#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/20/4072075.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_4072075
loop_
_publ_author_name
'Ochida, Atsuko'
'Hamasaka, Go'
'Yamauchi, Yoshihiro'
'Kawamorita, Soichiro'
'Oshima, Naoya'
'Hara, Kenji'
'Ohmiya, Hirohisa'
'Sawamura, Masaya'
_publ_section_title
;
 Synthesis, Properties, and Catalytic Applications of Caged, Compact
 Trialkylphosphine 4-Phenyl-1-phospha-4-silabicyclo[2.2.2]octane
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              5494
_journal_paper_doi               10.1021/om8005728
_journal_volume                  27
_journal_year                    2008
_chemical_formula_moiety         'C12 H20 B P Si '
_chemical_formula_sum            'C12 H20 B P Si'
_chemical_formula_weight         234.16
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_cell_angle_alpha                90
_cell_angle_beta                 97.056(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   6.3632(3)
_cell_length_b                   7.6482(3)
_cell_length_c                   13.6844(7)
_cell_measurement_reflns_used    7494
_cell_measurement_temperature    120.2
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.7
_cell_volume                     660.94(5)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        'teXsan Ver. 1.11'
_computing_publication_material  'teXsan Ver. 1.11'
_computing_structure_refinement  'teXsan Ver. 1.10'
_computing_structure_solution    SIR92
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.9994
_diffrn_measured_fraction_theta_max 0.9994
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID Imaging Plate'
_diffrn_measurement_method       ω
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.019
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            6031
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_exptl_absorpt_coefficient_mu    0.265
_exptl_absorpt_correction_T_max  0.987
_exptl_absorpt_correction_T_min  0.859
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Higashi, 1995)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.177
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.27
_refine_diff_density_min         -0.15
_refine_ls_abs_structure_Flack   0.6(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.265
_refine_ls_number_parameters     149
_refine_ls_number_reflns         1501
_refine_ls_R_factor_gt           0.0278
_refine_ls_shift/su_max          0.0004
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[σ²(Fo) + 0.00063|Fo|²]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0371
_reflns_number_gt                1501
_reflns_number_total             1631
_reflns_threshold_expression     F²>3.0σ(F²)
_cod_data_source_file            om8005728_si_002.cif
_cod_data_source_block           Ph-SMAP-BH3
_cod_original_cell_volume        660.93(5)
_cod_original_formula_sum        'C12 H20 B P Si '
_cod_database_code               4072075
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,1/2+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_calc_flag
P(1) P 0.69011(7) 0.249(1) 0.92794(3) 0.0180(1) Uani 1.00 d
Si(1) Si 0.70776(7) 0.266(1) 0.70780(3) 0.0196(1) Uani 1.00 d
C(1) C 0.8498(4) 0.078(1) 0.8814(2) 0.0216(5) Uani 1.00 d
C(2) C 0.8176(4) 0.059(1) 0.7668(2) 0.0261(5) Uani 1.00 d
C(3) C 0.4331(3) 0.225(1) 0.8530(1) 0.0217(4) Uani 1.00 d
C(4) C 0.4331(3) 0.280(1) 0.7436(1) 0.0246(5) Uani 1.00 d
C(5) C 0.8019(4) 0.451(1) 0.8854(2) 0.0219(5) Uani 1.00 d
C(6) C 0.8604(3) 0.444(1) 0.7788(2) 0.0219(5) Uani 1.00 d
C(7) C 0.7230(3) 0.277(1) 0.5725(1) 0.0230(4) Uani 1.00 d
C(8) C 0.5633(3) 0.211(1) 0.5033(2) 0.0307(5) Uani 1.00 d
C(9) C 0.5815(4) 0.219(1) 0.4031(1) 0.0343(6) Uani 1.00 d
C(10) C 0.7580(4) 0.290(1) 0.3707(1) 0.0367(6) Uani 1.00 d
C(11) C 0.9197(4) 0.356(1) 0.4381(2) 0.0384(6) Uani 1.00 d
C(12) C 0.9001(4) 0.351(1) 0.5377(2) 0.0309(5) Uani 1.00 d
B(1) B 0.6838(4) 0.233(1) 1.0677(1) 0.0234(5) Uani 1.00 d
H(1a) H 0.9951 0.1031 0.9017 0.0254 Uiso 1.00 calc
H(1bb) H 0.653(4) 0.093(4) 1.084(2) 0.029(6) Uiso 1.00 calc
H(1ba) H 0.830(4) 0.277(5) 1.101(2) 0.040(7) Uiso 1.00 calc
H(1bc) H 0.532(4) 0.314(4) 1.085(2) 0.045(8) Uiso 1.00 calc
H(1b) H 0.8154 -0.0314 0.9095 0.0254 Uiso 1.00 calc
H(2a) H 0.9504 0.0331 0.7443 0.0285 Uiso 1.00 calc
H(2b) H 0.7224 -0.0356 0.7488 0.0285 Uiso 1.00 calc
H(3a) H 0.3913 0.1030 0.8537 0.0262 Uiso 1.00 calc
H(3b) H 0.3311 0.2916 0.8813 0.0262 Uiso 1.00 calc
H(4a) H 0.3391 0.2050 0.7027 0.0294 Uiso 1.00 calc
H(4b) H 0.3818 0.3967 0.7365 0.0294 Uiso 1.00 calc
H(5a) H 0.6987 0.5396 0.8877 0.0256 Uiso 1.00 calc
H(5b) H 0.9244 0.4772 0.9286 0.0256 Uiso 1.00 calc
H(6a) H 0.8300 0.5527 0.7478 0.0273 Uiso 1.00 calc
H(6b) H 1.0094 0.4208 0.7817 0.0273 Uiso 1.00 calc
H(8) H 0.4393 0.1580 0.5236 0.0363 Uiso 1.00 calc
H(9) H 0.4704 0.1749 0.3544 0.0411 Uiso 1.00 calc
H(10) H 0.7704 0.2938 0.3016 0.0415 Uiso 1.00 calc
H(11) H 1.0428 0.4043 0.4141 0.0463 Uiso 1.00 calc
H(12) H 1.0118 0.3991 0.5838 0.0369 Uiso 1.00 calc
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.003 0.002
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
H H 0.000 0.000
;International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.2)
;
B B 0.001 0.001
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
P P 0.102 0.094
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
Si Si 0.082 0.070
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_publ_flag
C(1) P(1) C(3) 103.4(1) yes
C(1) P(1) C(5) 103.9(1) yes
C(1) P(1) B(1) 112.7(1) yes
C(3) P(1) C(5) 105.2(1) yes
C(3) P(1) B(1) 115.1(1) yes
C(5) P(1) B(1) 115.2(1) yes
C(2) Si(1) C(4) 104.3(1) yes
C(2) Si(1) C(6) 104.4(1) yes
C(2) Si(1) C(7) 113.8(1) yes
C(4) Si(1) C(6) 105.2(1) yes
C(4) Si(1) C(7) 114.81(10) yes
C(6) Si(1) C(7) 113.2(1) yes
P(1) C(1) C(2) 114.2(2) yes
Si(1) C(2) C(1) 110.3(2) yes
P(1) C(3) C(4) 114.0(1) yes
Si(1) C(4) C(3) 110.2(1) yes
P(1) C(5) C(6) 114.6(2) yes
Si(1) C(6) C(5) 110.2(2) yes
Si(1) C(7) C(8) 122.2(2) yes
Si(1) C(7) C(12) 120.0(2) yes
C(8) C(7) C(12) 117.8(2) yes
C(7) C(8) C(9) 120.6(2) yes
C(8) C(9) C(10) 120.5(2) yes
C(9) C(10) C(11) 120.0(2) yes
C(10) C(11) C(12) 119.6(2) yes
C(7) C(12) C(11) 121.5(2) yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
P(1) C(1) 1.816(3) yes
P(1) C(3) 1.829(2) yes
P(1) C(5) 1.828(3) yes
P(1) B(1) 1.922(2) yes
Si(1) C(2) 1.874(3) yes
Si(1) C(4) 1.875(2) yes
Si(1) C(6) 1.872(3) yes
Si(1) C(7) 1.868(2) yes
C(1) C(2) 1.564(3) yes
C(3) C(4) 1.556(3) yes
C(5) C(6) 1.551(3) yes
C(7) C(8) 1.398(3) yes
C(7) C(12) 1.397(3) yes
C(8) C(9) 1.391(3) yes
C(9) C(10) 1.370(4) yes
C(10) C(11) 1.389(4) yes
C(11) C(12) 1.384(3) yes
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_publ_flag
P(1) C(1) C(2) Si(1) 21.9(2) yes
P(1) C(3) C(4) Si(1) 23.6(2) yes
P(1) C(5) C(6) Si(1) 22.0(2) yes
Si(1) C(7) C(8) C(9) -179.1(2) yes
Si(1) C(7) C(12) C(11) 177.8(2) yes
C(1) P(1) C(3) C(4) -70.1(2) yes
C(1) P(1) C(5) C(6) 41.1(2) yes
C(1) C(2) Si(1) C(4) -67.9(2) yes
C(1) C(2) Si(1) C(6) 42.3(2) yes
C(1) C(2) Si(1) C(7) 166.2(2) yes
C(2) Si(1) C(4) C(3) 41.0(2) yes
C(2) Si(1) C(6) C(5) -68.0(2) yes
C(2) Si(1) C(7) C(8) 87.8(2) yes
C(2) Si(1) C(7) C(12) -91.0(2) yes
C(2) C(1) P(1) C(3) 41.5(2) yes
C(2) C(1) P(1) C(5) -68.2(2) yes
C(2) C(1) P(1) B(1) 166.4(2) yes
C(3) P(1) C(5) C(6) -67.3(2) yes
C(3) C(4) Si(1) C(6) -68.6(2) yes
C(3) C(4) Si(1) C(7) 166.3(2) yes
C(4) Si(1) C(6) C(5) 41.5(2) yes
C(4) Si(1) C(7) C(8) -32.4(3) yes
C(4) Si(1) C(7) C(12) 148.9(2) yes
C(4) C(3) P(1) C(5) 38.6(2) yes
C(4) C(3) P(1) B(1) 166.6(2) yes
C(5) C(6) Si(1) C(7) 167.7(2) yes
C(6) Si(1) C(7) C(8) -153.2(2) yes
C(6) Si(1) C(7) C(12) 28.0(3) yes
C(6) C(5) P(1) B(1) 164.8(2) yes
C(7) C(8) C(9) C(10) 1.1(4) yes
C(7) C(12) C(11) C(10) 1.5(5) yes
C(8) C(7) C(12) C(11) -1.0(4) yes
C(8) C(9) C(10) C(11) -0.6(5) yes
C(9) C(8) C(7) C(12) -0.3(4) yes
C(9) C(10) C(11) C(12) -0.7(5) yes
C(9) C(10) C(11) C(12) -0.7(5) yes
