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_7716815
_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 H20 Cu2 O10, 5[C3H7NO]'
_chemical_formula_sum            'C59 H55 Cu2 N5 O15'
_chemical_formula_weight         1201.16
_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             2024-07-15
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-07-17 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                   11.3494(3)
_cell_length_b                   36.6729(3)
_cell_length_c                   14.7750(2)
_cell_measurement_reflns_used    21903
_cell_measurement_temperature    99.98(16)
_cell_measurement_theta_max      76.5030
_cell_measurement_theta_min      4.0430
_cell_volume                     6149.58(19)
_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      99.98(16)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.995
_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    -25.00  32.00   0.50    2.00    --  -45.04  13.00 108.00  114
  2  \w   -122.00 -21.00   0.50    2.00    --  -45.04 -13.00 -63.00  202
  3  \w     55.00  95.00   0.50    2.00    --   45.04  13.00 108.00   80
  4  \w    -32.00  21.00   0.50    2.00    --   45.04 -13.00 -63.00  106
  5  \w   -138.00-113.00   0.50   10.00    --  -88.50 -13.00 -63.00   50
  6  \w     81.00 126.00   0.50   10.00    --  110.00  13.00 108.00   90
  7  \w     -1.00  28.00   0.50    2.00    --  -45.04  77.00 150.00   58
  8  \w    -78.00 -15.00   0.50    2.00    --  -45.04 125.00-180.00  126
  9  \w   -117.00 -85.00   0.50    2.00    --  -45.04 -77.00 -30.00   64
 10  \w    -28.00  33.00   0.50    2.00    --  -45.04  19.00 -90.00  122
 11  \w    -69.00 -30.00   0.50    2.00    --  -45.04  77.00 150.00   78
 12  \w     38.00  92.00   0.50    2.00    --   45.04-125.00 120.00  108
 13  \w    -48.00 -22.00   0.50   10.00    --  -88.50  45.00   0.00   52
 14  \w     45.00  85.00   0.50   10.00    --  110.00 -94.00   0.00   80
 15  \w     55.00  96.00   0.50   10.00    --  110.00 -94.00-150.00   82
 16  \w     81.00 106.00   0.50   10.00    --  110.00-104.00 -29.67   50
 17  \w     79.00 106.00   0.50   10.00    --  110.00-105.00  88.48   54
 18  \w     39.00  68.00   0.50   10.00    --  110.00 -61.00 150.00   58
 19  \w     41.00  69.00   0.50   10.00    --  110.00 -61.00 -60.00   56
 20  \w     94.00 120.00   0.50   10.00    --  110.00  45.00-120.00   52
 21  \w     41.00  74.00   0.50   10.00    --  110.00-105.00  88.48   66
 22  \w     84.00 138.00   0.50   10.00    --  110.00  15.00  30.00  108
 23  \w     38.00  69.00   0.50   10.00    --  110.00 -61.00  30.00   62
 24  \w     50.00  75.00   0.50   10.00    --  110.00-125.00-120.00   50
 25  \w     87.00 112.00   0.50   10.00    --  110.00-125.00-120.00   50
 26  \w     43.00  80.00   0.50   10.00    --  110.00-125.00 120.00   74
 27  \w     41.00  68.00   0.50   10.00    --  110.00 -88.00 118.14   54
 28  \w     51.00  77.00   0.50   10.00    --  110.00-125.00 -60.00   52
 29  \w     84.00 112.00   0.50   10.00    --  110.00-125.00 -60.00   56
 30  \w     92.00 163.00   0.50   10.00    --  110.00  45.00 -60.00  142
 31  \w     43.00  69.00   0.50   10.00    --  110.00-125.00  30.00   52
 32  \w     81.00 111.00   0.50   10.00    --  110.00-125.00  30.00   60
 33  \w     96.00 178.00   0.50   10.00    --  110.00  15.00 -90.00  164
 34  \w     39.00  87.00   0.50   10.00    --  110.00 -77.00 -60.00   96
 35  \w     96.00 121.00   0.50   10.00    --  110.00  30.00 150.00   50
 36  \w    134.00 160.00   0.50   10.00    --  110.00  30.00 150.00   52
 37  \w    104.00 163.00   0.50   10.00    --  110.00 125.00 120.00  118
 38  \w    116.00 172.00   0.50   10.00    --  110.00  15.00 -30.00  112
 39  \w     84.00 109.00   0.50   10.00    --  110.00 -85.00 -76.77   50
 40  \w     41.00  74.00   0.50   10.00    --  110.00 -85.00 -76.77   66
 41  \w    105.00 142.00   0.50   10.00    --  110.00  69.00 127.66   74
 42  \w     41.00  67.00   0.50   10.00    --  110.00 -61.00-180.00   52
 43  \w     39.00  64.00   0.50   10.00    --  110.00 -77.00-150.00   50
 44  \w     88.00 113.00   0.50   10.00    --  110.00  15.00 -30.00   50
 45  \w     41.00  92.00   0.50   10.00    --  110.00-125.00-150.00  102
 46  \w     96.00 175.00   0.50   10.00    --  110.00 125.00 150.00  158
 47  \w     81.00 112.00   0.50   10.00    --  110.00-125.00 150.00   62
 48  \w     86.00 112.00   0.50   10.00    --  110.00-125.00 120.00   52
 49  \w     38.00  93.00   0.50   10.00    --  110.00 -94.00 120.00  110
 50  \w     94.00 141.00   0.50   10.00    --  110.00 -88.00 118.14   94
 51  \w    128.00 154.00   0.50   10.00    --  110.00 125.00  90.00   52
 52  \w    111.00 136.00   0.50   10.00    --  110.00  45.00 120.00   50
 53  \w     93.00 123.00   0.50   10.00    --  110.00  30.00-180.00   60
 54  \w    135.00 160.00   0.50   10.00    --  110.00  30.00-180.00   50
 55  \w     39.00  65.00   0.50   10.00    --  110.00 -94.00 -90.00   52
 56  \w     80.00 106.00   0.50   10.00    --  110.00 -94.00 -90.00   52
 57  \w     42.00  67.00   0.50   10.00    --  110.00-125.00   0.00   50
 58  \w     82.00 107.00   0.50   10.00    --  110.00-125.00   0.00   50
 59  \w     48.00  73.00   0.50   10.00    --  110.00 -64.00-146.55   50
 60  \w     96.00 174.00   0.50   10.00    --  110.00  45.00-150.00  156
 61  \w    113.00 153.00   0.50   10.00    --  110.00  61.00   0.00   80
 62  \w     78.00 103.00   0.50   10.00    --  110.00 -77.00-120.00   50
 63  \w     52.00  77.00   0.50   10.00    --  110.00 -77.00   0.00   50
 64  \w     67.00  92.00   0.50   10.00    --  110.00 -77.00 -30.00   50
 65  \w     78.00 104.00   0.50   10.00    --  110.00 -94.00-120.00   52
 66  \w     54.00 106.00   0.50   10.00    --  110.00 -78.00  22.12  104
 67  \w     50.00  75.00   0.50   10.00    --  110.00-125.00  60.00   50
 68  \w     85.00 110.00   0.50   10.00    --  110.00-125.00  90.00   50
 69  \w     38.00  63.00   0.50   10.00    --  110.00 -61.00 120.00   50
 70  \w     98.00 171.00   0.50   10.00    --  110.00  45.00-180.00  146
 71  \w    134.00 159.00   0.50   10.00    --  110.00 125.00  30.00   50
 72  \w    110.00 135.00   0.50   10.00    --  110.00-159.00 142.98   50
 73  \w    104.00 152.00   0.50   10.00    --  110.00  45.00  90.00   96
 74  \w     95.00 120.00   0.50   10.00    --  110.00  30.00-150.00   50
 75  \w    113.00 139.00   0.50   10.00    --  110.00  61.00-180.00   52
 76  \w    117.00 142.00   0.50   10.00    --  110.00  61.00 120.00   50
 77  \w     46.00  73.00   0.50   10.00    --  110.00-104.00 -29.67   54
 78  \w     60.00 108.00   0.50   10.00    --  110.00 -83.00 134.79   96
 79  \w     89.00 114.00   0.50   10.00    --  110.00 -84.00 -32.79   50
 80  \w     44.00  69.00   0.50   10.00    --  110.00 -85.00  89.44   50
 81  \w    111.00 136.00   0.50   10.00    --  110.00 -85.00  89.44   50
 82  \w     52.00 106.00   0.50   10.00    --  110.00-107.00 154.58  108
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'Rigaku Oxford Diffraction XtaLAB Synergy, Dualflex, HyPix 6000-HE'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1020457000
_diffrn_orient_matrix_UB_12      0.0067615000
_diffrn_orient_matrix_UB_13      0.0667110000
_diffrn_orient_matrix_UB_21      -0.0888665000
_diffrn_orient_matrix_UB_22      0.0027221000
_diffrn_orient_matrix_UB_23      0.0785055000
_diffrn_orient_matrix_UB_31      0.0106697000
_diffrn_orient_matrix_UB_32      -0.0413781000
_diffrn_orient_matrix_UB_33      0.0159743000
_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  0.0768
_diffrn_reflns_av_unetI/netI     0.0294
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -45
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            58535
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.420
_diffrn_reflns_theta_min         2.410
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.412
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81325
_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    1.297
_exptl_crystal_description       prism
_exptl_crystal_F_000             2488
_exptl_crystal_recrystallization_method 'crystallized from DMF'
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.948
_refine_diff_density_min         -0.806
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.370
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     174
_refine_ls_number_reflns         3398
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.370
_refine_ls_R_factor_all          0.0957
_refine_ls_R_factor_gt           0.0910
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2891
_refine_ls_wR_factor_ref         0.2989
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2919
_reflns_number_total             3398
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02085e2.cif
_cod_data_source_block           cs2947
_cod_depositor_comments
'Adding full bibliography for 7716813--7716817.cif.'
_cod_database_code               7716815
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Cu2 C44 H22 O8 C3 H7 N O H2 O'
_chemical_oxdiff_usercomment     'Trevor Makal UVA Wise LJE-01-68-6'
_shelx_estimated_absorpt_t_max   0.849
_shelx_estimated_absorpt_t_min   0.710
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Others
 Fixed Sof: C13B(0.5) C8A(0.5) C13A(0.5) C12A(0.5) H12A(0.5) C11A(0.5)
 H11A(0.5) C10A(0.5) H10A(0.5) C9A(0.5) H9A(0.5) C8B(0.5) C10B(0.5) H10B(0.5)
 C9B(0.5) H9B(0.5) C11B(0.5) H11B(0.5) C12B(0.5)
3.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C3(H3), C12A(H12A), C11A(H11A), C10A(H10A), C9A(H9A), C10B(H10B),
 C9B(H9B), C11B(H11B)
3.b Fitted hexagon refined as free rotating group:
 C8A(C13A,C12A,C11A,C10A,C9A)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 782 electrons were 
found in a volume of 2969\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
5[C3H7NO] per formula unit which account for 800 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              23457
_shelx_fab_checksum              31923
_olex2_date_sample_data_collection 2022-11-30
_olex2_date_sample_submission    2022-11-30
_olex2_exptl_crystal_mounting_method
'mounted on a nylon loop with perfluoroether oil'
_olex2_submission_original_sample_id LJE-01-68-6
_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 2.785
_oxdiff_exptl_absorpt_empirical_full_min 0.422