#------------------------------------------------------------------------------
#$Date: 2017-10-13 14:42:48 +0300 (Fri, 13 Oct 2017) $
#$Revision: 201982 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/30/80/4308065.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_4308065
loop_
_publ_author_name
'Silke Courtenay'
'Denise Walsh'
'Sarah Hawkeswood'
'Pingrong Wei'
'Anjan Kumar Das'
'Douglas W. Stephan'
_publ_section_title
;
Boron and Aluminum Complexes of Sterically Demanding Phosphinimines and
Phosphinimides
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3623
_journal_page_last               3631
_journal_paper_doi               10.1021/ic0700351
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C30 H28 B F15 N P'
_chemical_formula_weight         729.31
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 91.77(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.384(18)
_cell_length_b                   12.84(2)
_cell_length_c                   21.46(4)
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.0
_cell_volume                     3135(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_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  0.0905
_diffrn_reflns_av_sigmaI/netI    0.0601
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            13287
_diffrn_reflns_theta_full        23.32
_diffrn_reflns_theta_max         23.32
_diffrn_reflns_theta_min         2.39
_exptl_absorpt_coefficient_mu    0.200
_exptl_absorpt_correction_T_max  0.145152
_exptl_absorpt_correction_T_min  0.065342
_exptl_absorpt_correction_type   empirical
_exptl_crystal_density_diffrn    1.545
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1480
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.319
_refine_diff_density_min         -0.329
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.979
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         4451
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.979
_refine_ls_R_factor_all          0.0671
_refine_ls_R_factor_gt           0.0499
_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)+(0.0860P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1234
_refine_ls_wR_factor_ref         0.1344
_reflns_number_gt                3308
_reflns_number_total             4451
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0700351si20070111_011533_2.cif
_cod_data_source_block           (t-Bu3PNH)B(C6F5)3
_cod_database_code               4308065
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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 0.20925(6) 0.85218(5) 0.23131(3) 0.0359(2) Uani 1 1 d . . .
N1 N 0.25788(18) 0.76187(16) 0.18391(9) 0.0351(5) Uani 1 1 d . . .
H1A H 0.2854 0.7131 0.2076 0.042 Uiso 1 1 calc R . .
F1 F 0.07863(15) 0.57224(15) 0.09909(9) 0.0664(5) Uani 1 1 d . . .
F2 F -0.0999(2) 0.5807(2) 0.01944(13) 0.1089(9) Uani 1 1 d . . .
F3 F -0.1316(2) 0.7515(2) -0.05724(13) 0.1253(10) Uani 1 1 d . . .
F4 F 0.0194(2) 0.91560(19) -0.04635(9) 0.0974(8) Uani 1 1 d . . .
F5 F 0.19469(17) 0.91275(14) 0.03653(8) 0.0646(5) Uani 1 1 d . . .
F6 F 0.49749(13) 0.72304(14) 0.18332(7) 0.0562(5) Uani 1 1 d . . .
F7 F 0.70023(17) 0.8079(2) 0.15570(12) 0.0996(8) Uani 1 1 d . . .
F8 F 0.7290(2) 0.9054(2) 0.04332(14) 0.1191(10) Uani 1 1 d . . .
F9 F 0.5451(2) 0.90872(15) -0.04192(9) 0.0910(8) Uani 1 1 d . . .
F10 F 0.34688(18) 0.81502(15) -0.01867(7) 0.0692(5) Uani 1 1 d . . .
F11 F 0.33775(17) 0.60660(14) 0.00420(7) 0.0636(5) Uani 1 1 d . . .
F12 F 0.38541(19) 0.40491(16) -0.00871(9) 0.0802(6) Uani 1 1 d . . .
F13 F 0.38267(19) 0.27371(14) 0.09231(10) 0.0800(6) Uani 1 1 d . . .
F14 F 0.32995(17) 0.35249(13) 0.20613(9) 0.0692(5) Uani 1 1 d . . .
F15 F 0.28488(16) 0.55306(13) 0.22148(7) 0.0568(5) Uani 1 1 d . . .
B1 B 0.2776(3) 0.7229(2) 0.11349(12) 0.0358(7) Uani 1 1 d . . .
C1 C 0.2411(3) 0.7949(3) 0.31200(12) 0.0507(8) Uani 1 1 d . . .
C2 C 0.2313(4) 0.8775(3) 0.36488(14) 0.0822(12) Uani 1 1 d . . .
H2A H 0.2479 0.8451 0.4045 0.123 Uiso 1 1 calc R . .
H2B H 0.1532 0.9058 0.3642 0.123 Uiso 1 1 calc R . .
H2C H 0.2868 0.9325 0.3585 0.123 Uiso 1 1 calc R . .
C3 C 0.1571(3) 0.7037(3) 0.32614(14) 0.0664(9) Uani 1 1 d . . .
H3A H 0.1753 0.6768 0.3671 0.100 Uiso 1 1 calc R . .
H3B H 0.1665 0.6494 0.2959 0.100 Uiso 1 1 calc R . .
H3C H 0.0774 0.7281 0.3242 0.100 Uiso 1 1 calc R . .
C4 C 0.3664(3) 0.7468(3) 0.31628(14) 0.0635(9) Uani 1 1 d . . .
H4A H 0.3807 0.7185 0.3572 0.095 Uiso 1 1 calc R . .
H4B H 0.4235 0.7998 0.3084 0.095 Uiso 1 1 calc R . .
H4C H 0.3724 0.6923 0.2859 0.095 Uiso 1 1 calc R . .
C5 C 0.2885(3) 0.9813(2) 0.22237(13) 0.0488(7) Uani 1 1 d . . .
C6 C 0.2939(3) 1.0100(2) 0.15289(14) 0.0602(9) Uani 1 1 d . . .
H6A H 0.3337 1.0754 0.1487 0.090 Uiso 1 1 calc R . .
H6B H 0.2155 1.0156 0.1354 0.090 Uiso 1 1 calc R . .
H6C H 0.3357 0.9568 0.1313 0.090 Uiso 1 1 calc R . .
C7 C 0.4166(3) 0.9711(3) 0.24705(18) 0.0698(10) Uani 1 1 d . . .
H7A H 0.4562 1.0366 0.2425 0.105 Uiso 1 1 calc R . .
H7B H 0.4560 0.9185 0.2238 0.105 Uiso 1 1 calc R . .
H7C H 0.4173 0.9520 0.2903 0.105 Uiso 1 1 calc R . .
C8 C 0.2302(3) 1.0727(3) 0.25687(18) 0.0722(10) Uani 1 1 d . . .
H8A H 0.2742 1.1354 0.2504 0.108 Uiso 1 1 calc R . .
H8B H 0.2292 1.0576 0.3007 0.108 Uiso 1 1 calc R . .
H8C H 0.1512 1.0818 0.2410 0.108 Uiso 1 1 calc R . .
C9 C 0.0450(2) 0.8705(2) 0.21963(13) 0.0478(7) Uani 1 1 d . . .
C10 C 0.0157(3) 0.9422(3) 0.16341(14) 0.0616(9) Uani 1 1 d . . .
H10A H -0.0679 0.9499 0.1587 0.092 Uiso 1 1 calc R . .
H10B H 0.0459 0.9119 0.1263 0.092 Uiso 1 1 calc R . .
H10C H 0.0511 1.0092 0.1704 0.092 Uiso 1 1 calc R . .
C11 C -0.0108(3) 0.7626(3) 0.20616(16) 0.0641(9) Uani 1 1 d . . .
H11A H -0.0943 0.7702 0.2001 0.096 Uiso 1 1 calc R . .
H11B H 0.0055 0.7170 0.2408 0.096 Uiso 1 1 calc R . .
H11C H 0.0217 0.7338 0.1692 0.096 Uiso 1 1 calc R . .
C12 C -0.0144(3) 0.9193(3) 0.27712(16) 0.0688(10) Uani 1 1 d . . .
H12A H -0.0972 0.9266 0.2685 0.103 Uiso 1 1 calc R . .
H12B H 0.0193 0.9866 0.2856 0.103 Uiso 1 1 calc R . .
H12C H -0.0018 0.8750 0.3127 0.103 Uiso 1 1 calc R . .
C13 C 0.1572(2) 0.7376(2) 0.06844(11) 0.0415(7) Uani 1 1 d . . .
C14 C 0.0729(3) 0.6583(2) 0.06238(13) 0.0521(8) Uani 1 1 d . . .
C15 C -0.0230(3) 0.6614(3) 0.02183(17) 0.0701(10) Uani 1 1 d . . .
C16 C -0.0409(4) 0.7459(4) -0.01577(16) 0.0808(12) Uani 1 1 d . . .
C17 C 0.0354(3) 0.8299(3) -0.01087(13) 0.0666(10) Uani 1 1 d . . .
C18 C 0.1296(3) 0.8242(2) 0.03161(13) 0.0511(8) Uani 1 1 d . . .
C19 C 0.4025(2) 0.7754(2) 0.08747(12) 0.0407(7) Uani 1 1 d . . .
C20 C 0.5017(2) 0.7725(2) 0.12693(13) 0.0458(7) Uani 1 1 d . . .
C21 C 0.6099(3) 0.8145(3) 0.11371(17) 0.0645(9) Uani 1 1 d . . .
C22 C 0.6260(3) 0.8620(3) 0.0576(2) 0.0731(10) Uani 1 1 d . . .
C23 C 0.5341(4) 0.8640(2) 0.01513(16) 0.0641(10) Uani 1 1 d . . .
C24 C 0.4275(3) 0.8176(2) 0.02947(13) 0.0491(8) Uani 1 1 d . . .
C25 C 0.3094(2) 0.5947(2) 0.11358(11) 0.0392(6) Uani 1 1 d . . .
C26 C 0.3373(3) 0.5470(2) 0.05654(12) 0.0462(7) Uani 1 1 d . . .
C27 C 0.3614(3) 0.4428(2) 0.04866(14) 0.0536(8) Uani 1 1 d . . .
C28 C 0.3602(3) 0.3759(2) 0.09869(15) 0.0554(8) Uani 1 1 d . . .
C29 C 0.3330(3) 0.4168(2) 0.15619(14) 0.0483(7) Uani 1 1 d . . .
C30 C 0.3099(2) 0.5222(2) 0.16204(12) 0.0420(7) Uani 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'
N N 0.0061 0.0033 '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
N1 P1 C9 110.75(13) . . ?
N1 P1 C5 112.41(15) . . ?
C9 P1 C5 110.42(15) . . ?
N1 P1 C1 103.38(16) . . ?
C9 P1 C1 109.11(13) . . ?
C5 P1 C1 110.54(14) . . ?
B1 N1 P1 148.70(17) . . ?
N1 B1 C13 111.9(2) . . ?
N1 B1 C19 109.3(2) . . ?
C13 B1 C19 116.8(2) . . ?
N1 B1 C25 109.74(19) . . ?
C13 B1 C25 106.5(2) . . ?
C19 B1 C25 102.0(2) . . ?
C3 C1 C4 105.0(3) . . ?
C3 C1 C2 108.3(3) . . ?
C4 C1 C2 108.2(3) . . ?
C3 C1 P1 111.6(2) . . ?
C4 C1 P1 110.8(2) . . ?
C2 C1 P1 112.5(3) . . ?
C6 C5 C7 106.7(3) . . ?
C6 C5 C8 108.2(3) . . ?
C7 C5 C8 108.3(3) . . ?
C6 C5 P1 109.9(2) . . ?
C7 C5 P1 109.8(2) . . ?
C8 C5 P1 113.7(2) . . ?
C10 C9 C11 108.0(3) . . ?
C10 C9 C12 106.9(3) . . ?
C11 C9 C12 108.9(3) . . ?
C10 C9 P1 111.4(2) . . ?
C11 C9 P1 108.2(2) . . ?
C12 C9 P1 113.3(2) . . ?
C18 C13 C14 112.6(3) . . ?
C18 C13 B1 125.9(3) . . ?
C14 C13 B1 121.4(2) . . ?
F1 C14 C15 114.4(3) . . ?
F1 C14 C13 121.1(3) . . ?
C15 C14 C13 124.4(3) . . ?
F2 C15 C16 120.0(3) . . ?
F2 C15 C14 120.0(4) . . ?
C16 C15 C14 119.9(4) . . ?
F3 C16 C15 122.2(4) . . ?
F3 C16 C17 118.3(4) . . ?
C15 C16 C17 119.5(3) . . ?
F4 C17 C16 121.3(3) . . ?
F4 C17 C18 120.2(4) . . ?
C16 C17 C18 118.6(3) . . ?
F5 C18 C17 114.5(3) . . ?
F5 C18 C13 120.7(3) . . ?
C17 C18 C13 124.8(3) . . ?
C20 C19 C24 111.7(3) . . ?
C20 C19 B1 117.7(2) . . ?
C24 C19 B1 130.5(3) . . ?
F6 C20 C21 114.7(3) . . ?
F6 C20 C19 120.0(2) . . ?
C21 C20 C19 125.2(3) . . ?
F7 C21 C22 119.8(3) . . ?
F7 C21 C20 120.3(3) . . ?
C22 C21 C20 119.9(3) . . ?
F8 C22 C23 119.7(4) . . ?
F8 C22 C21 121.9(4) . . ?
C23 C22 C21 118.4(3) . . ?
F9 C23 C22 121.2(3) . . ?
F9 C23 C24 118.9(4) . . ?
C22 C23 C24 119.9(3) . . ?
F10 C24 C19 121.1(3) . . ?
F10 C24 C23 114.4(3) . . ?
C19 C24 C23 124.4(3) . . ?
C30 C25 C26 111.2(3) . . ?
C30 C25 B1 130.4(2) . . ?
C26 C25 B1 118.4(2) . . ?
F11 C26 C27 116.1(3) . . ?
F11 C26 C25 118.6(3) . . ?
C27 C26 C25 125.3(3) . . ?
F12 C27 C28 119.4(3) . . ?
F12 C27 C26 120.4(3) . . ?
C28 C27 C26 120.3(3) . . ?
F13 C28 C27 121.6(3) . . ?
F13 C28 C29 120.6(3) . . ?
C27 C28 C29 117.8(3) . . ?
F14 C29 C30 121.0(3) . . ?
F14 C29 C28 119.1(3) . . ?
C30 C29 C28 120.0(3) . . ?
F15 C30 C29 114.3(2) . . ?
F15 C30 C25 120.2(3) . . ?
C29 C30 C25 125.5(3) . . ?
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 N1 1.649(3) . ?
P1 C9 1.894(4) . ?
P1 C5 1.899(4) . ?
P1 C1 1.906(4) . ?
N1 B1 1.614(4) . ?
F1 C14 1.357(4) . ?
F2 C15 1.357(5) . ?
F3 C16 1.344(4) . ?
F4 C17 1.347(4) . ?
F5 C18 1.359(4) . ?
F6 C20 1.369(4) . ?
F7 C21 1.349(4) . ?
F8 C22 1.342(4) . ?
F9 C23 1.362(4) . ?
F10 C24 1.361(4) . ?
F11 C26 1.359(4) . ?
F12 C27 1.360(4) . ?
F13 C28 1.345(4) . ?
F14 C29 1.354(4) . ?
F15 C30 1.374(4) . ?
B1 C13 1.664(4) . ?
B1 C19 1.684(4) . ?
B1 C25 1.685(5) . ?
C1 C3 1.548(5) . ?
C1 C4 1.555(5) . ?
C1 C2 1.560(5) . ?
C5 C6 1.539(5) . ?
C5 C7 1.541(5) . ?
C5 C8 1.548(5) . ?
C9 C10 1.546(4) . ?
C9 C11 1.546(5) . ?
C9 C12 1.557(4) . ?
C13 C18 1.394(4) . ?
C13 C14 1.402(4) . ?
C14 C15 1.376(5) . ?
C15 C16 1.363(6) . ?
C16 C17 1.387(6) . ?
C17 C18 1.388(5) . ?
C19 C20 1.392(4) . ?
C19 C24 1.395(4) . ?
C20 C21 1.382(5) . ?
C21 C22 1.367(5) . ?
C22 C23 1.366(5) . ?
C23 C24 1.396(5) . ?
C25 C30 1.395(4) . ?
C25 C26 1.414(4) . ?
C26 C27 1.377(5) . ?
C27 C28 1.375(5) . ?
C28 C29 1.385(5) . ?
C29 C30 1.385(5) . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 21155837
