From mixed group 13 cations [M(AlCp*)3]+ (M = Ga/In/Tl) to an Al4+ cluster
Dabringhaus, Philipp; Krossing, Ingo; Chemical Science 13 (2022) 12078–12086; doi:10.1039/D2SC04637G

data_1567741
_publ_section_title
;
 From mixed group 13 cations [M(AlCp*)3]+ (M = Ga/In/Tl) to an Al4+
 cluster
;
_journal_issue                   41
_journal_name_full               'Chemical Science'
_journal_page_first              12078
_journal_page_last               12086
_journal_paper_doi               10.1039/D2SC04637G
_journal_volume                  13
_journal_year                    2022
_chemical_formula_moiety         'C16 Al F36 O4, C9 H21 Ga N3, 3(C10 H15 Al)'
_chemical_formula_sum            'C55 H66 Al4 F36 Ga N3 O4'
_chemical_formula_weight         1694.57
_chemical_properties_physical    Air-sensitive,Moisture-sensitive,Heat-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_method
;FinalCif V107 by Daniel Kratzert, Freiburg 2022,
https://dkratzert.de/finalcif.html
;
_audit_update_record
;
2022-08-02 deposited with the CCDC.	2022-10-07 downloaded from the CCDC.
;
_cell_angle_alpha                117.464(12)
_cell_angle_beta                 90.245(14)
_cell_angle_gamma                90.863(16)
_cell_formula_units_Z            4
_cell_length_a                   17.181(7)
_cell_length_b                   21.399(6)
_cell_length_c                   21.691(5)
_cell_measurement_reflns_used    5010
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.3175
_cell_measurement_theta_min      2.2195
_cell_volume                     7075(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 (G. Sheldrick)'
_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 0.963
_diffrn_measured_fraction_theta_max 0.951
_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  0.0372
_diffrn_reflns_av_unetI/netI     0.0802
_diffrn_reflns_Laue_measured_fraction_full 0.963
_diffrn_reflns_Laue_measured_fraction_max 0.951
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            28962
_diffrn_reflns_point_group_measured_fraction_full 0.963
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.434
_diffrn_reflns_theta_min         1.579
_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    0.579
_exptl_absorpt_correction_T_max  0.745372
_exptl_absorpt_correction_T_min  0.664579
_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            yellow
_exptl_crystal_density_diffrn    1.591
_exptl_crystal_description       block
_exptl_crystal_F_000             3424
_exptl_crystal_recrystallization_method
'layering a solution of the complex in 1,2-difluorobenzene with n-pentane'
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.127
_exptl_crystal_size_min          0.126
_refine_diff_density_max         1.052
_refine_diff_density_min         -0.716
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2783
_refine_ls_number_reflns         28962
_refine_ls_number_restraints     39668
_refine_ls_restrained_S_all      0.928
_refine_ls_R_factor_all          0.1249
_refine_ls_R_factor_gt           0.0743
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0732P)^2^+29.0408P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1716
_refine_ls_wR_factor_ref         0.2022
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19856
_reflns_number_total             28962
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
'The data was integrated as a 2-component twin.'
_twin_individual_id              2
_twin_individual_twin_matrix_11  0.00102
_twin_individual_twin_matrix_12  0.00052
_twin_individual_twin_matrix_13  1.00002
_twin_individual_twin_matrix_21  -1.00019
_twin_individual_twin_matrix_22  -0.00037
_twin_individual_twin_matrix_23  -0.03697
_twin_individual_twin_matrix_31  0.00037
_twin_individual_twin_matrix_32  -0.99983
_twin_individual_twin_matrix_33  -0.01095
_cod_data_source_file            d2sc04637g2.cif
_cod_data_source_block           mo_IK_PD537A_0m_5
_cod_depositor_comments
'Adding full bibliography for 1567740--1567746.cif.'
_cod_database_code               1567741
_shelx_shelxl_version_number     2018/3
_olex2_diffrn_ambient_temperature_device 'Oxford Cryostream 800'
_shelx_res_checksum              33402