#------------------------------------------------------------------------------
#$Date: 2016-02-19 16:29:56 +0200 (Fri, 19 Feb 2016) $
#$Revision: 176759 $
#$URL: svn://www.crystallography.net/cod/cif/2/00/35/2003555.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2003555
loop_
_publ_author_name
'Bruckmann, J.'
'Krüger, C.'
_publ_section_title
;
 Tris(n-butyl)phosphine, Tris(tert-butyl)phosphine and
 Tris(trimethylsilyl)phosphine
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1152
_journal_page_last               1155
_journal_paper_doi               10.1107/S0108270194014356
_journal_volume                  51
_journal_year                    1995
_chemical_formula_sum            'C9 H27 P Si3'
_chemical_formula_weight         250.55
_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_type_scat_source           IntTabIV
_cell_angle_alpha                90
_cell_angle_beta                 113.91(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.859(2)
_cell_length_b                   15.010(6)
_cell_length_c                   11.947(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    102
_cell_measurement_theta_max      15
_cell_measurement_theta_min      8
_cell_volume                     1616.2(10)
_diffrn_measurement_device       'Enraf-Nonius CAD-4'
_diffrn_measurement_method       ω/2θ
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0020
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3767
_diffrn_reflns_theta_max         27.5
_diffrn_standards_decay_%        10.2
_diffrn_standards_interval_time  30
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.344
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.03
_exptl_crystal_description       cylindrical
_exptl_crystal_size_max          'Height 0.4 mm'
_exptl_crystal_size_rad          0.1
_refine_diff_density_max         0.42
_refine_diff_density_min         -0.37
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   1.9
_refine_ls_hydrogen_treatment    'refall isotropically'
_refine_ls_number_parameters     226
_refine_ls_number_reflns         2878
_refine_ls_R_factor_obs          0.034
_refine_ls_shift/esd_max         0.05
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/σ²(F)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.046
_reflns_number_observed          2878
_reflns_number_total             3442
_reflns_observed_criterion       I>2\s(I)
_cod_data_source_file            hr1046.cif
_cod_data_source_block           hr1046c
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value '1/\s^2^(F)' 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^(F)'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1616.0(10)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2003555
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
1/2+x,1/2-y,1/2+z
-x,-y,-z
1/2-x,1/2+y,1/2-z
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
P .2299(1) .2511(1) -.0269(1) 0.015(1)
Si(1) .1894(1) .1581(1) .1030(1) 0.016(1)
Si(2) .2688(1) .3856(1) .0631(1) 0.018(1)
Si(3) .4470(1) .2086(1) -.0298(1) 0.020(1)
C(1) .3110(2) .1751(2) .2686(2) 0.024(1)
C(2) -.0093(2) .1721(2) .0799(2) 0.024(1)
C(3) .2137(3) .0418(1) .0587(2) 0.026(2)
C(4) .4517(3) .4028(2) .1945(2) 0.028(1)
C(5) .1182(3) .4058(2) .1172(2) 0.026(1)
C(6) .2487(3) .4689(2) -.0581(2) 0.029(2)
C(7) .5902(3) .1676(2) .1182(2) 0.032(2)
C(8) .4035(3) .1185(2) -.1473(3) 0.033(2)
C(9) .5250(3) .3052(2) -.0823(3) 0.038(2)
H(1a) .281(3) .135(2) .316(3) 0.048(9)
H(1b) .414(3) .167(2) .287(3) 0.050(9)
H(1c) .296(3) .236(2) .293(2) 0.037(7)
H(2a) -.072(3) .161(2) .001(3) 0.053(9)
H(2b) -.028(3) .226(2) .102(2) 0.033(7)
H(2c) -.031(3) .129(2) .133(3) 0.036(7)
H(3a) .321(3) .030(2) .077(2) 0.033(7)
H(3b) .184(3) .002(2) .104(2) 0.036(7)
H(3c) .155(3) .035(2) -.026(3) 0.054(9)
H(4a) .451(3) .459(2) .223(3) 0.055(9)
H(4b) .473(3) .359(2) .261(3) 0.06(1)
H(4c) .524(3) .401(2) .165(3) 0.040(8)
H(5a) .020(3) .393(2) .058(3) 0.052(9)
H(5b) .131(3) .370(2) .187(3) 0.041(8)
H(5c) .125(3) .467(2) .144(2) 0.033(7)
H(6a) .324(3) .465(2) -.091(3) 0.041(8)
H(6b) .151(3) .462(2) -.125(3) 0.040(8)
H(6c) .259(3) .528(2) -.026(2) 0.037(7)
H(7a) .677(4) .153(2) .105(3) 0.06(1)
H(7b) .613(4) .209(2) .180(3) 0.07(1)
H(7c) .557(3) .115(2) .142(3) 0.044(9)
H(8a) .498(3) .097(2) -.155(3) 0.049(8)
H(8b) .340(3) .141(2) -.227(3) 0.043(8)
H(8c) .363(3) .069(2) -.128(3) 0.051(9)
H(9a) .609(4) .288(2) -.093(3) 0.06(1)
H(9b) .552(3) .355(2) -.021(3) 0.055(9)
H(9c) .460(3) .327(2) -.157(3) 0.053(9)
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_publ_flag
Si(3) P Si(2) 106.50(10) yes
Si(2) P Si(1) 105.80(10) yes
C(3) Si(1) C(1) 109.00(10) yes
C(2) Si(1) C(1) 108.90(10) yes
C(1) Si(1) P 115.50(10) yes
C(6) Si(2) C(4) 108.80(10) yes
C(5) Si(2) C(4) 108.50(10) yes
C(4) Si(2) P 116.50(10) yes
C(9) Si(3) C(7) 108.60(10) yes
C(8) Si(3) C(7) 109.20(10) yes
C(7) Si(3) P 116.00(10) yes
Si(3) P Si(1) 105.80(10) yes
C(3) Si(1) C(2) 108.00(10) yes
C(3) Si(1) P 107.90(10) yes
C(2) Si(1) P 107.30(10) yes
C(6) Si(2) C(5) 108.10(10) yes
C(6) Si(2) P 106.70(10) yes
C(5) Si(2) P 107.80(10) yes
C(9) Si(3) C(8) 108.10(10) yes
C(9) Si(3) P 108.00(10) yes
C(8) Si(3) P 106.70(10) yes
H(2a) C(2) Si(1) 111(2) no
H(3a) C(3) Si(1) 110.0(10) no
H(4a) C(4) Si(2) 107(2) no
H(5a) C(5) Si(2) 115(2) no
H(6a) C(6) Si(2) 114(2) no
H(7a) C(7) Si(3) 108(2) no
H(8a) C(8) Si(3) 111(2) no
H(9a) C(9) Si(3) 110(2) no
H(1c) C(1) Si(1) 109(2) no
H(1b) C(1) Si(1) 113(2) no
H(2c) C(2) Si(1) 109(2) no
H(2b) C(2) Si(1) 113(2) no
H(3c) C(3) Si(1) 108(2) no
H(3b) C(3) Si(1) 109(2) no
H(4c) C(4) Si(2) 108(2) no
H(4b) C(4) Si(2) 114(2) no
H(5c) C(5) Si(2) 108(2) no
H(5b) C(5) Si(2) 112(2) no
H(6c) C(6) Si(2) 111(2) no
H(6b) C(6) Si(2) 109(2) no
H(7c) C(7) Si(3) 110(2) no
H(7b) C(7) Si(3) 112(2) no
H(8c) C(8) Si(3) 113(2) no
H(8b) C(8) Si(3) 111(2) no
H(9c) C(9) Si(3) 112(2) no
H(9b) C(9) Si(3) 111(2) no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
P Si(1) 2.2410(10) yes
P Si(3) 2.2480(10) yes
Si(1) C(2) 1.876(2) yes
Si(2) C(4) 1.868(3) yes
Si(2) C(6) 1.862(3) yes
Si(3) C(8) 1.870(3) yes
P Si(2) 2.2460(10) yes
Si(1) C(1) 1.870(3) yes
Si(1) C(3) 1.868(2) yes
Si(2) C(5) 1.869(3) yes
Si(3) C(7) 1.865(3) yes
Si(3) C(9) 1.865(3) yes
C(1) H(1a) 0.95(3) no
C(1) H(1c) 0.99(3) no
C(2) H(2b) 0.90(3) no
C(3) H(3a) 1.00(3) no
C(3) H(3c) 0.95(4) no
C(4) H(4b) 0.99(4) no
C(5) H(5a) 0.96(3) no
C(5) H(5c) 0.97(3) no
C(6) H(6b) 0.98(3) no
C(7) H(7a) 0.96(4) no
C(7) H(7c) 0.93(3) no
C(8) H(8b) 0.96(3) no
C(9) H(9a) 0.93(4) no
C(9) H(9c) 0.92(4) no
C(1) H(1b) 0.96(3) no
C(2) H(2a) 0.92(4) no
C(2) H(2c) 0.99(3) no
C(3) H(3b) 0.93(3) no
C(4) H(4a) 0.91(3) no
C(4) H(4c) 0.92(3) no
C(5) H(5b) 0.96(3) no
C(6) H(6a) 0.98(3) no
C(6) H(6c) 0.95(3) no
C(7) H(7b) 0.92(4) no
C(8) H(8a) 1.02(3) no
C(8) H(8c) 0.91(3) no
C(9) H(9b) 1.00(3) no
