Substituent effects on through-space intervalence charge transfer in cofacial metal-organic frameworks.
Doheny, Patrick W.; Hua, Carol; Chan, Bun; Tuna, Floriana; Collison, David; Kepert, Cameron J.; D'Alessandro, Deanna M; Faraday discussions 231 (2021) 152–167; doi:10.1039/d1fd00021g

data_1564107
_publ_section_title
;
 Substituent effects on through-space intervalence charge transfer in
 cofacial metal-organic frameworks.
;
_journal_issue                   0
_journal_name_full               'Faraday discussions'
_journal_page_first              152
_journal_page_last               167
_journal_paper_doi               10.1039/d1fd00021g
_journal_volume                  231
_journal_year                    2021
_chemical_formula_moiety
'C32 H16 F2 N4 O4 S3 Zn, 1[C3H7NO], 1[C3H7NO]'
_chemical_formula_sum            'C38 H30 F2 N6 O6 S3 Zn'
_chemical_formula_weight         866.23
_chemical_name_systematic        ZnFTzTz
_space_group_crystal_system      orthorhombic
_space_group_IT_number           56
_space_group_name_Hall           '-P 2ab 2ac'
_space_group_name_H-M_alt        'P c c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-02-07
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2021-02-07 deposited with the CCDC.	2021-04-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   26.0566(2)
_cell_length_b                   18.5354(2)
_cell_length_c                   15.67380(10)
_cell_measurement_reflns_used    17473
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      73.2960
_cell_measurement_theta_min      2.9040
_cell_volume                     7569.97(11)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (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      150.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5861
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.993
_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    -68.00  15.00   1.00    7.50    --  -39.58  57.00-180.00   83
  2  \w    -86.00 -51.00   1.00    7.50    --  -39.58 178.00  90.00   35
  3  \w   -115.00 -16.00   1.00    7.50    --  -39.58 -38.00-120.00   99
  4  \w   -114.00 -10.00   1.00    7.50    --  -39.58 -57.00   0.00  104
  5  \w     85.00 128.00   1.00    7.50    --   39.58-178.00   0.00   43
  6  \w    101.00 130.00   1.00    7.50    --   39.58 178.00 120.00   29
  7  \w    -31.00  19.00   1.00    7.50    --   39.58 -38.00  60.00   50
  8  \w     38.00  64.00   1.00   30.00    --  108.86 -37.00  93.00   26
  9  \w     91.00 174.00   1.00   30.00    --  108.86  45.00-180.00   83
 10  \w     36.00 143.00   1.00   30.00    --  108.86 -77.00  60.00  107
 11  \w     35.00 120.00   1.00   30.00    --  108.86 -30.00   0.00   85
 12  \w     90.00 135.00   1.00   30.00    --  108.86  61.00 -30.00   45
 13  \w     31.00 109.00   1.00   30.00    --  108.86 -95.00-150.00   78
 14  \w     95.00 127.00   1.00   30.00    --  108.86 -37.00  93.00   32
 15  \w     34.00  85.00   1.00   30.00    --  108.86 -45.00-120.00   51
 16  \w     38.00 119.00   1.00   30.00    --  108.86-125.00  60.00   81
 17  \w     94.00 119.00   1.00   30.00    --  108.86-125.00 150.00   25
 18  \w     63.00 175.00   1.00   30.00    --  108.86  15.00 -60.00  112
 19  \w     30.00 140.00   1.00   30.00    --  108.86 -77.00-120.00  110
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0273573000
_diffrn_orient_matrix_UB_12      -0.0366091000
_diffrn_orient_matrix_UB_13      -0.0756228000
_diffrn_orient_matrix_UB_21      -0.0045009000
_diffrn_orient_matrix_UB_22      0.0702482000
_diffrn_orient_matrix_UB_23      -0.0520102000
_diffrn_orient_matrix_UB_31      0.0521932000
_diffrn_orient_matrix_UB_32      0.0251915000
_diffrn_orient_matrix_UB_33      0.0352446000
_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  0.0418
_diffrn_reflns_av_unetI/netI     0.0233
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            53560
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.991
_diffrn_reflns_theta_min         2.926
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.011
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.786
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
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    1.520
_exptl_crystal_description       block
_exptl_crystal_F_000             3552
_exptl_crystal_size_max          0.216
_exptl_crystal_size_mid          0.167
_exptl_crystal_size_min          0.063
_refine_diff_density_max         0.776
_refine_diff_density_min         -1.337
_refine_diff_density_rms         0.162
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     435
_refine_ls_number_reflns         7625
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0710
_refine_ls_R_factor_gt           0.0653
_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^)+(0.1368P)^2^+16.9300P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2036
_refine_ls_wR_factor_ref         0.2099
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6635
_reflns_number_total             7625
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1fd00021g2.cif
_cod_data_source_block           ZnFTzTz_sq
_cod_depositor_comments
'Adding full bibliography for 1564106--1564107.cif.'
_cod_database_code               1564107
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C20 H14 N4 O4 F2 S2 Zn1'
_shelx_estimated_absorpt_t_max   0.833
_shelx_estimated_absorpt_t_min   0.562
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 F1-C15 \\sim F1A-C13
 with sigma of 0.02
 F2-C24 \\sim F2A-C26
 with sigma of 0.02
3. Others
 Sof(H15)=Sof(F1A)=1-FVAR(1)
 Sof(F1)=Sof(H13)=FVAR(1)
 Sof(H24)=Sof(F2A)=1-FVAR(2)
 Sof(H26)=Sof(F2)=FVAR(2)
4.a Aromatic/amide H refined with riding coordinates:
 C25(H25), C15(H15), C31(H31), C32(H32), C9(H9), C26(H26), C7(H7), C4(H4),
 C16(H16), C3(H3), C10(H10), C8(H8), C24(H24), C23(H23), C29(H29), C13(H13),
 C30(H30), C14(H14)
;
_smtbx_masks_special_details
;
Channels containing disordered and only partially 
resolved dimethylformamide solvate molecules were 
accommodated in the refinement model with the use 
of SQUEEZE; Spek, A.L. (2015). Acta Cryst. C71, 9-19.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              80553
_shelx_fab_checksum              33209
_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 1.622
_oxdiff_exptl_absorpt_empirical_full_min 0.781