#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:42:24 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179760 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/56/7005687.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_7005687
loop_
_publ_author_name
'Welch, Gregory C.'
'Cabrera, Lourdes'
'Chase, Preston A.'
'Hollink, Emily'
'Masuda, Jason D.'
'Wei, Pingrong'
'Stephan, Douglas W.'
_publ_section_title
;
 Tuning Lewis acidity using the reactivity of "frustrated Lewis pairs":
 facile formation of phosphine-boranes and cationic
 phosphonium-boranes.
;
_journal_issue                   31
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3407
_journal_page_last               3414
_journal_paper_doi               10.1039/b704417h
_journal_year                    2007
_chemical_formula_sum            'C27 H22 B F14 P'
_chemical_formula_weight         654.23
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 91.0440(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.3212(7)
_cell_length_b                   16.4421(13)
_cell_length_c                   17.8541(14)
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.0
_cell_volume                     2735.9(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0327
_diffrn_reflns_av_sigmaI/netI    0.0227
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            25837
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.68
_exptl_absorpt_coefficient_mu    0.214
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.449990
_exptl_absorpt_correction_type   empirical
_exptl_crystal_density_diffrn    1.588
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1320
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.755
_refine_diff_density_min         -0.174
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     391
_refine_ls_number_reflns         4817
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0639
_refine_ls_R_factor_gt           0.0460
_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)+(0.0706P)²+0.8248P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1222
_refine_ls_wR_factor_ref         0.1376
_reflns_number_gt                3588
_reflns_number_total             4817
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b704417h.txt
_cod_data_source_block           iPr3PC6F4BH(C6F5)2
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7005687
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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 0.14494(7) 0.03911(4) 0.17946(4) 0.0528(2) Uani 1 1 d . . .
F1 F 0.6015(2) -0.18563(13) 0.14284(11) 0.0941(6) Uani 1 1 d . . .
F2 F 0.8540(2) -0.23914(15) 0.19284(13) 0.1124(7) Uani 1 1 d . . .
F3 F 1.0249(2) -0.33018(14) 0.10390(15) 0.1130(8) Uani 1 1 d . . .
F4 F 0.9321(2) -0.36967(13) -0.03653(14) 0.1056(7) Uani 1 1 d . . .
F5 F 0.67711(19) -0.31920(11) -0.08731(11) 0.0848(5) Uani 1 1 d . . .
F6 F 0.4552(2) -0.38450(10) 0.06573(10) 0.0805(5) Uani 1 1 d . . .
F7 F 0.3101(2) -0.51332(10) 0.01924(12) 0.0934(6) Uani 1 1 d . . .
F8 F 0.1445(2) -0.50700(12) -0.10753(12) 0.0937(6) Uani 1 1 d . . .
F9 F 0.1352(2) -0.36844(13) -0.18942(11) 0.0981(6) Uani 1 1 d . . .
F10 F 0.2804(2) -0.23639(11) -0.14385(10) 0.0825(5) Uani 1 1 d . . .
F11 F 0.3141(2) -0.25035(9) 0.12703(9) 0.0772(5) Uani 1 1 d . . .
F12 F 0.1700(2) -0.14310(10) 0.20270(9) 0.0800(5) Uani 1 1 d . . .
F13 F 0.27899(17) 0.05558(9) 0.01955(8) 0.0638(4) Uani 1 1 d . . .
F14 F 0.41319(16) -0.05161(9) -0.05585(8) 0.0629(4) Uani 1 1 d . . .
C1 C 0.6247(3) -0.24988(15) 0.02448(16) 0.0598(7) Uani 1 1 d . . .
C2 C 0.6786(3) -0.23181(18) 0.09548(17) 0.0679(7) Uani 1 1 d . . .
C3 C 0.8102(4) -0.2582(2) 0.12280(19) 0.0777(9) Uani 1 1 d . . .
C4 C 0.8960(3) -0.3046(2) 0.0781(2) 0.0795(9) Uani 1 1 d . . .
C5 C 0.8495(3) -0.32413(18) 0.0077(2) 0.0752(8) Uani 1 1 d . . .
C6 C 0.7170(3) -0.29710(17) -0.01705(18) 0.0662(7) Uani 1 1 d . . .
C7 C 0.3760(3) -0.30323(15) -0.03674(14) 0.0556(6) Uani 1 1 d . . .
C8 C 0.3765(3) -0.37622(16) 0.00186(15) 0.0595(7) Uani 1 1 d . . .
C9 C 0.3025(3) -0.44414(17) -0.02080(17) 0.0662(7) Uani 1 1 d . . .
C10 C 0.2203(3) -0.44148(18) -0.08535(18) 0.0677(8) Uani 1 1 d . . .
C11 C 0.2147(3) -0.37128(19) -0.12590(16) 0.0679(8) Uani 1 1 d . . .
C12 C 0.2909(3) -0.30434(17) -0.10123(15) 0.0609(7) Uani 1 1 d . . .
C13 C 0.3770(3) -0.15745(15) 0.03250(14) 0.0523(6) Uani 1 1 d . . .
C14 C 0.3064(3) -0.17419(15) 0.09828(15) 0.0583(6) Uani 1 1 d . . .
C15 C 0.2321(3) -0.11808(16) 0.13903(14) 0.0579(6) Uani 1 1 d . . .
C16 C 0.2195(3) -0.03690(15) 0.11684(13) 0.0513(6) Uani 1 1 d . . .
C17 C 0.2846(3) -0.01980(14) 0.04891(13) 0.0501(6) Uani 1 1 d . . .
C18 C 0.3571(3) -0.07780(15) 0.00945(13) 0.0505(6) Uani 1 1 d . . .
C19 C 0.1186(3) 0.13531(16) 0.12945(15) 0.0614(7) Uani 1 1 d . . .
H19A H 0.2084 0.1465 0.1037 0.074 Uiso 1 1 calc R . .
C20 C 0.0938(4) 0.20741(19) 0.18245(19) 0.0860(10) Uani 1 1 d . . .
H20A H 0.0813 0.2563 0.1536 0.129 Uiso 1 1 calc R . .
H20B H 0.1752 0.2134 0.2157 0.129 Uiso 1 1 calc R . .
H20C H 0.0094 0.1976 0.2111 0.129 Uiso 1 1 calc R . .
C21 C 0.0012(4) 0.13044(19) 0.06862(18) 0.0757(8) Uani 1 1 d . . .
H21A H -0.0075 0.1821 0.0439 0.113 Uiso 1 1 calc R . .
H21B H -0.0884 0.1166 0.0910 0.113 Uiso 1 1 calc R . .
H21C H 0.0259 0.0895 0.0327 0.113 Uiso 1 1 calc R . .
C22 C -0.0216(3) -0.00107(18) 0.21785(16) 0.0664(7) Uani 1 1 d . . .
H22A H 0.0062 -0.0452 0.2521 0.080 Uiso 1 1 calc R . .
C23 C -0.1215(4) -0.0386(2) 0.1588(2) 0.0885(10) Uani 1 1 d . . .
H23A H -0.2063 -0.0586 0.1824 0.133 Uiso 1 1 calc R . .
H23B H -0.0734 -0.0827 0.1346 0.133 Uiso 1 1 calc R . .
H23C H -0.1478 0.0019 0.1224 0.133 Uiso 1 1 calc R . .
C24 C -0.1005(4) 0.0623(3) 0.2651(2) 0.0982(11) Uani 1 1 d . . .
H24A H -0.1866 0.0388 0.2842 0.147 Uiso 1 1 calc R . .
H24B H -0.1245 0.1085 0.2345 0.147 Uiso 1 1 calc R . .
H24C H -0.0395 0.0793 0.3061 0.147 Uiso 1 1 calc R . .
C25 C 0.2777(3) 0.05683(19) 0.25435(15) 0.0673(7) Uani 1 1 d . . .
H25A H 0.2412 0.1016 0.2849 0.081 Uiso 1 1 calc R . .
C26 C 0.4188(4) 0.0859(3) 0.2211(2) 0.1068(14) Uani 1 1 d . . .
H26A H 0.4876 0.0956 0.2608 0.160 Uiso 1 1 calc R . .
H26B H 0.4025 0.1354 0.1938 0.160 Uiso 1 1 calc R . .
H26C H 0.4549 0.0451 0.1880 0.160 Uiso 1 1 calc R . .
C27 C 0.3004(4) -0.0148(3) 0.3063(2) 0.0986(12) Uani 1 1 d . . .
H27A H 0.3706 -0.0009 0.3442 0.148 Uiso 1 1 calc R . .
H27B H 0.3337 -0.0606 0.2782 0.148 Uiso 1 1 calc R . .
H27C H 0.2115 -0.0283 0.3295 0.148 Uiso 1 1 calc R . .
B1 B 0.4717(3) -0.22248(18) -0.01521(17) 0.0563(7) Uani 1 1 d . . .
H1 H 0.515(3) -0.191(2) -0.0784(19) 0.096 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'
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
C16 P1 C25 107.30(13) . . ?
C16 P1 C19 110.03(12) . . ?
C25 P1 C19 107.57(13) . . ?
C16 P1 C22 108.50(13) . . ?
C25 P1 C22 110.53(13) . . ?
C19 P1 C22 112.77(14) . . ?
C6 C1 C2 113.0(3) . . ?
C6 C1 B1 117.8(2) . . ?
C2 C1 B1 129.2(3) . . ?
F1 C2 C3 115.8(3) . . ?
F1 C2 C1 120.2(3) . . ?
C3 C2 C1 124.1(3) . . ?
F2 C3 C4 120.0(3) . . ?
F2 C3 C2 120.5(3) . . ?
C4 C3 C2 119.5(3) . . ?
F3 C4 C5 120.7(3) . . ?
F3 C4 C3 120.0(3) . . ?
C5 C4 C3 119.3(3) . . ?
F4 C5 C4 119.9(3) . . ?
F4 C5 C6 120.8(3) . . ?
C4 C5 C6 119.3(3) . . ?
F5 C6 C5 116.2(3) . . ?
F5 C6 C1 119.0(3) . . ?
C5 C6 C1 124.8(3) . . ?
C8 C7 C12 113.5(2) . . ?
C8 C7 B1 126.0(2) . . ?
C12 C7 B1 120.4(2) . . ?
F6 C8 C9 115.5(2) . . ?
F6 C8 C7 120.3(2) . . ?
C9 C8 C7 124.2(3) . . ?
F7 C9 C8 120.7(3) . . ?
F7 C9 C10 119.8(3) . . ?
C8 C9 C10 119.5(3) . . ?
F8 C10 C11 120.5(3) . . ?
F8 C10 C9 120.3(3) . . ?
C11 C10 C9 119.2(3) . . ?
F9 C11 C10 119.5(3) . . ?
F9 C11 C12 121.0(3) . . ?
C10 C11 C12 119.5(3) . . ?
F10 C12 C11 116.6(2) . . ?
F10 C12 C7 119.4(2) . . ?
C11 C12 C7 124.0(3) . . ?
C14 C13 C18 112.2(2) . . ?
C14 C13 B1 125.5(2) . . ?
C18 C13 B1 122.3(2) . . ?
F11 C14 C15 116.4(2) . . ?
F11 C14 C13 118.9(2) . . ?
C15 C14 C13 124.7(2) . . ?
F12 C15 C14 118.1(2) . . ?
F12 C15 C16 119.7(2) . . ?
C14 C15 C16 122.2(2) . . ?
C17 C16 C15 113.8(2) . . ?
C17 C16 P1 124.88(19) . . ?
C15 C16 P1 120.82(19) . . ?
F13 C17 C18 117.1(2) . . ?
F13 C17 C16 120.7(2) . . ?
C18 C17 C16 122.2(2) . . ?
F14 C18 C17 115.0(2) . . ?
F14 C18 C13 120.3(2) . . ?
C17 C18 C13 124.7(2) . . ?
C21 C19 C20 111.3(2) . . ?
C21 C19 P1 112.89(19) . . ?
C20 C19 P1 112.7(2) . . ?
C23 C22 C24 111.2(3) . . ?
C23 C22 P1 113.5(2) . . ?
C24 C22 P1 112.2(2) . . ?
C27 C25 C26 111.7(3) . . ?
C27 C25 P1 114.2(2) . . ?
C26 C25 P1 110.0(2) . . ?
C13 B1 C7 110.7(2) . . ?
C13 B1 C1 115.3(2) . . ?
C7 B1 C1 110.1(2) . . ?
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 C16 1.823(3) . ?
P1 C25 1.828(3) . ?
P1 C19 1.831(3) . ?
P1 C22 1.832(3) . ?
F1 C2 1.353(3) . ?
F2 C3 1.346(4) . ?
F3 C4 1.346(4) . ?
F4 C5 1.342(4) . ?
F5 C6 1.352(3) . ?
F6 C8 1.352(3) . ?
F7 C9 1.345(3) . ?
F8 C10 1.344(3) . ?
F9 C11 1.344(3) . ?
F10 C12 1.354(3) . ?
F11 C14 1.355(3) . ?
F12 C15 1.349(3) . ?
F13 C17 1.346(3) . ?
F14 C18 1.356(3) . ?
C1 C6 1.385(4) . ?
C1 C2 1.388(4) . ?
C1 B1 1.643(4) . ?
C2 C3 1.382(4) . ?
C3 C4 1.372(5) . ?
C4 C5 1.360(5) . ?
C5 C6 1.377(4) . ?
C7 C8 1.384(4) . ?
C7 C12 1.386(4) . ?
C7 B1 1.642(4) . ?
C8 C9 1.370(4) . ?
C9 C10 1.373(4) . ?
C10 C11 1.363(4) . ?
C11 C12 1.378(4) . ?
C13 C14 1.384(4) . ?
C13 C18 1.384(3) . ?
C13 B1 1.636(4) . ?
C14 C15 1.371(4) . ?
C15 C16 1.397(4) . ?
C16 C17 1.395(3) . ?
C17 C18 1.371(3) . ?
C19 C21 1.530(4) . ?
C19 C20 1.537(4) . ?
C22 C23 1.524(4) . ?
C22 C24 1.536(4) . ?
C25 C27 1.511(5) . ?
C25 C26 1.530(5) . ?
