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_7237202
_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         'C7.50 H9.50 Co N4.50 O0.50'
_chemical_formula_sum            'C7.5 H9.5 Co N4.5 O0.5'
_chemical_formula_weight         229.63
_chemical_name_systematic        ZIF-4-Co
_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             2018-06-15
_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                   14.7957(5)
_cell_length_b                   15.5641(5)
_cell_length_c                   18.4453(6)
_cell_measurement_reflns_used    5675
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.9480
_cell_measurement_theta_min      2.8540
_cell_volume                     4247.6(2)
_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(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 0.946
_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     -7.00  24.00   1.00    5.00    --  -27.51 -99.00  30.00   31
  2  \w     -2.00  90.00   1.00    5.00    --   26.41  57.00  90.00   92
  3  \w     47.00 106.00   1.00    5.00    --   26.41  77.00 -30.00   59
  4  \w     41.00 106.00   1.00    5.00    --   26.41 179.00 -90.00   65
;
_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      0.0416494000
_diffrn_orient_matrix_UB_12      -0.0056982000
_diffrn_orient_matrix_UB_13      -0.0184841000
_diffrn_orient_matrix_UB_21      -0.0237887000
_diffrn_orient_matrix_UB_22      -0.0082453000
_diffrn_orient_matrix_UB_23      -0.0326342000
_diffrn_orient_matrix_UB_31      0.0009480000
_diffrn_orient_matrix_UB_32      0.0444344000
_diffrn_orient_matrix_UB_33      -0.0084515000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0227
_diffrn_reflns_av_unetI/netI     0.0239
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.946
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            16292
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.946
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.480
_diffrn_reflns_theta_min         2.602
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.585
_exptl_absorpt_correction_T_max  0.973
_exptl_absorpt_correction_T_min  0.950
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
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    1.436
_exptl_crystal_description       prism
_exptl_crystal_F_000             1872
_exptl_crystal_recrystallization_method 'solvothermal synthesis'
_exptl_crystal_size_max          0.819
_exptl_crystal_size_mid          0.576
_exptl_crystal_size_min          0.34
_refine_diff_density_max         1.215
_refine_diff_density_min         -1.072
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     246
_refine_ls_number_reflns         5088
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0532
_refine_ls_R_factor_gt           0.0415
_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^)+(0.0569P)^2^+8.6382P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1105
_refine_ls_wR_factor_ref         0.1220
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4240
_reflns_number_total             5088
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ta08016j2.cif
_cod_data_source_block           ZIF-4-Co
_cod_original_formula_sum        'C7.50 H9.50 Co N4.50 O0.50'
_cod_database_code               7237202
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Co C6 N4 H6'
_shelx_estimated_absorpt_t_max   0.615
_shelx_estimated_absorpt_t_min   0.357
_reflns_odcompleteness_completeness 99.81
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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. Uiso/Uaniso restraints and constraints
Uanis(C22A) \\sim Ueq, Uanis(C23A) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
3.a Aromatic/amide H refined with riding coordinates:
 C11(H11), C12(H12), C13(H13), C21(H21), C22A(H22A), C23A(H23A), C31(H31),
 C32(H32), C33(H33), C41(H41), C42(H42), C43(H43), C01(H01)
3.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 1.252
_oxdiff_exptl_absorpt_empirical_full_min 0.909