Al(OCArF3)<sub>3</sub> - a thermally stable Lewis superacid.
Kögel, Julius F; Timoshkin, Alexey Y.; Schröder, Artem; Lork, Enno; Beckmann, Jens; Chemical science 9 (2018) 8178–8183; doi:10.1039/c8sc02981d

data_1550004
_publ_section_title
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 Al(OCArF3)<sub>3</sub> - a thermally stable Lewis superacid.
;
_journal_issue                   43
_journal_name_full               'Chemical science'
_journal_page_first              8178
_journal_page_last               8183
_journal_paper_doi               10.1039/c8sc02981d
_journal_volume                  9
_journal_year                    2018
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C10 H10 Fe, Al C57 F46 O3'
_chemical_formula_sum            'C67 H10 Al F46 Fe O3'
_chemical_formula_weight         1819.58
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-02-03
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-08-24 deposited with the CCDC.
2018-10-02 downloaded from the CCDC.
;
_cell_angle_alpha                97.981(2)
_cell_angle_beta                 101.382(2)
_cell_angle_gamma                98.800(2)
_cell_formula_units_Z            1
_cell_length_a                   11.6429(4)
_cell_length_b                   11.6834(4)
_cell_length_c                   12.0655(4)
_cell_measurement_reflns_used    9922
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      28.23
_cell_measurement_theta_min      2.27
_cell_volume                     1565.64(9)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Bruker PHOTON area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0716
_diffrn_reflns_av_unetI/netI     0.0957
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            36831
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.465
_diffrn_reflns_theta_min         2.222
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.445
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6743
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0994 before and 0.0737 after correction. The Ratio of minimum to maximum transmission is 0.9043. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.930
_exptl_crystal_description       block
_exptl_crystal_F_000             889
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Dichloromethane / Hexane'
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.653
_refine_diff_density_min         -0.505
_refine_diff_density_rms         0.095
_refine_ls_abs_structure_details
;
 Flack x determined using 4173 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.018(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1063
_refine_ls_number_reflns         15488
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0918
_refine_ls_R_factor_gt           0.0539
_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^)+(0.0656P)^2^+0.0856P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1199
_refine_ls_wR_factor_ref         0.1377
_reflns_Friedel_coverage         0.982
_reflns_Friedel_fraction_full    0.991
_reflns_Friedel_fraction_max     0.970
_reflns_number_gt                11028
_reflns_number_total             15488
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc02981d2.cif
_cod_data_source_block           koegelj180103_0m_a
_cod_depositor_comments
'Adding full bibliography for 1550001--1550014.cif.'
_cod_database_code               1550004
_shelx_shelxl_version_number     2016/6
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C100(H100), C101(H101), C102(H102), C103(H103), C104(H104), C105(H105),
 C106(H106), C107(H107), C108(H108), C109(H109)
;
_olex2_submission_special_instructions 'No special instructions were received'