#------------------------------------------------------------------------------
#$Date: 2016-03-26 14:59:58 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180283 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/69/7116999.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7116999
loop_
_publ_author_name
'Deepak Dange'
'Amelia Davey'
'Joseph A. B. Abdalla'
'Simon Aldridge'
'Cameron Jones'
_publ_section_title
;
 Utilisation of a lithium boryl as a reducing agent in low oxidation state
 group 15 chemistry: synthesis and characterisation of an amido-distibene
 and a boryl-dibismuthene
;
_journal_name_full               Chem.Commun.
_journal_page_first              7128
_journal_paper_doi               10.1039/C5cc01772F
_journal_volume                  51
_journal_year                    2015
_chemical_formula_sum            'C38 H40 Br2 N Sb Si'
_chemical_formula_weight         820.37
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-02-27 deposited with the CCDC.
2015-03-21 downloaded from the CCDC.
;
_cell_angle_alpha                95.865(5)
_cell_angle_beta                 95.903(5)
_cell_angle_gamma                100.813(5)
_cell_formula_units_Z            2
_cell_length_a                   10.1762(6)
_cell_length_b                   11.2391(8)
_cell_length_c                   15.5145(8)
_cell_measurement_temperature    123(2)
_cell_volume                     1720.21(19)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Apex X8'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0338
_diffrn_reflns_av_sigmaI/netI    0.0429
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            13213
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         3.03
_exptl_absorpt_coefficient_mu    3.187
_exptl_absorpt_correction_T_max  0.741
_exptl_absorpt_correction_T_min  0.642
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sortav (Blessing)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.584
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             820
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.868
_refine_diff_density_min         -0.410
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     393
_refine_ls_number_reflns         6406
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0363
_refine_ls_R_factor_gt           0.0274
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0267P)²+0.4142P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0581
_refine_ls_wR_factor_ref         0.0619
_reflns_number_gt                5540
_reflns_number_total             6406
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5cc01772f2.cif
_cod_data_source_block           compound1c
_cod_original_cell_volume        1720.21(18)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7116999
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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 . .
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'
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
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) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
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) .
