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#$Date: 2025-03-04 21:02:08 +0200 (Tue, 04 Mar 2025) $
#$Revision: 298096 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/57/31/1573183.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1573183
loop_
_publ_author_name
'Lückert, Paula L'
'Gilmer, Jannik'
'Virovets, Alexander'
'Lerner, Hans-Wolfram'
'Wagner, Matthias'
_publ_section_title
;
 Donor-free 9,10-dihydro-9,10-dialuminaanthracenes.
;
_journal_issue                   1
_journal_name_full               'Chemical science'
_journal_page_first              147
_journal_page_last               155
_journal_paper_doi               10.1039/d4sc06940d
_journal_volume                  16
_journal_year                    2024
_chemical_formula_moiety         'C13.90 H13.69 Al4 Br6.10'
_chemical_formula_sum            'C13.9 H13.69 Al4 Br6.1'
_chemical_formula_weight         776.11
_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
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2024-09-22 deposited with the CCDC.	2024-11-18 downloaded from the CCDC.
;
_cell_angle_alpha                109.179(10)
_cell_angle_beta                 102.057(9)
_cell_angle_gamma                104.104(10)
_cell_formula_units_Z            1
_cell_length_a                   8.1909(9)
_cell_length_b                   8.1869(9)
_cell_length_c                   9.8777(10)
_cell_measurement_reflns_used    2332
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      29.4400
_cell_measurement_theta_min      4.5670
_cell_volume                     575.78(13)
_computing_cell_refinement       'CrysAlisPro 1.171.42.43a (Rigaku OD, 2022)'
_computing_data_collection       'X-Area (Stoe & Cie, 2001)'
_computing_data_reduction        'CrysAlisPro 1.171.42.43a (Rigaku OD, 2022)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT (G. M. Sheldrick, 2015)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'image plate'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            'STOE image plate (34 cm diameter)'
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS II two-circle-diffractometer'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0596
_diffrn_reflns_av_unetI/netI     0.0800
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5874
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.279
_diffrn_reflns_theta_min         4.066
_diffrn_source                   'Genix 3D I\mS microfocus X-ray source'
_exptl_absorpt_coefficient_mu    10.783
_exptl_absorpt_correction_T_max  0.24079
_exptl_absorpt_correction_T_min  0.21920
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.43a (Rigaku Oxford Diffraction, 2022)
Spherical absorption correction
using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.238
_exptl_crystal_description       plate
_exptl_crystal_F_000             363
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.917
_refine_diff_density_min         -0.842
_refine_diff_density_rms         0.181
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     114
_refine_ls_number_reflns         2804
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0629
_refine_ls_R_factor_gt           0.0472
_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/[σ²(Fo²)+(0.0357P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0986
_refine_ls_wR_factor_ref         0.1077
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2211
_reflns_number_total             2804
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4sc06940d3.cif
_cod_data_source_block           2AlMeBr32_wa3327
_cod_depositor_comments
'Adding full bibliography for 1573178--1573190.cif.'
_cod_original_cell_volume        575.79(12)
_cod_original_formula_sum        'C13.90 H13.69 Al4 Br6.10'
_cod_database_code               1573183
_shelx_shelxl_version_number     2018/3
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.277
_shelx_estimated_absorpt_t_max   0.564
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Al1 Al 0.3628(2) 0.3020(2) 0.33817(17) 0.0263(3) Uani 1 1 d . . . . .
Al2 Al 0.3234(2) 0.4237(2) 0.70093(17) 0.0280(3) Uani 1 1 d . . . . .
Br1 Br 0.2385(3) 0.0671(2) 0.12826(19) 0.0434(6) Uani 0.266(3) 1 d . . P A 1
C1B C 0.2385(3) 0.0671(2) 0.12826(19) 0.0434(6) Uani 0.734(3) 1 d . . P A 2
H1BA H 0.299026 0.082899 0.055328 0.065 Uiso 0.734(3) 1 calc R U P A 2
H1BB H 0.113718 0.053994 0.089210 0.065 Uiso 0.734(3) 1 calc R U P A 2
H1BC H 0.245973 -0.043308 0.144104 0.065 Uiso 0.734(3) 1 calc R U P A 2
Br2 Br 0.11959(7) 0.31851(7) 0.45110(6) 0.03209(17) Uani 1 1 d . . . . .
Br3 Br 0.24199(8) 0.19402(8) 0.78067(7) 0.0383(2) Uani 0.956(3) 1 d . . P B 1
C3B C 0.24199(8) 0.19402(8) 0.78067(7) 0.0383(2) Uani 0.044(3) 1 d . . P B 2
H3BA H 0.193309 0.075314 0.693756 0.057 Uiso 0.044(3) 1 calc R U P B 2
H3BB H 0.151749 0.211594 0.829967 0.057 Uiso 0.044(3) 1 calc R U P B 2
H3BC H 0.345871 0.196269 0.852608 0.057 Uiso 0.044(3) 1 calc R U P B 2
Br4 Br 0.29532(11) 0.68494(10) 0.84339(8) 0.0426(3) Uani 0.830(3) 1 d . . P B 3
C4B C 0.29532(11) 0.68494(10) 0.84339(8) 0.0426(3) Uani 0.170(3) 1 d . . P B 4
H4BA H 0.391509 0.743971 0.939848 0.064 Uiso 0.170(3) 1 calc R U P B 4
H4BB H 0.180888 0.657561 0.862141 0.064 Uiso 0.170(3) 1 calc R U P B 4
H4BC H 0.301237 0.767720 0.790594 0.064 Uiso 0.170(3) 1 calc R U P B 4
C1 C 0.5606(6) 0.4352(6) 0.6638(5) 0.0233(9) Uani 1 1 d . . . . .
C2 C 0.5378(6) 0.3108(6) 0.5153(5) 0.0218(9) Uani 1 1 d . . . . .
C3 C 0.6457(7) 0.2019(7) 0.4997(6) 0.0281(11) Uani 1 1 d . . . . .
H3 H 0.633713 0.119179 0.401682 0.034 Uiso 1 1 calc R U . . .
C4 C 0.7684(7) 0.2115(7) 0.6226(7) 0.0336(12) Uani 1 1 d . . . . .
H4 H 0.835554 0.131254 0.607712 0.040 Uiso 1 1 calc R U . . .
C5 C 0.7974(7) 0.3335(7) 0.7666(6) 0.0342(12) Uani 1 1 d . . . . .
H5 H 0.888023 0.342596 0.849263 0.041 Uiso 1 1 calc R U . . .
C6 C 0.6919(7) 0.4435(7) 0.7893(6) 0.0298(11) Uani 1 1 d . . . . .
H6 H 0.706996 0.524603 0.888824 0.036 Uiso 1 1 calc R U . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 Al1 C1 106.8(2) . 2_666 ?
C2 Al1 C1B 124.20(14) . . ?
C1 Al1 C1B 119.18(15) 2_666 . ?
C2 Al1 Br1 124.20(14) . . ?
C1 Al1 Br1 119.18(15) 2_666 . ?
C2 Al1 Br2 97.18(12) . . ?
C1 Al1 Br2 99.92(12) 2_666 . ?
C1B Al1 Br2 103.85(8) . . ?
Br1 Al1 Br2 103.85(8) . . ?
C1 Al2 C4B 118.07(14) . . ?
C1 Al2 Br4 118.07(14) . . ?
C1 Al2 Br3 108.57(12) . . ?
C1 Al2 C3B 108.57(12) . . ?
C1 Al2 Br2 103.29(14) . . ?
C4B Al2 Br2 107.32(6) . . ?
Br4 Al2 Br2 107.32(6) . . ?
Br3 Al2 Br2 105.73(7) . . ?
C3B Al2 Br2 105.73(7) . . ?
Al1 C1B H1BA 109.5 . . ?
Al1 C1B H1BB 109.5 . . ?
H1BA C1B H1BB 109.5 . . ?
Al1 C1B H1BC 109.5 . . ?
H1BA C1B H1BC 109.5 . . ?
H1BB C1B H1BC 109.5 . . ?
Al2 Br2 Al1 91.14(5) . . ?
Al2 C3B H3BA 109.5 . . ?
Al2 C3B H3BB 109.5 . . ?
H3BA C3B H3BB 109.5 . . ?
Al2 C3B H3BC 109.5 . . ?
H3BA C3B H3BC 109.5 . . ?
H3BB C3B H3BC 109.5 . . ?
Al2 C4B H4BA 109.5 . . ?
Al2 C4B H4BB 109.5 . . ?
H4BA C4B H4BB 109.5 . . ?
Al2 C4B H4BC 109.5 . . ?
H4BA C4B H4BC 109.5 . . ?
H4BB C4B H4BC 109.5 . . ?
C2 C1 C6 119.1(4) . . ?
C2 C1 Al2 111.6(3) . . ?
C6 C1 Al2 112.9(3) . . ?
C2 C1 Al1 105.6(3) . 2_666 ?
C6 C1 Al1 105.7(4) . 2_666 ?
Al2 C1 Al1 99.58(17) . 2_666 ?
C3 C2 C1 117.9(4) . . ?
C3 C2 Al1 122.0(3) . . ?
C1 C2 Al1 120.1(3) . . ?
C4 C3 C2 121.5(4) . . ?
C4 C3 H3 119.3 . . ?
C2 C3 H3 119.3 . . ?
C3 C4 C5 122.1(4) . . ?
C3 C4 H4 118.9 . . ?
C5 C4 H4 118.9 . . ?
C4 C5 C6 118.8(5) . . ?
C4 C5 H5 120.6 . . ?
C6 C5 H5 120.6 . . ?
C5 C6 C1 120.5(5) . . ?
C5 C6 H6 119.8 . . ?
C1 C6 H6 119.8 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Al1 C2 1.985(5) . ?
Al1 C1 2.097(4) 2_666 ?
Al1 C1B 2.140(2) . ?
Al1 Br1 2.140(2) . ?
Al1 Br2 2.4883(14) . ?
Al2 C1 2.037(4) . ?
Al2 C4B 2.2372(16) . ?
Al2 Br4 2.2372(16) . ?
Al2 Br3 2.2766(14) . ?
Al2 C3B 2.2766(14) . ?
Al2 Br2 2.4084(17) . ?
C1B H1BA 0.9800 . ?
C1B H1BB 0.9800 . ?
C1B H1BC 0.9800 . ?
C3B H3BA 0.9800 . ?
C3B H3BB 0.9800 . ?
C3B H3BC 0.9800 . ?
C4B H4BA 0.9800 . ?
C4B H4BB 0.9800 . ?
C4B H4BC 0.9800 . ?
C1 C2 1.427(6) . ?
C1 C6 1.432(7) . ?
C2 C3 1.396(5) . ?
C3 C4 1.371(8) . ?
C3 H3 0.9500 . ?
C4 C5 1.373(8) . ?
C4 H4 0.9500 . ?
C5 C6 1.392(6) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 C3 0.1(6) . . . . ?
Al2 C1 C2 C3 -134.2(3) . . . . ?
Al1 C1 C2 C3 118.6(4) 2_666 . . . ?
C6 C1 C2 Al1 -177.9(3) . . . . ?
Al2 C1 C2 Al1 47.8(4) . . . . ?
Al1 C1 C2 Al1 -59.4(4) 2_666 . . . ?
C1 C2 C3 C4 0.8(7) . . . . ?
Al1 C2 C3 C4 178.8(4) . . . . ?
C2 C3 C4 C5 -2.8(7) . . . . ?
C3 C4 C5 C6 3.7(7) . . . . ?
C4 C5 C6 C1 -2.7(7) . . . . ?
C2 C1 C6 C5 0.8(7) . . . . ?
Al2 C1 C6 C5 134.6(4) . . . . ?
Al1 C1 C6 C5 -117.5(4) 2_666 . . . ?
