Meltable Mixed-Linker Zeolitic Imidazolate Frameworks and Their Microporous Glasses: From Melting Point Engineering to Selective Hydrocarbon Sorption.
Frentzel-Beyme, Louis; Kloß, Marvin; Kolodzeiski, Pascal; Pallach, Roman; Henke, Sebastian; Journal of the American Chemical Society 141 (2019) 12362–12371; doi:10.1021/jacs.9b05558

data_4128648
_publ_section_title
;
 Meltable Mixed-Linker Zeolitic Imidazolate Frameworks and Their
 Microporous Glasses: From Melting Point Engineering to Selective
 Hydrocarbon Sorption.
;
_journal_issue                   31
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12362
_journal_page_last               12371
_journal_paper_doi               10.1021/jacs.9b05558
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         '0.06(C106.88 H98.88 N64 Zn16)'
_chemical_formula_sum            'C6.68 H6.18 N4 Zn'
_chemical_formula_weight         207.87
_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_date             2018-06-15
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3510 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   15.4399(4)
_cell_length_b                   15.4843(6)
_cell_length_c                   18.1529(6)
_cell_measurement_reflns_used    9122
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      27.6160
_cell_measurement_theta_min      2.6310
_cell_volume                     4339.9(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0560
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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     34.00 110.00   0.50    5.00    --   33.45 179.00 -60.00  152
  2  \w     34.00 110.00   0.50    5.00    --   33.45 179.00 150.00  152
  3  \w    -11.00 106.00   0.50    5.00    --   33.45  19.00-150.00  234
  4  \w     28.00 128.00   0.50    5.00    --   98.33 -77.00-120.00  200
  5  \w     68.00 168.00   0.50    5.00    --   98.33  77.00   0.00  200
  6  \w     79.00 171.00   0.50    5.00    --   98.33 112.00  90.00  184
  7  \w     77.00 166.00   0.50    5.00    --   98.33  61.00-120.00  178
  8  \w     27.00 109.00   0.50    5.00    --   98.33 -95.00 120.00  164
  9  \w      3.00 104.00   0.50    5.00    --   33.45  77.00 -60.00  202
 10  \w     13.00 102.00   0.50    5.00    --   33.45  57.00  60.00  178
 11  \w     77.00 166.00   0.50    5.00    --   98.33  61.00-180.00  178
 12  \w     77.00 166.00   0.50    5.00    --   98.33  61.00  60.00  178
 13  \w     69.00 102.00   0.50    5.00    --   98.33  30.00 150.00   66
 14  \w     77.00 166.00   0.50    5.00    --   98.33  61.00 -60.00  178
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0294922000
_diffrn_orient_matrix_UB_12      0.0235392000
_diffrn_orient_matrix_UB_13      0.0221744000
_diffrn_orient_matrix_UB_21      0.0083236000
_diffrn_orient_matrix_UB_22      -0.0376434000
_diffrn_orient_matrix_UB_23      0.0211255000
_diffrn_orient_matrix_UB_31      0.0342450000
_diffrn_orient_matrix_UB_32      -0.0111428000
_diffrn_orient_matrix_UB_33      -0.0242905000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0478
_diffrn_reflns_av_unetI/netI     0.0255
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            41627
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.998
_diffrn_reflns_theta_min         2.244
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.219
_exptl_absorpt_correction_T_max  0.703
_exptl_absorpt_correction_T_min  0.528
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.273
_exptl_crystal_description       prism
_exptl_crystal_F_000             1668
_exptl_crystal_size_max          0.408
_exptl_crystal_size_mid          0.327
_exptl_crystal_size_min          0.245
_refine_diff_density_max         1.269
_refine_diff_density_min         -0.401
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         5767
_refine_ls_number_restraints     63
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.0628
_refine_ls_R_factor_gt           0.0516
_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^)+(0.0493P)^2^+7.6871P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1286
_refine_ls_wR_factor_ref         0.1346
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4704
_reflns_number_total             5767
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            asZIF-62-Zn-bim_0-17_final.cif
_cod_data_source_block           ZIF-62-Zn-bim_0-17
_cod_database_code               4128648
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Zn N4 C6 H6'
_chemical_oxdiff_usercomment     'MK87 ZIF-62 - 28:1'
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C23B-C22B \\sim C23A-C22A
 with sigma of 0.02
 N21-C22A \\sim N21-C22B
 with sigma of 0.02
 N22-C23A \\sim N22-C23B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C22A \\sim C22B \\sim C23A \\sim C23B: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
Uanis(C17) \\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C14)
\\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.1
4. Others
 Fixed Sof: H12(0.5) H13(0.5) C14(0.34) H14(0.34) C15(0.34) H15(0.34)
 C16(0.34) H16(0.34) C17(0.34) H17(0.34) C22A(0.5) H22A(0.5) C22B(0.5)
 H22B(0.5) C23A(0.5) H23A(0.5) C23B(0.5) H23B(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C11(H11), C12(H12), C13(H13), C14(H14), C15(H15), C16(H16), C17(H17),
 C21(H21), C22A(H22A), C22B(H22B), C23A(H23A), C23B(H23B), C31(H31), C32(H32),
 C33(H33), C41(H41), C42(H42), C43(H43)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.079
_oxdiff_exptl_absorpt_empirical_full_min 0.922