 94.59(14) . . ? O1 Ni2 O2 85.97(13) . . ? O3 Ni2 O2 79.92(14) . . ? N2 Ni2 O2 79.30(15) . . ? O13 Ni2 Ni1 145.64(11) . . ? O6 Ni2 Ni1 80.58(10) . . ? O1 Ni2 Ni1 45.16(10) . . ? O3 Ni2 Ni1 88.60(9) . . ? N2 Ni2 Ni1 119.62(12) . . ? O2 Ni2 Ni1 43.84(9) . . ? O12 Ni3 N3 95.46(16) . . ? O12 Ni3 O9 94.63(15) . . ? N3 Ni3 O9 89.53(15) . . ? O12 Ni3 O3 169.26(15) . . ? N3 Ni3 O3 80.26(15) . . ? O9 Ni3 O3 95.18(14) . . ? O12 Ni3 O4 96.69(14) . . ? N3 Ni3 O4 167.74(16) . . ? O9 Ni3 O4 91.08(14) . . ? O3 Ni3 O4 87.49(12) . . ? O12 Ni3 O2 90.49(14) . . ? N3 Ni3 O2 98.97(15) . . ? O9 Ni3 O2 169.63(13) . . ? O3 Ni3 O2 80.52(14) . . ? O4 Ni3 O2 79.35(13) . . ? O12 Ni3 Ni4 141.38(10) . . ? N3 Ni3 Ni4 122.74(13) . . ? O9 Ni3 Ni4 81.34(10) . . ? O3 Ni3 Ni4 45.12(9) . . ? O4 Ni3 Ni4 45.40(9) . . ? O2 Ni3 Ni4 89.02(9) . . ? O10 Ni4 O11 93.13(15) . . ? O10 Ni4 O3 91.55(13) . . ? O11 Ni4 O3 95.31(14) . . ? O10 Ni4 O4 93.68(14) . . ? O11 Ni4 O4 172.24(14) . . ? O3 Ni4 O4 88.22(13) . . ? O10 Ni4 N4 87.96(15) . . ? O11 Ni4 N4 97.11(16) . . ? O3 Ni4 N4 167.57(15) . . ? O4 Ni4 N4 79.43(15) . . ? O10 Ni4 O1 169.68(13) . . ? O11 Ni4 O1 93.06(15) . . ? O3 Ni4 O1 79.67(13) . . ? O4 Ni4 O1 80.75(13) . . ? N4 Ni4 O1 99.45(14) . . ? O10 Ni4 Ni3 80.45(10) . . ? O11 Ni4 Ni3 139.45(11) . . ? O3 Ni4 Ni3 45.46(9) . . ? O4 Ni4 Ni3 45.83(9) . . ? N4 Ni4 Ni3 122.36(12) . . ? O1 Ni4 Ni3 89.49(9) . . ? C5 N1 C1 120.0(4) . . ? C5 N1 Ni1 112.6(3) . . ? C1 N1 Ni1 127.0(3) . . ? C7 N2 C11 119.3(5) . . ? C7 N2 Ni2 127.2(4) . . ? C11 N2 Ni2 112.3(3) . . ? C17 N3 C13 118.8(5) . . ? C17 N3 Ni3 113.2(3) . . ? C13 N3 Ni3 127.8(4) . . ? C23 N4 C19 118.7(5) . . ? C23 N4 Ni4 112.9(3) . . ? C19 N4 Ni4 128.0(4) . . ? C6 O1 Ni2 128.0(3) . . ? C6 O1 Ni4 120.9(3) . . ? Ni2 O1 Ni4 100.18(14) . . ? C6 O1 Ni1 110.6(3) . . ? Ni2 O1 Ni1 90.45(13) . . ? Ni4 O1 Ni1 99.45(14) . . ? C12 O2 Ni1 127.2(3) . . ? C12 O2 Ni3 121.2(3) . . ? Ni1 O2 Ni3 100.98(15) . . ? C12 O2 Ni2 110.3(3) . . ? Ni1 O2 Ni2 90.93(13) . . ? Ni3 O2 Ni2 98.98(15) . . ? C18 O3 Ni4 130.8(3) . . ? C18 O3 Ni3 109.4(3) . . ? Ni4 O3 Ni3 89.42(13) . . ? C18 O3 Ni2 118.7(3) . . ? Ni4 O3 Ni2 100.81(13) . . ? Ni3 O3 Ni2 100.44(14) . . ? C24 O4 Ni4 110.7(3) . . ? C24 O4 Ni3 128.7(3) . . ? Ni4 O4 Ni3 88.76(12) . . ? C24 O4 Ni1 121.1(3) . . ? Ni4 O4 Ni1 100.13(14) . . ? Ni3 O4 Ni1 99.81(14) . . ? C25 O5 Ni1 126.7(4) . . ? C25 O6 Ni2 125.5(4) . . ? C27 O7 Ni1 139.0(3) . . ? C29 O9 Ni3 125.5(3) . . ? C29 O10 Ni4 127.7(3) . . ? C31 O11 Ni4 124.0(3) . . ? C32 O12 Ni3 123.4(3) . . ? C33 O13 C33A 29.1(10) . . ? C33 O13 Ni2 128.6(8) . . ? C33A O13 Ni2 139.7(6) . . ? C33A O14 C33 29.3(11) . . ? N1 C1 C2 121.8(5) . . ? C3 C2 C1 118.7(5) . . ? C4 C3 C2 119.1(5) . . ? C3 C4 C5 119.6(5) . . ? N1 C5 C4 120.9(5) . . ? N1 C5 C6 117.9(4) . . ? C4 C5 C6 121.2(5) . . ? O1 C6 C5 110.5(4) . . ? N2 C7 C8 122.7(6) . . ? C9 C8 C7 118.8(6) . . ? C8 C9 C10 119.2(6) . . ? C11 C10 C9 119.0(6) . . ? N2 C11 C10 120.9(5) . . ? N2 C11 C12 117.4(5) . . ? C10 C11 C12 121.7(5) . . ? O2 C12 C11 111.9(4) . . ? N3 C13 C14 123.0(5) . . ? C15 C14 C13 117.8(5) . . ? C14 C15 C16 119.3(5) . . ? C17 C16 C15 119.7(5) . . ? N3 C17 C16 121.3(5) . . ? N3 C17 C18 115.8(4) . . ? C16 C17 C18 122.9(5) . . ? O3 C18 C17 110.6(4) . . ? N4 C19 C20 122.1(5) . . ? C19 C20 C21 118.8(5) . . ? C20 C21 C22 119.2(5) . . ? C23 C22 C21 119.2(5) . . ? N4 C23 C22 121.9(5) . . ? N4 C23 C24 115.9(4) . . ? C22 C23 C24 122.2(5) . . ? O4 C24 C23 110.9(4) . . ? O5 C25 O6 127.0(5) . . ? O5 C25 C26 117.5(5) . . ? O6 C25 C26 115.5(5) . . ? O8 C27 O7 127.0(5) . . ? O8 C27 C28 116.9(5) . . ? O7 C27 C28 116.0(5) . . ? O10 C29 O9 124.5(5) . . ? O10 C29 C30 118.0(5) . . ? O9 C29 C30 117.5(4) . . ? O13 C33 O14 124.3(9) . . ? O13 C33 C34 117.2(10) . . ? O14 C33 C34 118.4(7) . . ? O14 C33A O13 123.7(13) . . ? O14 C33A C34A 121.5(15) . . ? O13 C33A C34A 110.9(10) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O11 H11 O14 0.847(10) 1.75(3) 2.562(6) 159(6) . O12 H12 O8 0.848(10) 1.697(12) 2.545(5) 179(5) . _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.793 _refine_diff_density_min -0.606 _refine_diff_density_rms 0.124