#------------------------------------------------------------------------------
#$Date: 2016-02-18 14:25:00 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176728 $
#$URL: svn://www.crystallography.net/cod/cif/8/00/01/8000170.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_8000170
loop_
_publ_author_name
'Nakata, Norio'
'Sekiguchi, Akira'
_publ_section_title
;
 Thia- and Selenasilaboriranes and 1,3,2,4-Dioxasilaboretane from a Stable
 Silaborene
;
_journal_issue                   5
_journal_name_full               'Chemistry Letters'
_journal_page_first              662
_journal_paper_doi               10.1246/cl.2007.662
_journal_volume                  36
_journal_year                    2007
_chemical_formula_moiety         'C27 H60 B N S Si3'
_chemical_formula_sum            'C27 H60 B N S Si3'
_chemical_formula_weight         525.90
_chemical_name_common            'SIBS ring'
_chemical_name_systematic
; 
 SiBS
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      11
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 104.666(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.4940(3)
_cell_length_b                   17.5210(11)
_cell_length_c                   11.4580(7)
_cell_measurement_temperature    120(2)
_cell_volume                     1649.66(16)
_computing_cell_refinement       'HKL scalepack'
_computing_data_collection       'MacScience Xpress'
_computing_data_reduction        Denzo
_computing_molecular_graphics    ORTEP
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.945
_diffrn_measured_fraction_theta_max 0.945
_diffrn_measurement_device_type  'MacScience DIP2030 Image plate'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0275
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            3006
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         2.17
_exptl_absorpt_coefficient_mu    0.223
_exptl_absorpt_correction_T_max  0.9464
_exptl_absorpt_correction_T_min  0.9065
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            paleyellow
_exptl_crystal_density_diffrn    1.059
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             584
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.250
_refine_diff_density_min         -0.266
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     287
_refine_ls_number_reflns         3006
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0549
_refine_ls_R_factor_gt           0.0479
_refine_ls_shift/su_max          0.027
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0753P)²+0.5998P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1236
_refine_ls_wR_factor_ref         0.1290
_reflns_number_gt                2592
_reflns_number_total             3006
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            36-662sup1.cif
_cod_data_source_block           SiBS
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21/m'
_cod_database_code               8000170
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, 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
Si1 Si 0.31447(8) 0.2500 0.84030(6) 0.03046(19) Uani 1 2 d S . .
S1 S 0.58216(8) 0.2500 0.88419(6) 0.0442(2) Uani 1 2 d S A .
B1 B 0.4738(3) 0.2500 1.0019(3) 0.0342(6) Uani 1 2 d S A .
Si2 Si 0.2414(2) 0.37880(9) 0.77729(18) 0.0349(4) Uani 0.539(4) 1 d P A 3
C1 C 0.3850(5) 0.4382(2) 0.8914(4) 0.0572(12) Uani 0.539(4) 1 d P A 3
H1 H 0.4971 0.4261 0.8900 0.086 Uiso 0.539(4) 1 calc PR A 3
H2 H 0.3698 0.4275 0.9718 0.086 Uiso 0.539(4) 1 calc PR A 3
H3 H 0.3635 0.4924 0.8725 0.086 Uiso 0.539(4) 1 calc PR A 3
C2 C 0.2869(7) 0.4013(3) 0.6237(5) 0.0532(12) Uani 0.539(4) 1 d P A 3
C3 C 0.450(2) 0.3685(9) 0.6245(13) 0.149(7) Uani 0.539(4) 1 d P A 3
H4 H 0.4504 0.3138 0.6429 0.224 Uiso 0.539(4) 1 calc PR A 3
H5 H 0.5341 0.3943 0.6859 0.224 Uiso 0.539(4) 1 calc PR A 3
H6 H 0.4709 0.3757 0.5451 0.224 Uiso 0.539(4) 1 calc PR A 3
C4 C 0.1582(9) 0.3663(4) 0.5157(4) 0.101(2) Uani 0.539(4) 1 d P A 3
H7 H 0.1516 0.3111 0.5274 0.152 Uiso 0.539(4) 1 calc PR A 3
H8 H 0.1902 0.3763 0.4407 0.152 Uiso 0.539(4) 1 calc PR A 3
H9 H 0.0518 0.3896 0.5109 0.152 Uiso 0.539(4) 1 calc PR A 3
C5 C 0.295(2) 0.4858(6) 0.5985(11) 0.079(4) Uani 0.539(4) 1 d P A 3
H10 H 0.1879 0.5089 0.5923 0.119 Uiso 0.539(4) 1 calc PR A 3
H11 H 0.3259 0.4931 0.5226 0.119 Uiso 0.539(4) 1 calc PR A 3
H12 H 0.3757 0.5100 0.6645 0.119 Uiso 0.539(4) 1 calc PR A 3
C6 C 0.0218(6) 0.4015(3) 0.7813(5) 0.0494(11) Uani 0.539(4) 1 d P A 3
C7 C -0.1023(6) 0.3524(4) 0.7001(8) 0.120(3) Uani 0.539(4) 1 d P A 3
H13 H -0.0811 0.2987 0.7231 0.181 Uiso 0.539(4) 1 calc PR A 3
H14 H -0.0964 0.3595 0.6165 0.181 Uiso 0.539(4) 1 calc PR A 3
H15 H -0.2110 0.3666 0.7073 0.181 Uiso 0.539(4) 1 calc PR A 3
C8 C -0.013(2) 0.4847(9) 0.7568(16) 0.103(6) Uani 0.539(4) 1 d P A 3
H16 H 0.0691 0.5152 0.8130 0.154 Uiso 0.539(4) 1 calc PR A 3
H17 H -0.1212 0.4967 0.7678 0.154 Uiso 0.539(4) 1 calc PR A 3
H18 H -0.0103 0.4964 0.6738 0.154 Uiso 0.539(4) 1 calc PR A 3
C9 C 0.0072(17) 0.3844(9) 0.9112(12) 0.099(5) Uani 0.539(4) 1 d P A 3
H19 H 0.0841 0.4165 0.9688 0.149 Uiso 0.539(4) 1 calc PR A 3
H20 H 0.0322 0.3305 0.9301 0.149 Uiso 0.539(4) 1 calc PR A 3
H21 H -0.1039 0.3954 0.9165 0.149 Uiso 0.539(4) 1 calc PR A 3
Si3 Si 0.2011(3) 0.36310(12) 0.7324(2) 0.0441(5) Uani 0.461(4) 1 d P A 4
C10 C 0.0380(11) 0.3353(3) 0.5923(6) 0.121(4) Uani 0.461(4) 1 d P A 4
H22 H 0.0874 0.3057 0.5382 0.181 Uiso 0.461(4) 1 calc PR A 4
H23 H -0.0123 0.3814 0.5508 0.181 Uiso 0.461(4) 1 calc PR A 4
H24 H -0.0451 0.3043 0.6156 0.181 Uiso 0.461(4) 1 calc PR A 4
C11 C 0.3617(11) 0.4195(3) 0.6776(6) 0.0657(18) Uani 0.461(4) 1 d P A 4
C12 C 0.4953(8) 0.4538(4) 0.7793(7) 0.087(2) Uani 0.461(4) 1 d P A 4
H25 H 0.4463 0.4884 0.8275 0.131 Uiso 0.461(4) 1 calc PR A 4
H26 H 0.5720 0.4823 0.7448 0.131 Uiso 0.461(4) 1 calc PR A 4
H27 H 0.5532 0.4128 0.8309 0.131 Uiso 0.461(4) 1 calc PR A 4
C13 C 0.4464(15) 0.3675(5) 0.6058(10) 0.059(2) Uani 0.461(4) 1 d P A 4
H28 H 0.4929 0.3235 0.6553 0.089 Uiso 0.461(4) 1 calc PR A 4
H29 H 0.5334 0.3959 0.5829 0.089 Uiso 0.461(4) 1 calc PR A 4
H30 H 0.3673 0.3499 0.5329 0.089 Uiso 0.461(4) 1 calc PR A 4
C14 C 0.271(3) 0.4872(10) 0.5989(17) 0.124(7) Uani 0.461(4) 1 d P A 4
H31 H 0.2197 0.5198 0.6482 0.186 Uiso 0.461(4) 1 calc PR A 4
H32 H 0.1875 0.4668 0.5307 0.186 Uiso 0.461(4) 1 calc PR A 4
H33 H 0.3495 0.5173 0.5685 0.186 Uiso 0.461(4) 1 calc PR A 4
C15 C 0.0914(8) 0.4193(3) 0.8297(7) 0.0576(16) Uani 0.461(4) 1 d P A 4
C16 C -0.0309(16) 0.3672(8) 0.8671(13) 0.072(4) Uani 0.461(4) 1 d P A 4
H34 H 0.0260 0.3229 0.9104 0.108 Uiso 0.461(4) 1 calc PR A 4
H35 H -0.1121 0.3499 0.7951 0.108 Uiso 0.461(4) 1 calc PR A 4
H36 H -0.0851 0.3952 0.9198 0.108 Uiso 0.461(4) 1 calc PR A 4
C17 C 0.2159(8) 0.4487(3) 0.9476(5) 0.0715(17) Uani 0.461(4) 1 d P A 4
H37 H 0.2936 0.4838 0.9256 0.107 Uiso 0.461(4) 1 calc PR A 4
H38 H 0.2747 0.4052 0.9920 0.107 Uiso 0.461(4) 1 calc PR A 4
H39 H 0.1569 0.4755 0.9986 0.107 Uiso 0.461(4) 1 calc PR A 4
C18 C -0.016(2) 0.4888(11) 0.7640(12) 0.077(6) Uani 0.461(4) 1 d P A 4
H40 H 0.0531 0.5239 0.7320 0.115 Uiso 0.461(4) 1 calc PR A 4
H41 H -0.0627 0.5160 0.8219 0.115 Uiso 0.461(4) 1 calc PR A 4
H42 H -0.1033 0.4695 0.6976 0.115 Uiso 0.461(4) 1 calc PR A 4
N1 N 0.5227(3) 0.2500 1.12774(17) 0.0370(5) Uani 1 2 d S . .
C19 C 0.7043(4) 0.2594(13) 1.1906(3) 0.031(3) Uani 0.50 1 d P A -1
C20 C 0.7365(5) 0.2807(3) 1.3241(3) 0.0523(11) Uani 0.50 1 d P A -1
H43 H 0.8498 0.2658 1.3639 0.063 Uiso 0.50 1 calc PR A -1
H44 H 0.7306 0.3370 1.3292 0.063 Uiso 0.50 1 calc PR A -1
C21 C 0.6314(5) 0.2486(17) 1.3944(3) 0.0683(16) Uani 1 2 d S A -1
H59 H 0.6612 0.2684 1.4781 0.082 Uiso 0.50 1 calc PR A -1
H60 H 0.6382 0.1922 1.3965 0.082 Uiso 0.50 1 calc PR A -1
C22 C 0.4611(6) 0.2752(3) 1.3271(4) 0.073(2) Uani 0.50 1 d P A -1
H45 H 0.3836 0.2616 1.3754 0.087 Uiso 0.50 1 calc PR A -1
H46 H 0.4615 0.3315 1.3198 0.087 Uiso 0.50 1 calc PR A -1
C23 C 0.4021(4) 0.2410(6) 1.2029(3) 0.0413(16) Uani 0.50 1 d PD A -1
C24 C 0.7955(8) 0.3136(4) 1.1317(6) 0.0531(15) Uani 0.50 1 d P A -1
H47 H 0.7757 0.3010 1.0459 0.080 Uiso 0.50 1 calc PR A -1
H48 H 0.9122 0.3096 1.1702 0.080 Uiso 0.50 1 calc PR A -1
H49 H 0.7588 0.3659 1.1404 0.080 Uiso 0.50 1 calc PR A -1
C25 C 0.7737(8) 0.1766(4) 1.1817(6) 0.0474(14) Uani 0.50 1 d P A -1
H50 H 0.7159 0.1400 1.2204 0.071 Uiso 0.50 1 calc PR A -1
H51 H 0.8900 0.1757 1.2224 0.071 Uiso 0.50 1 calc PR A -1
H52 H 0.7585 0.1629 1.0966 0.071 Uiso 0.50 1 calc PR A -1
C26 C 0.2407(5) 0.2797(3) 1.1422(4) 0.0583(13) Uani 0.50 1 d P A -1
H53 H 0.2094 0.2662 1.0564 0.087 Uiso 0.50 1 calc PR A -1
H54 H 0.2531 0.3352 1.1506 0.087 Uiso 0.50 1 calc PR A -1
H55 H 0.1562 0.2625 1.1806 0.087 Uiso 0.50 1 calc PR A -1
C27 C 0.3749(6) 0.1549(3) 1.2105(5) 0.0667(13) Uani 0.50 1 d PD A -1
H56 H 0.4778 0.1302 1.2509 0.100 Uiso 0.50 1 calc PR A -1
H57 H 0.3354 0.1340 1.1290 0.100 Uiso 0.50 1 calc PR A -1
H58 H 0.2942 0.1455 1.2566 0.100 Uiso 0.50 1 calc PR A -1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'
S S 0.1246 0.1234 '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
B1 Si1 S1 50.96(8) . .
B1 Si1 Si2 109.96(6) . 4_565
S1 Si1 Si2 104.01(4) . 4_565
B1 Si1 Si2 109.96(6) . .
S1 Si1 Si2 104.01(4) . .
Si2 Si1 Si2 139.86(11) 4_565 .
B1 Si1 Si3 124.45(7) . 4_565
S1 Si1 Si3 111.95(6) . 4_565
Si2 Si1 Si3 14.50(3) 4_565 4_565
Si2 Si1 Si3 125.47(12) . 4_565
B1 Si1 Si3 124.45(7) . .
S1 Si1 Si3 111.95(6) . .
Si2 Si1 Si3 125.47(12) 4_565 .
Si2 Si1 Si3 14.50(3) . .
Si3 Si1 Si3 111.03(14) 4_565 .
B1 S1 Si1 58.73(9) . .
N1 B1 S1 133.9(2) . .
N1 B1 Si1 155.8(2) . .
S1 B1 Si1 70.31(10) . .
C1 Si2 C6 109.6(2) . .
C1 Si2 C2 106.1(3) . .
C6 Si2 C2 113.5(3) . .
C1 Si2 Si1 103.92(15) . .
C6 Si2 Si1 111.51(16) . .
C2 Si2 Si1 111.63(17) . .
C3 C2 C5 107.0(10) . .
C3 C2 C4 108.4(8) . .
C5 C2 C4 106.8(7) . .
C3 C2 Si2 108.3(6) . .
C5 C2 Si2 113.7(5) . .
C4 C2 Si2 112.4(4) . .
C7 C6 C8 111.7(8) . .
C7 C6 C9 105.7(7) . .
C8 C6 C9 107.8(10) . .
C7 C6 Si2 113.8(4) . .
C8 C6 Si2 110.2(7) . .
C9 C6 Si2 107.2(6) . .
C10 Si3 C15 105.6(4) . .
C10 Si3 C11 106.4(4) . .
C15 Si3 C11 114.9(3) . .
C10 Si3 Si1 109.5(2) . .
C15 Si3 Si1 108.5(2) . .
C11 Si3 Si1 111.6(3) . .
C12 C11 C13 106.6(7) . .
C12 C11 C14 107.6(9) . .
C13 C11 C14 111.7(9) . .
C12 C11 Si3 114.0(4) . .
C13 C11 Si3 110.0(5) . .
C14 C11 Si3 107.0(10) . .
C16 C15 C17 108.2(7) . .
C16 C15 C18 104.1(10) . .
C17 C15 C18 109.5(8) . .
C16 C15 Si3 109.0(8) . .
C17 C15 Si3 110.5(4) . .
C18 C15 Si3 115.2(7) . .
B1 N1 C23 121.6(2) . .
B1 N1 C23 121.6(2) . 4_565
C23 N1 C23 12.0(9) . 4_565
B1 N1 C19 119.0(2) . .
C23 N1 C19 119.4(2) . .
C23 N1 C19 118.0(3) 4_565 .
B1 N1 C19 119.0(2) . 4_565
C23 N1 C19 118.0(3) . 4_565
C23 N1 C19 119.4(2) 4_565 4_565
C19 N1 C19 12.3(17) . 4_565
C24 C19 C20 108.4(11) . .
C24 C19 N1 115.6(8) . .
C20 C19 N1 113.5(3) . .
C24 C19 C25 108.1(5) . .
C20 C19 C25 108.3(9) . .
N1 C19 C25 102.6(11) . .
C21 C20 C19 118.6(8) . .
C20 C21 C22 103.8(10) . .
C23 C22 C21 113.6(8) . .
N1 C23 C22 112.8(4) . .
N1 C23 C26 110.8(4) . .
C22 C23 C26 107.4(6) . .
N1 C23 C27 105.7(6) . .
C22 C23 C27 110.8(5) . .
C26 C23 C27 109.4(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Si1 B1 1.998(3) .
Si1 S1 2.2009(9) .
Si1 Si2 2.4026(14) 4_565
Si1 Si2 2.4026(14) .
Si1 Si3 2.4040(18) 4_565
Si1 Si3 2.4040(18) .
S1 B1 1.816(3) .
B1 N1 1.396(3) .
Si2 C1 1.864(4) .
Si2 C6 1.918(6) .
Si2 C2 1.935(5) .
C2 C3 1.495(18) .
C2 C5 1.513(13) .
C2 C4 1.555(8) .
C6 C7 1.491(8) .
C6 C8 1.499(17) .
C6 C9 1.554(15) .
Si3 C10 1.900(6) .
Si3 C15 1.899(7) .
Si3 C11 1.914(7) .
C11 C12 1.529(10) .
C11 C13 1.524(12) .
C11 C14 1.570(19) .
C15 C16 1.523(14) .
C15 C17 1.577(10) .
C15 C18 1.591(17) .
N1 C23 1.504(4) .
N1 C23 1.504(4) 4_565
N1 C19 1.537(4) .
N1 C19 1.537(4) 4_565
C19 C24 1.491(17) .
C19 C20 1.530(8) .
C19 C25 1.58(2) .
C20 C21 1.458(13) .
C21 C22 1.529(10) .
C22 C23 1.509(7) .
C23 C26 1.529(7) .
C23 C27 1.532(10) .
