#------------------------------------------------------------------------------ #$Date: 2016-02-20 03:06:23 +0000 (Sat, 20 Feb 2016) $ #$Revision: 176774 $ #$URL: svn://www.crystallography.net/cod/cif/2/20/22/2202233.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_2202233 loop_ _publ_author_name 'Yun Chen' 'Ping Liu' 'Jian Wang' 'Wen-Dan Cheng' _publ_section_title ; Polymeric aqua(\m~4~-maleato-\k^4^O)pyridylnickel(II) ; _journal_issue 6 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first m393 _journal_page_last m395 _journal_paper_doi 10.1107/S1600536803011231 _journal_volume 59 _journal_year 2003 _chemical_formula_iupac 'Ni (C4 H2 O4) (C5 H5 N) (H2 O)]' _chemical_formula_moiety 'C9 H9 N Ni O5' _chemical_formula_sum 'C9 H9 N Ni O5' _chemical_formula_weight 269.88 _chemical_name_systematic aqua(\m~4~-maleato-\k^4^O)pyridylnickel(II) _space_group_IT_number 62 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall '-P 2ac 2n' _symmetry_space_group_name_H-M 'P n m a' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 17.9522(13) _cell_length_b 7.5712(5) _cell_length_c 7.4092(6) _cell_measurement_reflns_used 29 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 25.03 _cell_measurement_theta_min 2.27 _cell_volume 1007.06(13) _computing_cell_refinement SMART _computing_data_collection 'SMART (Siemens, 1996)' _computing_data_reduction 'XPREP/SAINT (Siemens, 1994)' _computing_molecular_graphics 'SHELXL97 (Sheldrick, 1997)' _computing_publication_material SHELXL97 _computing_structure_refinement 'SHELXTL (Siemens, 1994)' _computing_structure_solution 'SHELXTL (Siemens, 1994)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.991 _diffrn_measured_fraction_theta_max 0.991 _diffrn_measurement_device_type 'Siemens SMART CCD' _diffrn_measurement_method '\f and \w' _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 0.0751 _diffrn_reflns_av_sigmaI/netI 0.0650 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_number 3021 _diffrn_reflns_theta_full 25.03 _diffrn_reflns_theta_max 25.03 _diffrn_reflns_theta_min 2.27 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 1.931 _exptl_absorpt_correction_T_max 0.824 _exptl_absorpt_correction_T_min 0.695 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)' _exptl_crystal_colour green _exptl_crystal_density_diffrn 1.780 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 552 _exptl_crystal_size_max .22 _exptl_crystal_size_mid .14 _exptl_crystal_size_min .10 _refine_diff_density_max 0.489 _refine_diff_density_min -0.672 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 89 _refine_ls_number_reflns 950 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.040 _refine_ls_R_factor_all 0.0909 _refine_ls_R_factor_gt 0.0559 _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^)+(0.0554P)^2^+5.62P] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1195 _refine_ls_wR_factor_ref 0.1378 _reflns_number_gt 701 _reflns_number_total 950 _reflns_threshold_expression I>2\s(I) _cod_data_source_file ww6072.cif _cod_data_source_block I _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic' 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 1527 2010-12-29 10:47:43Z saulius The following automatic conversions were performed: '_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic' 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_database_code 2202233 _cod_database_fobs_code 2202233 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' 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 Ni 0.21377(6) 0.2500 0.76154(14) 0.0199(4) Uani d S 1 . . Ni OW 0.2997(3) 0.2500 0.5693(8) 0.0251(15) Uani d S 1 . . O N 0.1227(4) 0.2500 0.9358(9) 0.0241(17) Uani d S 1 . . N C1 0.1293(5) 0.2500 1.1162(12) 0.030(2) Uani d S 1 . . C H1A 0.1769 0.2500 1.1657 0.036 Uiso calc SR 1 . . H C5 0.0530(5) 0.2500 0.8700(13) 0.033(2) Uani d S 1 . . C H5A 0.0467 0.2500 0.7454 0.039 Uiso calc SR 1 . . H C3 -0.0014(6) 0.2500 1.1621(14) 0.043(3) Uani d S 1 . . C H3A -0.0428 0.2500 1.2376 0.052 Uiso calc SR 1 . . H C2 0.0691(5) 0.2500 1.2323(13) 0.034(2) Uani d S 1 . . C H2A 0.0764 0.2500 1.3565 0.041 Uiso calc SR 1 . . H C4 -0.0099(6) 0.2500 0.9770(14) 0.044(3) Uani d S 1 . . C H4A -0.0571 0.2500 0.9253 0.053 Uiso calc SR 1 . . H HWA 0.289(4) 0.332(9) 0.503(9) 0.06(3) Uiso d . 1 . . H O2 0.3425(2) 0.5621(6) 1.1137(6) 0.0285(10) Uani d . 1 . . O C6 0.3246(3) 0.4544(8) 0.9931(8) 0.0192(13) Uani d . 1 . . C C7 0.3873(3) 0.3375(8) 0.9326(7) 0.0229(13) Uani d . 1 . . C H7A 0.4302 0.3931 0.8912 0.028 Uiso calc R 1 . . H O1 0.2609(2) 0.4447(6) 0.9216(6) 0.0274(10) Uani d . 1 . . O 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 Ni 0.0159(6) 0.0217(5) 0.0220(6) 0.000 0.0001(5) 0.000 OW 0.020(3) 0.031(4) 0.024(3) 0.000 0.001(3) 0.000 N 0.026(4) 0.022(4) 0.024(4) 0.000 0.005(3) 0.000 C1 0.025(5) 0.043(6) 0.022(5) 0.000 -0.007(4) 0.000 C5 0.022(5) 0.053(6) 0.022(5) 0.000 -0.004(4) 0.000 C3 0.035(6) 0.056(7) 0.038(6) 0.000 0.014(5) 0.000 C2 0.043(5) 0.039(5) 0.021(5) 0.000 -0.006(5) 0.000 C4 0.024(5) 0.073(8) 0.035(6) 0.000 0.001(5) 0.000 O2 0.024(2) 0.028(2) 0.034(2) 0.003(2) -0.0040(19) -0.011(2) C6 0.019(3) 0.017(3) 0.021(3) -0.006(2) 0.001(3) -0.001(3) C7 0.017(3) 0.028(3) 0.024(3) -0.006(3) 0.006(2) 0.001(3) O1 0.019(2) 0.024(2) 0.039(3) 0.0002(19) -0.0032(19) -0.012(2) 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_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O2 Ni O2 8_655 2_564 87.3(2) yes O2 Ni O1 8_655 . 174.60(16) yes O2 Ni O1 2_564 . 90.78(17) yes O2 Ni O1 8_655 7_565 90.78(17) no O2 Ni O1 2_564 7_565 174.60(16) no O1 Ni O1 . 7_565 90.7(2) yes O2 Ni N 8_655 . 86.83(19) yes O2 Ni N 2_564 . 86.83(19) no O1 Ni N . . 88.02(18) yes O1 Ni N 7_565 . 88.02(18) no O2 Ni OW 8_655 . 89.99(17) yes O2 Ni OW 2_564 . 89.99(17) no O1 Ni OW . . 95.06(17) yes O1 Ni OW 7_565 . 95.06(17) no N Ni OW . . 175.6(3) yes Ni OW HWA . . 103(5) no C1 N C5 . . 116.3(8) no C1 N Ni . . 123.3(6) no C5 N Ni . . 120.4(6) no N C1 C2 . . 123.5(9) no N C1 H1A . . 118.2 no C2 C1 H1A . . 118.2 no N C5 C4 . . 123.7(9) no N C5 H5A . . 118.2 no C4 C5 H5A . . 118.2 no C2 C3 C4 . . 118.6(10) no C2 C3 H3A . . 120.7 no C4 C3 H3A . . 120.7 no C3 C2 C1 . . 119.1(9) no C3 C2 H2A . . 120.4 no C1 C2 H2A . . 120.4 no C5 C4 C3 . . 118.8(10) no C5 C4 H4A . . 120.6 no C3 C4 H4A . . 120.6 no C6 O2 Ni . 2_565 134.7(4) no O2 C6 O1 . . 124.7(5) no O2 C6 C7 . . 113.9(5) no O1 C6 C7 . . 121.3(5) no C7 C7 C6 7_565 . 126.1(3) no C7 C7 H7A 7_565 . 116.9 no C6 C7 H7A . . 116.9 no C6 O1 Ni . . 130.6(4) 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 Ni O2 8_655 2.060(4) yes Ni O2 2_564 2.060(4) yes Ni O1 . 2.072(4) yes Ni O1 7_565 2.072(4) yes Ni N . 2.083(7) yes Ni OW . 2.100(6) yes OW HWA . 0.82(7) no N C1 . 1.342(11) no N C5 . 1.344(11) no C1 C2 . 1.381(13) no C1 H1A . 0.9300 no C5 C4 . 1.379(13) no C5 H5A . 0.9300 no C3 C2 . 1.369(14) no C3 C4 . 1.380(14) no C3 H3A . 0.9300 no C2 H2A . 0.9300 no C4 H4A . 0.9300 no O2 C6 . 1.252(7) no O2 Ni 2_565 2.060(4) no C6 O1 . 1.263(6) no C6 C7 . 1.500(8) no C7 C7 7_565 1.325(12) no C7 H7A . 0.9300 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 _geom_hbond_publ_flag OW HWA O1 2_564 0.82(7) 2.01(7) 2.780(5) 159(?) yes C4 H4A OW 6_557 0.93 2.57 3.435(12) 155 yes