#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:35:57 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179337 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/34/4323498.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_4323498
loop_
_publ_author_name
'Matthew D. Butts'
'Jeffrey C. Bryan'
'Xiao-Liang Luo'
'Gregory J. Kubas'
_publ_section_title
;
 Comparison of H-H versus Si-H σ-Bond Coordination and Activation on 16e
 Metal Fragments. Organosilane, N2, and Ethylene Addition to the Agostic
 Complex W(CO)3(PR3)2 and Dynamic NMR Behavior of the Latter
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3341
_journal_page_last               3353
_journal_paper_doi               10.1021/ic960870a
_journal_volume                  36
_journal_year                    1997
_chemical_formula_moiety         'W, 3(C O), (C9 H21 P), H, (C12 H10 Si)'
_chemical_formula_sum            'C48 H64 O6 P2 Si2 W2'
_chemical_formula_weight         1222.81
_chemical_name_common
;
tri-isopropylphosphinetricarbonylhydridetungsten dimer μ-diphenylsilane
;
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_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                 90.390(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.760(2)
_cell_length_b                   17.427(2)
_cell_length_c                   17.957(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      42.4
_cell_measurement_theta_min      7.6
_cell_volume                     4931.8(10)
_computing_cell_refinement       XSCANS
_computing_data_collection       XSCANS
_computing_data_reduction        XSCANS
_computing_molecular_graphics    SHELXTL
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       omega
_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  0.0885
_diffrn_reflns_av_sigmaI/netI    0.0579
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            5382
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         2.58
_diffrn_standards_interval_count 147
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.820
_exptl_absorpt_correction_T_max  0.511
_exptl_absorpt_correction_T_min  0.178
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.647
_exptl_crystal_description       block
_exptl_crystal_F_000             2424
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.18
_refine_diff_density_max         3.691
_refine_diff_density_min         -3.228
_refine_diff_density_rms         0.292
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.050
_refine_ls_goodness_of_fit_obs   1.088
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     277
_refine_ls_number_reflns         4535
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_restrained_S_obs      1.088
_refine_ls_R_factor_all          0.0863
_refine_ls_R_factor_obs          0.0607
_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)+(0.1071P)²+6.5801P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1661
_refine_ls_wR_factor_obs         0.1462
_reflns_number_observed          3383
_reflns_number_total             4539
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic960870a_3.cif
_cod_data_source_block           wsil1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1071P)^2^+6.5801P] 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^)+(0.1071P)^2^+6.5801P] 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               4323498
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
_atom_site_refinement_flags
_atom_site_disorder_group
W W 0.59480(2) 0.24300(2) 0.71675(2) 0.0179(2) Uani 1 d . .
P P 0.7543(2) 0.2275(2) 0.71633(14) 0.0217(5) Uani 1 d . .
Si Si 0.4597(2) 0.2427(2) 0.64055(15) 0.0212(6) Uani 1 d . .
C1 C 0.5834(6) 0.1292(5) 0.7021(6) 0.020(2) Uani 1 d . .
O1 O 0.5738(5) 0.0639(5) 0.6936(4) 0.036(2) Uani 1 d . .
C2 C 0.6182(7) 0.2700(7) 0.6115(6) 0.030(2) Uani 1 d . .
O2 O 0.6349(5) 0.2874(6) 0.5510(4) 0.044(2) Uani 1 d . .
C3 C 0.5967(6) 0.3581(6) 0.7336(6) 0.025(2) Uani 1 d . .
O3 O 0.5950(5) 0.4218(5) 0.7414(5) 0.043(2) Uani 1 d . .
C10 C 0.7992(7) 0.1922(7) 0.6269(6) 0.030(2) Uani 1 d . .
H10 H 0.7919(7) 0.2349(7) 0.5903(6) 0.035 Uiso 1 calc R .
C11 C 0.8930(7) 0.1746(8) 0.6289(7) 0.038(3) Uani 1 d . .
H11A H 0.9133(13) 0.1667(49) 0.5780(7) 0.057 Uiso 1 calc R .
H11B H 0.9028(9) 0.1279(27) 0.6583(40) 0.057 Uiso 1 calc R .
H11C H 0.9236(9) 0.2176(21) 0.6517(43) 0.057 Uiso 1 calc R .
C12 C 0.7516(7) 0.1216(7) 0.5930(6) 0.036(3) Uani 1 d . .
H12A H 0.7773(32) 0.1078(29) 0.5453(22) 0.054 Uiso 1 calc R .
H12B H 0.6917(12) 0.1347(16) 0.5850(41) 0.054 Uiso 1 calc R .
H12C H 0.7557(44) 0.0781(15) 0.6274(21) 0.054 Uiso 1 calc R .
C13 C 0.7949(6) 0.1658(7) 0.7944(6) 0.028(2) Uani 1 d . .
H13 H 0.7596(6) 0.1793(7) 0.8386(6) 0.033 Uiso 1 calc R .
C14 C 0.7796(8) 0.0810(7) 0.7808(6) 0.037(3) Uani 1 d . .
H14A H 0.7922(50) 0.0521(8) 0.8264(14) 0.056 Uiso 1 calc R .
H14B H 0.8165(36) 0.0631(12) 0.7407(31) 0.056 Uiso 1 calc R .
H14C H 0.7201(13) 0.0729(9) 0.7665(43) 0.056 Uiso 1 calc R .
C15 C 0.8879(7) 0.1779(8) 0.8196(7) 0.043(3) Uani 1 d . .
H15A H 0.9046(20) 0.1367(30) 0.8539(41) 0.064 Uiso 1 calc R .
H15B H 0.8932(14) 0.2275(25) 0.8450(46) 0.064 Uiso 1 calc R .
H15C H 0.9250(10) 0.1772(55) 0.7760(9) 0.064 Uiso 1 calc R .
C16 C 0.8151(7) 0.3188(6) 0.7283(6) 0.029(2) Uani 1 d . .
H16 H 0.8765(7) 0.3045(6) 0.7305(6) 0.035 Uiso 1 calc R .
C17 C 0.7937(8) 0.3571(7) 0.8037(6) 0.037(3) Uani 1 d . .
H17A H 0.8246(40) 0.4057(23) 0.8082(20) 0.055 Uiso 1 calc R .
H17B H 0.8105(48) 0.3229(20) 0.8446(6) 0.055 Uiso 1 calc R .
H17C H 0.7326(10) 0.3669(44) 0.8061(20) 0.055 Uiso 1 calc R .
C18 C 0.8050(8) 0.3732(7) 0.6649(7) 0.042(3) Uani 1 d . .
H18A H 0.8349(48) 0.4211(20) 0.6763(22) 0.063 Uiso 1 calc R .
H18B H 0.7445(9) 0.3840(40) 0.6570(32) 0.063 Uiso 1 calc R .
H18C H 0.8287(50) 0.3503(21) 0.6198(13) 0.063 Uiso 1 calc R .
C30 C 0.4196(7) 0.3271(7) 0.5846(6) 0.029(2) Uani 1 d . .
C31 C 0.4536(8) 0.4003(7) 0.5858(6) 0.038(3) Uani 1 d . .
H31 H 0.5040(8) 0.4093(7) 0.6138(6) 0.046 Uiso 1 calc R .
C32 C 0.4167(10) 0.4609(8) 0.5478(7) 0.051(4) Uani 1 d . .
H32 H 0.4419(10) 0.5104(8) 0.5486(7) 0.061 Uiso 1 calc R .
C33 C 0.3410(9) 0.4477(8) 0.5077(7) 0.049(4) Uani 1 d . .
H33 H 0.3146(9) 0.4887(8) 0.4815(7) 0.059 Uiso 1 calc R .
C34 C 0.3061(8) 0.3776(8) 0.5063(6) 0.043(3) Uani 1 d . .
H34 H 0.2548(8) 0.3693(8) 0.4793(6) 0.051 Uiso 1 calc R .
C35 C 0.3437(7) 0.3175(7) 0.5437(6) 0.032(3) Uani 1 d . .
H35 H 0.3178(7) 0.2683(7) 0.5420(6) 0.039 Uiso 1 calc R .
C40 C 0.4432(6) 0.1613(6) 0.5731(5) 0.023(2) Uani 1 d . .
C41 C 0.4061(6) 0.0911(6) 0.5921(6) 0.026(2) Uani 1 d . .
H41 H 0.3906(6) 0.0825(6) 0.6425(6) 0.031 Uiso 1 calc R .
C42 C 0.3912(8) 0.0340(7) 0.5408(6) 0.037(3) Uani 1 d . .
H42 H 0.3646(8) -0.0125(7) 0.5555(6) 0.044 Uiso 1 calc R .
C43 C 0.4152(7) 0.0446(6) 0.4676(6) 0.031(3) Uani 1 d . .
H43 H 0.4054(7) 0.0054(6) 0.4318(6) 0.037 Uiso 1 calc R .
C44 C 0.4533(7) 0.1123(7) 0.4469(6) 0.033(3) Uani 1 d . .
H44 H 0.4698(7) 0.1200(7) 0.3967(6) 0.040 Uiso 1 calc R .
C45 C 0.4675(7) 0.1681(7) 0.4984(6) 0.031(3) Uani 1 d . .
H45 H 0.4952(7) 0.2139(7) 0.4830(6) 0.038 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'
O O 0.0106 0.0060 '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'
W W -0.8490 6.8722 '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
C2 W C1 97.3(4) . . ?
C2 W C3 84.5(5) . . ?
C1 W C3 175.6(4) . . ?
C2 W Si 69.2(3) . . ?
C1 W Si 81.5(3) . . ?
C3 W Si 95.4(3) . . ?
C2 W P 80.3(3) . . ?
C1 W P 89.0(3) . . ?
C3 W P 95.3(3) . . ?
Si W P 146.47(9) . . ?
C2 W Si 164.5(3) . 2_656 ?
C1 W Si 95.4(3) . 2_656 ?
C3 W Si 82.2(3) . 2_656 ?
Si W Si 103.96(7) . 2_656 ?
P W Si 108.92(8) . 2_656 ?
C2 W W 122.1(3) . 2_656 ?
C1 W W 88.1(3) . 2_656 ?
C3 W W 87.6(3) . 2_656 ?
Si W W 54.56(6) . 2_656 ?
P W W 157.63(6) . 2_656 ?
Si W W 49.40(6) 2_656 2_656 ?
C10 P C16 100.5(5) . . ?
C10 P C13 108.9(5) . . ?
C16 P C13 103.3(5) . . ?
C10 P W 114.9(3) . . ?
C16 P W 114.7(4) . . ?
C13 P W 113.2(3) . . ?
C40 Si C30 101.6(5) . . ?
C40 Si W 117.5(3) . . ?
C30 Si W 124.4(4) . . ?
C40 Si W 124.6(3) . 2_656 ?
C30 Si W 113.3(3) . 2_656 ?
W Si W 76.04(7) . 2_656 ?
O1 C1 W 177.7(9) . . ?
O2 C2 W 177.1(10) . . ?
O3 C3 W 177.3(10) . . ?
C11 C10 C12 108.5(9) . . ?
C11 C10 P 115.1(8) . . ?
C12 C10 P 114.3(7) . . ?
C14 C13 C15 109.3(9) . . ?
C14 C13 P 112.6(7) . . ?
C15 C13 P 117.3(8) . . ?
C18 C16 C17 111.8(10) . . ?
C18 C16 P 113.7(8) . . ?
C17 C16 P 110.6(8) . . ?
C31 C30 C35 116.4(10) . . ?
C31 C30 Si 125.6(8) . . ?
C35 C30 Si 117.7(9) . . ?
C32 C31 C30 122.3(12) . . ?
C31 C32 C33 118.7(13) . . ?
C34 C33 C32 120.3(12) . . ?
C33 C34 C35 120.6(12) . . ?
C34 C35 C30 121.7(12) . . ?
C41 C40 C45 115.2(9) . . ?
C41 C40 Si 123.8(8) . . ?
C45 C40 Si 120.9(8) . . ?
C42 C41 C40 122.5(10) . . ?
C41 C42 C43 119.6(11) . . ?
C44 C43 C42 119.6(10) . . ?
C45 C44 C43 120.1(11) . . ?
C44 C45 C40 122.9(11) . . ?
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
W C2 1.984(11) . ?
W C1 2.008(9) . ?
W C3 2.029(10) . ?
W Si 2.523(3) . ?
W P 2.528(3) . ?
W Si 2.708(3) 2_656 ?
W W 3.2256(8) 2_656 ?
P C10 1.864(10) . ?
P C16 1.869(11) . ?
P C13 1.877(9) . ?
Si C40 1.883(10) . ?
Si C30 1.887(11) . ?
Si W 2.708(3) 2_656 ?
C1 O1 1.158(12) . ?
C2 O2 1.160(14) . ?
C3 O3 1.119(13) . ?
C10 C11 1.509(14) . ?
C10 C12 1.56(2) . ?
C13 C14 1.52(2) . ?
C13 C15 1.546(14) . ?
C16 C18 1.488(15) . ?
C16 C17 1.55(2) . ?
C30 C31 1.38(2) . ?
C30 C35 1.410(15) . ?
C31 C32 1.38(2) . ?
C32 C33 1.41(2) . ?
C33 C34 1.34(2) . ?
C34 C35 1.38(2) . ?
C40 C41 1.400(15) . ?
C40 C45 1.403(15) . ?
C41 C42 1.38(2) . ?
C42 C43 1.38(2) . ?
C43 C44 1.38(2) . ?
C44 C45 1.36(2) . ?
