#------------------------------------------------------------------------------
#$Date: 2016-02-19 16:29:56 +0200 (Fri, 19 Feb 2016) $
#$Revision: 176759 $
#$URL: svn://www.crystallography.net/cod/cif/2/00/49/2004990.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_2004990
loop_
_publ_author_name
'Legzdins, P.'
'Rettig, S. J.'
'Sayers, S. F.'
_publ_section_title
;
 Dioxo(η⁵-pentamethylcyclopentadienyl)(trimethylsilylmethyl)tungsten(VI)
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1355
_journal_page_last               1357
_journal_paper_doi               10.1107/S0108270196001217
_journal_volume                  52
_journal_year                    1996
_chemical_formula_iupac          '[W O2 (C10 H15) (C4 H11 Si)]'
_chemical_formula_moiety         'C14 H26 O2 Si W'
_chemical_formula_sum            'C14 H26 O2 Si W'
_chemical_formula_weight         438.29
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.450(2)
_cell_length_b                   12.383(3)
_cell_length_c                   14.453(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    294.2
_cell_measurement_theta_max      15.7
_cell_measurement_theta_min      13.2
_cell_volume                     1691.3(6)
_computing_cell_refinement       'MSC/AFC Diffractometer Control Software'
_computing_data_collection
;MSC/AFC Diffractometer Control Software (Molecular Structure Corporation,
 1988)
;
_computing_data_reduction
'TEXSAN (Molecular Structure Corporation, 1992)'
_computing_publication_material  TEXSAN
_computing_structure_refinement  TEXSAN
_computing_structure_solution    'DIRDIF (Buerskens et al., 1994)'
_diffrn_ambient_temperature      294.2
_diffrn_measurement_device       'Rigaku AFC6S'
_diffrn_measurement_method       ω-2θ
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.00
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2242
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         1.75
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    6.90
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.423
_exptl_absorpt_correction_type
;
\y-scans (North, Phillips, & Mathews, 1968)
;
_exptl_absorpt_process_details   'ψ scans'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.721
_exptl_crystal_density_meas      ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             856
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.52
_refine_diff_density_min         -0.62
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   1.267
_refine_ls_hydrogen_treatment    'H atoms: C---H riding, see text'
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     91
_refine_ls_number_reflns         1202
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0962
_refine_ls_R_factor_obs          0.0284
_refine_ls_shift/esd_max         0.0002
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/σ²(F)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0313
_refine_ls_wR_factor_obs         0.0257
_reflns_number_observed          1202
_reflns_number_total             2242
_reflns_observed_criterion       I>3\s(I)
_cod_data_source_file            fg1161.cif
_cod_data_source_block           pl155
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'w = 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        1691.4(4)
_cod_database_code               2004990
loop_
_symmetry_equiv_pos_as_xyz
'   +x,   +y,   +z'
1/2+x,1/2-y,1/2-z
'   -x,1/2+y,   -z'
'1/2-x,   -y,1/2+z'
'   -x,   -y,   -z'
1/2-x,1/2+y,1/2+z
'   +x,1/2-y,   +z'
'1/2+x,   +y,1/2-z'
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
W(1) 0.0308(2) 0.0672(3) 0.0351(2) 0.0000 -0.0015(2) 0.0000
Si(1) 0.0440(10) 0.076(2) 0.041(2) 0.0000 -0.0090(10) 0.0000
O(1) 0.049(2) 0.087(4) 0.065(3) 0.016(3) -0.012(2) -0.015(3)
C(1) 0.035(5) 0.069(7) 0.036(5) 0.0000 -0.014(4) 0.0000
C(2) 0.034(3) 0.052(5) 0.044(3) 0.003(3) -0.007(3) -0.010(3)
C(3) 0.028(3) 0.061(4) 0.040(3) -0.006(2) -0.001(2) 0.008(3)
C(4) 0.037(5) 0.120(10) 0.034(5) 0.0000 -0.004(4) 0.0000
C(5) 0.074(5) 0.065(6) 0.085(5) 0.006(4) -0.019(4) -0.020(5)
C(6) 0.052(4) 0.106(7) 0.055(4) -0.018(4) -0.011(3) 0.019(4)
C(7) 0.042(4) 0.056(6) 0.043(4) 0.0000 -0.004(4) 0.0000
C(8) 0.071(7) 0.130(10) 0.047(6) 0.0000 -0.017(5) 0.0000
C(9) 0.062(4) 0.103(7) 0.081(5) 0.018(5) -0.018(4) -0.001(6)
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
W(1) 0.14269(3) 0.2500 0.40718(2) 0.0443(1) Uani
Si(1) 0.3193(3) 0.2500 0.6136(2) 0.0536(8) Uani
O(1) 0.2441(4) 0.1375(4) 0.3866(3) 0.067(2) Uani
C(1) -0.0123(8) 0.2500 0.2826(6) 0.047(3) Uani
C(2) -0.0527(6) 0.1567(5) 0.3337(4) 0.043(2) Uani
C(3) -0.1080(5) 0.1931(5) 0.4182(4) 0.043(2) Uani
C(4) 0.0554(9) 0.2500 0.1882(6) 0.065(3) Uani
C(5) -0.0377(7) 0.0429(6) 0.3020(5) 0.075(3) Uani
C(6) -0.1714(6) 0.1225(7) 0.4926(5) 0.071(2) Uani
C(7) 0.1427(9) 0.2500 0.5544(6) 0.047(2) Uani
C(8) 0.290(1) 0.2500 0.7408(7) 0.084(4) Uani
C(9) 0.4219(7) 0.1274(7) 0.5828(5) 0.082(3) Uani
H(1) 0.1586 0.2500 0.1948 0.0781 Uiso
H(2) 0.0244 0.1860 0.1537 0.0781 Uiso
H(3) -0.0768 0.0357 0.2395 0.0896 Uiso
H(4) 0.0626 0.0230 0.3014 0.0896 Uiso
H(5) -0.0892 -0.0049 0.3443 0.0896 Uiso
H(6) -0.1757 0.1628 0.5509 0.0854 Uiso
H(7) -0.2672 0.1008 0.4743 0.0854 Uiso
H(8) -0.1126 0.0580 0.5009 0.0854 Uiso
H(9) 0.0916 0.1854 0.5748 0.0565 Uiso
H(10) 0.3819 0.2500 0.7726 0.1006 Uiso
H(11) 0.2384 0.1847 0.7586 0.1006 Uiso
H(12) 0.3676 0.0629 0.5997 0.0988 Uiso
H(13) 0.4404 0.1270 0.5161 0.0988 Uiso
H(14) 0.5120 0.1276 0.6165 0.0988 Uiso
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C 0.003 0.002 'International Tables'
H 0.000 0.000 'International Tables'
O 0.011 0.006 'International Tables'
Si 0.082 0.070 'International Tables'
W -0.849 6.872 'International Tables'
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
4 1 2
-3 2 2
1 -2 3
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O(1) W(1) O(1) ? 7 108.5(3) yes
O(1) W(1) C(7) ? ? 100.0(2) yes
O(1) W(1) CP ? ? 117.7 yes
C(7) W(1) CP ? ? 110.0 yes
C(7) Si(1) C(8) ? ? 108.7(4) yes
C(7) Si(1) C(9) ? ? 110.8(3) yes
C(8) Si(1) C(9) ? ? 108.3(3) yes
C(9) Si(1) C(9) ? 7 109.8(5) yes
C(2) C(1) C(2) ? 7 108.5(7) yes
C(2) C(1) C(4) ? ? 125.7(4) yes
C(1) C(2) C(3) ? ? 106.9(6) yes
C(1) C(2) C(5) ? ? 125.7(6) yes
C(3) C(2) C(5) ? ? 127.4(6) yes
C(2) C(3) C(3) ? 7 108.7(4) yes
C(2) C(3) C(6) ? ? 125.6(6) yes
C(3) C(3) C(6) 7 ? 125.4(4) yes
Si(1) C(7) W(1) ? ? 117.1(4) yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
W(1) O(1) ? 1.717(4) yes
W(1) C(1) ? 2.321(8) yes
W(1) C(2) ? 2.424(6) yes
W(1) C(3) ? 2.477(4) yes
W(1) C(7) ? 2.128(8) yes
W(1) CP ? 2.11 yes
Si(1) C(7) ? 1.876(8) yes
Si(1) C(8) ? 1.860(10) yes
Si(1) C(9) ? 1.855(8) yes
C(1) C(2) ? 1.424(8) yes
C(1) C(4) ? 1.510(10) yes
C(2) C(3) ? 1.403(7) yes
C(2) C(5) ? 1.488(9) yes
C(3) C(3) 7 1.410(10) yes
C(3) C(6) ? 1.510(8) yes
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
O(1) C(4) 3.430(9) 2 no
O(1) H(2) 2.78 8 no
O(1) H(3) 2.79 8 no
C(2) H(1) 2.99 2_455 no
C(3) H(1) 2.83 2_455 no
H(5) H(9) 2.52 5_556 no
H(7) H(12) 2.48 5_556 no
H(8) H(8) 2.57 5_556 no
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
W(1) C(7) Si(1) C(8) ? ? ? 180 no
W(1) C(7) Si(1) C(9) ? ? ? -61.1(3) no
Si(1) C(7) W(1) O(1) ? ? ? 55.5(2) no
Si(1) C(7) W(1) C(1) ? ? ? 180 no
Si(1) C(7) W(1) C(2) ? ? ? 148.0(2) no
Si(1) C(7) W(1) C(3) ? ? ? 163.40(10) no
C(1) C(2) C(3) C(3) ? ? 7 2.6(5) no
C(1) C(2) C(3) C(6) ? ? ? 176.6(5) no
C(2) C(1) C(2) C(3) ? 7 7 4.2(8) no
C(2) C(1) C(2) C(5) ? 7 7 -176.0(4) no
C(2) C(3) C(3) C(2) ? 7 7 0 no
C(2) C(3) C(3) C(6) ? 7 7 174.0(6) no
C(3) C(2) C(1) C(4) ? ? ? 178.6(6) no
C(3) C(3) C(2) C(5) 7 7 7 177.6(5) no
C(4) C(1) C(2) C(5) ? ? ? -1.0(10) no
C(5) C(2) C(3) C(6) ? ? ? -3.6(9) no
C(6) C(3) C(3) C(6) ? 7 7 0 no
