#------------------------------------------------------------------------------ #$Date: 2016-02-20 03:06:23 +0000 (Sat, 20 Feb 2016) $ #$Revision: 176774 $ #$URL: svn://www.crystallography.net/cod/cif/2/20/33/2203380.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_2203380 loop_ _publ_author_name 'Qing-Qing Kang' 'La-Sheng Long' 'Rong-Bin Huang' 'Lan-Sun Zheng' _publ_section_title ; Polymeric bis(glycolato)nickel(II) ; _journal_issue 4 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first m406 _journal_page_last m407 _journal_paper_doi 10.1107/S1600536804005744 _journal_volume 60 _journal_year 2004 _chemical_formula_iupac '[Ni (C2 H3 O3)2]' _chemical_formula_moiety 'C4 H6 Ni O6' _chemical_formula_sum 'C4 H6 Ni O6' _chemical_formula_weight 208.80 _chemical_name_common 'Polymeric bis(glycolato)nickel(II)' _chemical_name_systematic ; poly[nickel(II)-bis(\a-hydroxyacetato-\k^3^O^1^,O^2^:O^1'^)] ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _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 105.443(2) _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 5.1304(7) _cell_length_b 7.6367(11) _cell_length_c 8.6076(12) _cell_measurement_reflns_used 1462 _cell_measurement_temperature 298(2) _cell_measurement_theta_max 27.850 _cell_measurement_theta_min 3.626 _cell_volume 325.06(8) _computing_cell_refinement 'SAINT (Bruker 2001)' _computing_data_collection 'SMART (Bruker, 2001)' _computing_data_reduction SAINT _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material SHELXL97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 298(2) _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.935 _diffrn_measurement_device_type 'Smart Apex 2000' _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 0.0153 _diffrn_reflns_av_sigmaI/netI 0.0196 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_number 1829 _diffrn_reflns_theta_full 25.00 _diffrn_reflns_theta_max 28.08 _diffrn_reflns_theta_min 3.63 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 3 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 2.962 _exptl_absorpt_correction_T_max 0.7176 _exptl_absorpt_correction_T_min 0.3990 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)' _exptl_crystal_colour green _exptl_crystal_density_diffrn 2.133 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 212 _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.12 _refine_diff_density_max 0.319 _refine_diff_density_min -0.357 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.113 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 52 _refine_ls_number_reflns 736 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.113 _refine_ls_R_factor_all 0.0218 _refine_ls_R_factor_gt 0.0209 _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^)+(0.0283P)^2^+0.1923P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0555 _refine_ls_wR_factor_ref 0.0560 _reflns_number_gt 702 _reflns_number_total 736 _reflns_threshold_expression I>2\s(I) _cod_data_source_file bt6422.cif _cod_data_source_block I _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 2203380 _cod_database_fobs_code 2203380 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -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_type_symbol Ni1 0.5000 1.0000 1.0000 0.01406(12) Uani d S 1 Ni O1 0.2283(2) 0.80972(17) 1.01304(14) 0.0201(3) Uani d . 1 O H1C 0.0986 0.8216 1.0509 0.030 Uiso calc R 1 H O2 0.5250(2) 0.84946(17) 0.81302(14) 0.0193(3) Uani d . 1 O O3 0.3199(2) 0.64427(18) 0.64455(15) 0.0214(3) Uani d . 1 O C1 0.1521(4) 0.7049(3) 0.8725(2) 0.0293(4) Uani d . 1 C H1A -0.0303 0.7345 0.8114 0.035 Uiso calc R 1 H H1B 0.1550 0.5823 0.9023 0.035 Uiso calc R 1 H C2 0.3465(3) 0.7358(2) 0.77028(19) 0.0167(3) Uani d . 1 C 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 Ni1 0.01379(19) 0.01679(19) 0.01220(18) -0.00018(10) 0.00450(12) -0.00083(10) O1 0.0198(6) 0.0262(7) 0.0176(6) -0.0055(5) 0.0106(5) -0.0052(5) O2 0.0190(6) 0.0226(6) 0.0187(6) -0.0040(5) 0.0090(5) -0.0043(5) O3 0.0190(6) 0.0286(7) 0.0185(6) -0.0059(5) 0.0081(5) -0.0083(5) C1 0.0285(10) 0.0381(11) 0.0270(10) -0.0155(8) 0.0176(8) -0.0147(8) C2 0.0155(8) 0.0206(8) 0.0145(8) 0.0014(6) 0.0050(6) 0.0005(6) 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' 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 Ni1 O2 . 3_677 180.0000(10) no O2 Ni1 O1 . 3_677 99.99(5) yes O2 Ni1 O1 3_677 3_677 80.01(5) no O2 Ni1 O1 . . 80.01(5) yes O2 Ni1 O1 3_677 . 99.99(5) no O1 Ni1 O1 3_677 . 180.0 no O2 Ni1 O3 . 2_556 91.84(5) no O2 Ni1 O3 3_677 2_556 88.16(5) no O1 Ni1 O3 3_677 2_556 91.81(5) no O1 Ni1 O3 . 2_556 88.19(5) yes O2 Ni1 O3 . 4_676 88.16(5) no O2 Ni1 O3 3_677 4_676 91.84(5) no O1 Ni1 O3 3_677 4_676 88.19(5) no O1 Ni1 O3 . 4_676 91.81(5) no O3 Ni1 O3 2_556 4_676 180.0000(10) no C1 O1 Ni1 . . 113.16(11) no C2 O2 Ni1 . . 115.92(10) no C2 O3 Ni1 . 2_546 133.60(11) no O1 C1 C2 . . 109.50(15) no O1 C1 H1A . . 109.8 ? C2 C1 H1A . . 109.8 ? O1 C1 H1B . . 109.8 ? C2 C1 H1B . . 109.8 ? H1A C1 H1B . . 108.2 ? O2 C2 O3 . . 122.82(15) no O2 C2 C1 . . 118.93(15) no O3 C2 C1 . . 118.25(15) 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 Ni1 O2 . 2.0095(12) yes Ni1 O2 3_677 2.0095(12) no Ni1 O1 3_677 2.0374(12) no Ni1 O1 . 2.0374(12) yes Ni1 O3 2_556 2.0899(12) yes Ni1 O3 4_676 2.0899(12) no O1 C1 . 1.416(2) no O1 H1C . 0.8200 ? O2 C2 . 1.244(2) no O3 C2 . 1.265(2) no O3 Ni1 2_546 2.0899(12) no C1 C2 . 1.514(2) no C1 H1A . 0.9700 ? C1 H1B . 0.9700 ? 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 O1 H1C O3 4_576 0.82 1.84 2.6568(17) 176.8