#------------------------------------------------------------------------------
#$Date: 2016-03-22 13:50:58 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178980 $
#$URL: svn://www.crystallography.net/cod/cif/4/12/03/4120313.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_4120313
loop_
_publ_author_name
'Kerstin Hansen'
'Tibor Szilvási'
'Burgert Blom'
'Shigeyoshi Inoue'
'Jan Epping'
'Matthias Driess'
_publ_section_title
;
 A Fragile Zwitterionic Phosphasilene as a Transfer Agent of the Elusive
 Parent Phosphinidene (:PH)
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11795
_journal_page_last               11798
_journal_paper_doi               10.1021/ja4072699
_journal_volume                  135
_journal_year                    2013
_chemical_formula_sum            'C29 H44 N2 P2 Si'
_chemical_formula_weight         510.69
_chemical_name_systematic
; 
 ? 
;
_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
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.8 (release 12-01-2007 CrysAlis171 .NET)
(compiled Jan 12 2007,17:49:11)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 117.333(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.7037(5)
_cell_length_b                   19.5075(6)
_cell_length_c                   13.6703(6)
_cell_measurement_reflns_used    3820
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      32.4395
_cell_measurement_theta_min      3.3484
_cell_volume                     3009.5(2)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.8 (release 12-01-2007 CrysAlis171 .NET)
(compiled Jan 12 2007,17:49:11)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.31.8 (release 12-01-2007 CrysAlis171 .NET)
(compiled Jan 12 2007,17:49:11)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.8 (release 12-01-2007 CrysAlis171 .NET)
(compiled Jan 12 2007,17:49:11)
;
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur S Sapphire'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) x-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0346
_diffrn_reflns_av_sigmaI/netI    0.0500
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            11533
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.36
_exptl_absorpt_coefficient_mu    0.203
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.96503
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.127
_exptl_crystal_description       block
_exptl_crystal_F_000             1104
_exptl_crystal_size_max          0.453
_exptl_crystal_size_mid          0.391
_exptl_crystal_size_min          0.193
_refine_diff_density_max         0.396
_refine_diff_density_min         -0.267
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     332
_refine_ls_number_reflns         5146
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0662
_refine_ls_R_factor_gt           0.0485
_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)+(0.0373P)²+1.5515P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0997
_refine_ls_wR_factor_ref         0.1066
_reflns_number_gt                4214
_reflns_number_total             5146
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja4072699_si_002.cif
_cod_data_source_block           d:\eigene~1\p21n
_cod_database_code               4120313
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
Si1 Si 0.11962(5) 0.09132(3) 0.28177(5) 0.01677(15) Uani 1 1 d .
P2 P 0.15499(5) -0.02244(3) 0.30586(6) 0.03116(18) Uani 1 1 d D
P1 P 0.22511(7) 0.14425(4) 0.44290(6) 0.0455(2) Uani 1 1 d D
N1 N -0.03206(14) 0.10626(9) 0.22798(15) 0.0181(4) Uani 1 1 d .
N2 N 0.15674(14) 0.11811(9) 0.18103(15) 0.0188(4) Uani 1 1 d .
C7 C -0.14601(17) 0.04736(11) 0.31026(18) 0.0197(5) Uani 1 1 d .
C6 C -0.09298(17) 0.10759(11) 0.29493(18) 0.0182(5) Uani 1 1 d .
C11 C -0.10306(18) 0.17041(11) 0.34237(19) 0.0210(5) Uani 1 1 d .
C19 C 0.36877(19) 0.12649(11) 0.22539(19) 0.0229(5) Uani 1 1 d .
C18 C 0.26058(18) 0.15857(11) 0.19980(18) 0.0192(5) Uani 1 1 d .
C2 C -0.10405(18) 0.10566(11) 0.11150(19) 0.0211(5) Uani 1 1 d .
C15 C -0.14375(19) -0.02158(11) 0.2588(2) 0.0243(5) Uani 1 1 d .
H15 H -0.0911 -0.0174 0.2227 0.029 Uiso 1 1 calc R
C10 C -0.16418(19) 0.17095(12) 0.4045(2) 0.0258(5) Uani 1 1 d .
H10 H -0.1710 0.2127 0.4369 0.031 Uiso 1 1 calc R
C27 C 0.38657(19) 0.04901(12) 0.2379(2) 0.0260(5) Uani 1 1 d .
H27 H 0.3080 0.0274 0.2181 0.031 Uiso 1 1 calc R
C3 C -0.04447(19) 0.09764(12) 0.04290(19) 0.0245(5) Uani 1 1 d .
H3 H -0.0941 0.0850 -0.0314 0.029 Uiso 1 1 calc R
C12 C -0.0571(2) 0.23797(11) 0.3201(2) 0.0279(6) Uani 1 1 d .
H12 H 0.0057 0.2270 0.2977 0.033 Uiso 1 1 calc R
C4 C 0.07080(19) 0.10562(11) 0.07010(19) 0.0233(5) Uani 1 1 d .
C8 C -0.20620(18) 0.05148(12) 0.37299(19) 0.0250(5) Uani 1 1 d .
H8 H -0.2422 0.0114 0.3836 0.030 Uiso 1 1 calc R
C1 C -0.22250(19) 0.11269(13) 0.0640(2) 0.0310(6) Uani 1 1 d .
H1A H -0.2615 0.1183 0.1084 0.037 Uiso 1 1 calc R
H1B H -0.2672 0.1120 -0.0139 0.037 Uiso 1 1 calc R
C23 C 0.2484(2) 0.23032(12) 0.1889(2) 0.0270(5) Uani 1 1 d .
C9 C -0.21515(19) 0.11251(12) 0.4205(2) 0.0266(5) Uani 1 1 d .
H9 H -0.2561 0.1140 0.4637 0.032 Uiso 1 1 calc R
C20 C 0.4646(2) 0.16730(13) 0.2388(2) 0.0327(6) Uani 1 1 d .
H20 H 0.5387 0.1464 0.2562 0.039 Uiso 1 1 calc R
C29 C 0.4712(2) 0.03021(13) 0.3584(2) 0.0327(6) Uani 1 1 d .
H29A H 0.5506 0.0478 0.3779 0.049 Uiso 1 1 calc R
H29B H 0.4745 -0.0198 0.3668 0.049 Uiso 1 1 calc R
H29C H 0.4422 0.0506 0.4070 0.049 Uiso 1 1 calc R
C5 C 0.1160(2) 0.09890(14) -0.0132(2) 0.0357(6) Uani 1 1 d .
H5A H 0.1672 0.0585 0.0039 0.054 Uiso 1 1 calc R
H5B H 0.1614 0.1399 -0.0112 0.054 Uiso 1 1 calc R
H5C H 0.0490 0.0939 -0.0868 0.054 Uiso 1 1 calc R
C17 C -0.0948(2) -0.07871(12) 0.3457(2) 0.0339(6) Uani 1 1 d .
H17A H -0.0225 -0.0627 0.4090 0.051 Uiso 1 1 calc R
H17B H -0.0765 -0.1191 0.3137 0.051 Uiso 1 1 calc R
H17C H -0.1541 -0.0908 0.3698 0.051 Uiso 1 1 calc R
C22 C 0.3471(2) 0.26858(13) 0.2028(2) 0.0361(6) Uani 1 1 d .
H22 H 0.3406 0.3170 0.1954 0.043 Uiso 1 1 calc R
C28 C 0.4331(2) 0.01978(14) 0.1612(2) 0.0399(7) Uani 1 1 d .
H28A H 0.3790 0.0323 0.0849 0.060 Uiso 1 1 calc R
H28B H 0.4381 -0.0303 0.1681 0.060 Uiso 1 1 calc R
H28C H 0.5119 0.0386 0.1814 0.060 Uiso 1 1 calc R
C16 C -0.2683(2) -0.04211(13) 0.1706(2) 0.0344(6) Uani 1 1 d .
H16A H -0.3200 -0.0489 0.2052 0.052 Uiso 1 1 calc R
H16B H -0.2634 -0.0848 0.1351 0.052 Uiso 1 1 calc R
H16C H -0.3007 -0.0057 0.1152 0.052 Uiso 1 1 calc R
C21 C 0.4535(2) 0.23763(13) 0.2271(2) 0.0397(7) Uani 1 1 d .
H21 H 0.5195 0.2647 0.2359 0.048 Uiso 1 1 calc R
C24 C 0.1321(2) 0.26675(12) 0.1598(2) 0.0347(6) Uani 1 1 d .
H24 H 0.0775 0.2328 0.1677 0.042 Uiso 1 1 calc R
C13 C -0.0019(2) 0.28417(14) 0.4222(3) 0.0432(7) Uani 1 1 d .
H13A H -0.0638 0.2998 0.4409 0.065 Uiso 1 1 calc R
H13B H 0.0352 0.3239 0.4068 0.065 Uiso 1 1 calc R
H13C H 0.0581 0.2583 0.4842 0.065 Uiso 1 1 calc R
C26 C 0.1474(3) 0.32640(14) 0.2378(3) 0.0601(10) Uani 1 1 d .
H26A H 0.1956 0.3623 0.2279 0.090 Uiso 1 1 calc R
H26B H 0.1869 0.3100 0.3141 0.090 Uiso 1 1 calc R
H26C H 0.0695 0.3451 0.2216 0.090 Uiso 1 1 calc R
C14 C -0.1573(3) 0.27534(14) 0.2244(3) 0.0491(8) Uani 1 1 d .
H14A H -0.1867 0.2468 0.1582 0.074 Uiso 1 1 calc R
H14B H -0.1276 0.3188 0.2109 0.074 Uiso 1 1 calc R
H14C H -0.2220 0.2844 0.2430 0.074 Uiso 1 1 calc R
C25 C 0.0742(3) 0.29046(17) 0.0397(3) 0.0623(10) Uani 1 1 d .
H25A H 0.1259 0.3237 0.0292 0.093 Uiso 1 1 calc R
H25B H -0.0023 0.3120 0.0216 0.093 Uiso 1 1 calc R
H25C H 0.0618 0.2509 -0.0085 0.093 Uiso 1 1 calc R
H4 H 0.2743(10) -0.0158(12) 0.3793(18) 0.040(7) Uiso 1 1 d D
H5 H 0.124(2) -0.0264(13) 0.3912(16) 0.053(8) Uiso 1 1 d D
H2 H 0.331(2) 0.1118(19) 0.466(4) 0.138(17) Uiso 1 1 d D
H1 H 0.224(3) 0.2090(9) 0.403(3) 0.102(13) Uiso 1 1 d 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'
N N 0.0061 0.0033 '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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
N2 Si1 N1 105.46(9)
N2 Si1 P1 112.69(7)
N1 Si1 P1 112.63(7)
N2 Si1 P2 107.73(7)
N1 Si1 P2 109.47(6)
P1 Si1 P2 108.72(4)
C2 N1 C6 116.87(16)
C2 N1 Si1 119.18(15)
C6 N1 Si1 123.08(14)
C4 N2 C18 118.02(18)
C4 N2 Si1 116.12(14)
C18 N2 Si1 125.47(15)
C8 C7 C6 118.5(2)
C8 C7 C15 117.9(2)
C6 C7 C15 123.5(2)
C7 C6 C11 120.0(2)
C7 C6 N1 120.54(19)
C11 C6 N1 119.46(19)
C10 C11 C6 118.6(2)
C10 C11 C12 119.2(2)
C6 C11 C12 122.1(2)
C20 C19 C18 118.4(2)
C20 C19 C27 118.4(2)
C18 C19 C27 123.25(19)
C19 C18 C23 121.18(19)
C19 C18 N2 120.52(19)
C23 C18 N2 118.28(18)
C1 C2 N1 122.7(2)
C1 C2 C3 119.8(2)
N1 C2 C3 117.55(18)
C7 C15 C17 111.7(2)
C7 C15 C16 111.17(18)
C17 C15 C16 108.83(19)
C9 C10 C11 121.7(2)
C19 C27 C28 112.1(2)
C19 C27 C29 110.52(19)
C28 C27 C29 110.13(19)
C4 C3 C2 129.1(2)
C14 C12 C11 109.75(19)
C14 C12 C13 110.6(2)
C11 C12 C13 112.5(2)
C3 C4 N2 121.3(2)
C3 C4 C5 121.9(2)
N2 C4 C5 116.76(19)
C9 C8 C7 121.7(2)
C22 C23 C18 118.0(2)
C22 C23 C24 119.4(2)
C18 C23 C24 122.59(19)
C10 C9 C8 119.5(2)
C21 C20 C19 121.1(2)
C21 C22 C23 121.4(2)
C22 C21 C20 120.0(2)
C23 C24 C25 110.7(2)
C23 C24 C26 112.1(2)
C25 C24 C26 111.3(2)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Si1 N2 1.7287(19)
Si1 N1 1.7429(17)
Si1 P1 2.2368(9)
Si1 P2 2.2581(9)
N1 C2 1.426(3)
N1 C6 1.445(3)
N2 C4 1.425(3)
N2 C18 1.455(3)
C7 C8 1.389(3)
C7 C6 1.417(3)
C7 C15 1.524(3)
C6 C11 1.420(3)
C11 C10 1.390(3)
C11 C12 1.528(3)
C19 C20 1.394(3)
C19 C18 1.400(3)
C19 C27 1.526(3)
C18 C23 1.409(3)
C2 C1 1.344(3)
C2 C3 1.459(3)
C15 C17 1.537(3)
C15 C16 1.538(3)
C10 C9 1.377(3)
C27 C28 1.531(3)
C27 C29 1.541(3)
C3 C4 1.344(3)
C12 C14 1.527(4)
C12 C13 1.534(4)
C4 C5 1.498(3)
C8 C9 1.385(3)
C23 C22 1.394(3)
C23 C24 1.520(3)
C20 C21 1.381(3)
C22 C21 1.376(3)
C24 C25 1.529(4)
C24 C26 1.530(4)
