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_4134160
_publ_section_title
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 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
'(C13.88 H13.13 Cl0.38 N8 Zn2)*0.780(C3 H7 N1 O1)'
_chemical_formula_sum            'C16.22 H18.58 Cl0.38 N8.78 O0.78 Zn2'
_chemical_formula_weight         493.27
_chemical_melting_point          '663 K (onset)'
_chemical_name_common            ZIF-UC-3
_chemical_name_systematic        Zn(Im)1.81(ClmbIm)0.19
_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   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                   15.8749(6)
_cell_length_b                   16.2805(6)
_cell_length_c                   18.0681(6)
_cell_measurement_reflns_used    2569
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      62.3230
_cell_measurement_theta_min      4.5880
_cell_volume                     4669.7(3)
_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_area_resol_mean 16.1183
_diffrn_measured_fraction_theta_full 0.9323
_diffrn_measured_fraction_theta_max 0.9956
_diffrn_measurement_details
;
  1 omega  -72.00  -32.00   1.0000   63.2350
omega____ theta____ kappa____ phi______ frames
    -      -51.2500  -61.0000  -30.0000 40

  2 omega -125.00  -48.00   1.0000   63.2350
omega____ theta____ kappa____ phi______ frames
    -      -51.2500  -61.0000   60.0000 77

  3 omega   75.00  130.00   1.0000   63.2350
omega____ theta____ kappa____ phi______ frames
    -       51.2500  125.0000  150.0000 55

  4 omega   40.00   90.00   1.0000   15.8100
omega____ theta____ kappa____ phi______ frames
    -        0.0000  178.0000    0.0000 50

  5 omega   74.00  126.00   1.0000   63.2350
omega____ theta____ kappa____ phi______ frames
    -       51.2500  125.0000 -120.0000 52

  6 omega   95.00  121.00   1.0000   63.2350
omega____ theta____ kappa____ phi______ frames
    -      102.5000   65.0000 -150.0000 26

  7 omega  129.00  177.00   1.0000   63.2350
omega____ theta____ kappa____ phi______ frames
    -      102.5000   65.0000 -150.0000 48

  8 omega  120.00  170.00   1.0000   63.2350
omega____ theta____ kappa____ phi______ frames
    -      102.5000  -21.0000  -30.0000 50

  9 omega  119.00  153.00   1.0000   63.2350
omega____ theta____ kappa____ phi______ frames
    -      102.5000  -21.0000    0.0000 34

 10 omega  112.00  176.00   1.0000   63.2350
omega____ theta____ kappa____ phi______ frames
    -      102.5000  -21.0000   30.0000 64

 11 omega   88.00  131.00   1.0000   63.2350
omega____ theta____ kappa____ phi______ frames
    -      102.5000  -65.0000   60.0000 43

 12 omega   49.00   75.00   1.0000   63.2350
omega____ theta____ kappa____ phi______ frames
    -      102.5000  -65.0000   60.0000 26

 13 omega   45.00   71.00   1.0000   63.2350
omega____ theta____ kappa____ phi______ frames
    -      102.5000  -54.0000   90.0000 26

 14 omega   34.00   64.00   1.0000   63.2350
omega____ theta____ kappa____ phi______ frames
    -      102.5000  -54.0000  120.0000 30

 15 omega   30.00   70.00   1.0000   63.2350
omega____ theta____ kappa____ phi______ frames
    -      102.5000  -43.0000  150.0000 40

 16 omega   25.00   69.00   1.0000   63.2350
omega____ theta____ kappa____ phi______ frames
    -      102.5000  -32.0000   60.0000 44

 17 omega   23.00   56.00   1.0000   63.2350
omega____ theta____ kappa____ phi______ frames
    -      102.5000  -32.0000  -30.0000 33

 18 omega   33.00   64.00   1.0000   63.2350
omega____ theta____ kappa____ phi______ frames
    -      102.5000  -32.0000  -60.0000 31

 19 omega   37.00   72.00   1.0000   63.2350
omega____ theta____ kappa____ phi______ frames
    -      102.5000  -43.0000  -90.0000 35

 20 omega   24.00   49.00   1.0000   63.2350
omega____ theta____ kappa____ phi______ frames
    -      102.5000  -32.0000  -90.0000 25

 21 omega   39.00   90.00   1.0000   15.8100
omega____ theta____ kappa____ phi______ frames
    -        0.0000  178.0000  150.0000 51
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0640141000
_diffrn_orient_matrix_UB_12      -0.0691849000
_diffrn_orient_matrix_UB_13      0.0147242000
_diffrn_orient_matrix_UB_21      -0.0619388000
_diffrn_orient_matrix_UB_22      0.0401654000
_diffrn_orient_matrix_UB_23      -0.0547494000
_diffrn_orient_matrix_UB_31      0.0384696000
_diffrn_orient_matrix_UB_32      -0.0504888000
_diffrn_orient_matrix_UB_33      -0.0637378000
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0422
_diffrn_reflns_av_sigmaI/netI    0.0466
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            11002
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        66.9682
_diffrn_reflns_theta_max         64.1878
_diffrn_reflns_theta_min         2.4454
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    3.10958
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74562
_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    1.401
_exptl_crystal_description       tetrahedal
_exptl_crystal_F_000             2225.76
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.932
_refine_diff_density_min         -1.143
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.205
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     232
_refine_ls_number_reflns         3879
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.406
_refine_ls_R_factor_all          0.1257
_refine_ls_R_factor_gt           0.0968
_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^)+(0.1893P)^2^+3.7539P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2950
_refine_ls_wR_factor_ref         0.3257
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2794
_reflns_number_total             3879
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b11639_si_002.cif
_cod_data_source_block           shelx
_cod_database_code               4134160
_shelx_shelxl_version_number     2018/3
_reflns_odcompleteness_completeness 93.23
_reflns_odcompleteness_theta     66.97
_reflns_odcompleteness_iscentric 1
_shelx_res_checksum              84933
_shelx_hkl_checksum              49848