#------------------------------------------------------------------------------
#$Date: 2022-03-05 00:06:00 +0200 (Sat, 05 Mar 2022) $
#$Revision: 273348 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/61/1566157.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_1566157
loop_
_publ_author_name
'Guo, Rui'
'Zhang, Xin'
'Li, Tong'
'Li, Qianli'
'Ruiz, David A.'
'Liu, Liu Leo'
'Tung, Chen-Ho'
'Kong, Lingbing'
_publ_section_title
;
 Unraveling the reactivity of a cationic iminoborane: avenues to unusual
 boron cations
;
_journal_issue                   8
_journal_name_full               'Chemical Science'
_journal_page_first              2303
_journal_page_last               2309
_journal_paper_doi               10.1039/D2SC00002D
_journal_volume                  13
_journal_year                    2022
_chemical_formula_moiety         'Al Br4, C33 H59 B N5 Si'
_chemical_formula_sum            'C33 H59 Al B Br4 N5 Si'
_chemical_formula_weight         911.37
_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     dual
_audit_creation_date             2021-09-03
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-09-11 deposited with the CCDC.	2022-01-26 downloaded from the CCDC.
;
_cell_angle_alpha                109.980(4)
_cell_angle_beta                 104.192(3)
_cell_angle_gamma                102.755(3)
_cell_formula_units_Z            2
_cell_length_a                   11.9613(4)
_cell_length_b                   13.4134(6)
_cell_length_c                   15.2453(6)
_cell_measurement_reflns_used    9154
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      75.9790
_cell_measurement_theta_min      3.2770
_cell_volume                     2100.41(17)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      173.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     35.00 120.00   1.00    0.10    --   48.45  56.00 159.00   85
  2  ω    -23.00  53.00   1.00    0.10    --   48.45 -56.00  16.00   76
  3  ω    -19.00  19.00   1.00    0.10    --  -48.45  56.00 159.00   38
  4  ω    -27.00  27.00   1.00    0.10    --  -48.45  19.00 150.00   54
  5  ω    -61.00 -33.00   1.00    0.10    --  -48.45  56.00 159.00   28
  6  ω   -119.00 -81.00   1.00    0.10    --  -48.45 -56.00  16.00   38
  7  ω    -80.00 -34.00   1.00    0.10    --  -48.45 -56.00  16.00   46
  8  ω    -59.00 -15.00   1.00    0.14    --  -86.25  56.00 159.00   44
  9  ω    -43.00 -13.00   1.00    0.14    --  -86.25  38.00 120.00   30
 10  ω    -43.00 -15.00   1.00    0.14    --  -86.25  38.00   0.00   28
 11  ω    -62.00 -14.00   1.00    0.14    --  -86.25  57.00 -60.00   48
 12  ω   -156.00 -72.00   1.00    0.14    --  -86.25 -56.00  16.00   84
 13  ω     92.00 176.00   1.00    0.14    --  106.49  57.00-120.00   84
 14  ω     92.00 175.00   1.00    0.14    --  106.49  57.00-180.00   83
 15  ω     93.00 155.00   1.00    0.14    --  106.49  56.00 159.00   62
 16  ω     95.00 174.00   1.00    0.14    --  106.49 125.00  60.00   79
 17  ω     95.00 126.00   1.00    0.14    --  106.49 125.00   0.00   31
 18  ω    129.00 178.00   1.00    0.14    --  106.49 125.00   0.00   49
 19  ω     39.00  65.00   1.00    0.14    --  106.49 -57.00-180.00   26
 20  ω     34.00 111.00   1.00    0.14    --  106.49-125.00   0.00   77
 21  ω     34.00 110.00   1.00    0.14    --  106.49-125.00  30.00   76
 22  ω     39.00 105.00   1.00    0.14    --  106.49 -99.00  30.00   66
 23  ω     37.00  64.00   1.00    0.14    --  106.49 -56.00  16.00   27
 24  ω     34.00 106.00   1.00    0.14    --  106.49 -99.00  90.00   72
 25  ω     35.00 106.00   1.00    0.14    --  106.49 -99.00 150.00   71
 26  ω     35.00 106.00   1.00    0.14    --  106.49 -99.00-150.00   71
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0278533000
_diffrn_orient_matrix_UB_12      0.1073951000
_diffrn_orient_matrix_UB_13      0.0020531000
_diffrn_orient_matrix_UB_21      0.1292729000
_diffrn_orient_matrix_UB_22      0.0724573000
_diffrn_orient_matrix_UB_23      0.0765071000
_diffrn_orient_matrix_UB_31      0.0488055000
_diffrn_orient_matrix_UB_32      -0.0054482000
_diffrn_orient_matrix_UB_33      -0.0855298000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0483
_diffrn_reflns_av_unetI/netI     0.0504
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            20493
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        67.078
_diffrn_reflns_theta_max         67.078
_diffrn_reflns_theta_min         3.293
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.361
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.53913
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.441
_exptl_crystal_description       block
_exptl_crystal_F_000             928
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.714
_refine_diff_density_min         -0.626
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     435
_refine_ls_number_reflns         7354
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0485
_refine_ls_R_factor_gt           0.0397
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0642P)²+0.0586P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1090
_refine_ls_wR_factor_ref         0.1148
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6066
_reflns_number_total             7354
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2sc00002d2.cif
_cod_data_source_block           klb-113
_cod_depositor_comments
'Adding full bibliography for 1566151--1566160.cif.'
_cod_original_cell_volume        2100.41(16)
_cod_database_code               1566157
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CBN
_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_max   0.296
_shelx_estimated_absorpt_t_min   0.296
_reflns_odcompleteness_completeness 98.28
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Si1-C33B \\sim Si1-C33A
 with sigma of 0.02
3. Rigid bond restraints
 C33A, C33B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
C33B \\sim C33A: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
Uanis(C33A) \\sim Ueq, Uanis(C33B) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
5. Others
 Sof(C33B)=Sof(H33A)=Sof(H33B)=Sof(H33C)=1-FVAR(1)
 Sof(C33A)=Sof(H33D)=Sof(H33E)=Sof(H33F)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C27(H27), C24(H24)
6.b Aromatic/amide H refined with riding coordinates:
 C30(H30), C5(H5), C3(H3)
6.c Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C28(H28A,H28B,H28C), C22(H22A,H22B,H22C), C23(H23A,H23B,
 H23C), C26(H26A,H26B,H26C), C25(H25A,H25B,H25C), C9(H9A,H9B,H9C), C10(H10A,
 H10B,H10C), C8(H8A,H8B,H8C), C17(H17A,H17B,H17C), C16(H16A,H16B,H16C),
 C18(H18A,H18B,H18C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C14(H14A,H14B,
 H14C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C33B(H33A,H33B,H33C),
 C33A(H33D,H33E,H33F)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.517
_oxdiff_exptl_absorpt_empirical_full_min 0.711
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
Br1 Br 1.02177(4) 0.65082(4) 0.35806(3) 0.04962(13) Uani 1 1 d . . . . .
Br2 Br 1.19595(4) 0.70906(4) 0.19614(3) 0.04943(13) Uani 1 1 d . . . . .
Br3 Br 1.31146(4) 0.89699(3) 0.46838(3) 0.04427(13) Uani 1 1 d . . . . .
Br4 Br 1.02777(4) 0.89704(4) 0.29435(3) 0.05131(14) Uani 1 1 d . . . . .
Al1 Al 1.13973(9) 0.78914(8) 0.33058(7) 0.0287(2) Uani 1 1 d . . . . .
Si1 Si 0.12416(8) 0.32791(7) 0.06304(7) 0.0282(2) Uani 1 1 d D . . . .
N1 N 0.4426(2) 0.3236(2) 0.19287(17) 0.0208(5) Uani 1 1 d . . . . .
N2 N 0.3273(2) 0.2784(2) 0.12544(18) 0.0230(5) Uani 1 1 d . . . . .
N3 N 0.2768(2) 0.3582(2) 0.14767(18) 0.0235(5) Uani 1 1 d . . . . .
N5 N 0.6740(2) 0.5154(2) 0.41864(18) 0.0254(5) Uani 1 1 d . . . . .
N4 N 0.6394(2) 0.6360(2) 0.35945(19) 0.0254(5) Uani 1 1 d . . . . .
C30 C 0.3532(3) 0.4563(3) 0.2272(2) 0.0255(6) Uani 1 1 d . . . . .
H30 H 0.334212 0.522806 0.254682 0.031 Uiso 1 1 calc R U . . .
C19 C 0.5946(3) 0.5269(2) 0.3452(2) 0.0225(6) Uani 1 1 d . . . . .
C27 C 0.6600(3) 0.4072(3) 0.4291(2) 0.0306(7) Uani 1 1 d . . . . .
H27 H 0.583878 0.350430 0.373728 0.037 Uiso 1 1 calc R U . . .
C29 C 0.6400(4) 0.4162(4) 0.5259(3) 0.0471(10) Uani 1 1 d . . . . .
H29A H 0.715545 0.465476 0.582343 0.071 Uiso 1 1 calc R U . . .
H29B H 0.617138 0.341213 0.525604 0.071 Uiso 1 1 calc R U . . .
H29C H 0.574237 0.447618 0.532208 0.071 Uiso 1 1 calc R U . . .
C28 C 0.7639(4) 0.3648(4) 0.4148(3) 0.0470(10) Uani 1 1 d . . . . .
H28A H 0.774629 0.364512 0.353072 0.070 Uiso 1 1 calc R U . . .
H28B H 0.745194 0.288104 0.410878 0.070 Uiso 1 1 calc R U . . .
H28C H 0.839436 0.414094 0.471326 0.070 Uiso 1 1 calc R U . . .
C21 C 0.7675(3) 0.6172(3) 0.4787(2) 0.0327(7) Uani 1 1 d . . . . .
C20 C 0.7460(3) 0.6922(3) 0.4422(2) 0.0313(7) Uani 1 1 d . . . . .
C22 C 0.8726(4) 0.6379(4) 0.5680(3) 0.0521(10) Uani 1 1 d . . . . .
H22A H 0.840970 0.617795 0.615379 0.078 Uiso 1 1 calc R U . . .
H22B H 0.923114 0.717684 0.600028 0.078 Uiso 1 1 calc R U . . .
H22C H 0.922367 0.591848 0.546832 0.078 Uiso 1 1 calc R U . . .
C23 C 0.8216(4) 0.8131(3) 0.4811(3) 0.0472(10) Uani 1 1 d . . . . .
H23A H 0.862834 0.823053 0.434987 0.071 Uiso 1 1 calc R U . . .
H23B H 0.882814 0.836235 0.546620 0.071 Uiso 1 1 calc R U . . .
H23C H 0.768541 0.859480 0.487158 0.071 Uiso 1 1 calc R U . . .
C24 C 0.5831(3) 0.6836(3) 0.2921(3) 0.0336(7) Uani 1 1 d . . . . .
H24 H 0.512975 0.619811 0.235741 0.040 Uiso 1 1 calc R U . . .
C26 C 0.6713(4) 0.7276(4) 0.2465(3) 0.0541(11) Uani 1 1 d . . . . .
H26A H 0.730759 0.800800 0.295805 0.081 Uiso 1 1 calc R U . . .
H26B H 0.625588 0.735962 0.188166 0.081 Uiso 1 1 calc R U . . .
H26C H 0.714352 0.674352 0.226288 0.081 Uiso 1 1 calc R U . . .
C25 C 0.5299(4) 0.7687(4) 0.3431(4) 0.0566(11) Uani 1 1 d . . . . .
H25A H 0.473251 0.734927 0.369995 0.085 Uiso 1 1 calc R U . . .
H25B H 0.485756 0.792330 0.294908 0.085 Uiso 1 1 calc R U . . .
H25C H 0.595996 0.834345 0.397508 0.085 Uiso 1 1 calc R U . . .
C1 C 0.5107(3) 0.2467(2) 0.1816(2) 0.0204(6) Uani 1 1 d . . . . .
C6 C 0.6011(3) 0.2597(2) 0.1380(2) 0.0215(6) Uani 1 1 d . . . . .
C5 C 0.6789(3) 0.1965(3) 0.1437(2) 0.0261(7) Uani 1 1 d . . . . .
H5 H 0.743301 0.207265 0.118159 0.031 Uiso 1 1 calc R U . . .
C4 C 0.6668(3) 0.1193(3) 0.1845(2) 0.0261(6) Uani 1 1 d . . . . .
C3 C 0.5678(3) 0.1009(3) 0.2166(2) 0.0267(7) Uani 1 1 d . . . . .
H3 H 0.554536 0.043337 0.239592 0.032 Uiso 1 1 calc R U . . .
C2 C 0.4870(3) 0.1616(2) 0.2170(2) 0.0237(6) Uani 1 1 d . . . . .
C7 C 0.6280(3) 0.3411(3) 0.0881(2) 0.0272(7) Uani 1 1 d . . . . .
C9 C 0.5216(3) 0.3795(3) 0.0477(3) 0.0350(8) Uani 1 1 d . . . . .
H9A H 0.447935 0.313511 0.005867 0.053 Uiso 1 1 calc R U . . .
H9B H 0.543541 0.419531 0.008097 0.053 Uiso 1 1 calc R U . . .
H9C H 0.505683 0.429719 0.103661 0.053 Uiso 1 1 calc R U . . .
C10 C 0.7389(3) 0.4440(3) 0.1639(3) 0.0342(8) Uani 1 1 d . . . . .
H10A H 0.717511 0.484719 0.220722 0.051 Uiso 1 1 calc R U . . .
H10B H 0.762922 0.493737 0.132456 0.051 Uiso 1 1 calc R U . . .
H10C H 0.807159 0.419230 0.187162 0.051 Uiso 1 1 calc R U . . .
C8 C 0.6611(3) 0.2818(3) -0.0040(3) 0.0345(8) Uani 1 1 d . . . . .
H8A H 0.739668 0.270687 0.018071 0.052 Uiso 1 1 calc R U . . .
H8B H 0.667173 0.328637 -0.041027 0.052 Uiso 1 1 calc R U . . .
H8C H 0.597272 0.208661 -0.047224 0.052 Uiso 1 1 calc R U . . .
C15 C 0.7569(3) 0.0549(3) 0.1949(3) 0.0309(7) Uani 1 1 d . . . . .
C17 C 0.8688(3) 0.0980(3) 0.1692(3) 0.0416(9) Uani 1 1 d . . . . .
H17A H 0.843092 0.081527 0.098126 0.062 Uiso 1 1 calc R U . . .
H17B H 0.927746 0.060522 0.184407 0.062 Uiso 1 1 calc R U . . .
H17C H 0.906975 0.179469 0.208634 0.062 Uiso 1 1 calc R U . . .
C16 C 0.6918(4) -0.0693(3) 0.1249(3) 0.0444(9) Uani 1 1 d . . . . .
H16A H 0.625281 -0.100496 0.144975 0.067 Uiso 1 1 calc R U . . .
H16B H 0.750161 -0.110099 0.128310 0.067 Uiso 1 1 calc R U . . .
H16C H 0.658000 -0.077162 0.056556 0.067 Uiso 1 1 calc R U . . .
C18 C 0.8017(4) 0.0675(4) 0.3028(3) 0.0471(10) Uani 1 1 d . . . . .
H18A H 0.841798 0.147371 0.348041 0.071 Uiso 1 1 calc R U . . .
H18B H 0.860108 0.027228 0.309885 0.071 Uiso 1 1 calc R U . . .
H18C H 0.731816 0.035781 0.319164 0.071 Uiso 1 1 calc R U . . .
C11 C 0.3751(3) 0.1240(3) 0.2474(2) 0.0286(7) Uani 1 1 d . . . . .
C12 C 0.4026(4) 0.0609(4) 0.3142(4) 0.0510(11) Uani 1 1 d . . . . .
H12A H 0.415751 -0.008165 0.276363 0.076 Uiso 1 1 calc R U . . .
H12B H 0.333087 0.041708 0.335716 0.076 Uiso 1 1 calc R U . . .
H12C H 0.476174 0.109333 0.372833 0.076 Uiso 1 1 calc R U . . .
C13 C 0.2694(3) 0.0412(3) 0.1512(3) 0.0404(8) Uani 1 1 d . . . . .
H13A H 0.249697 0.079292 0.107896 0.061 Uiso 1 1 calc R U . . .
H13B H 0.197447 0.013646 0.167190 0.061 Uiso 1 1 calc R U . . .
H13C H 0.293354 -0.022440 0.116897 0.061 Uiso 1 1 calc R U . . .
C14 C 0.3327(3) 0.2174(3) 0.3064(3) 0.0373(8) Uani 1 1 d . . . . .
H14A H 0.400526 0.271114 0.367677 0.056 Uiso 1 1 calc R U . . .
H14B H 0.264188 0.183951 0.323423 0.056 Uiso 1 1 calc R U . . .
H14C H 0.306266 0.256534 0.265720 0.056 Uiso 1 1 calc R U . . .
C31 C 0.0525(3) 0.1726(3) -0.0015(3) 0.0406(8) Uani 1 1 d . . . . .
H31A H 0.101338 0.140960 -0.039277 0.061 Uiso 1 1 calc R U . . .
H31B H -0.030493 0.153120 -0.047243 0.061 Uiso 1 1 calc R U . . .
H31C H 0.048678 0.141697 0.047758 0.061 Uiso 1 1 calc R U . . .
C32 C 0.1512(4) 0.3955(4) -0.0200(3) 0.0564(12) Uani 1 1 d . . . . .
H32A H 0.191963 0.476722 0.019364 0.085 Uiso 1 1 calc R U . . .
H32B H 0.072817 0.381518 -0.069300 0.085 Uiso 1 1 calc R U . . .
H32C H 0.203233 0.364182 -0.054168 0.085 Uiso 1 1 calc R U . . .
C33B C 0.0402(10) 0.3979(10) 0.1320(16) 0.040(3) Uani 0.54(6) 1 d D U P A 2
H33A H 0.038331 0.374808 0.186143 0.060 Uiso 0.54(6) 1 calc R U P A 2
H33B H -0.043689 0.377461 0.087314 0.060 Uiso 0.54(6) 1 calc R U P A 2
H33C H 0.080222 0.479616 0.159836 0.060 Uiso 0.54(6) 1 calc R U P A 2
B1 B 0.4696(3) 0.4389(3) 0.2616(2) 0.0219(7) Uani 1 1 d . . . . .
C33A C 0.0461(11) 0.3883(11) 0.1554(16) 0.032(3) Uani 0.46(6) 1 d D U P A 1
H33D H 0.048989 0.351403 0.201005 0.048 Uiso 0.46(6) 1 calc R U P A 1
H33E H -0.039390 0.374832 0.118564 0.048 Uiso 0.46(6) 1 calc R U P A 1
H33F H 0.088861 0.469454 0.193669 0.048 Uiso 0.46(6) 1 calc R U P A 1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.2130 0.2455 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 '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
Br1 Al1 Br2 109.88(4) . . ?
Br3 Al1 Br1 109.71(4) . . ?
Br3 Al1 Br2 109.28(4) . . ?
Br3 Al1 Br4 110.66(4) . . ?
Br4 Al1 Br1 109.29(4) . . ?
Br4 Al1 Br2 108.00(4) . . ?
N3 Si1 C31 107.16(15) . . ?
N3 Si1 C32 104.31(17) . . ?
N3 Si1 C33A 101.3(6) . . ?
C31 Si1 C33A 109.7(4) . . ?
C32 Si1 C31 113.9(2) . . ?
C32 Si1 C33A 118.8(7) . . ?
C33B Si1 N3 109.5(6) . . ?
C33B Si1 C31 114.2(4) . . ?
C33B Si1 C32 107.2(8) . . ?
N2 N1 C1 113.4(2) . . ?
N2 N1 B1 112.5(2) . . ?
C1 N1 B1 134.1(3) . . ?
N3 N2 N1 105.8(2) . . ?
N2 N3 Si1 116.71(19) . . ?
N2 N3 C30 113.9(2) . . ?
C30 N3 Si1 129.1(2) . . ?
C19 N5 C27 123.5(3) . . ?
C19 N5 C21 109.7(3) . . ?
C21 N5 C27 126.9(3) . . ?
C19 N4 C20 109.8(3) . . ?
C19 N4 C24 123.9(3) . . ?
C20 N4 C24 126.3(3) . . ?
N3 C30 H30 126.7 . . ?
N3 C30 B1 106.6(3) . . ?
B1 C30 H30 126.7 . . ?
N5 C19 N4 106.0(3) . . ?
N5 C19 B1 129.8(3) . . ?
N4 C19 B1 124.1(3) . . ?
N5 C27 H27 106.6 . . ?
N5 C27 C29 111.3(3) . . ?
N5 C27 C28 111.6(3) . . ?
C29 C27 H27 106.6 . . ?
C28 C27 H27 106.6 . . ?
C28 C27 C29 113.5(3) . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
N5 C21 C22 125.4(3) . . ?
C20 C21 N5 107.5(3) . . ?
C20 C21 C22 127.2(3) . . ?
N4 C20 C23 125.4(3) . . ?
C21 C20 N4 107.1(3) . . ?
C21 C20 C23 127.5(3) . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C20 C23 H23A 109.5 . . ?
C20 C23 H23B 109.5 . . ?
C20 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
N4 C24 H24 106.6 . . ?
N4 C24 C26 111.5(3) . . ?
N4 C24 C25 111.4(3) . . ?
C26 C24 H24 106.6 . . ?
C25 C24 H24 106.6 . . ?
C25 C24 C26 113.6(3) . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C6 C1 N1 119.0(2) . . ?
C6 C1 C2 121.9(3) . . ?
C2 C1 N1 119.1(2) . . ?
C1 C6 C7 127.0(3) . . ?
C5 C6 C1 117.1(3) . . ?
C5 C6 C7 115.8(3) . . ?
C6 C5 H5 118.4 . . ?
C4 C5 C6 123.3(3) . . ?
C4 C5 H5 118.4 . . ?
C5 C4 C3 117.2(3) . . ?
C5 C4 C15 122.5(3) . . ?
C3 C4 C15 120.3(3) . . ?
C4 C3 H3 118.0 . . ?
C4 C3 C2 124.1(3) . . ?
C2 C3 H3 118.0 . . ?
C1 C2 C11 126.5(3) . . ?
C3 C2 C1 115.8(3) . . ?
C3 C2 C11 117.5(3) . . ?
C6 C7 C8 109.1(2) . . ?
C9 C7 C6 116.4(3) . . ?
C9 C7 C8 104.9(3) . . ?
C10 C7 C6 107.6(3) . . ?
C10 C7 C9 109.9(3) . . ?
C10 C7 C8 108.7(3) . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C4 C15 C18 109.2(3) . . ?
C17 C15 C4 112.6(3) . . ?
C17 C15 C18 108.3(3) . . ?
C16 C15 C4 109.1(3) . . ?
C16 C15 C17 108.3(3) . . ?
C16 C15 C18 109.3(3) . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C18 H18A 109.5 . . ?
C15 C18 H18B 109.5 . . ?
C15 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C12 C11 C2 110.6(3) . . ?
C13 C11 C2 106.8(3) . . ?
C13 C11 C12 107.9(3) . . ?
C13 C11 C14 109.3(3) . . ?
C14 C11 C2 117.0(3) . . ?
C14 C11 C12 105.0(3) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C11 C14 H14A 109.5 . . ?
C11 C14 H14B 109.5 . . ?
C11 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
Si1 C31 H31A 109.5 . . ?
Si1 C31 H31B 109.5 . . ?
Si1 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
Si1 C32 H32A 109.5 . . ?
Si1 C32 H32B 109.5 . . ?
Si1 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
Si1 C33B H33A 109.5 . . ?
Si1 C33B H33B 109.5 . . ?
Si1 C33B H33C 109.5 . . ?
H33A C33B H33B 109.5 . . ?
H33A C33B H33C 109.5 . . ?
H33B C33B H33C 109.5 . . ?
N1 B1 C30 101.2(3) . . ?
N1 B1 C19 129.7(3) . . ?
C30 B1 C19 128.8(3) . . ?
Si1 C33A H33D 109.5 . . ?
Si1 C33A H33E 109.5 . . ?
Si1 C33A H33F 109.5 . . ?
H33D C33A H33E 109.5 . . ?
H33D C33A H33F 109.5 . . ?
H33E C33A H33F 109.5 . . ?
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
Br1 Al1 2.2965(10) . ?
Br2 Al1 2.3015(10) . ?
Br3 Al1 2.2848(11) . ?
Br4 Al1 2.2875(11) . ?
Si1 N3 1.823(3) . ?
Si1 C31 1.855(4) . ?
Si1 C32 1.839(4) . ?
Si1 C33B 1.804(10) . ?
Si1 C33A 1.927(13) . ?
N1 N2 1.355(3) . ?
N1 C1 1.442(4) . ?
N1 B1 1.449(4) . ?
N2 N3 1.327(3) . ?
N3 C30 1.369(4) . ?
N5 C19 1.356(4) . ?
N5 C27 1.490(4) . ?
N5 C21 1.388(4) . ?
N4 C19 1.362(4) . ?
N4 C20 1.387(4) . ?
N4 C24 1.488(4) . ?
C30 H30 0.9500 . ?
C30 B1 1.462(5) . ?
C19 B1 1.585(4) . ?
C27 H27 1.0000 . ?
C27 C29 1.522(5) . ?
C27 C28 1.509(5) . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C21 C20 1.347(5) . ?
C21 C22 1.503(5) . ?
C20 C23 1.494(5) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24 1.0000 . ?
C24 C26 1.519(5) . ?
C24 C25 1.507(5) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C1 C6 1.411(4) . ?
C1 C2 1.423(4) . ?
C6 C5 1.396(4) . ?
C6 C7 1.552(4) . ?
C5 H5 0.9500 . ?
C5 C4 1.377(4) . ?
C4 C3 1.392(5) . ?
C4 C15 1.534(4) . ?
C3 H3 0.9500 . ?
C3 C2 1.395(4) . ?
C2 C11 1.559(4) . ?
C7 C9 1.544(5) . ?
C7 C10 1.533(5) . ?
C7 C8 1.552(4) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C15 C17 1.532(5) . ?
C15 C16 1.525(5) . ?
C15 C18 1.536(5) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C11 C12 1.552(4) . ?
C11 C13 1.530(5) . ?
C11 C14 1.539(5) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33B H33A 0.9800 . ?
C33B H33B 0.9800 . ?
C33B H33C 0.9800 . ?
C33A H33D 0.9800 . ?
C33A H33E 0.9800 . ?
C33A H33F 0.9800 . ?
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
Si1 N3 C30 B1 -173.3(2) . . . . ?
N1 N2 N3 Si1 174.72(17) . . . . ?
N1 N2 N3 C30 0.4(3) . . . . ?
N1 C1 C6 C5 169.4(3) . . . . ?
N1 C1 C6 C7 -7.6(4) . . . . ?
N1 C1 C2 C3 -171.2(3) . . . . ?
N1 C1 C2 C11 14.2(4) . . . . ?
N2 N1 C1 C6 104.2(3) . . . . ?
N2 N1 C1 C2 -77.4(3) . . . . ?
N2 N1 B1 C30 1.0(3) . . . . ?
N2 N1 B1 C19 -173.9(3) . . . . ?
N2 N3 C30 B1 0.3(3) . . . . ?
N3 C30 B1 N1 -0.7(3) . . . . ?
N3 C30 B1 C19 174.3(3) . . . . ?
N5 C19 B1 N1 -50.1(5) . . . . ?
N5 C19 B1 C30 136.3(3) . . . . ?
N5 C21 C20 N4 -0.2(4) . . . . ?
N5 C21 C20 C23 -179.7(3) . . . . ?
N4 C19 B1 N1 134.1(3) . . . . ?
N4 C19 B1 C30 -39.5(5) . . . . ?
C19 N5 C27 C29 -116.4(3) . . . . ?
C19 N5 C27 C28 115.7(3) . . . . ?
C19 N5 C21 C20 -0.1(4) . . . . ?
C19 N5 C21 C22 179.8(3) . . . . ?
C19 N4 C20 C21 0.4(4) . . . . ?
C19 N4 C20 C23 179.9(3) . . . . ?
C19 N4 C24 C26 -119.4(3) . . . . ?
C19 N4 C24 C25 112.6(3) . . . . ?
C27 N5 C19 N4 -178.7(3) . . . . ?
C27 N5 C19 B1 4.9(5) . . . . ?
C27 N5 C21 C20 178.9(3) . . . . ?
C27 N5 C21 C22 -1.2(5) . . . . ?
C21 N5 C19 N4 0.3(3) . . . . ?
C21 N5 C19 B1 -176.1(3) . . . . ?
C21 N5 C27 C29 64.7(4) . . . . ?
C21 N5 C27 C28 -63.2(4) . . . . ?
C20 N4 C19 N5 -0.5(3) . . . . ?
C20 N4 C19 B1 176.2(3) . . . . ?
C20 N4 C24 C26 57.6(4) . . . . ?
C20 N4 C24 C25 -70.4(4) . . . . ?
C22 C21 C20 N4 179.9(3) . . . . ?
C22 C21 C20 C23 0.4(6) . . . . ?
C24 N4 C19 N5 177.0(3) . . . . ?
C24 N4 C19 B1 -6.4(4) . . . . ?
C24 N4 C20 C21 -176.9(3) . . . . ?
C24 N4 C20 C23 2.5(5) . . . . ?
C1 N1 N2 N3 178.3(2) . . . . ?
C1 N1 B1 C30 -178.0(3) . . . . ?
C1 N1 B1 C19 7.1(5) . . . . ?
C1 C6 C5 C4 3.5(5) . . . . ?
C1 C6 C7 C9 -23.8(4) . . . . ?
C1 C6 C7 C10 100.0(3) . . . . ?
C1 C6 C7 C8 -142.2(3) . . . . ?
C1 C2 C11 C12 -160.8(3) . . . . ?
C1 C2 C11 C13 82.1(4) . . . . ?
C1 C2 C11 C14 -40.7(4) . . . . ?
C6 C1 C2 C3 7.2(4) . . . . ?
C6 C1 C2 C11 -167.5(3) . . . . ?
C6 C5 C4 C3 3.3(5) . . . . ?
C6 C5 C4 C15 -176.9(3) . . . . ?
C5 C6 C7 C9 159.2(3) . . . . ?
C5 C6 C7 C10 -77.0(3) . . . . ?
C5 C6 C7 C8 40.8(4) . . . . ?
C5 C4 C3 C2 -5.3(5) . . . . ?
C5 C4 C15 C17 8.1(5) . . . . ?
C5 C4 C15 C16 -112.1(4) . . . . ?
C5 C4 C15 C18 128.5(3) . . . . ?
C4 C3 C2 C1 0.2(5) . . . . ?
C4 C3 C2 C11 175.3(3) . . . . ?
C3 C4 C15 C17 -172.0(3) . . . . ?
C3 C4 C15 C16 67.7(4) . . . . ?
C3 C4 C15 C18 -51.7(4) . . . . ?
C3 C2 C11 C12 24.7(4) . . . . ?
C3 C2 C11 C13 -92.5(3) . . . . ?
C3 C2 C11 C14 144.8(3) . . . . ?
C2 C1 C6 C5 -9.0(4) . . . . ?
C2 C1 C6 C7 174.1(3) . . . . ?
C7 C6 C5 C4 -179.2(3) . . . . ?
C15 C4 C3 C2 174.9(3) . . . . ?
C31 Si1 N3 N2 24.0(2) . . . . ?
C31 Si1 N3 C30 -162.7(3) . . . . ?
C32 Si1 N3 N2 -97.1(3) . . . . ?
C32 Si1 N3 C30 76.2(3) . . . . ?
C33B Si1 N3 N2 148.4(7) . . . . ?
C33B Si1 N3 C30 -38.3(8) . . . . ?
B1 N1 N2 N3 -0.8(3) . . . . ?
B1 N1 C1 C6 -76.8(4) . . . . ?
B1 N1 C1 C2 101.5(4) . . . . ?
C33A Si1 N3 N2 138.9(6) . . . . ?
C33A Si1 N3 C30 -47.7(7) . . . . ?
