# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_f _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H18 Co3 O18' _chemical_formula_weight 554.99 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.7894(9) _cell_length_b 5.4213(5) _cell_length_c 14.9847(13) _cell_angle_alpha 90.00 _cell_angle_beta 104.713(5) _cell_angle_gamma 90.00 _cell_volume 769.18(12) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour pink _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.396 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 558 _exptl_absorpt_coefficient_mu 3.301 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7782 _exptl_absorpt_correction_T_max 0.8904 _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type CCD _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count 0.5 _diffrn_standards_interval_time 20 _diffrn_standards_decay_% ? _diffrn_reflns_number 5024 _diffrn_reflns_av_R_equivalents 0.0315 _diffrn_reflns_av_sigmaI/netI 0.0359 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -4 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 26.39 _reflns_number_total 1569 _reflns_number_gt 1341 _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 'Platon (Spek, 2008)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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 w=1/[\s^2^(Fo^2^)+(0.0231P)^2^+0.4062P] 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 1569 _refine_ls_number_parameters 151 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0333 _refine_ls_R_factor_gt 0.0260 _refine_ls_wR_factor_ref 0.0560 _refine_ls_wR_factor_gt 0.0534 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.038 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.95718(4) 0.11446(7) 0.32120(2) 0.00847(11) Uani 1 d . . . Co2 Co 0.5000 0.0000 0.0000 0.00921(13) Uani 1 d S . . O1 O 0.9224(2) 0.2566(4) 0.44551(13) 0.0150(4) Uani 1 d D . . H1A H 0.8382(14) 0.252(6) 0.446(2) 0.018 Uiso 1 d D . . H1B H 0.978(3) 0.231(5) 0.4960(11) 0.018 Uiso 1 d D . . O2 O 0.8897(2) -0.2258(4) 0.36686(13) 0.0140(4) Uani 1 d D . . H2A H 0.934(3) -0.333(4) 0.3463(19) 0.017 Uiso 1 d D . . H2B H 0.8034(12) -0.241(5) 0.3442(18) 0.017 Uiso 1 d D . . O3 O 0.94948(18) -0.0500(3) 0.19630(12) 0.0097(4) Uani 1 d . . . C4 C 0.8164(3) -0.0255(5) 0.13368(17) 0.0087(5) Uani 1 d D . . H4 H 0.820(3) 0.080(4) 0.0847(13) 0.010 Uiso 1 d D . . C5 C 0.7083(3) 0.1085(5) 0.17563(17) 0.0094(5) Uani 1 d . . . O6 O 0.75078(18) 0.1970(3) 0.25526(12) 0.0104(4) Uani 1 d . . . O7 O 0.58340(18) 0.1376(3) 0.12770(12) 0.0111(4) Uani 1 d . . . C8 C 0.7624(3) -0.2710(5) 0.08681(18) 0.0102(5) Uani 1 d . . . O9 O 0.83742(19) -0.4599(3) 0.10866(12) 0.0125(4) Uani 1 d . . . O10 O 0.64818(19) -0.2728(3) 0.02381(12) 0.0130(4) Uani 1 d . . . O11 O 0.3790(2) -0.2700(4) 0.06193(13) 0.0157(4) Uani 1 d D . . H11A H 0.381(3) -0.407(3) 0.0379(19) 0.019 Uiso 1 d D . . H11B H 0.426(3) -0.301(5) 0.1151(10) 0.019 Uiso 1 d D . . O100 O 0.6069(2) 0.6550(4) 0.25635(17) 0.0254(5) Uani 1 d D . . H10A H 0.555(3) 0.646(6) 0.2914(19) 0.030 Uiso 1 d D . . H10B H 0.630(3) 0.511(3) 0.249(2) 0.030 Uiso 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 Co1 0.00802(18) 0.0080(2) 0.00856(18) -0.00067(14) 0.00052(14) -0.00074(14) Co2 0.0084(3) 0.0093(3) 0.0086(2) -0.0004(2) -0.0004(2) 0.0024(2) O1 0.0148(11) 0.0187(11) 0.0121(10) -0.0019(9) 0.0044(9) -0.0023(9) O2 0.0151(10) 0.0101(10) 0.0175(10) -0.0010(8) 0.0056(9) -0.0000(9) O3 0.0075(9) 0.0101(9) 0.0107(9) -0.0001(7) 0.0008(7) -0.0001(8) C4 0.0093(13) 0.0088(13) 0.0071(12) 0.0010(10) 0.0008(10) -0.0008(11) C5 0.0103(13) 0.0060(13) 0.0113(12) 0.0005(11) 0.0018(10) -0.0012(11) O6 0.0082(9) 0.0122(10) 0.0099(9) -0.0005(8) 0.0004(8) 0.0013(7) O7 0.0071(9) 0.0140(10) 0.0104(9) -0.0006(8) -0.0012(7) 0.0011(8) C8 0.0098(13) 0.0110(14) 0.0114(13) -0.0004(11) 0.0057(11) -0.0028(11) O9 0.0098(9) 0.0100(10) 0.0157(10) 0.0002(8) -0.0004(8) 0.0004(8) O10 0.0122(10) 0.0113(10) 0.0129(9) -0.0036(8) -0.0019(8) 0.0002(8) O11 0.0211(11) 0.0113(10) 0.0135(10) -0.0023(8) 0.0024(9) -0.0009(9) O100 0.0319(13) 0.0133(11) 0.0392(14) 0.0003(11) 0.0244(11) 0.0013(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 Co1 O3 2.0572(18) . ? Co1 O9 2.0583(18) 2_755 ? Co1 O6 2.0604(17) . ? Co1 O3 2.0819(18) 2_755 ? Co1 O1 2.1217(19) . ? Co1 O2 2.1302(19) . ? Co2 O7 2.0227(17) . ? Co2 O7 2.0227(17) 3_655 ? Co2 O10 2.0384(18) 3_655 ? Co2 O10 2.0385(18) . ? Co2 O11 2.228(2) 3_655 ? Co2 O11 2.228(2) . ? O1 H1A 0.828(10) . ? O1 H1B 0.824(10) . ? O2 H2A 0.830(10) . ? O2 H2B 0.830(10) . ? O3 C4 1.405(3) . ? O3 Co1 2.0819(18) 2_745 ? C4 C8 1.535(4) . ? C4 C5 1.543(4) . ? C4 H4 0.937(10) . ? C5 O6 1.255(3) . ? C5 O7 1.261(3) . ? C8 O9 1.254(3) . ? C8 O10 1.267(3) . ? O9 Co1 2.0582(18) 2_745 ? O11 H11A 0.826(10) . ? O11 H11B 0.831(10) . ? O100 H10A 0.821(10) . ? O100 H10B 0.827(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 O3 Co1 O9 100.66(7) . 2_755 ? O3 Co1 O6 81.55(7) . . ? O9 Co1 O6 177.78(7) 2_755 . ? O3 Co1 O3 100.37(4) . 2_755 ? O9 Co1 O3 80.35(7) 2_755 2_755 ? O6 Co1 O3 99.10(7) . 2_755 ? O3 Co1 O1 168.29(7) . . ? O9 Co1 O1 88.66(8) 2_755 . ? O6 Co1 O1 89.18(7) . . ? O3 Co1 O1 88.09(7) 2_755 . ? O3 Co1 O2 88.53(7) . . ? O9 Co1 O2 90.51(7) 2_755 . ? O6 Co1 O2 89.75(7) . . ? O3 Co1 O2 168.24(7) 2_755 . ? O1 Co1 O2 84.28(8) . . ? O7 Co2 O7 180.0 . 3_655 ? O7 Co2 O10 89.79(7) . 3_655 ? O7 Co2 O10 90.21(7) 3_655 3_655 ? O7 Co2 O10 90.21(7) . . ? O7 Co2 O10 89.79(7) 3_655 . ? O10 Co2 O10 180.0 3_655 . ? O7 Co2 O11 91.27(7) . 3_655 ? O7 Co2 O11 88.73(7) 3_655 3_655 ? O10 Co2 O11 83.13(7) 3_655 3_655 ? O10 Co2 O11 96.87(7) . 3_655 ? O7 Co2 O11 88.73(7) . . ? O7 Co2 O11 91.27(7) 3_655 . ? O10 Co2 O11 96.87(7) 3_655 . ? O10 Co2 O11 83.13(7) . . ? O11 Co2 O11 180.0 3_655 . ? Co1 O1 H1A 113(2) . . ? Co1 O1 H1B 122(2) . . ? H1A O1 H1B 114(3) . . ? Co1 O2 H2A 105(2) . . ? Co1 O2 H2B 109(2) . . ? H2A O2 H2B 111(3) . . ? C4 O3 Co1 112.34(14) . . ? C4 O3 Co1 111.14(15) . 2_745 ? Co1 O3 Co1 125.27(9) . 2_745 ? O3 C4 C8 112.1(2) . . ? O3 C4 C5 112.8(2) . . ? C8 C4 C5 113.7(2) . . ? O3 C4 H4 111.7(17) . . ? C8 C4 H4 104.3(17) . . ? C5 C4 H4 101.3(16) . . ? O6 C5 O7 122.2(2) . . ? O6 C5 C4 118.1(2) . . ? O7 C5 C4 119.6(2) . . ? C5 O6 Co1 114.88(17) . . ? C5 O7 Co2 126.35(17) . . ? O9 C8 O10 122.4(2) . . ? O9 C8 C4 118.6(2) . . ? O10 C8 C4 118.9(2) . . ? C8 O9 Co1 113.87(16) . 2_745 ? C8 O10 Co2 125.39(17) . . ? Co2 O11 H11A 110(2) . . ? Co2 O11 H11B 108(2) . . ? H11A O11 H11B 100(3) . . ? H10A O100 H10B 105(3) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.39 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.407 _refine_diff_density_min -0.443 _refine_diff_density_rms 0.094 _database_code_depnum_ccdc_archive 'CCDC 890223' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_f #TrackingRef 'web_deposit_cif_file_0_zhilin_1362078096.rz92.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H18 Ni3 O18' _chemical_formula_weight 554.33 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.914(7) _cell_length_b 5.449(4) _cell_length_c 15.142(11) _cell_angle_alpha 90.00 _cell_angle_beta 105.99(3) _cell_angle_gamma 90.00 _cell_volume 786.4(10) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.341 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 564 _exptl_absorpt_coefficient_mu 3.656 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7586 _exptl_absorpt_correction_T_max 0.8105 _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type CCD _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count 0.5 _diffrn_standards_interval_time 5 _diffrn_standards_decay_% ? _diffrn_reflns_number 8229 _diffrn_reflns_av_R_equivalents 0.0522 _diffrn_reflns_av_sigmaI/netI 0.0492 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 28.90 _reflns_number_total 2013 _reflns_number_gt 1556 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Saint' _computing_cell_refinement 'Bruker Saint' _computing_data_reduction 'Bruker Smart' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Platon (Spek, 2008)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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 w=1/[\s^2^(Fo^2^)+(0.0606P)^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 2013 _refine_ls_number_parameters 151 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0611 _refine_ls_R_factor_gt 0.0410 _refine_ls_wR_factor_ref 0.1076 _refine_ls_wR_factor_gt 0.0991 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.061 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.04340(5) 0.11932(9) 0.67802(3) 0.01396(15) Uani 1 d . . . Ni2 Ni 0.5000 0.0000 1.0000 0.01586(19) Uani 1 d S . . O1 O 0.0800(4) 0.2662(6) 0.55602(19) 0.0263(7) Uani 1 d D . . H1A H 0.160(2) 0.264(9) 0.549(3) 0.032 Uiso 1 d D . . H1B H 0.025(4) 0.231(9) 0.5056(17) 0.032 Uiso 1 d D . . O2 O 0.1087(3) -0.2193(5) 0.6346(2) 0.0227(6) Uani 1 d D . . H2A H 0.073(5) -0.321(7) 0.662(3) 0.027 Uiso 1 d D . . H2B H 0.1938(16) -0.236(9) 0.661(3) 0.027 Uiso 1 d D . . O3 O 0.0469(3) -0.0429(5) 0.80259(17) 0.0152(5) Uani 1 d . . . C4 C 0.1800(4) -0.0180(7) 0.8669(2) 0.0140(7) Uani 1 d . . . H4 H 0.187(4) 0.080(7) 0.918(3) 0.017 Uiso 1 d . . . C5 C 0.2887(4) 0.1138(6) 0.8258(2) 0.0142(7) Uani 1 d . . . O6 O 0.2450(3) 0.2035(5) 0.74467(18) 0.0185(6) Uani 1 d . . . O7 O 0.4143(3) 0.1437(5) 0.87363(18) 0.0191(6) Uani 1 d . . . C8 C 0.2350(4) -0.2648(7) 0.9156(2) 0.0154(7) Uani 1 d . . . O9 O 0.1574(3) -0.4528(5) 0.89374(19) 0.0195(6) Uani 1 d . . . O10 O 0.3511(3) -0.2689(5) 0.97853(19) 0.0224(6) Uani 1 d . . . O11 O 0.3876(3) 0.2627(6) 1.0632(2) 0.0255(6) Uani 1 d D . . H11A H 0.381(5) 0.399(4) 1.038(3) 0.031 Uiso 1 d D . . H11B H 0.438(4) 0.292(9) 1.1156(15) 0.031 Uiso 1 d D . . O100 O 0.6000(4) 0.1576(6) 0.7537(3) 0.0399(9) Uani 1 d D . . H10A H 0.561(6) 0.180(10) 0.795(3) 0.048 Uiso 1 d D . . H10B H 0.638(6) 0.021(5) 0.754(4) 0.048 Uiso 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 0.0114(3) 0.0135(3) 0.0152(2) 0.00031(17) 0.00069(17) 0.00083(18) Ni2 0.0113(4) 0.0162(4) 0.0168(3) 0.0014(3) -0.0016(3) -0.0027(3) O1 0.0300(18) 0.0301(17) 0.0195(14) 0.0044(13) 0.0081(13) 0.0056(15) O2 0.0254(16) 0.0156(14) 0.0278(15) -0.0014(12) 0.0085(13) 0.0013(13) O3 0.0109(13) 0.0147(12) 0.0181(12) 0.0017(10) 0.0010(10) -0.0012(10) C4 0.0118(18) 0.0156(18) 0.0141(16) 0.0005(14) 0.0024(14) -0.0005(14) C5 0.0147(18) 0.0117(17) 0.0151(16) -0.0001(13) 0.0025(14) -0.0007(14) O6 0.0141(14) 0.0209(14) 0.0177(13) 0.0043(10) -0.0001(10) -0.0021(11) O7 0.0131(14) 0.0224(14) 0.0185(13) 0.0029(11) -0.0011(10) -0.0036(11) C8 0.0130(18) 0.0148(17) 0.0179(17) 0.0006(15) 0.0033(14) 0.0011(15) O9 0.0139(14) 0.0132(13) 0.0272(15) 0.0020(11) -0.0013(11) -0.0018(11) O10 0.0169(14) 0.0172(14) 0.0260(14) 0.0063(11) -0.0062(11) -0.0050(12) O11 0.0263(17) 0.0217(16) 0.0264(15) 0.0039(13) 0.0040(13) 0.0021(13) O100 0.042(2) 0.0262(17) 0.061(2) 0.0014(17) 0.029(2) 0.0035(16) _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 2.027(3) 2_556 ? Ni1 O6 2.028(3) . ? Ni1 O3 2.075(3) . ? Ni1 O3 2.102(3) 2_556 ? Ni1 O2 2.119(3) . ? Ni1 O1 2.134(3) . ? Ni2 O7 2.025(3) . ? Ni2 O7 2.025(3) 3_657 ? Ni2 O10 2.042(3) 3_657 ? Ni2 O10 2.042(3) . ? Ni2 O11 2.189(3) 3_657 ? Ni2 O11 2.189(3) . ? O1 H1A 0.829(10) . ? O1 H1B 0.829(10) . ? O2 H2A 0.831(10) . ? O2 H2B 0.833(10) . ? O3 C4 1.414(4) . ? O3 Ni1 2.102(3) 2_546 ? C4 C8 1.558(5) . ? C4 C5 1.560(5) . ? C4 H4 0.93(4) . ? C5 O7 1.267(5) . ? C5 O6 1.282(4) . ? C8 O9 1.268(5) . ? C8 O10 1.276(4) . ? O9 Ni1 2.027(3) 2_546 ? O11 H11A 0.829(10) . ? O11 H11B 0.828(10) . ? O100 H10A 0.830(10) . ? O100 H10B 0.831(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 O6 177.07(11) 2_556 . ? O9 Ni1 O3 99.95(12) 2_556 . ? O6 Ni1 O3 82.91(11) . . ? O9 Ni1 O3 81.44(11) 2_556 2_556 ? O6 Ni1 O3 97.57(11) . 2_556 ? O3 Ni1 O3 98.47(7) . 2_556 ? O9 Ni1 O2 90.23(12) 2_556 . ? O6 Ni1 O2 90.45(12) . . ? O3 Ni1 O2 88.91(12) . . ? O3 Ni1 O2 169.69(11) 2_556 . ? O9 Ni1 O1 89.12(13) 2_556 . ? O6 Ni1 O1 88.10(13) . . ? O3 Ni1 O1 169.29(12) . . ? O3 Ni1 O1 88.45(12) 2_556 . ? O2 Ni1 O1 85.33(12) . . ? O7 Ni2 O7 179.999(1) . 3_657 ? O7 Ni2 O10 88.27(12) . 3_657 ? O7 Ni2 O10 91.73(12) 3_657 3_657 ? O7 Ni2 O10 91.73(12) . . ? O7 Ni2 O10 88.27(12) 3_657 . ? O10 Ni2 O10 180.0 3_657 . ? O7 Ni2 O11 88.36(12) . 3_657 ? O7 Ni2 O11 91.64(12) 3_657 3_657 ? O10 Ni2 O11 96.09(13) 3_657 3_657 ? O10 Ni2 O11 83.91(13) . 3_657 ? O7 Ni2 O11 91.63(12) . . ? O7 Ni2 O11 88.37(12) 3_657 . ? O10 Ni2 O11 83.91(13) 3_657 . ? O10 Ni2 O11 96.09(13) . . ? O11 Ni2 O11 179.998(2) 3_657 . ? Ni1 O1 H1A 120(3) . . ? Ni1 O1 H1B 119(3) . . ? H1A O1 H1B 107(5) . . ? Ni1 O2 H2A 102(3) . . ? Ni1 O2 H2B 108(3) . . ? H2A O2 H2B 102(4) . . ? C4 O3 Ni1 111.3(2) . . ? C4 O3 Ni1 109.9(2) . 2_546 ? Ni1 O3 Ni1 126.79(13) . 2_546 ? O3 C4 C8 112.4(3) . . ? O3 C4 C5 112.7(3) . . ? C8 C4 C5 113.3(3) . . ? O3 C4 H4 118(3) . . ? C8 C4 H4 99(3) . . ? C5 C4 H4 100(3) . . ? O7 C5 O6 121.2(4) . . ? O7 C5 C4 120.6(3) . . ? O6 C5 C4 118.0(3) . . ? C5 O6 Ni1 114.7(2) . . ? C5 O7 Ni2 125.5(2) . . ? O9 C8 O10 122.5(4) . . ? O9 C8 C4 117.7(3) . . ? O10 C8 C4 119.6(3) . . ? C8 O9 Ni1 114.8(2) . 2_546 ? C8 O10 Ni2 124.8(2) . . ? Ni2 O11 H11A 112(3) . . ? Ni2 O11 H11B 108(4) . . ? H11A O11 H11B 103(5) . . ? H10A O100 H10B 115(6) . . ? _diffrn_measured_fraction_theta_max 0.968 _diffrn_reflns_theta_full 28.90 _diffrn_measured_fraction_theta_full 0.968 _refine_diff_density_max 1.233 _refine_diff_density_min -0.726 _refine_diff_density_rms 0.149 _database_code_depnum_ccdc_archive 'CCDC 890224'