#------------------------------------------------------------------------------
#$Date: 2025-03-08 01:10:19 +0200 (Sat, 08 Mar 2025) $
#$Revision: 298334 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/57/40/1574073.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_1574073
loop_
_publ_author_name
'Driess, Matthias'
'Saddington, Artemis Mary'
'Yao, Shenglai'
'Lorent, Christian'
_publ_section_title
;
 Redox Non-Innocent Bis-Silylene Aluminium Complexes with a Carborane
 Backbone
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D5SC01104C
_journal_year                    2025
_chemical_formula_sum            'C32 H56 B10 Ga I2 N4 Si2'
_chemical_formula_weight         984.60
_space_group_crystal_system      orthorhombic
_space_group_IT_number           63
_space_group_name_Hall           '-C 2c 2'
_space_group_name_H-M_alt        'C m c m'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_audit_update_record
;
2025-01-20 deposited with the CCDC.	2025-03-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.2436(3)
_cell_length_b                   18.9817(3)
_cell_length_c                   13.9956(2)
_cell_measurement_reflns_used    6314
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      72.5210
_cell_measurement_theta_min      2.9860
_cell_volume                     6174.90(15)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Atlas'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0321
_diffrn_reflns_av_unetI/netI     0.0253
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            12678
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.109
_diffrn_reflns_theta_min         1.752
_exptl_absorpt_coefficient_mu    1.505
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.29306
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.059
_exptl_crystal_description       block
_exptl_crystal_F_000             1964
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.090
_refine_diff_density_max         0.469
_refine_diff_density_min         -1.359
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     140
_refine_ls_number_reflns         3236
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0418
_refine_ls_R_factor_gt           0.0380
_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)+(0.0598P)²+11.5113P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1049
_refine_ls_wR_factor_ref         0.1084
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2925
_reflns_number_total             3236
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d5sc01104c2.cif
_cod_data_source_block           4b
_cod_database_code               1574073
_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   0.743
_shelx_estimated_absorpt_t_max   0.876
_platon_squeeze_void_probe_radius 1.20
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'x, -y, -z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z+1/2'
'x+1/2, -y+1/2, -z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z-1/2'
'-x, y, z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, y+1/2, -z-1/2'
'-x+1/2, y+1/2, z'
'x+1/2, -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
I1 I 0.500000 0.32252(2) 0.10743(2) 0.05025(14) Uani 1 2 d S T P . .
Ga1 Ga 0.500000 0.23771(3) 0.250000 0.03045(16) Uani 1 4 d S TU P . .
Si1 Si 0.41891(4) 0.15665(5) 0.250000 0.01939(19) Uani 1 2 d S TU P . .
N1 N 0.35763(9) 0.17152(11) 0.17331(16) 0.0255(5) Uani 1 1 d . . . . .
C9 C 0.34463(13) 0.17934(15) 0.0694(2) 0.0332(6) Uani 1 1 d . . . . .
C2 C 0.32394(16) 0.18332(19) 0.250000 0.0264(8) Uani 1 2 d S T P . .
C3 C 0.26238(17) 0.2044(2) 0.250000 0.0322(8) Uani 1 2 d S T P . .
C7 C 0.1623(2) 0.1723(2) 0.250000 0.0507(13) Uani 1 2 d S T P . .
H7 H 0.133407 0.136932 0.250000 0.061 Uiso 1 2 calc R U P . .
C5 C 0.18905(18) 0.2937(2) 0.250000 0.0434(11) Uani 1 2 d S T P . .
H5 H 0.178229 0.341993 0.250000 0.052 Uiso 1 2 calc R U P . .
C4 C 0.24727(17) 0.2754(2) 0.250000 0.0344(9) Uani 1 2 d S T P . .
H4 H 0.276128 0.310803 0.250000 0.041 Uiso 1 2 calc R U P . .
C6 C 0.14687(19) 0.2418(3) 0.250000 0.0524(13) Uani 1 2 d S T P . .
H6 H 0.107357 0.254596 0.250000 0.063 Uiso 1 2 calc R U P . .
C11 C 0.33110(16) 0.25594(18) 0.0455(2) 0.0438(8) Uani 1 1 d . . . . .
H11A H 0.295525 0.270039 0.077869 0.066 Uiso 1 1 calc R U . . .
H11B H 0.326261 0.260987 -0.023710 0.066 Uiso 1 1 calc R U . . .
H11C H 0.362810 0.286035 0.067045 0.066 Uiso 1 1 calc R U . . .
C8 C 0.22007(18) 0.1529(2) 0.250000 0.0408(11) Uani 1 2 d S T P . .
H8 H 0.230478 0.104464 0.250000 0.049 Uiso 1 2 calc R U P . .
C10 C 0.39911(14) 0.15595(18) 0.0171(2) 0.0378(7) Uani 1 1 d . . . . .
H10A H 0.431366 0.186032 0.036374 0.057 Uiso 1 1 calc R U . . .
H10B H 0.393196 0.159952 -0.051973 0.057 Uiso 1 1 calc R U . . .
H10C H 0.407720 0.106879 0.033536 0.057 Uiso 1 1 calc R U . . .
C12 C 0.29549(15) 0.1311(2) 0.0404(3) 0.0487(8) Uani 1 1 d . . . . .
H12A H 0.304718 0.082553 0.058491 0.073 Uiso 1 1 calc R U . . .
H12B H 0.289894 0.133779 -0.028925 0.073 Uiso 1 1 calc R U . . .
H12C H 0.260163 0.145947 0.072881 0.073 Uiso 1 1 calc R U . . .
C1 C 0.44806(15) 0.06759(19) 0.250000 0.0219(7) Uani 1 2 d S T P . .
B1 B 0.500000 0.0530(2) 0.3359(3) 0.0218(8) Uani 1 2 d S T P . .
H1 H 0.500000 0.097243 0.388946 0.026 Uiso 1 2 calc R U P . .
B4 B 0.500000 -0.0426(2) 0.1474(3) 0.0273(8) Uani 1 2 d S T P . .
H4A H 0.499999 -0.068380 0.075432 0.033 Uiso 1 2 calc R U P . .
B2 B 0.43484(12) -0.00267(16) 0.3140(2) 0.0250(6) Uani 1 1 d . . . . .
H2 H 0.395789 -0.006265 0.360654 0.030 Uiso 1 1 calc R U . . .
B3 B 0.46193(19) -0.0765(2) 0.250000 0.0293(9) Uani 1 2 d S T P . .
H3 H 0.438533 -0.128089 0.250001 0.035 Uiso 1 2 calc R U P . .
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'
B B 0.0013 0.0007 '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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ga Ga 0.2307 1.6083 '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
Si1 Ga1 Si1 101.55(5) . 11_655 ?
Si1 Ga1 I1 113.395(12) . 10_556 ?
Si1 Ga1 I1 113.395(12) 11_655 10_556 ?
Si1 Ga1 I1 113.395(12) . . ?
Si1 Ga1 I1 113.396(12) 11_655 . ?
I1 Ga1 I1 102.21(3) 10_556 . ?
N1 Si1 N1 72.94(15) . 10_556 ?
N1 Si1 C1 116.01(11) . . ?
N1 Si1 C1 116.01(11) 10_556 . ?
N1 Si1 C2 36.51(7) . . ?
N1 Si1 C2 36.50(7) 10_556 . ?
C1 Si1 C2 124.75(15) . . ?
N1 Si1 Ga1 120.82(8) . . ?
N1 Si1 Ga1 120.81(8) 10_556 . ?
C1 Si1 Ga1 107.38(12) . . ?
C2 Si1 Ga1 127.86(10) . . ?
C2 N1 C9 129.9(2) . . ?
C2 N1 Si1 90.62(18) . . ?
C9 N1 Si1 138.96(19) . . ?
N1 C9 C12 110.6(3) . . ?
N1 C9 C11 110.5(2) . . ?
C12 C9 C11 111.2(3) . . ?
N1 C9 C10 105.6(2) . . ?
C12 C9 C10 108.7(3) . . ?
C11 C9 C10 110.1(3) . . ?
N1 C2 N1 105.6(3) 10_556 . ?
N1 C2 C3 127.18(16) 10_556 . ?
N1 C2 C3 127.19(16) . . ?
N1 C2 Si1 52.88(16) 10_556 . ?
N1 C2 Si1 52.87(16) . . ?
C3 C2 Si1 177.3(3) . . ?
C8 C3 C4 120.2(4) . . ?
C8 C3 C2 119.5(4) . . ?
C4 C3 C2 120.3(4) . . ?
C6 C7 C8 120.6(4) . . ?
C6 C5 C4 120.4(4) . . ?
C3 C4 C5 119.1(4) . . ?
C7 C6 C5 119.9(4) . . ?
C3 C8 C7 119.8(4) . . ?
B2 C1 B2 66.4(3) . 10_556 ?
B2 C1 B1 67.63(18) . . ?
B2 C1 B1 112.5(3) 10_556 . ?
B2 C1 B1 112.5(3) . 10_556 ?
B2 C1 B1 67.63(18) 10_556 10_556 ?
B1 C1 B1 88.3(2) . 10_556 ?
B2 C1 Si1 133.38(19) . . ?
B2 C1 Si1 133.38(19) 10_556 . ?
B1 C1 Si1 114.1(2) . . ?
B1 C1 Si1 114.1(2) 10_556 . ?
C1 B1 C1 88.8(2) 11_655 . ?
C1 B1 B4 104.3(2) 11_655 10_556 ?
C1 B1 B4 104.3(2) . 10_556 ?
C1 B1 B2 122.8(2) 11_655 . ?
C1 B1 B2 53.88(15) . . ?
B4 B1 B2 57.37(15) 10_556 . ?
C1 B1 B2 53.88(15) 11_655 11_655 ?
C1 B1 B2 122.8(2) . 11_655 ?
B4 B1 B2 57.37(15) 10_556 11_655 ?
B2 B1 B2 108.0(3) . 11_655 ?
B2 B4 B2 116.9(3) 4_655 10_556 ?
B2 B4 B3 109.2(3) 4_655 . ?
B2 B4 B3 59.53(19) 10_556 . ?
B2 B4 B3 59.53(19) 4_655 11_655 ?
B2 B4 B3 109.2(3) 10_556 11_655 ?
B3 B4 B3 58.7(3) . 11_655 ?
B2 B4 B1 62.52(16) 4_655 10_556 ?
B2 B4 B1 62.52(16) 10_556 10_556 ?
B3 B4 B1 104.6(3) . 10_556 ?
B3 B4 B1 104.6(3) 11_655 10_556 ?
C1 B2 B4 110.7(2) . 10_556 ?
C1 B2 B3 107.5(2) . . ?
B4 B2 B3 61.0(2) 10_556 . ?
C1 B2 B2 56.79(13) . 10_556 ?
B4 B2 B2 107.68(17) 10_556 10_556 ?
B3 B2 B2 59.75(12) . 10_556 ?
C1 B2 B1 58.49(18) . . ?
B4 B2 B1 60.12(18) 10_556 . ?
B3 B2 B1 104.0(2) . . ?
B2 B2 B1 99.43(14) 10_556 . ?
B3 B3 B2 110.74(16) 11_655 . ?
B3 B3 B2 110.74(16) 11_655 10_556 ?
B2 B3 B2 60.5(2) . 10_556 ?
B3 B3 B4 60.65(14) 11_655 10_556 ?
B2 B3 B4 59.46(16) . 10_556 ?
B2 B3 B4 107.0(3) 10_556 10_556 ?
B3 B3 B4 60.65(14) 11_655 . ?
B2 B3 B4 107.0(3) . . ?
B2 B3 B4 59.46(16) 10_556 . ?
B4 B3 B4 105.4(3) 10_556 . ?
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
I1 Ga1 2.5638(5) . ?
Ga1 Si1 2.4331(11) . ?
Ga1 Si1 2.4332(11) 11_655 ?
Si1 N1 1.806(2) . ?
Si1 N1 1.806(2) 10_556 ?
Si1 C1 1.821(4) . ?
Si1 C2 2.265(4) . ?
N1 C2 1.347(3) . ?
N1 C9 1.493(4) . ?
C9 C12 1.519(4) . ?
C9 C11 1.525(4) . ?
C9 C10 1.528(4) . ?
C2 C3 1.486(5) . ?
C3 C8 1.388(6) . ?
C3 C4 1.391(6) . ?
C7 C6 1.368(7) . ?
C7 C8 1.392(6) . ?
C5 C6 1.390(7) . ?
C5 C4 1.398(6) . ?
C1 B2 1.636(4) . ?
C1 B2 1.636(4) 10_556 ?
C1 B1 1.726(4) . ?
C1 B1 1.726(4) 10_556 ?
B1 B4 1.830(6) 10_556 ?
B1 B2 1.873(4) . ?
B1 B2 1.873(4) 11_655 ?
B4 B2 1.778(4) 4_655 ?
B4 B2 1.778(4) 10_556 ?
B4 B3 1.805(5) . ?
B4 B3 1.805(5) 11_655 ?
B2 B3 1.779(5) . ?
B2 B2 1.792(6) 10_556 ?
B3 B3 1.770(9) 11_655 ?
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 0.000 0.000 -0.011 1196 353 ' '
2 0.500 0.500 -0.007 1196 353 ' '
