Halogenated Metal-Organic Framework Glasses and Liquids.
Hou, Jingwei; Rios, Laura; Krajnc, Andraž; McCaul, Aoife; Li, Shichun; Bumstead, Alice; Sapnik, Adam; Deng, Zeyu; Lin, Rijia; Chater, Philip A.; Keeble, Dean S.; Keen, David A.; Appadoo, Dominique; Chan, Bun; Chen, Vicki; Mali, Gregor; Bennett, Thomas D.; Journal of the American Chemical Society  (2020) –; doi:10.1021/jacs.9b11639

data_4134162
_publ_section_title
;
 Halogenated Metal-Organic Framework Glasses and Liquids.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.9b11639
_journal_year                    2020
_chemical_formula_moiety         'C14.73 H12 F0.68 N8 Zn2'
_chemical_formula_sum            'C14.73 H12 F0.68 N8 Zn2'
_chemical_formula_weight         444.77
_chemical_melting_point          '694 K (onset)'
_chemical_name_common            ZIF-UC-4
_chemical_name_systematic        Zn(Im)1.66(FbIm)0.34
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.6970(8)
_cell_length_b                   15.9694(10)
_cell_length_c                   17.9282(16)
_cell_measurement_reflns_used    2234
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      62.5330
_cell_measurement_theta_min      4.6600
_cell_volume                     4494.1(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_measured_fraction_theta_full 0.9261
_diffrn_measured_fraction_theta_max 0.9912
_diffrn_measurement_details
;
  1 omega   17.00   59.00   1.0000  118.5550
omega____ theta____ kappa____ phi______ frames
    -       51.2500   61.0000   60.0000 42

  2 omega   77.00  104.00   1.0000  118.5550
omega____ theta____ kappa____ phi______ frames
    -       51.2500   61.0000   60.0000 27

  3 omega   98.00  130.00   1.0000  118.5550
omega____ theta____ kappa____ phi______ frames
    -       51.2500  125.0000   90.0000 32

  4 omega   73.00  102.00   1.0000  118.5550
omega____ theta____ kappa____ phi______ frames
    -      102.5000   65.0000   60.0000 29

  5 omega  129.00  167.00   1.0000  118.5550
omega____ theta____ kappa____ phi______ frames
    -      102.5000   11.0000   30.0000 38

  6 omega  116.00  176.00   1.0000  118.5550
omega____ theta____ kappa____ phi______ frames
    -      102.5000  -21.0000  -60.0000 60

  7 omega   79.00  175.00   1.0000  118.5550
omega____ theta____ kappa____ phi______ frames
    -      102.5000  104.0000  -60.0000 96

  8 omega   76.00  119.00   1.0000  118.5550
omega____ theta____ kappa____ phi______ frames
    -       51.2500  125.0000 -120.0000 43

  9 omega   82.00  127.00   1.0000  118.5550
omega____ theta____ kappa____ phi______ frames
    -       51.2500  125.0000 -180.0000 45

 10 omega   43.00   86.00   1.0000   29.6400
omega____ theta____ kappa____ phi______ frames
    -        0.0000  178.0000 -180.0000 43

 11 omega   66.00  149.00   1.0000  118.5550
omega____ theta____ kappa____ phi______ frames
    -      102.5000  138.0000    0.0000 83

 12 omega   54.00   88.00   1.0000  118.5550
omega____ theta____ kappa____ phi______ frames
    -      102.5000   11.0000   30.0000 34

 13 omega   43.00   69.00   1.0000  118.5550
omega____ theta____ kappa____ phi______ frames
    -      102.5000  -32.0000  -60.0000 26

 14 omega   39.00   85.00   1.0000  118.5550
omega____ theta____ kappa____ phi______ frames
    -      102.5000  -54.0000  -90.0000 46

 15 omega   42.00   67.00   1.0000  118.5550
omega____ theta____ kappa____ phi______ frames
    -      102.5000 -104.0000 -150.0000 25

 16 omega   24.00   49.00   1.0000  118.5550
omega____ theta____ kappa____ phi______ frames
    -      102.5000  -43.0000    0.0000 25

 17 omega   24.00   75.00   1.0000  118.5550
omega____ theta____ kappa____ phi______ frames
    -      102.5000 -104.0000   30.0000 51

 18 omega   19.00   54.00   1.0000  118.5550
omega____ theta____ kappa____ phi______ frames
    -      102.5000 -104.0000   60.0000 35

 19 omega   33.00   67.00   1.0000   29.6400
omega____ theta____ kappa____ phi______ frames
    -        0.0000 -178.0000  -90.0000 34

 20 omega  -68.00   31.00   1.0000  118.5550
omega____ theta____ kappa____ phi______ frames
    -      -51.2500   30.0000 -120.0000 99

;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0505883000
_diffrn_orient_matrix_UB_12      -0.0556197000
_diffrn_orient_matrix_UB_13      0.0544765000
_diffrn_orient_matrix_UB_21      -0.0173745000
_diffrn_orient_matrix_UB_22      0.0768162000
_diffrn_orient_matrix_UB_23      0.0497387000
_diffrn_orient_matrix_UB_31      -0.0822364000
_diffrn_orient_matrix_UB_32      0.0179216000
_diffrn_orient_matrix_UB_33      -0.0440624000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0308
_diffrn_reflns_av_sigmaI/netI    0.0486
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            11053
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        66.9682
_diffrn_reflns_theta_max         64.1726
_diffrn_reflns_theta_min         2.8151
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.78170
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.50656
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET)
(compiled Aug  4 2014,14:34:23)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Pink
_exptl_crystal_density_diffrn    1.314
_exptl_crystal_description       Tetrahedral
_exptl_crystal_F_000             1983.28
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.606
_refine_diff_density_min         -0.575
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     232
_refine_ls_number_reflns         3717
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.1017
_refine_ls_R_factor_gt           0.0663
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1119P)^2^+3.8564P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1901
_refine_ls_wR_factor_ref         0.2174
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2405
_reflns_number_total             3717
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b11639_si_003.cif
_cod_data_source_block           shelx
_cod_database_code               4134162
_shelx_shelxl_version_number     2018/3
_reflns_odcompleteness_completeness 92.61
_reflns_odcompleteness_theta     66.97
_reflns_odcompleteness_iscentric 1
_shelx_res_checksum              69869
_shelx_hkl_checksum              57585