A supramolecular porous material comprising Fe(ii) mesocates.
Wilson, Benjamin H.; Scott, Hayley S.; Qazvini, Omid T.; Telfer, Shane G.; Mathonière, Corine; Clérac, Rodolphe; Kruger, Paul E.; Chemical communications (Cambridge, England) 54 (2018) 13391–13394; doi:10.1039/c8cc07227b

data_7122560
_publ_section_title
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 A supramolecular porous material comprising Fe(ii) mesocates.
;
_journal_issue                   95
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              13391
_journal_page_last               13394
_journal_paper_doi               10.1039/c8cc07227b
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety         'C60 H54 Fe2 N24 O6, 6(B0.67 F2.67)'
_chemical_formula_sum            'C60 H54 B4 F16 Fe2 N24 O6'
_chemical_formula_weight         1666.21
_space_group_crystal_system      hexagonal
_space_group_IT_number           176
_space_group_name_Hall           '-P 6c'
_space_group_name_H-M_alt        'P 63/m'
_symmetry_space_group_name_Hall  '-P 6c'
_symmetry_space_group_name_H-M   'P 63/m'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-03-02
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2018-05-06 deposited with the CCDC.
2018-11-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   14.3872(3)
_cell_length_b                   14.3872(3)
_cell_length_c                   24.9442(4)
_cell_measurement_reflns_used    888
_cell_measurement_temperature    120.0(1)
_cell_measurement_theta_max      76.5140
_cell_measurement_theta_min      3.9430
_cell_volume                     4471.50(15)
_computing_cell_refinement
'CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)'
_computing_data_collection
'CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)'
_computing_data_reduction
'CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      120.0(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6501
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0259
_diffrn_reflns_av_unetI/netI     0.0174
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            15998
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.809
_diffrn_reflns_theta_min         3.544
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.379
_exptl_absorpt_correction_T_max  0.985
_exptl_absorpt_correction_T_min  0.968
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
'CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)'
_exptl_crystal_colour            'clear violet'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.238
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1692
_exptl_crystal_preparation
'The ligand and iron (II) tetrafluoroborate were stirred in nitromethane at room temperature for 12 hours'
_exptl_crystal_recrystallization_method
'vapour diffusion of toluene into an nitromethane solution of the complex'
_exptl_crystal_size_max          0.288
_exptl_crystal_size_mid          0.106
_exptl_crystal_size_min          0.083
_exptl_transmission_factor_max   0.985
_exptl_transmission_factor_min   0.968
_refine_diff_density_max         1.413
_refine_diff_density_min         -0.575
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     176
_refine_ls_number_reflns         3198
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0919
_refine_ls_R_factor_gt           0.0912
_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^)+(0.1437P)^2^+18.0914P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2683
_refine_ls_wR_factor_ref         0.2690
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3150
_reflns_number_total             3198
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc07227b2.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 7122560.cif.
;
_cod_original_cell_volume        4471.49(18)
_cod_database_code               7122560
_oxdiff_exptl_absorpt_empirical_full_min 0.732
_oxdiff_exptl_absorpt_empirical_full_max 1.454
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 F20-F23
 2.29 with sigma of 0.002
 F20-B26
 1.402 with sigma of 0.002
 F22-B26
 1.402 with sigma of 0.002
 B18-F21
 1.402 with sigma of 0.002
 F25-F21
 2.29 with sigma of 0.002
 F21-F24
 2.29 with sigma of 0.002
 F25-F24
 2.29 with sigma of 0.002
 F19-F24
 2.29 with sigma of 0.002
 F19-F25
 2.29 with sigma of 0.002
3. Uiso/Uaniso restraints and constraints
Uanis(F20) = Uanis(F23) = Uanis(F22) = Uanis(F19) = Uanis(B26)
Uanis(F21) = Uanis(F19) = Uanis(B18) = Uanis(F24) = Uanis(F25)
4. Others
 Fixed Sof: F19(0.66667) B26(0.33333) F24(0.33333) F22(0.33333) F23(0.33333)
 B18(0.33333) F25(0.33333) F20(0.33333) F21(0.33333)
5.a Aromatic/amide H refined with riding coordinates:
 N11(H11), C15(H15), C16(H16), C17(H17), C4(H4), C5(H5), C7(H7)
5.b Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C)
;
_shelx_res_checksum              62323
_shelx_hkl_checksum              16309
_shelx_fab_checksum              96542
_shelx_shelxl_version_number     2014/7
_olex2_exptl_crystal_mounting_method
'The crystal was collected on the loop and mounted directly under the cryo stream at 120 K'
_olex2_submission_special_instructions 'No special instructions were received'