Multivariate zeolitic imidazolate frameworks with an inverting trend in flexibility
Halder, Arijit; Klein, Ryan A.; Lively, Rachel; McGuirk, C. Michael; Chemical Communications  (2022) –; doi:10.1039/D2CC04362A

data_7130753
_publ_section_title
;
 Multivariate zeolitic imidazolate frameworks with an inverting trend in
 flexibility
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC04362A
_journal_year                    2022
_chemical_formula_moiety         'C42.588 H30 Cd3 F1.177 N12'
_chemical_formula_sum            'C42.59 H30 Cd3 F1.18 N12'
_chemical_formula_weight         1069.41
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-I 2y'
_space_group_name_H-M_alt        'I 1 2/m 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-03-15
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-08-04 deposited with the CCDC.	2022-09-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.481(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.0043(13)
_cell_length_b                   23.0932(17)
_cell_length_c                   16.3664(17)
_cell_measurement_reflns_used    4493
_cell_measurement_temperature    99.98(15)
_cell_measurement_theta_max      64.4050
_cell_measurement_theta_min      3.2620
_cell_volume                     5589.2(10)
_computing_cell_refinement       'CrysAlisPro 1.171.41.121a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.121a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.121a (Rigaku OD, 2021)'
_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  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.98(15)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.958
_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    -19.00   6.00   0.50    0.50    --   -0.16 -98.00 -96.00   50
  2  \w    -28.00  -3.00   0.50    0.50    --   -0.16  98.00  10.00   50
  3  \w    101.00 126.00   0.50   10.00    --   88.66  98.00  10.00   50
  4  \w     48.00 105.00   0.50   10.00    --   88.66 -98.00 -96.00  114
  5  \w    -98.00 -18.00   0.50   10.00    --  -88.97  98.00  10.00  160
  6  \w   -148.00-123.00   0.50   10.00    --  -88.97 -98.00 -96.00   50
  7  \w    -14.00  25.00   0.50    0.50    --   -0.16 -99.00   0.00   78
  8  \w    -13.00  13.00   0.50    0.50    --   -0.16 -99.00-180.00   52
  9  \w    -16.00  19.00   0.50    0.50    --   -0.16 -99.00-150.00   70
 10  \w    -17.00  29.00   0.50    0.50    --   -0.16 -99.00  90.00   92
 11  \w     17.00  44.00   0.50   10.00    --   88.66 -37.00 -60.00   54
 12  \w     16.00  43.00   0.50   10.00    --   88.66 -37.00 -30.00   54
 13  \w     78.00 106.00   0.50   10.00    --   88.66  37.00 -90.00   56
 14  \w     21.00  65.00   0.50   10.00    --   88.66 -57.00  60.00   88
 15  \w     25.00  58.00   0.50   10.00    --   88.66 -57.00 120.00   66
 16  \w     16.00  41.00   0.50   10.00    --   88.66 -37.00  90.00   50
 17  \w    131.00 160.00   0.50   10.00    --   88.66  37.00 -90.00   58
 18  \w     16.00  41.00   0.50   10.00    --   88.66 -37.00 -90.00   50
 19  \w     17.00  44.00   0.50   10.00    --   88.66 -37.00  60.00   54
 20  \w    -64.00 -30.00   0.50   10.00    --  -88.97  57.00   0.00   68
 21  \w    -61.00 -16.00   0.50   10.00    --  -88.97  57.00 -30.00   90
 22  \w   -157.00 -83.00   0.50   10.00    --  -88.97 -37.00 -90.00  148
 23  \w   -149.00 -76.00   0.50   10.00    --  -88.97 -37.00-120.00  146
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0418657000
_diffrn_orient_matrix_UB_12      -0.0461215000
_diffrn_orient_matrix_UB_13      -0.0409700000
_diffrn_orient_matrix_UB_21      -0.0025008000
_diffrn_orient_matrix_UB_22      0.0432721000
_diffrn_orient_matrix_UB_23      -0.0724826000
_diffrn_orient_matrix_UB_31      0.0954078000
_diffrn_orient_matrix_UB_32      0.0212451000
_diffrn_orient_matrix_UB_33      0.0585995000
_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  0.0764
_diffrn_reflns_av_unetI/netI     0.0532
_diffrn_reflns_Laue_measured_fraction_full 0.967
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            14503
_diffrn_reflns_point_group_measured_fraction_full 0.967
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.234
_diffrn_reflns_theta_min         3.285
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.376
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68544
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.121a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.271
_exptl_crystal_description       block
_exptl_crystal_F_000             2096
_exptl_crystal_recrystallization_method
'The material was recrystallised from --- by as supplied'
_exptl_crystal_size_max          0.161
_exptl_crystal_size_mid          0.107
_exptl_crystal_size_min          0.048
_refine_diff_density_max         2.116
_refine_diff_density_min         -0.790
_refine_diff_density_rms         0.155
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.138
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     297
_refine_ls_number_reflns         5047
_refine_ls_number_restraints     329
_refine_ls_restrained_S_all      1.116
_refine_ls_R_factor_all          0.1418
_refine_ls_R_factor_gt           0.1087
_refine_ls_shift/su_max          0.002
_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          0.3121
_refine_ls_wR_factor_ref         0.3411
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2832
_reflns_number_total             5047
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc04362a2.cif
_cod_data_source_block           51MOF
_cod_original_cell_volume        5589.2(9)
_cod_database_code               7130753
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         CNHFCdOCl
_shelx_estimated_absorpt_t_max   0.662
_shelx_estimated_absorpt_t_min   0.314
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C8-C23
 1.54 with sigma of 0.02
 C11-H11
 0.95 with sigma of 0.01
 C8-H8
 0.95 with sigma of 0.01
 C12-H12
 0.95 with sigma of 0.01
 H11-C10 \\sim H11-C12
 with sigma of 0.001
 H12-C13 \\sim H12-C11
 with sigma of 0.001
 N4-H8 \\sim N3-H8
 with sigma of 0.01
3. Restrained planarity
 C10, C11, H11, H10, C12, H12, H8
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
C17 \\sim C16 \\sim C15 \\sim C6 \\sim C5 \\sim C4 \\sim C7 \\sim C3 \\sim C2:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
6. Others
 Sof(H8)=Sof(H11)=Sof(H12)=1-FVAR(1)
 Sof(F1)=Sof(F2)=Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(H23C)=FVAR(1)
7.a Me refined with riding coordinates:
 C23(H23A,H23B,H23C)
7.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C4(H4), C5(H5), C6(H6), C10(H10), C13(H13), C16(H16),
 C17(H17), C18(H18), C20(H20), C21(H21), C22(H22)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              67822
_shelx_hkl_checksum              13767
_shelx_fab_checksum              6073
_olex2_date_sample_data_collection 2022-03-10
_olex2_date_sample_submission    2022-03-07
_olex2_exptl_crystal_mounting_method 'The crystal was mounted on a mylar loop'
_olex2_submission_original_sample_id 5:1MOF
_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 2.471
_oxdiff_exptl_absorpt_empirical_full_min 0.351