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_4128634
_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(C115.2 H95.2 Co16 N64)'
_chemical_formula_sum            'C7.2 H6.6 Co N4'
_chemical_formula_weight         208.09
_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             2018-10-29
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 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                   15.342(4)
_cell_length_b                   15.808(3)
_cell_length_c                   18.030(3)
_cell_measurement_reflns_used    2230
_cell_measurement_temperature    400(2)
_cell_measurement_theta_max      26.26
_cell_measurement_theta_min      2.26
_cell_volume                     4372.7(16)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      400(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0431
_diffrn_reflns_av_unetI/netI     0.0370
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            25592
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        27.500
_diffrn_reflns_theta_max         27.994
_diffrn_reflns_theta_min         2.577
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.528
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4122
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.1029 before and 0.0668 after correction.
The Ratio of minimum to maximum transmission is 0.5528.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'dark violet'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.264
_exptl_crystal_description       prism
_exptl_crystal_F_000             1677
_exptl_crystal_size_max          0.765
_exptl_crystal_size_mid          0.726
_exptl_crystal_size_min          0.599
_refine_diff_density_max         0.365
_refine_diff_density_min         -0.331
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         5250
_refine_ls_number_restraints     84
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0747
_refine_ls_R_factor_gt           0.0432
_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^)+(0.0514P)^2^+1.7827P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1136
_refine_ls_wR_factor_ref         0.1380
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3154
_reflns_number_total             5250
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            VT_dry_ZIF-62_Co_0-30_400K.cif
_cod_data_source_block           int1_zif-62_co_1_no_guest_400k
_cod_original_cell_volume        4372.5(17)
_cod_original_formula_sum        'C7.20 H6.60 Co N4'
_cod_database_code               4128634
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.461
_shelx_estimated_absorpt_t_min   0.388
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C23B-C22B \\sim C24B-C23B \\sim C25B-C24B \\sim C26B-C25B \\sim C27B-C26B
\\sim C27B-C22B
 with sigma of 0.02
 N22B-C21 \\sim N22A-C21 \\sim N21A-C21 \\sim N21B-C21
 with sigma of 0.02
 C16-C15 \\sim C17-C16 \\sim C13-C12 \\sim C14-C13 \\sim C15-C14 \\sim C17-C12
 with sigma of 0.02
 N22B-C23B \\sim N22A-C23A \\sim N21B-C22B \\sim N21A-C22A
 with sigma of 0.02
3. Restrained planarity
 C22B, C23B, C24B, C25B, C26B, C27B
 with sigma of 0.1
 C12, C13, C14, C15, C16, C17
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
N22B \\sim N22A \\sim N21A \\sim N21B: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
C25B \\sim C24B \\sim C26B \\sim C27B: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
C22A \\sim C23A: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
5. Others
 Fixed Sof: N21B(0.5) N21A(0.5) N22B(0.5) N22A(0.5) H12(0.5) H13(0.5) C14(0.4)
 H14(0.4) C15(0.4) H15(0.4) C16(0.4) H16(0.4) C17(0.4) H17(0.4) H21(0.5)
 C22A(0.5) H22A(0.5) C22B(0.5) C23A(0.5) H23A(0.5) C23B(0.5) C24B(0.2)
 H24B(0.2) C25B(0.2) H25B(0.2) C26B(0.2) H26B(0.2) C27B(0.2) H27B(0.2)
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), C23A(H23A), C24B(H24B), C25B(H25B), C26B(H26B),
 C27B(H27B), C31(H31), C32(H32), C33(H33), C41(H41), C42(H42), C43(H43)
;
_shelx_res_checksum              88134
_shelx_hkl_checksum              52363
_olex2_submission_special_instructions 'No special instructions were received'