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_4128642
_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 H99.2 Co16 N64), 0.5(C3 H7 N O)'
_chemical_formula_sum            'C7.9 H9.7 Co N4.5 O0.5'
_chemical_formula_weight         234.63
_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             2018-06-16
_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                   15.1566(12)
_cell_length_b                   15.6776(7)
_cell_length_c                   18.2216(15)
_cell_measurement_reflns_used    2730
_cell_measurement_temperature    100.1(5)
_cell_measurement_theta_max      26.3440
_cell_measurement_theta_min      2.7160
_cell_volume                     4329.8(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      100.1(5)
_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 0.988
_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    -13.00  63.00   1.00   10.00    --   20.94 -99.00 -90.00   76
  2  \w    -24.00  20.00   1.00   10.00    --  -22.03 -99.00 150.00   44
  3  \w    -91.00 -53.00   1.00   10.00    --  -22.03 179.00 -90.00   38
;
_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      -0.0103614000
_diffrn_orient_matrix_UB_12      -0.0383948000
_diffrn_orient_matrix_UB_13      0.0187200000
_diffrn_orient_matrix_UB_21      0.0416973000
_diffrn_orient_matrix_UB_22      0.0010237000
_diffrn_orient_matrix_UB_23      0.0175730000
_diffrn_orient_matrix_UB_31      -0.0184630000
_diffrn_orient_matrix_UB_32      0.0238715000
_diffrn_orient_matrix_UB_33      0.0293190000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0360
_diffrn_reflns_av_unetI/netI     0.0528
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            13241
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        27.500
_diffrn_reflns_theta_max         28.498
_diffrn_reflns_theta_min         2.598
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.556
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68043
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark violet'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.440
_exptl_crystal_description       prism
_exptl_crystal_F_000             1914
_exptl_crystal_size_max          0.528
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.189
_refine_diff_density_max         0.756
_refine_diff_density_min         -0.774
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     300
_refine_ls_number_reflns         5413
_refine_ls_number_restraints     93
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.1087
_refine_ls_R_factor_gt           0.0687
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0594P)^2^+16.9562P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1647
_refine_ls_wR_factor_ref         0.1919
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3655
_reflns_number_total             5413
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            asZIF-62-Co-bim_0-10_final.cif
_cod_data_source_block           ZIF-62-Co-bim_0-10
_cod_original_formula_sum        'C7.90 H9.70 Co N4.50 O0.50'
_cod_database_code               4128642
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Co C H N O'
_chemical_oxdiff_usercomment     'MK-JD05 - ZIF-62(Co) less bim'
_shelx_estimated_absorpt_t_max   0.757
_shelx_estimated_absorpt_t_min   0.494
_reflns_odcompleteness_completeness 99.86
_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
 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
 N01-C02 \\sim N01-C03
 with sigma of 0.02
3. Restrained planarity
 C12, C13, C14, C15, C16, C17
 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
5. Rigid body (RIGU) restrains
 C02, N01, C03, C01, O01
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: H12(0.8) H13(0.8) C14(0.2) H14(0.2) C15(0.2) H15(0.2) C16(0.2)
 H16(0.2) C17(0.2) H17(0.2) C22A(0.33333) H22A(0.33333) C22B(0.66667)
 H22B(0.66667) C23A(0.33333) H23A(0.33333) C23B(0.66667) H23B(0.66667)
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), C01(H01)
7.b Idealised Me refined as rotating group:
 C02(H02A,H02B,H02C), C03(H03A,H03B,H03C)
;
_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 1.253
_oxdiff_exptl_absorpt_empirical_full_min 0.784