#------------------------------------------------------------------------------
#$Date: 2016-02-16 02:10:39 +0100 (mar 16 de feb de 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/09/7010922.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7010922
loop_
_publ_author_name
'Long, La-Sheng'
'Chen, Xiao-Ming'
'Tong, Ming-Liang'
'Sun, Zi-Guang'
'Ren, Yan-Ping'
'Huang, Rong-Bin'
'Zheng, Lan-Sun'
_publ_section_title
;
 A unique open inorganic--organic framework with alternate hexa- and
 penta-coordinate cobalt(ii) sites. Synthesis, crystal structure and
 magnetic properties of [Co3(C4H4O4)2.5(OH)]n·0.5nH2O
;
_journal_issue                   19
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2888
_journal_paper_doi               10.1039/b105482c
_journal_year                    2001
_chemical_formula_sum            'C10 H12 Co3 O11.5'
_chemical_formula_weight         492.99
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                83.10(3)
_cell_angle_beta                 75.86(3)
_cell_angle_gamma                68.69(3)
_cell_formula_units_Z            2
_cell_length_a                   8.7501(18)
_cell_length_b                   9.1116(18)
_cell_length_c                   10.350(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      7.5
_cell_volume                     745.0(3)
_computing_cell_refinement       'SHELXTL-Plus (Sheldrick, 1990)'
_computing_data_collection       'SHELXTL-Plus (Sheldrick, 1990)'
_computing_data_reduction        'SHELXTL-Plus (Sheldrick, 1990)'
_computing_molecular_graphics    'SHELXTL V.5.0 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXTL-Plus (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Siemens CAD4'
_diffrn_measurement_method       'ω scan'
_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  0.0138
_diffrn_reflns_av_sigmaI/netI    0.0311
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            3122
_diffrn_reflns_theta_full        25.97
_diffrn_reflns_theta_max         25.97
_diffrn_reflns_theta_min         2.03
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 200
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    3.362
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'Deep Red'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       polyhedral
_exptl_crystal_F_000             490
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.516
_refine_diff_density_min         -0.390
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     233
_refine_ls_number_reflns         2918
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0345
_refine_ls_R_factor_gt           0.0273
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0269P)²+0.4812P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0596
_refine_ls_wR_factor_ref         0.0623
_reflns_number_gt                2547
_reflns_number_total             2918
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b105482c.txt
_cod_data_source_block           complex_1
_cod_original_cell_volume        745.1(3)
_cod_original_sg_symbol_H-M      p-1
_cod_original_formula_sum        'C10 H12 Co3 O11.50'
_cod_database_code               7010922
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.0000 0.0000 0.0000 0.01493(12) Uani 1 2 d S . .
Co2 Co 0.0000 0.0000 0.5000 0.01406(12) Uani 1 2 d S . .
Co3 Co -0.16462(4) -0.07713(5) 0.79555(4) 0.01458(10) Uani 1 1 d . . .
Co4 Co -0.56175(5) 0.13982(5) 0.89823(4) 0.02157(11) Uani 1 1 d . . .
O1 O -0.1796(2) 0.1204(2) -0.1072(2) 0.0192(4) Uani 1 1 d . . .
O2 O -0.4433(3) 0.2833(3) -0.0726(3) 0.0340(6) Uani 1 1 d . . .
C1 C -0.2920(3) 0.2560(4) -0.0806(3) 0.0205(6) Uani 1 1 d . . .
C2 C -0.2403(4) 0.3898(4) -0.0582(4) 0.0296(8) Uani 1 1 d . . .
H2A H -0.2544 0.3971 0.0370 0.036 Uiso 1 1 calc R . .
H2B H -0.3165 0.4871 -0.0893 0.036 Uiso 1 1 calc R . .
C3 C -0.0613(4) 0.3785(4) -0.1253(3) 0.0239(7) Uani 1 1 d . . .
H3A H -0.0321 0.3291 -0.2102 0.029 Uiso 1 1 calc R . .
H3B H -0.0591 0.4847 -0.1443 0.029 Uiso 1 1 calc R . .
C4 C 0.0727(3) 0.2893(3) -0.0491(3) 0.0165(6) Uani 1 1 d . . .
O3 O 0.2111(2) 0.3071(3) -0.0881(2) 0.0247(5) Uani 1 1 d . . .
O4 O 0.0402(2) 0.1977(2) 0.0495(2) 0.0184(4) Uani 1 1 d . . .
O5 O -0.1945(2) 0.0308(3) 0.1655(2) 0.0231(5) Uani 1 1 d . . .
O6 O -0.0737(2) 0.0773(2) 0.3145(2) 0.0186(4) Uani 1 1 d . . .
C5 C -0.1997(3) 0.0728(4) 0.2768(3) 0.0198(6) Uani 1 1 d . . .
C6 C -0.3679(4) 0.1236(6) 0.3717(4) 0.0495(12) Uani 1 1 d . . .
H6A H -0.3870 0.0297 0.4160 0.059 Uiso 1 1 calc R . .
H6B H -0.4532 0.1723 0.3198 0.059 Uiso 1 1 calc R . .
C7 C -0.3952(4) 0.2377(5) 0.4791(3) 0.0349(8) Uani 1 1 d . . .
H7A H -0.3114 0.2882 0.4531 0.042 Uiso 1 1 calc R . .
H7B H -0.5049 0.3192 0.4850 0.042 Uiso 1 1 calc R . .
C8 C -0.3842(4) 0.1575(4) 0.6130(3) 0.0217(6) Uani 1 1 d . . .
O7 O -0.2395(2) 0.0699(2) 0.6318(2) 0.0191(4) Uani 1 1 d . . .
O8 O -0.5165(3) 0.1762(3) 0.6976(2) 0.0351(6) Uani 1 1 d . . .
O9 O 0.1391(3) 0.2672(3) 0.3058(2) 0.0245(5) Uani 1 1 d . . .
O10 O 0.0261(3) 0.2086(3) 0.5152(2) 0.0256(5) Uani 1 1 d . . .
O1W O -0.3944(2) -0.0813(3) 0.8966(2) 0.0198(4) Uani 1 1 d . . .
H1W H -0.403(5) -0.143(5) 0.861(4) 0.043(13) Uiso 1 1 d . . .
C9 C 0.0855(3) 0.2933(4) 0.4287(3) 0.0192(6) Uani 1 1 d . . .
C10 C 0.0891(4) 0.4421(4) 0.4768(3) 0.0227(7) Uani 1 1 d . . .
H10A H 0.1507 0.4911 0.4051 0.027 Uiso 1 1 calc R . .
H10B H 0.1468 0.4157 0.5499 0.027 Uiso 1 1 calc R . .
O2W O -0.268(2) 0.4542(16) 0.2812(13) 0.187(6) Uani 0.50 1 d P . .
H2WA H -0.3568 0.5167 0.2583 0.224 Uiso 0.50 1 d PR . .
H2WB H -0.1938 0.4094 0.2143 0.224 Uiso 0.50 1 d PR . .
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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Co1 O1 180.00(18) 2 . ?
O1 Co1 O5 93.16(8) 2 . ?
O1 Co1 O5 86.84(8) . . ?
O1 Co1 O5 86.84(8) 2 2 ?
O1 Co1 O5 93.16(8) . 2 ?
O5 Co1 O5 180.00(17) . 2 ?
O1 Co1 O4 83.36(8) 2 . ?
O1 Co1 O4 96.64(8) . . ?
O5 Co1 O4 89.61(8) . . ?
O5 Co1 O4 90.39(8) 2 . ?
O1 Co1 O4 96.64(8) 2 2 ?
O1 Co1 O4 83.36(8) . 2 ?
O5 Co1 O4 90.39(8) . 2 ?
O5 Co1 O4 89.61(8) 2 2 ?
O4 Co1 O4 180.00(11) . 2 ?
O10 Co2 O10 180.0 . 2_556 ?
O10 Co2 O7 91.71(9) . . ?
O10 Co2 O7 88.29(9) 2_556 . ?
O10 Co2 O7 88.29(9) . 2_556 ?
O10 Co2 O7 91.71(9) 2_556 2_556 ?
O7 Co2 O7 180.0 . 2_556 ?
O10 Co2 O6 90.73(9) . . ?
O10 Co2 O6 89.27(9) 2_556 . ?
O7 Co2 O6 99.76(8) . . ?
O7 Co2 O6 80.24(8) 2_556 . ?
O10 Co2 O6 89.27(9) . 2_556 ?
O10 Co2 O6 90.73(9) 2_556 2_556 ?
O7 Co2 O6 80.24(8) . 2_556 ?
O7 Co2 O6 99.76(8) 2_556 2_556 ?
O6 Co2 O6 180.00(4) . 2_556 ?
O1W Co3 O9 88.04(9) . 2_556 ?
O1W Co3 O7 98.49(8) . . ?
O9 Co3 O7 88.78(9) 2_556 . ?
O1W Co3 O1 94.96(9) . 1_556 ?
O9 Co3 O1 176.93(8) 2_556 1_556 ?
O7 Co3 O1 90.15(8) . 1_556 ?
O1W Co3 O6 178.05(8) . 2_556 ?
O9 Co3 O6 90.12(9) 2_556 2_556 ?
O7 Co3 O6 80.81(8) . 2_556 ?
O1 Co3 O6 86.87(8) 1_556 2_556 ?
O1W Co3 O4 94.46(8) . 2_556 ?
O9 Co3 O4 99.23(9) 2_556 2_556 ?
O7 Co3 O4 165.00(7) . 2_556 ?
O1 Co3 O4 81.19(8) 1_556 2_556 ?
O6 Co3 O4 86.48(8) 2_556 2_556 ?
O3 Co4 O1W 156.48(8) 1_456 . ?
O3 Co4 O8 89.27(10) 1_456 . ?
O1W Co4 O8 95.74(10) . . ?
O3 Co4 O2 96.07(9) 1_456 1_556 ?
O1W Co4 O2 106.45(9) . 1_556 ?
O8 Co4 O2 93.93(11) . 1_556 ?
O3 Co4 O1W 93.29(10) 1_456 2_457 ?
O1W Co4 O1W 80.19(10) . 2_457 ?
O8 Co4 O1W 174.92(10) . 2_457 ?
O2 Co4 O1W 90.17(10) 1_556 2_457 ?
C1 O1 Co1 125.65(18) . . ?
C1 O1 Co3 134.22(17) . 1_554 ?
Co1 O1 Co3 96.28(9) . 1_554 ?
C1 O2 Co4 130.0(2) . 1_554 ?
O2 C1 O1 122.9(3) . . ?
O2 C1 C2 117.8(3) . . ?
O1 C1 C2 119.3(2) . . ?
C1 C2 C3 116.1(3) . . ?
C4 C3 C2 116.6(3) . . ?
O3 C4 O4 123.8(3) . . ?
O3 C4 C3 117.1(3) . . ?
O4 C4 C3 119.1(2) . . ?
C4 O3 Co4 127.0(2) . 1_654 ?
C4 O4 Co1 115.37(17) . . ?
C4 O4 Co3 133.88(17) . 2_556 ?
Co1 O4 Co3 94.51(9) . 2_556 ?
C5 O5 Co1 126.88(18) . . ?
C5 O6 Co3 131.13(19) . 2_556 ?
C5 O6 Co2 129.21(19) . . ?
Co3 O6 Co2 96.11(8) 2_556 . ?
O5 C5 O6 124.6(3) . . ?
O5 C5 C6 117.1(2) . . ?
O6 C5 C6 118.3(3) . . ?
C5 C6 C7 117.4(3) . . ?
C8 C7 C6 112.6(3) . . ?
O8 C8 O7 123.9(3) . . ?
O8 C8 C7 118.1(3) . . ?
O7 C8 C7 117.9(3) . . ?
C8 O7 Co3 131.46(19) . . ?
C8 O7 Co2 131.44(19) . . ?
Co3 O7 Co2 96.64(8) . . ?
C8 O8 Co4 131.8(2) . . ?
C9 O9 Co3 129.40(19) . 2_556 ?
C9 O10 Co2 130.59(19) . . ?
Co4 O1W Co3 108.52(11) . . ?
Co4 O1W Co4 99.81(10) . 2_457 ?
Co3 O1W Co4 120.73(10) . 2_457 ?
O10 C9 O9 126.0(3) . . ?
O10 C9 C10 116.3(3) . . ?
O9 C9 C10 117.7(3) . . ?
C9 C10 C10 110.8(3) . 2_566 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 O1 2.052(2) 2 ?
Co1 O1 2.052(2) . ?
Co1 O5 2.063(2) . ?
Co1 O5 2.063(2) 2 ?
Co1 O4 2.0976(19) . ?
Co1 O4 2.0976(19) 2 ?
Co2 O10 2.023(2) . ?
Co2 O10 2.023(2) 2_556 ?
Co2 O7 2.121(2) . ?
Co2 O7 2.121(2) 2_556 ?
Co2 O6 2.133(2) . ?
Co2 O6 2.133(2) 2_556 ?
Co3 O1W 2.038(2) . ?
Co3 O9 2.047(2) 2_556 ?
Co3 O7 2.111(2) . ?
Co3 O1 2.114(2) 1_556 ?
Co3 O6 2.118(2) 2_556 ?
Co3 O4 2.127(2) 2_556 ?
Co4 O3 2.001(2) 1_456 ?
Co4 O1W 2.014(2) . ?
Co4 O8 2.026(2) . ?
Co4 O2 2.027(2) 1_556 ?
Co4 O1W 2.103(2) 2_457 ?
O1 C1 1.279(4) . ?
O1 Co3 2.114(2) 1_554 ?
O2 C1 1.238(4) . ?
O2 Co4 2.027(2) 1_554 ?
C1 C2 1.506(4) . ?
C2 C3 1.522(4) . ?
C3 C4 1.504(4) . ?
C4 O3 1.243(3) . ?
C4 O4 1.282(4) . ?
O3 Co4 2.001(2) 1_654 ?
O4 Co3 2.127(2) 2_556 ?
O5 C5 1.242(4) . ?
O6 C5 1.272(3) . ?
O6 Co3 2.118(2) 2_556 ?
C5 C6 1.501(4) . ?
C6 C7 1.529(5) . ?
C7 C8 1.496(5) . ?
C8 O8 1.238(4) . ?
C8 O7 1.275(4) . ?
O9 C9 1.263(4) . ?
O9 Co3 2.047(2) 2_556 ?
O10 C9 1.252(4) . ?
O1W Co4 2.103(2) 2_457 ?
C9 C10 1.512(4) . ?
C10 C10 1.528(6) 2_566 ?
