#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/51/4075187.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_4075187
loop_
_publ_author_name
'Sakaba, Hiroyuki'
'Hirata, Takeshi'
'Kabuto, Chizuko'
'Kabuto, Kuninobu'
_publ_section_title
;
 Synthesis, Structure, and Dynamic Behavior of Tungsten Dihydride Silyl
 Complexes Cp*(CO)2W(H)2(SiHPhR) (R = Ph, H, Cl)
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              5145
_journal_paper_doi               10.1021/om060101r
_journal_volume                  25
_journal_year                    2006
_chemical_formula_moiety         'C18 H24 O2 Si W '
_chemical_formula_sum            'C18 H24 O2 Si W'
_chemical_formula_weight         484.32
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_cell_angle_alpha                90.0000
_cell_angle_beta                 91.597(4)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   8.5362(18)
_cell_length_b                   15.006(3)
_cell_length_c                   14.409(3)
_cell_measurement_reflns_used    6875
_cell_measurement_temperature    173.1
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      3.7
_cell_volume                     1845.0(7)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.7.0'
_computing_structure_refinement  CRYSTALS
_computing_structure_solution    SIR92
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       ω
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.025
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            16214
_diffrn_reflns_theta_full        27.40
_diffrn_reflns_theta_max         27.40
_exptl_absorpt_coefficient_mu    6.337
_exptl_absorpt_correction_T_max  0.531
_exptl_absorpt_correction_T_min  0.335
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.743
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             944.00
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.47
_refine_diff_density_min         -0.94
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_parameters     235
_refine_ls_number_reflns         4015
_refine_ls_R_factor_gt           0.0244
_refine_ls_shift/su_max          0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[0.0003Fo² + 1.0000σ(Fo²)]/(4Fo²)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0670
_reflns_number_gt                3568
_reflns_number_total             4015
_reflns_threshold_expression     F²>2.0σ(F²)
_cod_data_source_file            om060101rsi20060201_115927.cif
_cod_data_source_block           '__complex8b'
_cod_original_formula_sum        'C18 H24 O2 Si W '
_cod_database_code               4075187
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 +X,+Y,+Z
2 1/2-X,1/2+Y,1/2-Z
3 -X,-Y,-Z
4 1/2+X,1/2-Y,1/2+Z
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
W(1) W 0.248030(10) 0.372340(10) 0.347360(10) 0.01634(4) Uani 1.00 1 d .
Si(1) Si 0.45268(12) 0.31718(6) 0.23325(6) 0.0269(2) Uani 1.00 1 d .
O(1) O 0.1520(3) 0.4181(2) 0.14252(19) 0.0376(8) Uani 1.00 1 d .
O(2) O 0.3851(3) 0.55782(18) 0.4083(2) 0.0405(8) Uani 1.00 1 d .
C(1) C 0.1915(4) 0.4027(2) 0.2175(2) 0.0256(9) Uani 1.00 1 d .
C(2) C 0.3348(4) 0.4904(2) 0.3841(2) 0.0252(9) Uani 1.00 1 d .
C(3) C 0.0643(4) 0.2589(2) 0.3622(2) 0.0261(9) Uani 1.00 1 d .
C(4) C 0.0464(4) 0.3180(2) 0.4395(2) 0.0227(8) Uani 1.00 1 d .
C(5) C 0.1881(4) 0.3163(2) 0.4945(2) 0.0229(8) Uani 1.00 1 d .
C(6) C 0.2922(4) 0.2550(2) 0.4529(2) 0.0239(8) Uani 1.00 1 d .
C(7) C 0.2163(4) 0.2188(2) 0.3719(2) 0.0257(8) Uani 1.00 1 d .
C(8) C -0.0587(5) 0.2336(3) 0.2909(2) 0.0420(12) Uani 1.00 1 d .
C(9) C -0.1008(5) 0.3643(2) 0.4642(3) 0.0355(11) Uani 1.00 1 d .
C(10) C 0.2150(5) 0.3630(2) 0.5856(2) 0.0305(10) Uani 1.00 1 d .
C(11) C 0.4496(5) 0.2272(2) 0.4936(3) 0.0360(11) Uani 1.00 1 d .
C(12) C 0.2675(6) 0.1404(2) 0.3145(3) 0.0399(12) Uani 1.00 1 d .
C(13) C 0.5849(4) 0.4013(2) 0.1797(2) 0.0260(9) Uani 1.00 1 d .
C(14) C 0.6837(4) 0.4573(2) 0.2328(2) 0.0324(10) Uani 1.00 1 d .
C(15) C 0.7873(5) 0.5152(2) 0.1925(3) 0.0397(12) Uani 1.00 1 d .
C(16) C 0.7929(5) 0.5195(2) 0.0968(3) 0.0395(12) Uani 1.00 1 d .
C(17) C 0.6948(6) 0.4669(3) 0.0427(3) 0.0472(13) Uani 1.00 1 d .
C(18) C 0.5932(5) 0.4080(3) 0.0837(2) 0.0385(11) Uani 1.00 1 d .
H(1) H 0.102(5) 0.445(3) 0.338(3) 0.053(14) Uiso 1.00 1 c .
H(2) H 0.448(5) 0.381(2) 0.356(3) 0.036(12) Uiso 1.00 1 c .
H(3) H 0.392(5) 0.275(3) 0.152(3) 0.047(13) Uiso 1.00 1 c .
H(4) H 0.559(6) 0.258(3) 0.278(3) 0.069(17) Uiso 1.00 1 c .
H(5) H -0.1514 0.2668 0.3011 0.050 Uiso 1.00 1 c R
H(6) H -0.0806 0.1718 0.2957 0.050 Uiso 1.00 1 c R
H(7) H -0.0219 0.2463 0.2307 0.050 Uiso 1.00 1 c R
H(8) H -0.0758 0.4180 0.4962 0.043 Uiso 1.00 1 c R
H(9) H -0.1603 0.3268 0.5030 0.043 Uiso 1.00 1 c R
H(10) H -0.1603 0.3776 0.4093 0.043 Uiso 1.00 1 c R
H(11) H 0.3163 0.3486 0.6100 0.037 Uiso 1.00 1 c R
H(12) H 0.1381 0.3444 0.6279 0.037 Uiso 1.00 1 c R
H(13) H 0.2074 0.4256 0.5764 0.037 Uiso 1.00 1 c R
H(14) H 0.4945 0.1834 0.4549 0.043 Uiso 1.00 1 c R
H(15) H 0.4364 0.2032 0.5539 0.043 Uiso 1.00 1 c R
H(16) H 0.5168 0.2776 0.4976 0.043 Uiso 1.00 1 c R
H(17) H 0.1870 0.1258 0.2703 0.048 Uiso 1.00 1 c R
H(18) H 0.2873 0.0907 0.3540 0.049 Uiso 1.00 1 c R
H(19) H 0.3604 0.1554 0.2832 0.049 Uiso 1.00 1 c R
H(20) H 0.6803 0.4559 0.2932 0.039 Uiso 1.00 1 c R
H(21) H 0.8598 0.5492 0.2297 0.048 Uiso 1.00 1 c R
H(22) H 0.8545 0.5518 0.0664 0.048 Uiso 1.00 1 c R
H(23) H 0.6806 0.4697 -0.0251 0.057 Uiso 1.00 1 c R
H(24) H 0.5267 0.3740 0.0495 0.046 Uiso 1.00 1 c R
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.003 0.002
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.000 0.000
;
International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.4)
;
O O 0.011 0.006
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Si Si 0.082 0.070
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
W W -0.849 6.872
;
International Tables for Crystallography
(1992, 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
Si(1) W(1) C(1) 67.68(11)
Si(1) W(1) C(2) 101.71(11)
Si(1) W(1) C(3) 107.16(9)
Si(1) W(1) C(4) 140.54(8)
Si(1) W(1) C(5) 129.12(9)
Si(1) W(1) C(6) 94.20(9)
Si(1) W(1) C(7) 82.16(9)
C(1) W(1) C(2) 97.27(15)
C(1) W(1) C(3) 96.23(14)
C(1) W(1) C(4) 116.89(14)
C(1) W(1) C(5) 152.19(14)
C(1) W(1) C(6) 144.83(13)
C(1) W(1) C(7) 110.08(14)
C(2) W(1) C(3) 150.99(14)
C(2) W(1) C(4) 115.62(13)
C(2) W(1) C(5) 99.64(13)
C(2) W(1) C(6) 116.34(13)
C(2) W(1) C(7) 151.50(14)
C(3) W(1) C(4) 35.74(12)
C(3) W(1) C(5) 59.42(12)
C(3) W(1) C(6) 59.27(12)
C(3) W(1) C(7) 35.70(13)
C(4) W(1) C(5) 35.38(12)
C(4) W(1) C(6) 58.74(12)
C(4) W(1) C(7) 59.00(12)
C(5) W(1) C(6) 35.23(12)
C(5) W(1) C(7) 58.94(12)
C(6) W(1) C(7) 35.35(12)
W(1) Si(1) C(13) 118.33(12)
W(1) C(1) O(1) 176.7(3)
W(1) C(2) O(2) 177.8(3)
W(1) C(3) C(4) 72.9(2)
W(1) C(3) C(7) 72.8(2)
W(1) C(3) C(8) 125.7(2)
C(4) C(3) C(7) 107.4(3)
C(4) C(3) C(8) 126.9(3)
C(7) C(3) C(8) 125.2(3)
W(1) C(4) C(3) 71.4(2)
W(1) C(4) C(5) 72.4(2)
W(1) C(4) C(9) 127.6(2)
C(3) C(4) C(5) 108.2(3)
C(3) C(4) C(9) 125.7(3)
C(5) C(4) C(9) 125.7(3)
W(1) C(5) C(4) 72.23(19)
W(1) C(5) C(6) 72.35(19)
W(1) C(5) C(10) 126.1(2)
C(4) C(5) C(6) 107.9(2)
C(4) C(5) C(10) 125.7(3)
C(6) C(5) C(10) 126.1(3)
W(1) C(6) C(5) 72.42(19)
W(1) C(6) C(7) 72.22(19)
W(1) C(6) C(11) 125.7(2)
C(5) C(6) C(7) 108.4(3)
C(5) C(6) C(11) 125.0(3)
C(7) C(6) C(11) 126.3(3)
W(1) C(7) C(3) 71.46(19)
W(1) C(7) C(6) 72.42(19)
W(1) C(7) C(12) 130.3(2)
C(3) C(7) C(6) 108.0(3)
C(3) C(7) C(12) 123.3(3)
C(6) C(7) C(12) 127.8(3)
Si(1) C(13) C(14) 122.6(2)
Si(1) C(13) C(18) 120.4(3)
C(14) C(13) C(18) 117.0(3)
C(13) C(14) C(15) 122.0(3)
C(14) C(15) C(16) 119.3(4)
C(15) C(16) C(17) 120.1(4)
C(16) C(17) C(18) 120.2(4)
C(13) C(18) C(17) 121.4(4)
Si(1) W(1) H(1) 133.2(17)
Si(1) W(1) H(2) 51.7(15)
C(1) W(1) H(1) 67.0(17)
C(1) W(1) H(2) 105.7(16)
C(2) W(1) H(1) 73.2(17)
C(2) W(1) H(2) 63.0(13)
C(3) W(1) H(1) 88.8(17)
C(3) W(1) H(2) 136.3(13)
C(4) W(1) H(1) 73.1(17)
C(4) W(1) H(2) 136.8(15)
C(5) W(1) H(1) 97.1(17)
C(5) W(1) H(2) 101.6(15)
C(6) W(1) H(1) 130.5(17)
C(6) W(1) H(2) 82.4(14)
C(7) W(1) H(1) 124.4(17)
C(7) W(1) H(2) 100.6(13)
H(1) W(1) H(2) 134(2)
W(1) Si(1) H(3) 116(2)
W(1) Si(1) H(4) 111(2)
C(13) Si(1) H(3) 99.8(19)
C(13) Si(1) H(4) 103(2)
H(3) Si(1) H(4) 108(2)
C(3) C(8) H(5) 109.5
C(3) C(8) H(6) 109.5
C(3) C(8) H(7) 109.5
H(5) C(8) H(6) 109.5
H(5) C(8) H(7) 109.5
H(6) C(8) H(7) 109.5
C(4) C(9) H(8) 109.5
C(4) C(9) H(9) 109.5
C(4) C(9) H(10) 109.5
H(8) C(9) H(9) 109.5
H(8) C(9) H(10) 109.5
H(9) C(9) H(10) 109.5
C(5) C(10) H(11) 109.5
C(5) C(10) H(12) 109.5
C(5) C(10) H(13) 109.5
H(11) C(10) H(12) 109.5
H(11) C(10) H(13) 109.5
H(12) C(10) H(13) 109.5
C(6) C(11) H(14) 109.5
C(6) C(11) H(15) 109.5
C(6) C(11) H(16) 109.5
H(14) C(11) H(15) 109.5
H(14) C(11) H(16) 109.5
H(15) C(11) H(16) 109.5
C(7) C(12) H(17) 109.5
C(7) C(12) H(18) 109.5
C(7) C(12) H(19) 109.5
H(17) C(12) H(18) 109.5
H(17) C(12) H(19) 109.5
H(18) C(12) H(19) 109.5
C(13) C(14) H(20) 119.7
C(15) C(14) H(20) 118.3
C(14) C(15) H(21) 120.8
C(16) C(15) H(21) 119.7
C(15) C(16) H(22) 125.5
C(17) C(16) H(22) 114.4
C(16) C(17) H(23) 126.5
C(18) C(17) H(23) 113.0
C(13) C(18) H(24) 117.1
C(17) C(18) H(24) 121.4
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
W(1) Si(1) 2.5691(10)
W(1) C(1) 1.973(3)
W(1) C(2) 1.986(3)
W(1) C(3) 2.329(3)
W(1) C(4) 2.349(3)
W(1) C(5) 2.351(3)
W(1) C(6) 2.350(3)
W(1) C(7) 2.347(3)
Si(1) C(13) 1.874(3)
O(1) C(1) 1.145(4)
O(2) C(2) 1.149(4)
C(3) C(4) 1.435(5)
C(3) C(7) 1.433(5)
C(3) C(8) 1.497(5)
C(4) C(5) 1.428(5)
C(4) C(9) 1.487(5)
C(5) C(6) 1.423(5)
C(5) C(10) 1.499(5)
C(6) C(7) 1.426(5)
C(6) C(11) 1.510(5)
C(7) C(12) 1.509(5)
C(13) C(14) 1.402(5)
C(13) C(18) 1.390(5)
C(14) C(15) 1.380(6)
C(15) C(16) 1.382(6)
C(16) C(17) 1.376(6)
C(17) C(18) 1.383(6)
W(1) H(1) 1.66(5)
W(1) H(2) 1.71(4)
Si(1) H(3) 1.42(4)
Si(1) H(4) 1.41(5)
C(8) H(5) 0.950
C(8) H(6) 0.950
C(8) H(7) 0.950
C(9) H(8) 0.950
C(9) H(9) 0.950
C(9) H(10) 0.950
C(10) H(11) 0.950
C(10) H(12) 0.950
C(10) H(13) 0.950
C(11) H(14) 0.950
C(11) H(15) 0.950
C(11) H(16) 0.950
C(12) H(17) 0.950
C(12) H(18) 0.950
C(12) H(19) 0.950
C(14) H(20) 0.871
C(15) H(21) 0.954
C(16) H(22) 0.847
C(17) H(23) 0.982
C(18) H(24) 0.900
