#------------------------------------------------------------------------------ #$Date: 2016-02-14 04:40:26 +0000 (Sun, 14 Feb 2016) $ #$Revision: 176432 $ #$URL: svn://www.crystallography.net/cod/cif/2/20/22/2202269.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_2202269 loop_ _publ_author_name 'Carballo, Rosa ' 'Casti\~neiras, Alfonso' 'Covelo, Berta' 'Garc\'ia-Mart\'inez, Emilia' 'V\'azquez-L\'opez, Ezequiel M.' _publ_section_title ; (OC-6-32)-Diaquabis(glycolato)cobalt(II) ; _journal_issue 8 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first m588 _journal_page_last m590 _journal_paper_doi 10.1107/S1600536803015083 _journal_volume 59 _journal_year 2003 _chemical_formula_iupac '[Co (C2 H3 O3)2 (H2 O1)2]' _chemical_formula_moiety 'C4 H10 Co O8' _chemical_formula_sum 'C4 H10 Co O8' _chemical_formula_weight 245.05 _chemical_name_systematic ? _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 mixed _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 91.4537(14) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 11.5388(9) _cell_length_b 5.8330(4) _cell_length_c 12.4477(9) _cell_measurement_reflns_used 2202 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 28.01 _cell_measurement_theta_min 1.77 _cell_volume 837.53(11) _computing_cell_refinement 'SMART (Bruker, 1998)' _computing_data_collection 'SMART (Bruker, 1998)' _computing_data_reduction 'SAINT (Bruker, 1998)' _computing_molecular_graphics ; SHELXTL (Bruker, 2000) and SCHAKAL (Keller, 1999) ; _computing_publication_material 'SHELXTL (Bruker, 2000)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.983 _diffrn_measured_fraction_theta_max 0.968 _diffrn_measurement_device_type 'CCD area detector' _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 0.0230 _diffrn_reflns_av_sigmaI/netI 0.0326 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 5031 _diffrn_reflns_theta_full 26.50 _diffrn_reflns_theta_max 28.01 _diffrn_reflns_theta_min 1.77 _diffrn_standards_decay_% 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 2.064 _exptl_absorpt_correction_T_max 0.797 _exptl_absorpt_correction_T_min 0.611 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_crystal_colour pink _exptl_crystal_density_diffrn 1.943 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 500 _exptl_crystal_size_max .36 _exptl_crystal_size_mid .13 _exptl_crystal_size_min .11 _refine_diff_density_max 0.280 _refine_diff_density_min -0.251 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.944 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 142 _refine_ls_number_reflns 1964 _refine_ls_number_restraints 2 _refine_ls_restrained_S_all 0.950 _refine_ls_R_factor_all 0.0335 _refine_ls_R_factor_gt 0.0235 _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^)+(0.0247P)^2^+0.4285P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0505 _refine_ls_wR_factor_ref 0.0525 _reflns_number_gt 1602 _reflns_number_total 1964 _reflns_threshold_expression I>2\s(I) _cod_data_source_file ac6049.cif _cod_data_source_block I _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' 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 'Monoclinic' changed to 'monoclinic' 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_sg_symbol_Hall -P2ybc _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 2202269 _cod_database_fobs_code 2202269 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_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol Co 0.25965(2) 0.13328(4) 0.160112(18) 0.02436(8) Uani d . 1 . . Co O1 0.41268(13) 0.2949(3) 0.19709(14) 0.0380(4) Uani d . 1 . . O O2 0.22921(13) 0.0993(3) 0.32407(11) 0.0337(3) Uani d D 1 . . O O11 0.30574(11) 0.1296(2) -0.00242(9) 0.0320(3) Uani d . 1 . . O O12 0.40474(12) -0.0613(2) -0.12429(10) 0.0380(3) Uani d . 1 . . O O13 0.32193(13) -0.1998(2) 0.14107(10) 0.0328(3) Uani d D 1 . . O C11 0.35881(16) -0.0448(3) -0.03494(14) 0.0271(4) Uani d . 1 . . C C12 0.36884(17) -0.2502(3) 0.03888(14) 0.0306(4) Uani d . 1 . . C H12A 0.3276 -0.3789 0.0068 0.037 Uiso calc R 1 . . H H12B 0.4497 -0.2929 0.0481 0.037 Uiso calc R 1 . . H O21 0.16890(11) 0.4379(2) 0.14399(10) 0.0319(3) Uani d . 1 . . O O22 -0.00246(11) 0.60591(19) 0.12195(9) 0.0270(3) Uani d . 1 . . O O23 0.08599(12) 0.0252(2) 0.13200(11) 0.0345(3) Uani d . 1 . . O C21 0.06093(16) 0.4321(3) 0.12972(13) 0.0226(4) Uani d . 1 . . C C22 0.00151(15) 0.2011(3) 0.12315(14) 0.0245(4) Uani d . 1 . . C H22A -0.0531 0.1868 0.1807 0.029 Uiso calc R 1 . . H H22B -0.0410 0.1874 0.0552 0.029 Uiso calc R 1 . . H H11 0.477(2) 0.236(4) 0.1780(18) 0.060(8) Uiso d . 1 . . H H12 0.418(2) 0.360(4) 0.254(2) 0.060(8) Uiso d . 1 . . H H23 0.053(2) -0.111(4) 0.1269(17) 0.051(7) Uiso d . 1 . . H H13 0.278(2) -0.305(4) 0.161(2) 0.087(10) Uiso d D 1 . . H H21 0.1576(19) 0.091(4) 0.3427(16) 0.042(6) Uiso d . 1 . . H H22 0.260(2) 0.180(4) 0.3706(17) 0.065(8) Uiso d D 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 Co 0.02788(14) 0.01814(13) 0.02727(14) 0.00136(11) 0.00496(9) -0.00130(10) O1 0.0289(8) 0.0400(9) 0.0451(9) -0.0001(7) 0.0049(7) -0.0144(7) O2 0.0316(8) 0.0409(9) 0.0287(7) -0.0063(7) 0.0046(6) -0.0055(6) O11 0.0419(8) 0.0267(7) 0.0278(7) 0.0097(6) 0.0063(6) 0.0037(6) O12 0.0448(9) 0.0412(8) 0.0288(7) 0.0091(6) 0.0142(6) 0.0031(6) O13 0.0493(9) 0.0200(7) 0.0297(7) 0.0017(6) 0.0141(6) 0.0022(5) C11 0.0262(10) 0.0276(10) 0.0274(10) -0.0003(8) 0.0014(8) 0.0002(8) C12 0.0392(11) 0.0227(10) 0.0304(10) 0.0018(8) 0.0103(8) -0.0017(8) O21 0.0277(7) 0.0172(7) 0.0510(8) -0.0001(5) 0.0049(6) -0.0005(6) O22 0.0311(7) 0.0179(6) 0.0322(7) 0.0030(5) 0.0035(5) 0.0007(5) O23 0.0339(8) 0.0159(7) 0.0536(9) -0.0010(6) -0.0020(6) -0.0039(6) C21 0.0304(10) 0.0208(9) 0.0169(8) -0.0002(7) 0.0048(7) 0.0005(6) C22 0.0302(10) 0.0202(9) 0.0232(9) -0.0003(7) 0.0004(7) 0.0015(7) 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' Co Co 0.3494 0.9721 '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_publ_flag O1 Co O21 93.32(6) y O1 Co O13 99.04(6) y O21 Co O13 164.37(5) y O1 Co O2 89.40(6) y O21 Co O2 94.53(5) y O13 Co O2 95.14(5) y O1 Co O11 89.04(6) y O21 Co O11 93.16(5) y O13 Co O11 77.60(5) y O2 Co O11 172.23(5) y O1 Co O23 168.92(6) y O21 Co O23 76.45(5) y O13 Co O23 91.78(6) y O2 Co O23 87.21(6) y O11 Co O23 95.68(5) y Co O1 H11 120.4(16) ? Co O1 H12 117.8(18) ? H11 O1 H12 112(2) ? Co O2 H21 116.9(14) ? Co O2 H22 123.6(18) ? H21 O2 H22 104(2) ? C11 O11 Co 116.99(11) ? C12 O13 Co 115.65(11) ? C12 O13 H13 111.1(18) ? Co O13 H13 115.9(19) ? O12 C11 O11 124.72(17) ? O12 C11 C12 116.93(16) ? O11 C11 C12 118.35(15) ? O13 C12 C11 110.73(14) ? O13 C12 H12A 109.5 ? C11 C12 H12A 109.5 ? O13 C12 H12B 109.5 ? C11 C12 H12B 109.5 ? H12A C12 H12B 108.1 ? C21 O21 Co 119.26(11) ? C22 O23 Co 116.25(11) ? C22 O23 H23 110.4(15) ? Co O23 H23 133.3(15) ? O22 C21 O21 124.41(16) ? O22 C21 C22 116.98(15) ? O21 C21 C22 118.61(15) ? O23 C22 C21 109.31(14) ? O23 C22 H22A 109.8 ? C21 C22 H22A 109.8 ? O23 C22 H22B 109.8 ? C21 C22 H22B 109.8 ? H22A C22 H22B 108.3 ? 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 O1 . 2.0439(15) y Co O21 . 2.0696(12) y Co O13 . 2.0870(13) y Co O2 . 2.0891(14) y Co O11 . 2.1050(12) y Co O23 . 2.1213(14) y O1 H11 . 0.86(3) ? O1 H12 . 0.81(2) ? O2 H21 . 0.86(2) ? O2 H22 . 0.822(16) ? O11 C11 . 1.260(2) ? O12 C11 . 1.248(2) ? O13 C12 . 1.426(2) ? O13 H13 . 0.840(17) ? C11 C12 . 1.512(2) ? C12 H12A . 0.9700 ? C12 H12B . 0.9700 ? O21 C21 . 1.254(2) ? O22 C21 . 1.253(2) ? O23 C22 . 1.418(2) ? O23 H23 . 0.88(2) ? C21 C22 . 1.513(2) ? C22 H22A . 0.9700 ? C22 H22B . 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 H11 O12 3_655 0.86(3) 1.84(3) 2.686(2) 167(2) O1 H12 O12 4_566 0.81(2) 1.92(3) 2.716(2) 166(2) O23 H23 O22 1_545 0.88(2) 1.77(2) 2.6517(18) 175(2) O13 H13 O21 1_545 0.840(17) 1.964(19) 2.7547(19) 156(3) O2 H21 O22 2_545 0.86(2) 1.86(2) 2.7180(19) 174(2) O2 H22 O11 4_566 0.822(16) 1.991(17) 2.8016(18) 169(2)