#------------------------------------------------------------------------------
#$Date: 2019-11-17 09:19:48 +0100 (Sun 17 de Nov de 2019) $
#$Revision: 229313 $
#$URL: svn://www.crystallography.net/cod/cif/7/04/65/7046546.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_7046546
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.H2O]'
_chemical_formula_sum            'C38 H53 Cu2 N5 O16'
_chemical_formula_weight         962.93
_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                   18.4999(3)
_cell_length_b                   18.4999(3)
_cell_length_c                   24.0168(3)
_cell_measurement_reflns_used    25879
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      74.01
_cell_measurement_theta_min      0.966
_cell_volume                     7118.44(19)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD area detector'
_diffrn_measurement_method       multi-scan
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0717
_diffrn_reflns_av_unetI/netI     0.0538
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            25879
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.090
_diffrn_reflns_theta_min         2.758
_exptl_absorpt_coefficient_mu    1.696
_exptl_absorpt_correction_T_max  0.9478
_exptl_absorpt_correction_T_min  0.7735
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.348
_exptl_crystal_description       needle
_exptl_crystal_F_000             3012
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.040
_platon_squeeze_details
' The residual electron density of 1110.2 electrons per unit cell was tentatively assigned to 5 DMF and 1 H2O, which was mainly established according to the elemental analysis'
_refine_diff_density_max         0.449
_refine_diff_density_min         -0.335
_refine_diff_density_rms         0.070
_refine_ls_extinction_coef       0.00016(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     95
_refine_ls_number_reflns         2701
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0537
_refine_ls_R_factor_gt           0.0398
_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)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1313
_refine_ls_wR_factor_ref         0.1368
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2257
_reflns_number_total             2701
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8dt01017j2.cif
_cod_data_source_block           ZJNU-82
_cod_depositor_comments
'Adding full bibliography for 7046545--7046547.cif.'
_cod_original_cell_volume        7118.5(2)
_cod_database_code               7046546
_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   0.728
_shelx_estimated_absorpt_t_max   0.935
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'-y, -x, -z+1/2'
'-x+y, y, -z+1/2'
'x, x-y, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z-1/2'
'-y, x-y, -z-1/2'
'-x+y, -x, -z-1/2'
'-y, -x, z'
'-x+y, y, z'
'x, x-y, z'
'y, x, z-1/2'
'x-y, -y, z-1/2'
'-x, -x+y, 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 0.04826(2) 0.52413(2) 0.45518(2) 0.04446(18) Uani 1 2 d S T P
O1 O 0.11015(7) 0.62961(8) 0.49626(5) 0.0585(3) Uani 1 1 d . . .
O2 O 0.02799(8) 0.58894(9) 0.57163(5) 0.0599(4) Uani 1 1 d . . .
O1W O 0.12647(18) 0.56324(9) 0.38209(10) 0.0972(8) Uani 1 2 d S T P
H1WA H 0.1077 0.5229 0.3589 0.117 Uiso 1 1 d R U .
C1 C 0.08993(11) 0.64139(13) 0.54359(6) 0.0517(4) Uani 1 1 d . . .
C2 C 0.14548(10) 0.72496(11) 0.56966(7) 0.0508(4) Uani 1 1 d . . .
C3 C 0.22101(8) 0.77899(8) 0.54428(9) 0.0507(6) Uani 1 2 d S T P
H3A H 0.2353 0.7647 0.5106 0.061 Uiso 1 2 calc R U P
C4 C 0.12380(11) 0.74627(12) 0.62036(7) 0.0542(4) Uani 1 1 d . . .
H4A H 0.0736 0.7093 0.6375 0.065 Uiso 1 1 calc R U .
C5 C 0.17737(9) 0.82263(9) 0.64511(9) 0.0527(5) Uani 1 2 d S T P
C6 C 0.15456(9) 0.84544(9) 0.69979(10) 0.0557(6) Uani 1 2 d S T P
C9 C 0.17641(13) 0.82359(13) 0.7500 0.0568(8) Uani 1 4 d S T P
C7 C 0.11268(12) 0.88732(12) 0.70022(13) 0.1206(18) Uani 1 2 d S T P
H7A H 0.0982 0.9018 0.6666 0.145 Uiso 1 2 calc R U P
C8 C 0.09041(19) 0.90959(19) 0.7500 0.189(5) Uani 1 4 d S T P
H8A H 0.0614 0.9386 0.7500 0.227 Uiso 1 4 calc R U P
C10 C 0.22242(19) 0.77758(19) 0.7500 0.156(4) Uani 1 4 d S T P
H10B H 0.2324 0.7676 0.7877 0.233 Uiso 0.5 2 d R U P
H10A H 0.1900 0.7249 0.7312 0.233 Uiso 0.5 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 0.0181 0.0091 '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 -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 '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 90.24(9) 13_566 9_556
O2 Cu1 O1 167.91(5) 13_566 .
O2 Cu1 O1 89.03(6) 9_556 .
O2 Cu1 O1 89.03(6) 13_566 21_565
O2 Cu1 O1 167.91(5) 9_556 21_565
O1 Cu1 O1 89.17(8) . 21_565
O2 Cu1 O1W 95.45(7) 13_566 .
O2 Cu1 O1W 95.45(7) 9_556 .
O1 Cu1 O1W 96.63(7) . .
O1 Cu1 O1W 96.63(7) 21_565 .
O2 Cu1 Cu1 84.43(4) 13_566 13_566
O2 Cu1 Cu1 84.43(4) 9_556 13_566
O1 Cu1 Cu1 83.49(4) . 13_566
O1 Cu1 Cu1 83.49(4) 21_565 13_566
O1W Cu1 Cu1 179.83(8) . 13_566
C1 O1 Cu1 123.61(12) . .
C1 O2 Cu1 122.53(12) . 13_566
O1 C1 O2 125.92(18) . .
O1 C1 C2 116.68(16) . .
O2 C1 C2 117.39(15) . .
C3 C2 C4 120.43(17) . .
C3 C2 C1 118.90(16) . .
C4 C2 C1 120.57(16) . .
C2 C3 C2 119.4(2) 19_665 .
C5 C4 C2 119.97(17) . .
C4 C5 C4 119.7(2) 19_665 .
C4 C5 C6 120.10(11) 19_665 .
C4 C5 C6 120.10(11) . .
C7 C6 C9 119.7(3) . .
C7 C6 C5 119.5(2) . .
C9 C6 C5 120.8(3) . .
C6 C9 C6 119.7(4) . 16_557
C6 C9 C10 120.14(19) . .
C6 C9 C10 120.14(19) 16_557 .
C6 C7 C8 121.3(3) . .
C7 C8 C7 118.3(5) 16_557 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O2 1.9568(13) 13_566
Cu1 O2 1.9568(13) 9_556
Cu1 O1 1.9641(13) .
Cu1 O1 1.9642(13) 21_565
Cu1 O1W 2.157(2) .
Cu1 Cu1 2.6505(6) 13_566
O1 C1 1.249(2) .
O2 C1 1.263(2) .
O2 Cu1 1.9568(13) 13_566
C1 C2 1.500(3) .
C2 C3 1.388(2) .
C2 C4 1.399(2) .
C3 C2 1.388(2) 19_665
C4 C5 1.390(2) .
C5 C4 1.390(2) 19_665
C5 C6 1.503(3) .
C6 C7 1.342(4) .
C6 C9 1.394(3) .
C9 C6 1.394(3) 16_557
C9 C10 1.474(7) .
C7 C8 1.392(4) .
C8 C7 1.392(4) 16_557
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 -0.042 -0.030 -0.002 4494.7 1110.2
