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#$Date: 2023-05-05 05:45:37 +0300 (Fri, 05 May 2023) $
#$Revision: 283355 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/22/7712232.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_7712232
loop_
_publ_author_name
'Maliuta, Mariia'
'Senkovska, Irena'
'Thümmler, Ronja'
'Ehrling, Sebastian'
'Becker, Sophi'
'Romaka, Vitaliy'
'Bon, Volodymyr'
'Evans, Jack D.'
'Kaskel, Stefan'
_publ_section_title
;
 Particle size-dependent flexibility in DUT-8(Cu) pillared layer
 metal-organic framework.
;
_journal_issue                   9
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2816
_journal_page_last               2824
_journal_paper_doi               10.1039/d3dt00085k
_journal_volume                  52
_journal_year                    2023
_chemical_formula_sum            'C30 H24 Cu2 N2 O8'
_chemical_formula_weight         667.59
_chemical_name_systematic        DUT-8(Cu)-DMF
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-07-11 deposited with the CCDC.	2023-01-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.31(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   18.510(4)
_cell_length_b                   18.370(4)
_cell_length_c                   9.6800(19)
_cell_measurement_reflns_used    629
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.6
_cell_measurement_theta_min      6.5
_cell_volume                     3271.5(12)
_computing_cell_refinement       'XDSAPP 2.0 Sparta et al., 2016'
_computing_data_reduction        'XDSAPP 2.0 Sparta et al., 2016'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.894
_diffrn_measured_fraction_theta_max 0.894
_diffrn_measurement_device_type  'MX-225 CCD'
_diffrn_measurement_method       'Δφ scans'
_diffrn_radiation_monochromator  'Si 111'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.8939
_diffrn_reflns_av_R_equivalents  0.0367
_diffrn_reflns_av_unetI/netI     0.0390
_diffrn_reflns_Laue_measured_fraction_full 0.894
_diffrn_reflns_Laue_measured_fraction_max 0.894
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            7396
_diffrn_reflns_point_group_measured_fraction_full 0.894
_diffrn_reflns_point_group_measured_fraction_max 0.894
_diffrn_reflns_theta_full        31.701
_diffrn_reflns_theta_max         31.701
_diffrn_reflns_theta_min         3.636
_diffrn_source                   synchrotron
_diffrn_source_type              'BESSY BL MX-14.3'
_exptl_absorpt_coefficient_mu    1.250
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    0.678
_exptl_crystal_description       block
_exptl_crystal_F_000             680
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.180
_refine_diff_density_min         -0.143
_refine_diff_density_rms         0.028
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     109
_refine_ls_number_reflns         2593
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.1213
_refine_ls_R_factor_gt           0.1056
_refine_ls_shift/su_max          0.028
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.3800P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3546
_refine_ls_wR_factor_ref         0.3751
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2488
_reflns_number_total             2593
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3dt00085k3.cif
_cod_data_source_block           c2m
_cod_depositor_comments          'Adding full bibliography for 7712232.cif.'
_cod_original_cell_volume        3271.5(11)
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_database_code               7712232
_shelx_shelxl_version_number     2018/3
_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   0.864
_shelx_estimated_absorpt_t_max   0.907
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, 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 0.49930(4) 0.500000 0.63815(8) 0.0700(19) Uani 1 2 d S T P A .
N1 N 0.5004(2) 0.500000 0.8688(6) 0.070(2) Uani 1 2 d S T P . .
O1 O 0.4239(2) 0.4242(2) 0.5991(5) 0.091(2) Uani 1 1 d . . . . .
O2 O 0.4250(2) 0.4243(2) 0.3670(5) 0.093(2) Uani 1 1 d . . . . .
C6 C 0.1829(4) 0.1824(5) 0.4206(7) 0.104(3) Uani 1 1 d . . . . .
H6A H 0.166046 0.164862 0.332865 0.125 Uiso 1 1 calc R U . . .
C1 C 0.4023(3) 0.4028(2) 0.4789(6) 0.081(2) Uani 1 1 d . . . . .
C5 C 0.2361(4) 0.2361(4) 0.4333(8) 0.100(2) Uani 1 1 d . . . . .
C2 C 0.3452(3) 0.3450(3) 0.4657(6) 0.089(2) Uani 1 1 d . . . . .
C3 C 0.3178(5) 0.3185(6) 0.3330(8) 0.128(4) Uani 1 1 d . . . . .
H3A H 0.334947 0.337792 0.254051 0.153 Uiso 1 1 calc R U . . .
C4 C 0.2675(6) 0.2661(6) 0.3199(9) 0.136(4) Uani 1 1 d . . . . .
H4A H 0.252489 0.248413 0.231367 0.163 Uiso 1 1 calc R U . . .
C10 C 0.5053(16) 0.424(3) 0.9236(11) 0.288(15) Uani 0.5 1 d D U P A 1
H10A H 0.552519 0.403468 0.911109 0.346 Uiso 0.5 1 calc R U P A 1
H10B H 0.468348 0.393936 0.872504 0.346 Uiso 0.5 1 calc R U P A 1
C11 C 0.5669(11) 0.500000 0.9323(14) 0.284(15) Uani 1 2 d DS TU P A 2
H11A H 0.592373 0.542679 0.903920 0.340 Uiso 0.5 1 calc R U P A 2
H11B H 0.592373 0.457321 0.903920 0.340 Uiso 0.5 1 calc R U P A 2
C12 C 0.4316(11) 0.500000 0.9106(14) 0.285(15) Uani 1 2 d S TU P A 2
H12A H 0.405575 0.457316 0.873148 0.342 Uiso 0.5 1 calc R U P A 2
H12B H 0.405575 0.542684 0.873149 0.342 Uiso 0.5 1 calc R U P A 2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0060 0.0030 '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 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0180 0.0100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.1510 1.8940 '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
_geom_angle_publ_flag
O2 Cu1 O2 89.3(3) 5_666 2_656 ?
O2 Cu1 O1 89.2(2) 5_666 6_565 ?
O2 Cu1 O1 167.6(2) 2_656 6_565 ?
O2 Cu1 O1 167.6(2) 5_666 . ?
O2 Cu1 O1 89.2(2) 2_656 . ?
O1 Cu1 O1 89.5(3) 6_565 . ?
O2 Cu1 N1 95.53(16) 5_666 . ?
O2 Cu1 N1 95.53(16) 2_656 . ?
O1 Cu1 N1 96.89(17) 6_565 . ?
O1 Cu1 N1 96.89(17) . . ?
O2 Cu1 Cu1 83.70(14) 5_666 5_666 ?
O2 Cu1 Cu1 83.70(14) 2_656 5_666 ?
O1 Cu1 Cu1 83.87(14) 6_565 5_666 ?
O1 Cu1 Cu1 83.88(14) . 5_666 ?
N1 Cu1 Cu1 178.92(10) . 5_666 ?
C11 N1 C12 135.3(8) . . ?
C10 N1 C10 139(2) 6_565 . ?
C11 N1 Cu1 111.9(8) . . ?
C12 N1 Cu1 112.7(7) . . ?
C10 N1 Cu1 110.4(9) 6_565 . ?
C10 N1 Cu1 110.4(9) . . ?
C1 O1 Cu1 123.0(4) . . ?
C1 O2 Cu1 122.9(4) . 5_666 ?
C2 C6 C5 121.3(7) 7_556 . ?
C2 C6 H6A 119.3 7_556 . ?
C5 C6 H6A 119.3 . . ?
O1 C1 O2 126.5(5) . . ?
O1 C1 C2 117.0(5) . . ?
O2 C1 C2 116.5(5) . . ?
C6 C5 C4 123.9(8) . . ?
C6 C5 C5 120.9(9) . 7_556 ?
C4 C5 C5 115.2(9) . 7_556 ?
C6 C2 C3 118.4(6) 7_556 . ?
C6 C2 C1 121.5(6) 7_556 . ?
C3 C2 C1 120.2(6) . . ?
C4 C3 C2 120.8(8) . . ?
C4 C3 H3A 119.6 . . ?
C2 C3 H3A 119.6 . . ?
C3 C4 C5 123.4(9) . . ?
C3 C4 H4A 118.3 . . ?
C5 C4 H4A 118.3 . . ?
N1 C10 C10 109.7(10) . 2_657 ?
N1 C10 H10A 109.7 . . ?
C10 C10 H10A 109.7 2_657 . ?
N1 C10 H10B 109.7 . . ?
C10 C10 H10B 109.7 2_657 . ?
H10A C10 H10B 108.2 . . ?
N1 C11 C12 112.4(15) . 5_667 ?
N1 C11 H11A 109.1 . . ?
C12 C11 H11A 109.1 5_667 . ?
N1 C11 H11B 109.1 . . ?
C12 C11 H11B 109.1 5_667 . ?
H11A C11 H11B 107.9 . . ?
N1 C12 C11 112.3(15) . 5_667 ?
N1 C12 H12A 109.2 . . ?
C11 C12 H12A 109.2 5_667 . ?
N1 C12 H12B 109.2 . . ?
C11 C12 H12B 109.2 5_667 . ?
H12A C12 H12B 107.9 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 O2 1.978(4) 5_666 ?
Cu1 O2 1.978(4) 2_656 ?
Cu1 O1 1.979(4) 6_565 ?
Cu1 O1 1.979(4) . ?
Cu1 N1 2.231(6) . ?
Cu1 Cu1 2.6776(16) 5_666 ?
N1 C11 1.31(2) . ?
N1 C12 1.38(2) . ?
N1 C10 1.49(6) 6_565 ?
N1 C10 1.49(6) . ?
O1 C1 1.251(7) . ?
O2 C1 1.268(7) . ?
C6 C2 1.364(9) 7_556 ?
C6 C5 1.390(11) . ?
C6 H6A 0.9300 . ?
C1 C2 1.494(7) . ?
C5 C4 1.409(12) . ?
C5 C5 1.430(15) 7_556 ?
C2 C3 1.414(9) . ?
C3 C4 1.335(12) . ?
C3 H3A 0.9300 . ?
C4 H4A 0.9300 . ?
C10 C10 1.514(17) 2_657 ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 C12 1.518(13) 5_667 ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Cu1 O1 C1 O2 1.3(9) . . . . ?
Cu1 O1 C1 C2 179.8(3) . . . . ?
Cu1 O2 C1 O1 -1.2(9) 5_666 . . . ?
Cu1 O2 C1 C2 -179.7(3) 5_666 . . . ?
C2 C6 C5 C4 179.4(10) 7_556 . . . ?
C2 C6 C5 C5 0.8(16) 7_556 . . 7_556 ?
O1 C1 C2 C6 0.9(8) . . . 7_556 ?
O2 C1 C2 C6 179.6(6) . . . 7_556 ?
O1 C1 C2 C3 179.6(7) . . . . ?
O2 C1 C2 C3 -1.7(9) . . . . ?
C6 C2 C3 C4 -2.3(16) 7_556 . . . ?
C1 C2 C3 C4 179.0(9) . . . . ?
C2 C3 C4 C5 3.0(19) . . . . ?
C6 C5 C4 C3 178.9(8) . . . . ?
C5 C5 C4 C3 -2(2) 7_556 . . . ?
C10 N1 C10 C10 18(6) 6_565 . . 2_657 ?
Cu1 N1 C10 C10 -172(2) . . . 2_657 ?
C12 N1 C11 C12 0.000(4) . . . 5_667 ?
Cu1 N1 C11 C12 180.000(3) . . . 5_667 ?
C11 N1 C12 C11 0.000(4) . . . 5_667 ?
Cu1 N1 C12 C11 180.000(3) . . . 5_667 ?
