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_4134163
_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         'C14.27 H12 Cl0.57 N8 Zn2, 0.389(C3 H7 O1 N1)'
_chemical_formula_sum            'C15.44 H14.73 Cl0.57 N8.39 O0.39 Zn2'
_chemical_formula_weight         475.04
_chemical_melting_point          '705 K (onset)'
_chemical_name_common            ZIF-UC-5
_chemical_name_systematic        Zn(Im)1.72(ClbIm)0.28
_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                   15.7260(8)
_cell_length_b                   16.0184(11)
_cell_length_c                   18.1617(10)
_cell_measurement_reflns_used    2119
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      63.0470
_cell_measurement_theta_min      4.6300
_cell_volume                     4575.0(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 0.9290
_diffrn_measured_fraction_theta_max 0.9958
_diffrn_measurement_details
;
  1 omega   13.00  130.00   1.0000   57.5950
omega____ theta____ kappa____ phi______ frames
    -       51.2500   30.0000   30.0000 117

  2 omega  121.00  168.00   1.0000   57.5950
omega____ theta____ kappa____ phi______ frames
    -      102.5000  -21.0000  -30.0000 47

  3 omega  132.00  166.00   1.0000   57.5950
omega____ theta____ kappa____ phi______ frames
    -      102.5000  -21.0000 -150.0000 34

  4 omega   87.00  114.00   1.0000   57.5950
omega____ theta____ kappa____ phi______ frames
    -      102.5000  -89.0000   30.0000 27

  5 omega   55.00   86.00   1.0000   57.5950
omega____ theta____ kappa____ phi______ frames
    -      102.5000 -104.0000  -90.0000 31

  6 omega   46.00   84.00   1.0000   57.5950
omega____ theta____ kappa____ phi______ frames
    -      102.5000 -104.0000 -150.0000 38

  7 omega   25.00   75.00   1.0000   57.5950
omega____ theta____ kappa____ phi______ frames
    -      102.5000  -43.0000 -180.0000 50

  8 omega   28.00   83.00   1.0000   57.5950
omega____ theta____ kappa____ phi______ frames
    -      102.5000  -54.0000 -120.0000 55

  9 omega   39.00   85.00   1.0000   57.5950
omega____ theta____ kappa____ phi______ frames
    -      102.5000 -104.0000    0.0000 46

 10 omega   36.00   76.00   1.0000   57.5950
omega____ theta____ kappa____ phi______ frames
    -      102.5000  -89.0000   30.0000 40

 11 omega   47.00   79.00   1.0000   57.5950
omega____ theta____ kappa____ phi______ frames
    -      102.5000 -104.0000  120.0000 32

 12 omega   40.00   67.00   1.0000   57.5950
omega____ theta____ kappa____ phi______ frames
    -      102.5000 -104.0000  150.0000 27

 13 omega   26.00   93.00   1.0000   57.5950
omega____ theta____ kappa____ phi______ frames
    -      102.5000 -120.0000   95.0000 67

 14 omega  147.00  175.00   1.0000   57.5950
omega____ theta____ kappa____ phi______ frames
    -      102.5000  -22.0000  168.0000 28

 15 omega   53.00   84.00   1.0000   14.4000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  178.0000  120.0000 31

 16 omega   99.00  127.00   1.0000   57.5950
omega____ theta____ kappa____ phi______ frames
    -       51.2500  125.0000 -120.0000 28

 17 omega   13.00   69.00   1.0000   14.4000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000 -150.0000 56

 18 omega  -27.00   -2.00   1.0000   14.4000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000 -150.0000 25

 19 omega   22.00   52.00   1.0000   57.5950
omega____ theta____ kappa____ phi______ frames
    -      102.5000 -104.0000  -90.0000 30

 20 omega   23.00   52.00   1.0000   57.5950
omega____ theta____ kappa____ phi______ frames
    -      102.5000  -32.0000 -120.0000 29

 21 omega   21.00   65.00   1.0000   57.5950
omega____ theta____ kappa____ phi______ frames
    -      102.5000  -32.0000   30.0000 44

 22 omega   15.00   76.00   1.0000   57.5950
omega____ theta____ kappa____ phi______ frames
    -       51.2500 -125.0000   90.0000 61
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0712532000
_diffrn_orient_matrix_UB_12      -0.0654909000
_diffrn_orient_matrix_UB_13      0.0076088000
_diffrn_orient_matrix_UB_21      0.0661183000
_diffrn_orient_matrix_UB_22      -0.0661070000
_diffrn_orient_matrix_UB_23      0.0226833000
_diffrn_orient_matrix_UB_31      -0.0118116000
_diffrn_orient_matrix_UB_32      0.0243753000
_diffrn_orient_matrix_UB_33      0.0814018000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0265
_diffrn_reflns_av_sigmaI/netI    0.0372
_diffrn_reflns_av_unetI/netI     0.0220
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            11094
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        66.9682
_diffrn_reflns_theta_max         64.0128
_diffrn_reflns_theta_min         2.4328
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.33097
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95391
_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    1.375
_exptl_crystal_description       tetrahedral
_exptl_crystal_F_000             2125.60
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.844
_refine_diff_density_min         -0.614
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         3786
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0872
_refine_ls_R_factor_gt           0.0646
_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^)+(0.1112P)^2^+4.3903P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1888
_refine_ls_wR_factor_ref         0.2107
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2684
_reflns_number_total             3786
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b11639_si_004.cif
_cod_data_source_block           shelx
_cod_database_code               4134163
_shelx_shelxl_version_number     2018/3
_reflns_odcompleteness_completeness 92.90
_reflns_odcompleteness_theta     66.97
_reflns_odcompleteness_iscentric 1
_shelx_res_checksum              93592
_shelx_hkl_checksum              412