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_4128629
_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(C102.4 H82.4 Co16 N64)'
_chemical_formula_sum            'C6.4 H6.2 Co N4'
_chemical_formula_weight         198.08
_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                   15.5286(15)
_cell_length_b                   15.6454(13)
_cell_length_c                   18.0654(16)
_cell_measurement_reflns_used    9907
_cell_measurement_temperature    400(2)
_cell_measurement_theta_max      28.21
_cell_measurement_theta_min      3.45
_cell_volume                     4389.0(7)
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0416
_diffrn_reflns_av_unetI/netI     0.0268
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_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            43462
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        27.500
_diffrn_reflns_theta_max         27.994
_diffrn_reflns_theta_min         2.838
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.519
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5480
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.1350 before and 0.0618 after correction.
The Ratio of minimum to maximum transmission is 0.7349.
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    1.199
_exptl_crystal_description       prism
_exptl_crystal_F_000             1594
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.514
_exptl_crystal_size_min          0.471
_refine_diff_density_max         0.362
_refine_diff_density_min         -0.310
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         5271
_refine_ls_number_restraints     119
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0923
_refine_ls_R_factor_gt           0.0516
_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^)+(0.0429P)^2^+4.9383P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1227
_refine_ls_wR_factor_ref         0.1626
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3037
_reflns_number_total             5271
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            VT_dry_ZIF-62_Co_0-10_400K.cif
_cod_data_source_block           int1_zif-62_co_2_no_guest_400k
_cod_original_formula_sum        'C6.40 H6.20 Co N4'
_cod_database_code               4128629
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.535
_shelx_estimated_absorpt_t_min   0.463
_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
 N22B-C23B \\sim N21B-C22B
 with sigma of 0.02
 N21A-C22A \\sim N21A-C22C \\sim N22A-C23A \\sim N22A-C23C
 with sigma of 0.02
 C23A-C22A \\sim C23C-C22C
 with sigma of 0.02
 Co1-N21B \\sim Co1-N21A
 with sigma of 0.02
 Co2_$2-N22A \\sim Co2_$2-N22B
 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
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. Rigid bond restraints
 C22A, C22C, C23A, C23C
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C17, C16, C15, C14
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. 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
Uanis(C22A) \\sim Ueq, Uanis(C22C) \\sim Ueq, Uanis(C23C) \\sim Ueq,
Uanis(C23A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C15) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
6. Others
 Fixed Sof: N21B(0.5) N21A(0.5) N22B(0.5) N22A(0.5) 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) H21(0.5)
 C22B(0.5) C23B(0.5) C24B(0.1) H24B(0.1) C25B(0.1) H25B(0.1) C26B(0.1)
 H26B(0.1) C27B(0.1) H27B(0.1) C23A(0.33333) H23A(0.33333) C23C(0.16667)
 H23C(0.16667) C22A(0.33333) H22A(0.33333) C22C(0.16667) H22C(0.16667)
7.a Aromatic/amide H refined with riding coordinates:
 C11(H11), C12(H12), C13(H13), C14(H14), C15(H15), C16(H16), C17(H17),
 C21(H21), C24B(H24B), C25B(H25B), C26B(H26B), C27B(H27B), C31(H31), C32(H32),
 C33(H33), C41(H41), C42(H42), C43(H43), C23A(H23A), C23C(H23C), C22A(H22A),
 C22C(H22C)
;
_shelx_res_checksum              38438
_shelx_hkl_checksum              45720
_olex2_submission_special_instructions 'No special instructions were received'