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_4134161
_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         'C13.04 H12 Cl0.26 F0.26 N8 Zn2'
_chemical_formula_sum            'C13.04 H12 Cl0.26 F0.26 N8 Zn2'
_chemical_formula_weight         425.71
_chemical_melting_point          '679 K (onset)'
_chemical_name_common            ZIF-UC-2
_chemical_name_systematic        Zn(Im)1.87(ClFbIm)0.13
_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'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_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                   15.5560(5)
_cell_length_b                   15.6538(5)
_cell_length_c                   18.0875(6)
_cell_measurement_reflns_used    4413
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      63.9874
_cell_measurement_theta_min      2.4428
_cell_volume                     4404.5(2)
_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 0.9281
_diffrn_measured_fraction_theta_max 0.9966
_diffrn_measurement_details
;
  1 omega  -36.00   30.00   1.0000   14.4400
omega____ theta____ kappa____ phi______ frames
    -      -51.2500   30.0000  -30.0000 66

  2 omega   47.00   72.00   1.0000    3.6100
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000 -180.0000 25

  3 omega  -30.00   29.00   1.0000    3.6100
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000 -180.0000 59

  4 omega   53.00  109.00   1.0000   14.4400
omega____ theta____ kappa____ phi______ frames
    -       51.2500   45.0000 -180.0000 56

  5 omega  136.00  162.00   1.0000   14.4400
omega____ theta____ kappa____ phi______ frames
    -      102.5000  -21.0000  -90.0000 26

  6 omega  144.00  177.00   1.0000   14.4400
omega____ theta____ kappa____ phi______ frames
    -      102.5000   24.0000  -34.8564 33

  7 omega  147.00  172.00   1.0000   14.4400
omega____ theta____ kappa____ phi______ frames
    -      102.5000  104.0000   90.0000 25

  8 omega  100.00  132.00   1.0000   14.4400
omega____ theta____ kappa____ phi______ frames
    -      102.5000  104.0000   90.0000 32

  9 omega   82.00  108.00   1.0000   14.4400
omega____ theta____ kappa____ phi______ frames
    -      102.5000   77.0000   60.0000 26

 10 omega  112.00  176.00   1.0000   14.4400
omega____ theta____ kappa____ phi______ frames
    -      102.5000  -21.0000  120.0000 64

 11 omega   59.00   85.00   1.0000   14.4400
omega____ theta____ kappa____ phi______ frames
    -      102.5000  -54.0000   60.0000 26

 12 omega   41.00   72.00   1.0000   14.4400
omega____ theta____ kappa____ phi______ frames
    -      102.5000 -104.0000  120.0000 31

 13 omega   22.00   56.00   1.0000   14.4400
omega____ theta____ kappa____ phi______ frames
    -      102.5000  -32.0000   30.0000 34

 14 omega   34.00   68.00   1.0000   14.4400
omega____ theta____ kappa____ phi______ frames
    -      102.5000  -43.0000    0.0000 34

 15 omega   32.00   65.00   1.0000   14.4400
omega____ theta____ kappa____ phi______ frames
    -      102.5000  -32.0000  -30.0000 33

 16 omega   25.00   75.00   1.0000   14.4400
omega____ theta____ kappa____ phi______ frames
    -      102.5000  -43.0000  -90.0000 50

 17 omega   28.00   54.00   1.0000   14.4400
omega____ theta____ kappa____ phi______ frames
    -      102.5000  -32.0000 -150.0000 26

 18 omega   24.00   75.00   1.0000   14.4400
omega____ theta____ kappa____ phi______ frames
    -      102.5000  -43.0000 -150.0000 51

 19 omega   21.00   59.00   1.0000   14.4400
omega____ theta____ kappa____ phi______ frames
    -      102.5000  -32.0000  -60.0000 38

 20 omega   25.00   51.00   1.0000   14.4400
omega____ theta____ kappa____ phi______ frames
    -      102.5000  -32.0000    0.0000 26

 21 omega   33.00   58.00   1.0000   14.4400
omega____ theta____ kappa____ phi______ frames
    -      102.5000   24.0000  -34.8564 25

 22 omega   84.00  125.00   1.0000   14.4400
omega____ theta____ kappa____ phi______ frames
    -       51.2500  125.0000 -180.0000 41

 23 omega   73.00  130.00   1.0000   14.4400
omega____ theta____ kappa____ phi______ frames
    -       51.2500  125.0000 -150.0000 57

 24 omega   69.00   94.00   1.0000   14.4400
omega____ theta____ kappa____ phi______ frames
    -      102.5000  138.0000  -90.0000 25

 25 omega   35.00   60.00   1.0000    3.6100
omega____ theta____ kappa____ phi______ frames
    -        0.0000 -178.0000  -30.0000 25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0056584000
_diffrn_orient_matrix_UB_12      -0.0982359000
_diffrn_orient_matrix_UB_13      0.0000663000
_diffrn_orient_matrix_UB_21      -0.0773059000
_diffrn_orient_matrix_UB_22      0.0044068000
_diffrn_orient_matrix_UB_23      -0.0531500000
_diffrn_orient_matrix_UB_31      0.0616213000
_diffrn_orient_matrix_UB_32      -0.0035333000
_diffrn_orient_matrix_UB_33      -0.0665850000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0171
_diffrn_reflns_av_sigmaI/netI    0.0252
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            10790
_diffrn_reflns_theta_full        66.9682
_diffrn_reflns_theta_max         63.9874
_diffrn_reflns_theta_min         2.4428
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.06584
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82537
_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            white
_exptl_crystal_density_diffrn    1.283
_exptl_crystal_description       tetrahedral
_exptl_crystal_F_000             1892.48
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.757
_refine_diff_density_min         -0.482
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     251
_refine_ls_number_reflns         3641
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0535
_refine_ls_R_factor_gt           0.0459
_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^)+(0.0925P)^2^+1.6961P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1408
_refine_ls_wR_factor_ref         0.1511
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3021
_reflns_number_total             3641
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b11639_si_001.cif
_cod_data_source_block           shelx
_cod_database_code               4134161
_shelx_shelxl_version_number     2018/3
_reflns_odcompleteness_completeness 92.81
_reflns_odcompleteness_theta     66.97
_reflns_odcompleteness_iscentric 1
_shelx_res_checksum              2276
_shelx_hkl_checksum              1677