# Electronic Supplementary Material (ESI) for ChemComm.
# 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_compound1a
_database_code_depnum_ccdc_archive 'CCDC 1051441'
_audit_update_record             
;
2015-02-27 deposited with the CCDC.
2015-03-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H36 As Cl2 N Si'
_chemical_formula_weight         656.57

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'
Si Si 0.0817 0.0704 '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'
As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.8947(5)
_cell_length_b                   12.7255(8)
_cell_length_c                   15.2825(9)
_cell_angle_alpha                78.686(3)
_cell_angle_beta                 73.993(3)
_cell_angle_gamma                70.480(3)
_cell_volume                     1556.81(16)
_cell_formula_units_Z            2
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.401
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             680
_exptl_absorpt_coefficient_mu    1.329
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.773
_exptl_absorpt_correction_T_max  0.777
_exptl_absorpt_process_details   'Sortav (Blessing)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Apex X8'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            19087
_diffrn_reflns_av_R_equivalents  0.0237
_diffrn_reflns_av_sigmaI/netI    0.0300
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.42
_diffrn_reflns_theta_max         25.50
_reflns_number_total             5772
_reflns_number_gt                4970
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
 The AsCl2 and SiMe3 fragments of the molecule were found to be disordered
 over 2 sites. This disorder was modelled and the non-hydrogen atoms of the
 major disordered set refined anisotropically. Those of the minor set were 
 refined isotropically.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0282P)²+1.9477P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5772
_refine_ls_number_parameters     415
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0478
_refine_ls_R_factor_gt           0.0379
_refine_ls_wR_factor_ref         0.0863
_refine_ls_wR_factor_gt          0.0825
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_restrained_S_all      1.047
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
As1 As 0.56450(4) 0.37643(3) 0.19836(2) 0.02296(11) Uani 0.8627(14) 1 d P A 1
Cl1 Cl 0.59572(9) 0.22069(7) 0.14045(6) 0.0333(2) Uani 0.8627(14) 1 d P A 1
Cl2 Cl 0.34499(10) 0.36363(7) 0.30230(6) 0.0400(2) Uani 0.8627(14) 1 d P A 1
N1 N 0.7186(4) 0.3307(3) 0.2662(2) 0.0197(6) Uani 0.8627(14) 1 d P A 1
C6 C 0.8581(3) 0.4780(2) 0.21979(16) 0.0214(5) Uani 1 1 d . A .
C3 C 1.1161(3) 0.3433(2) 0.10328(17) 0.0241(5) Uani 1 1 d . . .
H3 H 1.2044 0.2976 0.0631 0.029 Uiso 1 1 calc R . .
C5 C 0.9869(3) 0.5164(2) 0.16611(17) 0.0239(5) Uani 1 1 d . . .
H5 H 0.9867 0.5899 0.1706 0.029 Uiso 1 1 calc R . .
C2 C 0.9925(3) 0.2993(2) 0.15663(16) 0.0216(5) Uani 1 1 d . A .
C21 C 1.0105(3) 0.1759(2) 0.15455(17) 0.0242(5) Uani 1 1 d . . .
H21 H 0.8974 0.1683 0.1711 0.029 Uiso 1 1 calc R . .
C14 C 0.5815(3) 0.6223(2) 0.22916(17) 0.0238(5) Uani 1 1 d . . .
C7 C 0.7152(3) 0.5557(2) 0.28015(17) 0.0230(5) Uani 1 1 d . . .
H7 H 0.6657 0.5059 0.3307 0.028 Uiso 1 1 calc R . .
C8 C 0.7681(3) 0.6295(2) 0.32644(17) 0.0251(6) Uani 1 1 d . . .
C28 C 1.0913(3) 0.1380(2) 0.05899(18) 0.0248(6) Uani 1 1 d . . .
C36 C 0.6438(4) 0.1320(3) 0.3913(2) 0.0241(7) Uani 0.8627(14) 1 d P A 1
H36A H 0.5254 0.1475 0.4158 0.036 Uiso 0.8627(14) 1 calc PR A 1
H36B H 0.7020 0.0734 0.4327 0.036 Uiso 0.8627(14) 1 calc PR A 1
H36C H 0.6735 0.1064 0.3307 0.036 Uiso 0.8627(14) 1 calc PR A 1
C4 C 1.1154(3) 0.4518(2) 0.10645(17) 0.0242(5) Uani 1 1 d . . .
C19 C 0.4187(3) 0.6285(2) 0.26894(19) 0.0311(6) Uani 1 1 d . . .
H19 H 0.3909 0.5909 0.3285 0.037 Uiso 1 1 calc R . .
C1 C 0.8599(3) 0.3682(2) 0.21426(16) 0.0213(5) Uani 1 1 d . . .
C13 C 0.6938(3) 0.7443(2) 0.32462(18) 0.0304(6) Uani 1 1 d . . .
H13 H 0.6148 0.7804 0.2888 0.037 Uiso 1 1 calc R . .
C15 C 0.6179(3) 0.6802(2) 0.14262(18) 0.0284(6) Uani 1 1 d . . .
H15 H 0.7283 0.6772 0.1139 0.034 Uiso 1 1 calc R . .
C20 C 1.2497(3) 0.4972(2) 0.04567(19) 0.0334(6) Uani 1 1 d . . .
H20A H 1.2165 0.5372 -0.0109 0.050 Uiso 1 1 calc R . .
H20B H 1.3499 0.4350 0.0306 0.050 Uiso 1 1 calc R . .
H20C H 1.2701 0.5489 0.0776 0.050 Uiso 1 1 calc R . .
C11 C 0.8478(4) 0.7562(3) 0.4266(2) 0.0423(8) Uani 1 1 d . . .
H11 H 0.8726 0.7989 0.4622 0.051 Uiso 1 1 calc R . .
C22 C 1.1000(3) 0.0992(2) 0.22624(18) 0.0268(6) Uani 1 1 d . . .
C17 C 0.3346(3) 0.7458(2) 0.1379(2) 0.0366(7) Uani 1 1 d . . .
H17 H 0.2506 0.7879 0.1066 0.044 Uiso 1 1 calc R . .
C30 C 1.0845(3) 0.1539(2) -0.09986(19) 0.0336(6) Uani 1 1 d . . .
H30 H 1.0297 0.1885 -0.1481 0.040 Uiso 1 1 calc R . .
C29 C 1.0149(3) 0.1866(2) -0.01275(18) 0.0299(6) Uani 1 1 d . . .
H29 H 0.9126 0.2436 -0.0021 0.036 Uiso 1 1 calc R . .
C33 C 1.2403(3) 0.0550(2) 0.0405(2) 0.0330(6) Uani 1 1 d . . .
H33 H 1.2953 0.0195 0.0886 0.040 Uiso 1 1 calc R . .
C24 C 1.1414(4) -0.0706(2) 0.3310(2) 0.0426(8) Uani 1 1 d . . .
H24 H 1.1103 -0.1359 0.3598 0.051 Uiso 1 1 calc R . .
C16 C 0.4942(3) 0.7422(2) 0.09826(19) 0.0326(6) Uani 1 1 d . . .
H16 H 0.5202 0.7826 0.0398 0.039 Uiso 1 1 calc R . .
C9 C 0.8865(4) 0.5798(2) 0.37720(19) 0.0350(7) Uani 1 1 d . . .
H9 H 0.9411 0.5015 0.3779 0.042 Uiso 1 1 calc R . .
C23 C 1.0581(4) 0.0027(2) 0.26832(19) 0.0335(6) Uani 1 1 d . . .
H23 H 0.9712 -0.0133 0.2539 0.040 Uiso 1 1 calc R . .
C32 C 1.3102(4) 0.0228(2) -0.0466(2) 0.0375(7) Uani 1 1 d . . .
H32 H 1.4129 -0.0336 -0.0577 0.045 Uiso 1 1 calc R . .
C18 C 0.2962(3) 0.6887(2) 0.2228(2) 0.0372(7) Uani 1 1 d . . .
H18 H 0.1857 0.6904 0.2500 0.045 Uiso 1 1 calc R . .
C12 C 0.7338(4) 0.8070(2) 0.3746(2) 0.0380(7) Uani 1 1 d . . .
H12 H 0.6820 0.8857 0.3728 0.046 Uiso 1 1 calc R . .
C27 C 1.2289(4) 0.1189(2) 0.2476(2) 0.0390(7) Uani 1 1 d . . .
H27 H 1.2603 0.1842 0.2193 0.047 Uiso 1 1 calc R . .
C31 C 1.2327(3) 0.0717(2) -0.11696(19) 0.0334(6) Uani 1 1 d . . .
H31 H 1.2805 0.0491 -0.1766 0.040 Uiso 1 1 calc R . .
C26 C 1.3128(4) 0.0447(3) 0.3100(2) 0.0504(9) Uani 1 1 d . . .
H26 H 1.4012 0.0593 0.3237 0.060 Uiso 1 1 calc R . .
C25 C 1.2686(4) -0.0498(3) 0.3519(2) 0.0478(8) Uani 1 1 d . . .
H25 H 1.3255 -0.1004 0.3949 0.057 Uiso 1 1 calc R . .
C35 C 0.5531(5) 0.3567(3) 0.4665(2) 0.0416(9) Uani 0.8627(14) 1 d P A 1
H35A H 0.5882 0.4225 0.4646 0.062 Uiso 0.8627(14) 1 calc PR A 1
H35B H 0.5468 0.3151 0.5280 0.062 Uiso 0.8627(14) 1 calc PR A 1
H35C H 0.4450 0.3811 0.4520 0.062 Uiso 0.8627(14) 1 calc PR A 1
C10 C 0.9260(4) 0.6427(3) 0.4268(2) 0.0436(8) Uani 1 1 d . . .
H10 H 1.0075 0.6075 0.4611 0.052 Uiso 1 1 calc R . .
As1A As 0.8227(6) 0.2355(2) 0.3780(2) 0.0640(14) Uani 0.1373(14) 1 d P A 2
Si1 Si 0.70295(16) 0.26454(8) 0.38131(6) 0.0285(2) Uani 0.8627(14) 1 d P A 1
C34 C 0.9000(5) 0.2384(4) 0.4130(3) 0.0429(10) Uani 0.8627(14) 1 d P A 1
H34A H 0.9747 0.1659 0.3946 0.064 Uiso 0.8627(14) 1 calc PR A 1
H34B H 0.8806 0.2372 0.4795 0.064 Uiso 0.8627(14) 1 calc PR A 1
H34C H 0.9488 0.2982 0.3818 0.064 Uiso 0.8627(14) 1 calc PR A 1
Si1A Si 0.5768(13) 0.3052(10) 0.2548(8) 0.094(3) Uiso 0.1373(14) 1 d PD A 2
Cl1A Cl 0.6734(12) 0.3428(8) 0.4860(6) 0.081(2) Uiso 0.1373(14) 1 d P A 2
Cl2A Cl 0.700(3) 0.1197(19) 0.4111(15) 0.181(9) Uiso 0.1373(14) 1 d P A 2
C36A C 0.399(3) 0.331(2) 0.3568(14) 0.052(6) Uiso 0.1373(14) 1 d PD A 2
H36D H 0.4346 0.2901 0.4123 0.078 Uiso 0.1373(14) 1 calc PR A 2
H36E H 0.3121 0.3051 0.3482 0.078 Uiso 0.1373(14) 1 calc PR A 2
H36F H 0.3559 0.4116 0.3629 0.078 Uiso 0.1373(14) 1 calc PR A 2
C35A C 0.591(4) 0.177(2) 0.207(2) 0.083(10) Uiso 0.1373(14) 1 d PD A 2
H35D H 0.7061 0.1402 0.1793 0.124 Uiso 0.1373(14) 1 calc PR A 2
H35E H 0.5261 0.1978 0.1610 0.124 Uiso 0.1373(14) 1 calc PR A 2
H35F H 0.5497 0.1248 0.2569 0.124 Uiso 0.1373(14) 1 calc PR A 2
C34A C 0.553(5) 0.416(3) 0.155(2) 0.105(15) Uiso 0.1373(14) 1 d PD A 2
H34D H 0.4659 0.4832 0.1754 0.157 Uiso 0.1373(14) 1 calc PR A 2
H34E H 0.5244 0.3881 0.1083 0.157 Uiso 0.1373(14) 1 calc PR A 2
H34F H 0.6562 0.4342 0.1292 0.157 Uiso 0.1373(14) 1 calc PR A 2
N1A N 0.753(3) 0.307(3) 0.283(2) 0.053(12) Uiso 0.1373(14) 1 d PD 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
As1 N1 1.818(4) . ?
As1 Cl2 2.1823(8) . ?
As1 Cl1 2.2300(8) . ?
N1 C1 1.463(4) . ?
N1 Si1 1.785(4) . ?
C6 C5 1.387(3) . ?
C6 C1 1.410(3) . ?
C6 C7 1.521(3) . ?
C3 C2 1.387(3) . ?
C3 C4 1.389(3) . ?
C5 C4 1.380(4) . ?
C2 C1 1.405(3) . ?
C2 C21 1.531(3) . ?
C21 C22 1.526(3) . ?
C21 C28 1.532(4) . ?
C14 C19 1.389(4) . ?
C14 C15 1.392(4) . ?
C14 C7 1.523(3) . ?
C7 C8 1.531(3) . ?
C8 C13 1.386(4) . ?
C8 C9 1.387(4) . ?
C28 C29 1.383(4) . ?
C28 C33 1.389(4) . ?
C36 Si1 1.896(3) . ?
C4 C20 1.503(3) . ?
C19 C18 1.388(4) . ?
C1 N1A 1.50(3) . ?
C13 C12 1.388(4) . ?
C15 C16 1.383(4) . ?
C11 C12 1.372(4) . ?
C11 C10 1.377(4) . ?
C22 C27 1.383(4) . ?
C22 C23 1.388(4) . ?
C17 C18 1.371(4) . ?
C17 C16 1.371(4) . ?
C30 C31 1.377(4) . ?
C30 C29 1.386(4) . ?
C33 C32 1.382(4) . ?
C24 C25 1.372(5) . ?
C24 C23 1.384(4) . ?
C9 C10 1.383(4) . ?
C32 C31 1.371(4) . ?
C27 C26 1.387(4) . ?
C26 C25 1.374(4) . ?
C35 Si1 1.856(3) . ?
As1A N1A 1.71(3) . ?
As1A Cl2A 2.03(2) . ?
As1A Cl1A 2.194(10) . ?
Si1 C34 1.852(4) . ?
Si1A N1A 1.747(8) . ?
Si1A C34A 1.867(8) . ?
Si1A C35A 1.868(8) . ?
Si1A C36A 1.882(8) . ?

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
N1 As1 Cl2 101.66(10) . . ?
N1 As1 Cl1 102.86(10) . . ?
Cl2 As1 Cl1 93.99(3) . . ?
C1 N1 Si1 122.8(3) . . ?
C1 N1 As1 108.5(2) . . ?
Si1 N1 As1 128.45(17) . . ?
C5 C6 C1 118.7(2) . . ?
C5 C6 C7 119.8(2) . . ?
C1 C6 C7 121.4(2) . . ?
C2 C3 C4 122.4(2) . . ?
C4 C5 C6 122.4(2) . . ?
C3 C2 C1 118.6(2) . . ?
C3 C2 C21 118.8(2) . . ?
C1 C2 C21 122.5(2) . . ?
C22 C21 C2 111.7(2) . . ?
C22 C21 C28 111.3(2) . . ?
C2 C21 C28 112.5(2) . . ?
C19 C14 C15 118.2(2) . . ?
C19 C14 C7 120.5(2) . . ?
C15 C14 C7 121.3(2) . . ?
C6 C7 C14 111.5(2) . . ?
C6 C7 C8 113.3(2) . . ?
C14 C7 C8 113.1(2) . . ?
C13 C8 C9 118.3(2) . . ?
C13 C8 C7 122.2(2) . . ?
C9 C8 C7 119.4(2) . . ?
C29 C28 C33 117.5(2) . . ?
C29 C28 C21 119.9(2) . . ?
C33 C28 C21 122.6(2) . . ?
C5 C4 C3 117.8(2) . . ?
C5 C4 C20 121.5(2) . . ?
C3 C4 C20 120.7(2) . . ?
C18 C19 C14 120.9(3) . . ?
C2 C1 C6 119.9(2) . . ?
C2 C1 N1 121.5(2) . . ?
C6 C1 N1 118.6(2) . . ?
C2 C1 N1A 114.6(14) . . ?
C6 C1 N1A 123.5(14) . . ?
N1 C1 N1A 17.5(8) . . ?
C8 C13 C12 120.6(3) . . ?
C16 C15 C14 120.4(2) . . ?
C12 C11 C10 119.5(3) . . ?
C27 C22 C23 118.1(2) . . ?
C27 C22 C21 122.3(2) . . ?
C23 C22 C21 119.5(2) . . ?
C18 C17 C16 120.0(3) . . ?
C31 C30 C29 120.4(3) . . ?
C28 C29 C30 121.2(3) . . ?
C32 C33 C28 121.2(3) . . ?
C25 C24 C23 120.5(3) . . ?
C17 C16 C15 120.6(3) . . ?
C10 C9 C8 120.8(3) . . ?
C24 C23 C22 120.8(3) . . ?
C31 C32 C33 120.6(3) . . ?
C17 C18 C19 120.0(3) . . ?
C11 C12 C13 120.4(3) . . ?
C22 C27 C26 120.9(3) . . ?
C32 C31 C30 119.0(3) . . ?
C25 C26 C27 120.3(3) . . ?
C24 C25 C26 119.4(3) . . ?
C11 C10 C9 120.3(3) . . ?
N1A As1A Cl2A 99.4(10) . . ?
N1A As1A Cl1A 103.0(13) . . ?
Cl2A As1A Cl1A 97.7(7) . . ?
N1 Si1 C34 108.48(17) . . ?
N1 Si1 C35 113.16(17) . . ?
C34 Si1 C35 103.17(19) . . ?
N1 Si1 C36 109.33(14) . . ?
C34 Si1 C36 113.18(18) . . ?
C35 Si1 C36 109.48(15) . . ?
N1A Si1A C34A 104.2(18) . . ?
N1A Si1A C35A 116.5(17) . . ?
C34A Si1A C35A 102.7(19) . . ?
N1A Si1A C36A 109.8(16) . . ?
C34A Si1A C36A 114.1(17) . . ?
C35A Si1A C36A 109.4(15) . . ?
C1 N1A As1A 117.2(9) . . ?
C1 N1A Si1A 116.9(17) . . ?
As1A N1A Si1A 125.7(18) . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        25.50
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.623
_refine_diff_density_min         -0.445
_refine_diff_density_rms         0.057
####################################################################### 
# 
# 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_compound1c
_database_code_depnum_ccdc_archive 'CCDC 1051442'
_audit_update_record             
;
2015-02-27 deposited with the CCDC.
2015-03-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H40 Br2 N Sb Si'
_chemical_formula_weight         820.37

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'
Si Si 0.0817 0.0704 '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'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.1762(6)
_cell_length_b                   11.2391(8)
_cell_length_c                   15.5145(8)
_cell_angle_alpha                95.865(5)
_cell_angle_beta                 95.903(5)
_cell_angle_gamma                100.813(5)
_cell_volume                     1720.21(18)
_cell_formula_units_Z            2
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.584
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             820
_exptl_absorpt_coefficient_mu    3.187
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.642
_exptl_absorpt_correction_T_max  0.741
_exptl_absorpt_process_details   'Sortav (Blessing)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Apex X8'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13213
_diffrn_reflns_av_R_equivalents  0.0338
_diffrn_reflns_av_sigmaI/netI    0.0429
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.03
_diffrn_reflns_theta_max         25.50
_reflns_number_total             6406
_reflns_number_gt                5540
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0267P)²+0.4142P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6406
_refine_ls_number_parameters     393
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0363
_refine_ls_R_factor_gt           0.0274
_refine_ls_wR_factor_ref         0.0619
_refine_ls_wR_factor_gt          0.0581
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_restrained_S_all      1.028
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Sb1 Sb 0.978982(17) 0.120681(15) 0.364170(11) 0.01706(6) Uani 1 1 d . . .
Br1 Br 1.06335(3) 0.23325(3) 0.516425(17) 0.03058(9) Uani 1 1 d . . .
Br2 Br 0.74597(3) 0.04741(3) 0.407658(19) 0.02836(8) Uani 1 1 d . . .
Si1 Si 0.81342(7) 0.34936(6) 0.31831(5) 0.01734(16) Uani 1 1 d . . .
N1 N 0.9355(2) 0.25954(18) 0.29873(13) 0.0147(5) Uani 1 1 d . . .
C2 C 1.1265(3) 0.3666(2) 0.23012(16) 0.0163(6) Uani 1 1 d . . .
C27 C 0.8848(3) -0.0014(2) 0.16061(16) 0.0160(5) Uani 1 1 d . . .
C32 C 1.0142(3) -0.0186(2) 0.14843(16) 0.0178(6) Uani 1 1 d . . .
H32 H 1.0694 0.0362 0.1180 0.021 Uiso 1 1 calc R . .
C22 C 0.7285(3) -0.0296(2) -0.01015(17) 0.0216(6) Uani 1 1 d . . .
H22 H 0.7716 -0.0917 0.0093 0.026 Uiso 1 1 calc R . .
C1 C 1.0039(2) 0.2802(2) 0.22280(16) 0.0138(5) Uani 1 1 d . . .
C5 C 1.0133(3) 0.2454(2) 0.06706(16) 0.0169(6) Uani 1 1 d . . .
H5 H 0.9752 0.2027 0.0114 0.020 Uiso 1 1 calc R . .
C20 C 0.8323(3) 0.1086(2) 0.13130(16) 0.0154(5) Uani 1 1 d . . .
H20 H 0.7706 0.1302 0.1739 0.018 Uiso 1 1 calc R . .
C14 C 1.2876(3) 0.5470(2) 0.32006(16) 0.0184(6) Uani 1 1 d . . .
C4 C 1.1303(3) 0.3329(2) 0.07280(16) 0.0176(6) Uani 1 1 d . . .
C31 C 1.0632(3) -0.1152(2) 0.18044(17) 0.0224(6) Uani 1 1 d . . .
H31 H 1.1510 -0.1267 0.1710 0.027 Uiso 1 1 calc R . .
C6 C 0.9493(2) 0.2173(2) 0.13947(16) 0.0147(5) Uani 1 1 d . . .
C7 C 1.2028(3) 0.4206(2) 0.32004(16) 0.0169(6) Uani 1 1 d . . .
H7 H 1.1337 0.4291 0.3604 0.020 Uiso 1 1 calc R . .
C38 C 0.6426(3) 0.2768(3) 0.26055(19) 0.0268(7) Uani 1 1 d . . .
H38A H 0.6415 0.2822 0.1978 0.040 Uiso 1 1 calc R . .
H38B H 0.5753 0.3193 0.2833 0.040 Uiso 1 1 calc R . .
H38C H 0.6215 0.1908 0.2702 0.040 Uiso 1 1 calc R . .
C28 C 0.8054(3) -0.0845(2) 0.20338(17) 0.0214(6) Uani 1 1 d . . .
H28 H 0.7155 -0.0765 0.2099 0.026 Uiso 1 1 calc R . .
C3 C 1.1843(3) 0.3918(2) 0.15576(16) 0.0176(6) Uani 1 1 d . . .
H3 H 1.2647 0.4521 0.1614 0.021 Uiso 1 1 calc R . .
C29 C 0.8555(3) -0.1798(2) 0.23688(18) 0.0256(6) Uani 1 1 d . . .
H29 H 0.8008 -0.2349 0.2674 0.031 Uiso 1 1 calc R . .
C30 C 0.9849(3) -0.1939(2) 0.22566(18) 0.0239(6) Uani 1 1 d . . .
H30 H 1.0197 -0.2581 0.2492 0.029 Uiso 1 1 calc R . .
C33 C 1.1983(3) 0.3646(3) -0.00677(17) 0.0241(6) Uani 1 1 d . . .
H33 H 1.1572 0.3000 -0.0564 0.029 Uiso 1 1 calc R . .
C21 C 0.7487(2) 0.0818(2) 0.04097(16) 0.0171(6) Uani 1 1 d . . .
C26 C 0.6851(3) 0.1719(3) 0.01019(18) 0.0234(6) Uani 1 1 d . . .
H26 H 0.6980 0.2495 0.0440 0.028 Uiso 1 1 calc R . .
C8 C 1.2861(3) 0.3312(2) 0.35544(16) 0.0179(6) Uani 1 1 d . . .
C13 C 1.2788(3) 0.2151(2) 0.31452(17) 0.0205(6) Uani 1 1 d . . .
H13 H 1.2259 0.1900 0.2593 0.025 Uiso 1 1 calc R . .
C19 C 1.2379(3) 0.6504(2) 0.34690(17) 0.0226(6) Uani 1 1 d . . .
H19 H 1.1520 0.6408 0.3672 0.027 Uiso 1 1 calc R . .
C9 C 1.3683(3) 0.3672(3) 0.43574(17) 0.0223(6) Uani 1 1 d . . .
H9 H 1.3760 0.4473 0.4647 0.027 Uiso 1 1 calc R . .
C37 C 0.8017(3) 0.3825(3) 0.43620(17) 0.0277(7) Uani 1 1 d . . .
H37A H 0.7684 0.3063 0.4596 0.041 Uiso 1 1 calc R . .
H37B H 0.7393 0.4382 0.4446 0.041 Uiso 1 1 calc R . .
H37C H 0.8910 0.4207 0.4669 0.041 Uiso 1 1 calc R . .
C16 C 1.4872(3) 0.6824(3) 0.28860(19) 0.0334(7) Uani 1 1 d . . .
H16 H 1.5730 0.6931 0.2682 0.040 Uiso 1 1 calc R . .
C10 C 1.4381(3) 0.2873(3) 0.47299(18) 0.0279(7) Uani 1 1 d . . .
H10 H 1.4945 0.3132 0.5269 0.034 Uiso 1 1 calc R . .
C17 C 1.4352(3) 0.7831(3) 0.31511(19) 0.0348(8) Uani 1 1 d . . .
H17 H 1.4849 0.8630 0.3130 0.042 Uiso 1 1 calc R . .
C15 C 1.4148(3) 0.5650(3) 0.29159(18) 0.0268(7) Uani 1 1 d . . .
H15 H 1.4523 0.4965 0.2740 0.032 Uiso 1 1 calc R . .
C36 C 0.8645(3) 0.4986(3) 0.2769(2) 0.0291(7) Uani 1 1 d . . .
H36A H 0.9422 0.5479 0.3154 0.044 Uiso 1 1 calc R . .
H36B H 0.7892 0.5417 0.2757 0.044 Uiso 1 1 calc R . .
H36C H 0.8889 0.4847 0.2178 0.044 Uiso 1 1 calc R . .
C34 C 1.3493(3) 0.3682(3) 0.0062(2) 0.0344(7) Uani 1 1 d . . .
H34A H 1.3857 0.3776 -0.0494 0.052 Uiso 1 1 calc R . .
H34B H 1.3659 0.2920 0.0266 0.052 Uiso 1 1 calc R . .
H34C H 1.3935 0.4373 0.0497 0.052 Uiso 1 1 calc R . .
C18 C 1.3115(3) 0.7671(3) 0.34447(19) 0.0308(7) Uani 1 1 d . . .
H18 H 1.2757 0.8362 0.3633 0.037 Uiso 1 1 calc R . .
C35 C 1.1728(4) 0.4853(4) -0.0322(2) 0.0528(10) Uani 1 1 d . . .
H35A H 1.0767 0.4774 -0.0524 0.079 Uiso 1 1 calc R . .
H35B H 1.2260 0.5087 -0.0792 0.079 Uiso 1 1 calc R . .
H35C H 1.1991 0.5480 0.0185 0.079 Uiso 1 1 calc R . .
C23 C 0.6460(3) -0.0522(3) -0.08980(18) 0.0261(7) Uani 1 1 d . . .
H23 H 0.6330 -0.1295 -0.1240 0.031 Uiso 1 1 calc R . .
C24 C 0.5835(3) 0.0364(3) -0.11907(18) 0.0267(7) Uani 1 1 d . . .
H24 H 0.5269 0.0205 -0.1733 0.032 Uiso 1 1 calc R . .
C12 C 1.3480(3) 0.1334(3) 0.35293(19) 0.0259(7) Uani 1 1 d . . .
H12 H 1.3410 0.0532 0.3242 0.031 Uiso 1 1 calc R . .
C25 C 0.6031(3) 0.1488(3) -0.06937(19) 0.0292(7) Uani 1 1 d . . .
H25 H 0.5604 0.2107 -0.0897 0.035 Uiso 1 1 calc R . .
C11 C 1.4263(3) 0.1698(3) 0.43237(19) 0.0273(7) Uani 1 1 d . . .
H11 H 1.4721 0.1143 0.4592 0.033 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
Sb1 N1 2.0379(19) . ?
Sb1 Br2 2.5428(4) . ?
Sb1 Br1 2.5460(4) . ?
Si1 N1 1.772(2) . ?
Si1 C37 1.850(3) . ?
Si1 C36 1.859(3) . ?
Si1 C38 1.867(3) . ?
N1 C1 1.446(3) . ?
C2 C3 1.379(4) . ?
C2 C1 1.416(4) . ?
C2 C7 1.532(3) . ?
C27 C28 1.386(4) . ?
C27 C32 1.395(4) . ?
C27 C20 1.528(3) . ?
C32 C31 1.392(4) . ?
C22 C21 1.380(4) . ?
C22 C23 1.393(4) . ?
C1 C6 1.413(3) . ?
C5 C4 1.383(4) . ?
C5 C6 1.390(4) . ?
C20 C6 1.522(4) . ?
C20 C21 1.533(3) . ?
C14 C19 1.394(4) . ?
C14 C15 1.396(4) . ?
C14 C7 1.517(4) . ?
C4 C3 1.393(4) . ?
C4 C33 1.517(4) . ?
C31 C30 1.374(4) . ?
C7 C8 1.538(3) . ?
C28 C29 1.393(4) . ?
C29 C30 1.381(4) . ?
C33 C35 1.511(4) . ?
C33 C34 1.521(4) . ?
C21 C26 1.398(4) . ?
C26 C25 1.389(4) . ?
C8 C13 1.377(4) . ?
C8 C9 1.404(3) . ?
C13 C12 1.401(4) . ?
C19 C18 1.389(4) . ?
C9 C10 1.380(4) . ?
C16 C17 1.381(4) . ?
C16 C15 1.393(4) . ?
C10 C11 1.382(4) . ?
C17 C18 1.369(5) . ?
C23 C24 1.368(4) . ?
C24 C25 1.381(4) . ?
C12 C11 1.376(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
N1 Sb1 Br2 97.81(6) . . ?
N1 Sb1 Br1 101.09(6) . . ?
Br2 Sb1 Br1 91.420(13) . . ?
N1 Si1 C37 112.00(11) . . ?
N1 Si1 C36 108.78(12) . . ?
C37 Si1 C36 106.99(14) . . ?
N1 Si1 C38 112.39(11) . . ?
C37 Si1 C38 109.08(14) . . ?
C36 Si1 C38 107.35(13) . . ?
C1 N1 Si1 115.99(15) . . ?
C1 N1 Sb1 116.14(14) . . ?
Si1 N1 Sb1 127.63(12) . . ?
C3 C2 C1 119.3(2) . . ?
C3 C2 C7 119.8(2) . . ?
C1 C2 C7 120.5(2) . . ?
C28 C27 C32 118.3(2) . . ?
C28 C27 C20 120.1(2) . . ?
C32 C27 C20 121.5(2) . . ?
C31 C32 C27 120.7(3) . . ?
C21 C22 C23 121.0(2) . . ?
C6 C1 C2 118.4(2) . . ?
C6 C1 N1 121.2(2) . . ?
C2 C1 N1 120.4(2) . . ?
C4 C5 C6 122.6(2) . . ?
C6 C20 C27 109.3(2) . . ?
C6 C20 C21 113.6(2) . . ?
C27 C20 C21 113.4(2) . . ?
C19 C14 C15 117.6(3) . . ?
C19 C14 C7 120.2(3) . . ?
C15 C14 C7 122.2(2) . . ?
C5 C4 C3 116.9(2) . . ?
C5 C4 C33 122.3(2) . . ?
C3 C4 C33 120.8(2) . . ?
C30 C31 C32 120.1(3) . . ?
C5 C6 C1 119.6(2) . . ?
C5 C6 C20 120.2(2) . . ?
C1 C6 C20 119.7(2) . . ?
C14 C7 C2 112.8(2) . . ?
C14 C7 C8 112.4(2) . . ?
C2 C7 C8 110.1(2) . . ?
C27 C28 C29 120.9(3) . . ?
C2 C3 C4 123.1(2) . . ?
C30 C29 C28 119.9(3) . . ?
C31 C30 C29 120.0(2) . . ?
C35 C33 C4 110.8(2) . . ?
C35 C33 C34 109.6(3) . . ?
C4 C33 C34 113.0(2) . . ?
C22 C21 C26 118.2(2) . . ?
C22 C21 C20 122.9(2) . . ?
C26 C21 C20 118.9(2) . . ?
C25 C26 C21 120.5(3) . . ?
C13 C8 C9 118.2(2) . . ?
C13 C8 C7 123.2(2) . . ?
C9 C8 C7 118.5(2) . . ?
C8 C13 C12 121.1(2) . . ?
C18 C19 C14 121.2(3) . . ?
C10 C9 C8 120.7(3) . . ?
C17 C16 C15 120.4(3) . . ?
C9 C10 C11 120.4(2) . . ?
C18 C17 C16 119.6(3) . . ?
C16 C15 C14 120.8(3) . . ?
C17 C18 C19 120.4(3) . . ?
C24 C23 C22 120.3(3) . . ?
C23 C24 C25 119.6(2) . . ?
C11 C12 C13 119.7(3) . . ?
C24 C25 C26 120.3(3) . . ?
C12 C11 C10 119.8(2) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.50
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.868
_refine_diff_density_min         -0.410
_refine_diff_density_rms         0.097
####################################################################### 
# 
# 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_compound1d
_database_code_depnum_ccdc_archive 'CCDC 1051443'
_audit_update_record             
;
2015-02-27 deposited with the CCDC.
2015-03-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C44 H52 Br2 N Sb Si'
_chemical_formula_weight         904.53

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'
Si Si 0.0817 0.0704 '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'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   10.104(2)
_cell_length_b                   17.041(3)
_cell_length_c                   23.615(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 101.92(3)
_cell_angle_gamma                90.00
_cell_volume                     3978.4(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.510
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1832
_exptl_absorpt_coefficient_mu    2.764
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.680
_exptl_absorpt_correction_T_max  0.769
_exptl_absorpt_process_details   'Sortav (Blessing)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Apex X8'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            27969
_diffrn_reflns_av_R_equivalents  0.0921
_diffrn_reflns_av_sigmaI/netI    0.0660
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         2.97
_diffrn_reflns_theta_max         25.50
_reflns_number_total             7298
_reflns_number_gt                6793
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0557P)²+6.1111P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7298
_refine_ls_number_parameters     450
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0436
_refine_ls_R_factor_gt           0.0414
_refine_ls_wR_factor_ref         0.1091
_refine_ls_wR_factor_gt          0.1077
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_restrained_S_all      1.052
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Sb1 Sb 0.37223(2) 0.713847(12) 0.115231(9) 0.01390(9) Uani 1 1 d . . .
Br1 Br 0.35931(4) 0.62340(2) 0.199311(15) 0.02396(11) Uani 1 1 d . . .
Si1 Si 0.70112(9) 0.64740(5) 0.10822(4) 0.01296(18) Uani 1 1 d . . .
N1 N 0.5754(3) 0.71931(15) 0.11537(12) 0.0119(5) Uani 1 1 d . . .
C1 C 0.6213(3) 0.80036(18) 0.11933(13) 0.0107(6) Uani 1 1 d . . .
Br2 Br 0.28853(4) 0.60223(2) 0.045124(15) 0.02255(11) Uani 1 1 d . . .
C2 C 0.6197(3) 0.84485(19) 0.06878(13) 0.0113(6) Uani 1 1 d . . .
C3 C 0.6853(3) 0.91774(19) 0.07282(13) 0.0114(6) Uani 1 1 d . . .
H3 H 0.6856 0.9468 0.0385 0.014 Uiso 1 1 calc R . .
C4 C 0.7497(3) 0.94852(19) 0.12568(14) 0.0128(6) Uani 1 1 d . . .
C5 C 0.7383(3) 0.90798(19) 0.17530(13) 0.0115(6) Uani 1 1 d . . .
H5 H 0.7757 0.9306 0.2119 0.014 Uiso 1 1 calc R . .
C6 C 0.6744(3) 0.83554(19) 0.17374(13) 0.0112(6) Uani 1 1 d . . .
C7 C 0.6538(3) 0.79831(18) 0.23036(14) 0.0118(6) Uani 1 1 d . . .
H7 H 0.6619 0.7402 0.2260 0.014 Uiso 1 1 calc R . .
C8 C 0.5115(3) 0.81428(19) 0.24064(14) 0.0137(6) Uani 1 1 d . . .
C9 C 0.4171(4) 0.8602(2) 0.20380(15) 0.0179(7) Uani 1 1 d . . .
H9 H 0.4423 0.8858 0.1719 0.021 Uiso 1 1 calc R . .
C10 C 0.2858(4) 0.8689(2) 0.21307(17) 0.0255(8) Uani 1 1 d . . .
H10 H 0.2222 0.8998 0.1871 0.031 Uiso 1 1 calc R . .
C11 C 0.2475(4) 0.8334(2) 0.25951(18) 0.0280(8) Uani 1 1 d . . .
H11 H 0.1578 0.8389 0.2654 0.034 Uiso 1 1 calc R . .
C12 C 0.3422(4) 0.7891(2) 0.29787(18) 0.0268(8) Uani 1 1 d . . .
H12 H 0.3172 0.7653 0.3305 0.032 Uiso 1 1 calc R . .
C13 C 0.4735(4) 0.7794(2) 0.28867(16) 0.0200(7) Uani 1 1 d . . .
H13 H 0.5371 0.7490 0.3150 0.024 Uiso 1 1 calc R . .
C14 C 0.7619(3) 0.8227(2) 0.28264(13) 0.0148(6) Uani 1 1 d . . .
C15 C 0.8783(4) 0.7786(2) 0.29941(15) 0.0203(7) Uani 1 1 d . . .
H15 H 0.8893 0.7317 0.2791 0.024 Uiso 1 1 calc R . .
C16 C 0.9802(4) 0.8022(3) 0.34594(16) 0.0273(8) Uani 1 1 d . . .
H16 H 1.0599 0.7716 0.3570 0.033 Uiso 1 1 calc R . .
C17 C 0.9642(4) 0.8702(3) 0.37571(16) 0.0314(10) Uani 1 1 d . . .
H17 H 1.0331 0.8863 0.4073 0.038 Uiso 1 1 calc R . .
C18 C 0.8486(4) 0.9147(2) 0.35966(16) 0.0273(8) Uani 1 1 d . . .
H18 H 0.8382 0.9616 0.3799 0.033 Uiso 1 1 calc R . .
C19 C 0.7474(4) 0.8907(2) 0.31381(15) 0.0207(7) Uani 1 1 d . . .
H19 H 0.6671 0.9210 0.3035 0.025 Uiso 1 1 calc R . .
C20 C 0.5358(3) 0.81898(18) 0.01034(13) 0.0116(6) Uani 1 1 d . . .
H20 H 0.5423 0.7605 0.0091 0.014 Uiso 1 1 calc R . .
C21 C 0.3872(3) 0.83853(19) 0.00827(13) 0.0133(6) Uani 1 1 d . . .
C22 C 0.2856(4) 0.7888(2) -0.02079(15) 0.0177(7) Uani 1 1 d . . .
H22 H 0.3088 0.7447 -0.0413 0.021 Uiso 1 1 calc R . .
C23 C 0.1498(4) 0.8036(2) -0.01981(15) 0.0218(7) Uani 1 1 d . . .
H23 H 0.0815 0.7688 -0.0389 0.026 Uiso 1 1 calc R . .
C24 C 0.1146(4) 0.8690(2) 0.00904(16) 0.0227(8) Uani 1 1 d . . .
H24 H 0.0226 0.8785 0.0103 0.027 Uiso 1 1 calc R . .
C25 C 0.2141(4) 0.9201(2) 0.03596(15) 0.0215(7) Uani 1 1 d . . .
H25 H 0.1901 0.9658 0.0546 0.026 Uiso 1 1 calc R . .
C26 C 0.3489(3) 0.90500(19) 0.03589(14) 0.0152(6) Uani 1 1 d . . .
H26 H 0.4164 0.9403 0.0549 0.018 Uiso 1 1 calc R . .
C27 C 0.5879(3) 0.84991(18) -0.04174(13) 0.0119(6) Uani 1 1 d . . .
C28 C 0.5098(3) 0.8960(2) -0.08417(15) 0.0179(7) Uani 1 1 d . . .
H28 H 0.4213 0.9107 -0.0805 0.021 Uiso 1 1 calc R . .
C29 C 0.5588(4) 0.9212(2) -0.13226(15) 0.0218(7) Uani 1 1 d . . .
H29 H 0.5037 0.9532 -0.1607 0.026 Uiso 1 1 calc R . .
C30 C 0.6858(4) 0.9000(2) -0.13874(15) 0.0207(7) Uani 1 1 d . . .
H30 H 0.7186 0.9163 -0.1718 0.025 Uiso 1 1 calc R . .
C31 C 0.7654(4) 0.8545(2) -0.09630(16) 0.0218(7) Uani 1 1 d . . .
H31 H 0.8539 0.8401 -0.1002 0.026 Uiso 1 1 calc R . .
C32 C 0.7181(3) 0.8299(2) -0.04869(16) 0.0200(7) Uani 1 1 d . . .
H32 H 0.7746 0.7989 -0.0201 0.024 Uiso 1 1 calc R . .
C33 C 0.8365(3) 1.02167(19) 0.12815(14) 0.0158(7) Uani 1 1 d . . .
H33 H 0.8066 1.0510 0.0910 0.019 Uiso 1 1 calc R . .
C34 C 0.9829(4) 0.9961(3) 0.1321(3) 0.0531(15) Uani 1 1 d . . .
H34A H 1.0397 1.0426 0.1311 0.080 Uiso 1 1 calc R . .
H34B H 0.9884 0.9619 0.0993 0.080 Uiso 1 1 calc R . .
H34C H 1.0148 0.9676 0.1683 0.080 Uiso 1 1 calc R . .
C35 C 0.8281(4) 1.0772(2) 0.17768(16) 0.0276(8) Uani 1 1 d . . .
H35A H 0.7339 1.0934 0.1750 0.041 Uiso 1 1 calc R . .
H35B H 0.8841 1.1235 0.1753 0.041 Uiso 1 1 calc R . .
H35C H 0.8608 1.0504 0.2146 0.041 Uiso 1 1 calc R . .
C36 C 0.8700(3) 0.6855(2) 0.15033(15) 0.0205(7) Uani 1 1 d . . .
H36 H 0.8505 0.7098 0.1863 0.025 Uiso 1 1 calc R . .
C37 C 0.9383(4) 0.7504(2) 0.12085(17) 0.0235(8) Uani 1 1 d . . .
H37A H 1.0215 0.7675 0.1471 0.035 Uiso 1 1 calc R . .
H37B H 0.8765 0.7950 0.1116 0.035 Uiso 1 1 calc R . .
H37C H 0.9603 0.7298 0.0852 0.035 Uiso 1 1 calc R . .
C38 C 0.9750(4) 0.6205(3) 0.17102(19) 0.0324(9) Uani 1 1 d . . .
H38A H 1.0035 0.5972 0.1375 0.049 Uiso 1 1 calc R . .
H38B H 0.9346 0.5799 0.1915 0.049 Uiso 1 1 calc R . .
H38C H 1.0538 0.6431 0.1972 0.049 Uiso 1 1 calc R . .
C39 C 0.7183(3) 0.6374(2) 0.03024(15) 0.0173(7) Uani 1 1 d . . .
H39 H 0.7336 0.6920 0.0174 0.021 Uiso 1 1 calc R . .
C40 C 0.8450(4) 0.5907(2) 0.02286(16) 0.0235(8) Uani 1 1 d . . .
H40A H 0.8361 0.5360 0.0343 0.035 Uiso 1 1 calc R . .
H40B H 0.9257 0.6139 0.0473 0.035 Uiso 1 1 calc R . .
H40C H 0.8534 0.5927 -0.0177 0.035 Uiso 1 1 calc R . .
C41 C 0.5960(4) 0.6074(2) -0.01356(15) 0.0212(7) Uani 1 1 d . . .
H41A H 0.6136 0.6121 -0.0527 0.032 Uiso 1 1 calc R . .
H41B H 0.5162 0.6386 -0.0106 0.032 Uiso 1 1 calc R . .
H41C H 0.5798 0.5522 -0.0055 0.032 Uiso 1 1 calc R . .
C42 C 0.6458(4) 0.55398(19) 0.14009(15) 0.0185(7) Uani 1 1 d . . .
H42 H 0.5450 0.5527 0.1279 0.022 Uiso 1 1 calc R . .
C43 C 0.6762(4) 0.5535(2) 0.20628(16) 0.0252(8) Uani 1 1 d . . .
H43A H 0.6216 0.5130 0.2200 0.038 Uiso 1 1 calc R . .
H43B H 0.6541 0.6049 0.2205 0.038 Uiso 1 1 calc R . .
H43C H 0.7724 0.5424 0.2208 0.038 Uiso 1 1 calc R . .
C44 C 0.6960(4) 0.4777(2) 0.11699(17) 0.0274(8) Uani 1 1 d . . .
H44A H 0.7945 0.4742 0.1295 0.041 Uiso 1 1 calc R . .
H44B H 0.6716 0.4775 0.0746 0.041 Uiso 1 1 calc R . .
H44C H 0.6539 0.4326 0.1321 0.041 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
Sb1 N1 2.055(3) . ?
Sb1 Br1 2.5381(5) . ?
Sb1 Br2 2.5487(6) . ?
Si1 N1 1.797(3) . ?
Si1 C39 1.893(3) . ?
Si1 C42 1.894(4) . ?
Si1 C36 1.903(4) . ?
N1 C1 1.454(4) . ?
C1 C2 1.411(4) . ?
C1 C6 1.419(4) . ?
C2 C3 1.402(4) . ?
C2 C20 1.528(4) . ?
C3 C4 1.386(4) . ?
C4 C5 1.385(4) . ?
C4 C33 1.518(4) . ?
C5 C6 1.390(4) . ?
C6 C7 1.532(4) . ?
C7 C14 1.528(4) . ?
C7 C8 1.531(4) . ?
C8 C9 1.391(5) . ?
C8 C13 1.403(5) . ?
C9 C10 1.397(5) . ?
C10 C11 1.376(6) . ?
C11 C12 1.396(6) . ?
C12 C13 1.397(5) . ?
C14 C15 1.383(5) . ?
C14 C19 1.397(5) . ?
C15 C16 1.401(5) . ?
C16 C17 1.381(6) . ?
C17 C18 1.378(6) . ?
C18 C19 1.388(5) . ?
C20 C27 1.528(4) . ?
C20 C21 1.528(4) . ?
C21 C22 1.397(5) . ?
C21 C26 1.401(5) . ?
C22 C23 1.400(5) . ?
C23 C24 1.390(6) . ?
C24 C25 1.383(5) . ?
C25 C26 1.387(5) . ?
C27 C28 1.384(5) . ?
C27 C32 1.401(5) . ?
C28 C29 1.397(5) . ?
C29 C30 1.372(5) . ?
C30 C31 1.385(5) . ?
C31 C32 1.375(5) . ?
C33 C35 1.520(5) . ?
C33 C34 1.527(5) . ?
C36 C38 1.542(5) . ?
C36 C37 1.543(5) . ?
C39 C41 1.526(5) . ?
C39 C40 1.547(5) . ?
C42 C43 1.530(5) . ?
C42 C44 1.536(5) . ?

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
N1 Sb1 Br1 103.83(8) . . ?
N1 Sb1 Br2 103.43(8) . . ?
Br1 Sb1 Br2 89.49(2) . . ?
N1 Si1 C39 111.18(14) . . ?
N1 Si1 C42 105.29(14) . . ?
C39 Si1 C42 113.87(15) . . ?
N1 Si1 C36 107.03(14) . . ?
C39 Si1 C36 106.67(16) . . ?
C42 Si1 C36 112.67(16) . . ?
C1 N1 Si1 115.6(2) . . ?
C1 N1 Sb1 110.38(19) . . ?
Si1 N1 Sb1 133.95(15) . . ?
C2 C1 C6 118.4(3) . . ?
C2 C1 N1 120.5(3) . . ?
C6 C1 N1 121.0(3) . . ?
C3 C2 C1 119.7(3) . . ?
C3 C2 C20 118.9(3) . . ?
C1 C2 C20 121.1(3) . . ?
C4 C3 C2 121.6(3) . . ?
C5 C4 C3 117.9(3) . . ?
C5 C4 C33 121.7(3) . . ?
C3 C4 C33 120.4(3) . . ?
C4 C5 C6 122.7(3) . . ?
C5 C6 C1 119.1(3) . . ?
C5 C6 C7 119.4(3) . . ?
C1 C6 C7 121.4(3) . . ?
C14 C7 C8 111.2(3) . . ?
C14 C7 C6 112.9(3) . . ?
C8 C7 C6 111.5(3) . . ?
C9 C8 C13 118.5(3) . . ?
C9 C8 C7 123.1(3) . . ?
C13 C8 C7 118.4(3) . . ?
C8 C9 C10 120.9(3) . . ?
C11 C10 C9 120.7(4) . . ?
C10 C11 C12 119.2(3) . . ?
C11 C12 C13 120.6(4) . . ?
C12 C13 C8 120.2(4) . . ?
C15 C14 C19 118.4(3) . . ?
C15 C14 C7 120.5(3) . . ?
C19 C14 C7 121.1(3) . . ?
C14 C15 C16 120.8(4) . . ?
C17 C16 C15 119.8(4) . . ?
C18 C17 C16 120.1(3) . . ?
C17 C18 C19 119.9(4) . . ?
C18 C19 C14 120.9(4) . . ?
C27 C20 C2 114.1(3) . . ?
C27 C20 C21 113.5(3) . . ?
C2 C20 C21 108.9(2) . . ?
C22 C21 C26 118.2(3) . . ?
C22 C21 C20 120.1(3) . . ?
C26 C21 C20 121.7(3) . . ?
C21 C22 C23 120.4(3) . . ?
C24 C23 C22 120.2(3) . . ?
C25 C24 C23 119.7(3) . . ?
C24 C25 C26 120.2(3) . . ?
C25 C26 C21 121.1(3) . . ?
C28 C27 C32 117.5(3) . . ?
C28 C27 C20 122.6(3) . . ?
C32 C27 C20 119.9(3) . . ?
C27 C28 C29 121.2(3) . . ?
C30 C29 C28 120.4(3) . . ?
C29 C30 C31 118.9(3) . . ?
C32 C31 C30 121.0(3) . . ?
C31 C32 C27 121.0(3) . . ?
C4 C33 C35 114.6(3) . . ?
C4 C33 C34 108.3(3) . . ?
C35 C33 C34 109.8(4) . . ?
C38 C36 C37 108.4(3) . . ?
C38 C36 Si1 113.9(3) . . ?
C37 C36 Si1 116.4(2) . . ?
C41 C39 C40 108.9(3) . . ?
C41 C39 Si1 117.8(2) . . ?
C40 C39 Si1 113.6(2) . . ?
C43 C42 C44 110.3(3) . . ?
C43 C42 Si1 113.4(2) . . ?
C44 C42 Si1 115.1(2) . . ?

_diffrn_measured_fraction_theta_max 0.986
_diffrn_reflns_theta_full        25.50
_diffrn_measured_fraction_theta_full 0.986
_refine_diff_density_max         0.643
_refine_diff_density_min         -1.671
_refine_diff_density_rms         0.137
####################################################################### 
# 
# 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_compound1e
_database_code_depnum_ccdc_archive 'CCDC 1051444'
_audit_update_record             
;
2015-02-27 deposited with the CCDC.
2015-03-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H40 Bi Br2 N Si'
_chemical_formula_weight         907.60

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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Bi Bi -4.1077 10.2566 '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'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.1646(5)
_cell_length_b                   11.2590(6)
_cell_length_c                   15.5011(7)
_cell_angle_alpha                95.931(4)
_cell_angle_beta                 96.150(4)
_cell_angle_gamma                100.498(4)
_cell_volume                     1720.51(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.752
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             884
_exptl_absorpt_coefficient_mu    7.508
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.252
_exptl_absorpt_correction_T_max  0.398
_exptl_absorpt_process_details   'Sortav (Blessing)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Apex X8'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            15473
_diffrn_reflns_av_R_equivalents  0.0419
_diffrn_reflns_av_sigmaI/netI    0.0536
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.03
_diffrn_reflns_theta_max         25.50
_reflns_number_total             6404
_reflns_number_gt                5758
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0276P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6404
_refine_ls_number_parameters     393
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0373
_refine_ls_R_factor_gt           0.0307
_refine_ls_wR_factor_ref         0.0661
_refine_ls_wR_factor_gt          0.0629
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_restrained_S_all      1.022
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Bi1 Bi 0.977665(14) 0.113409(15) 0.363843(10) 0.01701(6) Uani 1 1 d . . .
Si1 Si 0.81088(11) 0.35004(11) 0.31732(7) 0.0163(3) Uani 1 1 d . . .
C27 C 0.8825(4) 0.0012(4) 0.1602(3) 0.0142(9) Uani 1 1 d . . .
C26 C 0.7312(4) -0.0299(4) -0.0124(3) 0.0190(9) Uani 1 1 d . . .
H26 H 0.7768 -0.0904 0.0077 0.023 Uiso 1 1 calc R . .
C23 C 0.5991(4) 0.1437(5) -0.0742(3) 0.0269(11) Uani 1 1 d . . .
H23 H 0.5545 0.2042 -0.0953 0.032 Uiso 1 1 calc R . .
C21 C 0.7469(4) 0.0810(4) 0.0383(3) 0.0154(9) Uani 1 1 d . . .
C2 C 0.9471(4) 0.2192(4) 0.1362(3) 0.0136(9) Uani 1 1 d . . .
C4 C 1.1284(4) 0.3345(4) 0.0703(3) 0.0161(9) Uani 1 1 d . . .
C5 C 1.1819(4) 0.3927(4) 0.1533(3) 0.0158(9) Uani 1 1 d . . .
H5 H 1.2624 0.4527 0.1593 0.019 Uiso 1 1 calc R . .
C1 C 1.0009(4) 0.2822(4) 0.2200(2) 0.0118(8) Uani 1 1 d . . .
C8 C 1.2852(4) 0.5478(4) 0.3192(3) 0.0173(9) Uani 1 1 d . . .
C3 C 1.0111(4) 0.2473(4) 0.0642(3) 0.0144(9) Uani 1 1 d . . .
H3 H 0.9731 0.2049 0.0084 0.017 Uiso 1 1 calc R . .
C25 C 0.6487(4) -0.0548(4) -0.0933(3) 0.0225(10) Uani 1 1 d . . .
H25 H 0.6382 -0.1318 -0.1274 0.027 Uiso 1 1 calc R . .
C22 C 0.6801(4) 0.1680(4) 0.0062(3) 0.0215(10) Uani 1 1 d . . .
H22 H 0.6899 0.2453 0.0399 0.026 Uiso 1 1 calc R . .
C24 C 0.5838(4) 0.0319(5) -0.1230(3) 0.0256(11) Uani 1 1 d . . .
H24 H 0.5278 0.0148 -0.1776 0.031 Uiso 1 1 calc R . .
C12 C 1.4843(5) 0.6812(5) 0.2877(3) 0.0368(13) Uani 1 1 d . . .
H12 H 1.5692 0.6916 0.2663 0.044 Uiso 1 1 calc R . .
C9 C 1.2368(4) 0.6507(4) 0.3466(3) 0.0208(10) Uani 1 1 d . . .
H9 H 1.1508 0.6415 0.3664 0.025 Uiso 1 1 calc R . .
C34 C 1.3476(4) 0.3663(5) 0.0036(3) 0.0359(13) Uani 1 1 d . . .
H34A H 1.3924 0.4298 0.0510 0.054 Uiso 1 1 calc R . .
H34B H 1.3848 0.3827 -0.0507 0.054 Uiso 1 1 calc R . .
H34C H 1.3626 0.2868 0.0182 0.054 Uiso 1 1 calc R . .
C13 C 1.4122(4) 0.5645(5) 0.2908(3) 0.0264(11) Uani 1 1 d . . .
H13 H 1.4498 0.4958 0.2735 0.032 Uiso 1 1 calc R . .
C33 C 1.1954(4) 0.3657(4) -0.0088(3) 0.0251(11) Uani 1 1 d . . .
H33 H 1.1524 0.3031 -0.0592 0.030 Uiso 1 1 calc R . .
C7 C 1.1996(4) 0.4219(4) 0.3182(3) 0.0150(9) Uani 1 1 d . . .
H7 H 1.1297 0.4312 0.3578 0.018 Uiso 1 1 calc R . .
N1 N 0.9327(3) 0.2616(3) 0.2957(2) 0.0133(7) Uani 1 1 d . . .
C20 C 0.8301(4) 0.1100(4) 0.1284(3) 0.0138(9) Uani 1 1 d . . .
H20 H 0.7678 0.1328 0.1703 0.017 Uiso 1 1 calc R . .
C6 C 1.1238(4) 0.3676(4) 0.2279(3) 0.0135(9) Uani 1 1 d . . .
C38 C 0.6389(4) 0.2784(4) 0.2605(3) 0.0258(11) Uani 1 1 d . . .
H38A H 0.6365 0.2830 0.1976 0.039 Uiso 1 1 calc R . .
H38B H 0.5722 0.3217 0.2835 0.039 Uiso 1 1 calc R . .
H38C H 0.6177 0.1929 0.2706 0.039 Uiso 1 1 calc R . .
C36 C 0.8606(4) 0.5009(4) 0.2781(3) 0.0286(11) Uani 1 1 d . . .
H36A H 0.9353 0.5509 0.3188 0.043 Uiso 1 1 calc R . .
H36B H 0.7834 0.5420 0.2750 0.043 Uiso 1 1 calc R . .
H36C H 0.8891 0.4891 0.2199 0.043 Uiso 1 1 calc R . .
C37 C 0.8032(4) 0.3797(5) 0.4361(3) 0.0269(11) Uani 1 1 d . . .
H37A H 0.7764 0.3023 0.4592 0.040 Uiso 1 1 calc R . .
H37B H 0.7370 0.4312 0.4462 0.040 Uiso 1 1 calc R . .
H37C H 0.8922 0.4213 0.4657 0.040 Uiso 1 1 calc R . .
C28 C 1.0128(4) -0.0153(4) 0.1509(3) 0.0173(9) Uani 1 1 d . . .
H28 H 1.0689 0.0396 0.1213 0.021 Uiso 1 1 calc R . .
C32 C 0.8029(4) -0.0811(4) 0.2032(3) 0.0203(10) Uani 1 1 d . . .
H32 H 0.7129 -0.0725 0.2089 0.024 Uiso 1 1 calc R . .
C14 C 1.2805(4) 0.3318(4) 0.3546(3) 0.0167(9) Uani 1 1 d . . .
C29 C 1.0621(4) -0.1110(4) 0.1841(3) 0.0207(10) Uani 1 1 d . . .
H29 H 1.1504 -0.1222 0.1756 0.025 Uiso 1 1 calc R . .
C19 C 1.3635(4) 0.3670(4) 0.4348(3) 0.0218(10) Uani 1 1 d . . .
H19 H 1.3723 0.4474 0.4635 0.026 Uiso 1 1 calc R . .
C31 C 0.8518(4) -0.1756(4) 0.2380(3) 0.0239(10) Uani 1 1 d . . .
H31 H 0.7959 -0.2306 0.2676 0.029 Uiso 1 1 calc R . .
C30 C 0.9834(4) -0.1896(4) 0.2293(3) 0.0238(10) Uani 1 1 d . . .
H30 H 1.0186 -0.2528 0.2542 0.029 Uiso 1 1 calc R . .
C15 C 1.2723(4) 0.2142(4) 0.3145(3) 0.0190(9) Uani 1 1 d . . .
H15 H 1.2191 0.1884 0.2592 0.023 Uiso 1 1 calc R . .
C11 C 1.4338(5) 0.7810(5) 0.3153(3) 0.0394(14) Uani 1 1 d . . .
H11 H 1.4839 0.8604 0.3135 0.047 Uiso 1 1 calc R . .
C10 C 1.3102(5) 0.7665(5) 0.3458(3) 0.0331(12) Uani 1 1 d . . .
H10 H 1.2757 0.8357 0.3662 0.040 Uiso 1 1 calc R . .
C35 C 1.1746(6) 0.4889(6) -0.0318(4) 0.0541(17) Uani 1 1 d . . .
H35A H 1.0791 0.4845 -0.0525 0.081 Uiso 1 1 calc R . .
H35B H 1.2292 0.5125 -0.0780 0.081 Uiso 1 1 calc R . .
H35C H 1.2021 0.5495 0.0201 0.081 Uiso 1 1 calc R . .
C16 C 1.3408(4) 0.1335(4) 0.3539(3) 0.0239(10) Uani 1 1 d . . .
H16 H 1.3326 0.0529 0.3259 0.029 Uiso 1 1 calc R . .
C17 C 1.4202(4) 0.1695(4) 0.4332(3) 0.0261(11) Uani 1 1 d . . .
H17 H 1.4661 0.1142 0.4605 0.031 Uiso 1 1 calc R . .
C18 C 1.4321(4) 0.2873(5) 0.4724(3) 0.0275(11) Uani 1 1 d . . .
H18 H 1.4888 0.3137 0.5264 0.033 Uiso 1 1 calc R . .
Br1 Br 0.73423(4) 0.04306(4) 0.40811(3) 0.02965(12) Uani 1 1 d . . .
Br2 Br 1.06372(5) 0.22687(5) 0.52295(3) 0.03385(13) Uani 1 1 d . . .


_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
Bi1 N1 2.155(3) . ?
Bi1 Br2 2.6380(5) . ?
Bi1 Br1 2.6425(5) . ?
Si1 N1 1.762(3) . ?
Si1 C37 1.849(4) . ?
Si1 C36 1.864(5) . ?
Si1 C38 1.869(4) . ?
C27 C32 1.388(6) . ?
C27 C28 1.390(5) . ?
C27 C20 1.528(6) . ?
C26 C21 1.378(6) . ?
C26 C25 1.405(6) . ?
C23 C24 1.375(6) . ?
C23 C22 1.391(6) . ?
C21 C22 1.392(6) . ?
C21 C20 1.525(5) . ?
C2 C3 1.387(6) . ?
C2 C1 1.415(5) . ?
C2 C20 1.532(5) . ?
C4 C3 1.387(5) . ?
C4 C5 1.388(5) . ?
C4 C33 1.507(6) . ?
C5 C6 1.385(6) . ?
C1 C6 1.416(5) . ?
C1 N1 1.444(5) . ?
C8 C9 1.384(6) . ?
C8 C13 1.395(6) . ?
C8 C7 1.520(6) . ?
C25 C24 1.364(6) . ?
C12 C11 1.367(8) . ?
C12 C13 1.391(7) . ?
C9 C10 1.380(6) . ?
C34 C33 1.537(6) . ?
C33 C35 1.514(7) . ?
C7 C6 1.532(5) . ?
C7 C14 1.532(6) . ?
C28 C29 1.390(6) . ?
C32 C31 1.387(6) . ?
C14 C15 1.387(6) . ?
C14 C19 1.402(6) . ?
C29 C30 1.380(6) . ?
C19 C18 1.372(6) . ?
C31 C30 1.394(6) . ?
C15 C16 1.393(6) . ?
C11 C10 1.377(7) . ?
C16 C17 1.375(6) . ?
C17 C18 1.379(7) . ?

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
N1 Bi1 Br2 101.14(8) . . ?
N1 Bi1 Br1 96.85(8) . . ?
Br2 Bi1 Br1 90.666(16) . . ?
N1 Si1 C37 111.25(19) . . ?
N1 Si1 C36 108.80(18) . . ?
C37 Si1 C36 106.9(2) . . ?
N1 Si1 C38 112.61(18) . . ?
C37 Si1 C38 109.2(2) . . ?
C36 Si1 C38 107.8(2) . . ?
C32 C27 C28 118.0(4) . . ?
C32 C27 C20 120.6(3) . . ?
C28 C27 C20 121.4(4) . . ?
C21 C26 C25 120.8(4) . . ?
C24 C23 C22 119.7(4) . . ?
C26 C21 C22 118.0(4) . . ?
C26 C21 C20 122.7(4) . . ?
C22 C21 C20 119.2(4) . . ?
C3 C2 C1 119.6(3) . . ?
C3 C2 C20 120.7(3) . . ?
C1 C2 C20 119.2(3) . . ?
C3 C4 C5 116.8(4) . . ?
C3 C4 C33 122.2(4) . . ?
C5 C4 C33 121.0(4) . . ?
C6 C5 C4 123.2(4) . . ?
C2 C1 C6 118.2(3) . . ?
C2 C1 N1 121.4(3) . . ?
C6 C1 N1 120.4(3) . . ?
C9 C8 C13 117.7(4) . . ?
C9 C8 C7 120.3(4) . . ?
C13 C8 C7 122.0(4) . . ?
C2 C3 C4 122.8(4) . . ?
C24 C25 C26 119.9(4) . . ?
C23 C22 C21 121.1(4) . . ?
C25 C24 C23 120.4(4) . . ?
C11 C12 C13 120.5(5) . . ?
C10 C9 C8 121.8(4) . . ?
C12 C13 C8 120.4(5) . . ?
C4 C33 C35 110.8(4) . . ?
C4 C33 C34 113.0(4) . . ?
C35 C33 C34 108.6(4) . . ?
C8 C7 C6 113.4(3) . . ?
C8 C7 C14 112.8(3) . . ?
C6 C7 C14 109.8(3) . . ?
C1 N1 Si1 117.2(3) . . ?
C1 N1 Bi1 116.0(2) . . ?
Si1 N1 Bi1 126.52(17) . . ?
C21 C20 C27 113.5(3) . . ?
C21 C20 C2 113.9(3) . . ?
C27 C20 C2 109.6(3) . . ?
C5 C6 C1 119.3(3) . . ?
C5 C6 C7 119.9(3) . . ?
C1 C6 C7 120.6(3) . . ?
C29 C28 C27 121.0(4) . . ?
C31 C32 C27 121.5(4) . . ?
C15 C14 C19 117.5(4) . . ?
C15 C14 C7 123.6(3) . . ?
C19 C14 C7 118.8(4) . . ?
C30 C29 C28 120.4(4) . . ?
C18 C19 C14 121.0(4) . . ?
C32 C31 C30 119.7(4) . . ?
C29 C30 C31 119.4(4) . . ?
C14 C15 C16 121.0(4) . . ?
C12 C11 C10 120.0(5) . . ?
C11 C10 C9 119.6(5) . . ?
C17 C16 C15 120.5(4) . . ?
C16 C17 C18 118.9(4) . . ?
C19 C18 C17 121.1(4) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.50
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         2.252
_refine_diff_density_min         -1.188
_refine_diff_density_rms         0.144
####################################################################### 
# 
# 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_compound1f
_database_code_depnum_ccdc_archive 'CCDC 1051445'
_audit_update_record             
;
2015-02-27 deposited with the CCDC.
2015-03-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C44 H52 Bi Br2 N Si'
_chemical_formula_weight         991.76

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'
Si Si 0.0817 0.0704 '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'
Bi Bi -4.1077 10.2566 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   10.130(2)
_cell_length_b                   17.182(3)
_cell_length_c                   23.696(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 102.26(3)
_cell_angle_gamma                90.00
_cell_volume                     4030.3(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.634
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1960
_exptl_absorpt_coefficient_mu    6.418
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.625
_exptl_absorpt_correction_T_max  0.699
_exptl_absorpt_process_details   XDS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71080
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_source         'Australian Synchrotron'
_diffrn_radiation_monochromator  ?
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            27660
_diffrn_reflns_av_R_equivalents  0.0796
_diffrn_reflns_av_sigmaI/netI    0.0574
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         2.95
_diffrn_reflns_theta_max         25.25
_reflns_number_total             6842
_reflns_number_gt                5941
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Blu-Ice (McPhillips, 2002)'
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    X-Seed
_computing_publication_material  CifTAB

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
 the largest residual electron density peak (3.0 e/ ang.3) was located
 close to the Bi atom.
 The low value (94.0%) for completeness of data to theta = 25.25 deg. arises 
 from hardware constraints associated with the diffractometer used at the 
 Australian Synchrotron. 
 Its minimum crystal to detector distance is 72 mm and its
 goniometer only rotates about the phi axis.
 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0633P)²+17.5655P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6842
_refine_ls_number_parameters     450
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0556
_refine_ls_R_factor_gt           0.0480
_refine_ls_wR_factor_ref         0.1277
_refine_ls_wR_factor_gt          0.1237
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_restrained_S_all      1.085
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Bi1 Bi 0.36937(3) 0.215519(15) 0.116593(12) 0.02717(11) Uani 1 1 d . . .
Br1 Br 0.27836(8) 0.10099(5) 0.04417(4) 0.0380(2) Uani 1 1 d . . .
C40 C 0.9448(8) 0.2482(6) 0.1217(4) 0.043(2) Uani 1 1 d . . .
H40A H 1.0264 0.2663 0.1486 0.064 Uiso 1 1 calc R . .
H40B H 0.8823 0.2918 0.1111 0.064 Uiso 1 1 calc R . .
H40C H 0.9695 0.2271 0.0869 0.064 Uiso 1 1 calc R . .
Si1 Si 0.7058(2) 0.14861(11) 0.10894(8) 0.0250(4) Uani 1 1 d . . .
Br2 Br 0.35893(9) 0.12087(5) 0.20264(4) 0.0431(2) Uani 1 1 d . . .
C21 C 0.3917(6) 0.3370(4) 0.0099(3) 0.0211(13) Uani 1 1 d . . .
C22 C 0.2905(7) 0.2876(4) -0.0189(3) 0.0252(15) Uani 1 1 d . . .
H22 H 0.3137 0.2441 -0.0395 0.030 Uiso 1 1 calc R . .
C24 C 0.1194(7) 0.3663(5) 0.0108(3) 0.0344(18) Uani 1 1 d . . .
H24 H 0.0275 0.3761 0.0115 0.041 Uiso 1 1 calc R . .
C26 C 0.3539(7) 0.4030(4) 0.0378(3) 0.0221(14) Uani 1 1 d . . .
H26 H 0.4211 0.4384 0.0566 0.026 Uiso 1 1 calc R . .
C23 C 0.1545(7) 0.3013(5) -0.0176(3) 0.0342(18) Uani 1 1 d . . .
H23 H 0.0865 0.2662 -0.0362 0.041 Uiso 1 1 calc R . .
C25 C 0.2197(7) 0.4167(5) 0.0382(3) 0.0299(16) Uani 1 1 d . . .
H25 H 0.1957 0.4613 0.0576 0.036 Uiso 1 1 calc R . .
N1 N 0.5827(6) 0.2212(3) 0.1164(2) 0.0197(11) Uani 1 1 d . . .
C7 C 0.6617(7) 0.3004(4) 0.2302(3) 0.0207(13) Uani 1 1 d . . .
H7 H 0.6711 0.2428 0.2263 0.025 Uiso 1 1 calc R . .
C20 C 0.5404(6) 0.3186(4) 0.0112(3) 0.0195(13) Uani 1 1 d . . .
H20 H 0.5482 0.2606 0.0105 0.023 Uiso 1 1 calc R . .
C6 C 0.6826(6) 0.3368(4) 0.1742(3) 0.0182(13) Uani 1 1 d . . .
C1 C 0.6288(6) 0.3024(4) 0.1197(3) 0.0188(13) Uani 1 1 d . . .
C13 C 0.4787(8) 0.2794(4) 0.2866(3) 0.0325(17) Uani 1 1 d . . .
H13 H 0.5412 0.2482 0.3126 0.039 Uiso 1 1 calc R . .
C4 C 0.7563(6) 0.4502(4) 0.1252(3) 0.0202(13) Uani 1 1 d . . .
C27 C 0.5896(6) 0.3492(4) -0.0415(3) 0.0192(13) Uani 1 1 d . . .
C8 C 0.5185(7) 0.3154(4) 0.2393(3) 0.0215(14) Uani 1 1 d . . .
C3 C 0.6902(6) 0.4173(4) 0.0722(3) 0.0182(13) Uani 1 1 d . . .
H3 H 0.6898 0.4451 0.0375 0.022 Uiso 1 1 calc R . .
C5 C 0.7456(6) 0.4097(4) 0.1751(3) 0.0195(13) Uani 1 1 d . . .
H5 H 0.7829 0.4326 0.2115 0.023 Uiso 1 1 calc R . .
C2 C 0.6259(6) 0.3456(4) 0.0688(3) 0.0184(13) Uani 1 1 d . . .
C12 C 0.3484(9) 0.2895(5) 0.2950(4) 0.041(2) Uani 1 1 d . . .
H12 H 0.3227 0.2661 0.3274 0.049 Uiso 1 1 calc R . .
C11 C 0.2553(8) 0.3335(5) 0.2566(4) 0.039(2) Uani 1 1 d . . .
H11 H 0.1653 0.3382 0.2619 0.047 Uiso 1 1 calc R . .
C9 C 0.4254(7) 0.3610(4) 0.2029(3) 0.0254(14) Uani 1 1 d . . .
H9 H 0.4512 0.3869 0.1715 0.030 Uiso 1 1 calc R . .
C28 C 0.7168(7) 0.3279(5) -0.0503(3) 0.0324(17) Uani 1 1 d . . .
H28 H 0.7738 0.2964 -0.0224 0.039 Uiso 1 1 calc R . .
C10 C 0.2923(7) 0.3700(5) 0.2114(3) 0.0346(18) Uani 1 1 d . . .
H10 H 0.2291 0.4013 0.1857 0.042 Uiso 1 1 calc R . .
C15 C 0.8868(8) 0.2822(5) 0.2997(3) 0.0322(17) Uani 1 1 d . . .
H15 H 0.9003 0.2362 0.2794 0.039 Uiso 1 1 calc R . .
C14 C 0.7685(7) 0.3256(4) 0.2829(3) 0.0240(14) Uani 1 1 d . . .
C32 C 0.5113(7) 0.3972(4) -0.0822(3) 0.0267(15) Uani 1 1 d . . .
H32 H 0.4252 0.4140 -0.0772 0.032 Uiso 1 1 calc R . .
C30 C 0.6828(8) 0.3987(5) -0.1385(3) 0.0306(16) Uani 1 1 d . . .
H30 H 0.7142 0.4157 -0.1715 0.037 Uiso 1 1 calc R . .
C33 C 0.8405(7) 0.5225(4) 0.1272(3) 0.0246(14) Uani 1 1 d . . .
H33 H 0.8094 0.5510 0.0900 0.030 Uiso 1 1 calc R . .
C39 C 0.8770(7) 0.1848(5) 0.1506(3) 0.0321(17) Uani 1 1 d . . .
H39 H 0.8601 0.2083 0.1870 0.039 Uiso 1 1 calc R . .
C29 C 0.7614(8) 0.3515(5) -0.0984(4) 0.0362(18) Uani 1 1 d . . .
H29 H 0.8473 0.3349 -0.1038 0.043 Uiso 1 1 calc R . .
C19 C 0.7508(8) 0.3926(5) 0.3141(3) 0.0321(16) Uani 1 1 d . . .
H19 H 0.6698 0.4220 0.3038 0.039 Uiso 1 1 calc R . .
C37 C 0.5963(8) 0.1080(4) -0.0102(4) 0.0343(17) Uani 1 1 d . . .
H37A H 0.6028 0.1209 -0.0498 0.052 Uiso 1 1 calc R . .
H37B H 0.5163 0.1331 -0.0013 0.052 Uiso 1 1 calc R . .
H37C H 0.5890 0.0515 -0.0064 0.052 Uiso 1 1 calc R . .
C35 C 0.8320(9) 0.5775(5) 0.1758(4) 0.041(2) Uani 1 1 d . . .
H35A H 0.7370 0.5890 0.1753 0.061 Uiso 1 1 calc R . .
H35B H 0.8794 0.6259 0.1708 0.061 Uiso 1 1 calc R . .
H35C H 0.8740 0.5535 0.2127 0.061 Uiso 1 1 calc R . .
C34 C 0.9848(10) 0.4989(6) 0.1310(7) 0.077(4) Uani 1 1 d . . .
H34A H 1.0124 0.4623 0.1631 0.116 Uiso 1 1 calc R . .
H34B H 1.0427 0.5451 0.1376 0.116 Uiso 1 1 calc R . .
H34C H 0.9935 0.4738 0.0949 0.116 Uiso 1 1 calc R . .
C18 C 0.8526(9) 0.4162(5) 0.3605(3) 0.040(2) Uani 1 1 d . . .
H18 H 0.8419 0.4626 0.3809 0.048 Uiso 1 1 calc R . .
C38 C 0.8444(9) 0.0894(6) 0.0228(4) 0.044(2) Uani 1 1 d . . .
H38A H 0.8430 0.0379 0.0405 0.067 Uiso 1 1 calc R . .
H38B H 0.9272 0.1169 0.0412 0.067 Uiso 1 1 calc R . .
H38C H 0.8420 0.0833 -0.0186 0.067 Uiso 1 1 calc R . .
C36 C 0.7203(7) 0.1365(4) 0.0310(3) 0.0284(15) Uani 1 1 d . . .
H36 H 0.7357 0.1903 0.0176 0.034 Uiso 1 1 calc R . .
C31 C 0.5581(8) 0.4211(5) -0.1305(3) 0.0326(17) Uani 1 1 d . . .
H31 H 0.5029 0.4535 -0.1584 0.039 Uiso 1 1 calc R . .
C42 C 0.6478(8) 0.0570(5) 0.1399(3) 0.0340(17) Uani 1 1 d . . .
H42 H 0.5471 0.0567 0.1275 0.041 Uiso 1 1 calc R . .
C44 C 0.6786(10) 0.0582(5) 0.2068(3) 0.043(2) Uani 1 1 d . . .
H44A H 0.6228 0.0192 0.2209 0.065 Uiso 1 1 calc R . .
H44B H 0.6581 0.1099 0.2202 0.065 Uiso 1 1 calc R . .
H44C H 0.7743 0.0464 0.2217 0.065 Uiso 1 1 calc R . .
C43 C 0.6953(10) -0.0202(5) 0.1185(4) 0.044(2) Uani 1 1 d . . .
H43A H 0.7927 -0.0260 0.1333 0.066 Uiso 1 1 calc R . .
H43B H 0.6760 -0.0204 0.0762 0.066 Uiso 1 1 calc R . .
H43C H 0.6476 -0.0634 0.1323 0.066 Uiso 1 1 calc R . .
C41 C 0.9794(9) 0.1181(6) 0.1697(4) 0.052(2) Uani 1 1 d . . .
H41A H 1.0052 0.0955 0.1356 0.078 Uiso 1 1 calc R . .
H41B H 0.9380 0.0780 0.1896 0.078 Uiso 1 1 calc R . .
H41C H 1.0599 0.1388 0.1959 0.078 Uiso 1 1 calc R . .
C17 C 0.9686(8) 0.3721(6) 0.3769(3) 0.042(2) Uani 1 1 d . . .
H17 H 1.0363 0.3874 0.4092 0.051 Uiso 1 1 calc R . .
C16 C 0.9857(8) 0.3077(6) 0.3470(3) 0.043(2) Uani 1 1 d . . .
H16 H 1.0667 0.2786 0.3582 0.052 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
Bi1 N1 2.164(5) . ?
Bi1 Br2 2.6277(9) . ?
Bi1 Br1 2.6449(9) . ?
C40 C39 1.526(13) . ?
Si1 N1 1.798(6) . ?
Si1 C42 1.883(8) . ?
Si1 C36 1.895(7) . ?
Si1 C39 1.908(8) . ?
C21 C22 1.393(9) . ?
C21 C26 1.406(9) . ?
C21 C20 1.533(9) . ?
C22 C23 1.405(11) . ?
C24 C25 1.387(11) . ?
C24 C23 1.388(12) . ?
C26 C25 1.382(10) . ?
N1 C1 1.469(8) . ?
C7 C6 1.522(9) . ?
C7 C14 1.531(9) . ?
C7 C8 1.533(9) . ?
C20 C2 1.525(9) . ?
C20 C27 1.533(8) . ?
C6 C5 1.404(9) . ?
C6 C1 1.421(9) . ?
C1 C2 1.410(9) . ?
C13 C12 1.388(11) . ?
C13 C8 1.410(10) . ?
C4 C5 1.397(9) . ?
C4 C3 1.410(9) . ?
C4 C33 1.502(9) . ?
C27 C32 1.385(9) . ?
C27 C28 1.397(10) . ?
C8 C9 1.380(10) . ?
C3 C2 1.387(9) . ?
C12 C11 1.388(13) . ?
C11 C10 1.361(12) . ?
C9 C10 1.413(10) . ?
C28 C29 1.372(11) . ?
C15 C14 1.396(11) . ?
C15 C16 1.406(12) . ?
C14 C19 1.400(11) . ?
C32 C31 1.391(10) . ?
C30 C29 1.370(11) . ?
C30 C31 1.371(11) . ?
C33 C34 1.501(12) . ?
C33 C35 1.505(11) . ?
C39 C41 1.546(11) . ?
C19 C18 1.398(11) . ?
C37 C36 1.500(11) . ?
C18 C17 1.383(13) . ?
C38 C36 1.543(11) . ?
C42 C43 1.533(11) . ?
C42 C44 1.550(11) . ?
C17 C16 1.344(14) . ?

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
N1 Bi1 Br2 103.53(15) . . ?
N1 Bi1 Br1 104.04(14) . . ?
Br2 Bi1 Br1 88.69(3) . . ?
N1 Si1 C42 105.1(3) . . ?
N1 Si1 C36 111.8(3) . . ?
C42 Si1 C36 112.6(3) . . ?
N1 Si1 C39 107.2(3) . . ?
C42 Si1 C39 113.3(4) . . ?
C36 Si1 C39 106.8(3) . . ?
C22 C21 C26 118.4(6) . . ?
C22 C21 C20 120.1(6) . . ?
C26 C21 C20 121.4(6) . . ?
C21 C22 C23 120.7(7) . . ?
C25 C24 C23 119.5(7) . . ?
C25 C26 C21 120.5(6) . . ?
C24 C23 C22 119.9(7) . . ?
C26 C25 C24 120.9(7) . . ?
C1 N1 Si1 116.4(4) . . ?
C1 N1 Bi1 110.4(4) . . ?
Si1 N1 Bi1 133.0(3) . . ?
C6 C7 C14 112.9(5) . . ?
C6 C7 C8 111.4(5) . . ?
C14 C7 C8 111.3(5) . . ?
C2 C20 C27 113.8(5) . . ?
C2 C20 C21 108.9(5) . . ?
C27 C20 C21 113.6(5) . . ?
C5 C6 C1 118.0(6) . . ?
C5 C6 C7 120.1(5) . . ?
C1 C6 C7 121.6(6) . . ?
C2 C1 C6 119.6(6) . . ?
C2 C1 N1 120.4(5) . . ?
C6 C1 N1 120.0(5) . . ?
C12 C13 C8 120.0(7) . . ?
C5 C4 C3 116.6(6) . . ?
C5 C4 C33 122.0(6) . . ?
C3 C4 C33 121.3(6) . . ?
C32 C27 C28 117.5(6) . . ?
C32 C27 C20 122.4(6) . . ?
C28 C27 C20 120.1(6) . . ?
C9 C8 C13 118.2(6) . . ?
C9 C8 C7 123.3(6) . . ?
C13 C8 C7 118.4(6) . . ?
C2 C3 C4 122.4(6) . . ?
C4 C5 C6 123.2(6) . . ?
C3 C2 C1 119.6(6) . . ?
C3 C2 C20 119.5(6) . . ?
C1 C2 C20 120.6(6) . . ?
C13 C12 C11 120.6(7) . . ?
C10 C11 C12 120.3(7) . . ?
C8 C9 C10 121.3(7) . . ?
C29 C28 C27 121.6(7) . . ?
C11 C10 C9 119.5(7) . . ?
C14 C15 C16 118.9(8) . . ?
C15 C14 C19 119.2(7) . . ?
C15 C14 C7 119.7(6) . . ?
C19 C14 C7 121.1(7) . . ?
C27 C32 C31 120.3(7) . . ?
C29 C30 C31 119.2(7) . . ?
C34 C33 C4 108.5(6) . . ?
C34 C33 C35 109.7(8) . . ?
C4 C33 C35 114.8(6) . . ?
C40 C39 C41 108.8(7) . . ?
C40 C39 Si1 116.5(5) . . ?
C41 C39 Si1 113.0(6) . . ?
C30 C29 C28 120.4(7) . . ?
C18 C19 C14 119.8(8) . . ?
C17 C18 C19 120.2(8) . . ?
C37 C36 C38 109.8(6) . . ?
C37 C36 Si1 116.3(5) . . ?
C38 C36 Si1 114.5(5) . . ?
C30 C31 C32 121.1(7) . . ?
C43 C42 C44 110.0(7) . . ?
C43 C42 Si1 116.6(5) . . ?
C44 C42 Si1 112.0(6) . . ?
C16 C17 C18 120.0(8) . . ?
C17 C16 C15 121.8(8) . . ?

_diffrn_measured_fraction_theta_max 0.940
_diffrn_reflns_theta_full        25.25
_diffrn_measured_fraction_theta_full 0.940
_refine_diff_density_max         3.030
_refine_diff_density_min         -1.380
_refine_diff_density_rms         0.167
####################################################################### 
# 
# 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_compound1g
_database_code_depnum_ccdc_archive 'CCDC 1051446'
_audit_update_record             
;
2015-02-27 deposited with the CCDC.
2015-03-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C51 H42 Bi Br2 N Si'
_chemical_formula_weight         1065.75

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'
Si Si 0.0817 0.0704 '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'
Bi Bi -4.1077 10.2566 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.3779(4)
_cell_length_b                   12.1720(4)
_cell_length_c                   18.3157(7)
_cell_angle_alpha                82.925(2)
_cell_angle_beta                 88.322(2)
_cell_angle_gamma                66.682(2)
_cell_volume                     2108.00(13)
_cell_formula_units_Z            2
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.679
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1044
_exptl_absorpt_coefficient_mu    6.143
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.148
_exptl_absorpt_correction_T_max  0.887
_exptl_absorpt_process_details   'Sortav (Blessing)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Apex X8'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            20733
_diffrn_reflns_av_R_equivalents  0.0321
_diffrn_reflns_av_sigmaI/netI    0.0458
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         3.32
_diffrn_reflns_theta_max         26.50
_reflns_number_total             8685
_reflns_number_gt                7712
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0261P)²+2.0029P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8685
_refine_ls_number_parameters     506
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0358
_refine_ls_R_factor_gt           0.0289
_refine_ls_wR_factor_ref         0.0655
_refine_ls_wR_factor_gt          0.0635
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_restrained_S_all      1.040
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Bi1 Bi 0.162594(14) 0.636398(13) 0.333859(8) 0.01461(5) Uani 1 1 d . . .
Br1 Br 0.09373(4) 0.51199(4) 0.24529(2) 0.02602(10) Uani 1 1 d . . .
Br2 Br 0.38813(4) 0.45212(4) 0.37953(2) 0.02591(10) Uani 1 1 d . . .
Si1 Si 0.15813(10) 0.84084(9) 0.19370(5) 0.0113(2) Uani 1 1 d . . .
C28 C 0.2965(3) 0.9623(3) 0.41192(19) 0.0106(7) Uani 1 1 d . . .
C7 C 0.5257(4) 0.6008(3) 0.18250(19) 0.0119(7) Uani 1 1 d . . .
H7 H 0.4282 0.6423 0.1612 0.014 Uiso 1 1 calc R . .
C6 C 0.5251(4) 0.6516(3) 0.25470(19) 0.0102(7) Uani 1 1 d . . .
C29 C 0.3163(4) 0.9748(3) 0.4839(2) 0.0174(8) Uani 1 1 d . . .
H29 H 0.3162 0.9143 0.5220 0.021 Uiso 1 1 calc R . .
N1 N 0.2648(3) 0.7318(3) 0.26099(15) 0.0103(6) Uani 1 1 d . . .
C31 C 0.3350(4) 1.1640(3) 0.4470(2) 0.0186(8) Uani 1 1 d . . .
H31 H 0.3478 1.2327 0.4592 0.022 Uiso 1 1 calc R . .
C14 C 0.6218(4) 0.6309(3) 0.12625(19) 0.0131(8) Uani 1 1 d . . .
C1 C 0.3991(3) 0.7192(3) 0.28838(18) 0.0088(7) Uani 1 1 d . . .
C2 C 0.4065(3) 0.7709(3) 0.35203(18) 0.0085(7) Uani 1 1 d . . .
C4 C 0.6598(3) 0.6747(3) 0.3537(2) 0.0128(7) Uani 1 1 d . . .
C5 C 0.6519(3) 0.6326(3) 0.28831(19) 0.0110(7) Uani 1 1 d . . .
H5 H 0.7368 0.5886 0.2651 0.013 Uiso 1 1 calc R . .
C3 C 0.5356(3) 0.7466(3) 0.38372(19) 0.0116(7) Uani 1 1 d . . .
H3 H 0.5392 0.7803 0.4274 0.014 Uiso 1 1 calc R . .
C21 C 0.2751(3) 0.8543(3) 0.38837(19) 0.0104(7) Uani 1 1 d . . .
H21 H 0.1990 0.8874 0.3496 0.012 Uiso 1 1 calc R . .
C34 C -0.0272(3) 0.8691(3) 0.2225(2) 0.0131(7) Uani 1 1 d . . .
C40 C 0.1770(4) 0.7958(4) 0.0986(2) 0.0164(8) Uani 1 1 d . . .
C8 C 0.5586(4) 0.4658(3) 0.1914(2) 0.0149(8) Uani 1 1 d . . .
C20 C 0.7989(4) 0.6464(3) 0.3908(2) 0.0169(8) Uani 1 1 d . . .
H20A H 0.8739 0.5871 0.3654 0.025 Uiso 1 1 calc R . .
H20B H 0.7971 0.6133 0.4422 0.025 Uiso 1 1 calc R . .
H20C H 0.8161 0.7202 0.3890 0.025 Uiso 1 1 calc R . .
C46 C 0.1889(4) 0.9830(3) 0.18781(18) 0.0116(7) Uani 1 1 d . . .
C47 C 0.0822(4) 1.0943(4) 0.1942(2) 0.0190(8) Uani 1 1 d . . .
H47 H -0.0101 1.0988 0.2040 0.023 Uiso 1 1 calc R . .
C32 C 0.3150(4) 1.1525(4) 0.3750(2) 0.0207(9) Uani 1 1 d . . .
H32 H 0.3141 1.2135 0.3370 0.025 Uiso 1 1 calc R . .
C36 C -0.2514(4) 0.8593(4) 0.2028(2) 0.0239(9) Uani 1 1 d . . .
H36 H -0.3099 0.8370 0.1741 0.029 Uiso 1 1 calc R . .
C19 C 0.7655(4) 0.5630(4) 0.1260(2) 0.0173(8) Uani 1 1 d . . .
H19 H 0.8059 0.4925 0.1602 0.021 Uiso 1 1 calc R . .
C51 C 0.3228(4) 0.9810(3) 0.17301(19) 0.0143(8) Uani 1 1 d . . .
H51 H 0.3985 0.9062 0.1685 0.017 Uiso 1 1 calc R . .
C15 C 0.5664(4) 0.7302(4) 0.0736(2) 0.0205(9) Uani 1 1 d . . .
H15 H 0.4680 0.7764 0.0714 0.025 Uiso 1 1 calc R . .
C33 C 0.2963(4) 1.0532(3) 0.3577(2) 0.0174(8) Uani 1 1 d . . .
H33 H 0.2830 1.0463 0.3076 0.021 Uiso 1 1 calc R . .
C9 C 0.6412(4) 0.3854(4) 0.2465(2) 0.0214(9) Uani 1 1 d . . .
H9 H 0.6784 0.4133 0.2836 0.026 Uiso 1 1 calc R . .
C35 C -0.1152(4) 0.8373(3) 0.1815(2) 0.0186(8) Uani 1 1 d . . .
H35 H -0.0812 0.7999 0.1383 0.022 Uiso 1 1 calc R . .
C39 C -0.0823(4) 0.9236(3) 0.2854(2) 0.0165(8) Uani 1 1 d . . .
H39 H -0.0247 0.9460 0.3147 0.020 Uiso 1 1 calc R . .
C44 C 0.1949(4) 0.6503(4) 0.0156(2) 0.0230(9) Uani 1 1 d . . .
H44 H 0.2076 0.5708 0.0081 0.028 Uiso 1 1 calc R . .
C13 C 0.5063(4) 0.4230(4) 0.1373(2) 0.0206(9) Uani 1 1 d . . .
H13 H 0.4503 0.4778 0.0979 0.025 Uiso 1 1 calc R . .
C45 C 0.1929(4) 0.6800(4) 0.0860(2) 0.0196(8) Uani 1 1 d . . .
H45 H 0.2024 0.6207 0.1267 0.024 Uiso 1 1 calc R . .
C37 C -0.3024(4) 0.9129(4) 0.2648(2) 0.0214(9) Uani 1 1 d . . .
H37 H -0.3958 0.9274 0.2793 0.026 Uiso 1 1 calc R . .
C38 C -0.2180(4) 0.9457(4) 0.3060(2) 0.0227(9) Uani 1 1 d . . .
H38 H -0.2534 0.9838 0.3489 0.027 Uiso 1 1 calc R . .
C18 C 0.8507(4) 0.5966(4) 0.0765(2) 0.0256(10) Uani 1 1 d . . .
H18 H 0.9489 0.5498 0.0778 0.031 Uiso 1 1 calc R . .
C49 C 0.2391(4) 1.1944(4) 0.1724(2) 0.0223(9) Uani 1 1 d . . .
H49 H 0.2562 1.2660 0.1676 0.027 Uiso 1 1 calc R . .
C10 C 0.6720(5) 0.2623(4) 0.2492(2) 0.0297(10) Uani 1 1 d . . .
H10 H 0.7301 0.2070 0.2878 0.036 Uiso 1 1 calc R . .
C12 C 0.5348(4) 0.3018(4) 0.1401(3) 0.0290(10) Uani 1 1 d . . .
H12 H 0.4967 0.2740 0.1033 0.035 Uiso 1 1 calc R . .
C41 C 0.1618(4) 0.8801(4) 0.0377(2) 0.0219(9) Uani 1 1 d . . .
H41 H 0.1504 0.9596 0.0444 0.026 Uiso 1 1 calc R . .
C42 C 0.1630(4) 0.8499(4) -0.0327(2) 0.0303(10) Uani 1 1 d . . .
H42 H 0.1529 0.9085 -0.0739 0.036 Uiso 1 1 calc R . .
C50 C 0.3472(4) 1.0852(4) 0.1649(2) 0.0183(8) Uani 1 1 d . . .
H50 H 0.4387 1.0817 0.1541 0.022 Uiso 1 1 calc R . .
C11 C 0.6179(5) 0.2212(4) 0.1957(3) 0.0326(11) Uani 1 1 d . . .
H11 H 0.6380 0.1377 0.1973 0.039 Uiso 1 1 calc R . .
C17 C 0.7948(5) 0.6968(5) 0.0256(2) 0.0303(11) Uani 1 1 d . . .
H17 H 0.8537 0.7200 -0.0080 0.036 Uiso 1 1 calc R . .
C16 C 0.6516(5) 0.7634(4) 0.0240(2) 0.0292(10) Uani 1 1 d . . .
H16 H 0.6114 0.8323 -0.0114 0.035 Uiso 1 1 calc R . .
C48 C 0.1062(4) 1.1992(4) 0.1869(2) 0.0233(9) Uani 1 1 d . . .
H48 H 0.0311 1.2742 0.1918 0.028 Uiso 1 1 calc R . .
C30 C 0.3363(4) 1.0745(4) 0.5014(2) 0.0192(8) Uani 1 1 d . . .
H30 H 0.3510 1.0813 0.5513 0.023 Uiso 1 1 calc R . .
C43 C 0.1787(4) 0.7354(4) -0.0435(2) 0.0285(10) Uani 1 1 d . . .
H43 H 0.1783 0.7156 -0.0920 0.034 Uiso 1 1 calc R . .
C22 C 0.2229(3) 0.7903(3) 0.45080(19) 0.0116(7) Uani 1 1 d . . .
C23 C 0.0843(4) 0.8444(3) 0.4732(2) 0.0171(8) Uani 1 1 d . . .
H23 H 0.0233 0.9186 0.4472 0.021 Uiso 1 1 calc R . .
C27 C 0.3086(4) 0.6831(3) 0.4907(2) 0.0170(8) Uani 1 1 d . . .
H27 H 0.4038 0.6451 0.4773 0.020 Uiso 1 1 calc R . .
C25 C 0.1203(4) 0.6853(4) 0.5701(2) 0.0266(10) Uani 1 1 d . . .
H25 H 0.0853 0.6491 0.6105 0.032 Uiso 1 1 calc R . .
C24 C 0.0345(4) 0.7926(4) 0.5321(2) 0.0234(9) Uani 1 1 d . . .
H24 H -0.0600 0.8313 0.5464 0.028 Uiso 1 1 calc R . .
C26 C 0.2584(4) 0.6300(4) 0.5496(2) 0.0235(9) Uani 1 1 d . . .
H26 H 0.3186 0.5557 0.5759 0.028 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
Bi1 N1 2.183(3) . ?
Bi1 Br2 2.5895(4) . ?
Bi1 Br1 2.6392(4) . ?
Si1 N1 1.738(3) . ?
Si1 C46 1.870(4) . ?
Si1 C40 1.871(4) . ?
Si1 C34 1.886(4) . ?
C28 C29 1.375(5) . ?
C28 C33 1.392(5) . ?
C28 C21 1.530(5) . ?
C7 C14 1.525(5) . ?
C7 C6 1.526(5) . ?
C7 C8 1.528(5) . ?
C6 C5 1.391(5) . ?
C6 C1 1.412(5) . ?
C29 C30 1.385(5) . ?
N1 C1 1.439(4) . ?
C31 C32 1.374(5) . ?
C31 C30 1.379(5) . ?
C14 C15 1.385(5) . ?
C14 C19 1.390(5) . ?
C1 C2 1.409(5) . ?
C2 C3 1.382(5) . ?
C2 C21 1.533(4) . ?
C4 C5 1.375(5) . ?
C4 C3 1.384(5) . ?
C4 C20 1.507(5) . ?
C21 C22 1.512(5) . ?
C34 C35 1.391(5) . ?
C34 C39 1.394(5) . ?
C40 C41 1.387(6) . ?
C40 C45 1.402(5) . ?
C8 C9 1.362(5) . ?
C8 C13 1.391(5) . ?
C46 C47 1.386(5) . ?
C46 C51 1.398(5) . ?
C47 C48 1.384(6) . ?
C32 C33 1.372(5) . ?
C36 C37 1.368(6) . ?
C36 C35 1.384(5) . ?
C19 C18 1.385(5) . ?
C51 C50 1.379(5) . ?
C15 C16 1.384(6) . ?
C9 C10 1.398(6) . ?
C39 C38 1.376(5) . ?
C44 C43 1.367(6) . ?
C44 C45 1.378(5) . ?
C13 C12 1.380(6) . ?
C37 C38 1.374(6) . ?
C18 C17 1.373(6) . ?
C49 C48 1.376(6) . ?
C49 C50 1.378(5) . ?
C10 C11 1.380(6) . ?
C12 C11 1.370(6) . ?
C41 C42 1.381(5) . ?
C42 C43 1.376(6) . ?
C17 C16 1.382(6) . ?
C22 C27 1.383(5) . ?
C22 C23 1.398(5) . ?
C23 C24 1.373(5) . ?
C27 C26 1.384(5) . ?
C25 C24 1.369(6) . ?
C25 C26 1.384(6) . ?

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
N1 Bi1 Br2 96.93(7) . . ?
N1 Bi1 Br1 103.26(7) . . ?
Br2 Bi1 Br1 91.995(14) . . ?
N1 Si1 C46 111.60(15) . . ?
N1 Si1 C40 115.38(16) . . ?
C46 Si1 C40 106.83(17) . . ?
N1 Si1 C34 105.24(15) . . ?
C46 Si1 C34 110.44(16) . . ?
C40 Si1 C34 107.26(16) . . ?
C29 C28 C33 117.9(3) . . ?
C29 C28 C21 123.7(3) . . ?
C33 C28 C21 118.4(3) . . ?
C14 C7 C6 112.2(3) . . ?
C14 C7 C8 110.6(3) . . ?
C6 C7 C8 114.2(3) . . ?
C5 C6 C1 118.5(3) . . ?
C5 C6 C7 119.5(3) . . ?
C1 C6 C7 121.9(3) . . ?
C28 C29 C30 120.8(4) . . ?
C1 N1 Si1 127.6(2) . . ?
C1 N1 Bi1 113.7(2) . . ?
Si1 N1 Bi1 116.14(14) . . ?
C32 C31 C30 119.1(4) . . ?
C15 C14 C19 117.7(3) . . ?
C15 C14 C7 119.8(3) . . ?
C19 C14 C7 122.5(3) . . ?
C2 C1 C6 118.8(3) . . ?
C2 C1 N1 119.7(3) . . ?
C6 C1 N1 121.5(3) . . ?
C3 C2 C1 119.8(3) . . ?
C3 C2 C21 117.9(3) . . ?
C1 C2 C21 122.3(3) . . ?
C5 C4 C3 117.9(3) . . ?
C5 C4 C20 121.5(3) . . ?
C3 C4 C20 120.7(3) . . ?
C4 C5 C6 122.8(3) . . ?
C2 C3 C4 121.8(3) . . ?
C22 C21 C28 111.8(3) . . ?
C22 C21 C2 113.8(3) . . ?
C28 C21 C2 111.2(3) . . ?
C35 C34 C39 117.2(3) . . ?
C35 C34 Si1 121.5(3) . . ?
C39 C34 Si1 121.4(3) . . ?
C41 C40 C45 117.5(3) . . ?
C41 C40 Si1 120.6(3) . . ?
C45 C40 Si1 121.6(3) . . ?
C9 C8 C13 118.7(4) . . ?
C9 C8 C7 124.1(3) . . ?
C13 C8 C7 117.1(3) . . ?
C47 C46 C51 117.0(3) . . ?
C47 C46 Si1 122.7(3) . . ?
C51 C46 Si1 120.2(3) . . ?
C48 C47 C46 121.8(4) . . ?
C33 C32 C31 120.2(4) . . ?
C37 C36 C35 120.5(4) . . ?
C18 C19 C14 120.9(4) . . ?
C50 C51 C46 121.5(3) . . ?
C16 C15 C14 121.3(4) . . ?
C32 C33 C28 121.4(3) . . ?
C8 C9 C10 120.9(4) . . ?
C36 C35 C34 121.0(4) . . ?
C38 C39 C34 121.6(4) . . ?
C43 C44 C45 119.9(4) . . ?
C12 C13 C8 120.7(4) . . ?
C44 C45 C40 121.3(4) . . ?
C36 C37 C38 119.7(4) . . ?
C37 C38 C39 120.1(4) . . ?
C17 C18 C19 120.8(4) . . ?
C48 C49 C50 119.7(4) . . ?
C11 C10 C9 119.8(4) . . ?
C11 C12 C13 120.4(4) . . ?
C42 C41 C40 120.8(4) . . ?
C43 C42 C41 120.5(4) . . ?
C49 C50 C51 120.1(4) . . ?
C12 C11 C10 119.5(4) . . ?
C18 C17 C16 118.9(4) . . ?
C17 C16 C15 120.4(4) . . ?
C49 C48 C47 119.9(4) . . ?
C31 C30 C29 120.5(3) . . ?
C44 C43 C42 120.0(4) . . ?
C27 C22 C23 117.4(3) . . ?
C27 C22 C21 123.1(3) . . ?
C23 C22 C21 119.4(3) . . ?
C24 C23 C22 121.4(4) . . ?
C22 C27 C26 121.4(3) . . ?
C24 C25 C26 119.7(4) . . ?
C25 C24 C23 120.3(4) . . ?
C27 C26 C25 119.8(4) . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        26.50
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         1.073
_refine_diff_density_min         -0.765
_refine_diff_density_rms         0.116
####################################################################### 
# 
# 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_compound1S
_database_code_depnum_ccdc_archive 'CCDC 1051447'
_audit_update_record             
;
2015-02-27 deposited with the CCDC.
2015-03-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C82 H90 B Bi2 N3 Si'
_chemical_formula_weight         1574.43

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'
Bi Bi -4.1077 10.2566 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   13.6508(5)
_cell_length_b                   14.2481(6)
_cell_length_c                   20.2258(7)
_cell_angle_alpha                97.059(3)
_cell_angle_beta                 95.917(3)
_cell_angle_gamma                112.943(4)
_cell_volume                     3545.8(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.475
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1576
_exptl_absorpt_coefficient_mu    5.019
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.581
_exptl_absorpt_correction_T_max  0.660
_exptl_absorpt_process_details   'Sortav (Blessing)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Apex X8'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            27961
_diffrn_reflns_av_R_equivalents  0.0410
_diffrn_reflns_av_sigmaI/netI    0.0654
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.98
_diffrn_reflns_theta_max         25.50
_reflns_number_total             13193
_reflns_number_gt                9868
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger.
 A molecule of pentane of crystallisation was located in the asymmetric unit
 and its carbon atoms refined anisotropically. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0417P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         13193
_refine_ls_number_parameters     821
_refine_ls_number_restraints     16
_refine_ls_R_factor_all          0.0641
_refine_ls_R_factor_gt           0.0396
_refine_ls_wR_factor_ref         0.0924
_refine_ls_wR_factor_gt          0.0839
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_restrained_S_all      1.019
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Bi1 Bi 0.306703(14) 1.202221(16) 0.283749(12) 0.02750(7) Uani 1 1 d . . .
Si1 Si 0.56077(10) 1.38074(10) 0.30533(7) 0.0142(3) Uani 1 1 d . . .
N1 N 0.4870(3) 1.2513(3) 0.30588(19) 0.0116(9) Uani 1 1 d . . .
C1 C 0.5245(3) 1.1722(4) 0.3105(2) 0.0139(11) Uani 1 1 d . . .
B1 B 0.0611(5) 0.9589(5) 0.2157(3) 0.0236(14) Uani 1 1 d . . .
Bi2 Bi 0.238220(15) 0.985374(16) 0.258318(13) 0.03479(8) Uani 1 1 d . . .
N2 N 0.0099(3) 1.0257(3) 0.2016(2) 0.0215(10) Uani 1 1 d . . .
C2 C 0.5373(3) 1.1144(4) 0.2519(2) 0.0133(10) Uani 1 1 d . . .
N3 N -0.0210(3) 0.8563(3) 0.1932(2) 0.0257(11) Uani 1 1 d . . .
C3 C 0.5593(4) 1.0275(4) 0.2583(3) 0.0164(11) Uani 1 1 d . . .
H3 H 0.5640 0.9872 0.2187 0.020 Uiso 1 1 calc R . .
C4 C 0.5745(4) 0.9978(4) 0.3195(3) 0.0166(11) Uani 1 1 d . . .
C5 C 0.5692(4) 1.0591(4) 0.3766(2) 0.0153(11) Uani 1 1 d . . .
H5 H 0.5844 1.0427 0.4196 0.018 Uiso 1 1 calc R . .
C6 C 0.5428(3) 1.1435(3) 0.3737(2) 0.0135(10) Uani 1 1 d . . .
C7 C 0.5343(3) 1.2039(4) 0.4393(2) 0.0130(10) Uani 1 1 d . . .
H7 H 0.5464 1.2749 0.4306 0.016 Uiso 1 1 calc R . .
C8 C 0.6231(4) 1.2176(3) 0.4971(2) 0.0149(11) Uani 1 1 d . . .
C9 C 0.7311(4) 1.2662(4) 0.4892(3) 0.0233(12) Uani 1 1 d . . .
H9 H 0.7480 1.2861 0.4472 0.028 Uiso 1 1 calc R . .
C10 C 0.8133(4) 1.2857(4) 0.5420(3) 0.0307(14) Uani 1 1 d . . .
H10 H 0.8863 1.3180 0.5358 0.037 Uiso 1 1 calc R . .
C11 C 0.7902(4) 1.2584(4) 0.6037(3) 0.0312(14) Uani 1 1 d . . .
H11 H 0.8468 1.2735 0.6403 0.037 Uiso 1 1 calc R . .
C12 C 0.6850(4) 1.2096(4) 0.6116(3) 0.0271(13) Uani 1 1 d . . .
H12 H 0.6685 1.1892 0.6535 0.033 Uiso 1 1 calc R . .
C13 C 0.6022(4) 1.1896(4) 0.5589(3) 0.0200(12) Uani 1 1 d . . .
H13 H 0.5295 1.1560 0.5654 0.024 Uiso 1 1 calc R . .
C14 C 0.4225(4) 1.1584(4) 0.4593(2) 0.0149(11) Uani 1 1 d . . .
C15 C 0.3839(4) 1.2224(4) 0.4942(3) 0.0212(12) Uani 1 1 d . . .
H15 H 0.4261 1.2950 0.5037 0.025 Uiso 1 1 calc R . .
C16 C 0.2849(4) 1.1831(4) 0.5159(3) 0.0300(14) Uani 1 1 d . . .
H16 H 0.2588 1.2286 0.5387 0.036 Uiso 1 1 calc R . .
C17 C 0.2243(4) 1.0768(5) 0.5040(3) 0.0316(14) Uani 1 1 d . . .
H17 H 0.1565 1.0492 0.5188 0.038 Uiso 1 1 calc R . .
C18 C 0.2629(4) 1.0122(4) 0.4709(3) 0.0255(13) Uani 1 1 d . . .
H18 H 0.2222 0.9394 0.4633 0.031 Uiso 1 1 calc R . .
C19 C 0.3611(4) 1.0526(4) 0.4484(2) 0.0195(11) Uani 1 1 d . . .
H19 H 0.3867 1.0069 0.4252 0.023 Uiso 1 1 calc R . .
C20 C 0.5348(4) 1.1496(4) 0.1837(2) 0.0153(11) Uani 1 1 d . . .
H20 H 0.5071 1.2051 0.1890 0.018 Uiso 1 1 calc R . .
C21 C 0.6471(4) 1.1999(4) 0.1639(2) 0.0158(11) Uani 1 1 d . . .
C22 C 0.6604(4) 1.2679(4) 0.1185(3) 0.0197(11) Uani 1 1 d . . .
H22 H 0.6003 1.2797 0.0998 0.024 Uiso 1 1 calc R . .
C23 C 0.7606(4) 1.3188(4) 0.1001(3) 0.0251(13) Uani 1 1 d . . .
H23 H 0.7684 1.3650 0.0689 0.030 Uiso 1 1 calc R . .
C24 C 0.8484(4) 1.3028(4) 0.1267(3) 0.0247(13) Uani 1 1 d . . .
H24 H 0.9172 1.3390 0.1150 0.030 Uiso 1 1 calc R . .
C25 C 0.8353(4) 1.2336(4) 0.1705(3) 0.0260(13) Uani 1 1 d . . .
H25 H 0.8952 1.2205 0.1880 0.031 Uiso 1 1 calc R . .
C26 C 0.7362(4) 1.1830(4) 0.1895(3) 0.0207(12) Uani 1 1 d . . .
H26 H 0.7289 1.1362 0.2202 0.025 Uiso 1 1 calc R . .
C27 C 0.4579(4) 1.0664(4) 0.1253(2) 0.0185(11) Uani 1 1 d . . .
C28 C 0.3613(4) 1.0710(5) 0.1017(3) 0.0331(14) Uani 1 1 d . . .
H28 H 0.3426 1.1233 0.1231 0.040 Uiso 1 1 calc R . .
C29 C 0.2918(5) 0.9994(5) 0.0467(3) 0.0450(17) Uani 1 1 d . . .
H29 H 0.2258 1.0036 0.0309 0.054 Uiso 1 1 calc R . .
C30 C 0.3164(5) 0.9233(5) 0.0150(3) 0.0345(15) Uani 1 1 d . . .
H30 H 0.2681 0.8747 -0.0225 0.041 Uiso 1 1 calc R . .
C31 C 0.4107(5) 0.9177(4) 0.0377(3) 0.0303(14) Uani 1 1 d . . .
H31 H 0.4279 0.8641 0.0165 0.036 Uiso 1 1 calc R . .
C32 C 0.4823(4) 0.9900(4) 0.0918(3) 0.0225(12) Uani 1 1 d . . .
H32 H 0.5493 0.9867 0.1060 0.027 Uiso 1 1 calc R . .
C33 C 0.5983(4) 0.9030(4) 0.3239(3) 0.0241(12) Uani 1 1 d . . .
H33A H 0.5304 0.8409 0.3149 0.036 Uiso 1 1 calc R . .
H33B H 0.6362 0.9098 0.3693 0.036 Uiso 1 1 calc R . .
H33C H 0.6435 0.8970 0.2905 0.036 Uiso 1 1 calc R . .
C34 C 0.7015(4) 1.4227(4) 0.3518(2) 0.0162(11) Uani 1 1 d . . .
C35 C 0.7443(4) 1.4960(4) 0.4108(3) 0.0231(12) Uani 1 1 d . . .
H35 H 0.7013 1.5280 0.4292 0.028 Uiso 1 1 calc R . .
C36 C 0.8493(5) 1.5235(4) 0.4435(3) 0.0335(15) Uani 1 1 d . . .
H36 H 0.8770 1.5734 0.4839 0.040 Uiso 1 1 calc R . .
C37 C 0.9129(4) 1.4780(4) 0.4169(3) 0.0289(14) Uani 1 1 d . . .
H37 H 0.9847 1.4974 0.4389 0.035 Uiso 1 1 calc R . .
C38 C 0.8733(4) 1.4058(4) 0.3597(3) 0.0269(13) Uani 1 1 d . . .
H38 H 0.9167 1.3736 0.3422 0.032 Uiso 1 1 calc R . .
C39 C 0.7683(4) 1.3787(4) 0.3264(3) 0.0215(12) Uani 1 1 d . . .
H39 H 0.7419 1.3292 0.2857 0.026 Uiso 1 1 calc R . .
C40 C 0.5719(4) 1.4190(3) 0.2193(2) 0.0160(11) Uani 1 1 d . . .
C41 C 0.4820(4) 1.3871(4) 0.1687(3) 0.0224(12) Uani 1 1 d . . .
H41 H 0.4138 1.3413 0.1768 0.027 Uiso 1 1 calc R . .
C42 C 0.4889(4) 1.4197(4) 0.1075(3) 0.0285(13) Uani 1 1 d . . .
H42 H 0.4263 1.3959 0.0740 0.034 Uiso 1 1 calc R . .
C43 C 0.5871(5) 1.4872(4) 0.0946(3) 0.0294(14) Uani 1 1 d . . .
H43 H 0.5921 1.5100 0.0524 0.035 Uiso 1 1 calc R . .
C44 C 0.6768(4) 1.5209(4) 0.1430(3) 0.0271(13) Uani 1 1 d . . .
H44 H 0.7443 1.5673 0.1344 0.032 Uiso 1 1 calc R . .
C45 C 0.6697(4) 1.4874(4) 0.2046(3) 0.0204(12) Uani 1 1 d . . .
H45 H 0.7328 1.5116 0.2377 0.025 Uiso 1 1 calc R . .
C46 C 0.4872(4) 1.4539(4) 0.3451(3) 0.0212(12) Uani 1 1 d . . .
C47 C 0.4360(6) 1.4265(6) 0.3989(3) 0.053(2) Uani 1 1 d . . .
H47 H 0.4439 1.3728 0.4194 0.064 Uiso 1 1 calc R . .
C48 C 0.3739(7) 1.4733(6) 0.4245(4) 0.060(2) Uani 1 1 d . . .
H48 H 0.3383 1.4499 0.4611 0.072 Uiso 1 1 calc R . .
C49 C 0.3625(4) 1.5514(4) 0.3989(3) 0.0348(15) Uani 1 1 d . . .
H49 H 0.3215 1.5851 0.4180 0.042 Uiso 1 1 calc R . .
C50 C 0.4103(6) 1.5810(5) 0.3456(4) 0.055(2) Uani 1 1 d . . .
H50 H 0.4006 1.6345 0.3258 0.066 Uiso 1 1 calc R . .
C51 C 0.4736(6) 1.5348(5) 0.3192(4) 0.0471(18) Uani 1 1 d . . .
H51 H 0.5085 1.5589 0.2826 0.057 Uiso 1 1 calc R . .
C52 C -0.0233(4) 0.7589(4) 0.2078(3) 0.0255(13) Uani 1 1 d . . .
C53 C 0.0029(5) 0.6943(4) 0.1619(3) 0.0347(15) Uani 1 1 d . . .
C54 C 0.0026(5) 0.6032(4) 0.1813(3) 0.0371(15) Uani 1 1 d . . .
H54 H 0.0228 0.5589 0.1520 0.045 Uiso 1 1 calc R . .
C55 C -0.0261(4) 0.5762(4) 0.2416(3) 0.0280(13) Uani 1 1 d . . .
H55 H -0.0253 0.5140 0.2535 0.034 Uiso 1 1 calc R . .
C56 C -0.0557(4) 0.6386(4) 0.2847(3) 0.0239(13) Uani 1 1 d . . .
H56 H -0.0771 0.6180 0.3257 0.029 Uiso 1 1 calc R . .
C57 C -0.0552(4) 0.7320(4) 0.2695(3) 0.0226(12) Uani 1 1 d . . .
C58 C -0.0926(4) 0.7973(4) 0.3168(3) 0.0272(13) Uani 1 1 d . . .
H58 H -0.0753 0.8646 0.3007 0.033 Uiso 1 1 calc R . .
C59 C -0.0346(5) 0.8219(5) 0.3890(3) 0.0453(17) Uani 1 1 d . . .
H59A H -0.0497 0.7574 0.4065 0.068 Uiso 1 1 calc R . .
H59B H -0.0599 0.8662 0.4170 0.068 Uiso 1 1 calc R . .
H59C H 0.0432 0.8580 0.3901 0.068 Uiso 1 1 calc R . .
C60 C -0.2136(4) 0.7469(5) 0.3137(3) 0.0343(14) Uani 1 1 d . . .
H60A H -0.2491 0.7282 0.2664 0.052 Uiso 1 1 calc R . .
H60B H -0.2373 0.7955 0.3386 0.052 Uiso 1 1 calc R . .
H60C H -0.2326 0.6844 0.3339 0.052 Uiso 1 1 calc R . .
C61 C 0.0251(6) 0.7162(5) 0.0919(4) 0.0521(19) Uani 1 1 d . . .
H61 H 0.0228 0.7844 0.0874 0.062 Uiso 1 1 calc R . .
C62 C 0.1362(7) 0.7225(7) 0.0822(5) 0.085(3) Uani 1 1 d . . .
H62A H 0.1365 0.6535 0.0795 0.128 Uiso 1 1 calc R . .
H62B H 0.1898 0.7698 0.1205 0.128 Uiso 1 1 calc R . .
H62C H 0.1539 0.7484 0.0403 0.128 Uiso 1 1 calc R . .
C63 C -0.0601(7) 0.6328(7) 0.0363(4) 0.072(2) Uani 1 1 d . . .
H63A H -0.0592 0.5652 0.0400 0.108 Uiso 1 1 calc R . .
H63B H -0.0441 0.6493 -0.0081 0.108 Uiso 1 1 calc R . .
H63C H -0.1316 0.6305 0.0414 0.108 Uiso 1 1 calc R . .
C64 C 0.0495(4) 1.1373(4) 0.2168(3) 0.0205(12) Uani 1 1 d . . .
C65 C 0.0480(4) 1.1844(4) 0.2815(3) 0.0242(13) Uani 1 1 d . . .
C66 C 0.0894(4) 1.2932(4) 0.2946(3) 0.0281(13) Uani 1 1 d . . .
H66 H 0.0901 1.3279 0.3380 0.034 Uiso 1 1 calc R . .
C67 C 0.1288(4) 1.3503(4) 0.2458(3) 0.0307(14) Uani 1 1 d . . .
H67 H 0.1564 1.4237 0.2559 0.037 Uiso 1 1 calc R . .
C68 C 0.1286(4) 1.3023(4) 0.1827(3) 0.0238(13) Uani 1 1 d . . .
H68 H 0.1548 1.3428 0.1494 0.029 Uiso 1 1 calc R . .
C69 C 0.0908(4) 1.1952(4) 0.1669(3) 0.0207(12) Uani 1 1 d . . .
C70 C 0.0900(4) 1.1417(4) 0.0967(3) 0.0262(13) Uani 1 1 d . . .
H70 H 0.0950 1.0744 0.1008 0.031 Uiso 1 1 calc R . .
C71 C 0.1841(4) 1.2057(5) 0.0634(3) 0.0355(15) Uani 1 1 d . . .
H71A H 0.1758 1.2684 0.0542 0.053 Uiso 1 1 calc R . .
H71B H 0.1843 1.1644 0.0210 0.053 Uiso 1 1 calc R . .
H71C H 0.2522 1.2252 0.0939 0.053 Uiso 1 1 calc R . .
C72 C -0.0157(4) 1.1188(5) 0.0496(3) 0.0355(15) Uani 1 1 d . . .
H72A H -0.0250 1.1834 0.0482 0.053 Uiso 1 1 calc R . .
H72B H -0.0766 1.0700 0.0667 0.053 Uiso 1 1 calc R . .
H72C H -0.0128 1.0886 0.0041 0.053 Uiso 1 1 calc R . .
C73 C 0.0027(4) 1.1226(5) 0.3352(3) 0.0320(14) Uani 1 1 d . . .
H73 H 0.0152 1.0577 0.3281 0.038 Uiso 1 1 calc R . .
C74 C -0.1184(5) 1.0919(6) 0.3284(4) 0.054(2) Uani 1 1 d . . .
H74A H -0.1326 1.1544 0.3358 0.081 Uiso 1 1 calc R . .
H74B H -0.1471 1.0490 0.3620 0.081 Uiso 1 1 calc R . .
H74C H -0.1535 1.0527 0.2829 0.081 Uiso 1 1 calc R . .
C75 C 0.0553(5) 1.1799(7) 0.4066(4) 0.063(2) Uani 1 1 d . . .
H75A H 0.1338 1.2107 0.4094 0.094 Uiso 1 1 calc R . .
H75B H 0.0357 1.1312 0.4382 0.094 Uiso 1 1 calc R . .
H75C H 0.0303 1.2346 0.4184 0.094 Uiso 1 1 calc R . .
C76 C -0.0968(5) 0.9644(4) 0.1717(3) 0.0290(14) Uani 1 1 d . . .
H76 H -0.134(5) 0.992(5) 0.156(3) 0.040(19) Uiso 1 1 d . . .
C77 C -0.1145(5) 0.8647(5) 0.1666(3) 0.0314(15) Uani 1 1 d . . .
H77 H -0.173(5) 0.816(5) 0.147(3) 0.05(2) Uiso 1 1 d . . .
C78 C 0.2963(9) 0.5623(9) 0.1412(7) 0.127(4) Uani 1 1 d DU . .
H78A H 0.2652 0.5563 0.0942 0.191 Uiso 1 1 calc R . .
H78B H 0.2435 0.5623 0.1705 0.191 Uiso 1 1 calc R . .
H78C H 0.3154 0.5035 0.1455 0.191 Uiso 1 1 calc R . .
C79 C 0.3964(12) 0.6622(11) 0.1618(7) 0.186(7) Uani 1 1 d DU . .
H79A H 0.3764 0.7208 0.1748 0.223 Uiso 1 1 calc R . .
H79B H 0.4435 0.6576 0.2007 0.223 Uiso 1 1 calc R . .
C80 C 0.4537(8) 0.6780(7) 0.1022(7) 0.124(5) Uani 1 1 d D . .
H80A H 0.4096 0.6912 0.0654 0.149 Uiso 1 1 calc R . .
H80B H 0.4636 0.6145 0.0853 0.149 Uiso 1 1 calc R . .
C81 C 0.5635(7) 0.7694(7) 0.1218(4) 0.079(3) Uani 1 1 d D . .
H81A H 0.5544 0.8327 0.1401 0.094 Uiso 1 1 calc R . .
H81B H 0.6092 0.7553 0.1571 0.094 Uiso 1 1 calc R . .
C82 C 0.6160(7) 0.7849(8) 0.0599(4) 0.094(3) Uani 1 1 d D . .
H82A H 0.6351 0.7266 0.0463 0.141 Uiso 1 1 calc R . .
H82B H 0.6813 0.8495 0.0699 0.141 Uiso 1 1 calc R . .
H82C H 0.5657 0.7887 0.0231 0.141 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
Bi1 N1 2.259(4) . ?
Bi1 Bi2 2.8183(3) . ?
Si1 N1 1.724(4) . ?
Si1 C46 1.875(5) . ?
Si1 C34 1.877(5) . ?
Si1 C40 1.890(5) . ?
N1 C1 1.417(6) . ?
C1 C6 1.416(7) . ?
C1 C2 1.424(7) . ?
B1 N2 1.422(7) . ?
B1 N3 1.433(7) . ?
B1 Bi2 2.348(6) . ?
N2 C76 1.395(7) . ?
N2 C64 1.446(6) . ?
C2 C3 1.401(7) . ?
C2 C20 1.525(7) . ?
N3 C77 1.388(7) . ?
N3 C52 1.442(7) . ?
C3 C4 1.376(7) . ?
C4 C5 1.386(7) . ?
C4 C33 1.518(7) . ?
C5 C6 1.391(7) . ?
C6 C7 1.530(7) . ?
C7 C14 1.527(6) . ?
C7 C8 1.530(6) . ?
C8 C13 1.382(7) . ?
C8 C9 1.399(7) . ?
C9 C10 1.385(7) . ?
C10 C11 1.384(8) . ?
C11 C12 1.366(8) . ?
C12 C13 1.386(7) . ?
C14 C15 1.379(7) . ?
C14 C19 1.384(7) . ?
C15 C16 1.387(7) . ?
C16 C17 1.388(8) . ?
C17 C18 1.369(8) . ?
C18 C19 1.387(7) . ?
C20 C27 1.527(6) . ?
C20 C21 1.539(6) . ?
C21 C22 1.390(7) . ?
C21 C26 1.391(7) . ?
C22 C23 1.390(7) . ?
C23 C24 1.375(8) . ?
C24 C25 1.379(7) . ?
C25 C26 1.382(7) . ?
C27 C32 1.381(7) . ?
C27 C28 1.383(7) . ?
C28 C29 1.388(8) . ?
C29 C30 1.364(9) . ?
C30 C31 1.357(8) . ?
C31 C32 1.390(7) . ?
C34 C35 1.390(7) . ?
C34 C39 1.396(7) . ?
C35 C36 1.396(8) . ?
C36 C37 1.383(9) . ?
C37 C38 1.354(8) . ?
C38 C39 1.401(7) . ?
C40 C41 1.398(7) . ?
C40 C45 1.399(7) . ?
C41 C42 1.374(7) . ?
C42 C43 1.385(7) . ?
C43 C44 1.366(8) . ?
C44 C45 1.387(7) . ?
C46 C47 1.370(8) . ?
C46 C51 1.390(8) . ?
C47 C48 1.370(9) . ?
C48 C49 1.338(9) . ?
C49 C50 1.346(9) . ?
C50 C51 1.385(9) . ?
C52 C53 1.399(8) . ?
C52 C57 1.413(8) . ?
C53 C54 1.400(8) . ?
C53 C61 1.523(9) . ?
C54 C55 1.372(8) . ?
C55 C56 1.370(8) . ?
C56 C57 1.399(7) . ?
C57 C58 1.514(8) . ?
C58 C60 1.513(7) . ?
C58 C59 1.517(8) . ?
C61 C62 1.518(10) . ?
C61 C63 1.534(10) . ?
C64 C65 1.401(8) . ?
C64 C69 1.405(7) . ?
C65 C66 1.406(8) . ?
C65 C73 1.512(7) . ?
C66 C67 1.376(8) . ?
C67 C68 1.371(8) . ?
C68 C69 1.389(7) . ?
C69 C70 1.523(8) . ?
C70 C71 1.533(7) . ?
C70 C72 1.540(8) . ?
C73 C75 1.520(9) . ?
C73 C74 1.523(8) . ?
C76 C77 1.333(8) . ?
C78 C79 1.512(7) . ?
C79 C80 1.497(8) . ?
C80 C81 1.526(7) . ?
C81 C82 1.504(7) . ?

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
N1 Bi1 Bi2 99.82(10) . . ?
N1 Si1 C46 107.1(2) . . ?
N1 Si1 C34 109.9(2) . . ?
C46 Si1 C34 112.3(2) . . ?
N1 Si1 C40 116.0(2) . . ?
C46 Si1 C40 103.9(2) . . ?
C34 Si1 C40 107.5(2) . . ?
C1 N1 Si1 128.5(3) . . ?
C1 N1 Bi1 117.2(3) . . ?
Si1 N1 Bi1 113.86(19) . . ?
C6 C1 N1 120.2(4) . . ?
C6 C1 C2 118.1(4) . . ?
N1 C1 C2 121.5(4) . . ?
N2 B1 N3 105.0(4) . . ?
N2 B1 Bi2 134.1(4) . . ?
N3 B1 Bi2 120.8(4) . . ?
B1 Bi2 Bi1 92.24(15) . . ?
C76 N2 B1 108.0(4) . . ?
C76 N2 C64 121.2(4) . . ?
B1 N2 C64 130.7(4) . . ?
C3 C2 C1 119.0(4) . . ?
C3 C2 C20 119.8(4) . . ?
C1 C2 C20 121.1(4) . . ?
C77 N3 B1 107.9(5) . . ?
C77 N3 C52 121.1(4) . . ?
B1 N3 C52 129.4(5) . . ?
C4 C3 C2 123.0(5) . . ?
C3 C4 C5 117.3(5) . . ?
C3 C4 C33 121.1(5) . . ?
C5 C4 C33 121.6(4) . . ?
C4 C5 C6 122.7(5) . . ?
C5 C6 C1 119.7(4) . . ?
C5 C6 C7 119.0(4) . . ?
C1 C6 C7 121.3(4) . . ?
C14 C7 C8 111.7(4) . . ?
C14 C7 C6 113.0(4) . . ?
C8 C7 C6 111.9(4) . . ?
C13 C8 C9 117.7(4) . . ?
C13 C8 C7 123.0(4) . . ?
C9 C8 C7 119.1(4) . . ?
C10 C9 C8 120.5(5) . . ?
C11 C10 C9 120.6(5) . . ?
C12 C11 C10 119.2(5) . . ?
C11 C12 C13 120.5(5) . . ?
C8 C13 C12 121.4(5) . . ?
C15 C14 C19 117.9(4) . . ?
C15 C14 C7 119.9(4) . . ?
C19 C14 C7 121.9(5) . . ?
C14 C15 C16 121.4(5) . . ?
C15 C16 C17 119.6(5) . . ?
C18 C17 C16 119.5(5) . . ?
C17 C18 C19 120.2(5) . . ?
C14 C19 C18 121.2(5) . . ?
C2 C20 C27 114.8(4) . . ?
C2 C20 C21 113.4(4) . . ?
C27 C20 C21 109.8(4) . . ?
C22 C21 C26 118.2(4) . . ?
C22 C21 C20 117.6(4) . . ?
C26 C21 C20 124.2(4) . . ?
C21 C22 C23 120.8(5) . . ?
C24 C23 C22 120.4(5) . . ?
C23 C24 C25 119.2(5) . . ?
C24 C25 C26 120.9(5) . . ?
C25 C26 C21 120.6(5) . . ?
C32 C27 C28 117.7(5) . . ?
C32 C27 C20 123.4(5) . . ?
C28 C27 C20 118.8(5) . . ?
C27 C28 C29 120.3(6) . . ?
C30 C29 C28 121.1(6) . . ?
C31 C30 C29 119.3(5) . . ?
C30 C31 C32 120.4(6) . . ?
C27 C32 C31 121.2(5) . . ?
C35 C34 C39 117.2(5) . . ?
C35 C34 Si1 123.7(4) . . ?
C39 C34 Si1 119.1(4) . . ?
C34 C35 C36 121.1(5) . . ?
C37 C36 C35 120.0(5) . . ?
C38 C37 C36 120.3(5) . . ?
C37 C38 C39 119.9(5) . . ?
C34 C39 C38 121.5(5) . . ?
C41 C40 C45 116.2(5) . . ?
C41 C40 Si1 122.1(4) . . ?
C45 C40 Si1 121.5(4) . . ?
C42 C41 C40 122.1(5) . . ?
C41 C42 C43 120.0(5) . . ?
C44 C43 C42 119.6(5) . . ?
C43 C44 C45 120.2(5) . . ?
C44 C45 C40 121.7(5) . . ?
C47 C46 C51 114.8(5) . . ?
C47 C46 Si1 122.3(4) . . ?
C51 C46 Si1 122.7(4) . . ?
C46 C47 C48 122.8(6) . . ?
C49 C48 C47 121.2(6) . . ?
C48 C49 C50 118.5(6) . . ?
C49 C50 C51 121.0(6) . . ?
C50 C51 C46 121.6(6) . . ?
C53 C52 C57 122.3(5) . . ?
C53 C52 N3 120.9(5) . . ?
C57 C52 N3 116.8(5) . . ?
C52 C53 C54 117.0(5) . . ?
C52 C53 C61 123.0(5) . . ?
C54 C53 C61 119.9(6) . . ?
C55 C54 C53 121.7(6) . . ?
C56 C55 C54 120.2(5) . . ?
C55 C56 C57 121.5(5) . . ?
C56 C57 C52 117.1(5) . . ?
C56 C57 C58 120.2(5) . . ?
C52 C57 C58 122.6(5) . . ?
C60 C58 C57 111.0(4) . . ?
C60 C58 C59 110.9(5) . . ?
C57 C58 C59 112.8(5) . . ?
C62 C61 C53 110.8(6) . . ?
C62 C61 C63 109.4(7) . . ?
C53 C61 C63 111.4(5) . . ?
C65 C64 C69 122.1(5) . . ?
C65 C64 N2 118.8(4) . . ?
C69 C64 N2 119.1(5) . . ?
C64 C65 C66 117.0(5) . . ?
C64 C65 C73 122.4(5) . . ?
C66 C65 C73 120.6(5) . . ?
C67 C66 C65 121.2(5) . . ?
C68 C67 C66 120.6(5) . . ?
C67 C68 C69 121.0(5) . . ?
C68 C69 C64 118.0(5) . . ?
C68 C69 C70 121.1(5) . . ?
C64 C69 C70 120.9(5) . . ?
C69 C70 C71 113.1(4) . . ?
C69 C70 C72 110.6(5) . . ?
C71 C70 C72 107.9(5) . . ?
C65 C73 C75 113.3(5) . . ?
C65 C73 C74 110.5(5) . . ?
C75 C73 C74 108.8(6) . . ?
C77 C76 N2 109.5(5) . . ?
C76 C77 N3 109.6(5) . . ?
C80 C79 C78 107.2(10) . . ?
C79 C80 C81 110.3(10) . . ?
C82 C81 C80 108.4(8) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.50
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         2.456
_refine_diff_density_min         -1.732
_refine_diff_density_rms         0.126
####################################################################### 
# 
# 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_compound3a
_database_code_depnum_ccdc_archive 'CCDC 1051448'
_audit_update_record             
;
2015-02-27 deposited with the CCDC.
2015-03-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C63.50 H73.50 As B N3 Si'
_chemical_formula_weight         992.57

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'
As As 0.0499 2.0058 '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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.3574(10)
_cell_length_b                   12.6670(10)
_cell_length_c                   19.7946(18)
_cell_angle_alpha                99.963(7)
_cell_angle_beta                 104.228(7)
_cell_angle_gamma                100.574(7)
_cell_volume                     2874.0(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.147
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1055
_exptl_absorpt_coefficient_mu    0.652
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.906
_exptl_absorpt_correction_T_max  0.937
_exptl_absorpt_process_details   'Sortav (Blessing)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Apex X8'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            22745
_diffrn_reflns_av_R_equivalents  0.1102
_diffrn_reflns_av_sigmaI/netI    0.2025
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.96
_diffrn_reflns_theta_max         25.20
_reflns_number_total             10322
_reflns_number_gt                5036
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger.
 A half molecule of hexane of crystallisation was located in the asymmetric
 unit and its carbon atoms refined isotropically with an occupancy of 50%. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1443P)²+1.8747P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         10322
_refine_ls_number_parameters     649
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.1896
_refine_ls_R_factor_gt           0.1023
_refine_ls_wR_factor_ref         0.3149
_refine_ls_wR_factor_gt          0.2540
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_restrained_S_all      1.035
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
As1 As 0.66487(7) 0.68868(6) 0.74661(4) 0.0370(3) Uani 1 1 d D . .
Si1 Si 0.50221(18) 0.66693(17) 0.85384(12) 0.0346(5) Uani 1 1 d . . .
N1 N 0.9066(5) 0.7654(5) 0.8292(3) 0.0337(15) Uani 1 1 d . . .
C1 C 1.0013(8) 0.7464(7) 0.8759(5) 0.041(2) Uani 1 1 d . . .
B1 B 0.8026(8) 0.6863(6) 0.8278(5) 0.032(2) Uani 1 1 d . . .
H1 H 1.055(7) 0.780(6) 0.879(4) 0.03(3) Uiso 1 1 d . . .
N2 N 0.8482(5) 0.6202(5) 0.8761(3) 0.0333(15) Uani 1 1 d . . .
C2 C 0.9669(7) 0.6601(6) 0.9031(5) 0.0383(19) Uani 1 1 d . . .
H2 H 1.007(8) 0.637(8) 0.949(5) 0.08(3) Uiso 1 1 d . . .
N3 N 0.5264(5) 0.6719(4) 0.7712(3) 0.0266(13) Uani 1 1 d . . .
C3 C 0.9192(6) 0.8399(6) 0.7821(4) 0.0338(18) Uani 1 1 d . . .
C4 C 0.9306(6) 0.7967(6) 0.7157(4) 0.0370(19) Uani 1 1 d . . .
C5 C 0.9444(7) 0.8681(7) 0.6695(5) 0.047(2) Uani 1 1 d . . .
C6 C 0.9477(7) 0.9813(7) 0.6931(5) 0.052(2) Uani 1 1 d . . .
C7 C 0.9322(7) 1.0218(6) 0.7603(5) 0.044(2) Uani 1 1 d . . .
C8 C 0.9180(6) 0.9501(6) 0.8072(4) 0.0369(19) Uani 1 1 d . . .
C9 C 0.9086(7) 0.9972(6) 0.8795(4) 0.041(2) Uani 1 1 d . . .
H9 H 0.8803 0.9340 0.8997 0.049 Uiso 1 1 calc R . .
C10 C 0.8207(8) 1.0692(8) 0.8750(5) 0.063(3) Uani 1 1 d . . .
H10A H 0.8480 1.1339 0.8574 0.095 Uiso 1 1 calc R . .
H10B H 0.8115 1.0932 0.9226 0.095 Uiso 1 1 calc R . .
H10C H 0.7467 1.0263 0.8420 0.095 Uiso 1 1 calc R . .
C11 C 1.0247(7) 1.0608(6) 0.9300(4) 0.044(2) Uani 1 1 d . . .
H11A H 1.0756 1.0104 0.9375 0.066 Uiso 1 1 calc R . .
H11B H 1.0150 1.0942 0.9760 0.066 Uiso 1 1 calc R . .
H11C H 1.0583 1.1189 0.9093 0.066 Uiso 1 1 calc R . .
C12 C 0.9310(7) 0.6774(6) 0.6907(5) 0.044(2) Uani 1 1 d . . .
H12 H 0.9021 0.6365 0.7241 0.053 Uiso 1 1 calc R . .
C13 C 0.8507(8) 0.6251(7) 0.6161(5) 0.055(2) Uani 1 1 d . . .
H13A H 0.7742 0.6379 0.6137 0.083 Uiso 1 1 calc R . .
H13B H 0.8456 0.5455 0.6053 0.083 Uiso 1 1 calc R . .
H13C H 0.8805 0.6580 0.5810 0.083 Uiso 1 1 calc R . .
C14 C 1.0531(7) 0.6627(7) 0.6961(5) 0.056(3) Uani 1 1 d . . .
H14A H 1.0841 0.7007 0.6633 0.084 Uiso 1 1 calc R . .
H14B H 1.0511 0.5840 0.6831 0.084 Uiso 1 1 calc R . .
H14C H 1.1021 0.6942 0.7452 0.084 Uiso 1 1 calc R . .
C15 C 0.7945(6) 0.5200(6) 0.8913(4) 0.0363(19) Uani 1 1 d . . .
C16 C 0.7909(7) 0.5230(6) 0.9621(4) 0.0377(19) Uani 1 1 d . . .
C17 C 0.7446(8) 0.4211(7) 0.9767(5) 0.051(2) Uani 1 1 d . . .
H17 H 0.7410 0.4188 1.0239 0.061 Uiso 1 1 calc R . .
C18 C 0.7048(7) 0.3255(6) 0.9237(5) 0.052(2) Uani 1 1 d . . .
H18 H 0.6740 0.2585 0.9349 0.062 Uiso 1 1 calc R . .
C19 C 0.7090(7) 0.3254(6) 0.8555(5) 0.045(2) Uani 1 1 d . . .
H19 H 0.6783 0.2588 0.8196 0.054 Uiso 1 1 calc R . .
C20 C 0.7574(7) 0.4212(6) 0.8373(5) 0.039(2) Uani 1 1 d . . .
C21 C 0.7697(7) 0.4168(6) 0.7634(5) 0.044(2) Uani 1 1 d . . .
H21 H 0.7463 0.4824 0.7480 0.053 Uiso 1 1 calc R . .
C22 C 0.8956(8) 0.4250(7) 0.7616(5) 0.056(3) Uani 1 1 d . . .
H22A H 0.9453 0.4921 0.7957 0.084 Uiso 1 1 calc R . .
H22B H 0.9006 0.4278 0.7133 0.084 Uiso 1 1 calc R . .
H22C H 0.9205 0.3604 0.7748 0.084 Uiso 1 1 calc R . .
C23 C 0.6964(8) 0.3164(7) 0.7079(5) 0.067(3) Uani 1 1 d . . .
H23A H 0.7232 0.2511 0.7183 0.101 Uiso 1 1 calc R . .
H23B H 0.7019 0.3249 0.6605 0.101 Uiso 1 1 calc R . .
H23C H 0.6163 0.3075 0.7087 0.101 Uiso 1 1 calc R . .
C24 C 0.8314(7) 0.6255(6) 1.0215(4) 0.043(2) Uani 1 1 d . . .
H24 H 0.8482 0.6897 0.9995 0.051 Uiso 1 1 calc R . .
C25 C 0.7401(8) 0.6437(7) 1.0593(5) 0.049(2) Uani 1 1 d . . .
H25A H 0.6662 0.6338 1.0236 0.074 Uiso 1 1 calc R . .
H25B H 0.7629 0.7188 1.0894 0.074 Uiso 1 1 calc R . .
H25C H 0.7328 0.5904 1.0893 0.074 Uiso 1 1 calc R . .
C26 C 0.9421(7) 0.6245(7) 1.0754(5) 0.053(2) Uani 1 1 d . . .
H26A H 0.9288 0.5618 1.0976 0.079 Uiso 1 1 calc R . .
H26B H 0.9676 0.6934 1.1124 0.079 Uiso 1 1 calc R . .
H26C H 1.0014 0.6178 1.0510 0.079 Uiso 1 1 calc R . .
C27 C 0.4346(6) 0.6659(6) 0.7079(4) 0.0290(17) Uani 1 1 d . . .
C28 C 0.3724(6) 0.5646(5) 0.6608(4) 0.0287(17) Uani 1 1 d . . .
C29 C 0.2843(6) 0.5637(6) 0.6017(4) 0.0300(17) Uani 1 1 d . . .
H29 H 0.2433 0.4947 0.5701 0.036 Uiso 1 1 calc R . .
C30 C 0.2533(7) 0.6579(6) 0.5863(4) 0.0365(19) Uani 1 1 d . . .
C31 C 0.3188(6) 0.7576(6) 0.6309(4) 0.0374(19) Uani 1 1 d . . .
H31 H 0.3019 0.8236 0.6193 0.045 Uiso 1 1 calc R . .
C32 C 0.4073(6) 0.7667(6) 0.6914(4) 0.0304(17) Uani 1 1 d . . .
C33 C 0.4760(6) 0.8806(6) 0.7369(4) 0.0320(18) Uani 1 1 d . . .
H33 H 0.5478 0.8692 0.7681 0.038 Uiso 1 1 calc R . .
C34 C 0.4157(6) 0.9352(5) 0.7870(4) 0.0349(19) Uani 1 1 d . . .
C35 C 0.2953(6) 0.9186(6) 0.7724(4) 0.0345(18) Uani 1 1 d . . .
H35 H 0.2471 0.8716 0.7284 0.041 Uiso 1 1 calc R . .
C36 C 0.2464(7) 0.9685(6) 0.8201(4) 0.039(2) Uani 1 1 d . . .
H36 H 0.1651 0.9554 0.8090 0.047 Uiso 1 1 calc R . .
C37 C 0.3135(7) 1.0372(7) 0.8835(5) 0.050(2) Uani 1 1 d . . .
H37 H 0.2789 1.0716 0.9164 0.059 Uiso 1 1 calc R . .
C38 C 0.4315(7) 1.0564(7) 0.8998(5) 0.055(3) Uani 1 1 d . . .
H38 H 0.4780 1.1042 0.9439 0.066 Uiso 1 1 calc R . .
C39 C 0.4827(7) 1.0063(6) 0.8522(5) 0.048(2) Uani 1 1 d . . .
H39 H 0.5641 1.0205 0.8640 0.057 Uiso 1 1 calc R . .
C40 C 0.5137(7) 0.9550(5) 0.6895(4) 0.0351(19) Uani 1 1 d . . .
C41 C 0.4488(7) 1.0244(6) 0.6621(5) 0.045(2) Uani 1 1 d . . .
H41 H 0.3824 1.0323 0.6767 0.053 Uiso 1 1 calc R . .
C42 C 0.4795(8) 1.0823(6) 0.6137(5) 0.051(2) Uani 1 1 d . . .
H42 H 0.4333 1.1286 0.5948 0.061 Uiso 1 1 calc R . .
C43 C 0.5775(8) 1.0732(6) 0.5924(5) 0.047(2) Uani 1 1 d . . .
H43 H 0.5974 1.1106 0.5580 0.057 Uiso 1 1 calc R . .
C44 C 0.6444(7) 1.0090(6) 0.6225(5) 0.044(2) Uani 1 1 d . . .
H44 H 0.7138 1.0054 0.6106 0.053 Uiso 1 1 calc R . .
C45 C 0.6139(7) 0.9498(6) 0.6694(5) 0.042(2) Uani 1 1 d . . .
H45 H 0.6613 0.9046 0.6885 0.051 Uiso 1 1 calc R . .
C46 C 0.4063(7) 0.4568(5) 0.6706(4) 0.0319(17) Uani 1 1 d . . .
H46 H 0.4826 0.4777 0.7078 0.038 Uiso 1 1 calc R . .
C47 C 0.3245(7) 0.3809(6) 0.6983(4) 0.0368(19) Uani 1 1 d . . .
C48 C 0.2175(8) 0.3940(7) 0.7004(5) 0.057(3) Uani 1 1 d . . .
H48 H 0.1907 0.4539 0.6850 0.068 Uiso 1 1 calc R . .
C49 C 0.1487(9) 0.3195(8) 0.7251(6) 0.069(3) Uani 1 1 d . . .
H49 H 0.0739 0.3279 0.7250 0.083 Uiso 1 1 calc R . .
C50 C 0.1862(8) 0.2341(7) 0.7497(5) 0.058(3) Uani 1 1 d . . .
H50 H 0.1385 0.1841 0.7671 0.070 Uiso 1 1 calc R . .
C51 C 0.2941(8) 0.2221(7) 0.7487(5) 0.050(2) Uani 1 1 d . . .
H51 H 0.3222 0.1638 0.7658 0.060 Uiso 1 1 calc R . .
C52 C 0.3603(7) 0.2936(6) 0.7233(5) 0.045(2) Uani 1 1 d . . .
H52 H 0.4344 0.2836 0.7226 0.054 Uiso 1 1 calc R . .
C53 C 0.4249(7) 0.3987(6) 0.6023(4) 0.0345(18) Uani 1 1 d . . .
C54 C 0.5274(7) 0.4337(7) 0.5865(4) 0.044(2) Uani 1 1 d . . .
H54 H 0.5853 0.4926 0.6196 0.052 Uiso 1 1 calc R . .
C55 C 0.5477(8) 0.3854(7) 0.5239(4) 0.047(2) Uani 1 1 d . . .
H55 H 0.6181 0.4128 0.5146 0.056 Uiso 1 1 calc R . .
C56 C 0.4694(8) 0.3003(7) 0.4761(5) 0.050(2) Uani 1 1 d . . .
H56 H 0.4844 0.2666 0.4337 0.060 Uiso 1 1 calc R . .
C57 C 0.3654(8) 0.2623(7) 0.4902(5) 0.053(2) Uani 1 1 d . . .
H57 H 0.3090 0.2026 0.4567 0.064 Uiso 1 1 calc R . .
C58 C 0.3430(7) 0.3113(6) 0.5535(4) 0.0358(19) Uani 1 1 d . . .
H58 H 0.2721 0.2846 0.5626 0.043 Uiso 1 1 calc R . .
C59 C 0.1571(7) 0.6533(7) 0.5211(4) 0.048(2) Uani 1 1 d . . .
H59A H 0.1893 0.6696 0.4824 0.072 Uiso 1 1 calc R . .
H59B H 0.1139 0.7080 0.5329 0.072 Uiso 1 1 calc R . .
H59C H 0.1056 0.5795 0.5055 0.072 Uiso 1 1 calc R . .
C60 C 0.3562(7) 0.6885(7) 0.8523(5) 0.050(2) Uani 1 1 d . . .
H60A H 0.3528 0.7631 0.8463 0.074 Uiso 1 1 calc R . .
H60B H 0.3407 0.6794 0.8974 0.074 Uiso 1 1 calc R . .
H60C H 0.2985 0.6343 0.8124 0.074 Uiso 1 1 calc R . .
C61 C 0.6152(7) 0.7792(6) 0.9230(4) 0.041(2) Uani 1 1 d . . .
H61A H 0.6913 0.7666 0.9235 0.062 Uiso 1 1 calc R . .
H61B H 0.6036 0.7790 0.9702 0.062 Uiso 1 1 calc R . .
H61C H 0.6099 0.8506 0.9115 0.062 Uiso 1 1 calc R . .
C62 C 0.5024(7) 0.5296(6) 0.8749(5) 0.043(2) Uani 1 1 d . . .
H62A H 0.4339 0.4754 0.8430 0.065 Uiso 1 1 calc R . .
H62B H 0.5019 0.5339 0.9247 0.065 Uiso 1 1 calc R . .
H62C H 0.5714 0.5071 0.8680 0.065 Uiso 1 1 calc R . .
C63 C 1.1816(16) 0.9390(18) 0.5013(11) 0.094(8) Uiso 0.50 1 d PD . .
H63A H 1.1085 0.8899 0.4710 0.141 Uiso 0.50 1 calc PR . .
H63B H 1.2292 0.8959 0.5265 0.141 Uiso 0.50 1 calc PR . .
H63C H 1.2219 0.9748 0.4713 0.141 Uiso 0.50 1 calc PR . .
C64 C 1.1588(8) 1.0255(17) 0.5549(9) 0.095(8) Uiso 0.50 1 d PD . .
H64A H 1.2191 1.0943 0.5657 0.114 Uiso 0.50 1 calc PR . .
H64B H 1.1636 1.0002 0.6000 0.114 Uiso 0.50 1 calc PR . .
C65 C 1.0417(7) 1.0498(8) 0.5285(7) 0.053(5) Uiso 0.50 1 d PD . .
H65A H 1.0499 1.1154 0.5076 0.064 Uiso 0.50 1 calc PR . .
H65B H 1.0098 1.0665 0.5693 0.064 Uiso 0.50 1 calc PR . .
H1A H 0.634(7) 0.669(7) 0.6733(5) 0.064 Uiso 1 1 d D . .


_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
As1 N3 1.877(6) . ?
As1 B1 2.042(9) . ?
Si1 N3 1.743(6) . ?
Si1 C62 1.858(8) . ?
Si1 C60 1.867(8) . ?
Si1 C61 1.872(8) . ?
N1 C1 1.390(10) . ?
N1 C3 1.450(9) . ?
N1 B1 1.468(10) . ?
C1 C2 1.347(12) . ?
B1 N2 1.455(10) . ?
N2 C2 1.393(9) . ?
N2 C15 1.437(9) . ?
N3 C27 1.449(9) . ?
C3 C4 1.386(10) . ?
C3 C8 1.402(10) . ?
C4 C5 1.411(11) . ?
C4 C12 1.508(10) . ?
C5 C6 1.419(12) . ?
C6 C7 1.413(12) . ?
C7 C8 1.425(11) . ?
C8 C9 1.493(11) . ?
C9 C11 1.516(11) . ?
C9 C10 1.537(11) . ?
C12 C13 1.519(12) . ?
C12 C14 1.534(10) . ?
C15 C16 1.409(11) . ?
C15 C20 1.416(10) . ?
C16 C17 1.419(11) . ?
C16 C24 1.504(11) . ?
C17 C18 1.377(12) . ?
C18 C19 1.364(12) . ?
C19 C20 1.397(11) . ?
C20 C21 1.499(12) . ?
C21 C23 1.500(11) . ?
C21 C22 1.550(11) . ?
C24 C26 1.517(11) . ?
C24 C25 1.530(11) . ?
C27 C28 1.406(9) . ?
C27 C32 1.450(9) . ?
C28 C29 1.386(10) . ?
C28 C46 1.530(9) . ?
C29 C30 1.378(10) . ?
C30 C31 1.386(10) . ?
C30 C59 1.509(11) . ?
C31 C32 1.379(10) . ?
C32 C33 1.529(10) . ?
C33 C34 1.527(10) . ?
C33 C40 1.530(10) . ?
C34 C39 1.401(10) . ?
C34 C35 1.412(10) . ?
C35 C36 1.368(10) . ?
C36 C37 1.366(11) . ?
C37 C38 1.379(11) . ?
C38 C39 1.386(11) . ?
C40 C41 1.386(10) . ?
C40 C45 1.399(11) . ?
C41 C42 1.386(11) . ?
C42 C43 1.394(12) . ?
C43 C44 1.367(11) . ?
C44 C45 1.370(11) . ?
C46 C53 1.514(10) . ?
C46 C47 1.531(10) . ?
C47 C48 1.372(11) . ?
C47 C52 1.388(10) . ?
C48 C49 1.387(12) . ?
C49 C50 1.370(13) . ?
C50 C51 1.374(12) . ?
C51 C52 1.352(11) . ?
C53 C58 1.386(10) . ?
C53 C54 1.391(11) . ?
C54 C55 1.385(11) . ?
C55 C56 1.344(12) . ?
C56 C57 1.399(12) . ?
C57 C58 1.413(11) . ?
C63 C64 1.506(8) . ?
C64 C65 1.520(8) . ?
C65 C65 1.545(8) 2_776 ?

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
N3 As1 B1 113.6(3) . . ?
N3 Si1 C62 112.2(3) . . ?
N3 Si1 C60 110.0(3) . . ?
C62 Si1 C60 105.2(4) . . ?
N3 Si1 C61 107.5(3) . . ?
C62 Si1 C61 111.8(4) . . ?
C60 Si1 C61 110.3(4) . . ?
C1 N1 C3 121.7(7) . . ?
C1 N1 B1 109.2(7) . . ?
C3 N1 B1 128.2(6) . . ?
C2 C1 N1 109.3(8) . . ?
N2 B1 N1 102.5(6) . . ?
N2 B1 As1 143.8(6) . . ?
N1 B1 As1 111.5(5) . . ?
C2 N2 C15 119.3(6) . . ?
C2 N2 B1 109.1(6) . . ?
C15 N2 B1 131.1(6) . . ?
C1 C2 N2 109.9(7) . . ?
C27 N3 Si1 122.4(4) . . ?
C27 N3 As1 108.2(4) . . ?
Si1 N3 As1 129.4(3) . . ?
C4 C3 C8 124.9(7) . . ?
C4 C3 N1 117.6(6) . . ?
C8 C3 N1 117.4(7) . . ?
C3 C4 C5 118.5(7) . . ?
C3 C4 C12 123.2(7) . . ?
C5 C4 C12 118.3(7) . . ?
C4 C5 C6 118.9(8) . . ?
C7 C6 C5 121.1(8) . . ?
C6 C7 C8 120.3(7) . . ?
C3 C8 C7 116.3(7) . . ?
C3 C8 C9 124.9(7) . . ?
C7 C8 C9 118.8(7) . . ?
C8 C9 C11 111.4(6) . . ?
C8 C9 C10 111.6(7) . . ?
C11 C9 C10 111.1(7) . . ?
C4 C12 C13 112.8(7) . . ?
C4 C12 C14 111.5(7) . . ?
C13 C12 C14 111.2(7) . . ?
C16 C15 C20 122.7(7) . . ?
C16 C15 N2 117.5(7) . . ?
C20 C15 N2 119.5(7) . . ?
C15 C16 C17 116.4(7) . . ?
C15 C16 C24 124.5(7) . . ?
C17 C16 C24 119.2(8) . . ?
C18 C17 C16 121.1(9) . . ?
C19 C18 C17 121.1(8) . . ?
C18 C19 C20 121.4(8) . . ?
C19 C20 C15 117.2(8) . . ?
C19 C20 C21 120.2(7) . . ?
C15 C20 C21 122.6(7) . . ?
C20 C21 C23 115.0(8) . . ?
C20 C21 C22 112.3(7) . . ?
C23 C21 C22 107.5(7) . . ?
C16 C24 C26 111.5(6) . . ?
C16 C24 C25 112.5(7) . . ?
C26 C24 C25 110.3(7) . . ?
C28 C27 N3 121.8(6) . . ?
C28 C27 C32 118.8(7) . . ?
N3 C27 C32 119.5(6) . . ?
C29 C28 C27 119.2(6) . . ?
C29 C28 C46 119.5(6) . . ?
C27 C28 C46 121.1(6) . . ?
C30 C29 C28 123.2(6) . . ?
C29 C30 C31 117.0(7) . . ?
C29 C30 C59 121.6(7) . . ?
C31 C30 C59 121.3(7) . . ?
C32 C31 C30 123.8(7) . . ?
C31 C32 C27 117.8(6) . . ?
C31 C32 C33 120.1(6) . . ?
C27 C32 C33 122.1(6) . . ?
C34 C33 C32 114.0(6) . . ?
C34 C33 C40 112.4(5) . . ?
C32 C33 C40 110.5(6) . . ?
C39 C34 C35 116.8(7) . . ?
C39 C34 C33 118.8(7) . . ?
C35 C34 C33 124.3(7) . . ?
C36 C35 C34 121.5(7) . . ?
C37 C36 C35 120.6(7) . . ?
C36 C37 C38 119.8(8) . . ?
C37 C38 C39 120.5(8) . . ?
C38 C39 C34 120.7(8) . . ?
C41 C40 C45 117.7(8) . . ?
C41 C40 C33 122.3(7) . . ?
C45 C40 C33 119.8(6) . . ?
C42 C41 C40 120.8(8) . . ?
C41 C42 C43 120.5(8) . . ?
C44 C43 C42 118.3(8) . . ?
C43 C44 C45 121.6(8) . . ?
C44 C45 C40 120.8(7) . . ?
C53 C46 C28 109.9(6) . . ?
C53 C46 C47 112.4(6) . . ?
C28 C46 C47 114.4(6) . . ?
C48 C47 C52 117.5(8) . . ?
C48 C47 C46 124.1(7) . . ?
C52 C47 C46 118.4(7) . . ?
C47 C48 C49 119.8(8) . . ?
C50 C49 C48 121.6(9) . . ?
C49 C50 C51 118.6(9) . . ?
C52 C51 C50 119.8(8) . . ?
C51 C52 C47 122.7(8) . . ?
C58 C53 C54 117.6(7) . . ?
C58 C53 C46 122.7(7) . . ?
C54 C53 C46 119.7(7) . . ?
C55 C54 C53 122.1(8) . . ?
C56 C55 C54 121.1(9) . . ?
C55 C56 C57 118.6(8) . . ?
C56 C57 C58 121.0(8) . . ?
C53 C58 C57 119.6(8) . . ?
C63 C64 C65 112.6(7) . . ?
C64 C65 C65 110.6(7) . 2_776 ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.20
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         1.408
_refine_diff_density_min         -0.948
_refine_diff_density_rms         0.114
####################################################################### 
# 
# 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_compound3b
_database_code_depnum_ccdc_archive 'CCDC 1051449'
_audit_update_record             
;
2015-02-27 deposited with the CCDC.
2015-03-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C65.25 H80 As B N3 Si'
_chemical_formula_weight         1020.14

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'
As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.4034(7)
_cell_length_b                   13.3700(8)
_cell_length_c                   20.1020(12)
_cell_angle_alpha                77.434(5)
_cell_angle_beta                 77.587(5)
_cell_angle_gamma                65.731(6)
_cell_volume                     2936.5(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.154
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1089
_exptl_absorpt_coefficient_mu    0.640
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.804
_exptl_absorpt_correction_T_max  0.910
_exptl_absorpt_process_details   'Sortav (Blessing)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Apex X8'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            26319
_diffrn_reflns_av_R_equivalents  0.0357
_diffrn_reflns_av_sigmaI/netI    0.0506
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.96
_diffrn_reflns_theta_max         25.50
_reflns_number_total             10880
_reflns_number_gt                8557
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger.
 A molecule of pentane of crystallisation was located in the asymmetric unit
 and its carbon atoms refined isotropically, at 25% occupancy. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0692P)²+1.8426P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         10880
_refine_ls_number_parameters     678
_refine_ls_number_restraints     10
_refine_ls_R_factor_all          0.0694
_refine_ls_R_factor_gt           0.0492
_refine_ls_wR_factor_ref         0.1362
_refine_ls_wR_factor_gt          0.1240
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_restrained_S_all      1.062
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
As1 As 0.90705(2) 0.55193(2) 0.734037(15) 0.02472(10) Uani 1 1 d D . .
Si1 Si 1.03991(7) 0.67224(7) 0.79462(4) 0.02454(18) Uani 1 1 d . . .
N1 N 1.03519(18) 0.58594(18) 0.74148(11) 0.0200(5) Uani 1 1 d D . .
C1 C 1.1370(2) 0.5250(2) 0.69551(13) 0.0197(6) Uani 1 1 d . . .
B1 B 0.7469(3) 0.6372(3) 0.78859(16) 0.0232(7) Uani 1 1 d D . .
H1 H 0.9346(8) 0.4417(5) 0.7776(9) 0.028 Uiso 1 1 d D . .
N2 N 0.68024(19) 0.56814(19) 0.81797(12) 0.0243(5) Uani 1 1 d . . .
C2 C 1.1557(2) 0.5720(2) 0.62633(13) 0.0195(5) Uani 1 1 d . . .
N3 N 0.6602(2) 0.7488(2) 0.79457(13) 0.0288(5) Uani 1 1 d . . .
C3 C 1.2508(2) 0.5106(2) 0.58145(13) 0.0215(6) Uani 1 1 d . . .
H3 H 1.2630 0.5432 0.5350 0.026 Uiso 1 1 calc R . .
C4 C 1.3282(2) 0.4040(2) 0.60216(14) 0.0228(6) Uani 1 1 d . . .
C5 C 1.3068(2) 0.3577(2) 0.67053(14) 0.0242(6) Uani 1 1 d . . .
H5 H 1.3586 0.2845 0.6858 0.029 Uiso 1 1 calc R . .
C6 C 1.2121(2) 0.4151(2) 0.71716(13) 0.0213(6) Uani 1 1 d . . .
C7 C 1.0762(2) 0.6889(2) 0.59859(14) 0.0219(6) Uani 1 1 d . . .
H7 H 1.0029 0.7107 0.6335 0.026 Uiso 1 1 calc R . .
C8 C 1.1321(3) 0.7732(2) 0.59332(14) 0.0256(6) Uani 1 1 d . . .
C9 C 1.2455(3) 0.7444(3) 0.60805(16) 0.0314(7) Uani 1 1 d . . .
H9 H 1.2939 0.6684 0.6194 0.038 Uiso 1 1 calc R . .
C10 C 1.2904(3) 0.8245(3) 0.60660(18) 0.0441(8) Uani 1 1 d . . .
H10 H 1.3682 0.8025 0.6179 0.053 Uiso 1 1 calc R . .
C11 C 1.2241(4) 0.9344(3) 0.58916(19) 0.0502(10) Uani 1 1 d . . .
H11 H 1.2554 0.9889 0.5878 0.060 Uiso 1 1 calc R . .
C12 C 1.1110(4) 0.9647(3) 0.5736(2) 0.0574(11) Uani 1 1 d . . .
H12 H 1.0639 1.0407 0.5610 0.069 Uiso 1 1 calc R . .
C13 C 1.0658(3) 0.8848(3) 0.57609(19) 0.0456(9) Uani 1 1 d . . .
H13 H 0.9873 0.9072 0.5657 0.055 Uiso 1 1 calc R . .
C14 C 1.0337(2) 0.6903(2) 0.53188(14) 0.0249(6) Uani 1 1 d . . .
C15 C 1.0676(3) 0.7409(3) 0.46826(15) 0.0348(7) Uani 1 1 d . . .
H15 H 1.1229 0.7752 0.4636 0.042 Uiso 1 1 calc R . .
C16 C 1.0207(3) 0.7421(3) 0.41036(17) 0.0466(9) Uani 1 1 d . . .
H16 H 1.0436 0.7783 0.3668 0.056 Uiso 1 1 calc R . .
C17 C 0.9425(3) 0.6917(3) 0.41589(17) 0.0433(9) Uani 1 1 d . . .
H17 H 0.9102 0.6939 0.3766 0.052 Uiso 1 1 calc R . .
C18 C 0.9111(3) 0.6378(3) 0.47870(17) 0.0395(8) Uani 1 1 d . . .
H18 H 0.8583 0.6010 0.4828 0.047 Uiso 1 1 calc R . .
C19 C 0.9562(3) 0.6374(2) 0.53570(16) 0.0322(7) Uani 1 1 d . . .
H19 H 0.9337 0.5999 0.5788 0.039 Uiso 1 1 calc R . .
C20 C 1.1900(2) 0.3539(2) 0.78944(14) 0.0255(6) Uani 1 1 d . . .
H20 H 1.1048 0.3943 0.8083 0.031 Uiso 1 1 calc R . .
C21 C 1.2662(3) 0.3533(2) 0.84010(15) 0.0292(7) Uani 1 1 d . . .
C22 C 1.3828(3) 0.3476(3) 0.82119(15) 0.0324(7) Uani 1 1 d . . .
H22 H 1.4183 0.3441 0.7745 0.039 Uiso 1 1 calc R . .
C23 C 1.4485(3) 0.3471(3) 0.86919(17) 0.0430(9) Uani 1 1 d . . .
H23 H 1.5284 0.3424 0.8554 0.052 Uiso 1 1 calc R . .
C24 C 1.3974(3) 0.3534(4) 0.93702(18) 0.0585(11) Uani 1 1 d . . .
H24 H 1.4419 0.3533 0.9700 0.070 Uiso 1 1 calc R . .
C25 C 1.2814(3) 0.3599(4) 0.95673(18) 0.0613(12) Uani 1 1 d . . .
H25 H 1.2456 0.3653 1.0033 0.074 Uiso 1 1 calc R . .
C26 C 1.2171(3) 0.3585(3) 0.90894(16) 0.0447(9) Uani 1 1 d . . .
H26 H 1.1379 0.3611 0.9233 0.054 Uiso 1 1 calc R . .
C27 C 1.2024(3) 0.2371(2) 0.78386(15) 0.0304(7) Uani 1 1 d . . .
C28 C 1.3106(3) 0.1468(3) 0.7864(2) 0.0476(9) Uani 1 1 d . . .
H28 H 1.3764 0.1546 0.7985 0.057 Uiso 1 1 calc R . .
C29 C 1.3236(3) 0.0459(3) 0.7716(2) 0.0585(11) Uani 1 1 d . . .
H29 H 1.3990 -0.0142 0.7722 0.070 Uiso 1 1 calc R . .
C30 C 1.2286(4) 0.0317(3) 0.7560(2) 0.0521(10) Uani 1 1 d . . .
H30 H 1.2381 -0.0374 0.7451 0.063 Uiso 1 1 calc R . .
C31 C 1.1193(3) 0.1191(3) 0.75641(17) 0.0428(8) Uani 1 1 d . . .
H31 H 1.0521 0.1095 0.7477 0.051 Uiso 1 1 calc R . .
C32 C 1.1073(3) 0.2214(2) 0.76950(15) 0.0315(7) Uani 1 1 d . . .
H32 H 1.0320 0.2816 0.7685 0.038 Uiso 1 1 calc R . .
C33 C 1.4317(2) 0.3381(2) 0.55265(15) 0.0287(7) Uani 1 1 d . . .
H33 H 1.4214 0.3799 0.5052 0.034 Uiso 1 1 calc R . .
C34 C 1.5512(3) 0.3284(3) 0.56824(18) 0.0428(8) Uani 1 1 d . . .
H34A H 1.5509 0.4027 0.5651 0.064 Uiso 1 1 calc R . .
H34B H 1.6160 0.2877 0.5348 0.064 Uiso 1 1 calc R . .
H34C H 1.5634 0.2886 0.6148 0.064 Uiso 1 1 calc R . .
C35 C 1.4327(3) 0.2240(3) 0.55294(19) 0.0429(8) Uani 1 1 d . . .
H35A H 1.4474 0.1796 0.5982 0.064 Uiso 1 1 calc R . .
H35B H 1.4961 0.1871 0.5176 0.064 Uiso 1 1 calc R . .
H35C H 1.3553 0.2316 0.5433 0.064 Uiso 1 1 calc R . .
C36 C 1.1977(3) 0.6431(3) 0.80066(16) 0.0338(7) Uani 1 1 d . . .
H36A H 1.2340 0.5683 0.8254 0.051 Uiso 1 1 calc R . .
H36B H 1.2003 0.6974 0.8256 0.051 Uiso 1 1 calc R . .
H36C H 1.2420 0.6484 0.7543 0.051 Uiso 1 1 calc R . .
C37 C 0.9696(3) 0.8216(3) 0.76033(17) 0.0348(7) Uani 1 1 d . . .
H37A H 1.0234 0.8413 0.7213 0.052 Uiso 1 1 calc R . .
H37B H 0.9544 0.8663 0.7965 0.052 Uiso 1 1 calc R . .
H37C H 0.8940 0.8358 0.7451 0.052 Uiso 1 1 calc R . .
C38 C 0.9594(3) 0.6421(3) 0.88145(15) 0.0371(7) Uani 1 1 d . . .
H38A H 0.8752 0.6624 0.8781 0.056 Uiso 1 1 calc R . .
H38B H 0.9655 0.6852 0.9131 0.056 Uiso 1 1 calc R . .
H38C H 0.9954 0.5628 0.8987 0.056 Uiso 1 1 calc R . .
C39 C 0.7144(2) 0.4531(2) 0.81343(14) 0.0249(6) Uani 1 1 d . . .
C40 C 0.7562(3) 0.3724(3) 0.86869(15) 0.0320(7) Uani 1 1 d . . .
C41 C 0.7905(3) 0.2619(3) 0.86143(18) 0.0397(8) Uani 1 1 d . . .
H41 H 0.8201 0.2055 0.8984 0.048 Uiso 1 1 calc R . .
C42 C 0.7823(3) 0.2327(3) 0.80152(18) 0.0381(8) Uani 1 1 d . . .
H42 H 0.8065 0.1568 0.7973 0.046 Uiso 1 1 calc R . .
C43 C 0.7383(3) 0.3150(2) 0.74719(16) 0.0315(7) Uani 1 1 d . . .
H43 H 0.7325 0.2946 0.7061 0.038 Uiso 1 1 calc R . .
C44 C 0.7029(2) 0.4263(2) 0.75205(14) 0.0246(6) Uani 1 1 d . . .
C45 C 0.7664(3) 0.4035(3) 0.93506(17) 0.0430(8) Uani 1 1 d . . .
H45 H 0.7375 0.4862 0.9295 0.052 Uiso 1 1 calc R . .
C46 C 0.8956(4) 0.3563(5) 0.9473(2) 0.0757(15) Uani 1 1 d . . .
H46A H 0.9257 0.2751 0.9539 0.114 Uiso 1 1 calc R . .
H46B H 0.9010 0.3810 0.9885 0.114 Uiso 1 1 calc R . .
H46C H 0.9436 0.3821 0.9074 0.114 Uiso 1 1 calc R . .
C47 C 0.6893(5) 0.3668(5) 0.9965(2) 0.0855(17) Uani 1 1 d . . .
H47A H 0.6052 0.4044 0.9897 0.128 Uiso 1 1 calc R . .
H47B H 0.7005 0.3858 1.0383 0.128 Uiso 1 1 calc R . .
H47C H 0.7124 0.2864 1.0013 0.128 Uiso 1 1 calc R . .
C48 C 0.6507(3) 0.5157(2) 0.69355(14) 0.0275(6) Uani 1 1 d . . .
H48 H 0.6504 0.5867 0.7024 0.033 Uiso 1 1 calc R . .
C49 C 0.7248(3) 0.4927(3) 0.62312(15) 0.0360(7) Uani 1 1 d . . .
H49A H 0.8087 0.4758 0.6255 0.054 Uiso 1 1 calc R . .
H49B H 0.6951 0.5582 0.5888 0.054 Uiso 1 1 calc R . .
H49C H 0.7179 0.4294 0.6100 0.054 Uiso 1 1 calc R . .
C50 C 0.5210(3) 0.5330(3) 0.69341(17) 0.0376(8) Uani 1 1 d . . .
H50A H 0.5180 0.4644 0.6856 0.056 Uiso 1 1 calc R . .
H50B H 0.4878 0.5929 0.6566 0.056 Uiso 1 1 calc R . .
H50C H 0.4742 0.5526 0.7379 0.056 Uiso 1 1 calc R . .
C51 C 0.6617(3) 0.8587(2) 0.77339(18) 0.0336(7) Uani 1 1 d . . .
C52 C 0.6470(3) 0.9220(3) 0.8244(2) 0.0443(9) Uani 1 1 d . . .
C53 C 0.6402(3) 1.0307(3) 0.8031(3) 0.0579(11) Uani 1 1 d . . .
H53 H 0.6288 1.0756 0.8367 0.069 Uiso 1 1 calc R . .
C54 C 0.6495(3) 1.0739(3) 0.7352(3) 0.0574(11) Uani 1 1 d . . .
H54 H 0.6448 1.1481 0.7220 0.069 Uiso 1 1 calc R . .
C55 C 0.6658(3) 1.0104(3) 0.6855(2) 0.0454(9) Uani 1 1 d . . .
H55 H 0.6741 1.0413 0.6384 0.054 Uiso 1 1 calc R . .
C56 C 0.6705(3) 0.9019(2) 0.70273(17) 0.0335(7) Uani 1 1 d . . .
C57 C 0.6368(3) 0.8779(3) 0.9000(2) 0.0542(10) Uani 1 1 d . . .
H57 H 0.6613 0.7957 0.9049 0.065 Uiso 1 1 calc R . .
C58 C 0.7187(4) 0.9006(4) 0.9371(2) 0.0643(12) Uani 1 1 d . . .
H58A H 0.8013 0.8701 0.9144 0.096 Uiso 1 1 calc R . .
H58B H 0.7139 0.8653 0.9852 0.096 Uiso 1 1 calc R . .
H58C H 0.6933 0.9807 0.9355 0.096 Uiso 1 1 calc R . .
C59 C 0.5061(4) 0.9272(5) 0.9350(3) 0.0877(17) Uani 1 1 d . . .
H59A H 0.4804 1.0078 0.9315 0.132 Uiso 1 1 calc R . .
H59B H 0.5007 0.8946 0.9837 0.132 Uiso 1 1 calc R . .
H59C H 0.4545 0.9106 0.9121 0.132 Uiso 1 1 calc R . .
C60 C 0.6795(3) 0.8366(2) 0.64746(16) 0.0317(7) Uani 1 1 d . . .
H60 H 0.7377 0.7591 0.6590 0.038 Uiso 1 1 calc R . .
C61 C 0.5592(3) 0.8310(3) 0.64670(18) 0.0406(8) Uani 1 1 d . . .
H61A H 0.5324 0.7971 0.6920 0.061 Uiso 1 1 calc R . .
H61B H 0.5677 0.7862 0.6118 0.061 Uiso 1 1 calc R . .
H61C H 0.5002 0.9061 0.6358 0.061 Uiso 1 1 calc R . .
C62 C 0.7233(3) 0.8820(3) 0.57510(18) 0.0435(8) Uani 1 1 d . . .
H62A H 0.6629 0.9543 0.5602 0.065 Uiso 1 1 calc R . .
H62B H 0.7368 0.8304 0.5433 0.065 Uiso 1 1 calc R . .
H62C H 0.7981 0.8903 0.5752 0.065 Uiso 1 1 calc R . .
C63 C 0.5624(3) 0.6346(3) 0.83976(16) 0.0316(7) Uani 1 1 d . . .
H63 H 0.506(3) 0.601(2) 0.8597(16) 0.028(8) Uiso 1 1 d . . .
C64 C 0.5510(3) 0.7400(3) 0.82691(17) 0.0351(7) Uani 1 1 d . . .
H64 H 0.485(3) 0.803(3) 0.8345(15) 0.027(8) Uiso 1 1 d . . .
C65 C 1.093(2) -0.0967(17) 0.8950(8) 0.101(7) Uiso 0.25 1 d PD A -1
H65A H 1.0463 -0.1408 0.9197 0.151 Uiso 0.25 1 calc PR A -1
H65B H 1.1772 -0.1458 0.8857 0.151 Uiso 0.25 1 calc PR A -1
H65C H 1.0630 -0.0578 0.8514 0.151 Uiso 0.25 1 calc PR A -1
C66 C 1.0822(13) -0.0144(12) 0.9379(6) 0.049(4) Uiso 0.25 1 d PD A -1
H66A H 1.1632 -0.0191 0.9401 0.059 Uiso 0.25 1 calc PR A -1
H66B H 1.0377 0.0610 0.9151 0.059 Uiso 0.25 1 calc PR A -1
C67 C 1.0218(9) -0.0294(9) 1.0084(5) 0.035(3) Uiso 0.25 1 d PD A -1
H67A H 1.0753 -0.0354 1.0404 0.042 Uiso 0.25 1 calc PR A -1
H67B H 1.0123 -0.1012 1.0162 0.042 Uiso 0.25 1 calc PR A -1
C69 C 0.8110(11) 0.0093(17) 1.0586(10) 0.079(5) Uiso 0.25 1 d PD A -1
H69A H 0.8467 -0.0715 1.0609 0.119 Uiso 0.25 1 calc PR A -1
H69B H 0.7464 0.0401 1.0302 0.119 Uiso 0.25 1 calc PR A -1
H69C H 0.7787 0.0287 1.1051 0.119 Uiso 0.25 1 calc PR A -1
C68 C 0.9042(17) 0.0562(14) 1.0274(17) 0.33(4) Uiso 0.25 1 d PD A -1
H68A H 0.8784 0.1097 0.9858 0.392 Uiso 0.25 1 calc PR A -1
H68B H 0.9115 0.0971 1.0607 0.392 Uiso 0.25 1 calc PR A -1


_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
As1 N1 1.866(2) . ?
As1 B1 2.048(3) . ?
Si1 N1 1.759(2) . ?
Si1 C37 1.857(3) . ?
Si1 C36 1.858(3) . ?
Si1 C38 1.866(3) . ?
N1 C1 1.447(3) . ?
C1 C2 1.408(4) . ?
C1 C6 1.409(4) . ?
B1 N2 1.438(4) . ?
B1 N3 1.449(4) . ?
N2 C63 1.394(4) . ?
N2 C39 1.436(4) . ?
C2 C3 1.396(4) . ?
C2 C7 1.522(4) . ?
N3 C64 1.410(4) . ?
N3 C51 1.445(4) . ?
C3 C4 1.384(4) . ?
C4 C5 1.396(4) . ?
C4 C33 1.522(4) . ?
C5 C6 1.395(4) . ?
C6 C20 1.534(4) . ?
C7 C8 1.525(4) . ?
C7 C14 1.537(4) . ?
C8 C9 1.378(4) . ?
C8 C13 1.382(4) . ?
C9 C10 1.387(4) . ?
C10 C11 1.365(5) . ?
C11 C12 1.377(5) . ?
C12 C13 1.383(5) . ?
C14 C15 1.377(4) . ?
C14 C19 1.391(4) . ?
C15 C16 1.404(5) . ?
C16 C17 1.365(5) . ?
C17 C18 1.374(5) . ?
C18 C19 1.377(4) . ?
C20 C21 1.528(4) . ?
C20 C27 1.532(4) . ?
C21 C22 1.388(4) . ?
C21 C26 1.391(4) . ?
C22 C23 1.387(4) . ?
C23 C24 1.379(5) . ?
C24 C25 1.379(5) . ?
C25 C26 1.382(5) . ?
C27 C32 1.377(4) . ?
C27 C28 1.389(4) . ?
C28 C29 1.381(5) . ?
C29 C30 1.377(6) . ?
C30 C31 1.379(5) . ?
C31 C32 1.390(5) . ?
C33 C35 1.520(4) . ?
C33 C34 1.528(4) . ?
C39 C40 1.390(4) . ?
C39 C44 1.407(4) . ?
C40 C41 1.392(5) . ?
C40 C45 1.526(5) . ?
C41 C42 1.379(5) . ?
C42 C43 1.393(4) . ?
C43 C44 1.387(4) . ?
C44 C48 1.520(4) . ?
C45 C46 1.515(5) . ?
C45 C47 1.515(5) . ?
C48 C50 1.528(4) . ?
C48 C49 1.530(4) . ?
C51 C52 1.403(4) . ?
C51 C56 1.411(5) . ?
C52 C53 1.396(5) . ?
C52 C57 1.505(6) . ?
C53 C54 1.362(6) . ?
C54 C55 1.378(5) . ?
C55 C56 1.396(4) . ?
C56 C60 1.515(4) . ?
C57 C58 1.536(5) . ?
C57 C59 1.546(5) . ?
C60 C62 1.525(5) . ?
C60 C61 1.528(4) . ?
C63 C64 1.329(5) . ?
C65 C66 1.489(8) . ?
C66 C67 1.467(7) . ?
C67 C68 1.470(8) . ?
C69 C68 1.496(8) . ?

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
N1 As1 B1 115.48(11) . . ?
N1 Si1 C37 112.16(13) . . ?
N1 Si1 C36 109.76(13) . . ?
C37 Si1 C36 107.25(15) . . ?
N1 Si1 C38 107.64(13) . . ?
C37 Si1 C38 109.79(15) . . ?
C36 Si1 C38 110.24(15) . . ?
C1 N1 Si1 123.85(17) . . ?
C1 N1 As1 107.43(16) . . ?
Si1 N1 As1 128.70(12) . . ?
C2 C1 C6 119.1(2) . . ?
C2 C1 N1 119.8(2) . . ?
C6 C1 N1 120.9(2) . . ?
N2 B1 N3 104.1(2) . . ?
N2 B1 As1 111.6(2) . . ?
N3 B1 As1 141.7(2) . . ?
C63 N2 C39 121.4(2) . . ?
C63 N2 B1 109.3(2) . . ?
C39 N2 B1 128.0(2) . . ?
C3 C2 C1 119.5(2) . . ?
C3 C2 C7 118.4(2) . . ?
C1 C2 C7 122.1(2) . . ?
C64 N3 C51 117.7(2) . . ?
C64 N3 B1 107.2(2) . . ?
C51 N3 B1 135.0(2) . . ?
C4 C3 C2 122.4(2) . . ?
C3 C4 C5 117.4(2) . . ?
C3 C4 C33 121.8(2) . . ?
C5 C4 C33 120.8(2) . . ?
C4 C5 C6 122.4(2) . . ?
C5 C6 C1 119.2(2) . . ?
C5 C6 C20 118.4(2) . . ?
C1 C6 C20 122.3(2) . . ?
C2 C7 C8 112.6(2) . . ?
C2 C7 C14 111.0(2) . . ?
C8 C7 C14 114.2(2) . . ?
C9 C8 C13 117.3(3) . . ?
C9 C8 C7 123.1(3) . . ?
C13 C8 C7 119.6(3) . . ?
C8 C9 C10 121.2(3) . . ?
C11 C10 C9 120.9(3) . . ?
C10 C11 C12 118.8(3) . . ?
C11 C12 C13 120.2(3) . . ?
C8 C13 C12 121.6(3) . . ?
C15 C14 C19 117.8(3) . . ?
C15 C14 C7 124.0(3) . . ?
C19 C14 C7 118.2(2) . . ?
C14 C15 C16 120.3(3) . . ?
C17 C16 C15 120.7(3) . . ?
C16 C17 C18 119.5(3) . . ?
C17 C18 C19 119.9(3) . . ?
C18 C19 C14 121.8(3) . . ?
C21 C20 C27 112.6(2) . . ?
C21 C20 C6 114.2(2) . . ?
C27 C20 C6 109.3(2) . . ?
C22 C21 C26 117.8(3) . . ?
C22 C21 C20 123.4(3) . . ?
C26 C21 C20 118.7(3) . . ?
C23 C22 C21 121.3(3) . . ?
C24 C23 C22 119.8(3) . . ?
C23 C24 C25 119.8(3) . . ?
C24 C25 C26 120.2(3) . . ?
C25 C26 C21 121.1(3) . . ?
C32 C27 C28 118.0(3) . . ?
C32 C27 C20 119.7(2) . . ?
C28 C27 C20 122.1(3) . . ?
C29 C28 C27 120.9(3) . . ?
C30 C29 C28 120.7(3) . . ?
C29 C30 C31 119.0(3) . . ?
C30 C31 C32 120.1(3) . . ?
C27 C32 C31 121.2(3) . . ?
C35 C33 C4 112.1(2) . . ?
C35 C33 C34 110.5(3) . . ?
C4 C33 C34 111.2(2) . . ?
C40 C39 C44 122.1(3) . . ?
C40 C39 N2 120.1(3) . . ?
C44 C39 N2 117.8(2) . . ?
C39 C40 C41 118.1(3) . . ?
C39 C40 C45 121.2(3) . . ?
C41 C40 C45 120.7(3) . . ?
C42 C41 C40 121.2(3) . . ?
C41 C42 C43 119.7(3) . . ?
C44 C43 C42 121.2(3) . . ?
C43 C44 C39 117.7(3) . . ?
C43 C44 C48 120.8(3) . . ?
C39 C44 C48 121.5(2) . . ?
C46 C45 C47 110.8(3) . . ?
C46 C45 C40 110.6(3) . . ?
C47 C45 C40 111.9(3) . . ?
C44 C48 C50 110.6(2) . . ?
C44 C48 C49 113.0(2) . . ?
C50 C48 C49 110.9(2) . . ?
C52 C51 C56 121.8(3) . . ?
C52 C51 N3 118.6(3) . . ?
C56 C51 N3 119.5(3) . . ?
C53 C52 C51 117.8(4) . . ?
C53 C52 C57 119.4(3) . . ?
C51 C52 C57 122.8(3) . . ?
C54 C53 C52 121.4(4) . . ?
C53 C54 C55 120.3(3) . . ?
C54 C55 C56 121.7(4) . . ?
C55 C56 C51 116.9(3) . . ?
C55 C56 C60 120.7(3) . . ?
C51 C56 C60 122.3(3) . . ?
C52 C57 C58 112.4(3) . . ?
C52 C57 C59 110.8(4) . . ?
C58 C57 C59 109.7(3) . . ?
C56 C60 C62 114.2(3) . . ?
C56 C60 C61 110.8(3) . . ?
C62 C60 C61 108.4(3) . . ?
C64 C63 N2 108.9(3) . . ?
C63 C64 N3 110.5(3) . . ?
C67 C66 C65 114.2(8) . . ?
C66 C67 C68 117.7(9) . . ?
C67 C68 C69 112.8(9) . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.50
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.946
_refine_diff_density_min         -0.768
_refine_diff_density_rms         0.075
####################################################################### 
# 
# 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_compound4
_database_code_depnum_ccdc_archive 'CCDC 1051450'
_audit_update_record             
;
2015-02-27 deposited with the CCDC.
2015-03-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C98 H128 N2 Sb2 Si2'
_chemical_formula_weight         1633.70

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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.6918(10)
_cell_length_b                   13.6933(10)
_cell_length_c                   14.0983(11)
_cell_angle_alpha                72.740(7)
_cell_angle_beta                 77.066(7)
_cell_angle_gamma                67.955(7)
_cell_volume                     2151.2(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            purple
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.261
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             860
_exptl_absorpt_coefficient_mu    0.702
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.815
_exptl_absorpt_correction_T_max  0.872
_exptl_absorpt_process_details   'Sortav (Blessing)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Apex X8'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            16202
_diffrn_reflns_av_R_equivalents  0.0390
_diffrn_reflns_av_sigmaI/netI    0.0582
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.05
_diffrn_reflns_theta_max         25.50
_reflns_number_total             7999
_reflns_number_gt                6755
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger.
 A molecule of pentane of crystallisation was located in the asymmetric unit
 and its carbon atoms refined isotropically. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0588P)²+3.5250P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7999
_refine_ls_number_parameters     454
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0611
_refine_ls_R_factor_gt           0.0473
_refine_ls_wR_factor_ref         0.1285
_refine_ls_wR_factor_gt          0.1178
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_restrained_S_all      1.074
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Sb1 Sb 0.53835(2) 0.54585(2) 0.55220(2) 0.02361(11) Uani 1 1 d . . .
Si1 Si 0.32843(9) 0.79100(8) 0.54902(8) 0.0189(2) Uani 1 1 d . . .
N1 N 0.3880(3) 0.6536(2) 0.6109(2) 0.0177(6) Uani 1 1 d . . .
C8 C 0.5989(3) 0.5697(3) 0.7683(3) 0.0213(8) Uani 1 1 d . . .
C1 C 0.3446(3) 0.6173(3) 0.7140(3) 0.0162(7) Uani 1 1 d . . .
C4 C 0.2388(3) 0.5691(3) 0.9149(3) 0.0207(8) Uani 1 1 d . . .
C33 C 0.1772(4) 0.5531(4) 1.0207(3) 0.0291(10) Uani 1 1 d . . .
H33 H 0.2295 0.5499 1.0659 0.035 Uiso 1 1 calc R . .
C10 C 0.7001(4) 0.3767(4) 0.7983(3) 0.0308(10) Uani 1 1 d . . .
H10 H 0.6998 0.3045 0.8255 0.037 Uiso 1 1 calc R . .
C7 C 0.4903(3) 0.6666(3) 0.7742(3) 0.0190(8) Uani 1 1 d . . .
H7 H 0.4893 0.7177 0.7066 0.023 Uiso 1 1 calc R . .
C2 C 0.2606(3) 0.5661(3) 0.7397(3) 0.0184(8) Uani 1 1 d . . .
C14 C 0.4974(3) 0.7261(3) 0.8478(3) 0.0213(8) Uani 1 1 d . . .
C15 C 0.5333(3) 0.6703(3) 0.9416(3) 0.0248(9) Uani 1 1 d . . .
H15 H 0.5497 0.5940 0.9619 0.030 Uiso 1 1 calc R . .
C3 C 0.2109(3) 0.5427(3) 0.8386(3) 0.0216(8) Uani 1 1 d . . .
H3 H 0.1555 0.5072 0.8543 0.026 Uiso 1 1 calc R . .
C6 C 0.3828(3) 0.6342(3) 0.7936(3) 0.0184(8) Uani 1 1 d . . .
C42 C 0.2605(4) 0.8732(3) 0.6486(3) 0.0263(9) Uani 1 1 d . . .
H42 H 0.3127 0.8410 0.7017 0.032 Uiso 1 1 calc R . .
C44 C 0.1432(4) 0.8631(4) 0.7007(4) 0.0354(11) Uani 1 1 d . . .
H44A H 0.1126 0.9066 0.7510 0.053 Uiso 1 1 calc R . .
H44B H 0.1524 0.7870 0.7334 0.053 Uiso 1 1 calc R . .
H44C H 0.0900 0.8895 0.6508 0.053 Uiso 1 1 calc R . .
C11 C 0.8014(4) 0.3954(4) 0.7505(3) 0.0325(10) Uani 1 1 d . . .
H11 H 0.8701 0.3363 0.7437 0.039 Uiso 1 1 calc R . .
C5 C 0.3274(3) 0.6129(3) 0.8901(3) 0.0217(8) Uani 1 1 d . . .
H5 H 0.3507 0.6288 0.9418 0.026 Uiso 1 1 calc R . .
C37 C 0.2579(4) 0.7545(4) 0.3869(4) 0.0334(10) Uani 1 1 d . . .
H37A H 0.1935 0.7633 0.3540 0.050 Uiso 1 1 calc R . .
H37B H 0.2980 0.6771 0.4123 0.050 Uiso 1 1 calc R . .
H37C H 0.3110 0.7873 0.3387 0.050 Uiso 1 1 calc R . .
C36 C 0.2132(3) 0.8100(3) 0.4736(3) 0.0250(9) Uani 1 1 d . . .
H36 H 0.1601 0.7732 0.5203 0.030 Uiso 1 1 calc R . .
C13 C 0.7016(3) 0.5870(4) 0.7221(3) 0.0259(9) Uani 1 1 d . . .
H13 H 0.7029 0.6591 0.6966 0.031 Uiso 1 1 calc R . .
C9 C 0.6000(3) 0.4625(3) 0.8066(3) 0.0246(9) Uani 1 1 d . . .
H9 H 0.5309 0.4488 0.8386 0.030 Uiso 1 1 calc R . .
C39 C 0.4512(3) 0.8289(3) 0.4601(3) 0.0236(8) Uani 1 1 d . . .
H39 H 0.4859 0.7723 0.4203 0.028 Uiso 1 1 calc R . .
C40 C 0.4158(4) 0.9379(4) 0.3820(3) 0.0336(10) Uani 1 1 d . . .
H40A H 0.3781 0.9970 0.4165 0.050 Uiso 1 1 calc R . .
H40B H 0.3627 0.9366 0.3418 0.050 Uiso 1 1 calc R . .
H40C H 0.4841 0.9491 0.3382 0.050 Uiso 1 1 calc R . .
C12 C 0.8015(4) 0.5009(4) 0.7127(3) 0.0304(10) Uani 1 1 d . . .
H12 H 0.8706 0.5142 0.6801 0.036 Uiso 1 1 calc R . .
C38 C 0.1380(4) 0.9279(4) 0.4342(4) 0.0364(11) Uani 1 1 d . . .
H38A H 0.1843 0.9660 0.3826 0.055 Uiso 1 1 calc R . .
H38B H 0.1074 0.9644 0.4895 0.055 Uiso 1 1 calc R . .
H38C H 0.0744 0.9281 0.4053 0.055 Uiso 1 1 calc R . .
C19 C 0.4765(4) 0.8370(4) 0.8194(3) 0.0325(10) Uani 1 1 d . . .
H19 H 0.4529 0.8766 0.7555 0.039 Uiso 1 1 calc R . .
C35 C 0.0704(4) 0.6516(4) 1.0289(4) 0.0424(12) Uani 1 1 d . . .
H35A H 0.0926 0.7164 1.0135 0.064 Uiso 1 1 calc R . .
H35B H 0.0301 0.6410 1.0971 0.064 Uiso 1 1 calc R . .
H35C H 0.0197 0.6608 0.9814 0.064 Uiso 1 1 calc R . .
C41 C 0.5493(4) 0.8235(4) 0.5108(3) 0.0329(10) Uani 1 1 d . . .
H41A H 0.6112 0.8383 0.4595 0.049 Uiso 1 1 calc R . .
H41B H 0.5784 0.7510 0.5541 0.049 Uiso 1 1 calc R . .
H41C H 0.5207 0.8776 0.5510 0.049 Uiso 1 1 calc R . .
C21 C 0.2422(3) 0.4068(3) 0.7022(3) 0.0213(8) Uani 1 1 d . . .
C32 C 0.0237(3) 0.6646(3) 0.6772(3) 0.0255(9) Uani 1 1 d . . .
H32 H 0.0329 0.6698 0.7404 0.031 Uiso 1 1 calc R . .
C26 C 0.3473(3) 0.3353(3) 0.7303(3) 0.0261(9) Uani 1 1 d . . .
H26 H 0.4079 0.3622 0.7247 0.031 Uiso 1 1 calc R . .
C28 C 0.0953(4) 0.5879(4) 0.5337(3) 0.0274(9) Uani 1 1 d . . .
H28 H 0.1548 0.5410 0.4974 0.033 Uiso 1 1 calc R . .
C27 C 0.1122(3) 0.5957(3) 0.6257(3) 0.0208(8) Uani 1 1 d . . .
C20 C 0.2282(3) 0.5275(3) 0.6631(3) 0.0186(8) Uani 1 1 d . . .
H20 H 0.2871 0.5326 0.6031 0.022 Uiso 1 1 calc R . .
C22 C 0.1550(4) 0.3655(3) 0.7127(3) 0.0292(10) Uani 1 1 d . . .
H22 H 0.0819 0.4132 0.6950 0.035 Uiso 1 1 calc R . .
C34 C 0.1490(4) 0.4486(4) 1.0572(3) 0.0357(11) Uani 1 1 d . . .
H34A H 0.0962 0.4497 1.0153 0.054 Uiso 1 1 calc R . .
H34B H 0.1128 0.4420 1.1269 0.054 Uiso 1 1 calc R . .
H34C H 0.2196 0.3868 1.0529 0.054 Uiso 1 1 calc R . .
C16 C 0.5453(4) 0.7242(4) 1.0057(3) 0.0299(10) Uani 1 1 d . . .
H16 H 0.5686 0.6852 1.0698 0.036 Uiso 1 1 calc R . .
C17 C 0.5232(5) 0.8352(4) 0.9759(4) 0.0407(12) Uani 1 1 d . . .
H17 H 0.5312 0.8726 1.0194 0.049 Uiso 1 1 calc R . .
C43 C 0.2521(4) 0.9931(4) 0.6107(4) 0.0397(11) Uani 1 1 d . . .
H43A H 0.2045 1.0278 0.5561 0.060 Uiso 1 1 calc R . .
H43B H 0.3290 0.9981 0.5864 0.060 Uiso 1 1 calc R . .
H43C H 0.2175 1.0300 0.6657 0.060 Uiso 1 1 calc R . .
C18 C 0.4895(5) 0.8913(4) 0.8827(4) 0.0429(12) Uani 1 1 d . . .
H18 H 0.4751 0.9673 0.8618 0.051 Uiso 1 1 calc R . .
C25 C 0.3656(4) 0.2247(3) 0.7667(3) 0.0320(10) Uani 1 1 d . . .
H25 H 0.4382 0.1769 0.7856 0.038 Uiso 1 1 calc R . .
C24 C 0.2782(4) 0.1845(4) 0.7752(4) 0.0378(11) Uani 1 1 d . . .
H24 H 0.2906 0.1090 0.7989 0.045 Uiso 1 1 calc R . .
C31 C -0.0785(4) 0.7264(4) 0.6368(4) 0.0349(11) Uani 1 1 d . . .
H31 H -0.1380 0.7745 0.6720 0.042 Uiso 1 1 calc R . .
C30 C -0.0932(4) 0.7178(4) 0.5457(4) 0.0367(11) Uani 1 1 d . . .
H30 H -0.1627 0.7602 0.5181 0.044 Uiso 1 1 calc R . .
C29 C -0.0071(4) 0.6480(4) 0.4954(3) 0.0345(11) Uani 1 1 d . . .
H29 H -0.0181 0.6409 0.4336 0.041 Uiso 1 1 calc R . .
C23 C 0.1729(4) 0.2551(4) 0.7490(4) 0.0398(12) Uani 1 1 d . . .
H23 H 0.1120 0.2282 0.7557 0.048 Uiso 1 1 calc R . .
C45 C -0.1946(7) 0.8732(6) 0.8485(7) 0.097(3) Uiso 1 1 d D . .
H45A H -0.1140 0.8445 0.8212 0.146 Uiso 1 1 calc R . .
H45B H -0.2437 0.8806 0.8005 0.146 Uiso 1 1 calc R . .
H45C H -0.2108 0.8235 0.9116 0.146 Uiso 1 1 calc R . .
C47 C -0.1714(9) 0.9742(7) 0.9589(7) 0.121(3) Uiso 1 1 d D . .
H47A H -0.0886 0.9318 0.9529 0.145 Uiso 1 1 calc R . .
H47B H -0.2100 0.9341 1.0179 0.145 Uiso 1 1 calc R . .
C46 C -0.2181(10) 0.9839(7) 0.8676(7) 0.135(4) Uiso 1 1 d D . .
H46A H -0.1831 1.0277 0.8091 0.162 Uiso 1 1 calc R . .
H46B H -0.3019 1.0222 0.8753 0.162 Uiso 1 1 calc R . .
C48 C -0.1883(9) 1.0856(6) 0.9756(7) 0.111(3) Uiso 1 1 d D . .
H48A H -0.1364 1.1195 0.9250 0.133 Uiso 1 1 calc R . .
H48B H -0.2682 1.1339 0.9682 0.133 Uiso 1 1 calc R . .
C49 C -0.1623(10) 1.0708(8) 1.0796(7) 0.133(4) Uiso 1 1 d D . .
H49A H -0.2123 1.0352 1.1293 0.200 Uiso 1 1 calc R . .
H49B H -0.1759 1.1418 1.0915 0.200 Uiso 1 1 calc R . .
H49C H -0.0821 1.0259 1.0854 0.200 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
Sb1 N1 2.099(3) . ?
Sb1 Sb1 2.7104(5) 2_666 ?
Si1 N1 1.768(3) . ?
Si1 C36 1.893(4) . ?
Si1 C39 1.901(4) . ?
Si1 C42 1.910(4) . ?
N1 C1 1.444(5) . ?
C8 C13 1.392(6) . ?
C8 C9 1.401(6) . ?
C8 C7 1.520(5) . ?
C1 C2 1.413(5) . ?
C1 C6 1.425(5) . ?
C4 C3 1.382(5) . ?
C4 C5 1.397(5) . ?
C4 C33 1.517(6) . ?
C33 C34 1.518(6) . ?
C33 C35 1.523(7) . ?
C10 C9 1.380(6) . ?
C10 C11 1.390(6) . ?
C7 C14 1.532(5) . ?
C7 C6 1.532(5) . ?
C2 C3 1.392(6) . ?
C2 C20 1.521(5) . ?
C14 C19 1.387(6) . ?
C14 C15 1.395(6) . ?
C15 C16 1.389(6) . ?
C6 C5 1.386(6) . ?
C42 C43 1.539(6) . ?
C42 C44 1.542(6) . ?
C11 C12 1.383(6) . ?
C37 C36 1.519(6) . ?
C36 C38 1.541(6) . ?
C13 C12 1.383(6) . ?
C39 C41 1.537(6) . ?
C39 C40 1.544(6) . ?
C19 C18 1.388(6) . ?
C21 C22 1.383(6) . ?
C21 C26 1.386(6) . ?
C21 C20 1.533(5) . ?
C32 C27 1.388(6) . ?
C32 C31 1.394(6) . ?
C26 C25 1.392(6) . ?
C28 C29 1.381(6) . ?
C28 C27 1.401(5) . ?
C27 C20 1.530(5) . ?
C22 C23 1.391(6) . ?
C16 C17 1.386(6) . ?
C17 C18 1.380(7) . ?
C25 C24 1.381(6) . ?
C24 C23 1.377(7) . ?
C31 C30 1.383(7) . ?
C30 C29 1.372(7) . ?
C45 C46 1.524(6) . ?
C47 C46 1.486(7) . ?
C47 C48 1.540(7) . ?
C48 C49 1.513(7) . ?

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
N1 Sb1 Sb1 103.78(8) . 2_666 ?
N1 Si1 C36 111.36(16) . . ?
N1 Si1 C39 105.86(16) . . ?
C36 Si1 C39 108.87(18) . . ?
N1 Si1 C42 107.93(17) . . ?
C36 Si1 C42 108.42(19) . . ?
C39 Si1 C42 114.42(18) . . ?
C1 N1 Si1 118.9(2) . . ?
C1 N1 Sb1 116.7(2) . . ?
Si1 N1 Sb1 123.41(17) . . ?
C13 C8 C9 118.2(4) . . ?
C13 C8 C7 119.3(4) . . ?
C9 C8 C7 122.5(3) . . ?
C2 C1 C6 117.5(3) . . ?
C2 C1 N1 121.3(3) . . ?
C6 C1 N1 121.2(3) . . ?
C3 C4 C5 116.8(4) . . ?
C3 C4 C33 122.7(3) . . ?
C5 C4 C33 120.5(3) . . ?
C4 C33 C34 113.9(4) . . ?
C4 C33 C35 109.4(4) . . ?
C34 C33 C35 111.5(4) . . ?
C9 C10 C11 120.3(4) . . ?
C8 C7 C14 109.5(3) . . ?
C8 C7 C6 111.4(3) . . ?
C14 C7 C6 115.6(3) . . ?
C3 C2 C1 120.2(3) . . ?
C3 C2 C20 118.0(3) . . ?
C1 C2 C20 121.7(3) . . ?
C19 C14 C15 118.0(4) . . ?
C19 C14 C7 120.2(4) . . ?
C15 C14 C7 121.6(3) . . ?
C16 C15 C14 121.2(4) . . ?
C4 C3 C2 122.6(3) . . ?
C5 C6 C1 119.4(3) . . ?
C5 C6 C7 120.1(3) . . ?
C1 C6 C7 120.2(3) . . ?
C43 C42 C44 110.5(4) . . ?
C43 C42 Si1 113.9(3) . . ?
C44 C42 Si1 113.0(3) . . ?
C12 C11 C10 119.4(4) . . ?
C6 C5 C4 122.9(3) . . ?
C37 C36 C38 108.5(4) . . ?
C37 C36 Si1 113.7(3) . . ?
C38 C36 Si1 116.1(3) . . ?
C12 C13 C8 121.0(4) . . ?
C10 C9 C8 120.7(4) . . ?
C41 C39 C40 109.3(3) . . ?
C41 C39 Si1 115.1(3) . . ?
C40 C39 Si1 115.4(3) . . ?
C13 C12 C11 120.3(4) . . ?
C14 C19 C18 121.0(4) . . ?
C22 C21 C26 118.1(4) . . ?
C22 C21 C20 123.6(3) . . ?
C26 C21 C20 118.3(3) . . ?
C27 C32 C31 120.5(4) . . ?
C21 C26 C25 121.2(4) . . ?
C29 C28 C27 120.5(4) . . ?
C32 C27 C28 118.4(4) . . ?
C32 C27 C20 123.9(3) . . ?
C28 C27 C20 117.7(4) . . ?
C2 C20 C27 116.0(3) . . ?
C2 C20 C21 109.4(3) . . ?
C27 C20 C21 112.8(3) . . ?
C21 C22 C23 120.9(4) . . ?
C17 C16 C15 119.7(4) . . ?
C18 C17 C16 119.8(4) . . ?
C17 C18 C19 120.2(4) . . ?
C24 C25 C26 120.0(4) . . ?
C23 C24 C25 119.3(4) . . ?
C30 C31 C32 120.0(4) . . ?
C29 C30 C31 119.8(4) . . ?
C30 C29 C28 120.6(4) . . ?
C24 C23 C22 120.5(4) . . ?
C46 C47 C48 112.3(6) . . ?
C47 C46 C45 111.7(6) . . ?
C49 C48 C47 109.2(6) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.50
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         2.071
_refine_diff_density_min         -0.864
_refine_diff_density_rms         0.109
####################################################################### 
# 
# 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_compound5
_database_code_depnum_ccdc_archive 'CCDC 1051451'
_audit_update_record             
;
2015-02-27 deposited with the CCDC.
2015-03-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C52 H72 B2 Bi2 N4'
_chemical_formula_weight         1192.72

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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Bi Bi -4.1077 10.2566 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.5010(7)
_cell_length_b                   12.7973(14)
_cell_length_c                   21.8679(9)
_cell_angle_alpha                88.502(5)
_cell_angle_beta                 76.645(4)
_cell_angle_gamma                67.584(8)
_cell_volume                     2636.9(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.502
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1176
_exptl_absorpt_coefficient_mu    6.700
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.343
_exptl_absorpt_correction_T_max  0.476
_exptl_absorpt_process_details   'Sortav (Blessing)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Apex X8'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            19674
_diffrn_reflns_av_R_equivalents  0.0418
_diffrn_reflns_av_sigmaI/netI    0.0636
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         3.16
_diffrn_reflns_theta_max         25.50
_reflns_number_total             9810
_reflns_number_gt                7430
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger.
 Two crystallographically independent half molecules were refined in the 
 asymmetric unit. The atoms of one isopropyl group of one half molecule
 were found to be disordered over two sites. This disorder was modelled
 and the carbon atoms of the major set refined anisotropically, while
 those of the minor set were refined isotropically. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0272P)²+5.5366P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         9810
_refine_ls_number_parameters     572
_refine_ls_number_restraints     45
_refine_ls_R_factor_all          0.0650
_refine_ls_R_factor_gt           0.0406
_refine_ls_wR_factor_ref         0.0902
_refine_ls_wR_factor_gt          0.0788
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_restrained_S_all      1.045
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Bi1 Bi 0.13916(3) -0.00636(2) 0.490277(13) 0.04219(9) Uani 1 1 d . . .
N1 N 0.2392(5) -0.2399(4) 0.5698(2) 0.0293(12) Uani 1 1 d . . .
C1 C 0.2235(6) -0.1812(5) 0.6281(3) 0.0272(14) Uani 1 1 d . . .
B1 B 0.2226(8) -0.1961(7) 0.5109(3) 0.0363(19) Uani 1 1 d . . .
C20A C 0.047(3) -0.480(2) 0.3990(15) 0.079(11) Uiso 0.320(15) 1 d PD A 2
H20A H 0.0355 -0.5285 0.4333 0.119 Uiso 0.320(15) 1 calc PR A 2
H20B H 0.1201 -0.5257 0.3628 0.119 Uiso 0.320(15) 1 calc PR A 2
H20C H -0.0430 -0.4428 0.3867 0.119 Uiso 0.320(15) 1 calc PR A 2
C21A C -0.032(3) -0.307(2) 0.4703(15) 0.090(12) Uiso 0.320(15) 1 d PD A 2
H21A H -0.1124 -0.2695 0.4515 0.135 Uiso 0.320(15) 1 calc PR A 2
H21B H -0.0027 -0.2495 0.4852 0.135 Uiso 0.320(15) 1 calc PR A 2
H21C H -0.0588 -0.3481 0.5060 0.135 Uiso 0.320(15) 1 calc PR A 2
C19A C 0.092(3) -0.390(2) 0.4210(11) 0.077(10) Uiso 0.320(15) 1 d PD A 2
H19A H 0.1567 -0.4338 0.4480 0.092 Uiso 0.320(15) 1 calc PR A 2
Bi2 Bi 0.97083(3) 0.61588(2) 0.007370(11) 0.03560(9) Uani 1 1 d . . .
N2 N 0.2724(6) -0.2932(5) 0.4677(2) 0.0426(15) Uani 1 1 d . . .
C2 C 0.3413(7) -0.1667(6) 0.6390(3) 0.0367(16) Uani 1 1 d . . .
B2 B 0.9501(7) 0.6269(6) 0.1155(3) 0.0260(16) Uani 1 1 d . . .
N3 N 0.9631(5) 0.5482(4) 0.1638(2) 0.0213(10) Uani 1 1 d . . .
C3 C 0.3238(8) -0.1066(6) 0.6948(3) 0.0428(18) Uani 1 1 d . . .
H3 H 0.4023 -0.0949 0.7033 0.051 Uiso 1 1 calc R . .
N4 N 0.9148(5) 0.7325(4) 0.1483(2) 0.0238(11) Uani 1 1 d . . .
C4 C 0.1956(8) -0.0644(6) 0.7374(3) 0.0465(19) Uani 1 1 d . . .
H4 H 0.1859 -0.0245 0.7753 0.056 Uiso 1 1 calc R . .
C5 C 0.0802(8) -0.0795(6) 0.7255(3) 0.0404(17) Uani 1 1 d . . .
H5 H -0.0087 -0.0486 0.7553 0.048 Uiso 1 1 calc R . .
C6 C 0.0904(6) -0.1389(5) 0.6709(3) 0.0303(14) Uani 1 1 d . . .
C7 C -0.0351(6) -0.1598(6) 0.6590(3) 0.0344(16) Uani 1 1 d . . .
H7 H -0.0270 -0.1595 0.6126 0.041 Uiso 1 1 calc R . .
C8 C -0.0300(8) -0.2775(7) 0.6790(3) 0.0457(19) Uani 1 1 d . . .
H8A H -0.0257 -0.2842 0.7233 0.069 Uiso 1 1 calc R . .
H8B H 0.0542 -0.3364 0.6527 0.069 Uiso 1 1 calc R . .
H8C H -0.1154 -0.2868 0.6737 0.069 Uiso 1 1 calc R . .
C9 C -0.1771(7) -0.0682(7) 0.6904(4) 0.055(2) Uani 1 1 d . . .
H9A H -0.1930 -0.0713 0.7363 0.082 Uiso 1 1 calc R . .
H9B H -0.2530 -0.0804 0.6766 0.082 Uiso 1 1 calc R . .
H9C H -0.1771 0.0062 0.6787 0.082 Uiso 1 1 calc R . .
C10 C 0.4857(7) -0.2130(7) 0.5921(3) 0.0456(19) Uani 1 1 d . . .
H10 H 0.4781 -0.2566 0.5568 0.055 Uiso 1 1 calc R . .
C11 C 0.5973(9) -0.2926(10) 0.6224(5) 0.098(4) Uani 1 1 d . . .
H11A H 0.6891 -0.3207 0.5916 0.147 Uiso 1 1 calc R . .
H11B H 0.5717 -0.3566 0.6370 0.147 Uiso 1 1 calc R . .
H11C H 0.6039 -0.2524 0.6583 0.147 Uiso 1 1 calc R . .
C12 C 0.5277(10) -0.1169(9) 0.5646(5) 0.087(3) Uani 1 1 d . . .
H12A H 0.4554 -0.0677 0.5438 0.130 Uiso 1 1 calc R . .
H12B H 0.6193 -0.1485 0.5339 0.130 Uiso 1 1 calc R . .
H12C H 0.5353 -0.0727 0.5985 0.130 Uiso 1 1 calc R . .
C13 C 0.2873(9) -0.3040(7) 0.4014(3) 0.063(3) Uani 1 1 d . A .
C14 C 0.3891(12) -0.2840(7) 0.3595(4) 0.073(3) Uani 1 1 d D . .
C15 C 0.4055(14) -0.3003(9) 0.2942(4) 0.091(4) Uani 1 1 d D . .
H15 H 0.4789 -0.2895 0.2635 0.109 Uiso 1 1 calc R . .
C16 C 0.3069(15) -0.3329(10) 0.2790(6) 0.101(4) Uani 1 1 d . . .
H16 H 0.3156 -0.3430 0.2352 0.121 Uiso 1 1 calc R . .
C17 C 0.2004(14) -0.3525(11) 0.3163(6) 0.103(4) Uani 1 1 d U A .
H17 H 0.1399 -0.3782 0.3003 0.124 Uiso 1 1 calc R . .
C18 C 0.1839(12) -0.3331(11) 0.3796(4) 0.102(4) Uani 1 1 d D . .
C19 C 0.0414(12) -0.3154(12) 0.4206(7) 0.089(5) Uani 0.680(15) 1 d PDU A 1
H19 H 0.0309 -0.2822 0.4633 0.107 Uiso 0.680(15) 1 calc PR A 1
C20 C 0.052(2) -0.4365(12) 0.4245(10) 0.128(8) Uani 0.680(15) 1 d PDU A 1
H20D H 0.1035 -0.4781 0.3835 0.193 Uiso 0.680(15) 1 calc PR A 1
H20E H -0.0431 -0.4375 0.4359 0.193 Uiso 0.680(15) 1 calc PR A 1
H20F H 0.1037 -0.4724 0.4565 0.193 Uiso 0.680(15) 1 calc PR A 1
C21 C -0.0787(16) -0.2421(12) 0.3924(8) 0.099(6) Uani 0.680(15) 1 d PDU A 1
H21D H -0.0490 -0.1890 0.3655 0.148 Uiso 0.680(15) 1 calc PR A 1
H21E H -0.1613 -0.1996 0.4263 0.148 Uiso 0.680(15) 1 calc PR A 1
H21F H -0.1038 -0.2901 0.3672 0.148 Uiso 0.680(15) 1 calc PR A 1
C22 C 0.4927(10) -0.2511(7) 0.3845(5) 0.082(4) Uani 1 1 d . . .
H22 H 0.4383 -0.2056 0.4253 0.099 Uiso 1 1 calc R . .
C23 C 0.6179(12) -0.3517(9) 0.3991(5) 0.102(4) Uani 1 1 d . . .
H23A H 0.5815 -0.3963 0.4302 0.153 Uiso 1 1 calc R . .
H23B H 0.6782 -0.3234 0.4160 0.153 Uiso 1 1 calc R . .
H23C H 0.6736 -0.3996 0.3603 0.153 Uiso 1 1 calc R . .
C24 C 0.5527(12) -0.1760(10) 0.3422(6) 0.111(4) Uani 1 1 d U . .
H24A H 0.6054 -0.2167 0.3011 0.167 Uiso 1 1 calc R . .
H24B H 0.6166 -0.1565 0.3617 0.167 Uiso 1 1 calc R . .
H24C H 0.4748 -0.1066 0.3366 0.167 Uiso 1 1 calc R . .
C25 C 0.3191(7) -0.3902(6) 0.5013(3) 0.0427(17) Uani 1 1 d . . .
H25 H 0.3582 -0.4663 0.4841 0.051 Uiso 1 1 calc R . .
C26 C 0.2993(7) -0.3573(6) 0.5617(3) 0.0377(16) Uani 1 1 d . . .
H26 H 0.3228 -0.4069 0.5940 0.045 Uiso 1 1 calc R . .
C27 C 1.0086(6) 0.4279(5) 0.1577(3) 0.0223(13) Uani 1 1 d . . .
C28 C 1.1552(6) 0.3620(5) 0.1413(3) 0.0271(14) Uani 1 1 d . . .
C29 C 1.1986(7) 0.2451(6) 0.1321(3) 0.0370(16) Uani 1 1 d . . .
H29 H 1.2969 0.1984 0.1212 0.044 Uiso 1 1 calc R . .
C30 C 1.0990(8) 0.1965(6) 0.1387(3) 0.0428(18) Uani 1 1 d . . .
H30 H 1.1298 0.1170 0.1307 0.051 Uiso 1 1 calc R . .
C31 C 0.9561(7) 0.2622(6) 0.1567(3) 0.0351(16) Uani 1 1 d . . .
H31 H 0.8895 0.2271 0.1624 0.042 Uiso 1 1 calc R . .
C32 C 0.9083(7) 0.3787(6) 0.1666(3) 0.0305(15) Uani 1 1 d . . .
C33 C 0.7492(6) 0.4501(6) 0.1888(3) 0.0345(16) Uani 1 1 d . . .
H33 H 0.7385 0.5282 0.2012 0.041 Uiso 1 1 calc R . .
C34 C 0.6730(8) 0.4599(9) 0.1367(4) 0.073(3) Uani 1 1 d U . .
H34A H 0.6793 0.3848 0.1243 0.110 Uiso 1 1 calc R . .
H34B H 0.7173 0.4910 0.1004 0.110 Uiso 1 1 calc R . .
H34C H 0.5731 0.5103 0.1518 0.110 Uiso 1 1 calc R . .
C35 C 0.6800(8) 0.4057(7) 0.2459(4) 0.056(2) Uani 1 1 d . . .
H35A H 0.5816 0.4588 0.2617 0.083 Uiso 1 1 calc R . .
H35B H 0.7320 0.3976 0.2788 0.083 Uiso 1 1 calc R . .
H35C H 0.6813 0.3317 0.2344 0.083 Uiso 1 1 calc R . .
C36 C 1.2661(7) 0.4122(6) 0.1372(3) 0.0421(18) Uani 1 1 d . . .
H36 H 1.2172 0.4965 0.1384 0.051 Uiso 1 1 calc R . .
C37 C 1.3821(8) 0.3740(8) 0.0762(4) 0.058(2) Uani 1 1 d . . .
H37A H 1.4502 0.4094 0.0758 0.087 Uiso 1 1 calc R . .
H37B H 1.3394 0.3966 0.0401 0.087 Uiso 1 1 calc R . .
H37C H 1.4313 0.2914 0.0735 0.087 Uiso 1 1 calc R . .
C38 C 1.3305(9) 0.3835(9) 0.1945(4) 0.068(3) Uani 1 1 d . . .
H38A H 1.3832 0.3015 0.1933 0.102 Uiso 1 1 calc R . .
H38B H 1.2545 0.4082 0.2331 0.102 Uiso 1 1 calc R . .
H38C H 1.3950 0.4225 0.1938 0.102 Uiso 1 1 calc R . .
C39 C 0.9015(6) 0.8401(5) 0.1230(3) 0.0255(13) Uani 1 1 d . . .
C40 C 1.0223(6) 0.8672(5) 0.1069(3) 0.0265(14) Uani 1 1 d . . .
C41 C 1.0067(7) 0.9712(6) 0.0832(3) 0.0344(15) Uani 1 1 d . . .
H41 H 1.0874 0.9907 0.0715 0.041 Uiso 1 1 calc R . .
C42 C 0.8773(7) 1.0480(6) 0.0760(3) 0.0392(17) Uani 1 1 d . . .
H42 H 0.8687 1.1197 0.0603 0.047 Uiso 1 1 calc R . .
C43 C 0.7615(7) 1.0189(6) 0.0919(3) 0.0378(16) Uani 1 1 d . . .
H43 H 0.6726 1.0720 0.0871 0.045 Uiso 1 1 calc R . .
C44 C 0.7689(6) 0.9161(5) 0.1144(3) 0.0304(14) Uani 1 1 d . . .
C45 C 0.6385(6) 0.8857(6) 0.1288(3) 0.0396(17) Uani 1 1 d . . .
H45 H 0.6681 0.8057 0.1412 0.048 Uiso 1 1 calc R . .
C46 C 0.5789(9) 0.8927(9) 0.0698(4) 0.068(3) Uani 1 1 d . . .
H46A H 0.5457 0.9712 0.0577 0.103 Uiso 1 1 calc R . .
H46B H 0.4995 0.8677 0.0792 0.103 Uiso 1 1 calc R . .
H46C H 0.6536 0.8438 0.0350 0.103 Uiso 1 1 calc R . .
C47 C 0.5246(7) 0.9608(7) 0.1832(4) 0.053(2) Uani 1 1 d . . .
H47A H 0.5629 0.9535 0.2206 0.080 Uiso 1 1 calc R . .
H47B H 0.4437 0.9376 0.1921 0.080 Uiso 1 1 calc R . .
H47C H 0.4934 1.0398 0.1721 0.080 Uiso 1 1 calc R . .
C48 C 1.1673(6) 0.7840(5) 0.1130(3) 0.0313(14) Uani 1 1 d . . .
H48 H 1.1543 0.7181 0.1352 0.038 Uiso 1 1 calc R . .
C49 C 1.2671(7) 0.7399(7) 0.0488(3) 0.052(2) Uani 1 1 d . . .
H49A H 1.2240 0.7061 0.0241 0.078 Uiso 1 1 calc R . .
H49B H 1.3570 0.6825 0.0540 0.078 Uiso 1 1 calc R . .
H49C H 1.2847 0.8026 0.0269 0.078 Uiso 1 1 calc R . .
C50 C 1.2310(8) 0.8380(7) 0.1525(4) 0.054(2) Uani 1 1 d . . .
H50A H 1.3262 0.7843 0.1539 0.080 Uiso 1 1 calc R . .
H50B H 1.1707 0.8577 0.1953 0.080 Uiso 1 1 calc R . .
H50C H 1.2373 0.9067 0.1335 0.080 Uiso 1 1 calc R . .
C51 C 0.9093(6) 0.7165(5) 0.2121(3) 0.0277(14) Uani 1 1 d . . .
H51 H 0.8886 0.7738 0.2439 0.033 Uiso 1 1 calc R . .
C52 C 0.9384(6) 0.6064(5) 0.2209(3) 0.0261(14) Uani 1 1 d . . .
H52 H 0.9417 0.5733 0.2601 0.031 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
Bi1 B1 2.317(9) . ?
Bi1 Bi1 2.7956(6) 2_556 ?
N1 C26 1.387(8) . ?
N1 B1 1.414(9) . ?
N1 C1 1.440(7) . ?
C1 C2 1.391(8) . ?
C1 C6 1.403(8) . ?
B1 N2 1.430(10) . ?
C20A C19A 1.529(8) . ?
C21A C19A 1.530(8) . ?
C19A C18 1.538(8) . ?
Bi2 B2 2.326(7) . ?
Bi2 Bi2 2.8015(6) 2_765 ?
N2 C25 1.405(9) . ?
N2 C13 1.426(9) . ?
C2 C3 1.397(9) . ?
C2 C10 1.526(9) . ?
B2 N4 1.424(8) . ?
B2 N3 1.433(8) . ?
N3 C52 1.390(7) . ?
N3 C27 1.427(7) . ?
C3 C4 1.365(10) . ?
N4 C51 1.395(7) . ?
N4 C39 1.439(8) . ?
C4 C5 1.379(9) . ?
C5 C6 1.393(9) . ?
C6 C7 1.519(9) . ?
C7 C9 1.518(9) . ?
C7 C8 1.542(10) . ?
C10 C11 1.504(11) . ?
C10 C12 1.523(11) . ?
C13 C14 1.340(12) . ?
C13 C18 1.449(13) . ?
C14 C15 1.409(7) . ?
C14 C22 1.515(14) . ?
C15 C16 1.360(15) . ?
C16 C17 1.327(16) . ?
C17 C18 1.370(14) . ?
C18 C19 1.494(8) . ?
C19 C21 1.509(7) . ?
C19 C20 1.511(8) . ?
C22 C24 1.523(12) . ?
C22 C23 1.539(14) . ?
C25 C26 1.341(9) . ?
C27 C32 1.396(8) . ?
C27 C28 1.408(8) . ?
C28 C29 1.394(9) . ?
C28 C36 1.514(8) . ?
C29 C30 1.386(9) . ?
C30 C31 1.377(10) . ?
C31 C32 1.385(9) . ?
C32 C33 1.532(9) . ?
C33 C35 1.506(9) . ?
C33 C34 1.512(9) . ?
C36 C37 1.527(9) . ?
C36 C38 1.531(10) . ?
C39 C40 1.406(8) . ?
C39 C44 1.413(8) . ?
C40 C41 1.380(9) . ?
C40 C48 1.523(9) . ?
C41 C42 1.382(9) . ?
C42 C43 1.372(9) . ?
C43 C44 1.373(9) . ?
C44 C45 1.525(9) . ?
C45 C47 1.515(9) . ?
C45 C46 1.546(10) . ?
C48 C49 1.516(9) . ?
C48 C50 1.522(9) . ?
C51 C52 1.341(9) . ?

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
B1 Bi1 Bi1 92.19(18) . 2_556 ?
C26 N1 B1 108.5(5) . . ?
C26 N1 C1 121.6(5) . . ?
B1 N1 C1 129.2(6) . . ?
C2 C1 C6 122.5(6) . . ?
C2 C1 N1 118.3(5) . . ?
C6 C1 N1 119.2(5) . . ?
N1 B1 N2 105.3(6) . . ?
N1 B1 Bi1 126.2(5) . . ?
N2 B1 Bi1 128.4(5) . . ?
C20A C19A C21A 109.1(8) . . ?
C20A C19A C18 126(2) . . ?
C21A C19A C18 113.1(19) . . ?
B2 Bi2 Bi2 97.66(18) . 2_765 ?
C25 N2 C13 120.3(6) . . ?
C25 N2 B1 107.8(6) . . ?
C13 N2 B1 131.9(7) . . ?
C1 C2 C3 117.8(6) . . ?
C1 C2 C10 122.1(6) . . ?
C3 C2 C10 120.1(6) . . ?
N4 B2 N3 103.9(5) . . ?
N4 B2 Bi2 120.6(5) . . ?
N3 B2 Bi2 135.5(5) . . ?
C52 N3 C27 122.1(5) . . ?
C52 N3 B2 108.6(5) . . ?
C27 N3 B2 128.9(5) . . ?
C4 C3 C2 121.0(6) . . ?
C51 N4 B2 109.5(5) . . ?
C51 N4 C39 121.5(5) . . ?
B2 N4 C39 128.6(5) . . ?
C3 C4 C5 120.2(6) . . ?
C4 C5 C6 121.7(6) . . ?
C5 C6 C1 116.7(6) . . ?
C5 C6 C7 121.7(6) . . ?
C1 C6 C7 121.5(5) . . ?
C9 C7 C6 113.1(6) . . ?
C9 C7 C8 110.5(6) . . ?
C6 C7 C8 111.1(5) . . ?
C11 C10 C12 110.8(7) . . ?
C11 C10 C2 110.9(6) . . ?
C12 C10 C2 110.9(7) . . ?
C14 C13 N2 122.3(9) . . ?
C14 C13 C18 119.5(8) . . ?
N2 C13 C18 118.1(8) . . ?
C13 C14 C15 121.2(10) . . ?
C13 C14 C22 117.8(7) . . ?
C15 C14 C22 120.9(10) . . ?
C16 C15 C14 114.1(11) . . ?
C17 C16 C15 129.7(12) . . ?
C16 C17 C18 115.2(12) . . ?
C17 C18 C13 119.8(10) . . ?
C17 C18 C19 116.1(11) . . ?
C13 C18 C19 122.3(8) . . ?
C17 C18 C19A 113.2(14) . . ?
C13 C18 C19A 122.4(12) . . ?
C19 C18 C19A 34.3(11) . . ?
C18 C19 C21 112.8(12) . . ?
C18 C19 C20 100.4(13) . . ?
C21 C19 C20 112.6(7) . . ?
C14 C22 C24 113.9(10) . . ?
C14 C22 C23 114.5(8) . . ?
C24 C22 C23 108.1(8) . . ?
C26 C25 N2 108.6(6) . . ?
C25 C26 N1 109.8(6) . . ?
C32 C27 C28 121.7(6) . . ?
C32 C27 N3 119.9(5) . . ?
C28 C27 N3 118.3(5) . . ?
C29 C28 C27 117.9(5) . . ?
C29 C28 C36 119.2(6) . . ?
C27 C28 C36 122.8(6) . . ?
C30 C29 C28 120.3(6) . . ?
C31 C30 C29 120.7(7) . . ?
C30 C31 C32 120.8(6) . . ?
C31 C32 C27 118.4(6) . . ?
C31 C32 C33 120.2(5) . . ?
C27 C32 C33 121.4(6) . . ?
C35 C33 C34 110.3(6) . . ?
C35 C33 C32 112.1(6) . . ?
C34 C33 C32 111.9(6) . . ?
C28 C36 C37 112.9(6) . . ?
C28 C36 C38 109.8(6) . . ?
C37 C36 C38 110.6(6) . . ?
C40 C39 C44 121.2(6) . . ?
C40 C39 N4 118.8(5) . . ?
C44 C39 N4 120.0(5) . . ?
C41 C40 C39 117.8(6) . . ?
C41 C40 C48 120.4(5) . . ?
C39 C40 C48 121.8(6) . . ?
C40 C41 C42 122.0(6) . . ?
C43 C42 C41 118.8(7) . . ?
C42 C43 C44 122.7(6) . . ?
C43 C44 C39 117.5(6) . . ?
C43 C44 C45 120.7(6) . . ?
C39 C44 C45 121.8(6) . . ?
C47 C45 C44 111.5(5) . . ?
C47 C45 C46 110.4(6) . . ?
C44 C45 C46 110.9(6) . . ?
C49 C48 C50 110.6(6) . . ?
C49 C48 C40 111.1(5) . . ?
C50 C48 C40 111.0(5) . . ?
C52 C51 N4 108.3(5) . . ?
C51 C52 N3 109.7(5) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.50
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         1.582
_refine_diff_density_min         -1.312
_refine_diff_density_rms         0.140
