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_4128646
_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(C99.2 H91.2 N64 Zn16), 0.5(C3 H7 N O)'
_chemical_formula_sum            'C7.7 H9.2 N4.5 O0.5 Zn'
_chemical_formula_weight         238.17
_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                   15.4872(7)
_cell_length_b                   15.0774(11)
_cell_length_c                   18.3105(8)
_cell_measurement_reflns_used    5220
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      29.6810
_cell_measurement_theta_min      2.6190
_cell_volume                     4275.6(4)
_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      100.0(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0560
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.984
_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     -9.00  85.00   1.00   10.00    --   20.78  77.00 -90.00   94
  2  \w    -89.00 -14.00   1.00   10.00    --  -22.19 -38.00   0.00   75
  3  \w    -99.00 -40.00   1.00   10.00    --  -22.19 179.00 120.00   59
;
_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      -0.0451720000
_diffrn_orient_matrix_UB_12      0.0058473000
_diffrn_orient_matrix_UB_13      -0.0037574000
_diffrn_orient_matrix_UB_21      -0.0054142000
_diffrn_orient_matrix_UB_22      -0.0466082000
_diffrn_orient_matrix_UB_23      -0.0026799000
_diffrn_orient_matrix_UB_31      -0.0048287000
_diffrn_orient_matrix_UB_32      -0.0027773000
_diffrn_orient_matrix_UB_33      0.0384921000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0343
_diffrn_reflns_av_unetI/netI     0.0341
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            20351
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.000
_diffrn_reflns_theta_min         2.189
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.267
_exptl_absorpt_correction_T_max  0.978
_exptl_absorpt_correction_T_min  0.963
_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    1.480
_exptl_crystal_description       prism
_exptl_crystal_F_000             1934
_exptl_crystal_size_max          0.397
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.208
_refine_diff_density_max         0.707
_refine_diff_density_min         -0.566
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     338
_refine_ls_number_reflns         5594
_refine_ls_number_restraints     131
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0591
_refine_ls_R_factor_gt           0.0374
_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^)+(0.0417P)^2^+4.5346P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0888
_refine_ls_wR_factor_ref         0.1015
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4241
_reflns_number_total             5594
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            asZIF-62-Zn-bim_0-05_final.cif
_cod_data_source_block           ZIF-62-Zn-bim_0-05
_cod_original_formula_sum        'C7.70 H9.20 N4.50 O0.50 Zn'
_cod_database_code               4128646
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Zn N4 C6 H6'
_chemical_oxdiff_usercomment     'ZIF-4 mit noch weniger bim'
_shelx_estimated_absorpt_t_max   0.650
_shelx_estimated_absorpt_t_min   0.466
_reflns_odcompleteness_completeness 99.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.82
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,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
 C14-C13 \\sim C15-C14 \\sim C16-C15 \\sim C17-C16 \\sim C17-C12 \\sim C13-C12
 with sigma of 0.02
 O01-C01A \\sim O01-C01B
 with sigma of 0.02
 N01A-C03A \\sim N01A-C02A \\sim N01B-C03B \\sim N01B-C02B
 with sigma of 0.02
 N01A-C01A \\sim N01B-C01B
 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 0.01 and sigma for terminal atoms of 0.05
Uanis(N01B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 O01, C01A, C02A, C03A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C01A, N01A, C02A, C03A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C01B, N01B, C02B, C03B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: H12(0.5) H13(0.5) C14(0.1) H14(0.1) C15(0.1) H15(0.1) C16(0.1)
 H16(0.1) C17(0.1) H17(0.1) C22A(0.5) H22A(0.5) C22B(0.5) H22B(0.5) C23A(0.5)
 H23A(0.5) C23B(0.5) H23B(0.5) C01A(0.75) H01A(0.75) C02A(0.75) H02A(0.75)
 H02B(0.75) H02C(0.75) C03A(0.75) H03A(0.75) H03B(0.75) H03C(0.75) C02B(0.25)
 H02D(0.25) H02E(0.25) H02F(0.25) C03B(0.25) H03D(0.25) H03E(0.25) H03F(0.25)
 C01B(0.25) H01B(0.25) N01A(0.75) N01B(0.25)
6.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), C01A(H01A), C01B(H01B)
6.b Idealised Me refined as rotating group:
 C02A(H02A,H02B,H02C), C03A(H03A,H03B,H03C), C02B(H02D,H02E,H02F), C03B(H03D,
 H03E,H03F)
;
_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 1.163
_oxdiff_exptl_absorpt_empirical_full_min 0.906