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_4128649
_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 H101.44 Co16 N64), 0.5(C2.1 H4.9 N0.7 O0.7)'
_chemical_formula_sum            'C7.73 H8.79 Co N4.35 O0.35'
_chemical_formula_weight         227.17
_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             2018-11-16
_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                   15.282(2)
_cell_length_b                   15.664(2)
_cell_length_c                   18.179(2)
_cell_measurement_reflns_used    9958
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.12
_cell_measurement_theta_min      2.17
_cell_volume                     4351.6(9)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0388
_diffrn_reflns_av_unetI/netI     0.0248
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            44785
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        27.500
_diffrn_reflns_theta_max         28.488
_diffrn_reflns_theta_min         2.607
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.545
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.6393
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.0940 before and 0.0641 after correction.
The Ratio of minimum to maximum transmission is 0.8564.
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    1.387
_exptl_crystal_description       block
_exptl_crystal_F_000             1847
_exptl_crystal_size_max          0.528
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.189
_refine_diff_density_max         0.877
_refine_diff_density_min         -0.440
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     337
_refine_ls_number_reflns         5503
_refine_ls_number_restraints     147
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.0552
_refine_ls_R_factor_gt           0.0494
_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^)+(0.0725P)^2^+5.6506P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1463
_refine_ls_wR_factor_ref         0.1541
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4884
_reflns_number_total             5503
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            asZIF-62-Co-bim_0-17_final.cif
_cod_data_source_block           mo_sh_lfb186as_0m
_cod_original_cell_volume        4351.5(10)
_cod_database_code               4128649
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.759
_shelx_estimated_absorpt_t_min   0.496
_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
 N21-C22B \\sim N22-C23B
 with sigma of 0.02
 N21-C22A \\sim N21-C22B \\sim N22-C23A \\sim N22-C23B
 with sigma of 0.02
 C22A-C23A \\sim C23B-C22B
 with sigma of 0.02
 C17-C12 \\sim C17-C16 \\sim C15-C16 \\sim C15-C14 \\sim C14-C13
 with sigma of 0.01
 O01-C01B \\sim O01-C01A
 with sigma of 0.02
 N01B-C01B \\sim N01A-C01A
 with sigma of 0.02
 N01A-C02A \\sim N01B-C03B \\sim N01A-C03A \\sim N01B-C02B
 with sigma of 0.02
 C01A-C02A \\sim C01A-C03A \\sim C01B-C02B \\sim C01B-C03B
 with sigma of 0.02
 O01-N01A \\sim O01-N01B
 with sigma of 0.02
3. Restrained planarity
 C12, C13, C14, C15, C16, C17
 with sigma of 0.1
 O01, C01A, N01A, C02A, C03A
 with sigma of 0.1
 O01, C01B, N01B, C02B, C03B
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(C22A) \\sim Ueq, Uanis(C23A) \\sim Ueq, Uanis(C22B) \\sim Ueq,
Uanis(C23B) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.1
Uanis(C14) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C17)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C03B) \\sim Ueq, Uanis(C02B) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 O01, C01A, N01A, C03A, C02A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C02B, C03B, N01B, C01B, O01
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: H12(0.66) H13(0.66) 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(0.33333) H22A(0.33333)
 C22B(0.66667) H22B(0.66667) C23A(0.33333) H23A(0.33333) C23B(0.66667)
 H23B(0.66667) O01(0.7) N01A(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) C01B(0.2)
 H01B(0.2) N01B(0.2) C03B(0.2) H03D(0.2) H03E(0.2) H03F(0.2) C02B(0.2)
 H02D(0.2) H02E(0.2) H02F(0.2)
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), C22A(H22A), C22B(H22B), C23A(H23A), C23B(H23B), C31(H31), C32(H32),
 C33(H33), C41(H41), C42(H42), C43(H43), C01A(H01A), C01B(H01B)
7.b Idealised Me refined with riding coordinates:
 C02B(H02D,H02E,H02F)
7.c Idealised Me refined as rotating group:
 C02A(H02A,H02B,H02C), C03A(H03A,H03B,H03C), C03B(H03D,H03E,H03F)
;
_olex2_submission_special_instructions 'No special instructions were received'