#------------------------------------------------------------------------------ #$Date: 2011-09-10 06:16:28 +0300 (Sat, 10 Sep 2011) $ #$Revision: 25271 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/2015254.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_2015254 loop_ _publ_author_name 'Djeghri, Assia' 'Balegroune, Fadila' 'Guehria Laidoudi, Achoura' 'Toupet, Loic' _publ_section_title ; Poly[tetraaquadi-\m~3~-malonato-cobalt(II)calcium(II)] ; _journal_coeditor_code HJ1082 _journal_issue 4 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first m126 _journal_page_last m128 _journal_volume 62 _journal_year 2006 _chemical_formula_iupac '[Ca Co (C3 H2 O4)2 (H2 O)4]' _chemical_formula_moiety 'C6 H12 Ca Co O12' _chemical_formula_sum 'C6 H12 Ca Co O12' _chemical_formula_weight 375.17 _chemical_name_systematic ; Poly[tetraaquadi-\m~3~-malonato-cobalt(II)calcium(II)] ; _space_group_IT_number 15 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 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 122.94(2) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 13.874(2) _cell_length_b 7.5310(10) _cell_length_c 13.615(2) _cell_measurement_reflns_used 25 _cell_measurement_temperature 298 _cell_measurement_theta_max 13.64 _cell_measurement_theta_min 5.41 _cell_volume 1193.9(4) _computing_cell_refinement 'CAD-4 EXPRESS' _computing_data_collection 'CAD-4 EXPRESS (Enraf--Nonius, 1993)' _computing_data_reduction 'XCAD4 (Harms & Wocadlo, 1996)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' _computing_publication_material SHELXL97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1990)' _diffrn_ambient_temperature 298 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'Enraf--Nonius CAD-4' _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 0.71073 _diffrn_reflns_av_R_equivalents 0.0069 _diffrn_reflns_av_sigmaI/netI 0.0155 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 1353 _diffrn_reflns_theta_full 26.97 _diffrn_reflns_theta_max 26.97 _diffrn_reflns_theta_min 3.19 _diffrn_standards_decay_% 0.0 _diffrn_standards_interval_time 60 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 1.932 _exptl_absorpt_correction_T_max .768 _exptl_absorpt_correction_T_min .660 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North et al., 1968)' _exptl_crystal_colour pink _exptl_crystal_density_diffrn 2.087 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 764 _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.14 _refine_diff_density_max 0.284 _refine_diff_density_min -0.251 _refine_ls_extinction_coef 0.0020(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL97 _refine_ls_goodness_of_fit_ref 1.111 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 110 _refine_ls_number_reflns 1300 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.111 _refine_ls_R_factor_all 0.0244 _refine_ls_R_factor_gt 0.0195 _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^)+(0.0246P)^2^+0.8504P] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0486 _refine_ls_wR_factor_ref 0.0500 _reflns_number_gt 1177 _reflns_number_total 1300 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file hj1082.cif _[local]_cod_data_source_block I _[local]_cod_cif_authors_sg_H-M 'C 2/c' _cod_database_code 2015254 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' loop_ _atom_site_type_symbol _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 Ca Ca 0.5000 -0.12268(6) 0.2500 0.01694(12) Uani d S 1 Co Co 0.5000 0.5000 0.5000 0.01770(11) Uani d S 1 O O1 0.37589(10) 0.10287(15) 0.24175(10) 0.0252(3) Uani d . 1 O O2 0.45750(10) 0.26466(15) 0.40366(10) 0.0255(3) Uani d . 1 O O3 0.43766(10) 0.63445(15) 0.34394(9) 0.0246(3) Uani d . 1 O O4 0.33859(11) 0.67075(16) 0.15464(10) 0.0286(3) Uani d . 1 O O5 0.33756(11) 0.5107(2) 0.47682(13) 0.0326(3) Uani d . 1 O O6 0.40284(12) -0.03139(19) 0.04940(11) 0.0283(3) Uani d . 1 C C2 0.31086(13) 0.3977(2) 0.22178(13) 0.0216(3) Uani d . 1 H H2A 0.2761 0.3682 0.1415 0.026 Uiso calc R 1 H H2B 0.2511 0.4070 0.2359 0.026 Uiso calc R 1 C C1 0.38792(12) 0.2455(2) 0.29424(13) 0.0177(3) Uani d . 1 C C3 0.36624(13) 0.5778(2) 0.24204(13) 0.0174(3) Uani d . 1 H H5A 0.283(2) 0.544(3) 0.422(2) 0.051(8) Uiso d . 1 H H5B 0.329(2) 0.459(3) 0.521(2) 0.046(7) Uiso d . 1 H H6A 0.435(2) 0.062(4) 0.047(2) 0.055(8) Uiso d . 1 H H6B 0.399(2) -0.091(4) 0.003(2) 0.052(8) Uiso d . 1 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 Ca 0.0171(2) 0.0144(2) 0.0163(2) 0.000 0.00716(17) 0.000 Co 0.01973(16) 0.01414(16) 0.01387(15) -0.00079(11) 0.00566(12) -0.00127(11) O1 0.0235(6) 0.0196(6) 0.0247(6) 0.0020(5) 0.0079(5) -0.0070(5) O2 0.0305(6) 0.0165(5) 0.0183(5) 0.0022(5) 0.0060(5) -0.0015(4) O3 0.0278(6) 0.0181(5) 0.0182(5) -0.0051(5) 0.0061(5) 0.0001(4) O4 0.0382(7) 0.0230(6) 0.0196(6) -0.0044(5) 0.0125(5) 0.0027(5) O5 0.0218(6) 0.0488(9) 0.0243(7) 0.0033(6) 0.0106(6) 0.0093(6) O6 0.0322(7) 0.0254(7) 0.0211(6) -0.0042(5) 0.0105(5) -0.0018(5) C2 0.0194(7) 0.0165(7) 0.0192(7) -0.0016(6) 0.0042(6) -0.0005(6) C1 0.0175(7) 0.0159(7) 0.0195(7) -0.0018(6) 0.0098(6) -0.0017(6) C3 0.0170(7) 0.0158(7) 0.0196(7) 0.0026(6) 0.0101(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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ca Ca 0.2262 0.3064 '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 Ca O1 2_655 . 88.80(6) yes O1 Ca O6 2_655 2_655 78.29(5) ? O1 Ca O6 . 2_655 78.05(5) ? O1 Ca O6 2_655 . 78.05(5) yes O1 Ca O6 . . 78.29(5) yes O6 Ca O6 2_655 . 146.66(7) yes O1 Ca O4 2_655 1_545 155.76(4) ? O1 Ca O4 . 1_545 89.93(4) yes O6 Ca O4 2_655 1_545 125.01(5) ? O6 Ca O4 . 1_545 77.99(5) yes O1 Ca O4 2_655 2_645 89.93(4) ? O1 Ca O4 . 2_645 155.76(4) yes O6 Ca O4 2_655 2_645 77.99(5) ? O6 Ca O4 . 2_645 125.01(5) yes O4 Ca O4 1_545 2_645 100.82(6) yes O1 Ca O3 2_655 2_645 95.65(4) ? O1 Ca O3 . 2_645 153.40(4) yes O6 Ca O3 2_655 2_645 128.54(4) ? O6 Ca O3 . 2_645 77.03(4) yes O4 Ca O3 1_545 2_645 75.38(4) yes O4 Ca O3 2_645 2_645 50.73(4) yes O1 Ca O3 2_655 1_545 153.40(4) yes O1 Ca O3 . 1_545 95.65(4) yes O6 Ca O3 2_655 1_545 77.03(4) ? O6 Ca O3 . 1_545 128.54(4) yes O4 Ca O3 1_545 1_545 50.73(4) ? O4 Ca O3 2_645 1_545 75.38(4) ? O3 Ca O3 2_645 1_545 92.00(6) yes O1 Ca C3 2_655 2_645 97.02(4) ? O1 Ca C3 . 2_645 174.17(4) ? O6 Ca C3 2_655 2_645 103.28(5) ? O6 Ca C3 . 2_645 102.64(5) ? O4 Ca C3 1_545 2_645 84.67(5) ? O4 Ca C3 2_645 2_645 25.38(4) ? O3 Ca C3 2_645 2_645 25.93(4) ? O3 Ca C3 1_545 2_645 79.23(4) ? O1 Ca C3 2_655 1_545 174.17(4) ? O1 Ca C3 . 1_545 97.02(4) ? O6 Ca C3 2_655 1_545 102.64(5) ? O6 Ca C3 . 1_545 103.28(5) ? O4 Ca C3 1_545 1_545 25.38(4) ? O4 Ca C3 2_645 1_545 84.67(5) ? O3 Ca C3 2_645 1_545 79.23(4) ? O3 Ca C3 1_545 1_545 25.93(4) ? C3 Ca C3 2_645 1_545 77.16(6) ? O1 Ca H6A 2_655 . 61.6(6) ? O1 Ca H6A . . 76.1(5) ? O6 Ca H6A 2_655 . 132.1(6) ? O6 Ca H6A . . 16.8(6) ? O4 Ca H6A 1_545 . 94.6(6) ? O4 Ca H6A 2_645 . 123.9(5) ? O3 Ca H6A 2_645 . 83.0(5) ? O3 Ca H6A 1_545 . 144.8(6) ? C3 Ca H6A 2_645 . 106.5(5) ? C3 Ca H6A 1_545 . 120.0(6) ? O3 Co O3 . 5_666 180.00(4) ? O3 Co O2 . . 87.30(5) yes O3 Co O2 5_666 . 92.70(5) yes O3 Co O2 . 5_666 92.70(5) ? O3 Co O2 5_666 5_666 87.30(5) ? O2 Co O2 . 5_666 180.0 ? O3 Co O5 . 5_666 89.32(6) yes O3 Co O5 5_666 5_666 90.68(6) ? O2 Co O5 . 5_666 88.59(5) yes O2 Co O5 5_666 5_666 91.41(5) ? O3 Co O5 . . 90.68(6) yes O3 Co O5 5_666 . 89.32(6) ? O2 Co O5 . . 91.41(5) yes O2 Co O5 5_666 . 88.59(5) ? O5 Co O5 5_666 . 180.0 ? C1 O1 Ca . . 135.95(10) yes C1 O2 Co . . 127.49(10) yes C3 O3 Co . . 127.06(10) yes C3 O3 Ca . 1_565 88.26(9) yes Co O3 Ca . 1_565 140.69(5) yes C3 O4 Ca . 1_565 97.63(10) yes Co O5 H5A . . 125.2(19) yes Co O5 H5B . . 117.8(18) yes H5A O5 H5B . . 116(3) ? Ca O6 H6A . . 107.9(17) yes Ca O6 H6B . . 121(2) yes H6A O6 H6B . . 106(3) yes C3 C2 C1 . . 116.97(13) yes C3 C2 H2A . . 108.1 ? C1 C2 H2A . . 108.1 ? C3 C2 H2B . . 108.1 ? C1 C2 H2B . . 108.1 ? H2A C2 H2B . . 107.3 ? O1 C1 O2 . . 123.31(14) yes O1 C1 C2 . . 116.83(13) yes O2 C1 C2 . . 119.81(13) yes O4 C3 O3 . . 120.61(14) yes O4 C3 C2 . . 117.91(13) yes O3 C3 C2 . . 121.47(14) yes 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 Ca O1 2_655 2.3775(12) ? Ca O1 . 2.3775(12) yes Ca O6 2_655 2.3970(14) ? Ca O6 . 2.3970(14) yes Ca O4 1_545 2.4410(13) yes Ca O4 2_645 2.4410(13) ? Ca O3 2_645 2.6329(12) ? Ca O3 1_545 2.6329(12) yes Co O3 . 2.0711(12) yes Co O3 5_666 2.0711(12) ? Co O2 . 2.0900(11) yes Co O2 5_666 2.0900(11) ? Co O5 5_666 2.1004(14) ? Co O5 . 2.1004(14) yes O1 C1 . 1.2500(18) yes O2 C1 . 1.2681(19) yes O3 C3 . 1.2623(19) yes O4 C3 . 1.2476(19) yes O4 Ca 1_565 2.4410(13) ? O5 H5A . 0.77(3) yes O5 H5B . 0.78(3) yes O6 H6A . 0.84(3) yes O6 H6B . 0.75(3) yes C2 C3 . 1.509(2) yes C2 C1 . 1.511(2) yes C2 H2A . 0.9500 ? C2 H2B . 0.9500 ? 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 O5 H5A O1 4 0.77(3) 2.16(3) 2.920(2) 173(3) O5 H5B O4 6_566 0.78(3) 2.00(3) 2.773(2) 169(3) O6 H6A O2 2_655 0.84(3) 1.98(3) 2.7905(18) 161(2) O6 H6B O2 6 0.75(3) 2.33(3) 3.0388(19) 159(3) loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_4 _geom_torsion O1 Ca O1 C1 2_655 . -44.71(14) O6 Ca O1 C1 2_655 . 33.57(15) O6 Ca O1 C1 . . -122.76(16) O4 Ca O1 C1 1_545 . 159.49(15) O4 Ca O1 C1 2_645 . 42.5(2) O3 Ca O1 C1 2_645 . -144.98(14) O3 Ca O1 C1 1_545 . 109.00(15) C3 Ca O1 C1 1_545 . 135.06(15) O3 Co O2 C1 . . -19.46(13) O3 Co O2 C1 5_666 . 160.54(13) O5 Co O2 C1 5_666 . -108.85(13) O5 Co O2 C1 . . 71.15(13) O2 Co O3 C3 . . 23.17(13) O2 Co O3 C3 5_666 . -156.83(13) O5 Co O3 C3 5_666 . 111.79(13) O5 Co O3 C3 . . -68.21(13) O2 Co O3 Ca . 1_565 -126.44(9) O2 Co O3 Ca 5_666 1_565 53.56(9) O5 Co O3 Ca 5_666 1_565 -37.82(9) O5 Co O3 Ca . 1_565 142.18(9) Ca O1 C1 O2 . . -41.1(2) Ca O1 C1 C2 . . 141.51(12) Co O2 C1 O1 . . 172.61(11) Co O2 C1 C2 . . -10.0(2) C3 C2 C1 O1 . . -135.66(15) C3 C2 C1 O2 . . 46.8(2) Ca O4 C3 O3 1_565 . 17.75(16) Ca O4 C3 C2 1_565 . -162.82(12) Co O3 C3 O4 . . -177.58(11) Ca O3 C3 O4 1_565 . -16.28(15) Co O3 C3 C2 . . 3.0(2) Ca O3 C3 C2 1_565 . 164.32(13) Co O3 C3 Ca . 1_565 -161.30(12) C1 C2 C3 O4 . . 137.15(15) C1 C2 C3 O3 . . -43.4(2) C1 C2 C3 Ca . 1_565 70.4(4)