# Supplementary Material (ESI) for New Journal of Chemistry # This journal is (c) The Royal Society of Chemistry and The Centre National de la Recherche Scientifique, 2010 data_global _journal_name_full 'New J.Chem.' _journal_coden_cambridge 0440 #TrackingRef 'NJCWeilee.cif' #============================================================================== # 1. SUBMISSION DETAILS _publ_contact_author # Name and address of author for correspondence ; Dr. Jagadese J. Vittal Department of Chemistry National University of Singapore 3 Science Drive 3 SINGAPORE 117543 ; _publ_contact_author_phone '(65) 6516 2677' _publ_contact_author_fax '(65) 6779 1691' _publ_contact_author_email chmjjv@nus.edu.sg _publ_requested_coeditor_name ' ' _publ_contact_letter ; '' ; #============================================================================== # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _iucr_compatibility_tag ACTA95 _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; Alkali Metal Ion Directed Self-Assembled Ni(II) Molecular Clusters ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address 'Wei Lee Leong' ; Department of Chemistry National University of Singapore SINGAPORE 117543 ; 'Jagadese J. Vittal' ; Department of Chemistry National University of Singapore SINGAPORE 117543 ; _publ_contact_author_name 'Dr. Jagadese J. Vittal' #============================================================================== data_compound_H2mugly _database_code_depnum_ccdc_archive 'CCDC 768058' # data_7457a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C13 H15 N O6' _chemical_formula_weight 281.26 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/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 11.6019(13) _cell_length_b 15.159(2) _cell_length_c 7.5024(9) _cell_angle_alpha 90.00 _cell_angle_beta 103.930(3) _cell_angle_gamma 90.00 _cell_volume 1280.7(3) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 770 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 20.24 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.04 #_exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.459 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 592 _exptl_absorpt_coefficient_mu 0.117 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9592 _exptl_absorpt_correction_T_max 0.9953 _exptl_absorpt_process_details 'SADABS, Sheldrick,2005' _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 8861 _diffrn_reflns_av_R_equivalents 0.0492 _diffrn_reflns_av_sigmaI/netI 0.0584 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 27.46 _reflns_number_total 2927 _reflns_number_gt 1806 _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. The two restraints applied are: DFIX option to fix the O-H distance in water. ; _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^)+(0.1057P)^2^+1.3075P] 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 2927 _refine_ls_number_parameters 197 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1359 _refine_ls_R_factor_gt 0.0846 _refine_ls_wR_factor_ref 0.2384 _refine_ls_wR_factor_gt 0.2103 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _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 N1 N 0.4876(2) 0.87449(18) 0.1738(4) 0.0327(7) Uani 1 1 d . . . H1N H 0.480(3) 0.893(3) 0.051(6) 0.047(11) Uiso 1 1 d . . . H2N H 0.502(3) 0.812(3) 0.170(5) 0.048(11) Uiso 1 1 d . . . O1 O 0.3369(2) 0.71511(15) 0.2032(3) 0.0392(6) Uani 1 1 d . . . H1O H 0.3177 0.6623 0.1910 0.059 Uiso 1 1 calc R . . O2 O 0.5156(2) 1.05197(14) 0.1742(3) 0.0389(6) Uani 1 1 d . . . O3 O 0.6967(2) 1.04831(15) 0.3614(4) 0.0452(7) Uani 1 1 d . . . O4 O 0.2086(2) 0.99778(16) 0.0034(4) 0.0530(8) Uani 1 1 d . . . O5 O 0.1658(3) 1.1346(2) -0.0874(7) 0.0959(14) Uani 1 1 d . . . C1 C 0.2513(3) 0.7647(2) 0.0970(5) 0.0315(7) Uani 1 1 d . . . C2 C 0.1497(3) 0.7286(2) -0.0170(5) 0.0389(8) Uani 1 1 d . . . H2 H 0.1381 0.6672 -0.0206 0.047 Uiso 1 1 calc R . . C3 C 0.0664(3) 0.7829(3) -0.1239(5) 0.0431(9) Uani 1 1 d . . . H3 H -0.0026 0.7581 -0.1995 0.052 Uiso 1 1 calc R . . C4 C 0.0823(3) 0.8749(3) -0.1225(5) 0.0450(10) Uani 1 1 d . . . C5 C 0.1846(3) 0.9085(2) -0.0066(5) 0.0396(9) Uani 1 1 d . . . C6 C 0.2700(3) 0.8559(2) 0.1075(5) 0.0330(8) Uani 1 1 d . . . C7 C 0.3772(3) 0.8917(2) 0.2389(5) 0.0365(8) Uani 1 1 d . . . H7A H 0.3848 0.8643 0.3595 0.044 Uiso 1 1 calc R . . H7B H 0.3677 0.9554 0.2526 0.044 Uiso 1 1 calc R . . C8 C 0.5977(3) 0.9130(2) 0.2919(5) 0.0376(8) Uani 1 1 d . . . H8A H 0.6667 0.8867 0.2585 0.045 Uiso 1 1 calc R . . H8B H 0.6019 0.8978 0.4203 0.045 Uiso 1 1 calc R . . C9 C 0.6035(3) 1.0135(2) 0.2742(5) 0.0328(8) Uani 1 1 d . . . C10 C 0.1349(4) 1.0572(3) -0.1042(8) 0.0723(16) Uani 1 1 d . . . C11 C 0.0290(5) 1.0232(3) -0.2231(8) 0.0781(18) Uani 1 1 d . . . H11 H -0.0240 1.0632 -0.2963 0.094 Uiso 1 1 calc R . . C12 C 0.0010(4) 0.9354(4) -0.2357(6) 0.0635(14) Uani 1 1 d . . . C13 C -0.1114(4) 0.9013(5) -0.3618(7) 0.0885(19) Uani 1 1 d . . . H13A H -0.1535 0.9498 -0.4336 0.133 Uiso 1 1 calc R . . H13B H -0.1614 0.8750 -0.2895 0.133 Uiso 1 1 calc R . . H13C H -0.0918 0.8573 -0.4436 0.133 Uiso 1 1 calc R . . O1S O 0.6060(4) 0.7032(2) 0.2586(9) 0.1172(19) Uani 1 1 d D . . H1S H 0.572(4) 0.6516(19) 0.267(7) 0.080 Uiso 1 1 d D . . H2S H 0.676(3) 0.703(4) 0.343(6) 0.080 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 N1 0.0317(15) 0.0200(13) 0.0461(19) -0.0057(13) 0.0087(13) -0.0057(11) O1 0.0386(14) 0.0215(11) 0.0520(15) 0.0046(11) 0.0000(11) 0.0040(10) O2 0.0399(14) 0.0227(12) 0.0505(15) -0.0014(11) 0.0036(11) -0.0028(10) O3 0.0409(14) 0.0243(12) 0.0628(17) -0.0022(12) -0.0026(12) -0.0089(11) O4 0.0528(16) 0.0232(12) 0.095(2) 0.0182(14) 0.0404(16) 0.0124(12) O5 0.101(3) 0.0353(17) 0.178(4) 0.043(2) 0.084(3) 0.0286(18) C1 0.0299(17) 0.0248(16) 0.0395(18) 0.0012(14) 0.0075(14) 0.0012(13) C2 0.038(2) 0.0324(18) 0.045(2) -0.0025(16) 0.0065(16) -0.0069(15) C3 0.0276(18) 0.056(2) 0.043(2) 0.0078(18) 0.0035(15) -0.0069(17) C4 0.0294(18) 0.053(2) 0.054(2) 0.0198(19) 0.0135(17) 0.0104(17) C5 0.038(2) 0.0265(17) 0.061(2) 0.0130(16) 0.0249(18) 0.0062(15) C6 0.0306(17) 0.0245(16) 0.047(2) 0.0011(14) 0.0152(15) -0.0006(13) C7 0.0377(19) 0.0243(16) 0.050(2) -0.0081(15) 0.0149(16) -0.0040(14) C8 0.0317(18) 0.0243(16) 0.054(2) 0.0007(15) 0.0055(16) -0.0030(14) C9 0.0368(18) 0.0222(15) 0.0393(18) -0.0042(14) 0.0090(15) -0.0037(14) C10 0.059(3) 0.048(3) 0.129(5) 0.043(3) 0.058(3) 0.029(2) C11 0.070(3) 0.075(3) 0.103(4) 0.067(3) 0.047(3) 0.049(3) C12 0.038(2) 0.090(4) 0.068(3) 0.044(3) 0.024(2) 0.027(2) C13 0.042(3) 0.136(5) 0.082(4) 0.048(4) 0.004(2) 0.021(3) O1S 0.081(3) 0.0352(18) 0.256(6) 0.011(3) 0.081(3) -0.004(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C8 1.487(4) . ? N1 C7 1.500(4) . ? O1 C1 1.344(4) . ? O2 C9 1.255(4) . ? O3 C9 1.239(4) . ? O4 C10 1.365(5) . ? O4 C5 1.381(4) . ? O5 C10 1.225(6) . ? C1 C2 1.392(4) . ? C1 C6 1.399(4) . ? C2 C3 1.372(5) . ? C3 C4 1.407(5) . ? C4 C5 1.389(5) . ? C4 C12 1.438(5) . ? C5 C6 1.393(5) . ? C6 C7 1.491(5) . ? C8 C9 1.532(4) . ? C10 C11 1.429(8) . ? C11 C12 1.368(7) . ? C12 C13 1.506(7) . ? 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 C8 N1 C7 114.6(3) . . ? C10 O4 C5 121.7(4) . . ? O1 C1 C2 122.7(3) . . ? O1 C1 C6 115.9(3) . . ? C2 C1 C6 121.4(3) . . ? C3 C2 C1 119.8(3) . . ? C2 C3 C4 121.2(3) . . ? C5 C4 C3 117.3(3) . . ? C5 C4 C12 118.5(4) . . ? C3 C4 C12 124.2(4) . . ? O4 C5 C4 121.6(3) . . ? O4 C5 C6 115.0(3) . . ? C4 C5 C6 123.3(3) . . ? C5 C6 C1 116.9(3) . . ? C5 C6 C7 123.7(3) . . ? C1 C6 C7 119.4(3) . . ? C6 C7 N1 111.3(3) . . ? N1 C8 C9 112.8(3) . . ? O3 C9 O2 126.7(3) . . ? O3 C9 C8 115.4(3) . . ? O2 C9 C8 117.9(3) . . ? O5 C10 O4 116.5(5) . . ? O5 C10 C11 126.6(5) . . ? O4 C10 C11 117.0(4) . . ? C12 C11 C10 123.2(4) . . ? C11 C12 C4 118.0(4) . . ? C11 C12 C13 122.2(4) . . ? C4 C12 C13 119.9(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 N1 H1N O2 0.95(4) 1.89(4) 2.831(4) 169(4) 3_675 N1 H2N O1S 0.97(4) 2.05(4) 2.936(5) 151(3) . N1 H2N O1 0.97(4) 2.47(4) 3.021(4) 116(3) . O1 H1O O3 0.83 1.77 2.586(3) 166.8 2_645 O1 H1O O2 0.83 2.57 3.022(3) 115.3 2_645 O1S H1S O2 0.885(19) 1.93(2) 2.800(4) 168(5) 2_645 O1S H2S O5 0.897(19) 2.49(3) 3.321(8) 154(5) 2_645 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.846 _refine_diff_density_min -0.294 _refine_diff_density_rms 0.069 #===#END data_jj _database_code_depnum_ccdc_archive 'CCDC 768059' #TrackingRef 'NJCWeilee.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H15 N O5' _chemical_formula_weight 277.27 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 5.3583(5) _cell_length_b 5.8497(6) _cell_length_c 10.4352(10) _cell_angle_alpha 88.144(2) _cell_angle_beta 75.461(2) _cell_angle_gamma 82.331(2) _cell_volume 313.78(5) _cell_formula_units_Z 1 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 1161 _cell_measurement_theta_min 3.51 _cell_measurement_theta_max 27.56 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.12 #_exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.467 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 146 _exptl_absorpt_coefficient_mu 0.112 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9671 _exptl_absorpt_correction_T_max 0.9866 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2005)' _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3256 _diffrn_reflns_av_R_equivalents 0.0066 _diffrn_reflns_av_sigmaI/netI 0.0177 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 27.48 _reflns_number_total 1669 _reflns_number_gt 1624 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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. This 3 restraints may be due to the chiral space group. floating origin restraints" as described in the Bruker's manual. It says there that this is better than fxing the origin. This should not happen in a centro symmetric case where the origin is fixed. ; _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^)+(0.0624P)^2^+0.0729P] 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 riding _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 0.2(12) _refine_ls_number_reflns 1669 _refine_ls_number_parameters 184 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0398 _refine_ls_R_factor_gt 0.0388 _refine_ls_wR_factor_ref 0.1018 _refine_ls_wR_factor_gt 0.1007 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.069 _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 N1 N 0.4323(3) 1.0302(3) 0.74907(19) 0.0237(4) Uani 1 1 d . . . H1A H 0.6061 1.0138 0.7108 0.028 Uiso 1 1 calc R . . H1B H 0.3914 0.8910 0.7834 0.028 Uiso 1 1 calc R . . O1 O 0.6931(3) 1.0370(3) 0.41734(18) 0.0300(4) Uani 1 1 d . . . O2 O 1.0462(4) 1.1746(3) 0.3031(2) 0.0439(5) Uani 1 1 d . . . O3 O -0.0613(3) 0.7704(3) 0.67969(19) 0.0323(4) Uani 1 1 d . . . H3 H -0.1395 0.6554 0.6879 0.048 Uiso 1 1 calc R . . O4 O 0.3509(4) 1.6087(3) 0.86349(19) 0.0351(4) Uani 1 1 d . . . O5 O 0.6880(4) 1.4101(3) 0.7216(2) 0.0376(4) Uani 1 1 d . . . C1 C 0.8966(5) 1.0371(4) 0.3054(3) 0.0323(5) Uani 1 1 d . . . C2 C 0.9080(5) 0.8754(4) 0.2022(3) 0.0337(5) Uani 1 1 d . . . H2 H 1.0403 0.8766 0.1237 0.040 Uiso 1 1 calc R . . C3 C 0.7361(4) 0.7224(4) 0.2139(2) 0.0287(5) Uani 1 1 d . . . C4 C 0.5322(4) 0.7206(4) 0.3341(2) 0.0266(5) Uani 1 1 d . . . C5 C 0.3427(5) 0.5703(4) 0.3576(3) 0.0296(5) Uani 1 1 d . . . H5 H 0.3505 0.4576 0.2940 0.036 Uiso 1 1 calc R . . C6 C 0.1460(4) 0.5840(4) 0.4714(3) 0.0296(5) Uani 1 1 d . . . H6 H 0.0208 0.4814 0.4852 0.036 Uiso 1 1 calc R . . C7 C 0.1318(4) 0.7513(3) 0.5671(2) 0.0261(5) Uani 1 1 d . . . C8 C 0.3155(4) 0.9052(4) 0.5474(2) 0.0259(5) Uani 1 1 d . . . C9 C 0.5137(4) 0.8844(3) 0.4315(2) 0.0253(5) Uani 1 1 d . . . C10 C 0.7568(6) 0.5551(4) 0.1036(3) 0.0378(6) Uani 1 1 d . . . H10A H 0.9006 0.5831 0.0298 0.057 Uiso 1 1 calc R . . H10B H 0.5966 0.5762 0.0749 0.057 Uiso 1 1 calc R . . H10C H 0.7866 0.3985 0.1351 0.057 Uiso 1 1 calc R . . C11 C 0.2884(4) 1.0969(4) 0.6450(2) 0.0266(5) Uani 1 1 d . . . H11A H 0.3544 1.2322 0.5973 0.032 Uiso 1 1 calc R . . H11B H 0.1038 1.1400 0.6878 0.032 Uiso 1 1 calc R . . C12 C 0.3720(4) 1.2029(4) 0.8598(2) 0.0265(5) Uani 1 1 d . . . H12 H 0.1812 1.2338 0.8955 0.032 Uiso 1 1 calc R . . C13 C 0.4959(6) 1.1027(4) 0.9684(3) 0.0390(6) Uani 1 1 d . . . H13A H 0.6835 1.0919 0.9374 0.059 Uiso 1 1 calc R . . H13B H 0.4466 0.9502 0.9915 0.059 Uiso 1 1 calc R . . H13C H 0.4367 1.2019 1.0457 0.059 Uiso 1 1 calc R . . C14 C 0.4776(4) 1.4298(4) 0.8090(2) 0.0266(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.0259(8) 0.0163(7) 0.0281(10) -0.0019(7) -0.0043(7) -0.0040(6) O1 0.0318(8) 0.0259(8) 0.0350(9) -0.0031(7) -0.0088(7) -0.0113(6) O2 0.0437(10) 0.0435(10) 0.0484(12) -0.0016(8) -0.0082(9) -0.0249(8) O3 0.0315(8) 0.0248(8) 0.0390(10) 0.0002(6) -0.0032(7) -0.0092(6) O4 0.0419(9) 0.0198(7) 0.0397(10) -0.0026(7) -0.0019(7) -0.0056(6) O5 0.0333(8) 0.0238(7) 0.0497(11) -0.0029(7) 0.0047(8) -0.0105(6) C1 0.0305(11) 0.0309(11) 0.0376(14) 0.0052(10) -0.0094(10) -0.0109(9) C2 0.0319(11) 0.0380(12) 0.0309(13) 0.0025(10) -0.0044(10) -0.0103(9) C3 0.0303(11) 0.0283(11) 0.0288(12) 0.0009(9) -0.0099(10) -0.0037(9) C4 0.0271(10) 0.0239(10) 0.0303(12) -0.0002(8) -0.0092(9) -0.0049(8) C5 0.0343(11) 0.0254(10) 0.0329(12) -0.0020(9) -0.0135(10) -0.0069(8) C6 0.0306(11) 0.0235(10) 0.0395(13) 0.0028(9) -0.0141(10) -0.0110(9) C7 0.0270(11) 0.0215(10) 0.0318(12) 0.0028(9) -0.0112(10) -0.0036(8) C8 0.0286(11) 0.0203(9) 0.0319(12) 0.0001(8) -0.0128(9) -0.0040(8) C9 0.0258(10) 0.0215(10) 0.0324(13) 0.0027(9) -0.0123(9) -0.0075(8) C10 0.0447(14) 0.0358(13) 0.0319(13) -0.0023(10) -0.0062(11) -0.0081(11) C11 0.0293(10) 0.0185(9) 0.0332(12) -0.0015(8) -0.0100(9) -0.0024(8) C12 0.0299(10) 0.0192(9) 0.0289(11) -0.0040(8) -0.0013(9) -0.0087(8) C13 0.0586(16) 0.0264(11) 0.0353(14) 0.0032(10) -0.0133(12) -0.0148(11) C14 0.0330(11) 0.0192(9) 0.0300(11) 0.0007(8) -0.0096(9) -0.0086(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 N1 C11 1.496(3) . ? N1 C12 1.504(2) . ? O1 C9 1.376(2) . ? O1 C1 1.383(3) . ? O2 C1 1.205(3) . ? O3 C7 1.353(3) . ? O4 C14 1.239(3) . ? O5 C14 1.254(3) . ? C1 C2 1.441(4) . ? C2 C3 1.350(3) . ? C3 C4 1.443(3) . ? C3 C10 1.508(3) . ? C4 C9 1.396(3) . ? C4 C5 1.401(3) . ? C5 C6 1.373(4) . ? C6 C7 1.402(3) . ? C7 C8 1.394(3) . ? C8 C9 1.391(3) . ? C8 C11 1.507(3) . ? C12 C13 1.517(4) . ? C12 C14 1.538(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C11 N1 C12 113.25(16) . . ? C9 O1 C1 121.54(17) . . ? O2 C1 O1 116.7(2) . . ? O2 C1 C2 126.2(2) . . ? O1 C1 C2 117.1(2) . . ? C3 C2 C1 122.6(2) . . ? C2 C3 C4 118.9(2) . . ? C2 C3 C10 120.7(2) . . ? C4 C3 C10 120.4(2) . . ? C9 C4 C5 117.3(2) . . ? C9 C4 C3 118.55(19) . . ? C5 C4 C3 124.1(2) . . ? C6 C5 C4 121.4(2) . . ? C5 C6 C7 119.9(2) . . ? O3 C7 C8 118.21(19) . . ? O3 C7 C6 121.22(19) . . ? C8 C7 C6 120.6(2) . . ? C9 C8 C7 117.89(19) . . ? C9 C8 C11 121.44(19) . . ? C7 C8 C11 120.6(2) . . ? O1 C9 C8 115.90(18) . . ? O1 C9 C4 121.20(19) . . ? C8 C9 C4 122.90(19) . . ? N1 C11 C8 112.53(17) . . ? N1 C12 C13 108.74(18) . . ? N1 C12 C14 110.37(17) . . ? C13 C12 C14 109.98(18) . . ? O4 C14 O5 127.9(2) . . ? O4 C14 C12 116.2(2) . . ? O5 C14 C12 115.91(17) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.229 _refine_diff_density_min -0.225 _refine_diff_density_rms 0.054 #===#END data_compound_2a _database_code_depnum_ccdc_archive 'CCDC 768060' #data_8582 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C78 H96 N6 Na6 Ni7 O49' _chemical_formula_weight 2450.52 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' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M R-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 15.4367(9) _cell_length_b 15.4367(9) _cell_length_c 35.721(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 7371.6(10) _cell_formula_units_Z 3 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 1678 _cell_measurement_theta_min 2.66 _cell_measurement_theta_max 19.71 _exptl_crystal_description Block _exptl_crystal_colour Green _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 #_exptl_crystal_density_meas 'Not Measured' _exptl_crystal_density_diffrn 1.656 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3780 _exptl_absorpt_coefficient_mu 1.439 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7061 _exptl_absorpt_correction_T_max 0.8025 _exptl_absorpt_process_details 'Sadabs, (Sheldrick 2005)' _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 13252 _diffrn_reflns_av_R_equivalents 0.0871 _diffrn_reflns_av_sigmaI/netI 0.0887 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 43 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 25.48 _reflns_number_total 3003 _reflns_number_gt 1557 _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. The cation was highly disordered since they are located near 3-fold rotation. The mu-OH on the Na3 plane is diordered on both sides. We were not able to locate the H atoms of the water molecules attached to Na(I) or in the lattice. Treatment of oxygen atoms: We tried to assess the oxygen occupancies from the sizes of electron density and refined them. But the refinement was stable and the U(iso) was not converging. Further new prominent electron densities started appearing. Hence we refine a common U(iso) for all the O atoms of disordered water molecules. This seems to be the best model among many tried. ; _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^)+(0.1000P)^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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3003 _refine_ls_number_parameters 222 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1393 _refine_ls_R_factor_gt 0.0795 _refine_ls_wR_factor_ref 0.2110 _refine_ls_wR_factor_gt 0.1900 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _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 0.78792(7) 0.80967(7) 1.00279(2) 0.0553(4) Uani 1 1 d . . . Ni2 Ni 1.0000 1.0000 1.0000 0.0445(5) Uani 1 6 d S . . O1 O 0.7405(3) 0.8882(4) 0.96687(12) 0.0595(13) Uani 1 1 d . . . C1 C 0.7478(6) 0.8722(7) 0.9305(2) 0.070(2) Uani 1 1 d . . . C2 C 0.7997(6) 0.9482(7) 0.9044(2) 0.077(2) Uani 1 1 d . . . H2 H 0.8285 1.0154 0.9118 0.092 Uiso 1 1 calc R . . C3 C 0.8093(7) 0.9252(8) 0.8671(2) 0.089(3) Uani 1 1 d . . . H3 H 0.8462 0.9778 0.8503 0.107 Uiso 1 1 calc R . . C4 C 0.7669(7) 0.8293(9) 0.8547(2) 0.085(3) Uani 1 1 d . . . C5 C 0.7077(7) 0.7533(8) 0.8796(2) 0.087(3) Uani 1 1 d . . . C6 C 0.6985(6) 0.7716(7) 0.9177(2) 0.077(2) Uani 1 1 d . . . C7 C 0.6383(6) 0.6879(7) 0.9455(2) 0.079(2) Uani 1 1 d . . . H7A H 0.5911 0.7020 0.9588 0.095 Uiso 1 1 calc R . . H7B H 0.5997 0.6246 0.9320 0.095 Uiso 1 1 calc R . . N1 N 0.7040(5) 0.6780(4) 0.97284(16) 0.0697(18) Uani 1 1 d . . . H1 H 0.7462 0.6614 0.9606 0.084 Uiso 1 1 calc R . . C8 C 0.6460(7) 0.6007(7) 1.0023(2) 0.084(3) Uani 1 1 d . . . H8A H 0.6885 0.5777 1.0138 0.101 Uiso 1 1 calc R . . H8B H 0.5883 0.5430 0.9909 0.101 Uiso 1 1 calc R . . C9 C 0.6098(7) 0.6489(8) 1.0327(2) 0.086(3) Uani 1 1 d . . . O2 O 0.6577(4) 0.7440(5) 1.03493(13) 0.0739(16) Uani 1 1 d . . . O3 O 0.5411(5) 0.5893(5) 1.05347(15) 0.113(3) Uani 1 1 d . . . C10 C 0.7726(8) 0.7966(10) 0.8163(2) 0.094(3) Uani 1 1 d . . . C11 C 0.7244(10) 0.7000(11) 0.8070(3) 0.113(4) Uani 1 1 d . . . H11 H 0.7311 0.6814 0.7826 0.136 Uiso 1 1 calc R . . C12 C 0.6628(10) 0.6236(11) 0.8333(3) 0.109(4) Uani 1 1 d . . . C13 C 0.8353(9) 0.8764(10) 0.7874(3) 0.130(4) Uani 1 1 d . . . H13A H 0.8269 0.8454 0.7630 0.194 Uiso 1 1 calc R . . H13B H 0.9052 0.9093 0.7946 0.194 Uiso 1 1 calc R . . H13C H 0.8135 0.9254 0.7861 0.194 Uiso 1 1 calc R . . O4 O 0.6561(5) 0.6526(5) 0.86928(15) 0.103(2) Uani 1 1 d . . . O5 O 0.6124(7) 0.5364(7) 0.82752(19) 0.135(3) Uani 1 1 d . . . O6 O 0.8638(3) 0.9457(3) 1.02734(12) 0.0510(12) Uani 1 1 d . . . H6 H 0.867(5) 0.951(5) 1.051(2) 0.061 Uiso 1 1 d . . . Na1 Na 0.4142(3) 0.5806(3) 1.10642(11) 0.1152(14) Uani 1 1 d . . . O7 O 0.2227(6) 0.4246(7) 1.0918(2) 0.144(3) Uani 1 1 d . . . O8 O 0.3333 0.6667 1.0563(13) 0.198(6) Uiso 0.50 3 d SP . . O8A O 0.3333 0.6667 1.1338(10) 0.198(6) Uiso 0.50 3 d SP . . O1W O 0.356(5) 0.724(3) 1.0232(12) 0.198(6) Uiso 0.25 1 d P . . O2W O 0.3333 0.6667 1.1667 0.198(6) Uiso 1 6 d S . . O3W O 0.3333 0.6667 0.9940(7) 0.198(6) Uiso 1 3 d S . . O4W O 0.3333 0.6667 0.955(2) 0.198(6) Uiso 0.25 3 d SP . . 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 0.0535(7) 0.0602(7) 0.0436(5) -0.0031(4) -0.0013(4) 0.0220(5) Ni2 0.0511(9) 0.0511(9) 0.0312(10) 0.000 0.000 0.0256(4) O1 0.054(3) 0.074(4) 0.048(3) -0.007(2) -0.009(2) 0.029(3) C1 0.064(5) 0.099(7) 0.053(5) -0.010(4) -0.013(4) 0.046(5) C2 0.087(6) 0.094(7) 0.052(4) 0.000(4) -0.016(4) 0.047(5) C3 0.080(7) 0.119(9) 0.060(5) 0.001(5) -0.018(4) 0.044(6) C4 0.088(7) 0.121(9) 0.045(4) -0.008(5) -0.020(4) 0.051(6) C5 0.088(7) 0.110(8) 0.061(5) -0.020(5) -0.034(5) 0.048(6) C6 0.067(6) 0.108(8) 0.057(5) -0.013(5) -0.019(4) 0.045(6) C7 0.061(5) 0.097(7) 0.063(5) -0.023(4) -0.014(4) 0.026(5) N1 0.068(4) 0.064(4) 0.058(4) -0.011(3) 0.001(3) 0.018(4) C8 0.070(6) 0.071(6) 0.076(5) -0.012(4) -0.004(4) 0.008(5) C9 0.066(6) 0.084(7) 0.067(5) -0.010(5) 0.001(4) 0.006(6) O2 0.062(4) 0.080(4) 0.062(3) -0.015(3) 0.005(2) 0.022(3) O3 0.087(5) 0.111(5) 0.069(4) -0.008(3) 0.014(3) -0.005(4) C10 0.091(7) 0.149(10) 0.053(5) -0.014(6) -0.017(5) 0.067(8) C11 0.134(10) 0.164(12) 0.055(6) -0.027(7) -0.012(6) 0.084(10) C12 0.123(10) 0.130(11) 0.082(7) -0.049(7) -0.053(7) 0.068(9) C13 0.133(10) 0.191(13) 0.068(6) 0.000(7) -0.008(6) 0.084(9) O4 0.108(5) 0.123(6) 0.064(4) -0.035(4) -0.022(3) 0.048(5) O5 0.165(8) 0.135(7) 0.089(5) -0.053(5) -0.031(5) 0.064(7) O6 0.060(3) 0.058(3) 0.034(2) 0.002(2) 0.005(2) 0.029(3) Na1 0.097(3) 0.132(4) 0.091(3) 0.006(2) 0.008(2) 0.038(3) O7 0.131(7) 0.214(10) 0.104(5) -0.021(5) -0.010(4) 0.100(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 O6 2.023(5) . ? Ni1 O6 2.053(5) 12_657 ? Ni1 N1 2.078(6) . ? Ni1 O2 2.085(5) . ? Ni1 O1 2.089(5) 12_657 ? Ni1 O1 2.130(5) . ? Ni2 O6 2.077(4) 3_675 ? Ni2 O6 2.077(4) 12_657 ? Ni2 O6 2.077(4) . ? Ni2 O6 2.077(4) 2_765 ? Ni2 O6 2.077(4) 10_777 ? Ni2 O6 2.077(4) 11_567 ? O1 C1 1.336(8) . ? O1 Ni1 2.089(5) 11_567 ? C1 C2 1.397(11) . ? C1 C6 1.421(12) . ? C2 C3 1.403(11) . ? C3 C4 1.360(13) . ? C4 C5 1.389(13) . ? C4 C10 1.481(12) . ? C5 O4 1.395(11) . ? C5 C6 1.411(11) . ? C6 C7 1.525(12) . ? C7 N1 1.469(10) . ? N1 C8 1.504(10) . ? C8 C9 1.570(12) . ? C9 O3 1.242(10) . ? C9 O2 1.275(10) . ? O3 Na1 2.677(8) . ? C10 C11 1.334(14) . ? C10 C13 1.525(15) . ? C11 C12 1.432(17) . ? C12 O5 1.189(13) . ? C12 O4 1.383(11) . ? O5 Na1 2.873(10) 10_667 ? O6 Ni1 2.053(5) 11_567 ? Na1 O8A 2.437(16) . ? Na1 O7 2.774(10) . ? Na1 O8 2.86(3) . ? Na1 O5 2.873(10) 10_667 ? Na1 Na1 3.866(9) 2_665 ? Na1 Na1 3.866(9) 3_565 ? O8 O1W 1.41(4) . ? O8 O1W 1.41(4) 2_665 ? O8 O1W 1.41(4) 3_565 ? O8 Na1 2.86(3) 2_665 ? O8 Na1 2.86(3) 3_565 ? O8A O2W 1.17(4) . ? O8A Na1 2.437(16) 3_565 ? O8A Na1 2.437(16) 2_665 ? O1W O3W 1.30(4) . ? O1W O1W 1.33(8) 2_665 ? O1W O1W 1.33(8) 3_565 ? O2W O8A 1.17(4) 13_567 ? O3W O1W 1.30(4) 2_665 ? O3W O1W 1.30(4) 3_565 ? O3W O4W 1.38(8) . ? 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 O6 Ni1 O6 82.2(2) . 12_657 ? O6 Ni1 N1 173.0(2) . . ? O6 Ni1 N1 97.6(2) 12_657 . ? O6 Ni1 O2 100.5(2) . . ? O6 Ni1 O2 174.8(2) 12_657 . ? N1 Ni1 O2 80.2(2) . . ? O6 Ni1 O1 97.42(19) . 12_657 ? O6 Ni1 O1 82.00(19) 12_657 12_657 ? N1 Ni1 O1 89.5(2) . 12_657 ? O2 Ni1 O1 93.2(2) . 12_657 ? O6 Ni1 O1 81.70(18) . . ? O6 Ni1 O1 89.83(19) 12_657 . ? N1 Ni1 O1 91.3(2) . . ? O2 Ni1 O1 95.0(2) . . ? O1 Ni1 O1 171.82(19) 12_657 . ? O6 Ni2 O6 180.000(1) 3_675 12_657 ? O6 Ni2 O6 99.70(16) 3_675 . ? O6 Ni2 O6 80.30(16) 12_657 . ? O6 Ni2 O6 99.70(16) 3_675 2_765 ? O6 Ni2 O6 80.30(16) 12_657 2_765 ? O6 Ni2 O6 99.70(16) . 2_765 ? O6 Ni2 O6 80.30(16) 3_675 10_777 ? O6 Ni2 O6 99.70(16) 12_657 10_777 ? O6 Ni2 O6 180.000(1) . 10_777 ? O6 Ni2 O6 80.30(16) 2_765 10_777 ? O6 Ni2 O6 80.30(16) 3_675 11_567 ? O6 Ni2 O6 99.70(16) 12_657 11_567 ? O6 Ni2 O6 80.30(16) . 11_567 ? O6 Ni2 O6 180.0(2) 2_765 11_567 ? O6 Ni2 O6 99.70(16) 10_777 11_567 ? C1 O1 Ni1 129.6(5) . 11_567 ? C1 O1 Ni1 113.3(5) . . ? Ni1 O1 Ni1 95.61(17) 11_567 . ? O1 C1 C2 124.1(8) . . ? O1 C1 C6 117.8(7) . . ? C2 C1 C6 118.1(7) . . ? C1 C2 C3 120.7(9) . . ? C4 C3 C2 122.0(9) . . ? C3 C4 C5 117.8(8) . . ? C3 C4 C10 126.5(10) . . ? C5 C4 C10 115.6(10) . . ? C4 C5 O4 122.7(8) . . ? C4 C5 C6 122.5(10) . . ? O4 C5 C6 114.8(9) . . ? C5 C6 C1 118.6(9) . . ? C5 C6 C7 122.6(9) . . ? C1 C6 C7 118.8(7) . . ? N1 C7 C6 111.2(7) . . ? C7 N1 C8 112.2(7) . . ? C7 N1 Ni1 111.4(5) . . ? C8 N1 Ni1 104.4(4) . . ? N1 C8 C9 108.7(7) . . ? O3 C9 O2 127.2(9) . . ? O3 C9 C8 115.9(9) . . ? O2 C9 C8 116.7(7) . . ? C9 O2 Ni1 112.9(5) . . ? C9 O3 Na1 142.2(7) . . ? C11 C10 C4 121.0(10) . . ? C11 C10 C13 120.7(10) . . ? C4 C10 C13 118.3(11) . . ? C10 C11 C12 121.9(10) . . ? O5 C12 O4 114.5(12) . . ? O5 C12 C11 127.5(11) . . ? O4 C12 C11 117.9(11) . . ? C12 O4 C5 120.8(9) . . ? C12 O5 Na1 112.2(7) . 10_667 ? Ni1 O6 Ni1 100.17(19) . 11_567 ? Ni1 O6 Ni2 99.13(19) . . ? Ni1 O6 Ni2 98.17(18) 11_567 . ? O8A Na1 O3 144.9(6) . . ? O8A Na1 O7 86.3(3) . . ? O3 Na1 O7 110.2(2) . . ? O8A Na1 O8 62.4(11) . . ? O3 Na1 O8 90.7(7) . . ? O7 Na1 O8 76.2(2) . . ? O8A Na1 O5 93.5(8) . 10_667 ? O3 Na1 O5 118.9(3) . 10_667 ? O7 Na1 O5 81.6(3) . 10_667 ? O8 Na1 O5 147.9(6) . 10_667 ? O8A Na1 Na1 37.5(5) . 2_665 ? O3 Na1 Na1 107.7(2) . 2_665 ? O7 Na1 Na1 110.6(2) . 2_665 ? O8 Na1 Na1 47.5(5) . 2_665 ? O5 Na1 Na1 123.99(19) 10_667 2_665 ? O8A Na1 Na1 37.5(5) . 3_565 ? O3 Na1 Na1 134.88(18) . 3_565 ? O7 Na1 Na1 51.8(2) . 3_565 ? O8 Na1 Na1 47.5(5) . 3_565 ? O5 Na1 Na1 100.4(2) 10_667 3_565 ? Na1 Na1 Na1 60.000(1) 2_665 3_565 ? O1W O8 O1W 56(4) . 2_665 ? O1W O8 O1W 56(4) . 3_565 ? O1W O8 O1W 56(4) 2_665 3_565 ? O1W O8 Na1 96(2) . 2_665 ? O1W O8 Na1 142(3) 2_665 2_665 ? O1W O8 Na1 133(3) 3_565 2_665 ? O1W O8 Na1 133(3) . 3_565 ? O1W O8 Na1 96(2) 2_665 3_565 ? O1W O8 Na1 142(3) 3_565 3_565 ? Na1 O8 Na1 85.0(10) 2_665 3_565 ? O1W O8 Na1 142(3) . . ? O1W O8 Na1 133(3) 2_665 . ? O1W O8 Na1 95.9(19) 3_565 . ? Na1 O8 Na1 85.0(10) 2_665 . ? Na1 O8 Na1 85.0(10) 3_565 . ? O2W O8A Na1 113.7(8) . 3_565 ? O2W O8A Na1 113.7(8) . 2_665 ? Na1 O8A Na1 104.9(9) 3_565 2_665 ? O2W O8A Na1 113.7(8) . . ? Na1 O8A Na1 104.9(9) 3_565 . ? Na1 O8A Na1 104.9(9) 2_665 . ? O3W O1W O1W 59.1(17) . 2_665 ? O3W O1W O1W 59.1(18) . 3_565 ? O1W O1W O1W 60.00(6) 2_665 3_565 ? O3W O1W O8 111(4) . . ? O1W O1W O8 61.8(18) 2_665 . ? O1W O1W O8 61.8(18) 3_565 . ? O8A O2W O8A 180.00(3) . 13_567 ? O1W O3W O1W 62(4) 2_665 . ? O1W O3W O1W 62(4) 2_665 3_565 ? O1W O3W O1W 62(4) . 3_565 ? O1W O3W O4W 144(2) 2_665 . ? O1W O3W O4W 144(2) . . ? O1W O3W O4W 144(2) 3_565 . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 25.48 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.908 _refine_diff_density_min -0.588 _refine_diff_density_rms 0.115 #===#END data_compound_7 _database_code_depnum_ccdc_archive 'CCDC 768061' #data_8307jj _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C67.20 H108.20 K2 N4 Ni4 O42' _chemical_formula_weight 1957.22 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' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/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 22.5549(16) _cell_length_b 12.9601(9) _cell_length_c 15.0085(10) _cell_angle_alpha 90.00 _cell_angle_beta 105.823(2) _cell_angle_gamma 90.00 _cell_volume 4221.0(5) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 6147 _cell_measurement_theta_min 2.45 _cell_measurement_theta_max 26.03 _exptl_crystal_description Rod _exptl_crystal_colour green _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 #_exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.540 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2051 _exptl_absorpt_coefficient_mu 1.074 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6733 _exptl_absorpt_correction_T_max 0.9002 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2005)' _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 29384 _diffrn_reflns_av_R_equivalents 0.0444 _diffrn_reflns_av_sigmaI/netI 0.0524 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 27.49 _reflns_number_total 9687 _reflns_number_gt 7895 _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. There are 12 restraints in the model. This is due to the usage of DFIX option to keep the H atoms in the water molecules within the calculated values. ; _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^)+(0.0621P)^2^+2.6723P] 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 9687 _refine_ls_number_parameters 614 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0613 _refine_ls_R_factor_gt 0.0487 _refine_ls_wR_factor_ref 0.1273 _refine_ls_wR_factor_gt 0.1208 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _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 0.247999(15) 0.13031(3) 0.29165(2) 0.02122(10) Uani 1 1 d . . . Ni2 Ni 0.246823(16) -0.01294(3) 0.45230(2) 0.02175(10) Uani 1 1 d . . . K1 K 0.31492(4) 0.04005(6) 0.09168(5) 0.0467(2) Uani 1 1 d . . . O1 O 0.18563(9) 0.07251(15) 0.35618(12) 0.0259(4) Uani 1 1 d . . . O2 O 0.23787(9) 0.27577(15) 0.33888(12) 0.0281(4) Uani 1 1 d . . . O3 O 0.19430(12) 0.42821(16) 0.29540(14) 0.0416(6) Uani 1 1 d . . . O4 O 0.01289(9) 0.24993(17) 0.17494(13) 0.0315(5) Uani 1 1 d . . . O5 O -0.06747(11) 0.3250(2) 0.08266(15) 0.0514(7) Uani 1 1 d . . . O6 O 0.30820(8) 0.07333(14) 0.40647(12) 0.0245(4) Uani 1 1 d . . . O7 O 0.26153(9) 0.08411(14) 0.56603(13) 0.0270(4) Uani 1 1 d . . . O8 O 0.31984(11) 0.10576(17) 0.71117(15) 0.0417(6) Uani 1 1 d . . . O9 O 0.48872(9) -0.03122(15) 0.62764(13) 0.0290(4) Uani 1 1 d . . . O10 O 0.57078(10) -0.09181(19) 0.72828(16) 0.0426(6) Uani 1 1 d . . . O11 O 0.25037(10) -0.01108(15) 0.22916(13) 0.0285(4) Uani 1 1 d . . . O12 O 0.24199(10) -0.11668(15) 0.34413(13) 0.0297(4) Uani 1 1 d . . . O13 O 0.18452(10) -0.10005(17) 0.49662(14) 0.0325(5) Uani 1 1 d D . . H132 H 0.1508(11) -0.117(3) 0.458(2) 0.039 Uiso 1 1 d D . . H131 H 0.1764(16) -0.088(3) 0.5475(16) 0.039 Uiso 1 1 d D . . N1 N 0.17783(10) 0.18124(17) 0.17949(15) 0.0233(5) Uani 1 1 d . . . H1N H 0.1871(14) 0.165(2) 0.128(2) 0.028 Uiso 1 1 d . . . N2 N 0.31668(10) -0.09416(18) 0.54293(15) 0.0233(5) Uani 1 1 d . . . H2N H 0.3071(14) -0.158(3) 0.540(2) 0.028 Uiso 1 1 d . . . C1 C 0.13492(12) 0.1254(2) 0.35243(18) 0.0231(5) Uani 1 1 d . . . C2 C 0.11608(13) 0.1489(2) 0.43227(18) 0.0279(6) Uani 1 1 d . . . H2 H 0.1383 0.1224 0.4900 0.033 Uiso 1 1 calc R . . C3 C 0.06544(14) 0.2105(2) 0.42628(19) 0.0301(6) Uani 1 1 d . . . H3 H 0.0543 0.2271 0.4805 0.036 Uiso 1 1 calc R . . C4 C 0.03005(13) 0.2492(2) 0.34093(19) 0.0270(6) Uani 1 1 d . . . C5 C 0.04761(12) 0.2196(2) 0.26247(18) 0.0247(6) Uani 1 1 d . . . C6 C 0.09890(12) 0.1600(2) 0.26495(17) 0.0236(5) Uani 1 1 d . . . C7 C 0.11873(13) 0.1308(2) 0.18013(17) 0.0259(6) Uani 1 1 d . . . H7A H 0.1235 0.0557 0.1785 0.031 Uiso 1 1 calc R . . H7B H 0.0867 0.1512 0.1245 0.031 Uiso 1 1 calc R . . C8 C 0.17500(13) 0.2949(2) 0.18367(18) 0.0257(6) Uani 1 1 d . . . H8A H 0.1318 0.3169 0.1634 0.031 Uiso 1 1 calc R . . H8B H 0.1964 0.3245 0.1409 0.031 Uiso 1 1 calc R . . C9 C 0.20398(13) 0.3358(2) 0.28011(18) 0.0271(6) Uani 1 1 d . . . C10 C -0.03949(14) 0.3076(3) 0.1626(2) 0.0380(7) Uani 1 1 d . . . C11 C -0.05556(15) 0.3423(3) 0.2425(2) 0.0408(8) Uani 1 1 d . . . H11 H -0.0900 0.3857 0.2351 0.049 Uiso 1 1 calc R . . C12 C -0.02284(15) 0.3151(2) 0.3293(2) 0.0346(7) Uani 1 1 d . . . C13 C -0.04060(18) 0.3533(3) 0.4129(2) 0.0484(9) Uani 1 1 d . . . H13A H -0.0069 0.3930 0.4518 0.073 Uiso 1 1 calc R . . H13B H -0.0495 0.2949 0.4477 0.073 Uiso 1 1 calc R . . H13C H -0.0769 0.3966 0.3933 0.073 Uiso 1 1 calc R . . C14 C 0.36234(12) 0.0978(2) 0.46191(17) 0.0233(5) Uani 1 1 d . . . C15 C 0.38532(14) 0.1992(2) 0.46752(19) 0.0294(6) Uani 1 1 d . . . H15 H 0.3613 0.2515 0.4317 0.035 Uiso 1 1 calc R . . C16 C 0.44230(14) 0.2226(2) 0.5246(2) 0.0319(6) Uani 1 1 d . . . H16 H 0.4566 0.2909 0.5271 0.038 Uiso 1 1 calc R . . C17 C 0.47996(13) 0.1471(2) 0.57958(19) 0.0273(6) Uani 1 1 d . . . C18 C 0.45517(13) 0.0471(2) 0.57403(18) 0.0246(6) Uani 1 1 d . . . C19 C 0.39801(12) 0.0202(2) 0.51792(18) 0.0224(5) Uani 1 1 d . . . C20 C 0.37396(13) -0.0883(2) 0.51305(19) 0.0254(6) Uani 1 1 d . . . H20A H 0.3658 -0.1136 0.4493 0.030 Uiso 1 1 calc R . . H20B H 0.4054 -0.1328 0.5528 0.030 Uiso 1 1 calc R . . C21 C 0.32393(14) -0.0567(2) 0.63841(18) 0.0284(6) Uani 1 1 d . . . H21A H 0.3675 -0.0600 0.6732 0.034 Uiso 1 1 calc R . . H21B H 0.3008 -0.1017 0.6694 0.034 Uiso 1 1 calc R . . C22 C 0.30093(13) 0.0539(2) 0.63883(19) 0.0261(6) Uani 1 1 d . . . C23 C 0.54681(14) -0.0155(3) 0.6844(2) 0.0334(7) Uani 1 1 d . . . C24 C 0.57267(14) 0.0847(3) 0.6879(2) 0.0369(7) Uani 1 1 d . . . H24 H 0.6130 0.0961 0.7250 0.044 Uiso 1 1 calc R . . C25 C 0.54074(14) 0.1644(3) 0.6390(2) 0.0342(7) Uani 1 1 d . . . C26 C 0.56822(17) 0.2704(3) 0.6471(3) 0.0503(9) Uani 1 1 d . . . H26A H 0.6101 0.2681 0.6868 0.075 Uiso 1 1 calc R . . H26B H 0.5438 0.3168 0.6736 0.075 Uiso 1 1 calc R . . H26C H 0.5685 0.2950 0.5862 0.075 Uiso 1 1 calc R . . C27 C 0.24394(13) -0.0982(2) 0.26202(19) 0.0282(6) Uani 1 1 d . . . C28 C 0.23800(19) -0.1901(3) 0.1979(2) 0.0459(9) Uani 1 1 d . . . H28A H 0.2103 -0.1731 0.1380 0.069 Uiso 1 1 calc R . . H28B H 0.2217 -0.2485 0.2240 0.069 Uiso 1 1 calc R . . H28C H 0.2782 -0.2076 0.1905 0.069 Uiso 1 1 calc R . . O1W O 0.31541(9) 0.18566(15) 0.23294(13) 0.0266(4) Uani 1 1 d D . . H1WB H 0.3181(15) 0.2495(15) 0.224(2) 0.032 Uiso 1 1 d D . . H1WA H 0.3506(9) 0.168(3) 0.257(2) 0.032 Uiso 1 1 d D . . O2W O 0.24402(11) 0.20314(17) 0.02593(14) 0.0351(5) Uani 1 1 d D . . H2WB H 0.2403(16) 0.207(3) -0.0323(13) 0.042 Uiso 1 1 d D . . H2WA H 0.2590(16) 0.2629(17) 0.038(2) 0.042 Uiso 1 1 d D . . O3W O 0.34002(18) 0.0146(3) -0.0884(2) 0.0796(10) Uani 1 1 d D . . H3WA H 0.322(2) -0.044(2) -0.103(4) 0.095 Uiso 1 1 d D . . H3WB H 0.328(3) 0.044(4) -0.142(2) 0.095 Uiso 1 1 d D . . O4W O 0.36232(14) -0.1585(2) 0.0988(2) 0.0592(7) Uani 1 1 d D . . H4WA H 0.349(2) -0.178(4) 0.0426(16) 0.071 Uiso 1 1 d D . . H4WB H 0.3985(12) -0.188(3) 0.116(3) 0.071 Uiso 1 1 d D . . O5W O 0.28562(15) 0.6947(2) 0.4228(2) 0.0626(8) Uani 1 1 d D . . H5WA H 0.2559(16) 0.657(3) 0.428(3) 0.075 Uiso 1 1 d D . . H5WB H 0.2649(19) 0.744(3) 0.389(3) 0.075 Uiso 1 1 d D . . O1S O 0.21092(14) -0.0376(2) -0.04696(18) 0.0546(7) Uani 1 1 d . . . H1S H 0.211(2) 0.008(3) -0.085(3) 0.066 Uiso 1 1 d . . . C1S C 0.1509(5) -0.0887(8) -0.0667(6) 0.066(3) Uani 0.568(16) 1 d P A 1 H1S1 H 0.1506 -0.1412 -0.0198 0.079 Uiso 0.568(16) 1 calc PR A 1 H1S2 H 0.1406 -0.1215 -0.1278 0.079 Uiso 0.568(16) 1 calc PR A 1 C2S C 0.1063(7) -0.0036(12) -0.0640(11) 0.090(5) Uani 0.568(16) 1 d P A 1 H2S1 H 0.0651 -0.0319 -0.0760 0.135 Uiso 0.568(16) 1 calc PR A 1 H2S2 H 0.1073 0.0475 -0.1108 0.135 Uiso 0.568(16) 1 calc PR A 1 H2S3 H 0.1177 0.0286 -0.0033 0.135 Uiso 0.568(16) 1 calc PR A 1 C1SA C 0.1532(6) -0.0147(11) -0.0247(7) 0.059(4) Uani 0.432(16) 1 d P A 2 H1S3 H 0.1546 -0.0438 0.0362 0.071 Uiso 0.432(16) 1 calc PR A 2 H1S4 H 0.1485 0.0602 -0.0212 0.071 Uiso 0.432(16) 1 calc PR A 2 C2SA C 0.1000(10) -0.0567(18) -0.0935(12) 0.091(8) Uani 0.432(16) 1 d P A 2 H2S4 H 0.0628 -0.0410 -0.0758 0.137 Uiso 0.432(16) 1 calc PR A 2 H2S5 H 0.1044 -0.1310 -0.0971 0.137 Uiso 0.432(16) 1 calc PR A 2 H2S6 H 0.0975 -0.0263 -0.1535 0.137 Uiso 0.432(16) 1 calc PR A 2 O3S O 0.48573(13) 0.7249(2) 0.6499(2) 0.0463(7) Uani 0.80 1 d P B 1 H3S H 0.4995 0.7824 0.6696 0.069 Uiso 0.80 1 calc PR B 1 C5S C 0.5339(3) 0.6497(5) 0.6755(4) 0.0735(17) Uani 0.80 1 d P B 1 H5S1 H 0.5447 0.6380 0.7425 0.088 Uiso 0.80 1 calc PR B 1 H5S2 H 0.5707 0.6750 0.6596 0.088 Uiso 0.80 1 calc PR B 1 C6S C 0.5132(5) 0.5516(5) 0.6259(7) 0.129(4) Uani 0.80 1 d P B 1 H6S1 H 0.5459 0.5009 0.6432 0.194 Uiso 0.80 1 calc PR B 1 H6S2 H 0.5029 0.5634 0.5596 0.194 Uiso 0.80 1 calc PR B 1 H6S3 H 0.4771 0.5263 0.6424 0.194 Uiso 0.80 1 calc PR B 1 O6W O 0.5685(6) 0.5596(9) 0.6656(8) 0.038(3) Uiso 0.20 1 d P C 2 O2S O 0.15356(15) 0.5556(2) 0.15083(19) 0.0657(9) Uani 1 1 d . D 2 H2S H 0.1653 0.5121 0.1925 0.099 Uiso 1 1 calc R D 2 C3S C 0.0939(3) 0.5855(5) 0.1461(4) 0.093(2) Uani 1 1 d . D 2 H3SA H 0.0786 0.6273 0.0902 0.111 Uiso 1 1 calc R D 2 H3SB H 0.0953 0.6301 0.1993 0.111 Uiso 1 1 calc R D 2 C4S C 0.0509(3) 0.5064(4) 0.1449(6) 0.114(3) Uani 1 1 d . D 2 H4SA H 0.0111 0.5365 0.1417 0.172 Uiso 1 1 calc R D 2 H4SB H 0.0646 0.4653 0.2008 0.172 Uiso 1 1 calc R D 2 H4SC H 0.0476 0.4628 0.0912 0.172 Uiso 1 1 calc R D 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.02177(18) 0.02068(18) 0.01873(17) 0.00183(13) 0.00129(13) 0.00333(13) Ni2 0.02080(18) 0.02012(18) 0.02123(17) 0.00211(13) 0.00044(13) 0.00022(13) K1 0.0578(5) 0.0378(4) 0.0430(4) -0.0025(3) 0.0113(4) 0.0139(3) O1 0.0223(10) 0.0319(11) 0.0213(9) 0.0039(8) 0.0023(7) 0.0047(8) O2 0.0369(11) 0.0253(10) 0.0187(9) 0.0003(8) 0.0017(8) 0.0059(8) O3 0.0647(16) 0.0286(11) 0.0269(10) -0.0015(9) 0.0045(10) 0.0170(11) O4 0.0257(10) 0.0433(12) 0.0231(9) 0.0051(9) 0.0023(8) 0.0124(9) O5 0.0366(13) 0.0795(19) 0.0336(12) 0.0127(12) 0.0017(10) 0.0288(13) O6 0.0232(10) 0.0213(9) 0.0248(9) 0.0058(7) -0.0006(7) 0.0002(7) O7 0.0270(10) 0.0229(10) 0.0284(10) 0.0012(8) 0.0029(8) 0.0019(8) O8 0.0485(14) 0.0294(11) 0.0348(12) -0.0090(9) -0.0095(10) 0.0030(10) O9 0.0242(10) 0.0283(10) 0.0298(10) 0.0043(8) -0.0006(8) 0.0045(8) O10 0.0303(12) 0.0484(14) 0.0431(13) 0.0118(11) -0.0003(10) 0.0144(10) O11 0.0343(11) 0.0236(10) 0.0266(10) 0.0001(8) 0.0068(8) 0.0028(8) O12 0.0359(11) 0.0233(10) 0.0278(10) -0.0011(8) 0.0051(9) -0.0007(8) O13 0.0283(11) 0.0411(12) 0.0261(10) -0.0003(9) 0.0038(9) -0.0107(9) N1 0.0247(12) 0.0246(12) 0.0199(11) 0.0005(9) 0.0049(9) 0.0039(9) N2 0.0242(12) 0.0175(11) 0.0256(11) 0.0010(9) 0.0025(9) -0.0014(9) C1 0.0200(13) 0.0231(13) 0.0235(12) 0.0016(10) 0.0014(10) -0.0012(10) C2 0.0259(14) 0.0342(16) 0.0201(13) 0.0015(11) 0.0004(11) -0.0013(12) C3 0.0353(16) 0.0335(16) 0.0210(13) -0.0019(11) 0.0069(11) 0.0033(12) C4 0.0242(14) 0.0288(15) 0.0268(13) 0.0020(11) 0.0050(11) 0.0056(11) C5 0.0223(13) 0.0280(14) 0.0210(12) 0.0038(11) 0.0011(10) 0.0026(11) C6 0.0218(13) 0.0285(14) 0.0184(12) 0.0014(10) 0.0018(10) 0.0015(11) C7 0.0248(14) 0.0309(15) 0.0188(12) -0.0009(11) 0.0002(10) 0.0038(11) C8 0.0279(14) 0.0260(14) 0.0210(13) 0.0047(10) 0.0033(11) 0.0069(11) C9 0.0324(15) 0.0259(14) 0.0217(13) 0.0020(11) 0.0049(11) 0.0065(12) C10 0.0275(16) 0.0472(19) 0.0375(17) 0.0079(14) 0.0056(13) 0.0136(14) C11 0.0355(18) 0.0478(19) 0.0408(17) 0.0103(15) 0.0136(14) 0.0197(15) C12 0.0344(17) 0.0348(17) 0.0381(16) 0.0040(13) 0.0159(13) 0.0076(13) C13 0.057(2) 0.052(2) 0.0423(19) 0.0049(16) 0.0228(17) 0.0234(18) C14 0.0254(14) 0.0250(13) 0.0186(12) 0.0012(10) 0.0042(10) 0.0016(11) C15 0.0310(15) 0.0247(14) 0.0283(14) 0.0063(11) 0.0007(12) 0.0003(11) C16 0.0337(16) 0.0266(15) 0.0321(15) 0.0020(12) 0.0034(12) -0.0056(12) C17 0.0250(14) 0.0285(14) 0.0259(13) -0.0022(11) 0.0028(11) -0.0005(11) C18 0.0245(14) 0.0267(14) 0.0212(12) 0.0045(11) 0.0037(10) 0.0066(11) C19 0.0203(13) 0.0225(13) 0.0231(13) -0.0001(10) 0.0037(10) 0.0020(10) C20 0.0235(14) 0.0216(13) 0.0288(14) 0.0011(11) 0.0034(11) 0.0037(11) C21 0.0344(16) 0.0242(14) 0.0230(13) 0.0039(11) 0.0017(11) 0.0011(12) C22 0.0244(14) 0.0238(14) 0.0273(14) 0.0016(11) 0.0024(11) -0.0017(11) C23 0.0250(15) 0.0452(18) 0.0276(14) 0.0001(13) 0.0030(12) 0.0075(13) C24 0.0230(15) 0.0483(19) 0.0333(16) -0.0017(14) -0.0029(12) -0.0023(13) C25 0.0293(16) 0.0408(17) 0.0297(15) -0.0051(13) 0.0034(12) -0.0053(13) C26 0.040(2) 0.045(2) 0.057(2) -0.0026(17) -0.0024(16) -0.0161(16) C27 0.0247(14) 0.0284(15) 0.0286(14) -0.0030(12) 0.0024(11) 0.0013(11) C28 0.071(3) 0.0273(16) 0.0380(17) -0.0081(14) 0.0127(17) -0.0018(16) O1W 0.0236(10) 0.0251(10) 0.0290(10) 0.0058(8) 0.0038(8) 0.0025(8) O2W 0.0547(14) 0.0268(11) 0.0220(10) -0.0004(9) 0.0075(10) 0.0009(10) O3W 0.071(2) 0.095(3) 0.065(2) 0.0253(19) 0.0054(18) -0.0084(19) O4W 0.0575(18) 0.0551(17) 0.0563(16) -0.0129(14) 0.0005(14) 0.0174(14) O5W 0.068(2) 0.0370(15) 0.0669(18) 0.0155(13) -0.0077(15) -0.0023(13) O1S 0.0608(18) 0.0562(17) 0.0438(15) 0.0188(12) 0.0091(13) 0.0021(14) C1S 0.069(7) 0.068(6) 0.057(5) 0.017(5) 0.010(4) -0.009(4) C2S 0.083(13) 0.110(11) 0.094(11) 0.037(8) 0.055(10) 0.024(9) C1SA 0.049(7) 0.093(9) 0.038(5) -0.009(5) 0.017(5) -0.001(6) C2SA 0.074(13) 0.14(2) 0.055(8) -0.013(9) 0.015(7) -0.046(14) O3S 0.0312(15) 0.0302(15) 0.074(2) 0.0081(15) 0.0091(14) -0.0014(12) C5S 0.059(4) 0.090(5) 0.076(4) 0.018(3) 0.026(3) -0.003(3) C6S 0.227(12) 0.043(4) 0.166(8) 0.014(5) 0.136(9) 0.021(5) O2S 0.089(2) 0.0648(19) 0.0526(16) 0.0316(14) 0.0355(16) 0.0342(17) C3S 0.109(4) 0.110(5) 0.076(3) 0.054(3) 0.054(3) 0.067(4) C4S 0.070(4) 0.059(3) 0.182(7) 0.006(4) -0.020(4) 0.020(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 O6 2.0205(17) . ? Ni1 O2 2.0486(19) . ? Ni1 O1 2.0544(19) . ? Ni1 O11 2.0658(19) . ? Ni1 N1 2.079(2) . ? Ni1 O1W 2.082(2) . ? Ni1 K1 3.8890(9) . ? Ni2 O1 2.0314(18) . ? Ni2 O6 2.0394(19) . ? Ni2 O13 2.050(2) . ? Ni2 N2 2.067(2) . ? Ni2 O7 2.0729(19) . ? Ni2 O12 2.0877(19) . ? K1 O2W 2.672(2) . ? K1 O4W 2.777(3) . ? K1 O1W 2.836(2) . ? K1 O1S 2.861(3) . ? K1 O11 2.908(2) . ? K1 O3W 2.928(4) . ? K1 O10 3.256(2) 3_656 ? O1 C1 1.322(3) . ? O2 C9 1.265(3) . ? O3 C9 1.250(3) . ? O4 C10 1.367(3) . ? O4 C5 1.390(3) . ? O5 C10 1.215(4) . ? O6 C14 1.315(3) . ? O7 C22 1.268(3) . ? O8 C22 1.249(3) . ? O9 C23 1.369(4) . ? O9 C18 1.385(3) . ? O10 C23 1.229(4) . ? O10 K1 3.256(2) 3_656 ? O11 C27 1.256(4) . ? O12 C27 1.268(3) . ? N1 C8 1.476(3) . ? N1 C7 1.487(4) . ? N2 C21 1.479(3) . ? N2 C20 1.481(4) . ? C1 C2 1.410(4) . ? C1 C6 1.415(3) . ? C2 C3 1.376(4) . ? C3 C4 1.404(4) . ? C4 C5 1.395(4) . ? C4 C12 1.439(4) . ? C5 C6 1.383(4) . ? C6 C7 1.508(4) . ? C8 C9 1.512(4) . ? C10 C11 1.417(4) . ? C11 C12 1.358(4) . ? C12 C13 1.501(4) . ? C14 C15 1.407(4) . ? C14 C19 1.413(4) . ? C15 C16 1.370(4) . ? C16 C17 1.406(4) . ? C17 C18 1.404(4) . ? C17 C25 1.435(4) . ? C18 C19 1.379(4) . ? C19 C20 1.501(4) . ? C21 C22 1.525(4) . ? C23 C24 1.419(5) . ? C24 C25 1.354(5) . ? C25 C26 1.499(5) . ? C27 C28 1.514(4) . ? O1S C1SA 1.461(12) . ? O1S C1S 1.462(10) . ? C1S C2S 1.500(19) . ? C1SA C2SA 1.46(2) . ? O3S C5S 1.433(7) . ? C5S C6S 1.483(10) . ? O2S C3S 1.383(6) . ? C3S C4S 1.407(8) . ? 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 O6 Ni1 O2 98.84(7) . . ? O6 Ni1 O1 81.49(7) . . ? O2 Ni1 O1 90.98(8) . . ? O6 Ni1 O11 88.20(8) . . ? O2 Ni1 O11 172.96(8) . . ? O1 Ni1 O11 89.80(8) . . ? O6 Ni1 N1 173.17(9) . . ? O2 Ni1 N1 81.71(8) . . ? O1 Ni1 N1 91.69(8) . . ? O11 Ni1 N1 91.27(8) . . ? O6 Ni1 O1W 95.07(8) . . ? O2 Ni1 O1W 89.57(8) . . ? O1 Ni1 O1W 176.56(7) . . ? O11 Ni1 O1W 90.07(8) . . ? N1 Ni1 O1W 91.74(8) . . ? O6 Ni1 K1 103.67(6) . . ? O2 Ni1 K1 130.33(6) . . ? O1 Ni1 K1 135.55(6) . . ? O11 Ni1 K1 47.10(6) . . ? N1 Ni1 K1 80.83(7) . . ? O1W Ni1 K1 45.17(6) . . ? O1 Ni2 O6 81.60(7) . . ? O1 Ni2 O13 97.91(8) . . ? O6 Ni2 O13 179.26(8) . . ? O1 Ni2 N2 173.41(9) . . ? O6 Ni2 N2 92.03(8) . . ? O13 Ni2 N2 88.45(9) . . ? O1 Ni2 O7 100.32(8) . . ? O6 Ni2 O7 88.52(8) . . ? O13 Ni2 O7 92.11(8) . . ? N2 Ni2 O7 81.08(8) . . ? O1 Ni2 O12 85.27(8) . . ? O6 Ni2 O12 89.26(8) . . ? O13 Ni2 O12 90.15(8) . . ? N2 Ni2 O12 93.02(8) . . ? O7 Ni2 O12 173.61(8) . . ? O2W K1 O4W 158.84(8) . . ? O2W K1 O1W 68.26(6) . . ? O4W K1 O1W 131.66(8) . . ? O2W K1 O1S 73.76(8) . . ? O4W K1 O1S 86.14(9) . . ? O1W K1 O1S 127.82(8) . . ? O2W K1 O11 94.43(7) . . ? O4W K1 O11 91.35(8) . . ? O1W K1 O11 61.43(6) . . ? O1S K1 O11 88.05(7) . . ? O2W K1 O3W 89.73(9) . . ? O4W K1 O3W 76.21(10) . . ? O1W K1 O3W 143.42(9) . . ? O1S K1 O3W 67.38(9) . . ? O11 K1 O3W 152.85(9) . . ? O2W K1 O10 113.72(7) . 3_656 ? O4W K1 O10 87.11(7) . 3_656 ? O1W K1 O10 53.25(6) . 3_656 ? O1S K1 O10 169.39(7) . 3_656 ? O11 K1 O10 83.94(6) . 3_656 ? O3W K1 O10 118.74(9) . 3_656 ? O2W K1 Ni1 74.21(5) . . ? O4W K1 Ni1 118.38(7) . . ? O1W K1 Ni1 31.37(4) . . ? O1S K1 Ni1 104.68(6) . . ? O11 K1 Ni1 31.36(4) . . ? O3W K1 Ni1 163.73(8) . . ? O10 K1 Ni1 71.56(5) 3_656 . ? C1 O1 Ni2 136.52(17) . . ? C1 O1 Ni1 119.13(16) . . ? Ni2 O1 Ni1 96.52(8) . . ? C9 O2 Ni1 115.32(17) . . ? C10 O4 C5 121.7(2) . . ? C14 O6 Ni1 138.05(17) . . ? C14 O6 Ni2 121.15(16) . . ? Ni1 O6 Ni2 97.34(8) . . ? C22 O7 Ni2 116.05(17) . . ? C23 O9 C18 122.1(2) . . ? C23 O10 K1 114.4(2) . 3_656 ? C27 O11 Ni1 126.79(18) . . ? C27 O11 K1 128.11(18) . . ? Ni1 O11 K1 101.54(8) . . ? C27 O12 Ni2 128.75(18) . . ? C8 N1 C7 112.9(2) . . ? C8 N1 Ni1 108.34(16) . . ? C7 N1 Ni1 109.94(16) . . ? C21 N2 C20 113.7(2) . . ? C21 N2 Ni2 109.49(17) . . ? C20 N2 Ni2 110.24(16) . . ? O1 C1 C2 122.3(2) . . ? O1 C1 C6 118.4(2) . . ? C2 C1 C6 119.4(2) . . ? C3 C2 C1 120.5(3) . . ? C2 C3 C4 121.4(3) . . ? C5 C4 C3 116.8(2) . . ? C5 C4 C12 118.6(2) . . ? C3 C4 C12 124.6(3) . . ? C6 C5 O4 115.8(2) . . ? C6 C5 C4 124.0(2) . . ? O4 C5 C4 120.2(2) . . ? C5 C6 C1 117.8(2) . . ? C5 C6 C7 123.8(2) . . ? C1 C6 C7 118.4(2) . . ? N1 C7 C6 111.6(2) . . ? N1 C8 C9 112.2(2) . . ? O3 C9 O2 124.3(3) . . ? O3 C9 C8 117.4(2) . . ? O2 C9 C8 118.3(2) . . ? O5 C10 O4 115.6(3) . . ? O5 C10 C11 126.4(3) . . ? O4 C10 C11 118.0(3) . . ? C12 C11 C10 122.1(3) . . ? C11 C12 C4 119.1(3) . . ? C11 C12 C13 121.1(3) . . ? C4 C12 C13 119.7(3) . . ? O6 C14 C15 121.7(2) . . ? O6 C14 C19 119.0(2) . . ? C15 C14 C19 119.2(2) . . ? C16 C15 C14 120.8(3) . . ? C15 C16 C17 121.8(3) . . ? C18 C17 C16 116.1(2) . . ? C18 C17 C25 118.6(3) . . ? C16 C17 C25 125.3(3) . . ? C19 C18 O9 116.1(2) . . ? C19 C18 C17 124.1(2) . . ? O9 C18 C17 119.7(2) . . ? C18 C19 C14 118.0(2) . . ? C18 C19 C20 122.2(2) . . ? C14 C19 C20 119.9(2) . . ? N2 C20 C19 111.5(2) . . ? N2 C21 C22 111.4(2) . . ? O8 C22 O7 125.1(3) . . ? O8 C22 C21 118.3(2) . . ? O7 C22 C21 116.5(2) . . ? O10 C23 O9 114.9(3) . . ? O10 C23 C24 126.9(3) . . ? O9 C23 C24 118.2(3) . . ? C25 C24 C23 121.7(3) . . ? C24 C25 C17 119.6(3) . . ? C24 C25 C26 120.5(3) . . ? C17 C25 C26 119.8(3) . . ? O11 C27 O12 126.1(3) . . ? O11 C27 C28 117.2(3) . . ? O12 C27 C28 116.7(3) . . ? Ni1 O1W K1 103.46(8) . . ? C1SA O1S C1S 45.9(5) . . ? C1SA O1S K1 111.6(5) . . ? C1S O1S K1 146.8(4) . . ? O1S C1S C2S 104.6(10) . . ? C2SA C1SA O1S 112.0(12) . . ? O3S C5S C6S 109.7(6) . . ? O2S C3S C4S 117.0(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 O5W H5WB O12 0.867(19) 1.95(3) 2.776(3) 159(5) 1_565 O5W H5WA O1S 0.846(19) 1.95(3) 2.758(4) 160(5) 4_566 O4W H4WB O3S 0.876(19) 1.95(2) 2.813(4) 167(4) 4_565 O4W H4WA O5W 0.853(19) 1.98(3) 2.775(4) 156(4) 4_565 O3W H3WB O8 0.861(19) 2.31(2) 3.147(4) 164(5) 1_554 O3W H3WA O5W 0.862(19) 2.19(3) 3.000(5) 156(5) 4_565 O2W H2WA O7 0.846(18) 2.02(2) 2.827(3) 159(3) 4_565 O2W H2WB O2 0.856(18) 1.932(19) 2.786(3) 175(4) 4_565 O1W H1WA O10 0.810(18) 1.99(2) 2.755(3) 157(3) 3_656 O1W H1WB O8 0.844(18) 1.887(19) 2.728(3) 175(3) 4_565 N2 H2N O5W 0.86(3) 2.55(3) 3.247(4) 140(3) 1_545 N1 H1N O2W 0.88(3) 2.31(3) 3.082(3) 147(3) . O13 H132 O5 0.849(18) 1.96(2) 2.760(3) 156(3) 2_545 O1S H1S O3 0.82(4) 1.93(5) 2.695(3) 157(4) 4_565 O2S H2S O3 0.83 1.86 2.682(3) 173.1 . O3S H3S O10 0.83 2.29 3.078(4) 158.5 1_565 O3S H3S O9 0.83 2.49 3.181(3) 141.2 1_565 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.772 _refine_diff_density_min -0.415 _refine_diff_density_rms 0.085 #===#END data_compound_8 _database_code_depnum_ccdc_archive 'CCDC 768062' #data_8384 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39 H59 N3 Ni5 O30.50' _chemical_formula_weight 1351.44 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 Orthorhombic _symmetry_space_group_name_H-M C222(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x, y, -z+1/2' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 13.9467(5) _cell_length_b 26.2945(10) _cell_length_c 16.3610(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5999.9(4) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 3671 _cell_measurement_theta_min 2.74 _cell_measurement_theta_max 24.21 _exptl_crystal_description BLOCK _exptl_crystal_colour BLUE-GREEN _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 #_exptl_crystal_density_meas Not _exptl_crystal_density_diffrn 1.496 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2792 _exptl_absorpt_coefficient_mu 1.626 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7585 _exptl_absorpt_correction_T_max 0.8809 _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 21518 _diffrn_reflns_av_R_equivalents 0.0548 _diffrn_reflns_av_sigmaI/netI 0.0653 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 27.49 _reflns_number_total 6891 _reflns_number_gt 6111 _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. In totoal 17 restraints were applied. The hydrogen atoms bonded to O11, O12, O1W and N1 atoms are fixed in the appropriate geometry using the option DFIX. ; _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^)+(0.0666P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.020(17) _refine_ls_number_reflns 6891 _refine_ls_number_parameters 379 _refine_ls_number_restraints 17 _refine_ls_R_factor_all 0.0542 _refine_ls_R_factor_gt 0.0473 _refine_ls_wR_factor_ref 0.1212 _refine_ls_wR_factor_gt 0.1172 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.031 _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 0.90162(3) 0.77672(2) 0.10761(3) 0.01950(13) Uani 1 1 d . . . Ni2 Ni 1.0000 0.73062(3) 0.2500 0.01872(16) Uani 1 2 d S . . Ni3 Ni 1.11150(3) 0.78202(2) 0.06543(3) 0.02134(13) Uani 1 1 d D . . O1 O 1.0005(2) 0.83173(11) 0.08292(18) 0.0237(7) Uani 1 1 d . . . O2 O 0.90329(19) 0.78775(11) 0.23012(16) 0.0226(6) Uani 1 1 d . . . O3 O 0.8088(2) 0.80766(13) 0.33523(18) 0.0282(7) Uani 1 1 d . . . O4 O 0.8008(2) 0.97651(13) 0.1005(2) 0.0338(8) Uani 1 1 d . . . O5 O 0.6999(3) 1.03975(15) 0.1122(3) 0.0545(11) Uani 1 1 d . . . O6 O 0.8123(2) 0.71399(13) 0.13083(18) 0.0286(7) Uani 1 1 d . . . O7 O 0.8938(2) 0.67759(11) 0.23314(18) 0.0287(7) Uani 1 1 d . . . O8 O 0.8894(2) 0.76434(12) -0.01351(17) 0.0278(7) Uani 1 1 d . . . O9 O 1.0460(2) 0.76155(14) -0.04504(19) 0.0326(8) Uani 1 1 d . . . O10 O 1.02154(19) 0.73499(11) 0.12785(18) 0.0207(6) Uani 1 1 d D . . H10 H 1.035(3) 0.7026(9) 0.118(3) 0.031 Uiso 1 1 d D . . O11 O 1.1979(2) 0.82728(14) -0.0046(2) 0.0336(8) Uani 1 1 d D . . H11A H 1.233(3) 0.8388(15) 0.0313(15) 0.050 Uiso 1 1 d D . . H11B H 1.230(3) 0.8044(9) -0.027(2) 0.050 Uiso 1 1 d D . . O12 O 1.2033(2) 0.72257(14) 0.0418(2) 0.0311(7) Uani 1 1 d D . . H12A H 1.186(2) 0.7039(9) 0.078(2) 0.047 Uiso 1 1 d D . . H12B H 1.2531(12) 0.7367(10) 0.055(3) 0.047 Uiso 1 1 d D . . N1 N 0.7919(2) 0.82870(14) 0.1167(2) 0.0222(7) Uani 1 1 d D . . H1N H 0.738(2) 0.8145(17) 0.098(3) 0.027 Uiso 1 1 d D . . C1 C 0.9907(3) 0.88112(17) 0.0940(3) 0.0248(9) Uani 1 1 d . . . C2 C 1.0710(3) 0.91149(19) 0.1105(3) 0.0330(10) Uani 1 1 d . . . H2 H 1.1318 0.8964 0.1156 0.040 Uiso 1 1 calc R . . C3 C 1.0613(4) 0.96304(19) 0.1190(3) 0.0370(12) Uani 1 1 d . . . H3 H 1.1167 0.9828 0.1266 0.044 Uiso 1 1 calc R . . C4 C 0.9716(3) 0.98755(18) 0.1169(3) 0.0313(10) Uani 1 1 d . . . C5 C 0.8933(3) 0.95597(17) 0.1030(3) 0.0273(9) Uani 1 1 d . . . C6 C 0.8980(3) 0.90355(15) 0.0905(3) 0.0238(9) Uani 1 1 d . . . C7 C 0.8116(3) 0.87385(17) 0.0637(3) 0.0238(9) Uani 1 1 d . . . H7A H 0.7555 0.8963 0.0642 0.029 Uiso 1 1 calc R . . H7B H 0.8213 0.8623 0.0073 0.029 Uiso 1 1 calc R . . C8 C 0.7705(3) 0.84203(18) 0.2042(3) 0.0280(10) Uani 1 1 d . . . H8 H 0.7903 0.8778 0.2125 0.034 Uiso 1 1 calc R . . C9 C 0.8314(3) 0.80926(16) 0.2616(3) 0.0221(8) Uani 1 1 d . . . C10 C 0.6630(3) 0.8391(3) 0.2212(4) 0.069(2) Uani 1 1 d . . . H10A H 0.6287 0.8591 0.1807 0.104 Uiso 1 1 calc R . . H10B H 0.6498 0.8525 0.2753 0.104 Uiso 1 1 calc R . . H10C H 0.6421 0.8040 0.2182 0.104 Uiso 1 1 calc R . . C11 C 0.7836(4) 1.02691(19) 0.1117(3) 0.0384(11) Uani 1 1 d . . . C12 C 0.8654(4) 1.05865(19) 0.1222(3) 0.0417(13) Uani 1 1 d . . . H12 H 0.8556 1.0938 0.1278 0.050 Uiso 1 1 calc R . . C13 C 0.9558(4) 1.04110(19) 0.1245(3) 0.0391(12) Uani 1 1 d . . . C14 C 1.0390(4) 1.0765(2) 0.1334(4) 0.0552(16) Uani 1 1 d . . . H14A H 1.0179 1.1112 0.1236 0.083 Uiso 1 1 calc R . . H14B H 1.0883 1.0676 0.0941 0.083 Uiso 1 1 calc R . . H14C H 1.0649 1.0739 0.1883 0.083 Uiso 1 1 calc R . . C15 C 0.8226(3) 0.68070(19) 0.1851(3) 0.0317(10) Uani 1 1 d . . . C16 C 0.7459(4) 0.6407(3) 0.1949(4) 0.071(2) Uani 1 1 d . . . H16A H 0.6876 0.6564 0.2151 0.107 Uiso 1 1 calc R . . H16B H 0.7675 0.6151 0.2335 0.107 Uiso 1 1 calc R . . H16C H 0.7334 0.6248 0.1424 0.107 Uiso 1 1 calc R . . C17 C 0.9590(3) 0.76269(19) -0.0631(3) 0.0309(10) Uani 1 1 d . . . C18 C 0.9327(4) 0.7617(3) -0.1525(3) 0.068(2) Uani 1 1 d . . . H18A H 0.9559 0.7925 -0.1787 0.102 Uiso 1 1 calc R . . H18B H 0.8636 0.7599 -0.1580 0.102 Uiso 1 1 calc R . . H18C H 0.9617 0.7323 -0.1783 0.102 Uiso 1 1 calc R . . C1S C 0.3600(19) 0.9966(10) 0.190(2) 0.150(4) Uiso 0.50 1 d PD A -1 H1SA H 0.3214 1.0258 0.1942 0.180 Uiso 0.50 1 calc PR A -1 C2S C 0.486(2) 1.0493(8) 0.230(2) 0.150(4) Uiso 0.50 1 d PD A -1 H2S1 H 0.5503 1.0432 0.2493 0.225 Uiso 0.50 1 calc PR A -1 H2S2 H 0.4477 1.0643 0.2733 0.225 Uiso 0.50 1 calc PR A -1 H2S3 H 0.4876 1.0725 0.1836 0.225 Uiso 0.50 1 calc PR A -1 C3S C 0.5103(19) 0.9564(9) 0.2020(16) 0.150(4) Uiso 0.50 1 d PD A -1 H3S1 H 0.5735 0.9663 0.2210 0.225 Uiso 0.50 1 calc PR A -1 H3S2 H 0.5146 0.9440 0.1463 0.225 Uiso 0.50 1 calc PR A -1 H3S3 H 0.4853 0.9296 0.2369 0.225 Uiso 0.50 1 calc PR A -1 N1S N 0.4433(15) 1.0022(9) 0.2050(16) 0.150(4) Uiso 0.50 1 d PD A -1 O1S O 0.3185(14) 0.9567(7) 0.1696(12) 0.150(4) Uiso 0.50 1 d PD A -1 O1W O 0.6356(3) 1.13752(14) 0.1140(2) 0.0426(9) Uani 1 1 d D . . H1WA H 0.647(5) 1.1061(9) 0.108(4) 0.064 Uiso 1 1 d D . . H1WB H 0.642(5) 1.152(2) 0.160(2) 0.064 Uiso 1 1 d D . . O2W O 0.5389(7) 0.8551(5) 0.0324(7) 0.140(4) Uani 0.75 1 d P . . O3W O 0.3361(7) 0.8925(4) 0.0489(8) 0.150(5) Uani 0.75 1 d P . . O4W O 0.394(5) 0.934(2) 0.0278(19) 0.36(5) Uani 0.25 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 0.0162(2) 0.0223(3) 0.0200(2) 0.0000(2) -0.00067(19) 0.0004(2) Ni2 0.0169(3) 0.0201(4) 0.0192(3) 0.000 -0.0006(3) 0.000 Ni3 0.0172(2) 0.0259(3) 0.0209(2) -0.0004(2) 0.0029(2) 0.0006(2) O1 0.0196(13) 0.0245(15) 0.0269(17) 0.0011(12) 0.0014(12) -0.0008(12) O2 0.0199(13) 0.0271(15) 0.0208(14) 0.0004(12) -0.0021(12) 0.0044(12) O3 0.0184(15) 0.045(2) 0.0212(15) 0.0021(14) 0.0031(12) 0.0047(13) O4 0.0312(18) 0.0248(17) 0.045(2) -0.0020(15) -0.0049(15) 0.0029(13) O5 0.044(2) 0.033(2) 0.087(3) -0.009(2) -0.002(2) 0.0145(17) O6 0.0246(15) 0.0361(19) 0.0251(15) 0.0006(14) -0.0030(12) -0.0080(14) O7 0.0297(15) 0.0281(15) 0.0282(16) 0.0028(13) -0.0027(15) -0.0081(13) O8 0.0223(14) 0.0384(18) 0.0228(14) -0.0015(13) -0.0029(13) -0.0003(14) O9 0.0240(15) 0.050(2) 0.0236(15) -0.0047(15) 0.0022(13) 0.0003(14) O10 0.0178(13) 0.0213(14) 0.0229(15) -0.0005(12) 0.0003(11) 0.0020(11) O11 0.0324(17) 0.037(2) 0.0314(17) -0.0038(15) 0.0074(14) -0.0036(15) O12 0.0211(14) 0.0318(18) 0.0404(18) -0.0008(16) 0.0088(13) 0.0011(14) N1 0.0160(16) 0.0251(19) 0.0253(18) -0.0002(15) -0.0060(15) -0.0019(14) C1 0.026(2) 0.027(2) 0.022(2) 0.0010(17) 0.0039(17) -0.0021(18) C2 0.025(2) 0.031(3) 0.043(3) -0.004(2) -0.001(2) -0.0011(18) C3 0.035(3) 0.032(3) 0.045(3) 0.000(2) 0.003(2) -0.009(2) C4 0.034(2) 0.027(2) 0.033(3) -0.004(2) 0.002(2) -0.0017(19) C5 0.030(2) 0.027(2) 0.025(2) 0.0018(18) 0.002(2) 0.0058(19) C6 0.026(2) 0.0179(19) 0.028(2) 0.0031(16) 0.0015(18) -0.0040(18) C7 0.023(2) 0.023(2) 0.025(2) 0.0016(18) -0.0031(18) 0.0005(17) C8 0.025(2) 0.029(2) 0.030(2) 0.0011(19) 0.0039(18) 0.0066(19) C9 0.0176(18) 0.024(2) 0.025(2) -0.0018(18) 0.0031(17) -0.0012(15) C10 0.026(3) 0.139(7) 0.043(3) 0.033(4) 0.010(2) 0.039(3) C11 0.052(3) 0.022(2) 0.041(3) -0.003(2) -0.005(3) 0.008(2) C12 0.061(3) 0.019(2) 0.045(3) -0.004(2) 0.005(3) 0.005(2) C13 0.047(3) 0.026(3) 0.044(3) -0.006(2) 0.005(3) -0.004(2) C14 0.062(4) 0.030(3) 0.075(4) -0.013(3) -0.001(3) -0.007(3) C15 0.030(2) 0.040(3) 0.025(2) 0.001(2) -0.0049(19) -0.013(2) C16 0.067(4) 0.096(5) 0.051(4) 0.038(4) -0.032(3) -0.054(4) C17 0.031(2) 0.039(3) 0.023(2) -0.001(2) -0.0011(19) 0.004(2) C18 0.041(3) 0.141(8) 0.023(3) -0.013(3) 0.002(2) 0.005(4) O1W 0.059(2) 0.035(2) 0.0338(19) -0.0025(17) 0.0042(18) 0.0091(18) O2W 0.137(8) 0.152(10) 0.131(9) 0.009(8) 0.006(7) -0.020(7) O3W 0.137(8) 0.170(10) 0.142(9) -0.060(8) 0.047(7) -0.122(8) O4W 0.75(14) 0.26(6) 0.06(2) -0.05(3) 0.20(5) -0.10(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 O8 2.016(3) . ? Ni1 O2 2.025(3) . ? Ni1 O10 2.027(3) . ? Ni1 O1 2.039(3) . ? Ni1 N1 2.057(4) . ? Ni1 O6 2.102(3) . ? Ni2 O10 2.024(3) 3_755 ? Ni2 O10 2.024(3) . ? Ni2 O2 2.045(3) 3_755 ? Ni2 O2 2.045(3) . ? Ni2 O7 2.053(3) . ? Ni2 O7 2.053(3) 3_755 ? Ni2 Ni1 2.9629(6) 3_755 ? Ni3 O10 2.036(3) . ? Ni3 O11 2.045(3) . ? Ni3 O1 2.047(3) . ? Ni3 O12 2.057(3) . ? Ni3 O3 2.081(3) 3_755 ? Ni3 O9 2.096(3) . ? O1 C1 1.318(5) . ? O2 C9 1.261(5) . ? O3 C9 1.246(5) . ? O3 Ni3 2.081(3) 3_755 ? O4 C11 1.359(6) . ? O4 C5 1.400(5) . ? O5 C11 1.215(7) . ? O6 C15 1.255(6) . ? O7 C15 1.270(5) . ? O8 C17 1.266(5) . ? O9 C17 1.248(5) . ? N1 C7 1.496(5) . ? N1 C8 1.504(6) . ? C1 C2 1.402(6) . ? C1 C6 1.422(6) . ? C2 C3 1.369(7) . ? C3 C4 1.408(7) . ? C4 C5 1.390(6) . ? C4 C13 1.430(7) . ? C5 C6 1.395(6) . ? C6 C7 1.501(6) . ? C8 C10 1.527(6) . ? C8 C9 1.531(6) . ? C11 C12 1.424(8) . ? C12 C13 1.343(7) . ? C13 C14 1.495(7) . ? C15 C16 1.509(7) . ? C17 C18 1.507(7) . ? C1S N1S 1.20(3) . ? C1S O1S 1.245(17) . ? C2S N1S 1.431(17) . ? C3S N1S 1.526(17) . ? O3W O4W 1.40(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O8 Ni1 O2 175.67(12) . . ? O8 Ni1 O10 98.21(12) . . ? O2 Ni1 O10 84.63(11) . . ? O8 Ni1 O1 88.67(12) . . ? O2 Ni1 O1 94.97(12) . . ? O10 Ni1 O1 81.87(12) . . ? O8 Ni1 N1 96.65(14) . . ? O2 Ni1 N1 80.89(13) . . ? O10 Ni1 N1 164.02(13) . . ? O1 Ni1 N1 92.63(13) . . ? O8 Ni1 O6 90.05(12) . . ? O2 Ni1 O6 86.58(12) . . ? O10 Ni1 O6 92.00(12) . . ? O1 Ni1 O6 173.49(13) . . ? N1 Ni1 O6 93.86(13) . . ? O10 Ni2 O10 173.48(17) 3_755 . ? O10 Ni2 O2 84.21(11) 3_755 3_755 ? O10 Ni2 O2 90.99(11) . 3_755 ? O10 Ni2 O2 91.00(11) 3_755 . ? O10 Ni2 O2 84.21(11) . . ? O2 Ni2 O2 85.45(16) 3_755 . ? O10 Ni2 O7 93.68(11) 3_755 . ? O10 Ni2 O7 90.75(12) . . ? O2 Ni2 O7 175.03(12) 3_755 . ? O2 Ni2 O7 90.10(12) . . ? O10 Ni2 O7 90.75(12) 3_755 3_755 ? O10 Ni2 O7 93.68(11) . 3_755 ? O2 Ni2 O7 90.10(12) 3_755 3_755 ? O2 Ni2 O7 175.03(13) . 3_755 ? O7 Ni2 O7 94.44(17) . 3_755 ? O10 Ni2 Ni1 43.05(8) 3_755 3_755 ? O10 Ni2 Ni1 133.18(8) . 3_755 ? O2 Ni2 Ni1 43.03(8) 3_755 3_755 ? O2 Ni2 Ni1 97.46(8) . 3_755 ? O7 Ni2 Ni1 135.86(8) . 3_755 ? O7 Ni2 Ni1 80.68(8) 3_755 3_755 ? O10 Ni3 O11 176.00(14) . . ? O10 Ni3 O1 81.46(11) . . ? O11 Ni3 O1 98.77(13) . . ? O10 Ni3 O12 90.94(13) . . ? O11 Ni3 O12 88.29(14) . . ? O1 Ni3 O12 169.26(12) . . ? O10 Ni3 O3 97.71(12) . 3_755 ? O11 Ni3 O3 86.25(13) . 3_755 ? O1 Ni3 O3 95.05(12) . 3_755 ? O12 Ni3 O3 93.47(13) . 3_755 ? O10 Ni3 O9 90.45(13) . . ? O11 Ni3 O9 85.58(14) . . ? O1 Ni3 O9 87.40(12) . . ? O12 Ni3 O9 85.07(13) . . ? O3 Ni3 O9 171.74(12) 3_755 . ? C1 O1 Ni1 127.0(3) . . ? C1 O1 Ni3 136.6(3) . . ? Ni1 O1 Ni3 94.94(12) . . ? C9 O2 Ni1 117.3(3) . . ? C9 O2 Ni2 142.1(3) . . ? Ni1 O2 Ni2 93.42(11) . . ? C9 O3 Ni3 129.1(3) . 3_755 ? C11 O4 C5 122.3(4) . . ? C15 O6 Ni1 127.4(3) . . ? C15 O7 Ni2 127.2(3) . . ? C17 O8 Ni1 124.8(3) . . ? C17 O9 Ni3 128.4(3) . . ? Ni2 O10 Ni1 93.99(11) . . ? Ni2 O10 Ni3 128.40(15) . . ? Ni1 O10 Ni3 95.61(12) . . ? C7 N1 C8 113.8(4) . . ? C7 N1 Ni1 110.4(3) . . ? C8 N1 Ni1 111.8(3) . . ? O1 C1 C2 120.3(4) . . ? O1 C1 C6 119.8(4) . . ? C2 C1 C6 119.9(4) . . ? C3 C2 C1 120.3(4) . . ? C2 C3 C4 122.6(4) . . ? C5 C4 C3 115.4(4) . . ? C5 C4 C13 118.8(4) . . ? C3 C4 C13 125.8(4) . . ? C4 C5 C6 125.3(4) . . ? C4 C5 O4 119.9(4) . . ? C6 C5 O4 114.8(4) . . ? C5 C6 C1 116.5(4) . . ? C5 C6 C7 121.3(4) . . ? C1 C6 C7 121.7(4) . . ? N1 C7 C6 113.0(3) . . ? N1 C8 C10 110.8(4) . . ? N1 C8 C9 110.0(3) . . ? C10 C8 C9 113.9(4) . . ? O3 C9 O2 125.5(4) . . ? O3 C9 C8 118.1(4) . . ? O2 C9 C8 116.3(4) . . ? O5 C11 O4 116.2(5) . . ? O5 C11 C12 127.3(5) . . ? O4 C11 C12 116.5(5) . . ? C13 C12 C11 123.7(5) . . ? C12 C13 C4 118.7(5) . . ? C12 C13 C14 121.1(5) . . ? C4 C13 C14 120.2(5) . . ? O6 C15 O7 124.9(4) . . ? O6 C15 C16 118.8(4) . . ? O7 C15 C16 116.3(4) . . ? O9 C17 O8 126.4(4) . . ? O9 C17 C18 117.8(4) . . ? O8 C17 C18 115.8(4) . . ? N1S C1S O1S 128(3) . . ? C1S N1S C2S 124(3) . . ? C1S N1S C3S 119(2) . . ? C2S N1S C3S 116(2) . . ? 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 H1WB O7 0.85(2) 1.94(3) 2.744(5) 158(6) 7_655 O1W H1WA O5 0.85(2) 1.89(3) 2.723(5) 166(7) . O12 H12B O8 0.815(19) 2.02(2) 2.659(4) 135(4) 8_565 O12 H12A O1W 0.806(18) 1.97(2) 2.700(5) 150(4) 5_545 O11 H11B O6 0.834(19) 2.11(2) 2.826(4) 144(3) 8_565 O11 H11A O3 0.819(19) 2.40(3) 2.821(5) 112.7(18) 3_755 O11 H11A O3W 0.819(19) 2.039(18) 2.724(8) 141(3) 1_655 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.741 _refine_diff_density_min -0.379 _refine_diff_density_rms 0.113 #===#END