#------------------------------------------------------------------------------
#$Date: 2019-10-30 04:59:34 +0200 (Wed, 30 Oct 2019) $
#$Revision: 220526 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/14/7701452.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_7701452
loop_
_publ_author_name
'Gao, Xiaoxia'
'Xu, Tingting'
'Jiang, Zhenzhen'
'Yu, Honggui'
'Wang, Yingjie'
'He, Yabing'
_publ_section_title
;
 Rational construction and remarkable gas adsorption properties of a
 HKUST-1-like tbo-type MOF based on a tetraisophthalate linker
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C9DT03716K
_journal_year                    2019
_chemical_formula_moiety         '[C40H26Cu4O20].4DMF.2H2O'
_chemical_formula_sum            'C52 H58 Cu4 N4 O26'
_chemical_formula_weight         1409.18
_space_group_crystal_system      tetragonal
_space_group_IT_number           139
_space_group_name_Hall           '-I 4 2'
_space_group_name_H-M_alt        'I 4/m m m'
_symmetry_space_group_name_Hall  '-I 4 2'
_symmetry_space_group_name_H-M   'I 4/m m m'
_atom_sites_solution_hydrogens   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2019-10-06 deposited with the CCDC.    2019-10-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.0416(10)
_cell_length_b                   19.0416(10)
_cell_length_c                   18.6430(9)
_cell_measurement_reflns_used    1655
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.36
_cell_measurement_theta_min      2.629
_cell_volume                     6759.6(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 VENTURE PHOTON II'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0658
_diffrn_reflns_av_unetI/netI     0.0484
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            9413
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         2.185
_exptl_absorpt_coefficient_mu    1.318
_exptl_absorpt_correction_T_max  0.877
_exptl_absorpt_correction_T_min  0.827
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.385
_exptl_crystal_description       block
_exptl_crystal_F_000             2168
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.861
_refine_diff_density_min         -0.631
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     86
_refine_ls_number_reflns         1979
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0775
_refine_ls_R_factor_gt           0.0488
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0810P)²+4.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1394
_refine_ls_wR_factor_ref         0.1553
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1333
_reflns_number_total             1979
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9dt03716k2.cif
_cod_data_source_block           ZJNU-10
_cod_original_cell_volume        6759.6(8)
_cod_database_code               7701452
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.797
_shelx_estimated_absorpt_t_max   0.879
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'-x, y, -z'
'x, -y, -z'
'y, x, -z'
'-y, -x, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'y+1/2, x+1/2, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'y, -x, -z'
'-y, x, -z'
'x, -y, z'
'-x, y, z'
'-y, -x, z'
'y, x, z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, x+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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Cu1 Cu 0.71665(2) 0.71665(2) 0.30247(3) 0.0361(3) Uani 1 2 d S T P
O1 O 0.76724(15) 0.86960(14) 0.25329(14) 0.0488(7) Uani 1 1 d . . .
O2 O 0.70917(14) 0.81317(14) 0.33987(14) 0.0475(7) Uani 1 1 d . . .
O3 O 0.66548(19) 0.66548(19) 0.3935(3) 0.0819(16) Uani 1 2 d S T P
C1 C 0.7305(2) 0.8672(2) 0.3093(2) 0.0396(9) Uani 1 1 d . . .
C2 C 0.7095(2) 0.9370(2) 0.34183(19) 0.0387(9) Uani 1 1 d . U .
C3 C 0.7339(3) 1.0000 0.3145(3) 0.0421(13) Uani 1 2 d S TU P
H3 H 0.7689 1.0000 0.2781 0.050 Uiso 1 2 d R U P
C4 C 0.65694(19) 0.9374(2) 0.39395(18) 0.0372(8) Uani 1 1 d . U .
H4 H 0.6392 0.8944 0.4122 0.045 Uiso 1 1 d R U .
C5 C 0.6298(3) 1.0000 0.4194(2) 0.0321(11) Uani 1 2 d S TU P
C6 C 0.5628(3) 1.0000 0.4623(2) 0.0287(10) Uani 1 2 d S TU P
C7 C 0.5000 1.0000 0.4251(3) 0.0267(13) Uani 1 4 d DS TU P
C8 C 0.5000 1.0090(14) 0.3432(4) 0.034(4) Uani 0.5 2 d DS TU P
H8A H 0.4526 1.0075 0.3257 0.051 Uiso 0.25 1 d R U P
H8B H 0.5206 1.0535 0.3315 0.051 Uiso 0.25 1 d R U P
H8C H 0.5267 0.9720 0.3212 0.051 Uiso 0.25 1 d R U P
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'
Cu Cu 0.3201 1.2651 '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
O2 Cu1 O2 90.56(16) 24 .
O2 Cu1 O1 167.55(11) 24 16_665
O2 Cu1 O1 88.92(12) . 16_665
O2 Cu1 O1 88.93(12) 24 25_665
O2 Cu1 O1 167.55(11) . 25_665
O1 Cu1 O1 88.91(17) 16_665 25_665
O2 Cu1 O3 96.24(13) 24 .
O2 Cu1 O3 96.24(13) . .
O1 Cu1 O3 96.18(13) 16_665 .
O1 Cu1 O3 96.18(13) 25_665 .
O2 Cu1 Cu1 81.33(8) 24 25_665
O2 Cu1 Cu1 81.33(8) . 25_665
O1 Cu1 Cu1 86.30(8) 16_665 25_665
O1 Cu1 Cu1 86.30(8) 25_665 25_665
O3 Cu1 Cu1 176.51(16) . 25_665
C1 O1 Cu1 119.6(3) . 25_665
C1 O2 Cu1 125.8(2) . .
O2 C1 O1 126.3(4) . .
O2 C1 C2 117.1(3) . .
O1 C1 C2 116.6(3) . .
C3 C2 C4 119.5(4) . .
C3 C2 C1 121.6(3) . .
C4 C2 C1 118.3(3) . .
C2 C3 C2 120.1(5) 21_575 .
C2 C3 H3 119.9 21_575 .
C2 C3 H3 119.9 . .
C5 C4 C2 120.8(4) . .
C5 C4 H4 119.2 . .
C2 C4 H4 119.9 . .
C4 C5 C4 119.0(5) . 21_575
C4 C5 C6 120.0(2) . .
C4 C5 C6 120.0(2) 21_575 .
C6 C6 C7 120.1(3) 18_556 .
C6 C6 C5 122.1(2) 18_556 .
C7 C6 C5 117.8(4) . .
C6 C7 C6 119.9(5) . 2_675
C6 C7 C8 119.9(3) . 2_675
C6 C7 C8 119.9(3) 2_675 2_675
C6 C7 C8 119.9(3) . .
C6 C7 C8 119.9(3) 2_675 .
C8 C7 C8 13(2) 2_675 .
C8 C8 C7 83.6(10) 2_675 .
C8 C8 H8A 88.4 2_675 .
C7 C8 H8A 109.5 . .
C8 C8 H8B 152.1 2_675 .
C7 C8 H8B 108.9 . .
H8A C8 H8B 109.5 . .
C8 C8 H8C 42.9 2_675 .
C7 C8 H8C 110.0 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O2 1.971(3) 24
Cu1 O2 1.971(3) .
Cu1 O1 1.968(3) 16_665
Cu1 O1 1.968(3) 25_665
Cu1 O3 2.186(4) .
Cu1 Cu1 2.6557(12) 25_665
O1 C1 1.258(4) .
O1 Cu1 1.968(3) 25_665
O2 C1 1.244(5) .
C1 C2 1.515(5) .
C2 C3 1.384(5) .
C2 C4 1.394(5) .
C3 C2 1.384(5) 21_575
C3 H3 0.9499 .
C4 C5 1.383(4) .
C4 H4 0.9499 .
C5 C4 1.383(4) 21_575
C5 C6 1.504(6) .
C6 C6 1.406(8) 18_556
C6 C7 1.383(5) .
C7 C6 1.383(5) 2_675
C7 C8 1.538(9) 2_675
C7 C8 1.538(9) .
C8 C8 0.34(5) 2_675
C8 H8A 0.9599 .
C8 H8B 0.9599 .
C8 H8C 0.9600 .
