#------------------------------------------------------------------------------
#$Date: 2016-03-22 11:58:54 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178927 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/56/4115687.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_4115687
loop_
_publ_author_name
'Sarah L. Hinchley'
'Carole A. Morrison'
'David W. H. Rankin'
'Charles L. B. Macdonald'
'Robert J. Wiacek'
'Andreas Voigt'
'Alan H. Cowley'
'Michael F. Lappert'
'Grete Gundersen'
'Jason A. C. Clyburne'
'Philip P. Power'
_publ_section_title
;
 Spontaneous Generation of Stable Pnictinyl Radicals from
 "Jack-in-the-Box" Dipnictines: A Solid-State, Gas-Phase, and Theoretical
 Investigation of the Origins of Steric Stabilization1
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9045
_journal_page_last               9053
_journal_paper_doi               10.1021/ja010615b
_journal_volume                  123
_journal_year                    2001
_chemical_compound_source        selfmade
_chemical_formula_analytical     'C14 H38 Cl P Si4'
_chemical_formula_moiety         'C14 H38 Cl P Si4'
_chemical_formula_structural     'C14 H38 Cl P Si4'
_chemical_formula_sum            'C14 H38 Cl P Si4'
_chemical_formula_weight         385.22
_chemical_name_common            bis(disyl)chlorophosphine
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 95.080(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.3190(10)
_cell_length_b                   12.406(2)
_cell_length_c                   20.453(2)
_cell_measurement_reflns_used    37
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      12.4
_cell_measurement_theta_min      10.0
_cell_volume                     2355.3(5)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      183(2)
_diffrn_measurement_device       'Siemens P3'
_diffrn_measurement_method       'ω scans'
_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  0.0214
_diffrn_reflns_av_sigmaI/netI    0.0440
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            6906
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.00
_diffrn_standards_decay_%        2.0
_diffrn_standards_interval_count 96
_diffrn_standards_number         4
_exptl_absorpt_coefficient_mu    0.427
_exptl_absorpt_correction_T_max  0.96968
_exptl_absorpt_correction_T_min  0.56222
_exptl_absorpt_correction_type   SHELXA
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.086
_exptl_crystal_description       plate
_exptl_crystal_F_000             840
_exptl_crystal_size_max          0.90
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.307
_refine_diff_density_min         -0.243
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.018
_refine_ls_goodness_of_fit_obs   1.052
_refine_ls_matrix_type           full
_refine_ls_number_parameters     195
_refine_ls_number_reflns         5387
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_restrained_S_obs      1.052
_refine_ls_R_factor_all          0.0662
_refine_ls_R_factor_obs          0.0395
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0375P)²+0.7125P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0931
_refine_ls_wR_factor_obs         0.0806
_reflns_number_observed          3955
_reflns_number_total             5392
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja010615b_1.cif
_cod_data_source_block           jason5
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0375P)^2^+0.7125P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0375P)^2^+0.7125P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4115687
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
P1 P 0.52395(6) 0.72903(5) 0.30625(2) 0.02719(13) Uani 1 d .
Cl1 Cl 0.70177(7) 0.82765(5) 0.28865(3) 0.04042(15) Uani 1 d .
C1 C 0.5333(2) 0.6144(2) 0.24988(9) 0.0263(4) Uani 1 d .
H1 H 0.6160(2) 0.5682(2) 0.26731(9) 0.035(4) Uiso 1 calc R
C2 C 0.5926(2) 0.6785(2) 0.38818(9) 0.0267(4) Uani 1 d .
H2 H 0.5320(2) 0.6132(2) 0.39380(9) 0.035(4) Uiso 1 calc R
Si1 Si 0.56802(7) 0.65561(5) 0.16272(3) 0.03383(15) Uani 1 d .
C11 C 0.7643(3) 0.6727(3) 0.15457(13) 0.0552(7) Uani 1 d .
H11A H 0.8159(4) 0.6075(6) 0.1704(9) 0.082(2) Uiso 1 calc R
H11B H 0.8005(5) 0.7347(9) 0.1807(8) 0.082(2) Uiso 1 calc R
H11C H 0.7798(3) 0.6847(15) 0.1084(2) 0.082(2) Uiso 1 calc R
C12 C 0.5101(3) 0.5503(2) 0.10055(12) 0.0527(7) Uani 1 d .
H12A H 0.4054(4) 0.5414(11) 0.0985(7) 0.082(2) Uiso 1 calc R
H12B H 0.5570(16) 0.4817(4) 0.1131(5) 0.082(2) Uiso 1 calc R
H12C H 0.5377(18) 0.5725(7) 0.0574(2) 0.082(2) Uiso 1 calc R
C13 C 0.4688(3) 0.7830(2) 0.14093(12) 0.0475(6) Uani 1 d .
H13A H 0.3650(3) 0.7706(4) 0.1412(9) 0.082(2) Uiso 1 calc R
H13B H 0.4904(17) 0.8065(9) 0.0971(4) 0.082(2) Uiso 1 calc R
H13C H 0.4990(16) 0.8390(5) 0.1731(6) 0.082(2) Uiso 1 calc R
Si2 Si 0.36136(6) 0.53040(5) 0.25286(3) 0.03325(15) Uani 1 d .
C21 C 0.2981(3) 0.5220(2) 0.33715(13) 0.0551(7) Uani 1 d .
H21A H 0.3728(9) 0.4881(14) 0.3670(2) 0.082(2) Uiso 1 calc R
H21B H 0.2098(12) 0.4788(13) 0.3356(2) 0.082(2) Uiso 1 calc R
H21C H 0.2786(19) 0.5947(3) 0.3529(4) 0.082(2) Uiso 1 calc R
C22 C 0.2061(3) 0.5864(2) 0.19991(13) 0.0517(7) Uani 1 d .
H22A H 0.1864(13) 0.6600(6) 0.2140(6) 0.082(2) Uiso 1 calc R
H22B H 0.1209(6) 0.5413(9) 0.2038(7) 0.082(2) Uiso 1 calc R
H22C H 0.2295(8) 0.5873(14) 0.1541(2) 0.082(2) Uiso 1 calc R
C23 C 0.4012(3) 0.3890(2) 0.22935(14) 0.0514(7) Uani 1 d .
H23A H 0.4750(15) 0.3588(5) 0.2612(5) 0.082(2) Uiso 1 calc R
H23B H 0.4362(19) 0.3884(2) 0.1856(4) 0.082(2) Uiso 1 calc R
H23C H 0.3132(5) 0.3457(4) 0.2289(9) 0.082(2) Uiso 1 calc R
Si3 Si 0.78314(6) 0.62561(5) 0.40568(3) 0.03120(14) Uani 1 d .
C31 C 0.7741(3) 0.5089(2) 0.4632(2) 0.0636(9) Uani 1 d .
H31A H 0.7346(19) 0.5331(4) 0.5035(4) 0.082(2) Uiso 1 calc R
H31B H 0.8711(4) 0.4798(10) 0.4739(8) 0.082(2) Uiso 1 calc R
H31C H 0.7119(17) 0.4528(7) 0.4423(4) 0.082(2) Uiso 1 calc R
C32 C 0.8700(3) 0.5741(2) 0.33335(13) 0.0518(7) Uani 1 d .
H32A H 0.8687(18) 0.6304(5) 0.2997(4) 0.082(2) Uiso 1 calc R
H32B H 0.8172(12) 0.5109(9) 0.3154(6) 0.082(2) Uiso 1 calc R
H32C H 0.9699(7) 0.5538(14) 0.3469(2) 0.082(2) Uiso 1 calc R
C33 C 0.9093(2) 0.7291(2) 0.44357(12) 0.0435(6) Uani 1 d .
H33A H 0.8694(10) 0.7598(11) 0.4822(6) 0.082(2) Uiso 1 calc R
H33B H 0.9223(16) 0.7864(8) 0.4116(3) 0.082(2) Uiso 1 calc R
H33C H 1.0025(7) 0.6955(4) 0.4568(9) 0.082(2) Uiso 1 calc R
Si4 Si 0.52986(7) 0.77604(6) 0.45188(3) 0.0370(2) Uani 1 d .
C41 C 0.6111(3) 0.9120(2) 0.4441(2) 0.0668(9) Uani 1 d .
H41A H 0.7149(4) 0.9047(3) 0.4410(9) 0.082(2) Uiso 1 calc R
H41B H 0.5942(17) 0.9554(5) 0.4828(4) 0.082(2) Uiso 1 calc R
H41C H 0.5668(14) 0.9475(6) 0.4045(5) 0.082(2) Uiso 1 calc R
C42 C 0.5752(3) 0.7211(3) 0.53640(11) 0.0629(9) Uani 1 d .
H42A H 0.5323(17) 0.6494(7) 0.5396(3) 0.082(2) Uiso 1 calc R
H42B H 0.5370(18) 0.7693(8) 0.56863(13) 0.082(2) Uiso 1 calc R
H42C H 0.6800(3) 0.7158(14) 0.5452(4) 0.082(2) Uiso 1 calc R
C43 C 0.3298(3) 0.7890(3) 0.44233(13) 0.0551(8) Uani 1 d .
H43A H 0.2860(3) 0.7189(4) 0.4504(9) 0.082(2) Uiso 1 calc R
H43B H 0.2987(3) 0.8129(15) 0.3976(3) 0.082(2) Uiso 1 calc R
H43C H 0.2993(3) 0.8418(12) 0.4739(7) 0.082(2) Uiso 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'
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
C1 P1 C2 105.93(9)
C1 P1 Cl1 105.04(7)
C2 P1 Cl1 97.87(7)
P1 C1 Si1 113.55(11)
P1 C1 Si2 108.32(10)
Si1 C1 Si2 112.74(10)
P1 C2 Si3 122.07(11)
P1 C2 Si4 107.58(10)
Si3 C2 Si4 115.39(10)
C11 Si1 C13 110.61(14)
C11 Si1 C12 104.17(13)
C13 Si1 C12 108.84(12)
C11 Si1 C1 111.26(11)
C13 Si1 C1 109.20(11)
C12 Si1 C1 112.66(11)
C22 Si2 C23 111.28(12)
C22 Si2 C21 105.33(13)
C23 Si2 C21 105.72(13)
C22 Si2 C1 112.77(11)
C23 Si2 C1 108.48(11)
C21 Si2 C1 113.05(10)
C32 Si3 C33 105.33(12)
C32 Si3 C31 106.30(14)
C33 Si3 C31 109.48(13)
C32 Si3 C2 115.76(10)
C33 Si3 C2 112.69(10)
C31 Si3 C2 107.02(11)
C41 Si4 C43 108.88(15)
C41 Si4 C42 110.4(2)
C43 Si4 C42 105.66(12)
C41 Si4 C2 111.41(11)
C43 Si4 C2 110.30(11)
C42 Si4 C2 110.01(12)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
P1 C1 1.838(2)
P1 C2 1.849(2)
P1 Cl1 2.1161(8)
C1 Si1 1.910(2)
C1 Si2 1.917(2)
C2 Si3 1.898(2)
C2 Si4 1.907(2)
Si1 C11 1.864(3)
Si1 C13 1.865(3)
Si1 C12 1.869(2)
Si2 C22 1.863(2)
Si2 C23 1.864(3)
Si2 C21 1.874(3)
Si3 C32 1.861(3)
Si3 C33 1.863(2)
Si3 C31 1.872(3)
Si4 C41 1.861(3)
Si4 C43 1.865(3)
Si4 C42 1.871(3)
