Investigating the Melting Behaviour of Polymorphic Zeolitic Imidazolate Frameworks
Bumstead, Alice M.; Gómez, María Laura Ríos; Thorne, Michael Francis; Sapnik, Adam F.; Longley, Louis; Tuffnell, Joshua Mark; Keeble, Dean S.; Keen, David A.; Bennett, Thomas Douglas; CrystEngComm  (2020) –; doi:10.1039/D0CE00408A

data_7240461
_publ_section_title
;
 Investigating the Melting Behaviour of Polymorphic Zeolitic Imidazolate
 Frameworks
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D0CE00408A
_journal_year                    2020
_chemical_formula_moiety         'Zn1.00 C10.00 N4 H9.20 O0.33'
_chemical_formula_sum            'C240 H220.8 N96 O8 Zn24'
_chemical_formula_weight         256.08
_chemical_name_common            'ZIF-76 mbIm'
_chemical_name_systematic        Zn(Im)1.20(ClFbIm)0.80
_space_group_crystal_system      cubic
_space_group_IT_number           215
_space_group_name_Hall           'P -4 2 3'
_space_group_name_H-M_alt        'P -4 3 m'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2020-03-15 deposited with the CCDC.	2020-05-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            24
_cell_length_a                   22.6840(6)
_cell_length_b                   22.6840(6)
_cell_length_c                   22.6840(6)
_cell_measurement_reflns_used    2610
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      59.8430
_cell_measurement_theta_min      2.7510
_cell_volume                     11672.4(5)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET)
(compiled Aug  4 2014,14:34:23)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET)
(compiled Aug  4 2014,14:34:23)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET)
(compiled Aug  4 2014,14:34:23)
;
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SUPERFLIP (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1183
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.994
_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    -48.00 -11.00   1.00    2.52    --    0.00 106.00 -72.00   37
  2  \w     80.00 107.00   1.00   10.09    --   51.25  98.00  67.00   27
  3  \w     83.00 114.00   1.00   10.09    --   51.25 115.00 151.00   31
  4  \w    122.00 169.00   1.00   10.09    --  102.50  32.00 120.00   47
  5  \w    116.00 156.00   1.00   10.09    --  102.50 -21.00 -60.00   40
  6  \w     94.00 128.00   1.00   10.09    --   51.25 106.00 -72.00   34
  7  \w     60.00  86.00   1.00   10.09    --  102.50  32.00 120.00   26
  8  \w     25.00  74.00   1.00   10.09    --  102.50 -46.00  -5.00   49
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0296
_diffrn_reflns_av_sigmaI/netI    0.0304
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            9161
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.944
_diffrn_reflns_theta_full        64.5587
_diffrn_reflns_theta_max         63.881
_diffrn_reflns_theta_min         2.755
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.643
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73424
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.865
_exptl_crystal_description       cubic
_exptl_crystal_F_000             3216
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.413
_refine_diff_density_min         -0.518
_refine_diff_density_rms         0.146
_refine_ls_abs_structure_details
;
 Flack x determined using 787 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.51(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.365
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     175
_refine_ls_number_reflns         3425
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.365
_refine_ls_R_factor_all          0.1424
_refine_ls_R_factor_gt           0.1156
_refine_ls_shift/su_max          0.107
_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          0.2989
_refine_ls_wR_factor_ref         0.3534
_reflns_Friedel_coverage         0.756
_reflns_Friedel_fraction_full    0.945
_reflns_Friedel_fraction_max     0.885
_reflns_number_gt                2366
_reflns_number_total             3425
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce00408a2.cif
_cod_data_source_block           shelx
_cod_original_cell_volume        11672.4(9)
_cod_original_formula_sum        'Zn24 C240 H220.8 N96 O8'
_cod_database_code               7240461
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              69394