Synthesis of a partially fluorinated ZIF-8 analog for ethane/ethene separation
Holdt, Hans-Jurgen; Mondal, Suvendu Sekhar; Hovestadt, Maximilian; Dey, Subarna; Paula, Carolin; Glomb, Sebastian; Kelling, Alexandra; Schilde, Uwe; Janiak, Christoph; Hartmann, Martin; CrystEngComm  (2017) –; doi:10.1039/C7CE01438D

data_7229213
_publ_section_title
;
 Synthesis of a partially fluorinated ZIF-8 analog for ethane/ethene
 separation
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/C7CE01438D
_journal_year                    2017
_chemical_formula_moiety         'C12 H17.5 F4.50 N6 Zn1.50, 2(C3 H7 N O)'
_chemical_formula_sum            'C18 H24.5 F4.5 N8 O2 Zn1.5'
_chemical_formula_weight         568.51
_chemical_name_systematic
'(2-methyl-imidazolate)-(2-trifluoromethyl-imidazolate)-zinc(II) dimethylformamide solvate'
_space_group_crystal_system      cubic
_space_group_IT_number           217
_space_group_name_Hall           'I -4 2 3'
_space_group_name_H-M_alt        'I -4 3 m'
_symmetry_space_group_name_Hall  'I -4 2 3'
_symmetry_space_group_name_H-M   'I -4 3 m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-04-07 deposited with the CCDC.
2017-09-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.0786(6)
_cell_length_b                   17.0786(6)
_cell_length_c                   17.0786(6)
_cell_measurement_reflns_used    9050
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      24.46
_cell_measurement_theta_min      1.69
_cell_volume                     4981.5(3)
_computing_cell_refinement       'X-AREA (Stoe, 2015)'
_computing_data_collection       'X-AREA (Stoe, 2015)'
_computing_data_reduction        'X-RED (Stoe, 2015)'
_computing_publication_material
; 
 SHELXL-2014/7 (Sheldrick, 2014)
 Diamond (Blankenburg, 2015)
;
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      180(2)
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
; 
 180 frames, 5 min exposure time
;
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       '\w scan, \d \w = 1.0 deg'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0637
_diffrn_reflns_av_unetI/netI     0.0228
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            16222
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        24.918
_diffrn_reflns_theta_max         24.918
_diffrn_reflns_theta_min         1.686
_exptl_absorpt_coefficient_mu    1.520
_exptl_absorpt_correction_T_max  0.8269
_exptl_absorpt_correction_T_min  0.8258
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'X-AREA (Stoe, 2015)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.516
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2320
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.090
_refine_diff_density_max         0.199
_refine_diff_density_min         -0.246
_refine_diff_density_rms         0.057
_refine_ls_abs_structure_details
;
 Flack x determined using 265 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.007(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.143
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     48
_refine_ls_number_reflns         848
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.143
_refine_ls_R_factor_all          0.0450
_refine_ls_R_factor_gt           0.0383
_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^)+(0.0574P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0976
_refine_ls_wR_factor_ref         0.1003
_reflns_number_gt                702
_reflns_number_total             848
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce01438d2.cif
_cod_data_source_block           ZIF-318
_cod_original_cell_volume        4981.5(5)
_cod_original_formula_sum        'C18 H24.50 F4.50 N8 O2 Zn1.50'
_cod_database_code               7229213
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              42084