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_4128647
_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(C97.28 H96.64 N64 Zn16), 0.5(C3 H7 N O), 0.13(O)'
_chemical_formula_sum            'C7.58 H9.54 N4.5 O0.62 Zn'
_chemical_formula_weight         239.07
_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                   15.4061(8)
_cell_length_b                   15.2810(11)
_cell_length_c                   18.2918(14)
_cell_measurement_reflns_used    3797
_cell_measurement_temperature    100.0(5)
_cell_measurement_theta_max      32.1600
_cell_measurement_theta_min      2.6750
_cell_volume                     4306.3(5)
_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(5)
_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     -3.00  96.00   1.00   25.00    --   25.87  77.00  90.00   99
  2  \w     38.00  76.00   1.00   25.00    --   25.87  77.00-150.00   38
  3  \w     45.00  84.00   1.00   25.00    --   25.87  77.00 -60.00   39
;
_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      -0.0388354000
_diffrn_orient_matrix_UB_12      -0.0249062000
_diffrn_orient_matrix_UB_13      -0.0009788000
_diffrn_orient_matrix_UB_21      0.0220258000
_diffrn_orient_matrix_UB_22      -0.0357681000
_diffrn_orient_matrix_UB_23      0.0163146000
_diffrn_orient_matrix_UB_31      -0.0112818000
_diffrn_orient_matrix_UB_32      0.0159210000
_diffrn_orient_matrix_UB_33      0.0351693000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0363
_diffrn_reflns_av_unetI/netI     0.0392
_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       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            15439
_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         28.997
_diffrn_reflns_theta_min         2.227
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.252
_exptl_absorpt_correction_T_max  0.639
_exptl_absorpt_correction_T_min  0.434
_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    1.475
_exptl_crystal_description       prism
_exptl_crystal_F_000             1944
_exptl_crystal_size_max          0.546
_exptl_crystal_size_mid          0.386
_exptl_crystal_size_min          0.275
_refine_diff_density_max         0.586
_refine_diff_density_min         -0.466
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     327
_refine_ls_number_reflns         5720
_refine_ls_number_restraints     131
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0655
_refine_ls_R_factor_gt           0.0419
_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^)+(0.0459P)^2^+4.5189P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0997
_refine_ls_wR_factor_ref         0.1149
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4181
_reflns_number_total             5720
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            asZIF-62-Zn-bim_0-02_final.cif
_cod_data_source_block           ZIF-62-Zn-bim_0-02
_cod_original_cell_volume        4306.2(5)
_cod_original_formula_sum        'C7.58 H9.54 N4.50 O0.62 Zn'
_cod_database_code               4128647
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Zn N4 C6 H6'
_chemical_oxdiff_usercomment     'MK134 210:1'
_shelx_estimated_absorpt_t_max   0.576
_shelx_estimated_absorpt_t_min   0.373
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_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
 O01-C01B \\sim O01-C01A
 with sigma of 0.02
 N01B-C02B \\sim N01B-C03B \\sim N01A-C02A \\sim N01A-C03A
 with sigma of 0.02
 C13-C12 \\sim C17-C12 \\sim C17-C16 \\sim C16-C15 \\sim C14-C15 \\sim C14-C13
 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(C03B) \\sim Ueq, Uanis(C02B) \\sim Ueq, Uanis(C03A) \\sim Ueq,
Uanis(C02A) \\sim Ueq, Uanis(N01A) \\sim Ueq, Uanis(N01B) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 C01B, N01B, C03B, C02B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C01A, N01A, C03A, C02A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: 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(0.5) H01A(0.5) C02A(0.5) H02A(0.5) H02B(0.5)
 H02C(0.5) C03A(0.5) H03A(0.5) H03B(0.5) H03C(0.5) C03B(0.5) H03D(0.5)
 H03E(0.5) H03F(0.5) C01B(0.5) H01B(0.5) C02B(0.5) H02D(0.5) H02E(0.5)
 H02F(0.5) N01A(0.5) N01B(0.5) H12(0.96) H13(0.96) O02(0.25) C15(0.04)
 H15(0.04) C16(0.04) H16(0.04) C17(0.04) H17(0.04) C14(0.04) H14(0.04)
6.a Aromatic/amide H refined with riding coordinates:
 C11(H11), 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),
 C12(H12), C13(H13), C15(H15), C16(H16), C17(H17), C14(H14)
6.b Idealised Me refined as rotating group:
 C02A(H02A,H02B,H02C), C03A(H03A,H03B,H03C), C03B(H03D,H03E,H03F), C02B(H02D,
 H02E,H02F)
;
_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 1.102
_oxdiff_exptl_absorpt_empirical_full_min 0.941