#------------------------------------------------------------------------------
#$Date: 2016-03-21 14:49:46 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178725 $
#$URL: svn://www.crystallography.net/cod/cif/4/08/36/4083655.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_4083655
loop_
_publ_author_name
'Alhomaidan, Osamah'
'Hollink, Emily'
'Stephan, Douglas W.'
_publ_section_title
;
 Main Group Heterocycles from Lithiated Phosphinimines
;
_journal_issue                   12
_journal_name_full               Organometallics
_journal_page_first              3041
_journal_paper_doi               10.1021/om070154o
_journal_volume                  26
_journal_year                    2007
_chemical_formula_sum            'C36 H37 B F10 N P'
_chemical_formula_weight         715.45
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 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                 94.344(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.3506(19)
_cell_length_b                   23.052(4)
_cell_length_c                   12.2362(19)
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.0
_cell_volume                     3473.7(10)
_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  0.0341
_diffrn_reflns_av_sigmaI/netI    0.0382
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            16594
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.77
_exptl_absorpt_coefficient_mu    0.160
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.785328
_exptl_absorpt_correction_type   empirical
_exptl_crystal_density_diffrn    1.368
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1480
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.378
_refine_diff_density_min         -0.205
_refine_diff_density_rms         0.045
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   1.00(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     407
_refine_ls_number_reflns         6101
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0679
_refine_ls_R_factor_gt           0.0512
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0883P)²+1.3777P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1344
_refine_ls_wR_factor_ref         0.1490
_reflns_number_gt                4847
_reflns_number_total             6101
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om070154o.cif
_cod_data_source_block           '[(C6F5)2BCH2Pt-Bu2NPh]'
_cod_original_cell_volume        3473.7(9)
_cod_original_sg_symbol_H-M      Cc
_cod_database_code               4083655
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x, -y, z+1/2'
'x+1/2, y+1/2, 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
P1 P 0.50314(7) 0.37918(4) 0.66580(7) 0.0490(2) Uani 1 1 d .
N1 N 0.6339(2) 0.37726(12) 0.7098(2) 0.0458(6) Uani 1 1 d .
F1 F 0.5146(2) 0.23428(12) 0.9086(2) 0.0824(8) Uani 1 1 d .
F2 F 0.5585(3) 0.12202(13) 0.8907(3) 0.1096(11) Uani 1 1 d .
F3 F 0.7219(3) 0.08617(12) 0.7698(3) 0.1120(11) Uani 1 1 d .
F4 F 0.8386(2) 0.16592(13) 0.6666(2) 0.0924(8) Uani 1 1 d .
F5 F 0.79388(19) 0.27746(11) 0.6797(2) 0.0718(6) Uani 1 1 d .
F6 F 0.5051(2) 0.35823(14) 1.0179(2) 0.0838(7) Uani 1 1 d .
F7 F 0.6068(3) 0.37613(16) 1.2129(2) 0.1098(11) Uani 1 1 d .
F8 F 0.8263(3) 0.37535(13) 1.2406(2) 0.1048(11) Uani 1 1 d .
F9 F 0.9443(2) 0.35652(13) 1.0656(3) 0.0921(9) Uani 1 1 d .
F10 F 0.84347(18) 0.33529(11) 0.86871(19) 0.0728(6) Uani 1 1 d .
C1 C 0.4473(4) 0.45475(19) 0.6542(4) 0.0702(11) Uani 1 1 d .
C2 C 0.4389(6) 0.4780(3) 0.7699(5) 0.111(2) Uani 1 1 d .
H2A H 0.4101 0.5167 0.7662 0.166 Uiso 1 1 calc R
H2B H 0.5096 0.4784 0.8082 0.166 Uiso 1 1 calc R
H2C H 0.3915 0.4535 0.8081 0.166 Uiso 1 1 calc R
C3 C 0.3302(4) 0.4574(3) 0.6000(6) 0.0978(16) Uani 1 1 d .
H3A H 0.3061 0.4970 0.5964 0.147 Uiso 1 1 calc R
H3B H 0.2829 0.4351 0.6426 0.147 Uiso 1 1 calc R
H3C H 0.3288 0.4416 0.5272 0.147 Uiso 1 1 calc R
C4 C 0.5214(4) 0.4909(2) 0.5880(5) 0.0928(16) Uani 1 1 d .
H4A H 0.4938 0.5297 0.5812 0.139 Uiso 1 1 calc R
H4B H 0.5244 0.4742 0.5164 0.139 Uiso 1 1 calc R
H4C H 0.5930 0.4916 0.6245 0.139 Uiso 1 1 calc R
C5 C 0.4531(3) 0.33466(19) 0.5442(3) 0.0608(10) Uani 1 1 d .
C6 C 0.4696(4) 0.3631(2) 0.4327(3) 0.0781(13) Uani 1 1 d .
H6A H 0.4423 0.3379 0.3747 0.117 Uiso 1 1 calc R
H6B H 0.5456 0.3699 0.4267 0.117 Uiso 1 1 calc R
H6C H 0.4313 0.3994 0.4274 0.117 Uiso 1 1 calc R
C7 C 0.3306(4) 0.3216(3) 0.5501(4) 0.0874(14) Uani 1 1 d .
H7A H 0.3050 0.2987 0.4879 0.131 Uiso 1 1 calc R
H7B H 0.2909 0.3574 0.5500 0.131 Uiso 1 1 calc R
H7C H 0.3200 0.3006 0.6162 0.131 Uiso 1 1 calc R
C8 C 0.5093(4) 0.27511(19) 0.5516(4) 0.0733(12) Uani 1 1 d .
H8A H 0.4842 0.2519 0.4896 0.110 Uiso 1 1 calc R
H8B H 0.4924 0.2560 0.6178 0.110 Uiso 1 1 calc R
H8C H 0.5865 0.2803 0.5519 0.110 Uiso 1 1 calc R
C9 C 0.4788(3) 0.33894(19) 0.7849(3) 0.0592(9) Uani 1 1 d .
H9A H 0.4459 0.3614 0.8407 0.071 Uiso 1 1 calc R
H9B H 0.4401 0.3029 0.7701 0.071 Uiso 1 1 calc R
C10 C 0.6485(3) 0.26232(17) 0.7907(3) 0.0501(8) Uani 1 1 d .
C11 C 0.5931(3) 0.21955(18) 0.8441(3) 0.0610(10) Uani 1 1 d .
C12 C 0.6156(4) 0.16077(19) 0.8362(4) 0.0712(11) Uani 1 1 d .
C13 C 0.6969(4) 0.14274(19) 0.7761(4) 0.0737(13) Uani 1 1 d .
C14 C 0.7560(3) 0.18320(19) 0.7236(3) 0.0641(10) Uani 1 1 d .
C15 C 0.7316(3) 0.24124(17) 0.7325(3) 0.0546(9) Uani 1 1 d .
C16 C 0.6686(3) 0.34679(15) 0.9306(3) 0.0500(8) Uani 1 1 d .
C17 C 0.6145(4) 0.35679(19) 1.0231(3) 0.0629(10) Uani 1 1 d .
C18 C 0.6653(5) 0.36711(19) 1.1269(3) 0.0725(12) Uani 1 1 d .
C19 C 0.7749(5) 0.3669(2) 1.1406(3) 0.0759(13) Uani 1 1 d .
C20 C 0.8339(4) 0.35621(17) 1.0519(3) 0.0640(11) Uani 1 1 d .
C21 C 0.7810(3) 0.34621(17) 0.9509(3) 0.0570(9) Uani 1 1 d .
C22 C 0.7277(3) 0.41078(15) 0.6853(3) 0.0476(8) Uani 1 1 d .
C23 C 0.7687(3) 0.45470(16) 0.7582(3) 0.0611(10) Uani 1 1 d .
C24 C 0.8630(4) 0.4843(2) 0.7363(5) 0.0810(14) Uani 1 1 d .
H24A H 0.8906 0.5118 0.7865 0.097 Uiso 1 1 calc R
C25 C 0.9171(4) 0.4746(2) 0.6441(6) 0.0846(15) Uani 1 1 d .
C26 C 0.8746(3) 0.4335(2) 0.5726(4) 0.0718(12) Uani 1 1 d .
H26A H 0.9087 0.4272 0.5084 0.086 Uiso 1 1 calc R
C27 C 0.7834(3) 0.40069(17) 0.5905(3) 0.0534(8) Uani 1 1 d .
C28 C 0.7131(5) 0.4740(2) 0.8579(4) 0.0799(13) Uani 1 1 d .
H28A H 0.7551 0.5041 0.8952 0.120 Uiso 1 1 calc R
H28B H 0.7068 0.4417 0.9064 0.120 Uiso 1 1 calc R
H28C H 0.6420 0.4886 0.8355 0.120 Uiso 1 1 calc R
C29 C 1.0199(6) 0.5078(3) 0.6281(6) 0.123(2) Uiso 1 1 d .
H29A H 1.0477 0.4963 0.5602 0.185 Uiso 1 1 calc R
H29B H 1.0729 0.4996 0.6875 0.185 Uiso 1 1 calc R
H29C H 1.0045 0.5486 0.6262 0.185 Uiso 1 1 calc R
C30 C 0.7496(4) 0.3575(2) 0.5029(3) 0.0693(11) Uani 1 1 d .
H30A H 0.8000 0.3586 0.4469 0.104 Uiso 1 1 calc R
H30B H 0.6783 0.3670 0.4714 0.104 Uiso 1 1 calc R
H30C H 0.7489 0.3194 0.5342 0.104 Uiso 1 1 calc R
C31 C 0.1057(8) 0.3748(4) 0.8265(8) 0.148(3) Uiso 1 1 d .
H31A H 0.0768 0.4120 0.8282 0.178 Uiso 1 1 calc R
C32 C 0.1921(7) 0.3579(4) 0.9083(7) 0.140(3) Uiso 1 1 d .
H32A H 0.2198 0.3827 0.9636 0.168 Uiso 1 1 calc R
C33 C 0.2282(5) 0.3032(3) 0.8966(5) 0.0986(16) Uiso 1 1 d .
H33A H 0.2836 0.2898 0.9457 0.118 Uiso 1 1 calc R
C34 C 0.1886(6) 0.2681(3) 0.8189(6) 0.115(2) Uiso 1 1 d .
H34A H 0.2161 0.2306 0.8151 0.138 Uiso 1 1 calc R
C35 C 0.1053(7) 0.2861(4) 0.7414(7) 0.128(2) Uiso 1 1 d .
H35A H 0.0775 0.2618 0.6854 0.154 Uiso 1 1 calc R
C36 C 0.0691(8) 0.3390(4) 0.7524(7) 0.137(3) Uiso 1 1 d .
H36A H 0.0129 0.3515 0.7031 0.165 Uiso 1 1 calc R
B1 B 0.6122(3) 0.33107(19) 0.8071(3) 0.0472(9) 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
N1 P1 C9 86.59(16)
N1 P1 C5 119.76(16)
C9 P1 C5 107.5(2)
N1 P1 C1 113.07(18)
C9 P1 C1 117.7(2)
C5 P1 C1 110.56(19)
N1 P1 B1 43.23(14)
C9 P1 B1 44.07(15)
C5 P1 B1 117.11(17)
C1 P1 B1 132.20(17)
C22 N1 B1 132.8(3)
C22 N1 P1 133.9(2)
B1 N1 P1 92.56(19)
C4 C1 C2 112.9(5)
C4 C1 C3 109.4(4)
C2 C1 C3 104.9(4)
C4 C1 P1 108.5(3)
C2 C1 P1 107.8(3)
C3 C1 P1 113.3(3)
C8 C5 C6 110.0(4)
C8 C5 C7 105.2(4)
C6 C5 C7 108.6(4)
C8 C5 P1 108.8(3)
C6 C5 P1 114.3(3)
C7 C5 P1 109.5(3)
B1 C9 P1 87.9(2)
C15 C10 C11 113.8(4)
C15 C10 B1 128.0(3)
C11 C10 B1 118.2(3)
F1 C11 C12 116.5(4)
F1 C11 C10 120.1(4)
C12 C11 C10 123.5(4)
F2 C12 C13 120.2(4)
F2 C12 C11 119.9(4)
C13 C12 C11 119.8(4)
F3 C13 C12 120.8(5)
F3 C13 C14 120.0(5)
C12 C13 C14 119.2(4)
F4 C14 C13 119.6(4)
F4 C14 C15 120.6(4)
C13 C14 C15 119.7(4)
F5 C15 C14 115.6(3)
F5 C15 C10 120.5(3)
C14 C15 C10 123.9(4)
C17 C16 C21 113.2(3)
C17 C16 B1 126.2(3)
C21 C16 B1 120.4(3)
F6 C17 C16 120.8(4)
F6 C17 C18 114.8(4)
C16 C17 C18 124.4(4)
F7 C18 C19 119.9(4)
F7 C18 C17 120.8(5)
C19 C18 C17 119.3(4)
F8 C19 C18 120.6(5)
F8 C19 C20 120.1(5)
C18 C19 C20 119.3(4)
F9 C20 C21 121.0(4)
F9 C20 C19 119.2(4)
C21 C20 C19 119.8(4)
F10 C21 C20 116.5(4)
F10 C21 C16 119.5(3)
C20 C21 C16 124.0(4)
C27 C22 C23 117.5(3)
C27 C22 N1 122.1(3)
C23 C22 N1 120.4(3)
C24 C23 C22 119.5(4)
C24 C23 C28 116.7(4)
C22 C23 C28 123.8(4)
C25 C24 C23 123.0(5)
C26 C25 C24 116.9(4)
C26 C25 C29 123.6(6)
C24 C25 C29 119.4(6)
C25 C26 C27 123.5(5)
C26 C27 C22 119.5(4)
C26 C27 C30 115.7(4)
C22 C27 C30 124.8(3)
C36 C31 C32 120.9(10)
C33 C32 C31 113.9(9)
C34 C33 C32 123.1(7)
C33 C34 C35 121.1(7)
C36 C35 C34 116.3(8)
C31 C36 C35 124.5(10)
N1 B1 C16 116.2(3)
N1 B1 C9 91.4(3)
C16 B1 C9 118.0(3)
N1 B1 C10 118.1(3)
C16 B1 C10 102.7(3)
C9 B1 C10 110.9(3)
N1 B1 P1 44.21(14)
C16 B1 P1 137.4(3)
C9 B1 P1 47.99(16)
C10 B1 P1 119.9(2)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
P1 N1 1.664(3)
P1 C9 1.772(4)
P1 C5 1.874(4)
P1 C1 1.875(4)
P1 B1 2.384(4)
N1 C22 1.443(4)
N1 B1 1.635(5)
F1 C11 1.341(5)
F2 C12 1.346(5)
F3 C13 1.343(5)
F4 C14 1.339(5)
F5 C15 1.334(5)
F6 C17 1.348(5)
F7 C18 1.337(5)
F8 C19 1.349(5)
F9 C20 1.362(5)
F10 C21 1.337(4)
C1 C4 1.517(7)
C1 C2 1.525(7)
C1 C3 1.546(7)
C5 C8 1.538(6)
C5 C6 1.541(6)
C5 C7 1.549(6)
C9 B1 1.659(5)
C10 C15 1.381(5)
C10 C11 1.391(6)
C10 B1 1.663(6)
C11 C12 1.388(6)
C12 C13 1.354(7)
C13 C14 1.374(7)
C14 C15 1.378(6)
C16 C17 1.376(5)
C16 C21 1.391(5)
C16 B1 1.655(5)
C17 C18 1.394(6)
C18 C19 1.352(8)
C19 C20 1.373(7)
C20 C21 1.373(6)
C22 C27 1.412(5)
C22 C23 1.417(5)
C23 C24 1.393(6)
C23 C28 1.512(6)
C24 C25 1.371(8)
C25 C26 1.368(8)
C25 C29 1.508(8)
C26 C27 1.387(6)
C27 C30 1.499(6)
C31 C36 1.283(12)
C31 C32 1.459(13)
C32 C33 1.348(10)
C33 C34 1.315(9)
C34 C35 1.409(10)
C35 C36 1.309(11)
