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_7237204
_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 Co N4'
_chemical_formula_sum            'C7 H6.5 Co N4'
_chemical_formula_weight         205.59
_chemical_name_systematic        ZIF-62-Co-bim0.30
_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                   15.4329(12)
_cell_length_b                   15.6983(9)
_cell_length_c                   18.1310(12)
_cell_measurement_reflns_used    3527
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.2190
_cell_measurement_theta_min      2.8150
_cell_volume                     4392.6(5)
_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 0.999
_diffrn_measured_fraction_theta_max 1.000
_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     46.00 111.00   1.00   40.00    --   37.46 179.00-150.00   65
  2  \w     41.00  85.00   1.00   40.00    --   37.46  57.00-180.00   44
  3  \w     34.00  95.00   1.00   40.00    --   37.46  77.00 -90.00   61
  4  \w     34.00  59.00   1.00   40.00    --   37.46 179.00  60.00   25
  5  \w      7.00   9.00   1.00   40.00    --   37.46  77.00  60.00    2
;
_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      0.0133757000
_diffrn_orient_matrix_UB_12      0.0169521000
_diffrn_orient_matrix_UB_13      0.0344432000
_diffrn_orient_matrix_UB_21      0.0238937000
_diffrn_orient_matrix_UB_22      -0.0376795000
_diffrn_orient_matrix_UB_23      0.0071899000
_diffrn_orient_matrix_UB_31      0.0368563000
_diffrn_orient_matrix_UB_32      0.0182913000
_diffrn_orient_matrix_UB_33      -0.0171840000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0370
_diffrn_reflns_av_unetI/netI     0.0426
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            18464
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        27.500
_diffrn_reflns_theta_max         29.998
_diffrn_reflns_theta_min         2.595
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.520
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76112
_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            'dark violet'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.244
_exptl_crystal_description       prism
_exptl_crystal_F_000             1656
_exptl_crystal_recrystallization_method 'solvothermal synthesis'
_exptl_crystal_size_max          0.353
_exptl_crystal_size_mid          0.331
_exptl_crystal_size_min          0.165
_refine_diff_density_max         0.632
_refine_diff_density_min         -0.307
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         6396
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0925
_refine_ls_R_factor_gt           0.0551
_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^)+(0.0597P)^2^+4.5529P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1317
_refine_ls_wR_factor_ref         0.1615
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3919
_reflns_number_total             6396
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ta08016j2.cif
_cod_data_source_block           ZIF-62-Co-bim_0-30
_cod_original_formula_sum        'C7 H6.50 Co N4'
_cod_database_code               7237204
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Co N4 C7 H7'
_chemical_oxdiff_usercomment     'MK93 - ZIF-62(Co)'
_reflns_odcompleteness_completeness 99.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.82
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 N21-C22A \\sim N21-C22B \\sim N22-C23B \\sim N22-C23A
 with sigma of 0.02
 C23A-C22A \\sim C23B-C22B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C23A) \\sim Ueq, Uanis(C22A) \\sim Ueq, Uanis(C22B) \\sim Ueq,
Uanis(C23B) \\sim Ueq: 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 1.289
_oxdiff_exptl_absorpt_empirical_full_min 0.881