#------------------------------------------------------------------------------
#$Date: 2016-03-21 18:55:18 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178829 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/83/4108378.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_4108378
loop_
_publ_author_name
'Stephen J. Geier'
'Thomas M. Gilbert'
'Douglas W. Stephan'
_publ_section_title
;
 Activation of H2 by Phosphinoboranes R2PB(C6F5)2
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12632
_journal_page_last               12633
_journal_paper_doi               10.1021/ja805493y
_journal_volume                  130
_journal_year                    2008
_chemical_formula_sum            'C16 H10 B F10 P'
_chemical_formula_weight         434.02
_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                67.072(2)
_cell_angle_beta                 80.770(3)
_cell_angle_gamma                67.852(2)
_cell_formula_units_Z            2
_cell_length_a                   9.699(2)
_cell_length_b                   9.703(2)
_cell_length_c                   10.404(2)
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.0
_cell_volume                     835.1(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0247
_diffrn_reflns_av_sigmaI/netI    0.0294
_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       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            8063
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.13
_exptl_absorpt_coefficient_mu    0.269
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.817894
_exptl_absorpt_correction_type   empirical
_exptl_crystal_density_diffrn    1.726
_exptl_crystal_F_000             432
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.292
_refine_diff_density_min         -0.165
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         2933
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0544
_refine_ls_R_factor_gt           0.0390
_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)+(0.0515P)²+0.2087P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0942
_refine_ls_wR_factor_ref         0.1029
_reflns_number_gt                2274
_reflns_number_total             2933
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja805493y_si_002_1.cif
_cod_data_source_block           '[(mu-Et2P)B(C6F5)2]2'
_cod_database_code               4108378
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
P1 P 0.13373(6) 0.87346(7) -0.00653(6) 0.03595(18) Uani 1 1 d .
F10 F 0.04167(16) 0.90171(16) 0.28090(14) 0.0522(4) Uani 1 1 d .
F1 F 0.37877(16) 1.02674(17) -0.15700(18) 0.0646(5) Uani 1 1 d .
F6 F 0.26032(18) 1.29067(18) 0.01272(15) 0.0627(4) Uani 1 1 d .
F7 F 0.36357(19) 1.2661(2) 0.2409(2) 0.0759(5) Uani 1 1 d .
F2 F 0.45589(19) 1.2136(2) -0.39856(18) 0.0753(5) Uani 1 1 d .
F5 F -0.06783(18) 1.44589(17) -0.15527(19) 0.0700(5) Uani 1 1 d .
F4 F 0.0051(2) 1.62763(19) -0.4013(2) 0.0853(6) Uani 1 1 d .
B1 B 0.0885(3) 1.0997(3) -0.0102(3) 0.0367(6) Uani 1 1 d .
C1 C 0.1399(3) 1.2180(3) -0.1538(2) 0.0383(5) Uani 1 1 d .
F9 F 0.14890(19) 0.87940(19) 0.50881(15) 0.0689(5) Uani 1 1 d .
C12 C 0.1227(3) 0.9954(3) 0.2639(3) 0.0423(6) Uani 1 1 d .
F8 F 0.3100(2) 1.0610(2) 0.49476(18) 0.0836(6) Uani 1 1 d .
C7 C 0.1473(2) 1.0942(3) 0.1311(2) 0.0382(5) Uani 1 1 d .
C8 C 0.2292(3) 1.1847(3) 0.1318(3) 0.0437(6) Uani 1 1 d .
C10 C 0.2578(3) 1.0731(3) 0.3776(3) 0.0535(7) Uani 1 1 d .
C11 C 0.1757(3) 0.9812(3) 0.3847(3) 0.0487(6) Uani 1 1 d .
C2 C 0.2763(3) 1.1719(3) -0.2189(3) 0.0439(6) Uani 1 1 d .
C13 C 0.2266(3) 0.8225(3) -0.1589(3) 0.0469(6) Uani 1 1 d .
H13A H 0.1817 0.9100 -0.2430 0.056 Uiso 1 1 calc R
H13B H 0.3304 0.8113 -0.1604 0.056 Uiso 1 1 calc R
F3 F 0.2700(2) 1.5157(2) -0.52625(18) 0.0926(6) Uani 1 1 d .
C6 C 0.0563(3) 1.3770(3) -0.2192(3) 0.0462(6) Uani 1 1 d .
C5 C 0.0956(3) 1.4762(3) -0.3432(3) 0.0549(7) Uani 1 1 d .
C3 C 0.3213(3) 1.2680(3) -0.3423(3) 0.0512(7) Uani 1 1 d .
C9 C 0.2839(3) 1.1747(3) 0.2507(3) 0.0519(7) Uani 1 1 d .
C4 C 0.2287(3) 1.4205(3) -0.4058(3) 0.0569(7) Uani 1 1 d .
C14 C 0.2181(3) 0.6694(3) -0.1612(3) 0.0652(8) Uani 1 1 d .
H14A H 0.2685 0.6506 -0.2433 0.098 Uiso 1 1 calc R
H14B H 0.1157 0.6801 -0.1621 0.098 Uiso 1 1 calc R
H14C H 0.2648 0.5814 -0.0797 0.098 Uiso 1 1 calc R
C15 C 0.2627(3) 0.7157(3) 0.1312(3) 0.0484(6) Uani 1 1 d .
H15A H 0.2146 0.7123 0.2211 0.058 Uiso 1 1 calc R
H15B H 0.2810 0.6140 0.1231 0.058 Uiso 1 1 calc R
C16 C 0.4117(3) 0.7348(4) 0.1290(3) 0.0696(8) Uani 1 1 d .
H16A H 0.4713 0.6480 0.2043 0.104 Uiso 1 1 calc R
H16B H 0.3955 0.8338 0.1394 0.104 Uiso 1 1 calc R
H16C H 0.4623 0.7347 0.0418 0.104 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'
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'
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_3
C15 P1 C13 99.93(12) .
C15 P1 B1 113.93(11) .
C13 P1 B1 119.04(11) .
C15 P1 B1 120.10(11) 2_575
C13 P1 B1 112.94(11) 2_575
B1 P1 B1 92.30(10) 2_575
C1 B1 C7 113.62(18) .
C1 B1 P1 114.44(16) .
C7 B1 P1 111.08(16) .
C1 B1 P1 115.85(16) 2_575
C7 B1 P1 111.55(16) 2_575
P1 B1 P1 87.70(10) 2_575
C2 C1 C6 112.8(2) .
C2 C1 B1 123.2(2) .
C6 C1 B1 123.9(2) .
F10 C12 C11 115.1(2) .
F10 C12 C7 119.8(2) .
C11 C12 C7 125.1(2) .
C12 C7 C8 112.6(2) .
C12 C7 B1 123.1(2) .
C8 C7 B1 124.3(2) .
F6 C8 C9 114.9(2) .
F6 C8 C7 121.0(2) .
C9 C8 C7 124.1(2) .
F8 C10 C9 121.4(2) .
F8 C10 C11 119.8(3) .
C9 C10 C11 118.7(2) .
F9 C11 C12 121.0(2) .
F9 C11 C10 119.9(2) .
C12 C11 C10 119.1(2) .
F1 C2 C3 115.7(2) .
F1 C2 C1 119.7(2) .
C3 C2 C1 124.4(2) .
C14 C13 P1 114.12(18) .
C14 C13 H13A 108.7 .
P1 C13 H13A 108.7 .
C14 C13 H13B 108.7 .
P1 C13 H13B 108.7 .
H13A C13 H13B 107.6 .
F5 C6 C5 115.9(2) .
F5 C6 C1 119.4(2) .
C5 C6 C1 124.5(2) .
F4 C5 C4 120.1(2) .
F4 C5 C6 120.3(3) .
C4 C5 C6 119.5(2) .
F2 C3 C4 120.0(2) .
F2 C3 C2 120.6(2) .
C4 C3 C2 119.4(2) .
F7 C9 C10 119.9(2) .
F7 C9 C8 119.8(3) .
C10 C9 C8 120.3(2) .
F3 C4 C3 120.3(3) .
F3 C4 C5 120.5(3) .
C3 C4 C5 119.1(2) .
C13 C14 H14A 109.5 .
C13 C14 H14B 109.5 .
H14A C14 H14B 109.5 .
C13 C14 H14C 109.5 .
H14A C14 H14C 109.5 .
H14B C14 H14C 109.5 .
C16 C15 P1 115.17(18) .
C16 C15 H15A 108.5 .
P1 C15 H15A 108.5 .
C16 C15 H15B 108.5 .
P1 C15 H15B 108.5 .
H15A C15 H15B 107.5 .
C15 C16 H16A 109.5 .
C15 C16 H16B 109.5 .
H16A C16 H16B 109.5 .
C15 C16 H16C 109.5 .
H16A C16 H16C 109.5 .
H16B C16 H16C 109.5 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
P1 C15 1.840(2) .
P1 C13 1.840(2) .
P1 B1 2.056(3) .
P1 B1 2.058(3) 2_575
F10 C12 1.358(3) .
F1 C2 1.352(3) .
F6 C8 1.344(3) .
F7 C9 1.347(3) .
F2 C3 1.342(3) .
F5 C6 1.350(3) .
F4 C5 1.342(3) .
B1 C1 1.630(3) .
B1 C7 1.635(4) .
B1 P1 2.058(3) 2_575
C1 C2 1.382(3) .
C1 C6 1.384(3) .
F9 C11 1.342(3) .
C12 C11 1.373(3) .
C12 C7 1.385(3) .
F8 C10 1.340(3) .
C7 C8 1.391(3) .
C8 C9 1.378(4) .
C10 C9 1.359(4) .
C10 C11 1.378(4) .
C2 C3 1.380(3) .
C13 C14 1.527(3) .
C13 H13A 0.9700 .
C13 H13B 0.9700 .
F3 C4 1.341(3) .
C6 C5 1.374(3) .
C5 C4 1.364(4) .
C3 C4 1.363(4) .
C14 H14A 0.9600 .
C14 H14B 0.9600 .
C14 H14C 0.9600 .
C15 C16 1.519(4) .
C15 H15A 0.9700 .
C15 H15B 0.9700 .
C16 H16A 0.9600 .
C16 H16B 0.9600 .
C16 H16C 0.9600 .
