Cationic dialanes with fluxional π-bridged cyclopentadienyl ligands.
Dabringhaus, Philipp; Zedlitz, Silja; Krossing, Ingo; Chemical communications (Cambridge, England) 59 (2022) 187–190; doi:10.1039/d2cc05786g

data_7131013
_publ_section_title
;
 Cationic dialanes with fluxional &#x3c0;-bridged cyclopentadienyl
 ligands.
;
_journal_issue                   2
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              187
_journal_page_last               190
_journal_paper_doi               10.1039/d2cc05786g
_journal_volume                  59
_journal_year                    2022
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C16 Al F36 O4, C20 H25 Al2'
_chemical_formula_sum            'C36 H25 Al3 F36 O4'
_chemical_formula_weight         1286.43
_chemical_properties_physical    Air-sensitive,Moisture-sensitive,Hygroscopic
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_method
;FinalCif V109 by Daniel Kratzert, Freiburg 2022,
https://dkratzert.de/finalcif.html
;
_audit_update_record
;
2022-10-01 deposited with the CCDC.	2022-11-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   20.350(2)
_cell_length_b                   22.947(3)
_cell_length_c                   40.507(4)
_cell_measurement_reflns_used    9888
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.916
_cell_measurement_theta_min      2.196
_cell_volume                     18916(4)
_computing_cell_refinement       'SAINT V8.40B'
_computing_data_collection
'Bruker BIS V6.2.15 Patch 4/2021-03-15 && APEX4 2021.10-0'
_computing_data_reduction        'SAINT V8.40B'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 CPAD
_diffrn_detector_area_resol_mean 7.41
_diffrn_detector_type            'Bruker PHOTON III'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE dual wavelength Mo/Cu'
_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  0.0392
_diffrn_reflns_av_unetI/netI     0.0269
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       54
_diffrn_reflns_limit_l_min       -55
_diffrn_reflns_number            482475
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.166
_diffrn_reflns_theta_min         1.337
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           1.4
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.262
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.6753
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction:
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    1.807
_exptl_crystal_description       block
_exptl_crystal_F_000             10175
_exptl_crystal_recrystallization_method
'layering a solution of 1,2-difluorobenzene with n-heptane'
_exptl_crystal_size_max          0.272
_exptl_crystal_size_mid          0.196
_exptl_crystal_size_min          0.158
_refine_diff_density_max         0.694
_refine_diff_density_min         -0.402
_refine_diff_density_rms         0.053
_refine_ls_abs_structure_details
;
 Flack x determined using 18325 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.004(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     5952
_refine_ls_number_reflns         54386
_refine_ls_number_restraints     220340
_refine_ls_restrained_S_all      1.495
_refine_ls_R_factor_all          0.0625
_refine_ls_R_factor_gt           0.0488
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0574P)^2^+9.9550P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1127
_refine_ls_wR_factor_ref         0.1207
_reflns_Friedel_coverage         0.870
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.963
_reflns_number_gt                46133
_reflns_number_total             54386
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc05786g2.cif
_cod_data_source_block           P212121_a
_cod_depositor_comments
'Adding full bibliography for 7131010--7131014.cif.'
_cod_original_cell_volume        18915(4)
_cod_database_code               7131013
_shelx_shelxl_version_number     2018/3
_olex2_diffrn_ambient_temperature_device 'Oxford Cryostream 800'
_shelx_res_checksum              75102
_shelx_hkl_checksum              42927