#------------------------------------------------------------------------------
#$Date: 2016-03-26 01:49:11 +0100 (Sat 26 de Mar de 2016) $
#$Revision: 180156 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/52/7105249.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_7105249
loop_
_publ_author_name
'Geier, Stephen J'
'Stephan, Douglas W'
_publ_section_title
;
 Lewis acid mediated P-P bond hydrogenation and hydrosilylation.
;
_journal_issue                   7
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              1026
_journal_page_last               1028
_journal_paper_doi               10.1039/b925126j
_journal_volume                  46
_journal_year                    2010
_chemical_formula_sum            'C30 H21 B F15 P Si'
_chemical_formula_weight         736.34
_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
_cell_angle_alpha                95.866(3)
_cell_angle_beta                 99.447(3)
_cell_angle_gamma                105.895(2)
_cell_formula_units_Z            2
_cell_length_a                   9.5286(7)
_cell_length_b                   9.8618(7)
_cell_length_c                   17.2444(13)
_cell_measurement_reflns_used    7604
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      0.00
_cell_measurement_theta_min      0.00
_cell_volume                     1518.74(19)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0541
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            5223
_diffrn_reflns_theta_full        25.13
_diffrn_reflns_theta_max         25.13
_diffrn_reflns_theta_min         2.17
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.245
_exptl_absorpt_correction_T_max  0.7446
_exptl_absorpt_correction_T_min  0.6617
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.610
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             740
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.458
_refine_diff_density_min         -0.382
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     438
_refine_ls_number_reflns         5223
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0966
_refine_ls_R_factor_gt           0.0675
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0375P)²+9.4876P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1697
_refine_ls_wR_factor_ref         0.1828
_reflns_number_gt                3831
_reflns_number_total             5223
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b925126j.txt
_cod_data_source_block           sjg42_0ma
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7105249
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
P1 P 0.14716(15) 0.41981(15) 0.26393(8) 0.0174(3) Uani 1 1 d . . .
Si1 Si -0.04228(17) 0.51879(17) 0.28455(9) 0.0225(4) Uani 1 1 d . . .
B1 B 0.1567(7) 0.2148(6) 0.2803(4) 0.0198(13) Uani 1 1 d . . .
F2 F -0.1173(3) 0.1828(4) 0.16892(19) 0.0290(8) Uani 1 1 d . . .
F3 F -0.3916(3) 0.0225(4) 0.1721(2) 0.0361(9) Uani 1 1 d . . .
F4 F -0.4389(4) -0.1275(4) 0.2943(2) 0.0369(9) Uani 1 1 d . . .
F5 F -0.2071(4) -0.1071(4) 0.4144(2) 0.0409(9) Uani 1 1 d . . .
F6 F 0.0629(4) 0.0485(4) 0.4125(2) 0.0340(8) Uani 1 1 d . . .
F8 F 0.4003(4) 0.0755(4) 0.30927(19) 0.0306(8) Uani 1 1 d . . .
F9 F 0.5778(4) 0.0948(4) 0.4468(2) 0.0363(9) Uani 1 1 d . . .
F10 F 0.5694(4) 0.2722(4) 0.5772(2) 0.0393(9) Uani 1 1 d . . .
F11 F 0.3685(4) 0.4210(4) 0.56669(19) 0.0351(9) Uani 1 1 d . . .
F12 F 0.1785(4) 0.3944(4) 0.42962(18) 0.0283(8) Uani 1 1 d . . .
F14 F 0.4339(3) 0.3499(4) 0.23956(19) 0.0293(8) Uani 1 1 d . . .
F15 F 0.5344(4) 0.2882(5) 0.1094(2) 0.0478(11) Uani 1 1 d . . .
F16 F 0.3684(5) 0.0638(6) -0.0044(2) 0.0642(14) Uani 1 1 d . . .
F17 F 0.1053(5) -0.1025(5) 0.0198(2) 0.0556(12) Uani 1 1 d . . .
F18 F 0.0047(4) -0.0475(4) 0.1486(2) 0.0338(8) Uani 1 1 d . . .
C1 C -0.0098(6) 0.1231(6) 0.2888(3) 0.0184(11) Uani 1 1 d . . .
C2 C -0.1349(6) 0.1097(6) 0.2308(3) 0.0198(12) Uani 1 1 d . . .
C3 C -0.2773(6) 0.0293(6) 0.2307(3) 0.0248(13) Uani 1 1 d . . .
C4 C -0.3018(6) -0.0451(6) 0.2932(4) 0.0242(13) Uani 1 1 d . . .
C5 C -0.1847(7) -0.0351(6) 0.3533(4) 0.0271(13) Uani 1 1 d . . .
C6 C -0.0435(6) 0.0471(6) 0.3505(3) 0.0209(12) Uani 1 1 d . . .
C7 C 0.2806(6) 0.2364(6) 0.3608(3) 0.0174(11) Uani 1 1 d . . .
C8 C 0.3862(6) 0.1631(6) 0.3712(3) 0.0226(12) Uani 1 1 d . . .
C9 C 0.4802(6) 0.1722(6) 0.4417(3) 0.0253(13) Uani 1 1 d . . .
C10 C 0.4777(6) 0.2593(6) 0.5072(3) 0.0251(13) Uani 1 1 d . . .
C11 C 0.3758(6) 0.3365(6) 0.5023(3) 0.0254(13) Uani 1 1 d . . .
C12 C 0.2814(6) 0.3224(6) 0.4301(3) 0.0219(12) Uani 1 1 d . . .
C13 C 0.2107(6) 0.1604(6) 0.2000(3) 0.0199(12) Uani 1 1 d . . .
C14 C 0.3468(6) 0.2370(6) 0.1856(3) 0.0212(12) Uani 1 1 d . . .
C15 C 0.4012(6) 0.2069(7) 0.1188(4) 0.0323(15) Uani 1 1 d . . .
C16 C 0.3198(7) 0.0941(8) 0.0623(4) 0.0392(17) Uani 1 1 d . . .
C17 C 0.1860(7) 0.0106(7) 0.0738(4) 0.0358(16) Uani 1 1 d . . .
C18 C 0.1349(6) 0.0443(6) 0.1416(3) 0.0241(13) Uani 1 1 d . . .
C19 C 0.1966(6) 0.4744(6) 0.1714(3) 0.0228(12) Uani 1 1 d . . .
C20 C 0.1175(6) 0.3993(6) 0.0976(3) 0.0246(13) Uani 1 1 d . . .
H20A H 0.0348 0.3175 0.0943 0.030 Uiso 1 1 calc R . .
C21 C 0.1587(7) 0.4430(8) 0.0292(4) 0.0393(17) Uani 1 1 d . . .
H21A H 0.1042 0.3915 -0.0213 0.047 Uiso 1 1 calc R . .
C22 C 0.2789(8) 0.5616(9) 0.0339(4) 0.050(2) Uani 1 1 d . . .
H22A H 0.3071 0.5922 -0.0133 0.060 Uiso 1 1 calc R . .
C23 C 0.3571(8) 0.6348(8) 0.1068(4) 0.0485(19) Uani 1 1 d . . .
H23A H 0.4398 0.7164 0.1096 0.058 Uiso 1 1 calc R . .
C24 C 0.3191(7) 0.5933(7) 0.1758(4) 0.0331(15) Uani 1 1 d . . .
H24A H 0.3754 0.6447 0.2260 0.040 Uiso 1 1 calc R . .
C25 C -0.1987(6) 0.4031(7) 0.3225(4) 0.0331(15) Uani 1 1 d . . .
H25A H -0.2792 0.4490 0.3199 0.040 Uiso 1 1 calc R . .
H25B H -0.2386 0.3109 0.2861 0.040 Uiso 1 1 calc R . .
C26 C -0.1606(7) 0.3724(7) 0.4065(4) 0.0371(16) Uani 1 1 d . . .
H26A H -0.2499 0.3116 0.4205 0.056 Uiso 1 1 calc R . .
H26B H -0.1236 0.4624 0.4436 0.056 Uiso 1 1 calc R . .
H26C H -0.0836 0.3235 0.4096 0.056 Uiso 1 1 calc R . .
C27 C -0.1127(7) 0.5621(7) 0.1855(4) 0.0361(16) Uani 1 1 d . . .
H27A H -0.0281 0.6224 0.1663 0.043 Uiso 1 1 calc R . .
H27B H -0.1558 0.4725 0.1471 0.043 Uiso 1 1 calc R . .
C28 C -0.2312(8) 0.6402(9) 0.1878(5) 0.0499(19) Uani 1 1 d . . .
H28A H -0.2638 0.6607 0.1345 0.075 Uiso 1 1 calc R . .
H28B H -0.1888 0.7299 0.2250 0.075 Uiso 1 1 calc R . .
H28C H -0.3167 0.5800 0.2053 0.075 Uiso 1 1 calc R . .
C29 C 0.0558(7) 0.6815(6) 0.3596(4) 0.0287(14) Uani 1 1 d . . .
H29A H -0.0196 0.7201 0.3793 0.034 Uiso 1 1 calc R . .
H29B H 0.1130 0.6537 0.4054 0.034 Uiso 1 1 calc R . .
C30 C 0.1618(7) 0.7992(7) 0.3283(4) 0.0384(16) Uani 1 1 d . . .
H30A H 0.2091 0.8804 0.3710 0.058 Uiso 1 1 calc R . .
H30B H 0.1059 0.8299 0.2840 0.058 Uiso 1 1 calc R . .
H30C H 0.2385 0.7629 0.3098 0.058 Uiso 1 1 calc R . .
H1 H 0.260(6) 0.514(6) 0.310(3) 0.020(14) Uiso 1 1 d . . .
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'
F F 0.0171 0.0103 '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'
P P 0.1023 0.0942 '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
_geom_angle_publ_flag
C19 P1 B1 114.6(3) . . ?
C19 P1 Si1 105.11(18) . . ?
B1 P1 Si1 126.97(18) . . ?
C27 Si1 C29 112.6(3) . . ?
C27 Si1 C25 110.3(3) . . ?
C29 Si1 C25 109.6(3) . . ?
C27 Si1 P1 104.6(2) . . ?
C29 Si1 P1 103.6(2) . . ?
C25 Si1 P1 115.8(2) . . ?
C7 B1 C1 112.6(5) . . ?
C7 B1 C13 112.6(4) . . ?
C1 B1 C13 114.9(4) . . ?
C7 B1 P1 105.8(4) . . ?
C1 B1 P1 107.0(4) . . ?
C13 B1 P1 102.9(4) . . ?
C2 C1 C6 112.6(5) . . ?
C2 C1 B1 121.5(5) . . ?
C6 C1 B1 125.8(5) . . ?
F2 C2 C3 116.1(5) . . ?
F2 C2 C1 118.2(5) . . ?
C3 C2 C1 125.7(5) . . ?
F3 C3 C2 121.7(5) . . ?
F3 C3 C4 119.9(5) . . ?
C2 C3 C4 118.4(5) . . ?
F4 C4 C5 120.5(5) . . ?
F4 C4 C3 120.2(5) . . ?
C5 C4 C3 119.3(5) . . ?
F5 C5 C4 119.8(5) . . ?
F5 C5 C6 120.2(5) . . ?
C4 C5 C6 120.0(5) . . ?
F6 C6 C5 114.8(5) . . ?
F6 C6 C1 121.3(5) . . ?
C5 C6 C1 124.0(5) . . ?
C12 C7 C8 112.7(5) . . ?
C12 C7 B1 122.0(5) . . ?
C8 C7 B1 125.0(5) . . ?
F8 C8 C9 115.7(5) . . ?
F8 C8 C7 120.0(5) . . ?
C9 C8 C7 124.3(5) . . ?
F9 C9 C10 119.2(5) . . ?
F9 C9 C8 120.2(5) . . ?
C10 C9 C8 120.6(5) . . ?
F10 C10 C9 122.3(5) . . ?
F10 C10 C11 118.6(5) . . ?
C9 C10 C11 119.1(5) . . ?
F11 C11 C12 121.2(5) . . ?
F11 C11 C10 120.4(5) . . ?
C12 C11 C10 118.3(5) . . ?
F12 C12 C11 115.9(5) . . ?
F12 C12 C7 119.0(5) . . ?
C11 C12 C7 125.0(5) . . ?
C18 C13 C14 113.4(5) . . ?
C18 C13 B1 127.8(5) . . ?
C14 C13 B1 118.9(5) . . ?
F14 C14 C15 116.4(5) . . ?
F14 C14 C13 119.1(5) . . ?
C15 C14 C13 124.5(5) . . ?
F15 C15 C16 120.0(5) . . ?
F15 C15 C14 120.4(6) . . ?
C16 C15 C14 119.5(6) . . ?
F16 C16 C15 121.0(6) . . ?
F16 C16 C17 119.8(6) . . ?
C15 C16 C17 119.2(6) . . ?
F17 C17 C16 120.3(5) . . ?
F17 C17 C18 120.0(6) . . ?
C16 C17 C18 119.6(6) . . ?
F18 C18 C17 114.9(5) . . ?
F18 C18 C13 121.3(5) . . ?
C17 C18 C13 123.7(5) . . ?
C20 C19 C24 119.5(5) . . ?
C20 C19 P1 121.7(4) . . ?
C24 C19 P1 118.7(4) . . ?
C21 C20 C19 120.1(5) . . ?
C20 C21 C22 120.1(6) . . ?
C23 C22 C21 119.6(6) . . ?
C22 C23 C24 121.6(6) . . ?
C23 C24 C19 119.1(6) . . ?
C26 C25 Si1 116.1(4) . . ?
C28 C27 Si1 112.9(5) . . ?
C30 C29 Si1 114.3(4) . . ?
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
P1 C19 1.827(6) . ?
P1 B1 2.093(6) . ?
P1 Si1 2.333(2) . ?
Si1 C27 1.865(6) . ?
Si1 C29 1.865(6) . ?
Si1 C25 1.868(6) . ?
B1 C7 1.622(8) . ?
B1 C1 1.635(8) . ?
B1 C13 1.644(8) . ?
F2 C2 1.355(6) . ?
F3 C3 1.340(6) . ?
F4 C4 1.341(6) . ?
F5 C5 1.344(7) . ?
F6 C6 1.344(6) . ?
F8 C8 1.352(6) . ?
F9 C9 1.354(6) . ?
F10 C10 1.342(6) . ?
F11 C11 1.342(7) . ?
F12 C12 1.359(6) . ?
F14 C14 1.350(6) . ?
F15 C15 1.348(7) . ?
F16 C16 1.344(7) . ?
F17 C17 1.336(7) . ?
F18 C18 1.352(6) . ?
C1 C2 1.390(7) . ?
C1 C6 1.393(8) . ?
C2 C3 1.371(8) . ?
C3 C4 1.381(8) . ?
C4 C5 1.366(8) . ?
C5 C6 1.379(8) . ?
C7 C12 1.391(8) . ?
C7 C8 1.391(8) . ?
C8 C9 1.365(8) . ?
C9 C10 1.355(8) . ?
C10 C11 1.386(8) . ?
C11 C12 1.381(8) . ?
C13 C18 1.386(8) . ?
C13 C14 1.386(8) . ?
C14 C15 1.376(8) . ?
C15 C16 1.359(9) . ?
C16 C17 1.373(9) . ?
C17 C18 1.383(8) . ?
C19 C20 1.387(8) . ?
C19 C24 1.395(8) . ?
C20 C21 1.377(8) . ?
C21 C22 1.379(10) . ?
C22 C23 1.368(10) . ?
C23 C24 1.370(9) . ?
C25 C26 1.517(9) . ?
C27 C28 1.535(9) . ?
C29 C30 1.524(9) . ?
