#------------------------------------------------------------------------------
#$Date: 2019-03-05 10:52:05 +0200 (Tue, 05 Mar 2019) $
#$Revision: 213973 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/01/32/7013254.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_7013254
loop_
_publ_author_name
'Wei, Pingrong'
'Chan, Katie T. K.'
'Stephan, Douglas W.'
_publ_section_title
;
 Metallated triphenylphosphinimine complexes
;
_journal_issue                   19
_journal_name_full               'Dalton Transactions'
_journal_page_first              3804
_journal_paper_doi               10.1039/b305877h
_journal_year                    2003
_chemical_formula_sum            'C21 H23 B Cl2 N P Si'
_chemical_formula_weight         430.17
_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                 90.035(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.264(6)
_cell_length_b                   14.245(8)
_cell_length_c                   17.380(10)
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.0
_cell_volume                     2294(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_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  0.0530
_diffrn_reflns_av_sigmaI/netI    0.0821
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            9762
_diffrn_reflns_theta_full        23.34
_diffrn_reflns_theta_max         23.34
_diffrn_reflns_theta_min         2.34
_exptl_absorpt_coefficient_mu    0.411
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.729405
_exptl_absorpt_correction_type   sadabs
_exptl_crystal_density_diffrn    1.246
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             896
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.254
_refine_diff_density_min         -0.268
_refine_diff_density_rms         0.049
_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     244
_refine_ls_number_reflns         3289
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0975
_refine_ls_R_factor_gt           0.0452
_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)+(0.0337P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0810
_refine_ls_wR_factor_ref         0.0878
_reflns_number_gt                1835
_reflns_number_total             3289
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b305877h.txt
_cod_data_source_block           (o-C6H4PPh2NSiMe3)BCl2
_cod_original_cell_volume        2293(2)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7013254
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
B1 B -0.0207(5) 0.0380(3) 0.1701(2) 0.0438(12) Uani 1 1 d . . .
Cl1 Cl -0.15394(11) -0.06075(7) 0.14836(5) 0.0635(3) Uani 1 1 d . . .
Cl2 Cl -0.09266(12) 0.14640(7) 0.12207(6) 0.0685(3) Uani 1 1 d . . .
P1 P 0.14931(10) 0.01045(6) 0.28859(5) 0.0377(3) Uani 1 1 d . . .
N1 N -0.0048(3) 0.05180(17) 0.25966(13) 0.0387(7) Uani 1 1 d . . .
Si1 Si -0.13269(13) 0.11275(8) 0.31758(6) 0.0607(4) Uani 1 1 d . . .
C1 C 0.1356(4) 0.0091(2) 0.13945(18) 0.0369(9) Uani 1 1 d . . .
C2 C 0.2351(4) -0.0084(2) 0.19786(17) 0.0363(9) Uani 1 1 d . . .
C3 C 0.3758(4) -0.0391(2) 0.1834(2) 0.0476(10) Uani 1 1 d . . .
H3A H 0.4393 -0.0505 0.2238 0.057 Uiso 1 1 calc R . .
C4 C 0.4189(4) -0.0521(3) 0.1078(2) 0.0515(10) Uani 1 1 d . . .
H4A H 0.5125 -0.0717 0.0969 0.062 Uiso 1 1 calc R . .
C5 C 0.3220(5) -0.0359(2) 0.0488(2) 0.0529(11) Uani 1 1 d . . .
H5A H 0.3508 -0.0455 -0.0018 0.063 Uiso 1 1 calc R . .
C6 C 0.1827(4) -0.0056(3) 0.06363(18) 0.0501(10) Uani 1 1 d . . .
H6A H 0.1196 0.0051 0.0229 0.060 Uiso 1 1 calc R . .
C7 C 0.1324(4) -0.0997(2) 0.33897(17) 0.0397(9) Uani 1 1 d . . .
C8 C -0.0012(5) -0.1435(3) 0.3434(2) 0.0564(11) Uani 1 1 d . . .
H8A H -0.0822 -0.1142 0.3227 0.068 Uiso 1 1 calc R . .
C9 C -0.0154(6) -0.2313(3) 0.3785(2) 0.0779(14) Uani 1 1 d . . .
H9A H -0.1054 -0.2601 0.3810 0.093 Uiso 1 1 calc R . .
C10 C 0.1031(7) -0.2750(3) 0.4093(2) 0.0779(15) Uani 1 1 d . . .
H10A H 0.0931 -0.3325 0.4340 0.093 Uiso 1 1 calc R . .
C11 C 0.2354(6) -0.2343(3) 0.4036(2) 0.0689(13) Uani 1 1 d . . .
H11A H 0.3158 -0.2652 0.4232 0.083 Uiso 1 1 calc R . .
C12 C 0.2518(4) -0.1466(3) 0.3689(2) 0.0569(11) Uani 1 1 d . . .
H12A H 0.3429 -0.1195 0.3657 0.068 Uiso 1 1 calc R . .
C13 C 0.2524(4) 0.0913(2) 0.34597(18) 0.0398(10) Uani 1 1 d . . .
C14 C 0.2842(5) 0.0770(3) 0.4236(2) 0.0710(13) Uani 1 1 d . . .
H14A H 0.2565 0.0217 0.4479 0.085 Uiso 1 1 calc R . .
C15 C 0.3576(5) 0.1458(4) 0.4639(2) 0.0885(16) Uani 1 1 d . . .
H15A H 0.3792 0.1362 0.5156 0.106 Uiso 1 1 calc R . .
C16 C 0.3986(5) 0.2274(3) 0.4293(3) 0.0755(14) Uani 1 1 d . . .
H16A H 0.4456 0.2736 0.4577 0.091 Uiso 1 1 calc R . .
C17 C 0.3709(4) 0.2414(3) 0.3530(3) 0.0637(12) Uani 1 1 d . . .
H17A H 0.4012 0.2963 0.3289 0.076 Uiso 1 1 calc R . .
C18 C 0.2977(4) 0.1738(3) 0.3120(2) 0.0509(11) Uani 1 1 d . . .
H18A H 0.2782 0.1839 0.2602 0.061 Uiso 1 1 calc R . .
C19 C -0.1068(5) 0.0804(4) 0.4203(2) 0.1071(19) Uani 1 1 d . . .
H19A H -0.0118 0.0985 0.4366 0.161 Uiso 1 1 calc R . .
H19B H -0.1180 0.0138 0.4262 0.161 Uiso 1 1 calc R . .
H19C H -0.1774 0.1122 0.4513 0.161 Uiso 1 1 calc R . .
C20 C -0.3177(5) 0.0762(4) 0.2908(3) 0.1087(18) Uani 1 1 d . . .
H20A H -0.3355 0.0920 0.2379 0.163 Uiso 1 1 calc R . .
H20B H -0.3862 0.1080 0.3230 0.163 Uiso 1 1 calc R . .
H20C H -0.3273 0.0096 0.2975 0.163 Uiso 1 1 calc R . .
C21 C -0.1075(5) 0.2393(3) 0.3080(3) 0.117(2) Uani 1 1 d . . .
H21A H -0.1224 0.2573 0.2553 0.175 Uiso 1 1 calc R . .
H21B H -0.0112 0.2557 0.3234 0.175 Uiso 1 1 calc R . .
H21C H -0.1757 0.2714 0.3402 0.175 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'
N N 0.0061 0.0033 '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'
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'
Cl Cl 0.1484 0.1585 '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 B1 C1 106.1(3) . . ?
N1 B1 Cl2 111.7(3) . . ?
C1 B1 Cl2 112.7(3) . . ?
N1 B1 Cl1 110.3(2) . . ?
C1 B1 Cl1 109.3(3) . . ?
Cl2 B1 Cl1 106.8(2) . . ?
N1 P1 C2 99.96(15) . . ?
N1 P1 C13 113.95(15) . . ?
C2 P1 C13 110.46(16) . . ?
N1 P1 C7 112.92(16) . . ?
C2 P1 C7 109.66(15) . . ?
C13 P1 C7 109.52(16) . . ?
B1 N1 P1 110.0(2) . . ?
B1 N1 Si1 123.9(2) . . ?
P1 N1 Si1 125.94(15) . . ?
N1 Si1 C21 110.16(18) . . ?
N1 Si1 C20 109.68(17) . . ?
C21 Si1 C20 111.9(2) . . ?
N1 Si1 C19 109.68(17) . . ?
C21 Si1 C19 108.4(2) . . ?
C20 Si1 C19 106.9(2) . . ?
C2 C1 C6 116.8(3) . . ?
C2 C1 B1 113.8(3) . . ?
C6 C1 B1 129.3(3) . . ?
C1 C2 C3 122.8(3) . . ?
C1 C2 P1 108.8(3) . . ?
C3 C2 P1 128.4(3) . . ?
C4 C3 C2 118.8(3) . . ?
C5 C4 C3 119.5(4) . . ?
C4 C5 C6 121.3(3) . . ?
C5 C6 C1 120.7(3) . . ?
C8 C7 C12 118.1(3) . . ?
C8 C7 P1 119.7(3) . . ?
C12 C7 P1 122.0(3) . . ?
C7 C8 C9 120.7(4) . . ?
C10 C9 C8 120.1(5) . . ?
C11 C10 C9 120.0(5) . . ?
C10 C11 C12 120.8(4) . . ?
C7 C12 C11 120.3(4) . . ?
C18 C13 C14 118.3(3) . . ?
C18 C13 P1 118.0(3) . . ?
C14 C13 P1 123.7(3) . . ?
C15 C14 C13 119.3(4) . . ?
C16 C15 C14 121.2(4) . . ?
C15 C16 C17 120.1(4) . . ?
C16 C17 C18 119.5(4) . . ?
C17 C18 C13 121.6(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
B1 N1 1.576(4) . ?
B1 C1 1.597(5) . ?
B1 Cl2 1.877(4) . ?
B1 Cl1 1.909(4) . ?
P1 N1 1.624(3) . ?
P1 C2 1.787(3) . ?
P1 C13 1.798(3) . ?
P1 C7 1.803(4) . ?
N1 Si1 1.781(3) . ?
Si1 C21 1.825(5) . ?
Si1 C20 1.850(4) . ?
Si1 C19 1.860(4) . ?
C1 C2 1.393(4) . ?
C1 C6 1.404(4) . ?
C2 C3 1.397(4) . ?
C3 C4 1.387(4) . ?
C4 C5 1.382(5) . ?
C5 C6 1.385(5) . ?
C7 C8 1.389(5) . ?
C7 C12 1.393(5) . ?
C8 C9 1.397(5) . ?
C9 C10 1.371(6) . ?
C10 C11 1.359(6) . ?
C11 C12 1.395(5) . ?
C13 C18 1.381(4) . ?
C13 C14 1.395(4) . ?
C14 C15 1.384(5) . ?
C15 C16 1.363(6) . ?
C16 C17 1.365(5) . ?
C17 C18 1.377(5) . ?
