#------------------------------------------------------------------------------ #$Date: 2014-07-12 07:06:18 +0300 (Sat, 12 Jul 2014) $ #$Revision: 120112 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/05/26/7052618.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_7052618 loop_ _publ_author_name 'Gong, Yunnan' 'Liu, Chongbo' 'Wen, Huiliang' 'Yan, Liushui' 'Xiong, Zhiqiang' 'Ding, Liang' _publ_section_title ; Structural diversity and properties of M(ii) phenyl substituted pyrazole carboxylate complexes with 0D-, 1D-, 2D- and 3D frameworks ; _journal_issue 4 _journal_name_full 'New Journal of Chemistry' _journal_page_first 865 _journal_volume 35 _journal_year 2011 _chemical_formula_sum 'C20 H18 N4 Ni O6' _chemical_formula_weight 469.09 _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 geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 79.7360(10) _cell_angle_beta 82.9990(10) _cell_angle_gamma 75.0920(10) _cell_formula_units_Z 1 _cell_length_a 6.6139(7) _cell_length_b 6.9872(7) _cell_length_c 10.4414(11) _cell_measurement_reflns_used 1808 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 28.22 _cell_measurement_theta_min 3.38 _cell_volume 457.35(8) _computing_cell_refinement 'Bruker SMART' _computing_data_collection 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 296(2) _diffrn_measured_fraction_theta_full 0.989 _diffrn_measured_fraction_theta_max 0.989 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega 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 0.0289 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 3527 _diffrn_reflns_theta_full 25.50 _diffrn_reflns_theta_max 25.50 _diffrn_reflns_theta_min 3.05 _exptl_absorpt_coefficient_mu 1.112 _exptl_absorpt_correction_T_max 0.7460 _exptl_absorpt_correction_T_min 0.7174 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details sadabs _exptl_crystal_colour blue _exptl_crystal_density_diffrn 1.703 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 242 _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.28 _refine_diff_density_max 0.351 _refine_diff_density_min -0.286 _refine_diff_density_rms 0.057 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 142 _refine_ls_number_reflns 1683 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.077 _refine_ls_R_factor_all 0.0327 _refine_ls_R_factor_gt 0.0292 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0303P)^2^+0.2683P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0670 _refine_ls_wR_factor_ref 0.0689 _reflns_number_gt 1548 _reflns_number_total 1683 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file c0nj00904k.txt _[local]_cod_data_source_block 4 _[local]_cod_cif_authors_sg_H-M P-1 _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1555 2011-01-17 13:19:09Z saulius ; _cod_database_code 7052618 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 Ni1 Ni 0.5000 0.0000 0.5000 0.01709(13) Uani 1 2 d S . . O1 O 0.3139(3) 0.8312(2) 0.44969(16) 0.0297(4) Uani 1 1 d . . . O2 O 0.0696(2) 0.9497(2) 0.30675(15) 0.0248(4) Uani 1 1 d . . . O3 O 0.6455(2) 0.0138(2) 0.30931(15) 0.0289(4) Uani 1 1 d . . . H1W H 0.7728 -0.0072 0.3122 0.043 Uiso 1 1 d R . . H2W H 0.6113 -0.0846 0.2742 0.043 Uiso 1 1 d R . . N1 N 0.2812(3) 0.2630(3) 0.44194(17) 0.0189(4) Uani 1 1 d . . . N2 N 0.1528(3) 0.3029(3) 0.34414(16) 0.0192(4) Uani 1 1 d . . . H2 H 0.1171 0.2125 0.3119 0.023 Uiso 1 1 calc R . . C1 C 0.2940(3) 0.4400(3) 0.4634(2) 0.0175(4) Uani 1 1 d . . . H1 H 0.3697 0.4580 0.5279 0.021 Uiso 1 1 calc R . . C2 C 0.1808(3) 0.5968(3) 0.37821(19) 0.0166(4) Uani 1 1 d . . . C3 C 0.0875(3) 0.5017(3) 0.3032(2) 0.0173(4) Uani 1 1 d . . . C4 C 0.1849(3) 0.8095(3) 0.3774(2) 0.0180(4) Uani 1 1 d . . . C5 C -0.0626(3) 0.5775(3) 0.2011(2) 0.0200(5) Uani 1 1 d . . . C6 C -0.0292(4) 0.7220(3) 0.0968(2) 0.0274(5) Uani 1 1 d . . . H6 H 0.0916 0.7693 0.0886 0.033 Uiso 1 1 calc R . . C7 C -0.1744(5) 0.7960(4) 0.0048(2) 0.0394(7) Uani 1 1 d . . . H7 H -0.1496 0.8914 -0.0656 0.047 Uiso 1 1 calc R . . C8 C -0.3545(5) 0.7300(4) 0.0164(3) 0.0436(7) Uani 1 1 d . . . H8 H -0.4536 0.7835 -0.0445 0.052 Uiso 1 1 calc R . . C9 C -0.3889(4) 0.5834(4) 0.1190(3) 0.0385(6) Uani 1 1 d . . . H9 H -0.5104 0.5372 0.1265 0.046 Uiso 1 1 calc R . . C10 C -0.2419(4) 0.5055(4) 0.2105(2) 0.0271(5) Uani 1 1 d . . . H10 H -0.2635 0.4049 0.2783 0.033 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0195(2) 0.0099(2) 0.0228(2) -0.00227(14) -0.00732(15) -0.00281(15) O1 0.0303(9) 0.0150(8) 0.0486(10) -0.0051(7) -0.0208(8) -0.0059(7) O2 0.0309(9) 0.0123(7) 0.0326(8) -0.0012(6) -0.0128(7) -0.0043(6) O3 0.0261(9) 0.0297(9) 0.0298(8) -0.0049(7) -0.0039(7) -0.0037(7) N1 0.0203(9) 0.0133(9) 0.0240(9) -0.0018(7) -0.0076(7) -0.0036(7) N2 0.0221(10) 0.0120(9) 0.0257(9) -0.0057(7) -0.0083(8) -0.0034(7) C1 0.0167(11) 0.0141(10) 0.0232(10) -0.0040(8) -0.0043(8) -0.0043(8) C2 0.0158(10) 0.0122(10) 0.0220(10) -0.0030(8) -0.0023(8) -0.0032(8) C3 0.0184(11) 0.0122(10) 0.0218(10) -0.0019(8) -0.0012(8) -0.0051(8) C4 0.0165(10) 0.0135(10) 0.0252(11) -0.0049(8) -0.0014(9) -0.0041(8) C5 0.0229(11) 0.0148(10) 0.0231(10) -0.0077(8) -0.0056(9) -0.0008(9) C6 0.0369(14) 0.0182(11) 0.0290(12) -0.0031(9) -0.0062(10) -0.0090(10) C7 0.0626(19) 0.0251(13) 0.0292(13) -0.0005(10) -0.0162(13) -0.0049(13) C8 0.0482(17) 0.0407(16) 0.0404(15) -0.0096(13) -0.0274(13) 0.0055(13) C9 0.0266(14) 0.0539(17) 0.0399(14) -0.0169(13) -0.0101(11) -0.0084(12) C10 0.0281(13) 0.0304(13) 0.0261(11) -0.0083(10) -0.0033(10) -0.0093(10) 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 N1 Ni1 N1 180.0 . 2_656 ? N1 Ni1 O1 90.97(6) . 1_545 ? N1 Ni1 O1 89.03(6) 2_656 1_545 ? N1 Ni1 O1 89.03(6) . 2_666 ? N1 Ni1 O1 90.97(6) 2_656 2_666 ? O1 Ni1 O1 180.00(5) 1_545 2_666 ? N1 Ni1 O3 90.38(7) . 2_656 ? N1 Ni1 O3 89.62(7) 2_656 2_656 ? O1 Ni1 O3 90.93(7) 1_545 2_656 ? O1 Ni1 O3 89.07(7) 2_666 2_656 ? N1 Ni1 O3 89.62(7) . . ? N1 Ni1 O3 90.38(7) 2_656 . ? O1 Ni1 O3 89.07(7) 1_545 . ? O1 Ni1 O3 90.93(7) 2_666 . ? O3 Ni1 O3 180.0 2_656 . ? C4 O1 Ni1 150.44(14) . 1_565 ? Ni1 O3 H1W 109.4 . . ? Ni1 O3 H2W 105.6 . . ? H1W O3 H2W 111.2 . . ? C1 N1 N2 105.20(16) . . ? C1 N1 Ni1 122.98(14) . . ? N2 N1 Ni1 128.20(13) . . ? C3 N2 N1 111.82(16) . . ? C3 N2 H2 124.1 . . ? N1 N2 H2 124.1 . . ? N1 C1 C2 112.21(18) . . ? N1 C1 H1 123.9 . . ? C2 C1 H1 123.9 . . ? C1 C2 C3 104.12(17) . . ? C1 C2 C4 121.85(18) . . ? C3 C2 C4 133.97(18) . . ? N2 C3 C2 106.60(17) . . ? N2 C3 C5 120.38(18) . . ? C2 C3 C5 132.96(18) . . ? O2 C4 O1 125.04(19) . . ? O2 C4 C2 120.73(18) . . ? O1 C4 C2 114.21(17) . . ? C6 C5 C10 119.2(2) . . ? C6 C5 C3 121.1(2) . . ? C10 C5 C3 119.74(19) . . ? C7 C6 C5 120.3(2) . . ? C7 C6 H6 119.8 . . ? C5 C6 H6 119.8 . . ? C8 C7 C6 120.6(2) . . ? C8 C7 H7 119.7 . . ? C6 C7 H7 119.7 . . ? C7 C8 C9 119.9(2) . . ? C7 C8 H8 120.1 . . ? C9 C8 H8 120.1 . . ? C8 C9 C10 119.9(2) . . ? C8 C9 H9 120.0 . . ? C10 C9 H9 120.0 . . ? C9 C10 C5 120.1(2) . . ? C9 C10 H10 119.9 . . ? C5 C10 H10 119.9 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N1 2.0706(17) . ? Ni1 N1 2.0706(17) 2_656 ? Ni1 O1 2.0755(14) 1_545 ? Ni1 O1 2.0755(14) 2_666 ? Ni1 O3 2.1005(15) 2_656 ? Ni1 O3 2.1005(15) . ? O1 C4 1.259(2) . ? O1 Ni1 2.0755(14) 1_565 ? O2 C4 1.257(2) . ? O3 H1W 0.8200 . ? O3 H2W 0.9213 . ? N1 C1 1.320(3) . ? N1 N2 1.353(2) . ? N2 C3 1.351(3) . ? N2 H2 0.8600 . ? C1 C2 1.395(3) . ? C1 H1 0.9300 . ? C2 C3 1.396(3) . ? C2 C4 1.492(3) . ? C3 C5 1.479(3) . ? C5 C6 1.385(3) . ? C5 C10 1.390(3) . ? C6 C7 1.379(3) . ? C6 H6 0.9300 . ? C7 C8 1.369(4) . ? C7 H7 0.9300 . ? C8 C9 1.385(4) . ? C8 H8 0.9300 . ? C9 C10 1.387(3) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? 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 O3 H1W O2 0.82 1.90 2.721(2) 176.2 1_645 N2 H2 O2 0.86 1.95 2.764(2) 157.0 1_545 loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Ni1 N1 C1 -76(100) 2_656 . . . ? O1 Ni1 N1 C1 171.64(17) 1_545 . . . ? O1 Ni1 N1 C1 -8.36(17) 2_666 . . . ? O3 Ni1 N1 C1 80.70(17) 2_656 . . . ? O3 Ni1 N1 C1 -99.30(17) . . . . ? N1 Ni1 N1 N2 79(100) 2_656 . . . ? O1 Ni1 N1 N2 -33.07(17) 1_545 . . . ? O1 Ni1 N1 N2 146.93(17) 2_666 . . . ? O3 Ni1 N1 N2 -124.01(17) 2_656 . . . ? O3 Ni1 N1 N2 55.99(17) . . . . ? C1 N1 N2 C3 0.8(2) . . . . ? Ni1 N1 N2 C3 -157.92(15) . . . . ? N2 N1 C1 C2 -1.9(2) . . . . ? Ni1 N1 C1 C2 158.22(14) . . . . ? N1 C1 C2 C3 2.2(2) . . . . ? N1 C1 C2 C4 -175.39(19) . . . . ? N1 N2 C3 C2 0.6(2) . . . . ? N1 N2 C3 C5 -177.01(18) . . . . ? C1 C2 C3 N2 -1.6(2) . . . . ? C4 C2 C3 N2 175.6(2) . . . . ? C1 C2 C3 C5 175.5(2) . . . . ? C4 C2 C3 C5 -7.3(4) . . . . ? Ni1 O1 C4 O2 -20.3(5) 1_565 . . . ? Ni1 O1 C4 C2 158.3(2) 1_565 . . . ? C1 C2 C4 O2 -174.6(2) . . . . ? C3 C2 C4 O2 8.6(4) . . . . ? C1 C2 C4 O1 6.8(3) . . . . ? C3 C2 C4 O1 -170.0(2) . . . . ? N2 C3 C5 C6 -133.4(2) . . . . ? C2 C3 C5 C6 49.7(3) . . . . ? N2 C3 C5 C10 47.6(3) . . . . ? C2 C3 C5 C10 -129.3(3) . . . . ? C10 C5 C6 C7 1.2(3) . . . . ? C3 C5 C6 C7 -177.8(2) . . . . ? C5 C6 C7 C8 1.0(4) . . . . ? C6 C7 C8 C9 -2.0(4) . . . . ? C7 C8 C9 C10 0.7(4) . . . . ? C8 C9 C10 C5 1.5(4) . . . . ? C6 C5 C10 C9 -2.4(3) . . . . ? C3 C5 C10 C9 176.6(2) . . . . ? _journal_paper_doi 10.1039/c0nj00904k