Soft interactions with hard Lewis acids: generation of mono- and dicationic alkaline-earth metal arene-complexes by direct oxidation.
Schorpp, Marcel; Krossing, Ingo; Chemical science 11 (2020) 2068–2076; doi:10.1039/c9sc06254h

data_1557028
_publ_section_title
;
 Soft interactions with hard Lewis acids: generation of mono- and
 dicationic alkaline-earth metal arene-complexes by direct oxidation.
;
_journal_issue                   8
_journal_name_full               'Chemical science'
_journal_page_first              2068
_journal_page_last               2076
_journal_paper_doi               10.1039/c9sc06254h
_journal_volume                  11
_journal_year                    2020
_chemical_formula_moiety         'C16 Al F36 O4, C24 H8 Al Ca F32 O3, C12 H18'
_chemical_formula_sum            'C52 H26 Al2 Ca F68 O7'
_chemical_formula_weight         2148.77
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_method           'FinalCif by Daniel Kratzert, Freiburg 2019'
_audit_update_record
;
2019-12-03 deposited with the CCDC.	2020-01-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.018(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
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_cell_length_b                   20.654(7)
_cell_length_c                   20.031(8)
_cell_measurement_reflns_used    9702
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      54.149
_cell_measurement_theta_min      4.498
_cell_volume                     7340(5)
_computing_data_collection
'Bruker BIS 2015.5.1.2/11-Jun-2015 P2 && APEX2_2014.11-0'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT (G. Sheldrick)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 8.3
_diffrn_detector_type            'Bruker APEXII'
_diffrn_measured_fraction_theta_full 0.952
_diffrn_measured_fraction_theta_max 0.917
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX2 QUAZAR'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_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  0.0615
_diffrn_reflns_av_unetI/netI     0.0667
_diffrn_reflns_Laue_measured_fraction_full 0.952
_diffrn_reflns_Laue_measured_fraction_max 0.917
_diffrn_reflns_number            25915
_diffrn_reflns_point_group_measured_fraction_full 0.901
_diffrn_reflns_point_group_measured_fraction_max 0.857
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.441
_diffrn_reflns_theta_min         1.018
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           0.6
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.332
_exptl_absorpt_correction_T_max  0.745372
_exptl_absorpt_correction_T_min  0.484876
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
TWINABS - Bruker AXS scaling for twinned crystals - Version 2012/1: Krause, L.,
Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.945
_exptl_crystal_description       block
_exptl_crystal_F_000             4208
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.23
_refine_diff_density_max         1.205
_refine_diff_density_min         -0.696
_refine_diff_density_rms         0.123
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   1.15(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2475
_refine_ls_number_reflns         25915
_refine_ls_number_restraints     35197
_refine_ls_restrained_S_all      0.863
_refine_ls_R_factor_all          0.1221
_refine_ls_R_factor_gt           0.0863
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0577P)^2^+66.9813P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2002
_refine_ls_wR_factor_ref         0.2190
_reflns_Friedel_coverage         0.816
_reflns_Friedel_fraction_full    0.847
_reflns_Friedel_fraction_max     0.793
_reflns_number_gt                19648
_reflns_number_total             25915
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc06254h2.cif
_cod_data_source_block           P21_a
_cod_depositor_comments
;Adding full bibliography for 1557027--1557034.cif.

 Adding full bibliography for 1557027--1557034.cif.
;
_cod_original_cell_volume        7339(5)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               1557028
_shelx_shelxl_version_number     2018/3
_olex2_diffrn_ambient_temperature_device 'Oxford Cryostream 800'
_shelx_res_checksum              13943