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_7130754
_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         'C82.973 H48.918 Cd6 F1.946 N24'
_chemical_formula_sum            'C82.98 H48.94 Cd6 F1.96 N24'
_chemical_formula_weight         2093.80
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-07-13
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-08-04 deposited with the CCDC.	2022-09-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 113.343(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   16.2010(13)
_cell_length_b                   23.0159(19)
_cell_length_c                   16.2213(16)
_cell_measurement_reflns_used    5856
_cell_measurement_temperature    99.99(18)
_cell_measurement_theta_max      74.5190
_cell_measurement_theta_min      3.2460
_cell_volume                     5553.5(9)
_computing_cell_refinement       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.41.123a (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  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.99(18)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.921
_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    -51.00  25.00   0.50    4.00    --  -47.19  47.00-152.00  152
  2  \w   -120.00 -34.00   0.50    4.00    --  -47.19 -47.00  58.00  172
  3  \w    -24.00  55.00   0.50    4.00    --   47.19 -47.00  58.00  158
  4  \w   -175.00 -91.00   0.50   24.00    -- -104.00 -47.00  58.00  168
  5  \w     97.00 178.00   0.50   24.00    --  110.25  47.00-152.00  162
  6  \w    -25.00  28.00   0.50    4.00    --  -47.19  19.00 -60.00  106
  7  \w    -25.00  28.00   0.50    4.00    --  -47.19  19.00   0.00  106
  8  \w     34.00 120.00   0.50    4.00    --   47.19  47.00-152.00  172
  9  \w    -69.00 -31.00   0.50   24.00    -- -104.00  61.00-120.00   76
 10  \w    -69.00 -31.00   0.50   24.00    -- -104.00  61.00 -30.00   76
 11  \w    -69.00 -31.00   0.50   24.00    -- -104.00  61.00   0.00   76
 12  \w   -112.00 -31.00   0.50   24.00    -- -104.00 125.00  60.00  162
 13  \w     38.00  73.00   0.50   24.00    --  110.25 -61.00  60.00   70
 14  \w     38.00 106.00   0.50   24.00    --  110.25 -94.00-180.00  136
 15  \w     98.00 178.00   0.50   24.00    --  110.25  45.00 120.00  160
 16  \w     98.00 178.00   0.50   24.00    --  110.25  45.00 -90.00  160
 17  \w     38.00  73.00   0.50   24.00    --  110.25 -61.00  90.00   70
 18  \w     38.00  73.00   0.50   24.00    --  110.25 -61.00 120.00   70
 19  \w     38.00 108.00   0.50   24.00    --  110.25 -77.00-150.00  140
 20  \w     38.00 106.00   0.50   24.00    --  110.25 -94.00  30.00  136
 21  \w     38.00  73.00   0.50   24.00    --  110.25 -61.00  30.00   70
 22  \w     38.00 108.00   0.50   24.00    --  110.25 -77.00 -60.00  140
 23  \w     38.00  73.00   0.50   24.00    --  110.25 -61.00   0.00   70
 24  \w     38.00  73.00   0.50   24.00    --  110.25 -61.00 150.00   70
 25  \w     38.00  73.00   0.50   24.00    --  110.25 -61.00 -30.00   70
 26  \w   -120.00 -24.00   0.50    4.00    --  -47.19 -77.00 -30.00  192
;
_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      -0.0927572500
_diffrn_orient_matrix_UB_12      0.0270591500
_diffrn_orient_matrix_UB_13      -0.0549155500
_diffrn_orient_matrix_UB_21      -0.0379213500
_diffrn_orient_matrix_UB_22      -0.0279945500
_diffrn_orient_matrix_UB_23      0.0637021500
_diffrn_orient_matrix_UB_31      0.0261635000
_diffrn_orient_matrix_UB_32      0.0545104000
_diffrn_orient_matrix_UB_33      0.0601765000
_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  0.1822
_diffrn_reflns_av_unetI/netI     0.0907
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.921
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            20592
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.921
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.038
_diffrn_reflns_theta_min         3.263
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.422
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.27740
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.123a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.252
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2041
_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         1.278
_refine_diff_density_min         -1.824
_refine_diff_density_rms         0.158
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.335
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     288
_refine_ls_number_reflns         5628
_refine_ls_number_restraints     296
_refine_ls_restrained_S_all      1.309
_refine_ls_R_factor_all          0.1896
_refine_ls_R_factor_gt           0.1411
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001
_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          0.3979
_refine_ls_wR_factor_ref         0.4508
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2602
_reflns_number_total             5628
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc04362a2.cif
_cod_data_source_block           141MOF
_cod_database_code               7130754
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'Cd CHNO'
_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
 C11-C10 \\sim C7-C1 \\sim C22-C21
 with sigma of 0.01
 C22-C22_$1 \\sim C23-C22 \\sim C24-C23 \\sim C24-C24_$1 \\sim C24_$1-C23_$1
\\sim C23_$1-C22_$1
 with sigma of 0.01
3. Restrained planarity
 N6, C21, C22, C23, C24
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
C22 \\sim C23 \\sim C24: 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 0.004 and sigma for 1-3 distances of 0.004
 C22, C23, C24
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
6. Others
 Sof(F1)=Sof(F2)=Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(H8C)=FVAR(1)
 Fixed Sof: C24(0.5) H24(0.5)
7.a Me refined with riding coordinates:
 C8(H8A,H8B,H8C)
7.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C10(H10), C12(H12), C13(H13), C14(H14), C15(H15), C17(H17),
 C19(H19), C20(H20), C21(H21), C23(H23), C24(H24)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              34179
_shelx_hkl_checksum              8018
_shelx_fab_checksum              10419
_olex2_date_sample_submission    2022-03-30
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder in paratone oil'
_olex2_submission_original_sample_id 912
_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 3.764
_oxdiff_exptl_absorpt_empirical_full_min 0.181