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_1550012
_publ_section_title
;
 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_formula_moiety         'C57 Al F46 O3, C16 H36 N'
_chemical_formula_sum            'C73 H36 Al F46 N O3'
_chemical_formula_weight         1876.01
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_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     iterative
_audit_creation_date             2018-08-03
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-08-24 deposited with the CCDC.
2018-10-02 downloaded from the CCDC.
;
_cell_angle_alpha                71.8670(10)
_cell_angle_beta                 75.4450(10)
_cell_angle_gamma                63.6220(10)
_cell_formula_units_Z            2
_cell_length_a                   13.3297(5)
_cell_length_b                   14.3059(4)
_cell_length_c                   22.5568(8)
_cell_measurement_reflns_used    9904
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      27.88
_cell_measurement_theta_min      2.67
_cell_volume                     3629.8(2)
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0415
_diffrn_reflns_av_unetI/netI     0.0231
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            195049
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.383
_diffrn_reflns_theta_min         2.338
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.197
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6681
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1322 before and 0.0560 after correction. The Ratio of minimum to maximum transmission is 0.8961. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.716
_exptl_crystal_description       block
_exptl_crystal_F_000             1864
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Dichloromethane / Hexane'
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.491
_refine_diff_density_min         -0.369
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1121
_refine_ls_number_reflns         18093
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0559
_refine_ls_R_factor_gt           0.0389
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0292P)^2^+3.5278P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0839
_refine_ls_wR_factor_ref         0.0906
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14442
_reflns_number_total             18093
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc02981d2.cif
_cod_data_source_block           koegelj180608_0m
_cod_depositor_comments
'Adding full bibliography for 1550001--1550014.cif.'
_cod_database_code               1550012
_shelx_shelxl_version_number     2016/4
_shelx_estimated_absorpt_t_max   0.981
_shelx_estimated_absorpt_t_min   0.943
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C100(H10A,H10B), C101(H10C,H10D), C102(H10E,H10F), C104(H10J,H10K), C105(H10L,
 H10M), C106(H10N,H10O), C108(H10S,H10T), C109(H10U,H10V), C112(H11D,H11E),
 C113(H11F,H11G), C114(H11H,H11I), C110(H11M,H11N)
2.b Idealised Me refined as rotating group:
 C103(H10G,H10H,H10I), C107(H10P,H10Q,H10R), C111(H11A,H11B,H11C), C115(H11J,
 H11K,H11L)
;
_shelx_res_checksum              82120
_shelx_fab_checksum              92359
_olex2_submission_special_instructions 'No special instructions were received'