Porous purple glass ‒ a cobalt imidazolate glass with accessible porosity from a meltable cobalt imidazolate framework
Frentzel-Beyme, Louis; Kloß, Marvin; Pallach, Roman; Salamon, Soma; Moldenhauer, Henning; Landers, Joachim; Wende, Heiko; Debus, Jörg; Henke, Sebastian; Journal of Materials Chemistry A 7 (2019) 985–; doi:10.1039/C8TA08016J

data_7237203
_publ_section_title
;
 Porous purple glass -- a cobalt imidazolate glass with accessible
 porosity from a meltable cobalt imidazolate framework
;
_journal_issue                   3
_journal_name_full               'Journal of Materials Chemistry A'
_journal_page_first              985
_journal_paper_doi               10.1039/C8TA08016J
_journal_volume                  7
_journal_year                    2019
_chemical_formula_moiety         'C7 H6.50 N4 Zn'
_chemical_formula_sum            'C7 H6.5 N4 Zn'
_chemical_formula_weight         212.03
_chemical_name_systematic        ZIF-62-Zn-bim0.35
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2018-06-15
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3510 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-06-16 deposited with the CCDC.
2019-01-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   15.4567(8)
_cell_length_b                   15.5793(8)
_cell_length_c                   18.1340(8)
_cell_measurement_reflns_used    3558
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.3900
_cell_measurement_theta_min      2.8540
_cell_volume                     4366.8(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (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)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_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 0.962
_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     60.00  88.00   1.00   27.50    --   19.08  77.00  60.00   28
  2  \w    -11.00  76.00   1.00   27.50    --   19.08  77.00 -60.00   87
  3  \w     15.00  52.00   1.00   27.50    --   19.08  77.00-150.00   37
;
_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      -0.0129645000
_diffrn_orient_matrix_UB_12      -0.0364599000
_diffrn_orient_matrix_UB_13      0.0206329000
_diffrn_orient_matrix_UB_21      0.0413521000
_diffrn_orient_matrix_UB_22      -0.0186676000
_diffrn_orient_matrix_UB_23      -0.0054254000
_diffrn_orient_matrix_UB_31      0.0150230000
_diffrn_orient_matrix_UB_32      0.0198822000
_diffrn_orient_matrix_UB_33      0.0328039000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0301
_diffrn_reflns_av_unetI/netI     0.0439
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            13192
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.496
_diffrn_reflns_theta_min         2.169
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.207
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88340
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
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    1.290
_exptl_crystal_description       prism
_exptl_crystal_F_000             1704
_exptl_crystal_recrystallization_method 'solvothermal synthesis'
_exptl_crystal_size_max          0.351
_exptl_crystal_size_mid          0.291
_exptl_crystal_size_min          0.173
_refine_diff_density_max         0.925
_refine_diff_density_min         -0.435
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         5327
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0772
_refine_ls_R_factor_gt           0.0512
_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^)+(0.0601P)^2^+6.6894P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1267
_refine_ls_wR_factor_ref         0.1411
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3676
_reflns_number_total             5327
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ta08016j2.cif
_cod_data_source_block           ZIF-62-Zn-bim_0-35
_cod_original_cell_volume        4366.7(4)
_cod_original_formula_sum        'C7 H6.50 N4 Zn'
_cod_database_code               7237203
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Zn N2 C5 H3'
_chemical_oxdiff_usercomment     'MK06 ZIF-62'
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.04
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C23B-C22B \\sim C23A-C22A
 with sigma of 0.02
 N21-C22A \\sim N21-C22B
 with sigma of 0.02
 N22-C23A \\sim N22-C23B
 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
4. Others
 Fixed Sof: H12(0.5) H13(0.5) C14(0.5) H14(0.5) C15(0.5) H15(0.5) C16(0.5)
 H16(0.5) C17(0.5) H17(0.5) C22A(0.5) H22A(0.5) C22B(0.5) H22B(0.5) C23A(0.5)
 H23A(0.5) C23B(0.5) H23B(0.5)
5.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)
;
_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 1.074
_oxdiff_exptl_absorpt_empirical_full_min 0.874