# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_amji182
_database_code_depnum_ccdc_archive 'CCDC 1416375'
_audit_update_record             
;
2015-08-27 deposited with the CCDC.
2015-09-08 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_THETM01_amji182             
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: 
Extremely poor diffracting crystal, No diffraction was observed 
beyond 1.1 \%A after 170 seconds of X-ray exposure per frame 
in a Supernova microfocus diffractometer. 
Data was cut after 1.1 \%A of resolution   
;
_vrf_PLAT340_amji182             
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............     0.0230 Ang.  
RESPONSE: 
Weak diffracting data caused the low C-C bond precision
;
# end Validation Reply Form


_audit_creation_date             2015-08-26
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.05.21 svn.r2940 for OlexSys, GUI svn.r4846)
;
_shelxl_version_number           2014/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C36 H44 B5 Cl8 N8, 3(Al Cl4), C H2 Cl2'
_chemical_formula_sum            'C37 H46 Al3 B5 Cl22 N8'
_chemical_formula_weight         1517.71
_chemical_melting_point          ?
_chemical_oxdiff_formula         C9H10N2B1Al1Cl5
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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'I 1 2/a 1'
_space_group_name_Hall           '-I 2ya'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, 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'

_cell_length_a                   22.085(4)
_cell_length_b                   13.0664(19)
_cell_length_c                   23.157(6)
_cell_angle_alpha                90
_cell_angle_beta                 96.490(18)
_cell_angle_gamma                90
_cell_volume                     6640(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1163
_cell_measurement_temperature    150.02(10)
_cell_measurement_theta_max      19.9490
_cell_measurement_theta_min      3.3970
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.979
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.31164
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear dark brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.518
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             3048
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0697
_diffrn_reflns_av_unetI/netI     0.1245
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            5396
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        18.846
_diffrn_reflns_theta_max         18.846
_diffrn_reflns_theta_min         3.080
_diffrn_ambient_temperature      150.02(10)
_diffrn_detector_area_resol_mean 8.0714
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -53.00   46.00   1.0000  170.0000
omega____ theta____ kappa____ phi______ frames
    -       -5.7757    0.0000  -30.0000 99

#__ type_ start__ end____ width___ exp.time_
  2 omega    3.00   58.00   1.0000  170.0000
omega____ theta____ kappa____ phi______ frames
    -        6.3225   57.0000 -180.0000 55
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0008292000
_diffrn_orient_matrix_UB_12      -0.0271391000
_diffrn_orient_matrix_UB_13      0.0263269000
_diffrn_orient_matrix_UB_21      -0.0239821000
_diffrn_orient_matrix_UB_22      -0.0310725000
_diffrn_orient_matrix_UB_23      -0.0134993000
_diffrn_orient_matrix_UB_31      0.0216907000
_diffrn_orient_matrix_UB_32      -0.0352818000
_diffrn_orient_matrix_UB_33      -0.0086140000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1587
_reflns_number_total             2585
_reflns_odcompleteness_completeness 98.56
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     18.81
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.760
_refine_diff_density_min         -0.456
_refine_diff_density_rms         0.117
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         2585
_refine_ls_number_restraints     174
_refine_ls_R_factor_all          0.1521
_refine_ls_R_factor_gt           0.0922
_refine_ls_restrained_S_all      1.035
_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)+(0.0822P)²+234.7403P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2207
_refine_ls_wR_factor_ref         0.2559
_refine_special_details          
;
atomic displacement parameters correspondig to Carbon, Nitrogen and 
Boron atoms were restrained using Rigu, Simu and EADP commands. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
N13 \\sim N18 \\sim N15 \\sim N14: within 2A with sigma of 0.002 and sigma for
terminal atoms of 0.004
C20 \\sim C22 \\sim C21 \\sim C23 \\sim C30 \\sim N14: within 2A with sigma of
0.002 and sigma for terminal atoms of 0.004
C34 \\sim B40 \\sim N13 \\sim C38 \\sim N18: within 2A with sigma of 0.002 and
sigma for terminal atoms of 0.004
Uanis(C17) = Uanis(C31)
Uanis(B29) = Uanis(B35) = Uanis(B40)
Uanis(N13) = Uanis(N18) = Uanis(N15) = Uanis(N14)
3. Rigid body (RIGU) restrains
 C37, Cl33, Cl24
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C16, C17, C19, C20, C21, C22, C23, C25, C27, C28, C30, C31, C32, C34, C36,
 C37, C38, C1, C2
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C1, N18, C16, C34, B40, N13, C38
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
4. Others
 Fixed Sof: Cl24(0.5) Cl33(0.5) C37(0.5) H37A(0.5) H37B(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C37(H37A,H37B)
5.b Me refined with riding coordinates:
 C16(H16A,H16B,H16C), C27(H27A,H27B,H27C), C1(H1A,H1B,H1C), C2(H2A,H2B,H2C)
5.c Aromatic/amide H refined with riding coordinates:
 C17(H17), C19(H19), C21(H21), C22(H22), C23(H23), C25(H25), C28(H28),
 C30(H30), C31(H31), C36(H36)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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
Cl1 Cl 0.8071(2) 0.1785(3) 0.3259(2) 0.0417(14) Uani 1 1 d . . . . .
Cl2 Cl 0.8712(2) 0.2983(3) 0.4276(2) 0.0408(14) Uani 1 1 d . . . . .
Cl3 Cl 0.5641(2) 0.1433(4) 0.4187(2) 0.0438(15) Uani 1 1 d . . . . .
Cl4 Cl 0.67056(19) 0.0330(4) 0.37379(19) 0.0391(14) Uani 1 1 d . . . . .
Cl5 Cl 0.3746(2) 0.2640(4) 0.7058(3) 0.0666(18) Uani 1 1 d . . . . .
Cl6 Cl 0.3016(2) 0.2490(4) 0.5624(2) 0.0651(18) Uani 1 1 d . . . . .
Cl7 Cl 0.5310(2) 0.2885(5) 0.7430(3) 0.082(2) Uani 1 1 d . . . . .
Cl8 Cl 0.4313(3) 0.4723(4) 0.7854(3) 0.084(2) Uani 1 1 d . . . . .
Cl9 Cl 0.3103(3) 0.4322(4) 0.4567(3) 0.076(2) Uani 1 1 d . . . . .
Cl10 Cl 0.4342(3) 0.2243(5) 0.8459(3) 0.092(2) Uani 1 1 d . . . . .
Al11 Al 0.2500 0.3419(6) 0.5000 0.048(3) Uani 1 2 d S T P . .
Al12 Al 0.4443(3) 0.3124(5) 0.7705(3) 0.056(2) Uani 1 1 d . . . . .
N13 N 0.5877(6) -0.0633(10) 0.4376(6) 0.0348(14) Uani 1 1 d . . . . .
N14 N 0.7949(6) 0.3887(10) 0.3379(6) 0.0348(14) Uani 1 1 d . . . . .
N15 N 0.6967(6) 0.3701(11) 0.3655(6) 0.0348(14) Uani 1 1 d . . . . .
C16 C 0.5794(7) 0.0199(13) 0.5660(7) 0.036(3) Uani 1 1 d . . . . .
H16A H 0.5525 0.0586 0.5389 0.054 Uiso 1 1 calc R . . . .
H16B H 0.5564 -0.0298 0.5849 0.054 Uiso 1 1 calc R . . . .
H16C H 0.5997 0.0652 0.5946 0.054 Uiso 1 1 calc R . . . .
C17 C 0.7158(7) 0.2545(12) 0.4502(7) 0.026(3) Uani 1 1 d . . . . .
H17 H 0.6756 0.2716 0.4542 0.031 Uiso 1 1 calc R . . . .
N18 N 0.6254(6) -0.0331(10) 0.5347(6) 0.0348(14) Uani 1 1 d . . . . .
C19 C 0.5267(8) -0.2067(14) 0.4032(8) 0.041(5) Uani 1 1 d . . . . .
H19 H 0.5059 -0.2435 0.3728 0.049 Uiso 1 1 calc R . . . .
C20 C 0.7391(8) 0.4247(13) 0.3326(8) 0.0357(16) Uani 1 1 d . . . . .
C21 C 0.7703(8) 0.5547(13) 0.2714(8) 0.0372(18) Uani 1 1 d . . . . .
H21 H 0.7620 0.6110 0.2472 0.045 Uiso 1 1 calc R . . . .
C22 C 0.7245(8) 0.5151(13) 0.2993(7) 0.0366(17) Uani 1 1 d . . . . .
H22 H 0.6861 0.5452 0.2969 0.044 Uiso 1 1 calc R . . . .
C23 C 0.8273(8) 0.5157(13) 0.2773(7) 0.0368(17) Uani 1 1 d . . . . .
H23 H 0.8578 0.5473 0.2592 0.044 Uiso 1 1 calc R . . . .
Cl24 Cl 0.5249(10) 0.487(2) 0.4858(12) 0.199(10) Uani 0.5 1 d . . . A -1
C25 C 0.5297(9) -0.2417(15) 0.4584(9) 0.050(5) Uani 1 1 d . . . . .
H25 H 0.5092 -0.3017 0.4656 0.060 Uiso 1 1 calc R . . . .
C27 C 0.6599(8) 0.4399(14) 0.3981(8) 0.047(6) Uani 1 1 d . . . . .
H27A H 0.6329 0.4004 0.4189 0.071 Uiso 1 1 calc R . . . .
H27B H 0.6865 0.4796 0.4250 0.071 Uiso 1 1 calc R . . . .
H27C H 0.6366 0.4848 0.3713 0.071 Uiso 1 1 calc R . . . .
C28 C 0.5557(8) -0.1134(14) 0.3925(9) 0.050(5) Uani 1 1 d . . . . .
H28 H 0.5529 -0.0866 0.3551 0.061 Uiso 1 1 calc R . . . .
B29 B 0.7500 0.177(2) 0.5000 0.0344(16) Uani 1 2 d S T P . .
C30 C 0.8403(8) 0.4292(13) 0.3103(7) 0.0359(16) Uani 1 1 d . . . . .
H30 H 0.8788 0.3995 0.3135 0.043 Uiso 1 1 calc R . . . .
C31 C 0.7023(7) 0.0978(12) 0.5256(7) 0.026(3) Uani 1 1 d . . . . .
H31 H 0.7075 0.0886 0.5657 0.031 Uiso 1 1 calc R . . . .
C32 C 0.7391(7) 0.2946(12) 0.4056(7) 0.023(4) Uani 1 1 d . . . . .
Cl33 Cl 0.5010(9) 0.5240(15) 0.3680(10) 0.174(7) Uani 0.5 1 d . . . A -1
C34 C 0.6580(8) 0.0459(13) 0.4976(7) 0.0342(16) Uani 1 1 d . . . . .
B35 B 0.8016(9) 0.2904(16) 0.3777(9) 0.0344(16) Uani 1 1 d . . . . .
C36 C 0.5614(8) -0.1926(13) 0.5037(8) 0.043(5) Uani 1 1 d . . . . .
H36 H 0.5644 -0.2192 0.5412 0.052 Uiso 1 1 calc R . . . .
C37 C 0.471(4) 0.459(6) 0.427(4) 0.20(3) Uani 0.5 1 d . . . A -1
H37A H 0.4308 0.4860 0.4330 0.240 Uiso 0.5 1 calc R . . A -1
H37B H 0.4673 0.3861 0.4199 0.240 Uiso 0.5 1 calc R . . A -1
C38 C 0.5889(8) -0.1018(13) 0.4918(8) 0.0349(16) Uani 1 1 d . . . . .
B40 B 0.6245(9) 0.0403(16) 0.4335(9) 0.0344(16) Uani 1 1 d . . . . .
C1 C 0.6674(8) -0.0930(13) 0.5749(7) 0.039(3) Uani 1 1 d . . . . .
H1A H 0.6966 -0.1265 0.5536 0.059 Uiso 1 1 calc R . . . .
H1B H 0.6882 -0.0485 0.6035 0.059 Uiso 1 1 calc R . . . .
H1C H 0.6449 -0.1435 0.5938 0.059 Uiso 1 1 calc R . . . .
C2 C 0.6562(8) 0.3085(15) 0.3229(8) 0.049(6) Uani 1 1 d . . . . .
H2A H 0.6275 0.2713 0.3429 0.073 Uiso 1 1 calc R . . . .
H2B H 0.6347 0.3534 0.2948 0.073 Uiso 1 1 calc R . . . .
H2C H 0.6804 0.2613 0.3034 0.073 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
Cl1 B35 1.90(2) . ?
Cl2 B35 1.82(2) . ?
Cl3 B40 1.90(2) . ?
Cl4 B40 1.81(2) . ?
Cl5 Al12 2.120(8) . ?
Cl6 Al11 2.118(7) . ?
Cl7 Al12 2.108(9) . ?
Cl8 Al12 2.142(9) . ?
Cl9 Al11 2.114(7) . ?
Cl10 Al12 2.123(9) . ?
Al11 Cl6 2.118(7) 2_556 ?
Al11 Cl9 2.115(7) 2_556 ?
N13 C28 1.36(2) . ?
N13 C38 1.35(2) . ?
N13 B40 1.59(2) . ?
N14 C20 1.310(19) . ?
N14 C30 1.356(19) . ?
N14 B35 1.58(2) . ?
N15 C20 1.46(2) . ?
N15 C27 1.482(19) . ?
N15 C32 1.59(2) . ?
N15 C2 1.49(2) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C16 N18 1.485(19) . ?
C17 H17 0.9300 . ?
C17 B29 1.65(2) . ?
C17 C32 1.31(2) . ?
N18 C34 1.57(2) . ?
N18 C38 1.50(2) . ?
N18 C1 1.463(19) . ?
C19 H19 0.9300 . ?
C19 C25 1.35(2) . ?
C19 C28 1.41(2) . ?
C20 C22 1.43(2) . ?
C21 H21 0.9300 . ?
C21 C22 1.36(2) . ?
C21 C23 1.35(2) . ?
C22 H22 0.9300 . ?
C23 H23 0.9300 . ?
C23 C30 1.38(2) . ?
Cl24 C37 1.75(8) . ?
C25 H25 0.9300 . ?
C25 C36 1.35(2) . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C28 H28 0.9300 . ?
B29 C17 1.65(2) 2_656 ?
B29 C31 1.63(2) . ?
B29 C31 1.63(2) 2_656 ?
C30 H30 0.9300 . ?
C31 H31 0.9300 . ?
C31 C34 1.30(2) . ?
C32 B35 1.59(3) . ?
Cl33 C37 1.80(7) . ?
C34 B40 1.58(3) . ?
C36 H36 0.9300 . ?
C36 C38 1.37(2) . ?
C37 H37A 0.9700 . ?
C37 H37B 0.9700 . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?

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
Cl6 Al11 Cl6 110.1(5) 2_556 . ?
Cl9 Al11 Cl6 108.9(2) 2_556 2_556 ?
Cl9 Al11 Cl6 108.9(2) . . ?
Cl9 Al11 Cl6 108.4(2) 2_556 . ?
Cl9 Al11 Cl6 108.4(2) . 2_556 ?
Cl9 Al11 Cl9 112.2(5) . 2_556 ?
Cl5 Al12 Cl8 107.7(4) . . ?
Cl5 Al12 Cl10 106.5(4) . . ?
Cl7 Al12 Cl5 110.7(4) . . ?
Cl7 Al12 Cl8 109.6(4) . . ?
Cl7 Al12 Cl10 110.6(4) . . ?
Cl10 Al12 Cl8 111.6(4) . . ?
C28 N13 B40 126.2(15) . . ?
C38 N13 C28 119.2(15) . . ?
C38 N13 B40 114.6(15) . . ?
C20 N14 C30 123.6(15) . . ?
C20 N14 B35 111.8(14) . . ?
C30 N14 B35 124.6(15) . . ?
C20 N15 C27 112.7(14) . . ?
C20 N15 C32 103.8(12) . . ?
C20 N15 C2 106.8(13) . . ?
C27 N15 C32 114.0(13) . . ?
C27 N15 C2 110.3(14) . . ?
C2 N15 C32 108.8(12) . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N18 C16 H16A 109.5 . . ?
N18 C16 H16B 109.5 . . ?
N18 C16 H16C 109.5 . . ?
B29 C17 H17 116.4 . . ?
C32 C17 H17 116.4 . . ?
C32 C17 B29 127.2(14) . . ?
C16 N18 C34 110.0(12) . . ?
C16 N18 C38 104.8(12) . . ?
C38 N18 C34 105.9(12) . . ?
C1 N18 C16 111.1(13) . . ?
C1 N18 C34 113.8(12) . . ?
C1 N18 C38 110.7(13) . . ?
C25 C19 H19 120.6 . . ?
C25 C19 C28 118.9(19) . . ?
C28 C19 H19 120.6 . . ?
N14 C20 N15 115.3(15) . . ?
N14 C20 C22 120.1(16) . . ?
C22 C20 N15 124.5(16) . . ?
C22 C21 H21 118.6 . . ?
C23 C21 H21 118.6 . . ?
C23 C21 C22 122.8(18) . . ?
C20 C22 H22 122.1 . . ?
C21 C22 C20 115.7(17) . . ?
C21 C22 H22 122.1 . . ?
C21 C23 H23 120.0 . . ?
C21 C23 C30 120.0(18) . . ?
C30 C23 H23 120.0 . . ?
C19 C25 H25 118.7 . . ?
C19 C25 C36 122.6(19) . . ?
C36 C25 H25 118.7 . . ?
N15 C27 H27A 109.5 . . ?
N15 C27 H27B 109.5 . . ?
N15 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
N13 C28 C19 119.2(18) . . ?
N13 C28 H28 120.4 . . ?
C19 C28 H28 120.4 . . ?
C17 B29 C17 104.4(19) . 2_656 ?
C31 B29 C17 112.2(8) 2_656 2_656 ?
C31 B29 C17 113.4(8) . 2_656 ?
C31 B29 C17 112.2(8) . . ?
C31 B29 C17 113.4(8) 2_656 . ?
C31 B29 C31 101.5(19) . 2_656 ?
N14 C30 C23 117.6(17) . . ?
N14 C30 H30 121.2 . . ?
C23 C30 H30 121.2 . . ?
B29 C31 H31 115.5 . . ?
C34 C31 B29 128.9(15) . . ?
C34 C31 H31 115.5 . . ?
N15 C32 B35 105.5(13) . . ?
C17 C32 N15 116.8(14) . . ?
C17 C32 B35 137.8(16) . . ?
N18 C34 B40 106.8(14) . . ?
C31 C34 N18 115.7(15) . . ?
C31 C34 B40 137.4(17) . . ?
Cl2 B35 Cl1 109.6(11) . . ?
N14 B35 Cl1 105.3(12) . . ?
N14 B35 Cl2 110.0(13) . . ?
N14 B35 C32 100.4(14) . . ?
C32 B35 Cl1 113.8(13) . . ?
C32 B35 Cl2 116.8(14) . . ?
C25 C36 H36 121.5 . . ?
C25 C36 C38 117.0(18) . . ?
C38 C36 H36 121.5 . . ?
Cl24 C37 Cl33 102(4) . . ?
Cl24 C37 H37A 111.3 . . ?
Cl24 C37 H37B 111.3 . . ?
Cl33 C37 H37A 111.3 . . ?
Cl33 C37 H37B 111.3 . . ?
H37A C37 H37B 109.2 . . ?
N13 C38 N18 110.2(14) . . ?
N13 C38 C36 123.0(17) . . ?
C36 C38 N18 126.8(16) . . ?
Cl4 B40 Cl3 110.1(11) . . ?
N13 B40 Cl3 105.2(12) . . ?
N13 B40 Cl4 109.6(13) . . ?
C34 B40 Cl3 112.4(13) . . ?
C34 B40 Cl4 118.4(14) . . ?
C34 B40 N13 99.9(15) . . ?
N18 C1 H1A 109.5 . . ?
N18 C1 H1B 109.5 . . ?
N18 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N15 C2 H2A 109.5 . . ?
N15 C2 H2B 109.5 . . ?
N15 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?

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
N14 C20 C22 C21 4(2) . . . . ?
N15 C20 C22 C21 -179.8(16) . . . . ?
N15 C32 B35 Cl1 -95.0(14) . . . . ?
N15 C32 B35 Cl2 135.8(13) . . . . ?
N15 C32 B35 N14 17.0(15) . . . . ?
C16 N18 C34 C31 82.0(18) . . . . ?
C16 N18 C34 B40 -96.9(15) . . . . ?
C16 N18 C38 N13 106.0(15) . . . . ?
C16 N18 C38 C36 -76(2) . . . . ?
C17 B29 C31 C34 161.2(16) 2_656 . . . ?
C17 B29 C31 C34 43(2) . . . . ?
C17 C32 B35 Cl1 85(2) . . . . ?
C17 C32 B35 Cl2 -44(3) . . . . ?
C17 C32 B35 N14 -162.7(19) . . . . ?
N18 C34 B40 Cl3 96.5(14) . . . . ?
N18 C34 B40 Cl4 -133.4(13) . . . . ?
N18 C34 B40 N13 -14.6(16) . . . . ?
C19 C25 C36 C38 3(3) . . . . ?
C20 N14 C30 C23 3(2) . . . . ?
C20 N14 B35 Cl1 105.8(14) . . . . ?
C20 N14 B35 Cl2 -136.2(14) . . . . ?
C20 N14 B35 C32 -12.5(18) . . . . ?
C20 N15 C32 C17 163.2(15) . . . . ?
C20 N15 C32 B35 -16.6(16) . . . . ?
C21 C23 C30 N14 -3(2) . . . . ?
C22 C21 C23 C30 4(3) . . . . ?
C23 C21 C22 C20 -4(3) . . . . ?
C25 C19 C28 N13 3(3) . . . . ?
C25 C36 C38 N13 -3(3) . . . . ?
C25 C36 C38 N18 178.9(16) . . . . ?
C27 N15 C20 N14 133.2(16) . . . . ?
C27 N15 C20 C22 -43(2) . . . . ?
C27 N15 C32 C17 40(2) . . . . ?
C27 N15 C32 B35 -139.5(15) . . . . ?
C28 N13 C38 N18 -178.6(14) . . . . ?
C28 N13 C38 C36 3(3) . . . . ?
C28 N13 B40 Cl3 71.6(19) . . . . ?
C28 N13 B40 Cl4 -47(2) . . . . ?
C28 N13 B40 C34 -171.8(16) . . . . ?
C28 C19 C25 C36 -3(3) . . . . ?
B29 C17 C32 N15 -177.9(15) . . . . ?
B29 C17 C32 B35 2(3) . . . . ?
B29 C31 C34 N18 173.2(15) . . . . ?
B29 C31 C34 B40 -8(3) . . . . ?
C30 N14 C20 N15 179.6(14) . . . . ?
C30 N14 C20 C22 -4(3) . . . . ?
C30 N14 B35 Cl1 -71.6(18) . . . . ?
C30 N14 B35 Cl2 46(2) . . . . ?
C30 N14 B35 C32 170.1(15) . . . . ?
C31 B29 C31 C34 -78.2(17) 2_656 . . . ?
C31 C34 B40 Cl3 -82(3) . . . . ?
C31 C34 B40 Cl4 48(3) . . . . ?
C31 C34 B40 N13 167(2) . . . . ?
C32 N15 C20 N14 9.4(18) . . . . ?
C32 N15 C20 C22 -166.6(15) . . . . ?
C32 C17 B29 C17 87.4(17) . . . 2_656 ?
C32 C17 B29 C31 -149.4(16) . . . . ?
C32 C17 B29 C31 -35(2) . . . 2_656 ?
C34 N18 C38 N13 -10.3(17) . . . . ?
C34 N18 C38 C36 167.9(16) . . . . ?
B35 N14 C20 N15 2(2) . . . . ?
B35 N14 C20 C22 178.3(15) . . . . ?
B35 N14 C30 C23 -179.6(15) . . . . ?
C38 N13 C28 C19 -3(2) . . . . ?
C38 N13 B40 Cl3 -107.4(14) . . . . ?
C38 N13 B40 Cl4 134.3(14) . . . . ?
C38 N13 B40 C34 9.2(18) . . . . ?
C38 N18 C34 C31 -165.2(15) . . . . ?
C38 N18 C34 B40 15.9(16) . . . . ?
B40 N13 C28 C19 178.3(15) . . . . ?
B40 N13 C38 N18 0.5(19) . . . . ?
B40 N13 C38 C36 -177.8(16) . . . . ?
C1 N18 C34 C31 -43.3(19) . . . . ?
C1 N18 C34 B40 137.8(15) . . . . ?
C1 N18 C38 N13 -134.2(14) . . . . ?
C1 N18 C38 C36 44(2) . . . . ?
C2 N15 C20 N14 -105.5(17) . . . . ?
C2 N15 C20 C22 79(2) . . . . ?
C2 N15 C32 C17 -83.3(17) . . . . ?
C2 N15 C32 B35 96.9(15) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_amji272
_database_code_depnum_ccdc_archive 'CCDC 1416376'
_audit_update_record             
;
2015-08-27 deposited with the CCDC.
2015-09-08 downloaded from the CCDC.
;
_audit_creation_date             2015-08-26
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.05.21 svn.r2940 for OlexSys, GUI svn.r4846)
;
_shelxl_version_number           2014/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C23 H30 B Br O2 Si'
_chemical_formula_sum            'C23 H30 B Br O2 Si'
_chemical_formula_weight         457.28
_chemical_melting_point          ?
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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   11.5585(7)
_cell_length_b                   18.4820(8)
_cell_length_c                   12.0048(9)
_cell_angle_alpha                90
_cell_angle_beta                 115.161(8)
_cell_angle_gamma                90
_cell_volume                     2321.2(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    2300
_cell_measurement_temperature    150.02(10)
_cell_measurement_theta_max      26.3130
_cell_measurement_theta_min      3.5700
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.838
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.95794
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.309
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             952
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0291
_diffrn_reflns_av_unetI/netI     0.0700
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.824
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            8379
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.824
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.979
_diffrn_reflns_theta_min         3.410
_diffrn_ambient_temperature      150.02(10)
_diffrn_detector_area_resol_mean 8.0714
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.824
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_diffrn_special_details          
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -41.00   40.00   1.0000   22.5000
omega____ theta____ kappa____ phi______ frames
    -       18.2292  -57.0000  120.0000 81

#__ type_ start__ end____ width___ exp.time_
  2 omega  -24.00   71.00   1.0000   22.5000
omega____ theta____ kappa____ phi______ frames
    -       18.2292   19.0000  -30.0000 95
;
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3511
_reflns_number_total             5079
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies (2013)'
_computing_data_collection       'CrysAlisPro, Agilent Technologies (2013)'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies (2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.641
_refine_diff_density_min         -0.985
_refine_diff_density_rms         0.082
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     326
_refine_ls_number_reflns         5079
_refine_ls_number_restraints     135
_refine_ls_R_factor_all          0.0929
_refine_ls_R_factor_gt           0.0555
_refine_ls_restrained_S_all      1.094
_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)+(0.0398P)²+3.5971P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1156
_refine_ls_wR_factor_ref         0.1343
_refine_special_details          
;
the tetramethyl dicarboxo ligand was modelled over two positions. 
The C-C distances of the methyl groups were restrained using
DFIX commands. The atomic displacement parameters of the disorder 
moiety were restrained using RIGU and SIMU commands.  
;
_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
 C205-C206
 2.4 with sigma of 0.02
 C105-C106
 2.4 with sigma of 0.02
 C106-C102
 2.4 with sigma of 0.02
 C102-C105
 2.4 with sigma of 0.02
 C104-C103
 2.4 with sigma of 0.02
 C107-C103
 2.4 with sigma of 0.02
 C104-C103
 2.4 with sigma of 0.02
 C107-C103
 2.4 with sigma of 0.02
 C206-C202
 2.4 with sigma of 0.02
 C205-C202
 2.4 with sigma of 0.02
 C207-C203
 2.4 with sigma of 0.02
 C204-C203
 2.4 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C203 \\sim O101: within 2A with sigma of 0.002 and sigma for terminal atoms of
0.004
4. Rigid body (RIGU) restrains
 O100, O101, C202, C207, C205, C204, C206, C203
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 O201, O200, C102, C104, C107, C106, C103, C105
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5. Others
 Sof(C205)=Sof(H20A)=Sof(H20B)=Sof(H20C)=Sof(C202)=Sof(C203)=Sof(C206)=
 Sof(H20D)=Sof(H20E)=Sof(H20F)=Sof(C204)=Sof(H20G)=Sof(H20H)=Sof(H20I)=
 Sof(O100)=Sof(O101)=Sof(C207)=Sof(H20J)=Sof(H20K)=Sof(H20L)=1-FVAR(1)
 Sof(C104)=Sof(H10A)=Sof(H10B)=Sof(H10C)=Sof(C102)=Sof(C103)=Sof(C107)=
 Sof(H10D)=Sof(H10E)=Sof(H10F)=Sof(C105)=Sof(H10G)=Sof(H10H)=Sof(H10I)=
 Sof(O200)=Sof(O201)=Sof(C106)=Sof(H10J)=Sof(H10K)=Sof(H10L)=FVAR(1)
6.a Me refined with riding coordinates:
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C104(H10A,H10B,
 H10C), C205(H20A,H20B,H20C), C107(H10D,H10E,H10F), C206(H20D,H20E,H20F),
 C105(H10G,H10H,H10I), C204(H20G,H20H,H20I), C106(H10J,H10K,H10L), C207(H20J,
 H20K,H20L)
6.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C10(H10), C11(H11), C13(H13), C14(H14)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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
B1 B 0.1449(4) 0.6074(2) 0.2838(4) 0.0199(9) Uani 1 1 d . . . . .
C1 C -0.0759(3) 0.63146(18) 0.2843(4) 0.0216(8) Uani 1 1 d . . . . .
C2 C -0.0512(4) 0.66408(19) 0.3962(4) 0.0289(9) Uani 1 1 d . . . . .
H2 H 0.0264 0.6537 0.4658 0.035 Uiso 1 1 calc R . . . .
C3 C -0.1384(5) 0.7117(2) 0.4078(5) 0.0390(11) Uani 1 1 d . . . . .
H3 H -0.1212 0.7326 0.4855 0.047 Uiso 1 1 calc R . . . .
C4 C -0.2499(4) 0.7285(2) 0.3067(5) 0.0452(12) Uani 1 1 d . . . . .
H4 H -0.3098 0.7609 0.3145 0.054 Uiso 1 1 calc R . . . .
C5 C -0.2736(4) 0.6983(2) 0.1954(5) 0.0422(12) Uani 1 1 d . . . . .
H5 H -0.3502 0.7104 0.1257 0.051 Uiso 1 1 calc R . . . .
C6 C -0.1881(3) 0.6504(2) 0.1821(4) 0.0306(9) Uani 1 1 d . . . . .
H6 H -0.2056 0.6304 0.1036 0.037 Uiso 1 1 calc R . . . .
C7 C 0.0139(3) 0.57605(18) 0.2730(3) 0.0181(7) Uani 1 1 d . . . . .
C8 C -0.0235(3) 0.50645(18) 0.2496(3) 0.0182(7) Uani 1 1 d . . . . .
C9 C -0.1533(3) 0.48395(17) 0.2376(3) 0.0182(7) Uani 1 1 d . . . . .
C10 C -0.2508(3) 0.46849(19) 0.1223(3) 0.0244(8) Uani 1 1 d . . . . .
H10 H -0.2356 0.4736 0.0509 0.029 Uiso 1 1 calc R . . . .
C11 C -0.3698(3) 0.4457(2) 0.1104(4) 0.0279(9) Uani 1 1 d . . . . .
H11 H -0.4358 0.4355 0.0313 0.033 Uiso 1 1 calc R . . . .
C12 C -0.3914(3) 0.43799(19) 0.2130(4) 0.0265(9) Uani 1 1 d . . . . .
C13 C -0.2974(4) 0.4532(2) 0.3288(4) 0.0333(10) Uani 1 1 d . . . . .
H13 H -0.3135 0.4478 0.3996 0.040 Uiso 1 1 calc R . . . .
C14 C -0.1790(3) 0.4764(2) 0.3396(4) 0.0262(8) Uani 1 1 d . . . . .
H14 H -0.1141 0.4874 0.4188 0.031 Uiso 1 1 calc R . . . .
C15 C 0.1000(4) 0.4276(2) 0.0955(3) 0.0277(9) Uani 1 1 d . . . . .
H15A H 0.0166 0.4285 0.0242 0.042 Uiso 1 1 calc R . . . .
H15B H 0.1489 0.4707 0.0945 0.042 Uiso 1 1 calc R . . . .
H15C H 0.1470 0.3842 0.0920 0.042 Uiso 1 1 calc R . . . .
C16 C 0.2317(4) 0.4248(2) 0.3783(4) 0.0352(10) Uani 1 1 d . . . . .
H16A H 0.2159 0.4243 0.4523 0.053 Uiso 1 1 calc R . . . .
H16B H 0.2795 0.3814 0.3767 0.053 Uiso 1 1 calc R . . . .
H16C H 0.2814 0.4679 0.3791 0.053 Uiso 1 1 calc R . . . .
C17 C -0.0106(4) 0.3421(2) 0.2408(4) 0.0333(10) Uani 1 1 d . . . . .
H17A H -0.0241 0.3404 0.3161 0.050 Uiso 1 1 calc R . . . .
H17B H -0.0935 0.3413 0.1689 0.050 Uiso 1 1 calc R . . . .
H17C H 0.0399 0.3000 0.2384 0.050 Uiso 1 1 calc R . . . .
C104 C 0.3715(15) 0.6299(10) 0.1618(14) 0.028(3) Uani 0.375(9) 1 d D . P A 1
H10A H 0.3977 0.5828 0.1429 0.042 Uiso 0.375(9) 1 calc R . P A 1
H10B H 0.2954 0.6468 0.0908 0.042 Uiso 0.375(9) 1 calc R . P A 1
H10C H 0.4411 0.6648 0.1803 0.042 Uiso 0.375(9) 1 calc R . P A 1
C205 C 0.3693(12) 0.7490(6) 0.3930(9) 0.061(3) Uani 0.625(9) 1 d D . P A 2
H20A H 0.2995 0.7795 0.3367 0.092 Uiso 0.625(9) 1 calc R . P A 2
H20B H 0.3829 0.7587 0.4779 0.092 Uiso 0.625(9) 1 calc R . P A 2
H20C H 0.4477 0.7600 0.3837 0.092 Uiso 0.625(9) 1 calc R . P A 2
C102 C 0.3392(10) 0.6221(6) 0.2796(11) 0.029(2) Uani 0.375(9) 1 d D . P A 1
C202 C 0.2883(6) 0.6562(4) 0.2245(6) 0.0271(15) Uani 0.625(9) 1 d D . P A 2
C103 C 0.3025(11) 0.6891(6) 0.3053(13) 0.037(2) Uani 0.375(9) 1 d D . P A 1
C203 C 0.3339(7) 0.6676(5) 0.3620(6) 0.0412(16) Uani 0.625(9) 1 d D . P A 2
C107 C 0.4420(10) 0.5852(6) 0.3983(10) 0.028(3) Uani 0.375(9) 1 d D . P A 1
H10D H 0.4656 0.5381 0.3766 0.043 Uiso 0.375(9) 1 calc R . P A 1
H10E H 0.5180 0.6161 0.4337 0.043 Uiso 0.375(9) 1 calc R . P A 1
H10F H 0.4066 0.5784 0.4586 0.043 Uiso 0.375(9) 1 calc R . P A 1
C206 C 0.4353(8) 0.6227(6) 0.4438(9) 0.080(3) Uani 0.625(9) 1 d D . P A 2
H20D H 0.5141 0.6337 0.4352 0.120 Uiso 0.625(9) 1 calc R . P A 2
H20E H 0.4485 0.6318 0.5288 0.120 Uiso 0.625(9) 1 calc R . P A 2
H20F H 0.4128 0.5717 0.4233 0.120 Uiso 0.625(9) 1 calc R . P A 2
C105 C 0.2516(14) 0.7415(6) 0.1981(13) 0.042(3) Uani 0.375(9) 1 d D . P A 1
H10G H 0.2281 0.7871 0.2249 0.064 Uiso 0.375(9) 1 calc R . P A 1
H10H H 0.3176 0.7507 0.1690 0.064 Uiso 0.375(9) 1 calc R . P A 1
H10I H 0.1760 0.7207 0.1311 0.064 Uiso 0.375(9) 1 calc R . P A 1
C204 C 0.2219(8) 0.7197(5) 0.1457(7) 0.052(2) Uani 0.625(9) 1 d D . P A 2
H20G H 0.2836 0.7588 0.1592 0.078 Uiso 0.625(9) 1 calc R . P A 2
H20H H 0.1849 0.7053 0.0589 0.078 Uiso 0.625(9) 1 calc R . P A 2
H20I H 0.1538 0.7364 0.1676 0.078 Uiso 0.625(9) 1 calc R . P A 2
O200 O 0.2249(8) 0.5766(5) 0.2425(10) 0.027(2) Uani 0.375(9) 1 d . . P A 1
O100 O 0.1868(6) 0.6013(4) 0.1965(6) 0.0336(15) Uani 0.625(9) 1 d . . P A 2
O201 O 0.1884(9) 0.6752(4) 0.3342(11) 0.031(2) Uani 0.375(9) 1 d . . P A 1
O101 O 0.2231(6) 0.6469(5) 0.3823(5) 0.0444(15) Uani 0.625(9) 1 d . . P A 2
Si1 Si 0.07647(9) 0.42655(5) 0.23930(9) 0.0197(2) Uani 1 1 d . . . . .
Br1 Br -0.55448(4) 0.40599(3) 0.19529(5) 0.04908(18) Uani 1 1 d . . . . .
C106 C 0.3924(19) 0.7260(8) 0.4246(14) 0.049(3) Uani 0.375(9) 1 d D . P A 1
H10J H 0.3561 0.7726 0.4323 0.073 Uiso 0.375(9) 1 calc R . P A 1
H10K H 0.4031 0.6951 0.4947 0.073 Uiso 0.375(9) 1 calc R . P A 1
H10L H 0.4757 0.7338 0.4233 0.073 Uiso 0.375(9) 1 calc R . P A 1
C207 C 0.3994(12) 0.6178(8) 0.2003(10) 0.056(3) Uani 0.625(9) 1 d D . P A 2
H20J H 0.4697 0.6521 0.2176 0.084 Uiso 0.625(9) 1 calc R . P A 2
H20K H 0.4308 0.5756 0.2543 0.084 Uiso 0.625(9) 1 calc R . P A 2
H20L H 0.3658 0.6023 0.1142 0.084 Uiso 0.625(9) 1 calc R . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
B1 C7 1.574(5) . ?
B1 O200 1.347(10) . ?
B1 O100 1.333(7) . ?
B1 O201 1.390(9) . ?
B1 O101 1.356(7) . ?
C1 C2 1.387(5) . ?
C1 C6 1.398(5) . ?
C1 C7 1.505(5) . ?
C2 H2 0.9500 . ?
C2 C3 1.388(5) . ?
C3 H3 0.9500 . ?
C3 C4 1.378(7) . ?
C4 H4 0.9500 . ?
C4 C5 1.364(7) . ?
C5 H5 0.9500 . ?
C5 C6 1.386(5) . ?
C6 H6 0.9500 . ?
C7 C8 1.348(5) . ?
C8 C9 1.504(4) . ?
C8 Si1 1.911(3) . ?
C9 C10 1.394(5) . ?
C9 C14 1.384(5) . ?
C10 H10 0.9500 . ?
C10 C11 1.387(5) . ?
C11 H11 0.9500 . ?
C11 C12 1.365(5) . ?
C12 C13 1.381(5) . ?
C12 Br1 1.899(3) . ?
C13 H13 0.9500 . ?
C13 C14 1.386(5) . ?
C14 H14 0.9500 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C15 Si1 1.858(4) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C16 Si1 1.860(4) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C17 Si1 1.862(4) . ?
C104 H10A 0.9800 . ?
C104 H10B 0.9800 . ?
C104 H10C 0.9800 . ?
C104 C102 1.615(19) . ?
C205 H20A 0.9800 . ?
C205 H20B 0.9800 . ?
C205 H20C 0.9800 . ?
C205 C203 1.562(13) . ?
C102 C103 1.384(14) . ?
C102 C107 1.571(17) . ?
C102 O200 1.467(12) . ?
C202 C203 1.520(9) . ?
C202 C204 1.498(12) . ?
C202 O100 1.478(7) . ?
C202 C207 1.597(13) . ?
C103 C105 1.516(19) . ?
C103 O201 1.522(12) . ?
C103 C106 1.53(2) . ?
C203 C206 1.432(13) . ?
C203 O101 1.453(8) . ?
C107 H10D 0.9800 . ?
C107 H10E 0.9800 . ?
C107 H10F 0.9800 . ?
C206 H20D 0.9800 . ?
C206 H20E 0.9800 . ?
C206 H20F 0.9800 . ?
C105 H10G 0.9800 . ?
C105 H10H 0.9800 . ?
C105 H10I 0.9800 . ?
C204 H20G 0.9800 . ?
C204 H20H 0.9800 . ?
C204 H20I 0.9800 . ?
C106 H10J 0.9800 . ?
C106 H10K 0.9800 . ?
C106 H10L 0.9800 . ?
C207 H20J 0.9800 . ?
C207 H20K 0.9800 . ?
C207 H20L 0.9800 . ?

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
O200 B1 C7 126.9(5) . . ?
O200 B1 O201 111.3(5) . . ?
O100 B1 C7 124.2(4) . . ?
O100 B1 O101 113.6(4) . . ?
O201 B1 C7 121.7(4) . . ?
O101 B1 C7 122.1(4) . . ?
C2 C1 C6 118.3(3) . . ?
C2 C1 C7 121.2(3) . . ?
C6 C1 C7 120.6(3) . . ?
C1 C2 H2 119.6 . . ?
C1 C2 C3 120.9(4) . . ?
C3 C2 H2 119.6 . . ?
C2 C3 H3 119.9 . . ?
C4 C3 C2 120.1(4) . . ?
C4 C3 H3 119.9 . . ?
C3 C4 H4 120.2 . . ?
C5 C4 C3 119.6(4) . . ?
C5 C4 H4 120.2 . . ?
C4 C5 H5 119.4 . . ?
C4 C5 C6 121.2(4) . . ?
C6 C5 H5 119.4 . . ?
C1 C6 H6 120.0 . . ?
C5 C6 C1 120.0(4) . . ?
C5 C6 H6 120.0 . . ?
C1 C7 B1 114.7(3) . . ?
C8 C7 B1 125.5(3) . . ?
C8 C7 C1 119.7(3) . . ?
C7 C8 C9 120.1(3) . . ?
C7 C8 Si1 127.0(2) . . ?
C9 C8 Si1 112.7(2) . . ?
C10 C9 C8 120.3(3) . . ?
C14 C9 C8 121.6(3) . . ?
C14 C9 C10 118.1(3) . . ?
C9 C10 H10 119.6 . . ?
C11 C10 C9 120.8(3) . . ?
C11 C10 H10 119.6 . . ?
C10 C11 H11 120.2 . . ?
C12 C11 C10 119.6(4) . . ?
C12 C11 H11 120.2 . . ?
C11 C12 C13 121.3(3) . . ?
C11 C12 Br1 119.0(3) . . ?
C13 C12 Br1 119.7(3) . . ?
C12 C13 H13 120.6 . . ?
C12 C13 C14 118.7(4) . . ?
C14 C13 H13 120.6 . . ?
C9 C14 C13 121.6(4) . . ?
C9 C14 H14 119.2 . . ?
C13 C14 H14 119.2 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
Si1 C15 H15A 109.5 . . ?
Si1 C15 H15B 109.5 . . ?
Si1 C15 H15C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
Si1 C16 H16A 109.5 . . ?
Si1 C16 H16B 109.5 . . ?
Si1 C16 H16C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
Si1 C17 H17A 109.5 . . ?
Si1 C17 H17B 109.5 . . ?
Si1 C17 H17C 109.5 . . ?
H10A C104 H10B 109.5 . . ?
H10A C104 H10C 109.5 . . ?
H10B C104 H10C 109.5 . . ?
C102 C104 H10A 109.5 . . ?
C102 C104 H10B 109.5 . . ?
C102 C104 H10C 109.5 . . ?
H20A C205 H20B 109.5 . . ?
H20A C205 H20C 109.5 . . ?
H20B C205 H20C 109.5 . . ?
C203 C205 H20A 109.5 . . ?
C203 C205 H20B 109.5 . . ?
C203 C205 H20C 109.5 . . ?
C103 C102 C104 108.8(11) . . ?
C103 C102 C107 111.8(11) . . ?
C103 C102 O200 105.0(9) . . ?
C107 C102 C104 117.7(9) . . ?
O200 C102 C104 107.4(10) . . ?
O200 C102 C107 105.2(8) . . ?
C203 C202 C207 109.0(7) . . ?
C204 C202 C203 115.1(7) . . ?
C204 C202 C207 118.0(7) . . ?
O100 C202 C203 102.6(5) . . ?
O100 C202 C204 104.5(6) . . ?
O100 C202 C207 106.0(7) . . ?
C102 C103 C105 115.3(12) . . ?
C102 C103 O201 106.2(9) . . ?
C102 C103 C106 117.2(12) . . ?
C105 C103 O201 103.9(9) . . ?
C105 C103 C106 112.0(10) . . ?
O201 C103 C106 99.8(11) . . ?
C202 C203 C205 109.1(7) . . ?
C206 C203 C205 109.9(7) . . ?
C206 C203 C202 117.9(9) . . ?
C206 C203 O101 104.8(7) . . ?
O101 C203 C205 112.0(8) . . ?
O101 C203 C202 102.8(5) . . ?
C102 C107 H10D 109.5 . . ?
C102 C107 H10E 109.5 . . ?
C102 C107 H10F 109.5 . . ?
H10D C107 H10E 109.5 . . ?
H10D C107 H10F 109.5 . . ?
H10E C107 H10F 109.5 . . ?
C203 C206 H20D 109.5 . . ?
C203 C206 H20E 109.5 . . ?
C203 C206 H20F 109.5 . . ?
H20D C206 H20E 109.5 . . ?
H20D C206 H20F 109.5 . . ?
H20E C206 H20F 109.5 . . ?
C103 C105 H10G 109.5 . . ?
C103 C105 H10H 109.5 . . ?
C103 C105 H10I 109.5 . . ?
H10G C105 H10H 109.5 . . ?
H10G C105 H10I 109.5 . . ?
H10H C105 H10I 109.5 . . ?
C202 C204 H20G 109.5 . . ?
C202 C204 H20H 109.5 . . ?
C202 C204 H20I 109.5 . . ?
H20G C204 H20H 109.5 . . ?
H20G C204 H20I 109.5 . . ?
H20H C204 H20I 109.5 . . ?
B1 O200 C102 108.5(7) . . ?
B1 O100 C202 106.4(5) . . ?
B1 O201 C103 103.9(6) . . ?
B1 O101 C203 107.7(5) . . ?
C15 Si1 C8 112.53(16) . . ?
C15 Si1 C16 111.55(19) . . ?
C15 Si1 C17 108.14(18) . . ?
C16 Si1 C8 109.52(17) . . ?
C16 Si1 C17 107.2(2) . . ?
C17 Si1 C8 107.65(16) . . ?
C103 C106 H10J 109.5 . . ?
C103 C106 H10K 109.5 . . ?
C103 C106 H10L 109.5 . . ?
H10J C106 H10K 109.5 . . ?
H10J C106 H10L 109.5 . . ?
H10K C106 H10L 109.5 . . ?
C202 C207 H20J 109.5 . . ?
C202 C207 H20K 109.5 . . ?
C202 C207 H20L 109.5 . . ?
H20J C207 H20K 109.5 . . ?
H20J C207 H20L 109.5 . . ?
H20K C207 H20L 109.5 . . ?

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
B1 C7 C8 C9 -178.0(3) . . . . ?
B1 C7 C8 Si1 6.5(5) . . . . ?
C1 C2 C3 C4 -1.6(6) . . . . ?
C1 C7 C8 C9 -1.3(5) . . . . ?
C1 C7 C8 Si1 -176.8(3) . . . . ?
C2 C1 C6 C5 -2.7(5) . . . . ?
C2 C1 C7 B1 -71.2(4) . . . . ?
C2 C1 C7 C8 111.8(4) . . . . ?
C2 C3 C4 C5 -0.2(6) . . . . ?
C3 C4 C5 C6 0.6(6) . . . . ?
C4 C5 C6 C1 0.9(6) . . . . ?
C6 C1 C2 C3 3.0(5) . . . . ?
C6 C1 C7 B1 110.0(4) . . . . ?
C6 C1 C7 C8 -67.0(5) . . . . ?
C7 B1 O200 C102 -176.2(6) . . . . ?
C7 B1 O100 C202 162.3(4) . . . . ?
C7 B1 O201 C103 -170.0(6) . . . . ?
C7 B1 O101 C203 -179.5(5) . . . . ?
C7 C1 C2 C3 -175.8(3) . . . . ?
C7 C1 C6 C5 176.2(3) . . . . ?
C7 C8 C9 C10 105.7(4) . . . . ?
C7 C8 C9 C14 -75.8(5) . . . . ?
C8 C9 C10 C11 178.1(3) . . . . ?
C8 C9 C14 C13 -177.7(3) . . . . ?
C9 C10 C11 C12 -0.3(6) . . . . ?
C10 C9 C14 C13 0.9(5) . . . . ?
C10 C11 C12 C13 0.7(6) . . . . ?
C10 C11 C12 Br1 -179.5(3) . . . . ?
C11 C12 C13 C14 -0.2(6) . . . . ?
C12 C13 C14 C9 -0.6(6) . . . . ?
C14 C9 C10 C11 -0.4(5) . . . . ?
C104 C102 C103 C105 23.1(15) . . . . ?
C104 C102 C103 O201 137.6(10) . . . . ?
C104 C102 C103 C106 -112.0(15) . . . . ?
C104 C102 O200 B1 -135.0(10) . . . . ?
C205 C203 O101 B1 134.7(8) . . . . ?
C102 C103 O201 B1 -19.1(12) . . . . ?
C202 C203 O101 B1 17.7(8) . . . . ?
C103 C102 O200 B1 -19.3(12) . . . . ?
C203 C202 O100 B1 24.3(7) . . . . ?
C107 C102 C103 C105 154.8(10) . . . . ?
C107 C102 C103 O201 -90.7(10) . . . . ?
C107 C102 C103 C106 19.7(16) . . . . ?
C107 C102 O200 B1 98.8(9) . . . . ?
C206 C203 O101 B1 -106.1(9) . . . . ?
C105 C103 O201 B1 103.0(10) . . . . ?
C204 C202 C203 C205 -31.2(9) . . . . ?
C204 C202 C203 C206 -157.5(7) . . . . ?
C204 C202 C203 O101 87.8(7) . . . . ?
C204 C202 O100 B1 -96.1(7) . . . . ?
O200 B1 C7 C1 -158.9(7) . . . . ?
O200 B1 C7 C8 17.9(8) . . . . ?
O200 B1 O201 C103 7.0(9) . . . . ?
O200 C102 C103 C105 -91.6(12) . . . . ?
O200 C102 C103 O201 22.8(13) . . . . ?
O200 C102 C103 C106 133.3(13) . . . . ?
O100 B1 C7 C1 -121.1(5) . . . . ?
O100 B1 C7 C8 55.7(7) . . . . ?
O100 B1 O101 C203 -2.6(7) . . . . ?
O100 C202 C203 C205 -144.0(8) . . . . ?
O100 C202 C203 C206 89.7(8) . . . . ?
O100 C202 C203 O101 -25.0(8) . . . . ?
O201 B1 C7 C1 17.6(8) . . . . ?
O201 B1 C7 C8 -165.5(7) . . . . ?
O201 B1 O200 C102 7.0(10) . . . . ?
O101 B1 C7 C1 55.4(6) . . . . ?
O101 B1 C7 C8 -127.8(6) . . . . ?
O101 B1 O100 C202 -14.5(7) . . . . ?
Si1 C8 C9 C10 -78.3(4) . . . . ?
Si1 C8 C9 C14 100.3(3) . . . . ?
Br1 C12 C13 C14 180.0(3) . . . . ?
C106 C103 O201 B1 -141.3(10) . . . . ?
C207 C202 C203 C205 103.9(10) . . . . ?
C207 C202 C203 C206 -22.4(11) . . . . ?
C207 C202 C203 O101 -137.0(8) . . . . ?
C207 C202 O100 B1 138.6(7) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
