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#$Date: 2019-11-17 10:19:48 +0200 (Sun, 17 Nov 2019) $
#$Revision: 229313 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/65/7046547.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_7046547
loop_
_publ_author_name
'He, Minghui'
'Wang, Yao'
'Gao, Xiaoxia'
'Li, Saidan'
'He, Yabing'
_publ_section_title
;
 Three ligand-originated MOF isomers: the positional effect of the methyl
 group on structures and selective
 C₂H₂/CH₄ and
 CO₂/CH₄ adsorption properties.
;
_journal_issue                   27
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8983
_journal_page_last               8991
_journal_paper_doi               10.1039/c8dt01017j
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C23 H16 Cu2 O10 [5DMF]'
_chemical_formula_sum            'C38 H51 Cu2 N5 O15'
_chemical_formula_weight         944.94
_space_group_crystal_system      hexagonal
_space_group_IT_number           194
_space_group_name_Hall           '-P 6c 2c'
_space_group_name_H-M_alt        'P 63/m m c'
_symmetry_space_group_name_Hall  '-P 6c 2c'
_symmetry_space_group_name_H-M   'P 63/m m c'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-04-09 deposited with the CCDC.
2018-06-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   18.4882(4)
_cell_length_b                   18.4882(4)
_cell_length_c                   23.4316(11)
_cell_measurement_reflns_used    40995
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      0.996
_cell_volume                     6936.2(4)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0634
_diffrn_reflns_av_unetI/netI     0.0345
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            40995
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.490
_diffrn_reflns_theta_min         1.272
_exptl_absorpt_coefficient_mu    0.987
_exptl_absorpt_correction_T_max  0.9112
_exptl_absorpt_correction_T_min  0.8947
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.357
_exptl_crystal_description       block
_exptl_crystal_F_000             2952
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.100
_platon_squeeze_details
' The residual electron density of 736.2 electrons per unit cell was tentatively assigned to 5 DMF, which was mainly established according to the elemental analysis'
_refine_diff_density_max         0.366
_refine_diff_density_min         -0.345
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     96
_refine_ls_number_reflns         2968
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0885
_refine_ls_R_factor_gt           0.0532
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0950P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1566
_refine_ls_wR_factor_ref         0.1670
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1768
_reflns_number_total             2968
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8dt01017j2.cif
_cod_data_source_block           ZJNU-83
_cod_depositor_comments
'Adding full bibliography for 7046545--7046547.cif.'
_cod_database_code               7046547
_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   0.891
_shelx_estimated_absorpt_t_max   0.908
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x-y, x, z+1/2'
'-y, x-y, z'
'-x, -y, z+1/2'
'-x+y, -x, z'
'y, -x+y, z+1/2'
'-y, -x, -z+1/2'
'x-y, -y, -z'
'x, x-y, -z+1/2'
'y, x, -z'
'-x+y, y, -z+1/2'
'-x, -x+y, -z'
'-x, -y, -z'
'-x+y, -x, -z-1/2'
'y, -x+y, -z'
'x, y, -z-1/2'
'x-y, x, -z'
'-y, x-y, -z-1/2'
'y, x, z-1/2'
'-x+y, y, z'
'-x, -x+y, z-1/2'
'-y, -x, z'
'x-y, -y, z-1/2'
'x, 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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.52389(2) 0.47611(2) 0.04620(2) 0.0559(2) Uani 1 2 d S T P . .
O1 O 0.41031(13) 0.43910(14) 0.07316(10) 0.0707(6) Uani 1 1 d . . . . .
O2 O 0.37130(12) 0.48138(14) -0.00506(10) 0.0713(6) Uani 1 1 d . . . . .
O1W O 0.56130(14) 0.43870(14) 0.1245(2) 0.1365(17) Uani 1 2 d S T P . .
H1WA H 0.6117 0.4498 0.1215 0.164 Uiso 1 1 d R U . . .
C1 C 0.35961(19) 0.45024(19) 0.04393(15) 0.0604(8) Uani 1 1 d . . . . .
C2 C 0.27500(17) 0.42066(18) 0.06973(13) 0.0560(7) Uani 1 1 d . . . . .
C3 C 0.25146(18) 0.37325(19) 0.11871(13) 0.0637(8) Uani 1 1 d . . . . .
H3 H 0.2886 0.3580 0.1357 0.076 Uiso 1 1 calc R U . . .
C4 C 0.22146(13) 0.4429(3) 0.04431(17) 0.0582(10) Uani 1 2 d S T P . .
H4 H 0.2367 0.4734 0.0095 0.070 Uiso 1 2 calc R U P . .
C5 C 0.17353(14) 0.3471(3) 0.14399(18) 0.0643(11) Uani 1 2 d S T P . .
C6 C 0.16903(19) 0.3381(4) 0.2500 0.0590(14) Uani 1 4 d S T P . .
H6 H 0.1987 0.3974 0.2500 0.071 Uiso 1 4 calc R U P . .
C7 C 0.14882(13) 0.2976(3) 0.1992(2) 0.0651(11) Uani 1 2 d S T P . .
C8 C 0.1063(2) 0.2126(4) 0.1991(3) 0.167(4) Uani 1 2 d DS T P . .
C9 C 0.0834(4) 0.1667(7) 0.1440(5) 0.220(11) Uani 0.5 2 d DS T P . .
H8A H 0.0908 0.1820 0.1644 0.264 Uiso 0.5 2 d R U P A 2
H9A H 0.0538 0.1079 0.1504 0.264 Uiso 0.5 2 d R U P . .
H9B H 0.0486 0.1820 0.1228 0.264 Uiso 0.5 1 d R U P . .
C10 C 0.0857(3) 0.1713(6) 0.2500 0.230(9) Uani 1 4 d S T P . .
H10A H 0.0560 0.1120 0.2500 0.276 Uiso 1 4 calc 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 0.0030 0.0020 '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 0.3200 1.2650 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0110 0.0060 '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'
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 88.94(13) 10 13_665
O2 Cu1 O1 89.04(10) 10 .
O2 Cu1 O1 168.11(9) 13_665 .
O2 Cu1 O1 168.12(9) 10 22_665
O2 Cu1 O1 89.04(10) 13_665 22_665
O1 Cu1 O1 90.53(14) . 22_665
O2 Cu1 O1W 97.75(11) 10 .
O2 Cu1 O1W 97.75(11) 13_665 .
O1 Cu1 O1W 94.13(12) . .
O1 Cu1 O1W 94.12(12) 22_665 .
O2 Cu1 Cu1 83.75(7) 10 13_665
O2 Cu1 Cu1 83.75(7) 13_665 13_665
O1 Cu1 Cu1 84.38(7) . 13_665
O1 Cu1 Cu1 84.38(7) 22_665 13_665
O1W Cu1 Cu1 177.87(14) . 13_665
C1 O1 Cu1 121.6(2) . .
C1 O2 Cu1 123.22(19) . 13_665
Cu1 O1W H1WA 109.6 . .
O1 C1 O2 127.0(3) . .
O1 C1 C2 116.5(3) . .
O2 C1 C2 116.4(3) . .
C3 C2 C4 120.2(3) . .
C3 C2 C1 120.5(3) . .
C4 C2 C1 119.2(3) . .
C2 C3 C5 121.1(3) . .
C2 C3 H3 119.5 . .
C5 C3 H3 119.5 . .
C2 C4 C2 119.7(4) . 20
C2 C4 H4 120.1 . .
C2 C4 H4 120.1 20 .
C3 C5 C3 117.6(4) . 20
C3 C5 C7 121.1(2) . .
C3 C5 C7 121.1(2) 20 .
C7 C6 C7 123.0(6) 16_556 .
C7 C6 H6 118.5 16_556 .
C7 C6 H6 118.5 . .
C6 C7 C8 118.5(5) . .
C6 C7 C5 120.0(4) . .
C8 C7 C5 121.4(5) . .
C10 C8 C7 119.0(6) . .
C10 C8 C9 121.4(7) . .
C7 C8 C9 119.6(7) . .
C10 C8 H8A 119.9 . .
C7 C8 H8A 121.1 . .
C9 C8 H8A 1.5 . .
C8 C9 H8A 2.6 . .
C8 C9 H9A 110.5 . .
H8A C9 H9A 108.0 . .
C8 C9 H9B 109.0 . .
H8A C9 H9B 109.9 . .
H9A C9 H9B 109.2 . .
C8 C10 C8 122.0(8) 16_556 .
C8 C10 H10A 119.0 16_556 .
C8 C10 H10A 119.0 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O2 1.944(2) 10
Cu1 O2 1.944(2) 13_665
Cu1 O1 1.960(2) .
Cu1 O1 1.960(2) 22_665
Cu1 O1W 2.192(4) .
Cu1 Cu1 2.6512(10) 13_665
O1 C1 1.258(3) .
O2 C1 1.254(4) .
O2 Cu1 1.944(2) 13_665
O1W H1WA 0.8514 .
C1 C2 1.502(4) .
C2 C3 1.376(4) .
C2 C4 1.383(3) .
C3 C5 1.401(4) .
C3 H3 0.9500 .
C4 C2 1.383(3) 20
C4 H4 0.9500 .
C5 C3 1.401(4) 20
C5 C7 1.516(6) .
C6 C7 1.355(5) 16_556
C6 C7 1.355(5) .
C6 H6 0.9500 .
C7 C8 1.362(7) .
C8 C10 1.363(7) .
C8 C9 1.487(11) .
C8 H8A 0.9503 .
C9 H8A 0.5371 .
C9 H9A 0.9540 .
C9 H9B 0.9588 .
C10 C8 1.363(7) 16_556
C10 H10A 0.9500 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
Cu1 O1 C1 O2 3.2(5) . .
Cu1 O1 C1 C2 -178.80(18) . .
Cu1 O2 C1 O1 -2.3(5) 13_665 .
Cu1 O2 C1 C2 179.78(18) 13_665 .
O1 C1 C2 C3 -9.2(4) . .
O2 C1 C2 C3 169.0(3) . .
O1 C1 C2 C4 169.6(3) . .
O2 C1 C2 C4 -12.2(4) . .
C4 C2 C3 C5 -0.4(5) . .
C1 C2 C3 C5 178.4(3) . .
C3 C2 C4 C2 3.0(6) . 20
C1 C2 C4 C2 -175.8(2) . 20
C2 C3 C5 C3 -2.1(6) . 20
C2 C3 C5 C7 -177.6(3) . .
C7 C6 C7 C8 -0.001(3) 16_556 .
C7 C6 C7 C5 180.000(2) 16_556 .
C3 C5 C7 C6 87.7(3) . .
C3 C5 C7 C6 -87.7(3) 20 .
C3 C5 C7 C8 -92.3(3) . .
C3 C5 C7 C8 92.3(3) 20 .
C6 C7 C8 C10 0.000(1) . .
C5 C7 C8 C10 180.000(1) . .
C6 C7 C8 C9 179.999(1) . .
C5 C7 C8 C9 -0.002(2) . .
C9 C8 C10 C8 180.002(3) . 16_556
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
1 -0.038 -0.027 -0.002 4236.3 736.2
