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_7716816
_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         'C28 H25 N2 O6 Zn, 2(C3 H7 N O)'
_chemical_formula_sum            'C34 H39 N4 O8 Zn'
_chemical_formula_weight         697.06
_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_Hall           'F 2 -2d'
_space_group_name_H-M_alt        'F d d 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-04-03
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   38.9726(6)
_cell_length_b                   24.8157(5)
_cell_length_c                   13.8024(2)
_cell_measurement_reflns_used    12826
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      76.9250
_cell_measurement_theta_min      3.7770
_cell_volume                     13348.7(4)
_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 2018/2 (Sheldrick, 2018)'
_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 1.000
_diffrn_measured_fraction_theta_max 0.989
_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   -117.00 -27.00   0.50    4.00    --  -44.79 -51.00-145.00  180
  2  \w    -60.00  29.00   0.50    4.00    --  -44.79  51.00   0.00  178
  3  \w    -60.00 -15.00   0.50   20.00    --  -88.50  51.00   0.00   90
  4  \w   -161.00 -70.00   0.50   20.00    --  -88.50 -51.00-145.00  182
  5  \w     92.00 178.00   0.50   20.00    --  110.00  51.00   0.00  172
  6  \w    -85.00 -13.00   0.50    4.00    --  -44.79 125.00  60.00  144
  7  \w    -28.00  56.00   0.50    4.00    --   44.79 -51.00-145.00  168
  8  \w    -53.00 -28.00   0.50   20.00    --  -88.50  45.00-180.00   50
  9  \w     59.00  85.00   0.50   20.00    --  110.00-113.00-136.18   52
 10  \w     39.00  64.00   0.50   20.00    --  110.00 -61.00-120.00   50
 11  \w     44.00  70.00   0.50   20.00    --  110.00-125.00  60.00   52
 12  \w    153.00 178.00   0.50   20.00    --  110.00  95.00-110.84   50
 13  \w     43.00  68.00   0.50   20.00    --  110.00 -61.00 150.00   50
 14  \w     47.00  72.00   0.50   20.00    --  110.00-125.00  30.00   50
 15  \w     85.00 112.00   0.50   20.00    --  110.00-125.00  30.00   54
 16  \w     55.00  81.00   0.50   20.00    --  110.00 -94.00-150.00   52
 17  \w     38.00  63.00   0.50   20.00    --  110.00 -61.00   0.00   50
 18  \w     47.00  93.00   0.50   20.00    --  110.00 -77.00 -90.00   92
 19  \w     76.00 102.00   0.50   20.00    --  110.00 -94.00  60.00   52
 20  \w    105.00 131.00   0.50   20.00    --  110.00  95.00-110.84   52
 21  \w     39.00  64.00   0.50   20.00    --  110.00 -94.00  60.00   50
 22  \w     39.00 102.00   0.50   20.00    --  110.00 -77.00 -30.00  126
 23  \w     39.00  66.00   0.50   20.00    --  110.00 -77.00  90.00   54
 24  \w     71.00  96.00   0.50   20.00    --  110.00 -77.00  90.00   50
 25  \w     97.00 122.00   0.50   20.00    --  110.00  45.00-120.00   50
 26  \w     40.00  77.00   0.50   20.00    --  110.00 -77.00 150.00   74
 27  \w     38.00  66.00   0.50   20.00    --  110.00 -61.00 -90.00   56
 28  \w     39.00  64.00   0.50   20.00    --  110.00 -61.00 -60.00   50
 29  \w    112.00 169.00   0.50   20.00    --  110.00  15.00 -90.00  114
 30  \w     51.00 102.00   0.50   20.00    --  110.00 -77.00 120.00  102
 31  \w    152.00 177.00   0.50   20.00    --  110.00 126.00  93.87   50
 32  \w     85.00 135.00   0.50   20.00    --  110.00  77.00-120.00  100
 33  \w    142.00 171.00   0.50   20.00    --  110.00  77.00-120.00   58
 34  \w     41.00  67.00   0.50   20.00    --  110.00 -77.00   0.00   52
 35  \w     38.00  69.00   0.50   20.00    --  110.00 -61.00-180.00   62
 36  \w     40.00  68.00   0.50   20.00    --  110.00 -61.00-150.00   56
 37  \w    116.00 142.00   0.50   20.00    --  110.00  30.00 120.00   52
 38  \w    146.00 177.00   0.50   20.00    --  110.00  59.00 -93.41   62
 39  \w     74.00 105.00   0.50   20.00    --  110.00-125.00  60.00   62
;
_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      -0.0076380000
_diffrn_orient_matrix_UB_12      -0.0367617000
_diffrn_orient_matrix_UB_13      0.0873702000
_diffrn_orient_matrix_UB_21      0.0232994000
_diffrn_orient_matrix_UB_22      -0.0438982000
_diffrn_orient_matrix_UB_23      -0.0436031000
_diffrn_orient_matrix_UB_31      0.0310103000
_diffrn_orient_matrix_UB_32      0.0238885000
_diffrn_orient_matrix_UB_33      0.0541787000
_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  0.0485
_diffrn_reflns_av_unetI/netI     0.0300
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       49
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            30940
_diffrn_reflns_point_group_measured_fraction_full 0.917
_diffrn_reflns_point_group_measured_fraction_max 0.895
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.352
_diffrn_reflns_theta_min         3.836
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.498
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.762
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.387
_exptl_crystal_description       prism
_exptl_crystal_F_000             5840
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.587
_refine_diff_density_min         -1.205
_refine_diff_density_rms         0.133
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.30(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     442
_refine_ls_number_reflns         6325
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0801
_refine_ls_R_factor_gt           0.0762
_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^)+(0.1899P)^2^+2.7196P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2121
_refine_ls_wR_factor_ref         0.2194
_reflns_Friedel_coverage         0.734
_reflns_Friedel_fraction_full    0.826
_reflns_Friedel_fraction_max     0.792
_reflns_number_gt                5764
_reflns_number_total             6325
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02085e2.cif
_cod_data_source_block           cs2957
_cod_depositor_comments
'Adding full bibliography for 7716813--7716817.cif.'
_cod_database_code               7716816
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C34 H39 N4 O8 Zn'
_chemical_oxdiff_usercomment     'Trevor Makal (UVA Wise) TM3125 10'
_shelx_estimated_absorpt_t_max   0.916
_shelx_estimated_absorpt_t_min   0.796
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.70(5)
 0.30(5)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 O8-C32B
 1.25 with sigma of 0.02
 C32B-N4
 1.31 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uiso(C32B) = Uiso(C33B) = Uiso(C34B)
5. Others
 Sof(C34B)=Sof(H34D)=Sof(H34E)=Sof(H34F)=Sof(C32B)=Sof(H32B)=Sof(C33B)=
 Sof(H33D)=Sof(H33E)=Sof(H33F)=1-FVAR(1)
 Sof(C32)=Sof(H32)=Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(H33C)=Sof(C34)=Sof(H34A)=
 Sof(H34B)=Sof(H34C)=FVAR(1)
6.a Me refined with riding coordinates:
 C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C34B(H34D,H34E,H34F), C33B(H33D,
 H33E,H33F)
6.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C6(H6), C11(H11), C12(H12), C13(H13), C14(H14), C18(H18),
 C19(H19), C20(H20), C21(H21), C23(H23), C26(H26), C29(H29), C32(H32),
 C32B(H32B)
6.c Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C27(H27A,H27B,H27C), C28(H28A,H28B,
 H28C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C)
;
_shelx_res_checksum              38549
_olex2_date_sample_data_collection 2022-11-16
_olex2_date_sample_submission    2022-11-03
_olex2_exptl_crystal_mounting_method
'Mounted on nylon loop with perfluoroether oil'
_olex2_submission_original_sample_id 'TM3125 10'
_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 1.649
_oxdiff_exptl_absorpt_empirical_full_min 0.598