#------------------------------------------------------------------------------
#$Date: 2019-11-23 03:54:56 +0200 (Sat, 23 Nov 2019) $
#$Revision: 232058 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/69/4346905.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_4346905
loop_
_publ_author_name
'Yang, Qingxiang'
'Ren, ShuangShuang'
'Hao, Ying'
'Zhao, Qianqian'
'Chen, Zhijun'
'Zheng, Hegen'
_publ_section_title
;
 Cyclopentaneteracarboxylic Metal-Organic Frameworks: Tuning the Distance
 between Layers and Pore Structures with N-Ligands.
;
_journal_issue                   10
_journal_name_full               'Inorganic chemistry'
_journal_page_first              4951
_journal_page_last               4957
_journal_paper_doi               10.1021/acs.inorgchem.5b02340
_journal_volume                  55
_journal_year                    2016
_chemical_formula_sum            'C28 H34 Co4 N4 O25'
_chemical_formula_weight         1063.31
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_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                93.488(2)
_cell_angle_beta                 104.357(2)
_cell_angle_gamma                113.993(2)
_cell_formula_units_Z            1
_cell_length_a                   9.0838(10)
_cell_length_b                   9.6157(11)
_cell_length_c                   12.4252(14)
_cell_measurement_reflns_used    2859
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.20
_cell_measurement_theta_min      2.63
_cell_volume                     944.40(19)
_computing_cell_refinement       'SMART (Bruker, 2000)'
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SMART (Bruker, 2000)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0571
_diffrn_reflns_av_sigmaI/netI    0.0796
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6719
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.72
_exptl_absorpt_coefficient_mu    1.829
_exptl_absorpt_correction_T_max  0.833
_exptl_absorpt_correction_T_min  0.833
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.870
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             539
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.011
_refine_diff_density_min         -1.003
_refine_diff_density_rms         0.215
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     284
_refine_ls_number_reflns         3261
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0665
_refine_ls_R_factor_gt           0.0570
_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/[σ²(Fo²)+(0.1301P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1683
_refine_ls_wR_factor_ref         0.1878
_reflns_number_gt                2737
_reflns_number_total             3261
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5b02340_si_005.cif
_cod_data_source_block           4
_cod_original_cell_volume        944.40(18)
_cod_original_sg_symbol_H-M      p-1
_cod_database_code               4346905
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
C1 C 0.6684(6) 0.3466(5) 0.0596(4) 0.0208(10) Uani 1 1 d .
C2 C 0.2957(6) 0.1498(5) 0.0251(4) 0.0180(10) Uani 1 1 d .
C3 C 0.1738(6) 0.1487(6) 0.2207(4) 0.0239(11) Uani 1 1 d .
C4 C 0.7326(6) 0.1844(6) 0.2442(4) 0.0230(10) Uani 1 1 d .
C5 C 0.6441(6) 0.2843(6) 0.2579(4) 0.0226(10) Uani 1 1 d .
H5 H 0.7192 0.3702 0.3210 0.027 Uiso 1 1 calc R
C6 C 0.5875(6) 0.3547(5) 0.1524(4) 0.0199(10) Uani 1 1 d .
H6 H 0.6309 0.4654 0.1814 0.024 Uiso 1 1 calc R
C7 C 0.3913(6) 0.2904(5) 0.1193(4) 0.0206(10) Uani 1 1 d .
H7 H 0.3587 0.3727 0.0981 0.025 Uiso 1 1 calc R
C8 C 0.3549(6) 0.2505(5) 0.2327(4) 0.0204(10) Uani 1 1 d .
H8 H 0.3852 0.3485 0.2808 0.024 Uiso 1 1 calc R
C9 C 0.4810(6) 0.1888(6) 0.2886(4) 0.0274(11) Uani 1 1 d .
H9A H 0.4384 0.0794 0.2596 0.033 Uiso 1 1 calc R
H9B H 0.5023 0.2038 0.3699 0.033 Uiso 1 1 calc R
C10 C 0.8668(7) -0.1693(7) 0.3980(5) 0.0371(13) Uani 1 1 d .
H10 H 0.9833 -0.1156 0.4140 0.045 Uiso 1 1 calc R
C11 C 0.8057(7) -0.2676(7) 0.4672(5) 0.0384(14) Uani 1 1 d .
H11 H 0.8788 -0.2790 0.5293 0.046 Uiso 1 1 calc R
C12 C 0.6333(7) -0.3501(6) 0.4435(4) 0.0263(11) Uani 1 1 d .
C13 C 0.5280(7) -0.3289(7) 0.3516(5) 0.0350(13) Uani 1 1 d .
H13 H 0.4113 -0.3830 0.3342 0.042 Uiso 1 1 calc R
C14 C 0.5993(7) -0.2258(7) 0.2863(5) 0.0361(13) Uani 1 1 d .
H14 H 0.5283 -0.2109 0.2248 0.043 Uiso 1 1 calc R
N2 N 0.5759(6) -0.4552(5) 0.5174(4) 0.0331(11) Uani 1 1 d .
Co1 Co 0.86683(8) 0.00495(7) 0.20409(5) 0.0212(3) Uani 1 1 d .
Co2 Co 0.5000 0.0000 0.0000 0.0173(3) Uani 1 2 d S
Co3 Co 1.0000 0.5000 0.0000 0.0226(3) Uani 1 2 d S
N1 N 0.7685(5) -0.1451(5) 0.3076(3) 0.0276(9) Uani 1 1 d .
O1 O 0.6021(4) 0.2306(4) -0.0176(3) 0.0237(7) Uani 1 1 d .
O2 O 0.8054(5) 0.4606(4) 0.0712(3) 0.0364(9) Uani 1 1 d .
O3 O 0.3061(4) 0.0262(3) 0.0438(3) 0.0208(7) Uani 1 1 d .
O4 O 0.2105(4) 0.1643(4) -0.0677(3) 0.0262(8) Uani 1 1 d .
O5 O 0.0602(5) 0.1743(4) 0.1553(3) 0.0364(9) Uani 1 1 d .
O6 O 0.1317(5) 0.0420(5) 0.2767(3) 0.0388(10) Uani 1 1 d .
O7 O 0.6626(4) 0.0661(4) 0.1642(3) 0.0250(8) Uani 1 1 d .
O8 O 0.8709(5) 0.2119(5) 0.3094(3) 0.0422(11) Uani 1 1 d .
O9 O 0.9333(5) 0.2658(4) -0.0706(3) 0.0333(9) Uani 1 1 d .
H9F H 0.8462 0.1966 -0.0430 0.040 Uiso 0.50 1 d PR
H9G H 1.0308 0.2457 -0.0485 0.040 Uiso 0.50 1 d PR
O10 O 1.1374(6) 0.4773(5) 0.1540(3) 0.0401(10) Uani 1 1 d D
H10B H 1.1127 0.3702 0.1535 0.048 Uiso 0.50 1 d PRD
O1W O 0.3159(10) 0.9291(9) 0.4571(7) 0.115(3) Uani 1 1 d .
H1WC H 0.3462 0.9898 0.4116 0.138 Uiso 1 1 d R
H1WD H 0.2992 0.8388 0.4300 0.138 Uiso 1 1 d R
O2W O 0.0863(16) 0.6379(12) 0.3179(8) 0.171(5) Uani 1 1 d .
H2WA H 0.0717 0.7004 0.2757 0.205 Uiso 1 1 d R
H2WB H -0.0084 0.5746 0.3233 0.205 Uiso 1 1 d R
O3W O 0.0000 0.5000 0.5000 0.216(9) Uani 1 2 d S
H3WD H 0.0490 0.4655 0.4630 0.259 Uiso 0.50 1 d PR
H3WB H 0.0547 0.5979 0.5190 0.259 Uiso 0.50 1 d PR
H10F H 1.106(10) 0.487(4) 0.210(5) 0.07(3) Uiso 1 1 d D
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'
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
O2 C1 O1 124.7(4) . .
O2 C1 C6 114.3(4) . .
O1 C1 C6 121.0(4) . .
O3 C2 O4 124.2(4) . .
O3 C2 C7 118.0(4) . .
O4 C2 C7 117.8(4) . .
O6 C3 O5 119.1(5) . .
O6 C3 C8 121.9(5) . .
O5 C3 C8 118.9(4) . .
O6 C3 Co1 62.2(3) . 1_455
O5 C3 Co1 57.0(3) . 1_455
C8 C3 Co1 173.7(3) . 1_455
O8 C4 O7 118.3(5) . .
O8 C4 C5 121.4(4) . .
O7 C4 C5 120.3(4) . .
C4 C5 C9 109.5(4) . .
C4 C5 C6 117.3(4) . .
C9 C5 C6 105.8(4) . .
C1 C6 C7 118.6(4) . .
C1 C6 C5 114.3(4) . .
C7 C6 C5 107.3(4) . .
C2 C7 C6 114.5(4) . .
C2 C7 C8 111.4(4) . .
C6 C7 C8 102.3(4) . .
C3 C8 C9 115.4(4) . .
C3 C8 C7 114.4(4) . .
C9 C8 C7 105.8(4) . .
C8 C9 C5 105.1(4) . .
N1 C10 C11 123.9(5) . .
C10 C11 C12 118.8(5) . .
C11 C12 C13 119.2(5) . .
C11 C12 N2 116.4(5) . .
C13 C12 N2 124.4(5) . .
C14 C13 C12 118.6(5) . .
N1 C14 C13 122.9(5) . .
N2 N2 C12 114.0(6) 2_646 .
O4 Co1 N1 95.20(15) 2_655 .
O4 Co1 O5 96.54(15) 2_655 1_655
N1 Co1 O5 155.18(17) . 1_655
O4 Co1 O7 99.68(13) 2_655 .
N1 Co1 O7 94.04(16) . .
O5 Co1 O7 105.41(14) 1_655 .
O4 Co1 O6 100.32(15) 2_655 1_655
N1 Co1 O6 96.00(15) . 1_655
O5 Co1 O6 60.39(14) 1_655 1_655
O7 Co1 O6 156.66(15) . 1_655
O4 Co1 O8 157.00(14) 2_655 .
N1 Co1 O8 92.88(17) . .
O5 Co1 O8 84.70(17) 1_655 .
O7 Co1 O8 58.21(12) . .
O6 Co1 O8 100.20(15) 1_655 .
O4 Co1 C3 100.69(15) 2_655 1_655
N1 Co1 C3 125.57(17) . 1_655
O5 Co1 C3 30.31(15) 1_655 1_655
O7 Co1 C3 132.89(15) . 1_655
O6 Co1 C3 30.10(15) 1_655 1_655
O8 Co1 C3 91.95(15) . 1_655
O3 Co2 O3 180.0 . 2_655
O3 Co2 O1 89.88(13) . .
O3 Co2 O1 90.12(13) 2_655 .
O3 Co2 O1 90.11(13) . 2_655
O3 Co2 O1 89.88(13) 2_655 2_655
O1 Co2 O1 180.0 . 2_655
O3 Co2 O7 84.83(13) . 2_655
O3 Co2 O7 95.17(13) 2_655 2_655
O1 Co2 O7 91.41(13) . 2_655
O1 Co2 O7 88.59(13) 2_655 2_655
O3 Co2 O7 95.17(13) . .
O3 Co2 O7 84.83(13) 2_655 .
O1 Co2 O7 88.59(13) . .
O1 Co2 O7 91.41(13) 2_655 .
O7 Co2 O7 180.0 2_655 .
O2 Co3 O2 180.0 2_765 .
O2 Co3 O10 86.99(17) 2_765 2_765
O2 Co3 O10 93.01(17) . 2_765
O2 Co3 O10 93.01(17) 2_765 .
O2 Co3 O10 86.99(17) . .
O10 Co3 O10 180.0 2_765 .
O2 Co3 O9 80.76(14) 2_765 .
O2 Co3 O9 99.24(14) . .
O10 Co3 O9 89.42(15) 2_765 .
O10 Co3 O9 90.58(15) . .
O2 Co3 O9 99.24(14) 2_765 2_765
O2 Co3 O9 80.76(14) . 2_765
O10 Co3 O9 90.58(15) 2_765 2_765
O10 Co3 O9 89.42(15) . 2_765
O9 Co3 O9 179.999(1) . 2_765
C10 N1 C14 116.6(4) . .
C10 N1 Co1 122.6(4) . .
C14 N1 Co1 120.8(3) . .
C1 O1 Co2 126.9(3) . .
C1 O2 Co3 133.2(3) . .
C2 O3 Co2 114.4(3) . .
C2 O4 Co1 116.9(3) . 2_655
C3 O5 Co1 92.7(3) . 1_455
C3 O6 Co1 87.7(3) . 1_455
C4 O7 Co2 137.7(3) . .
C4 O7 Co1 95.0(3) . .
Co2 O7 Co1 119.65(15) . .
C4 O8 Co1 88.4(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 O2 1.246(6) .
C1 O1 1.251(6) .
C1 C6 1.527(6) .
C2 O3 1.260(6) .
C2 O4 1.269(6) .
C2 C7 1.517(6) .
C3 O6 1.257(6) .
C3 O5 1.266(6) .
C3 C8 1.496(7) .
C3 Co1 2.505(5) 1_455
C4 O8 1.226(6) .
C4 O7 1.283(6) .
C4 C5 1.507(7) .
C5 C9 1.550(7) .
C5 C6 1.581(7) .
C6 C7 1.561(6) .
C7 C8 1.560(6) .
C8 C9 1.534(7) .
C10 N1 1.347(7) .
C10 C11 1.360(7) .
C11 C12 1.379(8) .
C12 C13 1.381(8) .
C12 N2 1.435(6) .
C13 C14 1.378(8) .
C14 N1 1.355(7) .
N2 N2 1.235(9) 2_646
Co1 O4 2.039(3) 2_655
Co1 N1 2.069(4) .
Co1 O5 2.103(4) 1_655
Co1 O7 2.121(3) .
Co1 O6 2.217(4) 1_655
Co1 O8 2.296(4) .
Co1 C3 2.505(5) 1_655
Co2 O3 2.069(3) .
Co2 O3 2.070(3) 2_655
Co2 O1 2.076(3) .
Co2 O1 2.076(3) 2_655
Co2 O7 2.082(3) 2_655
Co2 O7 2.082(3) .
Co3 O2 2.080(3) 2_765
Co3 O2 2.080(3) .
Co3 O10 2.087(4) 2_765
Co3 O10 2.087(4) .
Co3 O9 2.143(3) .
Co3 O9 2.143(3) 2_765
O4 Co1 2.039(3) 2_655
O5 Co1 2.103(4) 1_455
O6 Co1 2.217(4) 1_455
