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_7229212
_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
;
 C4.5 H3 F3 N2 O1.5, 0.5(C3 H7 N O)
;
_chemical_formula_sum            'C6 H6.5 F3 N2.5 O2 Zn'
_chemical_formula_weight         268.01
_chemical_name_systematic
'(\m-formato)-(\m-hydroxo)-2-trifluoromethyl-imidazolate-zinc(II) dimethylformamide hemisolvate'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   mixed
_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                   14.2627(4)
_cell_length_b                   13.4623(5)
_cell_length_c                   9.8745(7)
_cell_measurement_reflns_used    17184
_cell_measurement_temperature    210(2)
_cell_measurement_theta_max      29.70
_cell_measurement_theta_min      1.43
_cell_volume                     1895.99(16)
_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      210(2)
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
; 
 206 frames, 3 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  0.0465
_diffrn_reflns_av_unetI/netI     0.0193
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            13168
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.996
_diffrn_reflns_theta_max         24.996
_diffrn_reflns_theta_min         2.509
_exptl_absorpt_coefficient_mu    2.617
_exptl_absorpt_correction_T_max  0.6459
_exptl_absorpt_correction_T_min  0.5066
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'X-AREA (Stoe, 2015)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.878
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1064
_exptl_crystal_size_max          1.00
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.468
_refine_diff_density_min         -0.394
_refine_diff_density_rms         0.057
_refine_ls_extinction_coef       0.0022(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     187
_refine_ls_number_reflns         1740
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.220
_refine_ls_R_factor_all          0.0274
_refine_ls_R_factor_gt           0.0240
_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^)+(0.0356P)^2^+1.7628P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0650
_refine_ls_wR_factor_ref         0.0670
_reflns_number_gt                1550
_reflns_number_total             1740
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce01438d2.cif
_cod_data_source_block           CP-1
_cod_original_formula_sum        'C6 H6.50 F3 N2.50 O2 Zn'
_cod_database_code               7229212
_vref_plat213_alert_2_a
;
PROBLEM: Atom F1B has ADP max/min Ratio ... 5.2 prolat
RESPONSE: This alert is generated because of the degree of
          disordering of the fluorine atoms. Refinements
          in further splitted positions led not to better
          results.  
;
_shelx_res_checksum              87621