#------------------------------------------------------------------------------ #$Date: 2015-04-02 12:22:18 +0100 (Thu, 02 Apr 2015) $ #$Revision: 134621 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/83/2008356.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2008356 loop_ _publ_author_name 'Sobanska, Sophie' 'Lagrenee, Michel' 'Wignacourt, Jean-Pierre' 'Holt, Elizabeth M.' _publ_section_title ;Diaquabis(pyridazin-1-ium-3,6-dicarboxylato-N^2^,O^3^)copper(II) dihydrate ; _journal_issue 4 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 553 _journal_page_last 555 _journal_paper_doi 10.1107/S0108270199000116 _journal_volume 55 _journal_year 1999 _chemical_formula_iupac '[Cu (C6 H3 N2 O4)2 (H2 O)2], 2H2 O' _chemical_formula_moiety 'C12 H14 Cu N4 O12' _chemical_formula_sum 'C12 H14 Cu N4 O12' _chemical_formula_weight 469.81 _chemical_name_common ; Copper(II)diaquadi(3,6-dicarboxylatopyridazinium)dihydrate ; _chemical_name_systematic ; Copper(II)diaquadi(3,6-dicarboxylatopyridazinium)dihydrate ; _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _cell_angle_alpha 74.52(3) _cell_angle_beta 79.40(3) _cell_angle_gamma 70.30(3) _cell_formula_units_Z 1 _cell_length_a 5.406(4) _cell_length_b 6.512(4) _cell_length_c 13.118(5) _cell_measurement_reflns_used 25 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 29.6 _cell_measurement_theta_min 15.0 _cell_volume 416.7(4) _computing_cell_refinement XSCANS _computing_data_collection 'XSCANS (Siemens, 1991)' _computing_data_reduction XSCANS _computing_molecular_graphics 'XP (Siemens, 1990)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1990)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.919 _diffrn_measured_fraction_theta_max 0.919 _diffrn_measurement_device_type 'Phillips PW1100' _diffrn_measurement_method \w-2\q _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71069 _diffrn_reflns_av_R_equivalents 0.017 _diffrn_reflns_av_sigmaI/netI 0.0497 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 2343 _diffrn_reflns_theta_full 30.05 _diffrn_reflns_theta_max 30.05 _diffrn_reflns_theta_min 3.24 _diffrn_standards_decay_% <1 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time 60 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 1.391 _exptl_absorpt_correction_type none _exptl_crystal_colour green-blue _exptl_crystal_density_diffrn 1.872 _exptl_crystal_density_method 'not measured' _exptl_crystal_description needle _exptl_crystal_F_000 239 _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _refine_diff_density_max 0.49 _refine_diff_density_min -0.57 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.083 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 133 _refine_ls_number_reflns 2253 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.083 _refine_ls_R_factor_all 0.038 _refine_ls_R_factor_gt 0.035 _refine_ls_shift/su_max <0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0355P)^2^+0.2065P] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref 0.090 _reflns_number_gt 2144 _reflns_number_total 2253 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file fr1155.cif _[local]_cod_data_source_block FR1155 _[local]_cod_cif_authors_sg_H-M 'P -1 ' _cod_depositor_comments ; The following automatic conversions were performed: '_refine_ls_weighting_scheme' value 'calc w = 1/[\s^2^(Fo^2^)+(0.0355P)^2^+0.2065P] where P = (Fo^2^+2Fc^2^)/3' was changed to 'calc'. New tag '_refine_ls_weighting_details' was created. The value of the new tag was set to 'w = 1/[\s^2^(Fo^2^)+(0.0355P)^2^+0.2065P] where P = (Fo^2^+2Fc^2^)/3'. Automatic conversion script Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas ; _cod_database_code 2008356 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol Cu1 0.5 0.5 0.5 0.02645(12) Uani d S 1 . . Cu N1 0.6633(3) 0.5295(3) 0.35174(13) 0.0227(3) Uani d . 1 . . N N2 0.9081(3) 0.4187(3) 0.32161(13) 0.0246(3) Uani d . 1 . . N H2 1.0320 0.3842 0.3659 0.050 Uiso d R 1 . . H C3 0.9876(4) 0.4497(3) 0.21853(16) 0.0249(4) Uani d . 1 . . C C4 0.8285(5) 0.5928(4) 0.14063(17) 0.0297(4) Uani d . 1 . . C H4A 0.8933 0.6102 0.0666 0.080 Uiso d R 1 . . H C5 0.5754(5) 0.7080(4) 0.17333(16) 0.0295(4) Uani d . 1 . . C H5A 0.4563 0.8106 0.1234 0.080 Uiso d R 1 . . H C7 0.2236(4) 0.7753(3) 0.33136(16) 0.0244(4) Uani d . 1 . . C C8 1.2709(4) 0.3193(4) 0.19226(17) 0.0287(4) Uani d . 1 . . C O1 0.1948(3) 0.7219(3) 0.43240(12) 0.0289(3) Uani d . 1 . . O O2 0.0534(3) 0.8954(3) 0.27335(14) 0.0385(4) Uani d . 1 . . O O3 1.4177(3) 0.2143(3) 0.26413(13) 0.0368(4) Uani d . 1 . . O O4 1.3492(4) 0.3295(4) 0.09490(13) 0.0442(5) Uani d . 1 . . O C6 0.4989(4) 0.6706(3) 0.28176(16) 0.0231(4) Uani d . 1 . . C O88 0.6679(3) 0.7944(3) 0.52700(15) 0.0362(4) Uani d . 1 . . O H88A 0.8263 0.7777 0.4991 0.050 Uiso d R 1 . . H H88B 0.6982 0.7868 0.5894 0.050 Uiso d R 1 . . H O99 0.8729(4) 0.1202(3) 0.07403(15) 0.0446(4) Uani d . 1 . . O H99A 0.9164 0.0379 0.1342 0.050 Uiso d R 1 . . H H99B 0.7157 0.1535 0.0590 0.050 Uiso d R 1 . . H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Cu1 0.02031(18) 0.0334(2) 0.01536(17) 0.00197(13) -0.00034(11) -0.00253(13) N1 0.0212(7) 0.0262(8) 0.0182(7) -0.0046(6) -0.0011(6) -0.0048(6) N2 0.0212(8) 0.0307(9) 0.0187(7) -0.0036(6) -0.0018(6) -0.0059(6) C3 0.0261(9) 0.0269(9) 0.0219(9) -0.0082(7) 0.0009(7) -0.0077(7) C4 0.0345(11) 0.0330(11) 0.0194(9) -0.0099(9) 0.0009(8) -0.0049(8) C5 0.0336(11) 0.0307(10) 0.0192(9) -0.0058(8) -0.0043(8) -0.0012(8) C7 0.0232(9) 0.0228(9) 0.0247(9) -0.0047(7) -0.0031(7) -0.0036(7) C8 0.0268(10) 0.0331(11) 0.0252(9) -0.0083(8) 0.0044(7) -0.0106(8) O1 0.0214(7) 0.0356(8) 0.0210(7) 0.0001(6) -0.0022(5) -0.0033(6) O2 0.0299(8) 0.0450(10) 0.0305(8) -0.0001(7) -0.0109(7) -0.0011(7) O3 0.0267(8) 0.0475(10) 0.0283(8) -0.0006(7) -0.0012(6) -0.0103(7) O4 0.0318(9) 0.0694(13) 0.0232(8) -0.0042(8) 0.0039(6) -0.0157(8) C6 0.0248(9) 0.0224(9) 0.0210(9) -0.0060(7) -0.0031(7) -0.0041(7) O88 0.0237(7) 0.0351(9) 0.0453(10) -0.0043(6) -0.0034(7) -0.0075(7) O99 0.0464(10) 0.0500(11) 0.0312(9) -0.0109(9) -0.0053(8) -0.0025(8) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 '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' H H 0.0000 0.0000 '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_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O1 Cu1 O1 2_666 . 180.0 no O1 Cu1 N1 2_666 2_666 82.26(8) yes O1 Cu1 N1 . 2_666 97.74(8) no O1 Cu1 N1 2_666 . 97.74(8) no O1 Cu1 N1 . . 82.26(8) no N1 Cu1 N1 2_666 . 180.0 no N2 N1 C6 . . 121.86(17) no N2 N1 Cu1 . . 124.82(13) no C6 N1 Cu1 . . 113.30(14) no N1 N2 C3 . . 118.02(18) no N1 N2 H2 . . 118.1 no C3 N2 H2 . . 116.9 no N2 C3 C4 . . 123.7(2) no N2 C3 C8 . . 114.06(19) no C4 C3 C8 . . 122.26(19) no C5 C4 C3 . . 117.57(19) no C5 C4 H4A . . 121.3 no C3 C4 H4A . . 121.2 no C4 C5 C6 . . 117.1(2) no C4 C5 H5A . . 121.5 no C6 C5 H5A . . 121.3 no O2 C7 O1 . . 126.6(2) no O2 C7 C6 . . 119.04(19) no O1 C7 C6 . . 114.37(17) no O3 C8 O4 . . 123.0(2) no O3 C8 C3 . . 120.61(19) no O4 C8 C3 . . 116.3(2) no C7 O1 Cu1 . . 115.84(13) no N1 C6 C5 . . 121.75(19) no N1 C6 C7 . . 114.05(17) no C5 C6 C7 . . 124.15(18) no H88A O88 H88B . . 96.0 no H99A O99 H99B . . 119.8 no loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Cu1 O1 2_666 1.9603(19) yes Cu1 O1 . 1.9603(19) no Cu1 N1 2_666 1.9701(18) yes Cu1 N1 . 1.9701(18) no N1 N2 . 1.321(2) yes N1 C6 . 1.333(3) yes N2 C3 . 1.324(3) yes N2 H2 . 0.900 no C3 C4 . 1.388(3) yes C3 C8 . 1.507(3) yes C4 C5 . 1.372(3) yes C4 H4A . 0.9600 no C5 C6 . 1.386(3) yes C5 H5A . 0.9600 no C7 O2 . 1.222(3) yes C7 O1 . 1.271(3) yes C7 C6 . 1.516(3) yes C8 O3 . 1.246(3) yes C8 O4 . 1.261(3) yes O88 H88A . 0.8500 no O88 H88B . 0.8499 no O99 H99A . 0.8500 no O99 H99B . 0.8500 no loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA N2 H2 O1 2_666 0.90 2.72 3.109(3) 108 N2 H2 O3 1_555 0.90 2.36 2.688(3) 102 O88 H88A O1 1_655 0.85 1.98 2.825(3) 177 O88 H88B O3 2_766 0.85 1.91 2.682(3) 151 O99 H99A O2 1_645 0.85 1.97 2.804(3) 168 O99 H99B O4 1_455 0.85 1.97 2.694(3) 143