#------------------------------------------------------------------------------
#$Date: 2019-11-23 03:54:17 +0200 (Sat, 23 Nov 2019) $
#$Revision: 232055 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/69/4346902.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_4346902
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            'C15 H13 Co2 N O10'
_chemical_formula_weight         485.12
_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                94.6640(10)
_cell_angle_beta                 103.8370(10)
_cell_angle_gamma                114.8300(10)
_cell_formula_units_Z            2
_cell_length_a                   9.1461(6)
_cell_length_b                   9.6587(6)
_cell_length_c                   12.7617(12)
_cell_measurement_reflns_used    3166
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.40
_cell_measurement_theta_min      2.37
_cell_volume                     972.10(13)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0142
_diffrn_reflns_av_sigmaI/netI    0.0255
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            5509
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.68
_exptl_absorpt_coefficient_mu    1.758
_exptl_absorpt_correction_T_max  0.839
_exptl_absorpt_correction_T_min  0.839
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.657
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             489
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
;
_refine_diff_density_max         0.575
_refine_diff_density_min         -0.345
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     238
_refine_ls_number_reflns         3414
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0315
_refine_ls_R_factor_gt           0.0276
_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)+(0.0431P)²+0.1836P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0723
_refine_ls_wR_factor_ref         0.0744
_reflns_number_gt                3014
_reflns_number_total             3414
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5b02340_si_004.cif
_cod_data_source_block           3
_cod_original_sg_symbol_H-M      p-1
_cod_database_code               4346902
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 0.7680(3) 0.3103(3) 0.26077(19) 0.0276(5) Uani 1 1 d .
O6 O 1.2889(2) 0.33961(19) 0.56496(13) 0.0328(4) Uani 1 1 d .
O8 O 1.4367(2) 0.3155(2) 0.34400(17) 0.0451(5) Uani 1 1 d .
O7 O 1.3719(2) 0.4530(2) 0.23421(16) 0.046 Uani 1 1 d .
C4 C 1.3271(3) 0.3453(3) 0.28446(19) 0.029 Uani 1 1 d .
C5 C 1.1434(3) 0.2450(3) 0.27326(19) 0.027 Uani 1 1 d .
H5 H 1.1096 0.1451 0.2256 0.032 Uiso 1 1 calc R
O4 O 0.6881(2) 0.03979(19) 0.42573(16) 0.0438(5) Uani 1 1 d .
O3 O 0.8982(2) 0.26993(17) 0.51671(13) 0.0309(4) Uani 1 1 d .
C2 C 0.8286(3) 0.1528(2) 0.43908(19) 0.0255(5) Uani 1 1 d .
Co1 Co 0.63442(4) 0.48780(3) 0.30123(2) 0.02605(10) Uani 1 1 d .
Co2 Co 1.0000 0.5000 0.5000 0.02236(11) Uani 1 2 d S
Co3 Co 0.5000 0.0000 0.5000 0.02839(12) Uani 1 2 d S
O5 O 1.19384(19) 0.47428(17) 0.45825(13) 0.0268(3) Uani 1 1 d .
O2 O 0.8361(2) 0.42898(19) 0.33894(13) 0.0310(4) Uani 1 1 d .
C3 C 1.2030(3) 0.3501(2) 0.47568(19) 0.0244(5) Uani 1 1 d .
O9 O 0.4335(2) -0.23585(18) 0.43150(16) 0.0401(4) Uani 1 1 d .
H9D H 0.3356 -0.3052 0.4494 0.060 Uiso 0.50 1 d PR
H9E H 0.5260 -0.2581 0.4618 0.060 Uiso 0.50 1 d PR
C9 C 1.1063(3) 0.2072(2) 0.38250(18) 0.0248(5) Uani 1 1 d .
H9A H 1.1370 0.1250 0.4026 0.030 Uiso 1 1 calc R
N1 N 0.7288(3) 0.6350(2) 0.19837(16) 0.0316(4) Uani 1 1 d .
C7 C 0.8580(3) 0.2113(3) 0.24750(19) 0.0282(5) Uani 1 1 d .
H7 H 0.7833 0.1239 0.1851 0.034 Uiso 1 1 calc R
C6 C 1.0224(3) 0.3069(3) 0.2195(2) 0.0317(5) Uani 1 1 d .
H6A H 1.0025 0.2913 0.1403 0.038 Uiso 1 1 calc R
H6B H 1.0672 0.4172 0.2493 0.038 Uiso 1 1 calc R
C15 C 0.9200(3) 0.9575(3) -0.0030(2) 0.0363(6) Uani 1 1 d .
H15 H 0.8393 0.9705 -0.0555 0.044 Uiso 1 1 calc R
C12 C 0.8581(3) 0.8444(3) 0.06557(19) 0.0325(5) Uani 1 1 d .
C8 C 0.9106(3) 0.1419(2) 0.34911(19) 0.0255(5) Uani 1 1 d .
H8 H 0.8651 0.0301 0.3200 0.031 Uiso 1 1 calc R
O1 O 0.6301(2) 0.2797(2) 0.19409(16) 0.0458(5) Uani 1 1 d .
O10 O 0.3553(3) 0.0151(2) 0.35246(17) 0.0493(5) Uani 1 1 d D
H10C H 0.3311 -0.0704 0.3121 0.074 Uiso 0.50 1 d PRD
H10D H 0.4284 0.0711 0.3115 0.074 Uiso 0.50 1 d PRD
C11 C 0.9632(3) 0.8225(3) 0.1531(2) 0.0422(6) Uani 1 1 d .
H11 H 1.0798 0.8780 0.1688 0.051 Uiso 1 1 calc R
C14 C 0.6279(3) 0.6547(4) 0.1135(2) 0.0474(7) Uani 1 1 d .
H14 H 0.5118 0.5970 0.0987 0.057 Uiso 1 1 calc R
C13 C 0.6863(4) 0.7562(4) 0.0461(2) 0.0506(8) Uani 1 1 d .
H13 H 0.6101 0.7653 -0.0124 0.061 Uiso 1 1 calc R
C10 C 0.8963(3) 0.7191(3) 0.2172(2) 0.0422(6) Uani 1 1 d .
H10A H 0.9698 0.7070 0.2758 0.051 Uiso 1 1 calc R
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
O1 C1 O2 118.7(2) . .
O1 C1 C7 120.9(2) . .
O2 C1 C7 120.3(2) . .
C3 O6 Co1 116.73(15) . 2_766
C4 O8 Co1 92.69(14) . 1_655
C4 O7 Co1 88.08(15) . 1_655
O7 C4 O8 119.4(2) . .
O7 C4 C5 121.8(2) . .
O8 C4 C5 118.8(2) . .
O7 C4 Co1 62.21(12) . 1_655
O8 C4 Co1 57.20(12) . 1_655
C5 C4 Co1 174.48(17) . 1_655
C4 C5 C6 115.54(19) . .
C4 C5 C9 114.89(19) . .
C6 C5 C9 106.23(17) . .
C2 O4 Co3 133.27(15) . .
C2 O3 Co2 125.54(14) . .
O4 C2 O3 124.4(2) . .
O4 C2 C8 114.42(19) . .
O3 C2 C8 121.17(18) . .
O6 Co1 N1 95.98(7) 2_766 .
O6 Co1 O8 97.36(8) 2_766 1_455
N1 Co1 O8 152.74(8) . 1_455
O6 Co1 O2 100.37(6) 2_766 .
N1 Co1 O2 94.96(7) . .
O8 Co1 O2 105.83(7) 1_455 .
O6 Co1 O7 98.12(7) 2_766 1_455
N1 Co1 O7 94.82(7) . 1_455
O8 Co1 O7 59.81(7) 1_455 1_455
O2 Co1 O7 158.03(7) . 1_455
O6 Co1 O1 157.87(7) 2_766 .
N1 Co1 O1 91.56(8) . .
O8 Co1 O1 84.89(8) 1_455 .
O2 Co1 O1 58.16(6) . .
O7 Co1 O1 101.95(7) 1_455 .
O6 Co1 C4 99.64(7) 2_766 1_455
N1 Co1 C4 123.79(8) . 1_455
O8 Co1 C4 30.11(7) 1_455 1_455
O2 Co1 C4 133.70(7) . 1_455
O7 Co1 C4 29.72(7) 1_455 1_455
O1 Co1 C4 93.30(7) . 1_455
O3 Co2 O3 179.999(2) 2_766 .
O3 Co2 O5 89.41(6) 2_766 2_766
O3 Co2 O5 90.59(6) . 2_766
O3 Co2 O5 90.59(6) 2_766 .
O3 Co2 O5 89.41(6) . .
O5 Co2 O5 180.0 2_766 .
O3 Co2 O2 89.02(7) 2_766 2_766
O3 Co2 O2 90.98(7) . 2_766
O5 Co2 O2 95.67(6) 2_766 2_766
O5 Co2 O2 84.33(6) . 2_766
O3 Co2 O2 90.98(7) 2_766 .
O3 Co2 O2 89.02(7) . .
O5 Co2 O2 84.33(6) 2_766 .
O5 Co2 O2 95.67(6) . .
O2 Co2 O2 180.00(6) 2_766 .
O4 Co3 O4 180.0 . 2_656
O4 Co3 O10 92.88(8) . 2_656
O4 Co3 O10 87.12(8) 2_656 2_656
O4 Co3 O10 87.12(8) . .
O4 Co3 O10 92.88(8) 2_656 .
O10 Co3 O10 180.0 2_656 .
O4 Co3 O9 80.60(6) . .
O4 Co3 O9 99.40(6) 2_656 .
O10 Co3 O9 90.00(8) 2_656 .
O10 Co3 O9 90.00(8) . .
O4 Co3 O9 99.40(6) . 2_656
O4 Co3 O9 80.60(6) 2_656 2_656
O10 Co3 O9 90.00(8) 2_656 2_656
O10 Co3 O9 90.00(8) . 2_656
O9 Co3 O9 180.0 . 2_656
C3 O5 Co2 114.68(13) . .
C1 O2 Co2 137.46(15) . .
C1 O2 Co1 95.83(14) . .
Co2 O2 Co1 119.57(7) . .
O6 C3 O5 123.8(2) . .
O6 C3 C9 118.4(2) . .
O5 C3 C9 117.8(2) . .
C3 C9 C5 111.63(17) . .
C3 C9 C8 114.51(17) . .
C5 C9 C8 101.99(18) . .
C14 N1 C10 116.9(2) . .
C14 N1 Co1 121.94(16) . .
C10 N1 Co1 121.13(16) . .
C1 C7 C6 110.29(19) . .
C1 C7 C8 117.26(18) . .
C6 C7 C8 105.85(18) . .
C5 C6 C7 104.66(19) . .
C15 C15 C12 125.9(3) 2_775 .
C11 C12 C13 116.5(2) . .
C11 C12 C15 123.5(2) . .
C13 C12 C15 120.0(2) . .
C2 C8 C9 118.63(19) . .
C2 C8 C7 113.90(18) . .
C9 C8 C7 107.08(17) . .
C1 O1 Co1 87.12(15) . .
C10 C11 C12 120.4(2) . .
N1 C14 C13 123.5(3) . .
C14 C13 C12 120.0(3) . .
N1 C10 C11 122.6(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 O1 1.239(3) .
C1 O2 1.271(3) .
C1 C7 1.523(3) .
O6 C3 1.258(3) .
O6 Co1 2.0417(16) 2_766
O8 C4 1.256(3) .
O8 Co1 2.1047(17) 1_655
O7 C4 1.240(3) .
O7 Co1 2.2139(18) 1_655
C4 C5 1.509(3) .
C4 Co1 2.501(2) 1_655
C5 C6 1.521(3) .
C5 C9 1.548(3) .
O4 C2 1.249(3) .
O4 Co3 2.0714(16) .
O3 C2 1.256(3) .
O3 Co2 2.0700(15) .
C2 C8 1.533(3) .
Co1 O6 2.0417(16) 2_766
Co1 N1 2.0745(18) .
Co1 O8 2.1047(17) 1_455
Co1 O2 2.1114(16) .
Co1 O7 2.2140(18) 1_455
Co1 O1 2.3175(19) .
Co1 C4 2.501(2) 1_455
Co2 O3 2.0700(15) 2_766
Co2 O5 2.0709(15) 2_766
Co2 O5 2.0710(15) .
Co2 O2 2.0917(16) 2_766
Co2 O2 2.0917(16) .
Co3 O4 2.0714(16) 2_656
Co3 O10 2.082(2) 2_656
Co3 O10 2.082(2) .
Co3 O9 2.1405(16) .
Co3 O9 2.1405(16) 2_656
O5 C3 1.271(3) .
C3 C9 1.518(3) .
C9 C8 1.558(3) .
N1 C14 1.328(3) .
N1 C10 1.346(3) .
C7 C6 1.545(3) .
C7 C8 1.573(3) .
C15 C15 1.323(5) 2_775
C15 C12 1.467(3) .
C12 C11 1.382(4) .
C12 C13 1.383(4) .
C11 C10 1.379(3) .
C14 C13 1.379(4) .
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.034 0.466 1.000 172 52 ' '
