#------------------------------------------------------------------------------
#$Date: 2019-11-23 03:54:30 +0200 (Sat, 23 Nov 2019) $
#$Revision: 232056 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/69/4346903.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_4346903
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            'C14 H12 Co2 N O10'
_chemical_formula_weight         472.11
_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                88.0440(10)
_cell_angle_beta                 78.6410(10)
_cell_angle_gamma                65.8860(10)
_cell_formula_units_Z            2
_cell_length_a                   9.0477(2)
_cell_length_b                   9.7882(2)
_cell_length_c                   11.3856(3)
_cell_measurement_reflns_used    3514
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.40
_cell_measurement_theta_min      2.28
_cell_volume                     901.09(4)
_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 0.989
_diffrn_measured_fraction_theta_max 0.989
_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  0.0978
_diffrn_reflns_av_sigmaI/netI    0.0781
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            6785
_diffrn_reflns_theta_full        28.40
_diffrn_reflns_theta_max         28.40
_diffrn_reflns_theta_min         1.83
_exptl_absorpt_coefficient_mu    1.894
_exptl_absorpt_correction_T_max  0.827
_exptl_absorpt_correction_T_min  0.827
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.740
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             474
_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         0.594
_refine_diff_density_min         -0.754
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     249
_refine_ls_number_reflns         4471
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_gt           0.0425
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0568P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1096
_refine_ls_wR_factor_ref         0.1122
_reflns_number_gt                3672
_reflns_number_total             4471
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5b02340_si_002.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      p-1
_cod_database_code               4346903
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
O8 O 0.2900(2) 0.0526(2) 0.4289(2) 0.0405(5) Uani 1 1 d .
O7 O 0.1074(2) 0.2703(2) 0.51756(17) 0.0274(4) Uani 1 1 d .
C9 C 0.1585(3) 0.1682(3) 0.4371(2) 0.0235(5) Uani 1 1 d .
O5 O -0.4158(2) 0.5091(2) 0.20887(19) 0.0363(5) Uani 1 1 d .
O6 O -0.4663(2) 0.3535(2) 0.3337(2) 0.0349(5) Uani 1 1 d .
C7 C -0.3635(3) 0.3924(3) 0.2656(2) 0.0234(5) Uani 1 1 d .
O4 O -0.2801(2) 0.3270(2) 0.57075(17) 0.0294(4) Uani 1 1 d .
Co1 Co 0.33263(4) 0.53523(4) 0.28218(3) 0.02301(11) Uani 1 1 d .
Co2 Co 0.0000 0.5000 0.5000 0.01938(12) Uani 1 2 d S
Co3 Co 0.5000 0.0000 0.5000 0.02507(13) Uani 1 2 d S
O3 O -0.2019(2) 0.4831(2) 0.45286(16) 0.0235(4) Uani 1 1 d .
O1 O 0.1385(2) 0.4640(2) 0.32715(16) 0.0274(4) Uani 1 1 d .
C6 C -0.2094(3) 0.3571(3) 0.4726(2) 0.0214(5) Uani 1 1 d .
O9 O 0.5558(3) -0.2167(2) 0.4213(2) 0.0364(5) Uani 1 1 d .
H9 H 0.6395 -0.2790 0.4406 0.055 Uiso 1 1 calc R
C4 C -0.1819(3) 0.2947(3) 0.2525(2) 0.0232(5) Uani 1 1 d .
H4 H -0.1582 0.2067 0.2014 0.028 Uiso 1 1 calc R
C2 C 0.1023(3) 0.2685(3) 0.2266(2) 0.0239(5) Uani 1 1 d .
H2 H 0.1688 0.1959 0.1593 0.029 Uiso 1 1 calc R
N1 N 0.2111(3) 0.7045(3) 0.1760(2) 0.0297(5) Uani 1 1 d .
C1 C 0.0630(3) 0.1778(3) 0.3374(2) 0.0224(5) Uani 1 1 d .
H1 H 0.1022 0.0746 0.3055 0.027 Uiso 1 1 calc R
O2 O 0.3165(2) 0.3571(3) 0.16586(19) 0.0374(5) Uani 1 1 d .
C8 C 0.1923(3) 0.3662(3) 0.2410(2) 0.0237(5) Uani 1 1 d .
C5 C -0.1288(3) 0.2360(3) 0.3727(2) 0.0215(5) Uani 1 1 d .
H5 H -0.1586 0.1517 0.3953 0.026 Uiso 1 1 calc R
C12 C 0.0443(3) 0.9381(3) 0.0369(2) 0.0267(5) Uani 1 1 d .
C3 C -0.0662(3) 0.3658(3) 0.1935(2) 0.0272(5) Uani 1 1 d .
H3A H -0.1060 0.4686 0.2239 0.033 Uiso 1 1 calc R
H3B H -0.0570 0.3648 0.1071 0.033 Uiso 1 1 calc R
O10 O 0.6040(3) 0.0567(3) 0.3366(2) 0.0457(6) Uani 1 1 d .
H10 H 0.5794 0.1472 0.3381 0.069 Uiso 1 1 calc R
C13 C -0.0389(4) 0.8857(4) 0.1275(3) 0.0545(11) Uani 1 1 d .
H13 H -0.1538 0.9273 0.1440 0.065 Uiso 1 1 calc R
C11 C 0.2152(4) 0.8710(5) 0.0175(4) 0.0520(10) Uani 1 1 d .
H11 H 0.2780 0.9036 -0.0420 0.062 Uiso 1 1 calc R
C10 C 0.2918(4) 0.7550(5) 0.0876(4) 0.0535(11) Uani 1 1 d .
H10A H 0.4067 0.7098 0.0718 0.064 Uiso 1 1 calc R
C14 C 0.0473(4) 0.7705(4) 0.1954(3) 0.0530(11) Uani 1 1 d .
H14 H -0.0127 0.7383 0.2573 0.064 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
C9 O8 Co3 132.7(2) . .
C9 O7 Co2 127.98(17) . .
O8 C9 O7 124.3(2) . .
O8 C9 C1 114.2(2) . .
O7 C9 C1 121.5(2) . .
C7 O5 Co1 89.06(15) . 1_455
C7 O6 Co1 91.10(15) . 1_455
O5 C7 O6 119.1(2) . .
O5 C7 C4 122.0(2) . .
O6 C7 C4 118.9(2) . .
O5 C7 Co1 60.73(13) . 1_455
O6 C7 Co1 58.49(13) . 1_455
C4 C7 Co1 175.18(19) . 1_455
C6 O4 Co1 117.81(17) . 2_566
O4 Co1 N1 95.49(9) 2_566 .
O4 Co1 O1 99.67(8) 2_566 .
N1 Co1 O1 94.64(9) . .
O4 Co1 O6 96.13(9) 2_566 1_655
N1 Co1 O6 157.45(9) . 1_655
O1 Co1 O6 102.36(8) . 1_655
O4 Co1 O5 99.65(9) 2_566 1_655
N1 Co1 O5 98.38(8) . 1_655
O1 Co1 O5 155.49(9) . 1_655
O6 Co1 O5 60.60(7) 1_655 1_655
O4 Co1 O2 157.58(8) 2_566 .
N1 Co1 O2 91.50(9) . .
O1 Co1 O2 58.46(7) . .
O6 Co1 O2 85.02(8) 1_655 .
O5 Co1 O2 100.36(8) 1_655 .
O4 Co1 C7 100.03(8) 2_566 1_655
N1 Co1 C7 127.99(9) . 1_655
O1 Co1 C7 130.33(8) . 1_655
O6 Co1 C7 30.41(8) 1_655 1_655
O5 Co1 C7 30.21(8) 1_655 1_655
O2 Co1 C7 92.26(8) . 1_655
O1 Co2 O1 180.0 2_566 .
O1 Co2 O3 84.61(7) 2_566 .
O1 Co2 O3 95.39(7) . .
O1 Co2 O3 95.39(7) 2_566 2_566
O1 Co2 O3 84.61(7) . 2_566
O3 Co2 O3 179.999(1) . 2_566
O1 Co2 O7 91.97(8) 2_566 .
O1 Co2 O7 88.03(8) . .
O3 Co2 O7 90.43(7) . .
O3 Co2 O7 89.57(7) 2_566 .
O1 Co2 O7 88.03(8) 2_566 2_566
O1 Co2 O7 91.97(8) . 2_566
O3 Co2 O7 89.57(7) . 2_566
O3 Co2 O7 90.43(7) 2_566 2_566
O7 Co2 O7 180.00(5) . 2_566
O8 Co3 O8 180.0 . 2_656
O8 Co3 O10 86.41(10) . .
O8 Co3 O10 93.59(10) 2_656 .
O8 Co3 O10 93.59(10) . 2_656
O8 Co3 O10 86.41(10) 2_656 2_656
O10 Co3 O10 179.999(1) . 2_656
O8 Co3 O9 80.67(8) . .
O8 Co3 O9 99.33(8) 2_656 .
O10 Co3 O9 89.59(9) . .
O10 Co3 O9 90.41(9) 2_656 .
O8 Co3 O9 99.33(8) . 2_656
O8 Co3 O9 80.67(8) 2_656 2_656
O10 Co3 O9 90.41(9) . 2_656
O10 Co3 O9 89.59(9) 2_656 2_656
O9 Co3 O9 180.0 . 2_656
C6 O3 Co2 114.19(14) . .
C8 O1 Co2 138.39(18) . .
C8 O1 Co1 95.42(15) . .
Co2 O1 Co1 120.52(9) . .
O4 C6 O3 123.9(2) . .
O4 C6 C5 118.0(2) . .
O3 C6 C5 118.1(2) . .
C7 C4 C3 115.4(2) . .
C7 C4 C5 113.9(2) . .
C3 C4 C5 106.3(2) . .
C8 C2 C3 109.6(2) . .
C8 C2 C1 118.3(2) . .
C3 C2 C1 105.75(19) . .
C10 N1 C14 116.5(2) . .
C10 N1 Co1 122.26(19) . .
C14 N1 Co1 121.2(2) . .
C9 C1 C5 118.1(2) . .
C9 C1 C2 114.4(2) . .
C5 C1 C2 106.92(19) . .
C8 O2 Co1 87.66(17) . .
O2 C8 O1 118.2(3) . .
O2 C8 C2 120.9(2) . .
O1 C8 C2 120.8(2) . .
C6 C5 C4 111.8(2) . .
C6 C5 C1 114.5(2) . .
C4 C5 C1 101.9(2) . .
C13 C12 C11 116.7(2) . .
C13 C12 C12 121.8(3) . 2_575
C11 C12 C12 121.5(3) . 2_575
C4 C3 C2 105.1(2) . .
C12 C13 C14 120.4(3) . .
C12 C11 C10 119.4(3) . .
N1 C10 C11 124.0(3) . .
N1 C14 C13 123.1(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
O8 C9 1.252(3) .
O8 Co3 2.0764(19) .
O7 C9 1.253(3) .
O7 Co2 2.0734(18) .
C9 C1 1.536(3) .
O5 C7 1.255(3) .
O5 Co1 2.176(2) 1_455
O6 C7 1.263(3) .
O6 Co1 2.1266(19) 1_455
C7 C4 1.506(3) .
C7 Co1 2.494(2) 1_455
O4 C6 1.262(3) .
O4 Co1 2.041(2) 2_566
Co1 O4 2.041(2) 2_566
Co1 N1 2.077(2) .
Co1 O1 2.1112(18) .
Co1 O6 2.1266(19) 1_655
Co1 O5 2.176(2) 1_655
Co1 O2 2.293(2) .
Co1 C7 2.494(2) 1_655
Co2 O1 2.0693(18) 2_566
Co2 O1 2.0693(18) .
Co2 O3 2.0719(17) .
Co2 O3 2.0719(17) 2_566
Co2 O7 2.0735(18) 2_566
Co3 O8 2.0764(19) 2_656
Co3 O10 2.079(2) .
Co3 O10 2.079(2) 2_656
Co3 O9 2.152(2) .
Co3 O9 2.152(2) 2_656
O3 C6 1.273(3) .
O1 C8 1.269(3) .
C6 C5 1.513(4) .
C4 C3 1.522(4) .
C4 C5 1.554(3) .
C2 C8 1.518(4) .
C2 C3 1.546(3) .
C2 C1 1.584(4) .
N1 C10 1.326(4) .
N1 C14 1.327(4) .
C1 C5 1.560(3) .
O2 C8 1.244(3) .
C12 C13 1.366(4) .
C12 C11 1.384(4) .
C12 C12 1.490(5) 2_575
C13 C14 1.391(4) .
C11 C10 1.386(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 0.500 0.000 1.000 104 32 ' '
