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_7716817
_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, 5.5[C3H7NO]'
_chemical_formula_sum            'C60.5 H60.5 Cu2 N5.5 O15.5'
_chemical_formula_weight         1239.72
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-03-20
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2024-01-11 deposited with the CCDC.	2024-08-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.262(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.1907(3)
_cell_length_b                   14.79129(19)
_cell_length_c                   22.8997(6)
_cell_measurement_reflns_used    35013
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      33.8230
_cell_measurement_theta_min      2.9660
_cell_volume                     6207.4(2)
_computing_cell_refinement       'CrysAlisPro 1.171.42.71a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.71a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.71a (Rigaku OD, 2022)'
_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 (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.985
_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     -1.00  60.00   0.50   40.00    --   17.84-107.00 -58.00  122
  2  \w     42.00  96.00   0.50   40.00    --   17.84 178.00 -30.00  108
  3  \w    -62.00   3.00   0.50   40.00    --   17.84 -19.00 150.00  130
  4  \w    -95.00 -51.00   0.50   40.00    --  -18.23 -38.00 120.00   88
  5  \w    -11.00  41.00   0.50   40.00    --   17.84  77.00-180.00  104
  6  \w    -11.00  41.00   0.50   40.00    --   17.84  77.00  60.00  104
  7  \w    -59.00  20.00   0.50   40.00    --   17.84 -38.00  60.00  158
  8  \w    -95.00   5.00   0.50   40.00    --  -18.23 -38.00  90.00  200
  9  \w    -95.00   4.00   0.50   40.00    --  -18.23 -38.00 120.00  198
 10  \w    -26.00   4.00   0.50   40.00    --  -18.23 -38.00 120.00   60
 11  \w    -44.00 -17.00   0.50   40.00    --  -18.23  77.00 -90.00   54
 12  \w    -35.00   4.00   0.50   40.00    --  -18.23  81.00 -50.57   78
 13  \w    -34.00   5.00   0.50   40.00    --  -18.23 -77.00  30.00   78
;
_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      -0.0370834000
_diffrn_orient_matrix_UB_12      0.0077293000
_diffrn_orient_matrix_UB_13      -0.0017858000
_diffrn_orient_matrix_UB_21      0.0058070000
_diffrn_orient_matrix_UB_22      -0.0197258000
_diffrn_orient_matrix_UB_23      0.0292740000
_diffrn_orient_matrix_UB_31      0.0093687000
_diffrn_orient_matrix_UB_32      0.0429862000
_diffrn_orient_matrix_UB_33      0.0137209000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0416
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            29748
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        30.629
_diffrn_reflns_theta_max         30.629
_diffrn_reflns_theta_min         2.545
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.754
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.399
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.71a (Rigaku Oxford Diffraction, 2022)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
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    1.327
_exptl_crystal_description       prism
_exptl_crystal_F_000             2576
_exptl_crystal_size_max          0.262
_exptl_crystal_size_mid          0.162
_exptl_crystal_size_min          0.123
_refine_diff_density_max         2.057
_refine_diff_density_min         -0.795
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     506
_refine_ls_number_reflns         29748
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.1418
_refine_ls_R_factor_gt           0.1000
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1421P)^2^+11.6678P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2859
_refine_ls_wR_factor_ref         0.3179
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19494
_reflns_number_total             29748
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by -179.9841\% 
around [1.00 -0.00 0.00] (reciprocal) or [0.97 0.00 0.24] (direct)
;
_cod_data_source_file            d4dt02085e2.cif
_cod_data_source_block           cs2947_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7716813--7716817.cif.'
_cod_original_formula_sum        'C60.50 H60.50 Cu2 N5.50 O15.50'
_cod_database_code               7716817
_chemical_oxdiff_formula         'C60.5 H60.5 Cu2 N5.5 O15.5'
_chemical_oxdiff_usercomment     'Trevor Makal (LJE 01 76 2)'
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.516(2)
 0.484(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C10(H10), C11(H11), C12(H12), C13(H13),
 C16(H16), C18(H18), C20(H20), C25(H25), C26(H26), C27(H27), C28(H28), C32(H32),
  C33(H33), C34(H34), C35(H35), C38(H38), C40(H40), C42(H42)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 893 electrons were 
found in a volume of 3665\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
5.5[C3H7NO] per unit cell 
which account for 880 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.1
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              19431
_shelx_fab_checksum              99947
_shelx_shelxl_version_number     2018/3
_olex2_date_sample_data_collection 2022-11-30
_olex2_date_sample_submission    2022-11-03
_olex2_submission_original_sample_id 'LJE 01 76 2'
_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 1.416
_oxdiff_exptl_absorpt_empirical_full_min 0.745
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2