Torsional flexibility in zinc-benzenedicarboxylate metal-organic frameworks.
Meekel, Emily G.; Nicholas, Thomas C.; Slater, Ben; Goodwin, Andrew L.; CrystEngComm 26 (2024) 673–680; doi:10.1039/d3ce01078c

data_7247930
_publ_section_title
;
 Torsional flexibility in zinc-benzenedicarboxylate metal-organic
 frameworks.
;
_journal_issue                   5
_journal_name_full               CrystEngComm
_journal_page_first              673
_journal_page_last               680
_journal_paper_doi               10.1039/d3ce01078c
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety         'C8 H3 Br0.408 Cl0.592 O4 Zn'
_chemical_formula_sum            'C8 H3 Br0.41 Cl0.59 O4 Zn'
_chemical_formula_weight         282.05
_space_group_crystal_system      trigonal
_space_group_IT_number           166
_space_group_name_Hall           '-R 3 2"'
_space_group_name_H-M_alt        'R -3 m :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-05-29
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-10-19 deposited with the CCDC.	2023-12-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   28.4902(4)
_cell_length_b                   28.4902(4)
_cell_length_c                   7.90730(10)
_cell_measurement_reflns_used    3984
_cell_measurement_temperature    295.01(10)
_cell_measurement_theta_max      75.4570
_cell_measurement_theta_min      5.3730
_cell_volume                     5558.40(13)
_computing_cell_refinement       'CrysAlisPro 1.171.41.83a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.83a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.83a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      295.01(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 13.3333
_diffrn_detector_type            'Eiger 1M'
_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     20.00  81.00   0.50    0.10    --   42.29-107.00 156.00  122
  2  \w    138.00 163.00   0.50    0.10    --  110.00 107.00-104.00   50
  3  \w    108.00 134.00   0.50    0.10    --  110.00 -84.00 159.00   52
  4  \w     42.00  83.00   0.50    0.10    --  110.00 -84.00 159.00   82
  5  \w    -10.00  36.00   0.50    0.10    --  -44.75  15.00 -90.00   92
  6  \w     -7.00  36.00   0.50    0.10    --  -44.75  15.00 -30.00   86
  7  \w    -25.00  20.00   0.50    0.10    --  -44.75  15.00-180.00   90
  8  \w     87.00 128.00   0.50    0.10    --  110.00  61.00  30.00   82
  9  \w    136.00 173.00   0.50    0.10    --  110.00  61.00-120.00   74
 10  \w     45.00  73.00   0.50    0.10    --  110.00 -70.00  38.00   56
 11  \w     38.00 112.00   0.50    0.10    --  110.00-125.00  30.00  148
 12  \w    121.00 159.00   0.50    0.10    --  110.00  61.00-150.00   76
 13  \w     89.00 115.00   0.50    0.10    --  110.00  61.00-150.00   52
 14  \w     91.00 124.00   0.50    0.10    --  110.00  61.00-120.00   66
 15  \w     44.00  69.00   0.50    0.10    --  110.00 -63.00 171.00   50
 16  \w     35.00  76.00   0.50    0.10    --  110.00 -95.00 -90.00   82
 17  \w    137.00 177.00   0.50    0.10    --  110.00  63.00 -51.00   80
 18  \w    102.00 134.00   0.50    0.10    --  110.00  63.00 -51.00   64
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, Eiger 1M'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0544673000
_diffrn_orient_matrix_UB_12      -0.0030364000
_diffrn_orient_matrix_UB_13      0.0383342000
_diffrn_orient_matrix_UB_21      -0.0263376000
_diffrn_orient_matrix_UB_22      -0.0394820000
_diffrn_orient_matrix_UB_23      -0.1490510000
_diffrn_orient_matrix_UB_31      -0.0153946000
_diffrn_orient_matrix_UB_32      -0.0482691000
_diffrn_orient_matrix_UB_33      0.1195157000
_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  0.0330
_diffrn_reflns_av_unetI/netI     0.0201
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            7373
_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         75.614
_diffrn_reflns_theta_min         5.379
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.419
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54812
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.83a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.517
_exptl_crystal_description       rod
_exptl_crystal_F_000             2472
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.701
_refine_diff_density_min         -1.139
_refine_diff_density_rms         0.155
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     70
_refine_ls_number_reflns         1362
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.0560
_refine_ls_R_factor_gt           0.0541
_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^)+(0.1242P)^2^+16.9618P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1769
_refine_ls_wR_factor_ref         0.1792
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1278
_reflns_number_total             1362
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce01078c1.cif
_cod_data_source_block           em-01-81_1
_cod_depositor_comments
'Adding full bibliography for 7247925--7247930.cif.'
_cod_original_cell_volume        5558.40(17)
_cod_original_sg_symbol_H-M      'R -3 m'
_cod_database_code               7247930
_shelx_shelxl_version_number     2019/1
_chemical_oxdiff_formula         'Zn1 Br0.5 Cl0.5 C8 O4 H3'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Shared sites
{Br, Cl1}
3. Uiso/Uaniso restraints and constraints
Uanis(Cl1) = Uanis(Br)
Uanis(Br) = Uanis(Cl1)
4. Others
 Sof(Cl1)=0.5*(1-FVAR(2))
 Sof(Br)=0.5*FVAR(2)
5.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4)
;
_shelx_res_checksum              18840
_ins_header
;
TITL EM-01-81_1 in R-3m 
REM R-3m (#166 in standard setting)
CELL 1.54184  28.490246  28.490246   7.907254  90.0000  90.0000 120.0000
ZERR   23.00   0.000419   0.000419   0.000130   0.0000   0.0000   0.0000
LATT  3
SYMM -y, x-y, z 
SYMM -x+y,-x, z 
SYMM  y, x,-z 
SYMM  x-y,-y,-z 
SYMM -x,-x+y,-z 
SFAC C H O Cl Zn Br
UNIT 184.00 69.00 92.00 11.50 23.00 11.50
REM  CrysAlisPro recorded range (K): Min=295.0; max=295.0; aver:295.0
TEMP 22
TREF
HKLF 4
END
;
_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 1.745
_oxdiff_exptl_absorpt_empirical_full_min 0.636