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#$Date: 2025-04-05 06:00:57 +0300 (Sat, 05 Apr 2025) $
#$Revision: 298897 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/75/7717597.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_7717597
loop_
_publ_author_name
'Lückert, Paula L'
'Gilmer, Jannik'
'Virovets, Alexander'
'Lerner, Hans-Wolfram'
'Wagner, Matthias'
_publ_section_title
;
 Donor-free 9-aluminafluorenes: molecular structures and reactivity.
;
_journal_issue                   6
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2301
_journal_page_last               2307
_journal_paper_doi               10.1039/d4dt03148b
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C20 H20 Al Br2 N4, Br [+ solvent]'
_chemical_formula_sum            'C20 H20 Al Br3 N4'
_chemical_formula_weight         583.11
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           52
_space_group_name_Hall           '-P 2a 2bc'
_space_group_name_H-M_alt        'P n n a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2019/3
_audit_update_record
;
2024-10-28 deposited with the CCDC.	2024-12-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.1189(5)
_cell_length_b                   7.9834(3)
_cell_length_c                   22.9967(7)
_cell_measurement_reflns_used    8978
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.9930
_cell_measurement_theta_min      2.9580
_cell_volume                     2592.12(16)
_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_publication_material  'IUCr PublCIF online service'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0677
_diffrn_reflns_av_unetI/netI     0.0237
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            35509
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.675
_diffrn_reflns_theta_min         2.701
_diffrn_source                   'Genix 3D I\mS microfocus X-ray source'
_exptl_absorpt_coefficient_mu    4.714
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.15172
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.43a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.494
_exptl_crystal_description       needle
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.810
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.916
_refine_diff_density_min         -0.403
_refine_diff_density_rms         0.067
_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     132
_refine_ls_number_reflns         2469
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0381
_refine_ls_R_factor_gt           0.0293
_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/[σ²(Fo²)+(0.0330P)²+2.7748P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0706
_refine_ls_wR_factor_ref         0.0744
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2074
_reflns_number_total             2469
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4dt03148b3.cif
_cod_data_source_block           5_Br_wa3248_AV
_cod_depositor_comments
'Adding full bibliography for 7717596--7717605.cif.'
_cod_original_cell_volume        2592.12(15)
_cod_database_code               7717597
_shelx_shelxl_version_number     2019/3
_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   0.115
_shelx_estimated_absorpt_t_max   0.650
_platon_squeeze_void_probe_radius 1.20
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z'
'-x+1/2, y+1/2, -z+1/2'
'x, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z'
'x-1/2, -y-1/2, z-1/2'
'-x, y-1/2, z-1/2'
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 0.750000 0.500000 0.52365(5) 0.0301(3) Uani 1 2 d S T P . .
Br1A Br 0.88242(2) 0.70651(5) 0.52115(2) 0.03263(12) Uani 0.95 1 d . . P A 1
Br1B Br 0.8855(5) 0.8126(10) 0.5152(3) 0.0369(14) Uiso 0.05 1 d . . P B 2
Br2 Br 0.93164(3) 0.750000 0.750000 0.03983(14) Uani 1 2 d S T P . .
N1 N 0.81935(18) 0.3612(3) 0.46083(11) 0.0324(6) Uani 1 1 d . . . . .
C2 C 0.8296(2) 0.1956(4) 0.46599(14) 0.0386(8) Uani 1 1 d . . . . .
H2 H 0.801289 0.140659 0.498233 0.046 Uiso 1 1 calc R U . . .
C3 C 0.8800(3) 0.1012(4) 0.42622(15) 0.0479(9) Uani 1 1 d . . . . .
H3 H 0.886745 -0.016198 0.431522 0.057 Uiso 1 1 calc R U . . .
C4 C 0.9202(3) 0.1793(5) 0.37871(15) 0.0474(9) Uani 1 1 d . . . . .
H4 H 0.954701 0.116684 0.350654 0.057 Uiso 1 1 calc R U . . .
C5 C 0.9095(2) 0.3481(4) 0.37296(14) 0.0391(8) Uani 1 1 d . . . . .
H5 H 0.936397 0.404752 0.340611 0.047 Uiso 1 1 calc R U . . .
C6 C 0.8595(2) 0.4359(4) 0.41410(13) 0.0347(7) Uani 1 1 d . . . . .
H6 H 0.852927 0.553644 0.409616 0.042 Uiso 1 1 calc R U . . .
N11 N 0.68532(17) 0.6361(3) 0.58775(11) 0.0312(6) Uani 1 1 d . . . . .
C12 C 0.7358(2) 0.7012(4) 0.63243(12) 0.0333(7) Uani 1 1 d . . . . .
H12 H 0.801828 0.679010 0.634291 0.040 Uiso 1 1 calc R U . . .
C13 C 0.6957(2) 0.7975(4) 0.67498(14) 0.0388(8) Uani 1 1 d . . . . .
H13 H 0.733486 0.840055 0.705820 0.047 Uiso 1 1 calc R U . . .
C14 C 0.6003(3) 0.8325(5) 0.67287(16) 0.0470(9) Uani 1 1 d . . . . .
H14 H 0.571453 0.902137 0.701314 0.056 Uiso 1 1 calc R U . . .
C15 C 0.5475(2) 0.7635(4) 0.62818(14) 0.0420(8) Uani 1 1 d . . . . .
H15 H 0.481051 0.781614 0.626438 0.050 Uiso 1 1 calc R U . . .
C16 C 0.5912(2) 0.6695(4) 0.58672(14) 0.0372(7) Uani 1 1 d . . . . .
H16 H 0.554258 0.625493 0.555772 0.045 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'
N N 0.0061 0.0033 '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
N11 Al1 N11 87.83(14) . 2_665 ?
N11 Al1 N1 177.98(11) . . ?
N11 Al1 N1 90.42(10) 2_665 . ?
N11 Al1 N1 90.42(10) . 2_665 ?
N11 Al1 N1 177.98(11) 2_665 2_665 ?
N1 Al1 N1 91.34(15) . 2_665 ?
N11 Al1 Br1A 91.89(7) . 2_665 ?
N11 Al1 Br1A 90.01(7) 2_665 2_665 ?
N1 Al1 Br1A 89.12(8) . 2_665 ?
N1 Al1 Br1A 89.04(8) 2_665 2_665 ?
N11 Al1 Br1A 90.01(7) . . ?
N11 Al1 Br1A 91.89(7) 2_665 . ?
N1 Al1 Br1A 89.04(8) . . ?
N1 Al1 Br1A 89.12(8) 2_665 . ?
Br1A Al1 Br1A 177.36(6) 2_665 . ?
C2 N1 C6 117.5(3) . . ?
C2 N1 Al1 121.3(2) . . ?
C6 N1 Al1 121.1(2) . . ?
N1 C2 C3 122.5(3) . . ?
N1 C2 H2 118.8 . . ?
C3 C2 H2 118.8 . . ?
C4 C3 C2 119.3(3) . . ?
C4 C3 H3 120.3 . . ?
C2 C3 H3 120.3 . . ?
C5 C4 C3 118.5(3) . . ?
C5 C4 H4 120.7 . . ?
C3 C4 H4 120.7 . . ?
C4 C5 C6 119.7(3) . . ?
C4 C5 H5 120.1 . . ?
C6 C5 H5 120.1 . . ?
N1 C6 C5 122.5(3) . . ?
N1 C6 H6 118.8 . . ?
C5 C6 H6 118.8 . . ?
C12 N11 C16 117.0(3) . . ?
C12 N11 Al1 121.0(2) . . ?
C16 N11 Al1 122.0(2) . . ?
N11 C12 C13 122.8(3) . . ?
N11 C12 H12 118.6 . . ?
C13 C12 H12 118.6 . . ?
C12 C13 C14 119.6(3) . . ?
C12 C13 H13 120.2 . . ?
C14 C13 H13 120.2 . . ?
C13 C14 C15 118.2(3) . . ?
C13 C14 H14 120.9 . . ?
C15 C14 H14 120.9 . . ?
C16 C15 C14 119.7(3) . . ?
C16 C15 H15 120.2 . . ?
C14 C15 H15 120.2 . . ?
N11 C16 C15 122.8(3) . . ?
N11 C16 H16 118.6 . . ?
C15 C16 H16 118.6 . . ?
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 N11 2.046(3) . ?
Al1 N11 2.046(3) 2_665 ?
Al1 N1 2.067(3) . ?
Al1 N1 2.067(3) 2_665 ?
Al1 Br1A 2.4934(3) 2_665 ?
Al1 Br1A 2.4934(3) . ?
N1 C2 1.335(4) . ?
N1 C6 1.354(4) . ?
C2 C3 1.382(5) . ?
C2 H2 0.9500 . ?
C3 C4 1.380(5) . ?
C3 H3 0.9500 . ?
C4 C5 1.363(5) . ?
C4 H4 0.9500 . ?
C5 C6 1.372(4) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
N11 C12 1.354(4) . ?
N11 C16 1.355(4) . ?
C12 C13 1.367(4) . ?
C12 H12 0.9500 . ?
C13 C14 1.377(5) . ?
C13 H13 0.9500 . ?
C14 C15 1.384(5) . ?
C14 H14 0.9500 . ?
C15 C16 1.362(4) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
C2 H2 Br1B^b 0.95 2.90 3.355(9) 110.4 1_545 yes
C2 H2 Br1B^b 0.95 2.69 3.242(7) 117.5 2_665 yes
C3 H3 Br1B^b 0.95 2.36 3.083(9) 132.4 1_545 yes
C16 H16 Br1A^a 0.95 2.91 3.380(3) 111.9 2_665 yes
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 N1 C2 C3 0.8(5) . . . . ?
Al1 N1 C2 C3 -176.5(3) . . . . ?
N1 C2 C3 C4 -1.0(6) . . . . ?
C2 C3 C4 C5 0.5(6) . . . . ?
C3 C4 C5 C6 0.1(5) . . . . ?
C2 N1 C6 C5 -0.1(5) . . . . ?
Al1 N1 C6 C5 177.2(2) . . . . ?
C4 C5 C6 N1 -0.3(5) . . . . ?
C16 N11 C12 C13 -0.4(5) . . . . ?
Al1 N11 C12 C13 177.7(2) . . . . ?
N11 C12 C13 C14 -0.6(5) . . . . ?
C12 C13 C14 C15 2.0(5) . . . . ?
C13 C14 C15 C16 -2.5(6) . . . . ?
C12 N11 C16 C15 -0.1(5) . . . . ?
Al1 N11 C16 C15 -178.2(3) . . . . ?
C14 C15 C16 N11 1.6(5) . . . . ?
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.250 -0.014 0.750 219 51 'unclear disordered solvent'
2 0.750 -0.014 0.250 219 51 'unclear disordered solvent'
