#------------------------------------------------------------------------------
#$Date: 2016-03-22 11:39:11 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178909 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/38/4113865.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_4113865
loop_
_publ_author_name
'Vladimir K. Dioumaev'
'Leo J. Procopio'
'Patrick J. Carroll'
'Donald H. Berry'
_publ_section_title
;
 Synthesis and Reactivity of Silyl Ruthenium Complexes: The Importance of
 Trans Effects in C-H Activation, Si-C Bond Formation, and Dehydrogenative
 Coupling of Silanes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8043
_journal_page_last               8058
_journal_paper_doi               10.1021/ja035131p
_journal_volume                  125
_journal_year                    2003
_chemical_formula_sum            'C16 H48 P4 Ru Si'
_chemical_formula_weight         493.58
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 103.982(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   15.2642(2)
_cell_length_b                   10.9388(1)
_cell_length_c                   31.0714(4)
_cell_measurement_reflns_used    18969
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      0.0
_cell_volume                     5034.34(11)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SIR92 (Altomare, 1993)'
_diffrn_ambient_temperature      200(2)
_diffrn_measurement_device       'image plate area detector'
_diffrn_measurement_device_type  'Rigaku R-AXIS IIc'
_diffrn_measurement_method       'phi oscillations'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0403
_diffrn_reflns_av_sigmaI/netI    0.0288
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            18969
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.51
_exptl_absorpt_coefficient_mu    0.922
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.302
_exptl_crystal_F_000             2096
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.504
_refine_diff_density_min         -0.583
_refine_diff_density_rms         0.084
_refine_ls_extinction_coef       0.00104(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.215
_refine_ls_goodness_of_fit_obs   1.238
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     200
_refine_ls_number_reflns         4272
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.215
_refine_ls_restrained_S_obs      1.238
_refine_ls_R_factor_all          0.0653
_refine_ls_R_factor_obs          0.0554
_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)+(0.0520P)²+16.5345P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1295
_refine_ls_wR_factor_obs         0.1239
_reflns_number_observed          3787
_reflns_number_total             4272
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja035131psi20030313_065835.cif
_cod_data_source_block           7a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0520P)^2^+16.5345P] 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^)+(0.0520P)^2^+16.5345P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        5034.34(10)
_cod_original_sg_symbol_H-M      'C 2/c '
_cod_database_code               4113865
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'
'-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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
Ru1 Ru 0.19211(2) 0.25185(3) 0.120809(11) 0.0262(2) Uani 1 d
P1 P 0.09047(10) 0.23127(12) 0.05037(4) 0.0422(3) Uani 1 d
P2 P 0.09522(9) 0.23951(12) 0.16863(4) 0.0393(3) Uani 1 d
P3 P 0.32698(8) 0.25616(12) 0.17464(4) 0.0382(3) Uani 1 d
P4 P 0.17716(10) 0.46846(12) 0.11631(5) 0.0459(4) Uani 1 d
Si1 Si 0.20316(10) 0.02672(12) 0.12198(5) 0.0420(4) Uani 1 d
C1 C 0.0899(6) 0.3525(6) 0.0092(2) 0.077(2) Uani 1 d
C2 C -0.0317(5) 0.2155(8) 0.0419(2) 0.088(3) Uani 1 d
C3 C 0.1088(4) 0.1071(5) 0.0141(2) 0.0542(14) Uani 1 d
C4 C 0.0936(5) 0.3659(7) 0.2079(2) 0.075(2) Uani 1 d
C5 C -0.0272(4) 0.2271(7) 0.1469(2) 0.070(2) Uani 1 d
C6 C 0.1052(4) 0.1163(6) 0.2100(2) 0.064(2) Uani 1 d
C7 C 0.3954(5) 0.3950(8) 0.1801(3) 0.095(3) Uani 1 d
C8 C 0.3341(5) 0.2354(7) 0.2335(2) 0.081(2) Uani 1 d
C9 C 0.4160(5) 0.1539(8) 0.1685(3) 0.106(3) Uani 1 d
C10 C 0.2161(5) 0.5702(6) 0.1650(3) 0.082(2) Uani 1 d
C11 C 0.2314(6) 0.5528(6) 0.0784(3) 0.089(2) Uani 1 d
C12 C 0.0618(5) 0.5287(5) 0.0995(2) 0.066(2) Uani 1 d
C13 C 0.2565(5) -0.0611(6) 0.1754(2) 0.073(2) Uani 1 d
C14 C 0.2714(4) -0.0492(5) 0.0850(2) 0.066(2) Uani 1 d
C15 C 0.0918(5) -0.0622(5) 0.1066(2) 0.065(2) Uani 1 d
C16 C 0.2885(4) 0.2606(5) 0.0778(2) 0.0536(14) Uani 1 d
H1A H 0.1499 0.3660 0.0064 0.091 Uiso 1 d
H1B H 0.0672 0.4262 0.0187 0.091 Uiso 1 d
H1C H 0.0529 0.3286 -0.0186 0.091 Uiso 1 d
H2C H -0.0587 0.2070 0.0112 0.113 Uiso 1 d
H2A H -0.0554 0.2851 0.0533 0.113 Uiso 1 d
H2B H -0.0444 0.1442 0.0572 0.113 Uiso 1 d
H3B H 0.1689 0.1116 0.0102 0.067 Uiso 1 d
H3C H 0.0674 0.1146 -0.0141 0.067 Uiso 1 d
H3A H 0.1003 0.0307 0.0269 0.067 Uiso 1 d
H4A H 0.0817 0.4411 0.1920 0.092 Uiso 1 d
H4B H 0.1501 0.3709 0.2288 0.092 Uiso 1 d
H4C H 0.0473 0.3517 0.2230 0.092 Uiso 1 d
H5C H -0.0567 0.2330 0.1706 0.088 Uiso 1 d
H5A H -0.0419 0.1509 0.1323 0.088 Uiso 1 d
H5B H -0.0483 0.2916 0.1264 0.088 Uiso 1 d
H6B H 0.0602 0.1262 0.2262 0.079 Uiso 1 d
H6C H 0.1635 0.1202 0.2302 0.079 Uiso 1 d
H6A H 0.0983 0.0394 0.1956 0.079 Uiso 1 d
H7A H 0.4025 0.4178 0.1514 0.117 Uiso 1 d
H7B H 0.4536 0.3785 0.1988 0.117 Uiso 1 d
H7C H 0.3672 0.4580 0.1920 0.117 Uiso 1 d
H8C H 0.3952 0.2404 0.2494 0.099 Uiso 1 d
H8A H 0.3104 0.1574 0.2380 0.099 Uiso 1 d
H8B H 0.2999 0.2973 0.2433 0.099 Uiso 1 d
H9B H 0.4335 0.1735 0.1418 0.127 Uiso 1 d
H9C H 0.3959 0.0724 0.1674 0.127 Uiso 1 d
H9A H 0.4669 0.1646 0.1930 0.127 Uiso 1 d
H10A H 0.2782 0.5894 0.1680 0.100 Uiso 1 d
H10B H 0.2091 0.5298 0.1909 0.100 Uiso 1 d
H10C H 0.1816 0.6432 0.1607 0.100 Uiso 1 d
H11C H 0.2170 0.6373 0.0791 0.109 Uiso 1 d
H11A H 0.2118 0.5219 0.0495 0.109 Uiso 1 d
H11B H 0.2957 0.5437 0.0884 0.109 Uiso 1 d
H12B H 0.0294 0.4894 0.0734 0.085 Uiso 1 d
H12C H 0.0632 0.6145 0.0945 0.085 Uiso 1 d
H12A H 0.0312 0.5148 0.1227 0.085 Uiso 1 d
H13A H 0.3170 -0.0349 0.1870 0.092 Uiso 1 d
H13B H 0.2548 -0.1459 0.1703 0.092 Uiso 1 d
H13C H 0.2230 -0.0438 0.1977 0.092 Uiso 1 d
H14C H 0.2477 -0.0248 0.0552 0.081 Uiso 1 d
H14A H 0.2673 -0.1352 0.0874 0.081 Uiso 1 d
H14B H 0.3326 -0.0243 0.0946 0.081 Uiso 1 d
H15B H 0.0628 -0.0565 0.1303 0.082 Uiso 1 d
H15C H 0.1037 -0.1443 0.1012 0.082 Uiso 1 d
H15A H 0.0540 -0.0265 0.0807 0.082 Uiso 1 d
H16A H 0.2564 0.2701 0.0477 0.069 Uiso 1 d
H16B H 0.3226 0.1863 0.0806 0.069 Uiso 1 d
H16C H 0.3286 0.3272 0.0864 0.069 Uiso 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'
Ru Ru -1.2594 0.8363 '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'
Si Si 0.0817 0.0704 '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
C16 Ru1 P3 80.3(2)
C16 Ru1 P2 177.6(2)
P3 Ru1 P2 97.49(5)
C16 Ru1 P1 80.2(2)
P3 Ru1 P1 159.74(5)
P2 Ru1 P1 102.00(5)
C16 Ru1 P4 89.41(15)
P3 Ru1 P4 94.47(5)
P2 Ru1 P4 91.63(5)
P1 Ru1 P4 90.47(5)
C16 Ru1 Si1 89.95(15)
P3 Ru1 Si1 87.94(5)
P2 Ru1 Si1 89.11(5)
P1 Ru1 Si1 86.90(5)
P4 Ru1 Si1 177.36(5)
C2 P1 C3 98.3(3)
C2 P1 C1 97.8(4)
C3 P1 C1 94.7(3)
C2 P1 Ru1 124.0(2)
C3 P1 Ru1 118.5(2)
C1 P1 Ru1 117.8(2)
C5 P2 C6 96.2(3)
C5 P2 C4 97.1(3)
C6 P2 C4 95.7(3)
C5 P2 Ru1 121.0(2)
C6 P2 Ru1 121.8(2)
C4 P2 Ru1 119.2(2)
C9 P3 C8 99.5(4)
C9 P3 C7 95.6(4)
C8 P3 C7 96.7(4)
C9 P3 Ru1 118.1(2)
C8 P3 Ru1 123.4(2)
C7 P3 Ru1 118.1(2)
C12 P4 C11 100.7(3)
C12 P4 C10 96.5(3)
C11 P4 C10 96.7(4)
C12 P4 Ru1 116.5(2)
C11 P4 Ru1 118.9(2)
C10 P4 Ru1 122.8(2)
C14 Si1 C15 102.0(3)
C14 Si1 C13 97.1(3)
C15 Si1 C13 97.3(3)
C14 Si1 Ru1 118.0(2)
C15 Si1 Ru1 116.7(2)
C13 Si1 Ru1 121.6(2)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Ru1 C16 2.215(6)
Ru1 P3 2.3181(12)
Ru1 P2 2.3400(13)
Ru1 P1 2.3680(13)
Ru1 P4 2.3813(13)
Ru1 Si1 2.4681(14)
P1 C2 1.828(7)
P1 C3 1.829(6)
P1 C1 1.841(6)
P2 C5 1.833(6)
P2 C6 1.843(6)
P2 C4 1.848(7)
P3 C9 1.805(7)
P3 C8 1.819(7)
P3 C7 1.827(7)
P4 C12 1.834(6)
P4 C11 1.843(7)
P4 C10 1.857(7)
Si1 C14 1.916(6)
Si1 C15 1.916(6)
Si1 C13 1.921(6)
