#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:32:24 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179250 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/70/4317010.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_4317010
loop_
_publ_author_name
'Jian-Qiang Liu'
'Bin Liu'
'Yao-Yu Wang'
'Ping Liu'
'Guo-Ping Yang'
'Rui-Ting Liu'
'Qi-Zhen Shi'
'Stuart R. Batten'
_publ_section_title
;
 An Unusual 3D Entangled Co(II) Coordination Polymer Directed by
 Ferromagnetic Molecular Building Block
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10422
_journal_page_last               10426
_journal_paper_doi               10.1021/ic101286j
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'C34 H33 Co2 O15'
_chemical_formula_weight         799.46
_chemical_name_systematic
; 
 ? 
;
_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                 105.241(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.842(2)
_cell_length_b                   24.652(4)
_cell_length_c                   10.5305(17)
_cell_measurement_reflns_used    3105
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.30
_cell_measurement_theta_min      1.65
_cell_volume                     3467.0(9)
_computing_cell_refinement       APEX2
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        APEX2
_computing_molecular_graphics    APEX2
_computing_publication_material  APEX2
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX SMART II'
_diffrn_measurement_method       ω
_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  0.0315
_diffrn_reflns_av_sigmaI/netI    0.0419
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            8609
_diffrn_reflns_theta_full        25.20
_diffrn_reflns_theta_max         25.20
_diffrn_reflns_theta_min         1.65
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.029
_exptl_absorpt_correction_T_max  0.8285
_exptl_absorpt_correction_T_min  0.7615
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.532
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1644
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.865
_refine_diff_density_min         -0.462
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         3105
_refine_ls_number_restraints     219
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0654
_refine_ls_R_factor_gt           0.0504
_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/[σ²(Fo²)+(0.1060P)²+0.8505P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1456
_refine_ls_wR_factor_ref         0.1555
_reflns_number_gt                2344
_reflns_number_total             3105
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic101286j_si_001.cif
_cod_data_source_block           1
_cod_database_code               4317010
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_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 1.0000 0.41717(3) -0.2500 0.0376(2) Uani 1 2 d SU . .
Co2 Co 1.0000 0.5000 0.0000 0.0319(2) Uani 1 2 d SU . .
O3 O 0.9541(2) 0.42177(9) 0.0273(3) 0.0458(7) Uani 1 1 d U . .
O4 O 1.40006(16) -0.02906(8) 0.6301(2) 0.0295(5) Uani 1 1 d U . .
O5 O 1.38268(18) 0.00905(10) 0.8144(2) 0.0403(6) Uani 1 1 d U . .
O6 O 0.9426(3) 0.36603(11) -0.1399(3) 0.0586(8) Uani 1 1 d U . .
O7 O 0.9784(2) 0.07935(11) 0.4045(3) 0.0528(7) Uani 1 1 d U . .
O8 O 0.8373(2) 0.20818(10) 0.2790(3) 0.0510(7) Uani 1 1 d U . .
C7 C 1.2566(2) 0.02556(12) 0.6185(3) 0.0271(7) Uani 1 1 d U . .
C8 C 1.0695(3) 0.06360(15) 0.4802(4) 0.0391(8) Uani 1 1 d U . .
C9 C 0.9349(3) 0.37641(14) -0.0259(4) 0.0367(8) Uani 1 1 d U . .
C10 C 1.2029(2) 0.05986(14) 0.6780(3) 0.0351(8) Uani 1 1 d U . .
H10A H 1.2299 0.0700 0.7652 0.042 Uiso 1 1 calc R . .
C11 C 1.1088(3) 0.07972(14) 0.6102(4) 0.0398(9) Uani 1 1 d U . .
H11A H 1.0735 0.1031 0.6509 0.048 Uiso 1 1 calc R . .
C12 C 0.8582(3) 0.24617(13) 0.1956(4) 0.0382(8) Uani 1 1 d U . .
C13 C 0.9035(2) 0.33137(13) 0.0481(4) 0.0334(7) Uani 1 1 d U . .
C14 C 0.8855(3) 0.34121(14) 0.1699(4) 0.0405(9) Uani 1 1 d U . .
H14A H 0.8893 0.3765 0.2019 0.049 Uiso 1 1 calc R . .
C15 C 1.3527(2) 0.00151(12) 0.6931(3) 0.0267(7) Uani 1 1 d U . .
C16 C 0.8975(3) 0.27890(14) 0.0019(4) 0.0421(9) Uani 1 1 d U . .
H16A H 0.9087 0.2720 -0.0799 0.050 Uiso 1 1 calc R . .
C17 C 1.1232(3) 0.03052(15) 0.4192(4) 0.0428(9) Uani 1 1 d U . .
H17A H 1.0965 0.0207 0.3318 0.051 Uiso 1 1 calc R . .
C18 C 1.2170(3) 0.01162(14) 0.4869(4) 0.0356(8) Uani 1 1 d U . .
H18A H 1.2534 -0.0103 0.4444 0.043 Uiso 1 1 calc R . .
C19 C 0.8622(3) 0.29987(14) 0.2438(4) 0.0453(9) Uani 1 1 d U . .
H19A H 0.8492 0.3071 0.3244 0.054 Uiso 1 1 calc R . .
C20 C 0.8749(3) 0.23616(13) 0.0749(4) 0.0430(9) Uani 1 1 d U . .
H20A H 0.8710 0.2010 0.0422 0.052 Uiso 1 1 calc R . .
C21 C 0.8189(3) 0.11916(16) 0.3512(5) 0.0515(11) Uani 1 1 d U . .
H21A H 0.7694 0.1363 0.3884 0.062 Uiso 1 1 calc R . .
H21B H 0.7934 0.0837 0.3189 0.062 Uiso 1 1 calc R . .
C22 C 0.9150(3) 0.11209(16) 0.4584(4) 0.0484(10) Uani 1 1 d U . .
H22A H 0.9459 0.1470 0.4851 0.058 Uiso 1 1 calc R . .
H22B H 0.9018 0.0946 0.5346 0.058 Uiso 1 1 calc R . .
C23 C 0.8318(3) 0.15293(14) 0.2368(4) 0.0461(10) Uani 1 1 d U . .
H23A H 0.8927 0.1427 0.2137 0.055 Uiso 1 1 calc R . .
H23B H 0.7755 0.1477 0.1605 0.055 Uiso 1 1 calc R . .
O1W O 1.0000 0.1941(4) 0.7500 0.183(4) Uani 1 2 d SDU . .
H1W H 0.9558 0.2162 0.7083 0.220 Uiso 0.50 1 d PRD . .
O2W O 0.8758(11) 0.2540(9) 0.6265(14) 0.432(11) Uani 1 1 d DU . .
H2WA H 0.8324 0.2548 0.5525 0.519 Uiso 1 1 d RD . .
H2WB H 0.9110 0.2813 0.6178 0.519 Uiso 1 1 d RD . .
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'
Co Co 0.3494 0.9721 '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'
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
O6 Co1 O6 102.42(17) 2_754 . ?
O6 Co1 O4 116.60(12) 2_754 4_755 ?
O6 Co1 O4 110.41(11) . 4_755 ?
O6 Co1 O4 110.41(11) 2_754 3_454 ?
O6 Co1 O4 116.60(12) . 3_454 ?
O4 Co1 O4 101.05(12) 4_755 3_454 ?
O3 Co2 O3 180.00(4) . 5_765 ?
O3 Co2 O5 87.94(11) . 7_756 ?
O3 Co2 O5 92.06(11) 5_765 7_756 ?
O3 Co2 O5 92.06(11) . 3_454 ?
O3 Co2 O5 87.94(11) 5_765 3_454 ?
O5 Co2 O5 180.0 7_756 3_454 ?
O3 Co2 O4 92.71(9) . 4_755 ?
O3 Co2 O4 87.29(9) 5_765 4_755 ?
O5 Co2 O4 94.50(8) 7_756 4_755 ?
O5 Co2 O4 85.50(8) 3_454 4_755 ?
O3 Co2 O4 87.29(9) . 8_455 ?
O3 Co2 O4 92.71(9) 5_765 8_455 ?
O5 Co2 O4 85.50(8) 7_756 8_455 ?
O5 Co2 O4 94.50(8) 3_454 8_455 ?
O4 Co2 O4 180.0 4_755 8_455 ?
C9 O3 Co2 143.9(3) . . ?
C15 O4 Co1 113.9(2) . 3_546 ?
C15 O4 Co2 126.17(18) . 4_745 ?
Co1 O4 Co2 98.71(8) 3_546 4_745 ?
C15 O5 Co2 149.7(2) . 3_546 ?
C9 O6 Co1 124.6(2) . . ?
C8 O7 C22 120.3(3) . . ?
C12 O8 C23 117.2(3) . . ?
C10 C7 C18 119.0(3) . . ?
C10 C7 C15 121.4(3) . . ?
C18 C7 C15 119.5(3) . . ?
O7 C8 C17 115.4(3) . . ?
O7 C8 C11 123.9(3) . . ?
C17 C8 C11 120.7(3) . . ?
O3 C9 O6 123.3(3) . . ?
O3 C9 C13 119.4(3) . . ?
O6 C9 C13 117.3(3) . . ?
C7 C10 C11 121.5(3) . . ?
C7 C10 H10A 119.2 . . ?
C11 C10 H10A 119.2 . . ?
C8 C11 C10 118.3(3) . . ?
C8 C11 H11A 120.9 . . ?
C10 C11 H11A 120.9 . . ?
O8 C12 C20 126.0(3) . . ?
O8 C12 C19 114.0(3) . . ?
C20 C12 C19 120.0(3) . . ?
C16 C13 C14 118.7(3) . . ?
C16 C13 C9 121.0(3) . . ?
C14 C13 C9 120.1(3) . . ?
C19 C14 C13 121.3(3) . . ?
C19 C14 H14A 119.3 . . ?
C13 C14 H14A 119.3 . . ?
O5 C15 O4 122.4(3) . . ?
O5 C15 C7 119.6(3) . . ?
O4 C15 C7 117.9(3) . . ?
C13 C16 C20 121.3(4) . . ?
C13 C16 H16A 119.4 . . ?
C20 C16 H16A 119.4 . . ?
C8 C17 C18 120.6(3) . . ?
C8 C17 H17A 119.7 . . ?
C18 C17 H17A 119.7 . . ?
C17 C18 C7 119.9(3) . . ?
C17 C18 H18A 120.1 . . ?
C7 C18 H18A 120.1 . . ?
C14 C19 C12 119.1(4) . . ?
C14 C19 H19A 120.5 . . ?
C12 C19 H19A 120.5 . . ?
C12 C20 C16 119.6(3) . . ?
C12 C20 H20A 120.2 . . ?
C16 C20 H20A 120.2 . . ?
C22 C21 C23 113.1(3) . . ?
C22 C21 H21A 109.0 . . ?
C23 C21 H21A 109.0 . . ?
C22 C21 H21B 109.0 . . ?
C23 C21 H21B 109.0 . . ?
H21A C21 H21B 107.8 . . ?
O7 C22 C21 106.4(4) . . ?
O7 C22 H22A 110.4 . . ?
C21 C22 H22A 110.4 . . ?
O7 C22 H22B 110.4 . . ?
C21 C22 H22B 110.4 . . ?
H22A C22 H22B 108.6 . . ?
O8 C23 C21 106.5(4) . . ?
O8 C23 H23A 110.4 . . ?
C21 C23 H23A 110.4 . . ?
O8 C23 H23B 110.4 . . ?
C21 C23 H23B 110.4 . . ?
H23A C23 H23B 108.6 . . ?
H2WA O2W H2WB 99.7 . . ?
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 O6 2.012(3) 2_754 ?
Co1 O6 2.012(3) . ?
Co1 O4 2.085(2) 4_755 ?
Co1 O4 2.085(2) 3_454 ?
Co2 O3 2.074(2) . ?
Co2 O3 2.074(2) 5_765 ?
Co2 O5 2.200(2) 7_756 ?
Co2 O5 2.200(2) 3_454 ?
Co2 O4 2.302(2) 4_755 ?
Co2 O4 2.302(2) 8_455 ?
O3 C9 1.248(4) . ?
O4 C15 1.291(4) . ?
O4 Co1 2.085(2) 3_546 ?
O4 Co2 2.302(2) 4_745 ?
O5 C15 1.249(4) . ?
O5 Co2 2.200(2) 3_546 ?
O6 C9 1.259(5) . ?
O7 C8 1.360(4) . ?
O7 C22 1.416(5) . ?
O8 C12 1.366(4) . ?
O8 C23 1.428(5) . ?
C7 C10 1.380(5) . ?
C7 C18 1.393(5) . ?
C7 C15 1.480(4) . ?
C8 C17 1.372(5) . ?
C8 C11 1.391(5) . ?
C9 C13 1.485(5) . ?
C10 C11 1.398(5) . ?
C10 H10A 0.9300 . ?
C11 H11A 0.9300 . ?
C12 C20 1.373(5) . ?
C12 C19 1.414(5) . ?
C13 C16 1.377(5) . ?
C13 C14 1.391(5) . ?
C14 C19 1.371(5) . ?
C14 H14A 0.9300 . ?
C16 C20 1.387(5) . ?
C16 H16A 0.9300 . ?
C17 C18 1.387(5) . ?
C17 H17A 0.9300 . ?
C18 H18A 0.9300 . ?
C19 H19A 0.9300 . ?
C20 H20A 0.9300 . ?
C21 C22 1.511(6) . ?
C21 C23 1.514(5) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
O1W H1W 0.8500 . ?
O2W H2WA 0.8501 . ?
O2W H2WB 0.8501 . ?
