#------------------------------------------------------------------------------ #$Date: 2012-02-28 14:14:52 +0200 (Tue, 28 Feb 2012) $ #$Revision: 35911 $ #$URL: file:///home/coder/svn-repositories/cod/cif/8/10/31/8103126.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_8103126 loop_ _publ_author_name 'Bo Xiao' 'Xia Zhang' 'Li-Jun Yang' 'Yu-Ting Wang' _publ_section_title ; Crystal structure of diaquabis(6-hydroxy-3-pyridazinecarboxylato)nickel(II) dihydrate, Ni(H2O)2(C5H3N2O3)2 · 2H2O ; _journal_issue 1 _journal_name_full 'Zeitschrift f\"ur Kristallographie - New Crystal Structures' _journal_page_first 23 _journal_volume 226 _journal_year 2011 _chemical_formula_sum 'C10 H14 N4 Ni O10' _chemical_formula_weight 408.96 _chemical_name_systematic ; diaqua-bis(6-hydroxy-3-pyridazinecarboxylic)nickel(II)dihydrate, [Ni(C~5~H~3~N~2~O~3~)~2~(H~2~O)~2~]^.^2H~2~O ; _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 _audit_update_record ; 2010-12-11 # Formatted by publCIF ; _cell_angle_alpha 61.470(15) _cell_angle_beta 81.414(11) _cell_angle_gamma 80.900(12) _cell_formula_units_Z 1 _cell_length_a 6.2893(8) _cell_length_b 8.3099(12) _cell_length_c 8.4622(12) _cell_measurement_reflns_used 1250 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 28.9731 _cell_measurement_theta_min 3.2857 _cell_volume 382.28(11) _computing_cell_refinement 'Bruker FRAMBO' _computing_data_collection 'Bruker FRAMBO' _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 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'multiwire proportional' _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 0.0305 _diffrn_reflns_av_sigmaI/netI 0.0614 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_number 2282 _diffrn_reflns_theta_full 25.50 _diffrn_reflns_theta_max 25.50 _diffrn_reflns_theta_min 3.29 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 1.333 _exptl_absorpt_correction_T_max 0.8564 _exptl_absorpt_correction_T_min 0.7316 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details sadabs _exptl_crystal_colour green _exptl_crystal_density_diffrn 1.776 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 210 _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.12 _refine_diff_density_max 1.313 _refine_diff_density_min -0.811 _refine_diff_density_rms 0.178 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.080 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 115 _refine_ls_number_reflns 1421 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.080 _refine_ls_R_factor_all 0.0681 _refine_ls_R_factor_gt 0.0592 _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^)+(0.1020P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1588 _refine_ls_wR_factor_ref 0.1622 _reflns_number_gt 1172 _reflns_number_total 1421 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file 1267-3340.cff _[local]_cod_data_source_block a _[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_values 1715 2011-07-08 13:25:40Z adriana ; _cod_original_cell_volume 382.28(9) _cod_database_code 8103126 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 Ni1 Ni 0.0000 0.0000 1.0000 0.0237(3) Uani 1 2 d S O1 O 0.2592(5) 0.0323(5) 1.0941(5) 0.0291(8) Uani 1 1 d . O2 O 0.4488(6) 0.2425(5) 1.0862(5) 0.0366(9) Uani 1 1 d . O3 O -0.2308(6) 0.7078(5) 0.5305(5) 0.0400(10) Uani 1 1 d . H3D H -0.2897 0.6475 0.4993 0.060 Uiso 1 1 calc R O4 O 0.1889(5) -0.0276(5) 0.7908(4) 0.0299(8) Uani 1 1 d . H1W H 0.3163 -0.0712 0.8220 0.045 Uiso 1 1 d R H2W H 0.1981 0.0728 0.6935 0.045 Uiso 1 1 d R O5 O 0.5680(7) 0.2871(6) 0.6490(6) 0.0534(12) Uani 1 1 d . H3W H 0.5906 0.1717 0.7159 0.080 Uiso 1 1 d R H4W H 0.6301 0.3533 0.6761 0.080 Uiso 1 1 d R N1 N 0.0041(6) 0.2905(5) 0.8609(5) 0.0220(9) Uani 1 1 d . N2 N -0.1294(6) 0.4191(6) 0.7368(5) 0.0267(9) Uani 1 1 d . C1 C -0.1040(8) 0.6032(7) 0.6461(6) 0.0260(11) Uani 1 1 d . C2 C 0.0668(8) 0.6610(7) 0.6950(7) 0.0324(12) Uani 1 1 d . H2 H 0.0869 0.7853 0.6419 0.039 Uiso 1 1 calc R C3 C 0.1992(8) 0.5342(7) 0.8187(7) 0.0301(11) Uani 1 1 d . H3 H 0.3131 0.5694 0.8500 0.036 Uiso 1 1 calc R C4 C 0.1606(7) 0.3468(7) 0.8997(6) 0.0218(10) Uani 1 1 d . C5 C 0.3047(7) 0.1948(7) 1.0384(6) 0.0254(11) 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 Ni1 0.0246(5) 0.0146(5) 0.0248(5) -0.0013(4) -0.0100(3) -0.0014(3) O1 0.0297(18) 0.0176(19) 0.0317(19) -0.0024(17) -0.0131(14) -0.0011(14) O2 0.035(2) 0.028(2) 0.046(2) -0.013(2) -0.0236(17) 0.0006(16) O3 0.051(2) 0.021(2) 0.035(2) 0.0028(18) -0.0252(18) -0.0018(17) O4 0.0309(19) 0.021(2) 0.0291(19) -0.0034(17) -0.0088(14) 0.0009(14) O5 0.064(3) 0.024(2) 0.060(3) 0.002(2) -0.039(2) -0.013(2) N1 0.023(2) 0.015(2) 0.0181(19) 0.0011(17) -0.0077(15) 0.0006(15) N2 0.031(2) 0.017(2) 0.021(2) 0.0015(18) -0.0117(16) 0.0033(16) C1 0.036(3) 0.013(2) 0.020(2) 0.000(2) -0.0086(19) 0.0027(19) C2 0.044(3) 0.014(3) 0.033(3) -0.002(2) -0.012(2) -0.004(2) C3 0.031(3) 0.026(3) 0.031(3) -0.009(2) -0.009(2) -0.005(2) C4 0.026(2) 0.015(2) 0.021(2) -0.004(2) -0.0080(18) 0.0000(18) C5 0.021(2) 0.026(3) 0.029(3) -0.012(2) -0.0049(19) -0.0013(19) 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 O1 Ni1 O1 180.0 2_557 . O1 Ni1 O4 87.97(13) 2_557 . O1 Ni1 O4 92.03(13) . . O1 Ni1 O4 92.03(13) 2_557 2_557 O1 Ni1 O4 87.97(13) . 2_557 O4 Ni1 O4 180.000(1) . 2_557 O1 Ni1 N1 78.44(14) 2_557 2_557 O1 Ni1 N1 101.56(14) . 2_557 O4 Ni1 N1 88.50(14) . 2_557 O4 Ni1 N1 91.50(14) 2_557 2_557 O1 Ni1 N1 101.56(14) 2_557 . O1 Ni1 N1 78.44(14) . . O4 Ni1 N1 91.50(14) . . O4 Ni1 N1 88.50(14) 2_557 . N1 Ni1 N1 180.00(12) 2_557 . C5 O1 Ni1 117.6(3) . . C1 O3 H3D 109.5 . . Ni1 O4 H1W 109.4 . . Ni1 O4 H2W 114.0 . . H1W O4 H2W 107.6 . . H3W O5 H4W 115.2 . . C4 N1 N2 118.0(4) . . C4 N1 Ni1 113.3(3) . . N2 N1 Ni1 128.7(3) . . N1 N2 C1 124.0(4) . . O3 C1 N2 118.7(5) . . O3 C1 C2 124.8(5) . . N2 C1 C2 116.5(4) . . C3 C2 C1 119.7(5) . . C3 C2 H2 120.2 . . C1 C2 H2 120.2 . . C2 C3 C4 118.6(5) . . C2 C3 H3 120.7 . . C4 C3 H3 120.7 . . N1 C4 C3 123.2(4) . . N1 C4 C5 115.0(4) . . C3 C4 C5 121.8(4) . . O2 C5 O1 127.1(5) . . O2 C5 C4 117.3(5) . . O1 C5 C4 115.6(4) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Ni1 O1 2.023(3) 2_557 Ni1 O1 2.023(3) . Ni1 O4 2.067(3) . Ni1 O4 2.067(3) 2_557 Ni1 N1 2.124(4) 2_557 Ni1 N1 2.124(4) . O1 C5 1.265(6) . O2 C5 1.232(6) . O3 C1 1.245(6) . O3 H3D 0.8200 . O4 H1W 0.8500 . O4 H2W 0.8500 . O5 H3W 0.8499 . O5 H4W 0.8500 . N1 C4 1.297(6) . N1 N2 1.363(5) . N2 C1 1.369(6) . C1 C2 1.429(7) . C2 C3 1.352(7) . C2 H2 0.9300 . C3 C4 1.416(7) . C3 H3 0.9300 . C4 C5 1.528(7) . 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 O5 H4W N2 0.85 1.90 2.690(6) 153.9 1_655 O5 H3W O1 0.85 1.92 2.690(5) 149.5 2_657 O4 H2W O3 0.85 1.91 2.763(5) 177.0 2_566 O4 H1W O2 0.85 1.85 2.667(5) 159.6 2_657 O3 H3D O5 0.82 2.15 2.771(5) 132.1 2_566 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 O1 Ni1 O1 C5 -50(100) 2_557 O4 Ni1 O1 C5 92.4(3) . O4 Ni1 O1 C5 -87.6(3) 2_557 N1 Ni1 O1 C5 -178.7(3) 2_557 N1 Ni1 O1 C5 1.3(3) . O1 Ni1 N1 C4 -179.9(3) 2_557 O1 Ni1 N1 C4 0.1(3) . O4 Ni1 N1 C4 -91.7(3) . O4 Ni1 N1 C4 88.3(3) 2_557 N1 Ni1 N1 C4 157(100) 2_557 O1 Ni1 N1 N2 -1.9(4) 2_557 O1 Ni1 N1 N2 178.1(4) . O4 Ni1 N1 N2 86.3(4) . O4 Ni1 N1 N2 -93.7(4) 2_557 N1 Ni1 N1 N2 -25(100) 2_557 C4 N1 N2 C1 2.3(7) . Ni1 N1 N2 C1 -175.6(3) . N1 N2 C1 O3 177.4(4) . N1 N2 C1 C2 -3.7(7) . O3 C1 C2 C3 -178.0(5) . N2 C1 C2 C3 3.2(7) . C1 C2 C3 C4 -1.5(7) . N2 N1 C4 C3 -0.4(7) . Ni1 N1 C4 C3 177.9(4) . N2 N1 C4 C5 -179.4(4) . Ni1 N1 C4 C5 -1.2(5) . C2 C3 C4 N1 0.0(8) . C2 C3 C4 C5 179.0(4) . Ni1 O1 C5 O2 176.4(4) . Ni1 O1 C5 C4 -2.3(5) . N1 C4 C5 O2 -176.5(4) . C3 C4 C5 O2 4.5(7) . N1 C4 C5 O1 2.3(6) . C3 C4 C5 O1 -176.8(4) .