#------------------------------------------------------------------------------ #$Date: 2012-02-28 12:14:52 +0000 (Tue, 28 Feb 2012) $ #$Revision: 35911 $ #$URL: svn://www.crystallography.net/cod/cif/1/50/00/1500033.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1500033 loop_ _publ_author_name 'Carmen R. Maldonado' 'Miguel Quir\'os' 'Juan M. Salas' _publ_contact_author_address ; Departamento de Qu\'imica Inorg\'anica Facultad de Ciencias Universidad de Granada 18071 Granada SPAIN ; _publ_contact_author_email mquiros@ugr.es _publ_contact_author_fax 34-58-248526 _publ_contact_author_name 'Miguel Quir\'os' _publ_contact_author_phone 34-58-240441 _journal_name_full Polyhedron _journal_page_first 911 _journal_page_last 916 _journal_volume 28 _journal_year 2009 _chemical_formula_moiety 'C22 H26 N12 Ni O6, 2 (H2 O)' _chemical_formula_sum 'C22 H30 N12 Ni O8' _chemical_formula_weight 649.29 _chemical_name_systematic ; ? ; _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 83.422(1) _cell_angle_beta 69.440(1) _cell_angle_gamma 61.375(1) _cell_formula_units_Z 1 _cell_length_a 8.4471(4) _cell_length_b 8.6061(4) _cell_length_c 11.4137(6) _cell_measurement_reflns_used 6266 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 28.1 _cell_measurement_theta_min 2.7 _cell_volume 680.47(6) _computing_cell_refinement 'Bruker SMART' _computing_data_collection 'Bruker SMART (Bruker, 1999)' _computing_data_reduction 'Bruker SAINT (Bruker, 1999)' _computing_molecular_graphics 'Xtal_GX (Hall & du Boulay, 1997)' _computing_publication_material SHELXL-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997a)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997b)' _diffrn_ambient_temperature 100(2) _diffrn_detector_area_resol_mean 8.26 _diffrn_measured_fraction_theta_full 0.990 _diffrn_measured_fraction_theta_max 0.925 _diffrn_measurement_device_type 'Bruker SMART APEX CCD system' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0190 _diffrn_reflns_av_sigmaI/netI 0.0195 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 7924 _diffrn_reflns_theta_full 26.80 _diffrn_reflns_theta_max 28.10 _diffrn_reflns_theta_min 1.91 _diffrn_standards_decay_% 0.0 _diffrn_standards_number 235 _exptl_absorpt_coefficient_mu 0.784 _exptl_absorpt_correction_T_max 0.859 _exptl_absorpt_correction_T_min 0.743 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Bruker SADABS (Bruker, 1999)' _exptl_crystal_colour purple _exptl_crystal_density_diffrn 1.584 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prismatic _exptl_crystal_F_000 338 _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _refine_diff_density_max 0.537 _refine_diff_density_min -0.384 _refine_diff_density_rms 0.066 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.147 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 210 _refine_ls_number_reflns 3077 _refine_ls_number_restraints 4 _refine_ls_restrained_S_all 1.147 _refine_ls_R_factor_all 0.0287 _refine_ls_R_factor_gt 0.0284 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0400P)^2^+0.3000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0772 _refine_ls_wR_factor_ref 0.0773 _reflns_number_gt 3020 _reflns_number_total 3077 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file dmaxpycompound3.cif _[local]_cod_data_source_block niaxpyr _cod_database_code 1500033 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' 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 Ni Ni 0.5000 0.5000 0.5000 0.01093(9) Uani 1 2 d S . . N1 N 0.83659(17) 0.41187(16) 0.27434(11) 0.0153(2) Uani 1 1 d . . . N2 N 0.66164(17) 0.42992(16) 0.31259(11) 0.0138(2) Uani 1 1 d . . . N3 N 0.62022(17) 0.37901(16) 0.22333(11) 0.0151(2) Uani 1 1 d . . . C3A C 0.7825(2) 0.32516(18) 0.12444(13) 0.0144(3) Uani 1 1 d . . . N4 N 0.81997(18) 0.25761(17) 0.00842(11) 0.0167(2) Uani 1 1 d . . . C4 C 0.6714(2) 0.2479(2) -0.02346(15) 0.0222(3) Uani 1 1 d . . . H41 H 0.6344 0.3342 -0.0853 0.027 Uiso 1 1 d R . . H42 H 0.5591 0.2744 0.0522 0.027 Uiso 1 1 d R . . H43 H 0.7216 0.1281 -0.0588 0.027 Uiso 1 1 d R . . C5 C 0.9973(2) 0.20715(19) -0.08081(13) 0.0176(3) Uani 1 1 d . . . O5 O 1.03566(16) 0.14882(15) -0.18611(10) 0.0230(2) Uani 1 1 d . . . N6 N 1.13390(18) 0.22448(18) -0.04868(12) 0.0188(3) Uani 1 1 d . . . C6 C 1.3237(2) 0.1663(2) -0.14685(15) 0.0272(4) Uani 1 1 d . . . H61 H 1.3755 0.0433 -0.1764 0.033 Uiso 1 1 d R . . H62 H 1.4109 0.1744 -0.1124 0.033 Uiso 1 1 d R . . H63 H 1.3106 0.2429 -0.2171 0.033 Uiso 1 1 d R . . C7 C 1.1054(2) 0.2976(2) 0.06587(14) 0.0177(3) Uani 1 1 d . . . O7 O 1.23137(16) 0.31511(17) 0.08280(11) 0.0253(3) Uani 1 1 d . . . C7A C 0.9173(2) 0.34490(19) 0.15360(13) 0.0150(3) Uani 1 1 d . . . N1P N 0.35328(16) 0.76517(15) 0.46105(11) 0.0130(2) Uani 1 1 d . . . C2P C 0.2748(2) 0.81106(19) 0.37042(13) 0.0154(3) Uani 1 1 d . . . H2P H 0.2860 0.7200 0.3233 0.018 Uiso 1 1 d R . . C3P C 0.1784(2) 0.9855(2) 0.34263(14) 0.0182(3) Uani 1 1 d . . . H3P H 0.1215 1.0137 0.2794 0.022 Uiso 1 1 d R . . C4P C 0.1664(2) 1.1182(2) 0.40875(14) 0.0197(3) Uani 1 1 d . . . H4P H 0.1036 1.2388 0.3905 0.024 Uiso 1 1 d R . . C5P C 0.2475(2) 1.07200(19) 0.50233(14) 0.0185(3) Uani 1 1 d . . . H5P H 0.2418 1.1603 0.5490 0.022 Uiso 1 1 d R . . C6P C 0.3372(2) 0.89487(19) 0.52668(13) 0.0160(3) Uani 1 1 d . . . H6P H 0.3892 0.8642 0.5925 0.019 Uiso 1 1 d R . . O1W O 0.70872(14) 0.55642(13) 0.51311(9) 0.0145(2) Uani 1 1 d D . . H11W H 0.756(2) 0.531(2) 0.5695(14) 0.017 Uiso 1 1 d D . . H12W H 0.800(2) 0.521(2) 0.4467(12) 0.017 Uiso 1 1 d D . . O2W O 0.88019(18) 0.47083(16) 0.69068(11) 0.0248(2) Uani 1 1 d D . . H21W H 0.930(3) 0.3680(16) 0.7154(19) 0.030 Uiso 1 1 d D . . H22W H 0.821(3) 0.540(2) 0.7554(14) 0.030 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 Ni 0.01153(13) 0.01068(13) 0.01020(13) -0.00027(8) -0.00363(9) -0.00479(10) N1 0.0143(6) 0.0171(6) 0.0138(6) 0.0004(4) -0.0038(4) -0.0074(5) N2 0.0140(5) 0.0149(5) 0.0126(5) 0.0005(4) -0.0050(4) -0.0065(5) N3 0.0154(6) 0.0175(6) 0.0127(6) -0.0011(4) -0.0048(4) -0.0074(5) C3A 0.0154(6) 0.0142(6) 0.0128(6) 0.0009(5) -0.0051(5) -0.0062(5) N4 0.0161(6) 0.0216(6) 0.0123(6) -0.0018(5) -0.0045(5) -0.0083(5) C4 0.0220(7) 0.0297(8) 0.0186(7) -0.0030(6) -0.0081(6) -0.0131(7) C5 0.0190(7) 0.0174(7) 0.0137(7) 0.0011(5) -0.0053(5) -0.0066(6) O5 0.0251(6) 0.0271(6) 0.0126(5) -0.0036(4) -0.0033(4) -0.0103(5) N6 0.0149(6) 0.0241(6) 0.0127(6) -0.0007(5) -0.0014(5) -0.0075(5) C6 0.0172(7) 0.0372(9) 0.0178(7) -0.0025(6) 0.0021(6) -0.0105(7) C7 0.0155(7) 0.0206(7) 0.0154(7) 0.0013(5) -0.0046(5) -0.0077(6) O7 0.0176(5) 0.0390(7) 0.0210(6) -0.0025(5) -0.0041(4) -0.0154(5) C7A 0.0144(6) 0.0169(7) 0.0131(6) 0.0008(5) -0.0046(5) -0.0069(5) N1P 0.0120(5) 0.0129(5) 0.0129(5) 0.0006(4) -0.0033(4) -0.0057(4) C2P 0.0159(6) 0.0167(7) 0.0136(6) 0.0005(5) -0.0042(5) -0.0082(5) C3P 0.0163(7) 0.0198(7) 0.0157(7) 0.0041(5) -0.0056(5) -0.0070(6) C4P 0.0169(7) 0.0141(6) 0.0222(7) 0.0034(5) -0.0041(6) -0.0050(5) C5P 0.0171(7) 0.0138(7) 0.0222(7) -0.0024(5) -0.0037(6) -0.0067(6) C6P 0.0156(6) 0.0160(7) 0.0169(7) -0.0003(5) -0.0056(5) -0.0073(5) O1W 0.0149(5) 0.0164(5) 0.0128(5) -0.0003(4) -0.0053(4) -0.0072(4) O2W 0.0312(6) 0.0239(6) 0.0243(6) 0.0030(5) -0.0158(5) -0.0128(5) 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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ni N2 179.999(1) 2_666 . ? N2 Ni N1P 91.03(4) 2_666 2_666 ? N2 Ni N1P 88.97(4) . 2_666 ? N2 Ni N1P 88.97(4) 2_666 . ? N2 Ni N1P 91.03(4) . . ? N1P Ni N1P 180.00(7) 2_666 . ? N2 Ni O1W 87.07(4) 2_666 2_666 ? N2 Ni O1W 92.93(4) . 2_666 ? N1P Ni O1W 87.78(4) 2_666 2_666 ? N1P Ni O1W 92.22(4) . 2_666 ? N2 Ni O1W 92.93(4) 2_666 . ? N2 Ni O1W 87.08(4) . . ? N1P Ni O1W 92.22(4) 2_666 . ? N1P Ni O1W 87.78(4) . . ? O1W Ni O1W 180.0 2_666 . ? N2 N1 C7A 105.32(11) . . ? N1 N2 N3 113.76(11) . . ? N1 N2 Ni 117.69(9) . . ? N3 N2 Ni 128.09(9) . . ? C3A N3 N2 103.41(11) . . ? N3 C3A N4 127.74(13) . . ? N3 C3A C7A 110.10(12) . . ? N4 C3A C7A 122.16(13) . . ? C5 N4 C3A 119.06(13) . . ? C5 N4 C4 119.47(12) . . ? C3A N4 C4 121.39(12) . . ? N4 C4 H41 109.6 . . ? N4 C4 H42 109.6 . . ? H41 C4 H42 109.5 . . ? N4 C4 H43 109.3 . . ? H41 C4 H43 109.5 . . ? H42 C4 H43 109.5 . . ? O5 C5 N4 121.12(14) . . ? O5 C5 N6 120.85(14) . . ? N4 C5 N6 118.03(13) . . ? C5 N6 C7 126.48(12) . . ? C5 N6 C6 116.27(13) . . ? C7 N6 C6 117.20(13) . . ? N6 C6 H61 109.6 . . ? N6 C6 H62 109.5 . . ? H61 C6 H62 109.5 . . ? N6 C6 H63 109.3 . . ? H61 C6 H63 109.5 . . ? H62 C6 H63 109.5 . . ? O7 C7 N6 121.61(13) . . ? O7 C7 C7A 126.86(14) . . ? N6 C7 C7A 111.53(13) . . ? N1 C7A C3A 107.41(12) . . ? N1 C7A C7 129.94(13) . . ? C3A C7A C7 122.65(13) . . ? C6P N1P C2P 118.07(12) . . ? C6P N1P Ni 120.01(9) . . ? C2P N1P Ni 121.92(9) . . ? N1P C2P C3P 122.80(13) . . ? N1P C2P H2P 118.6 . . ? C3P C2P H2P 118.6 . . ? C4P C3P C2P 118.77(13) . . ? C4P C3P H3P 120.6 . . ? C2P C3P H3P 120.7 . . ? C3P C4P C5P 118.82(14) . . ? C3P C4P H4P 120.7 . . ? C5P C4P H4P 120.5 . . ? C6P C5P C4P 118.92(14) . . ? C6P C5P H5P 120.5 . . ? C4P C5P H5P 120.6 . . ? N1P C6P C5P 122.58(13) . . ? N1P C6P H6P 118.8 . . ? C5P C6P H6P 118.7 . . ? Ni O1W H11W 127.5(13) . . ? Ni O1W H12W 108.5(13) . . ? H11W O1W H12W 105.7(18) . . ? H21W O2W H22W 106(2) . . ? 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 Ni N2 2.0637(12) 2_666 ? Ni N2 2.0637(12) . ? Ni N1P 2.0942(12) 2_666 ? Ni N1P 2.0943(12) . ? Ni O1W 2.0950(10) 2_666 ? Ni O1W 2.0950(10) . ? N1 N2 1.3195(17) . ? N1 C7A 1.3571(18) . ? N2 N3 1.3608(16) . ? N3 C3A 1.3386(18) . ? C3A N4 1.3774(18) . ? C3A C7A 1.3785(19) . ? N4 C5 1.3697(19) . ? N4 C4 1.4638(19) . ? C4 H41 0.9800 . ? C4 H42 0.9800 . ? C4 H43 0.9800 . ? C5 O5 1.2290(18) . ? C5 N6 1.401(2) . ? N6 C7 1.4092(19) . ? N6 C6 1.4743(19) . ? C6 H61 0.9800 . ? C6 H62 0.9800 . ? C6 H63 0.9800 . ? C7 O7 1.2235(19) . ? C7 C7A 1.4319(19) . ? N1P C6P 1.3419(18) . ? N1P C2P 1.3427(18) . ? C2P C3P 1.385(2) . ? C2P H2P 0.9500 . ? C3P C4P 1.384(2) . ? C3P H3P 0.9500 . ? C4P C5P 1.387(2) . ? C4P H4P 0.9500 . ? C5P C6P 1.385(2) . ? C5P H5P 0.9500 . ? C6P H6P 0.9500 . ? O1W H11W 0.831(9) . ? O1W H12W 0.825(9) . ? O2W H21W 0.842(9) . ? O2W H22W 0.839(9) . ? 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 H11W O2W 0.831(9) 1.899(9) 2.7286(15) 176.4(19) . O1W H12W N1 0.825(9) 2.137(15) 2.7501(16) 131.0(16) . O2W H21W O5 0.842(9) 2.056(11) 2.8809(17) 166(2) 1_556 O2W H22W O7 0.839(9) 2.143(12) 2.9467(16) 160(2) 2_766