Structural diversity and solvent-induced transformations of a copper-based metal-organic framework with highly aromatic ligands.
Edwards, Abigail; Elkins, Landon J.; Slebodnick, Carla; Wang, Jinglei; Zhang, Qiang; Makal, Tegan A.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 14496–14504; doi:10.1039/d4dt02085e

data_7716814
_publ_section_title
;
 Structural diversity and solvent-induced transformations of a
 copper-based metal-organic framework with highly aromatic ligands.
;
_journal_issue                   34
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14496
_journal_page_last               14504
_journal_paper_doi               10.1039/d4dt02085e
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C44 H22 Cu2 O10, 5[C2H6SO]'
_chemical_formula_sum            'C54 H52 Cu2 O15 S5'
_chemical_formula_weight         1228.33
_space_group_crystal_system      orthorhombic
_space_group_IT_number           66
_space_group_name_Hall           '-C 2 2c'
_space_group_name_H-M_alt        'C c c m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-07-05
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-07-18 deposited with the CCDC.	2024-08-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.4087(3)
_cell_length_b                   36.7583(8)
_cell_length_c                   15.4789(4)
_cell_measurement_reflns_used    11748
_cell_measurement_temperature    99.9(3)
_cell_measurement_theta_max      76.6580
_cell_measurement_theta_min      4.3560
_cell_volume                     5922.3(3)
_computing_cell_refinement       'CrysAlisPro 1.171.42.94a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.94a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.94a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.9(3)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -120.00 -33.00   0.50    5.00    --  -47.20 -52.00  21.00  174
  2  \w    -61.00  25.00   0.50    5.00    --  -47.20  52.00 166.00  172
  3  \w    -24.00  57.00   0.50    5.00    --   47.20 -52.00  21.00  162
  4  \w     34.00 120.00   0.50    5.00    --   47.20  52.00 166.00  172
  5  \w    -61.00 -14.00   0.50   30.00    --  -86.25  52.00 166.00   94
  6  \w   -159.00 -72.00   0.50   30.00    --  -86.25 -52.00  21.00  174
  7  \w     94.00 178.00   0.50   30.00    --  107.75  52.00 166.00  168
  8  \w    -86.00 -13.00   0.50    5.00    --  -47.20 125.00-120.00  146
  9  \w   -120.00 -85.00   0.50    5.00    --  -47.20 -77.00-120.00   70
 10  \w   -120.00 -85.00   0.50    5.00    --  -47.20 -77.00-150.00   70
 11  \w    -37.00 -11.00   0.50   30.00    --  -86.25  30.00 -60.00   52
 12  \w    -53.00 -14.00   0.50   30.00    --  -86.25  45.00   0.00   78
 13  \w    -37.00 -11.00   0.50   30.00    --  -86.25  30.00 -30.00   52
 14  \w     95.00 178.00   0.50   30.00    --  107.75 125.00  90.00  166
 15  \w     35.00  69.00   0.50   30.00    --  107.75 -61.00-180.00   68
 16  \w     35.00  69.00   0.50   30.00    --  107.75 -61.00  60.00   68
 17  \w     35.00 103.00   0.50   30.00    --  107.75 -77.00   0.00  136
 18  \w     35.00  69.00   0.50   30.00    --  107.75 -61.00 120.00   68
 19  \w     95.00 178.00   0.50   30.00    --  107.75  30.00 -60.00  166
 20  \w     35.00 103.00   0.50   30.00    --  107.75 -77.00-120.00  136
 21  \w     35.00  69.00   0.50   30.00    --  107.75 -61.00-120.00   68
 22  \w     35.00  69.00   0.50   30.00    --  107.75 -61.00 -90.00   68
 23  \w     35.00 103.00   0.50   30.00    --  107.75 -77.00  30.00  136
 24  \w     35.00  69.00   0.50   30.00    --  107.75 -61.00 -30.00   68
 25  \w     35.00 106.00   0.50   30.00    --  107.75 -94.00 120.00  142
 26  \w     95.00 178.00   0.50   30.00    --  107.75  45.00-120.00  166
 27  \w   -120.00 -32.00   0.50    5.00    --  -47.20 -57.00  90.00  176
 28  \w   -120.00 -32.00   0.50    5.00    --  -47.20 -57.00 -30.00  176
 29  \w     32.00  57.00   0.50    5.00    --   47.20  57.00-150.00   50
 30  \w     32.00 120.00   0.50    5.00    --   47.20  57.00 -90.00  176
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1278329000
_diffrn_orient_matrix_UB_12      0.0210850000
_diffrn_orient_matrix_UB_13      0.0038526000
_diffrn_orient_matrix_UB_21      -0.0540987000
_diffrn_orient_matrix_UB_22      0.0283757000
_diffrn_orient_matrix_UB_23      -0.0638387000
_diffrn_orient_matrix_UB_31      -0.0513718000
_diffrn_orient_matrix_UB_32      0.0225466000
_diffrn_orient_matrix_UB_33      0.0761994000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0808
_diffrn_reflns_av_unetI/netI     0.0303
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            31846
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.137
_diffrn_reflns_theta_min         4.415
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.055
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.34162
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.94a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.378
_exptl_crystal_description       plate
_exptl_crystal_F_000             2536
_exptl_crystal_recrystallization_method
'Crystals grown in DMF and then soaked in DMSO.'
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.685
_refine_diff_density_min         -0.373
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     186
_refine_ls_number_reflns         3226
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0758
_refine_ls_R_factor_gt           0.0671
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0984P)^2^+19.1137P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1987
_refine_ls_wR_factor_ref         0.2056
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2648
_reflns_number_total             3226
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02085e2.cif
_cod_data_source_block           cs3105
_cod_depositor_comments
'Adding full bibliography for 7716813--7716817.cif.'
_cod_database_code               7716814
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Cu2 C44 H22 O8 H2 O C3 H7 N O C2 H6 S O'
_chemical_oxdiff_usercomment     'Abigail/Trevor Makal (TM4014 1)'
_shelx_estimated_absorpt_t_max   0.941
_shelx_estimated_absorpt_t_min   0.657
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Others
 Fixed Sof: C8A(0.5) C8B(0.5) C9A(0.5) H9A(0.5) C9B(0.5) H9B(0.5) C10A(0.5)
 H10A(0.5) C10B(0.5) H10B(0.5) C11A(0.5) H11A(0.5) C11B(0.5) H11B(0.5)
 C12A(0.5) H12A(0.5) C12B(0.5) H12B(0.5) C13A(0.5) C13B(0.5)
3.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C9A(H9A), C9B(H9B), C10A(H10A), C10B(H10B), C11A(H11A),
 C11B(H11B), C12A(H12A), C12B(H12B)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 835 electrons were 
found in a volume of 2698\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
5 DMSO per formula unit which account for 840 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              69074
_shelx_fab_checksum              36475
_olex2_date_sample_data_collection 2023-07-17
_olex2_date_sample_submission    2023-07-17
_olex2_exptl_crystal_mounting_method
'Mounted on a nylon loop with perfluoroether oil.'
_olex2_submission_original_sample_id 'TM4014 1'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.814
_oxdiff_exptl_absorpt_empirical_full_min 0.515