#------------------------------------------------------------------------------ #$Date: 2013-08-29 16:37:19 +0100 (Thu, 29 Aug 2013) $ #$Revision: 88064 $ #$URL: svn://www.crystallography.net/cod/cif/2/20/42/2204271.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_2204271 loop_ _publ_author_name 'Katharina Stenzel' 'Michel Fleck' _publ_section_title ; Poly[[[diaquacobalt(II)]-di-\m-glycine] dichloride] ; _journal_issue 10 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first m1470 _journal_page_last m1472 _journal_volume 60 _journal_year 2004 _chemical_formula_iupac '[Co (C2 H5 N O2)2 (H2 O)2] 2Cl' _chemical_formula_moiety 'Co, 2(C2 H5 N O2), 2Cl, 2(H2 O)' _chemical_formula_sum 'C4 H14 Cl2 Co N2 O6' _chemical_formula_weight 316.00 _chemical_name_common 'Diglycine cobalt dichloride dihydrate' _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 90.00 _cell_angle_beta 91.55(3) _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 10.568(2) _cell_length_b 5.9880(10) _cell_length_c 8.844(2) _cell_measurement_reflns_used 1496 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 28.283 _cell_measurement_theta_min 2.037 _cell_volume 559.45(19) _computing_cell_refinement 'HKL SCALEPACK (Otwinowski & Minor 1997)' _computing_data_collection 'COLLECT (Nonius BV, 2003)' _computing_data_reduction 'HKL DENZO (Otwinowski & Minor 1997) and SCALEPACK' _computing_molecular_graphics 'DIAMOND (Bergerhoff et al., 1997) and ORTEP3 (Farrugia, 1997)' _computing_publication_material SHELXL97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 293(2) _diffrn_detector_area_resol_mean 9 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type 'Nonius Kappa CCD diffractometer' _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 0.0120 _diffrn_reflns_av_sigmaI/netI 0.0193 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_number 2525 _diffrn_reflns_theta_full 28.28 _diffrn_reflns_theta_max 28.28 _diffrn_reflns_theta_min 3.86 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 2.022 _exptl_absorpt_correction_T_max 0.8234 _exptl_absorpt_correction_T_min 0.5822 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ' (Program?; Otwinowski & Minor, 1997)' _exptl_crystal_colour pink _exptl_crystal_density_diffrn 1.876 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' _exptl_crystal_description fragment _exptl_crystal_F_000 322 _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _refine_diff_density_max 0.572 _refine_diff_density_min -0.496 _refine_ls_extinction_coef 0.033(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 99 _refine_ls_number_reflns 1376 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.076 _refine_ls_R_factor_all 0.0244 _refine_ls_R_factor_gt 0.0219 _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^)+(0.0275P)^2^+0.3111P] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0561 _refine_ls_wR_factor_ref 0.0579 _reflns_number_gt 1274 _reflns_number_total 1376 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file bt6514.cif _[local]_cod_data_source_block I _[local]_cod_cif_authors_sg_H-M 'P 21/c' _cod_depositor_comments ; The following automatic conversions were performed: '_chemical_melting_point' value 'not determined' was changed to '?' - the value is undefined or not given. Automatic conversion script Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana The following automatic conversions were performed: '_chemical_melting_point' value 'not determined' was changed to '?' - the value is undefined or not given. Automatic conversion script Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana ; _cod_database_code 2204271 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -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 Co 0.5000 0.0000 0.5000 0.01638(12) Uani d S 1 Co O1 0.65086(10) 0.36581(19) 0.88140(11) 0.0229(2) Uani d . 1 O O2 0.55048(10) 0.1680(2) 0.70159(12) 0.0286(3) Uani d . 1 O C1 0.64769(13) 0.2505(2) 0.76336(15) 0.0187(3) Uani d . 1 C C2 0.77360(15) 0.2165(3) 0.68777(18) 0.0265(3) Uani d . 1 C H1C 0.782(2) 0.074(5) 0.657(3) 0.042(6) Uiso d . 1 H H2C 0.772(2) 0.311(4) 0.603(3) 0.039(6) Uiso d . 1 H N 0.88136(13) 0.2833(3) 0.78734(17) 0.0267(3) Uani d . 1 N H1N 0.865(2) 0.419(5) 0.827(3) 0.044(6) Uiso d . 1 H H2N 0.952(2) 0.298(4) 0.730(3) 0.043(6) Uiso d . 1 H H3N 0.900(2) 0.179(5) 0.857(3) 0.052(7) Uiso d . 1 H O1W 0.38810(13) 0.2699(3) 0.43828(17) 0.0364(3) Uani d . 1 O H1W 0.316(3) 0.285(5) 0.456(3) 0.052(7) Uiso d . 1 H H2W 0.406(3) 0.316(5) 0.369(3) 0.056(9) Uiso d . 1 H Cl 1.11073(4) 0.28327(8) 0.55838(5) 0.03446(14) Uani d . 1 Cl 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 Co 0.01380(16) 0.02165(18) 0.01379(16) 0.00019(9) 0.00210(10) 0.00073(9) O1 0.0167(5) 0.0321(6) 0.0201(5) 0.0005(4) 0.0027(4) -0.0086(4) O2 0.0205(5) 0.0431(7) 0.0222(5) -0.0062(5) 0.0026(4) -0.0115(5) C1 0.0185(6) 0.0215(7) 0.0162(6) 0.0007(5) 0.0030(5) 0.0001(5) C2 0.0200(7) 0.0368(9) 0.0228(7) 0.0011(6) 0.0043(6) -0.0104(7) N 0.0174(6) 0.0350(8) 0.0280(7) -0.0002(5) 0.0041(5) -0.0061(6) O1W 0.0269(7) 0.0416(8) 0.0415(8) 0.0124(6) 0.0140(6) 0.0178(6) Cl 0.0270(2) 0.0331(2) 0.0438(3) 0.00645(16) 0.01172(17) 0.00402(17) 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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 O1W Co O1W . 3_656 180.00(8) O1W Co O1 . 4_565 90.32(5) O1W Co O1 3_656 4_565 89.68(5) O1W Co O1 . 2_646 89.68(5) O1W Co O1 3_656 2_646 90.32(5) O1 Co O1 4_565 2_646 180.00(4) O1W Co O2 . 3_656 91.14(6) O1W Co O2 3_656 3_656 88.86(6) O1 Co O2 4_565 3_656 86.44(5) O1 Co O2 2_646 3_656 93.56(5) O1W Co O2 . . 88.86(6) O1W Co O2 3_656 . 91.14(6) O1 Co O2 4_565 . 93.56(5) O1 Co O2 2_646 . 86.44(5) O2 Co O2 3_656 . 180.0 C1 O1 Co . 2_656 128.79(10) C1 O2 Co . . 138.16(10) O1 C1 O2 . . 125.80(13) O1 C1 C2 . . 115.92(13) O2 C1 C2 . . 118.25(13) N C2 C1 . . 111.85(12) N C2 H1C . . 110.4(15) C1 C2 H1C . . 110.9(15) N C2 H2C . . 108.0(14) C1 C2 H2C . . 106.0(14) H1C C2 H2C . . 109(2) C2 N H1N . . 109.0(15) C2 N H2N . . 108.7(14) H1N N H2N . . 107(2) C2 N H3N . . 111.7(17) H1N N H3N . . 114(2) H2N N H3N . . 107(2) Co O1W H1W . . 126(2) Co O1W H2W . . 112(2) H1W O1W H2W . . 115(3) 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 Co O1W . 2.0673(14) y Co O1W 3_656 2.0673(14) y Co O1 4_565 2.0924(11) y Co O1 2_646 2.0924(11) y Co O2 3_656 2.1031(11) y Co O2 . 2.1031(11) y O1 C1 . 1.2513(17) ? O1 Co 2_656 2.0924(11) ? O2 C1 . 1.2520(18) ? C1 C2 . 1.519(2) ? C2 N . 1.476(2) ? C2 H1C . 0.90(3) ? C2 H2C . 0.94(2) ? N H1N . 0.90(3) ? N H2N . 0.91(3) ? N H3N . 0.89(3) ? O1W H1W . 0.79(3) ? O1W H2W . 0.70(3) ? 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 N H1N Cl 2_756 0.90(3) 2.41(3) 3.2905(17) 163(2) N H2N Cl . 0.91(3) 2.30(3) 3.2002(17) 169(2) N H1N Cl 2_756 0.90(3) 2.41(3) 3.2905(17) 163(2) O1W H1W Cl 1_455 0.79(3) 2.38(3) 3.1457(17) 167(3) O1W H2W O2 4_565 0.70(3) 2.16(3) 2.768(2) 146(3) _cod_database_fobs_code 2204271