#------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/2/00/63/2006397.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_2006397
loop_
_publ_author_name
'Kreiter, Cornelius G.'
'Schwarz, C. Bettina'
'Frank, Walter'
'Reiß, Guido J.'
_publ_contact_author
;
      Walter Frank
      Fachbereich Chemie
      Universität Kaiserslautern
      Erwin-Schrödinger-Straße
      67663 Kaiserslautern
      Germany
;
_publ_section_title
;Photochemical Reactions of Transition Metal Organyl Complexes with Olefins.
 18.
 Dicarbonylbis(η⁵-cyclopentadienyl)(μ-1,4-η:4,5-η-1,4-pentadien-1,4-diyl)oxoditungsten(W---W)
;
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1018
_journal_page_last               1020
_journal_paper_doi               10.1107/S0108270197004393
_journal_volume                  53
_journal_year                    1997
_chemical_formula_iupac          '[W2 O (C5 H5)2 (C5 H6) (C O)2]'
_chemical_formula_sum            'C17 H16 O3 W2'
_chemical_formula_weight         636.01
_chemical_name_systematic
;
Dicarbonylbis(η⁵-cyclopentadienyl)-(μ-1,4-η:4,5-η-1,4-pentadien-
1,4-diyl)oxoditungsten(W-W)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 95.48(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.6460(11)
_cell_length_b                   10.8490(13)
_cell_length_c                   15.9600(2)
_cell_measurement_reflns_used    50
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.54
_cell_measurement_theta_min      9.22
_cell_volume                     1490.2(3)
_computing_cell_refinement       'CAD4 Software'
_computing_data_collection       'CAD4 Software (Enraf-Nonius 1989)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1993)'
_computing_molecular_graphics    'SHELXTL-Plus (Sheldrick, 1991)'
_computing_publication_material  SHELXL-93
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'ENRAF-NONIUS CAD4 4-circle diffractometer'
_diffrn_measurement_method       'ω/θ scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0388
_diffrn_reflns_av_sigmaI/netI    0.0376
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5433
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         2.27
_diffrn_standards_decay_%        none
_diffrn_standards_interval_time  60
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    15.435
_exptl_absorpt_correction_T_max  0.0824
_exptl_absorpt_correction_T_min  0.0410
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
'transmission factors calculated using SHELX-76 (Sheldrick, 1976)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.835
_exptl_crystal_density_meas      ?
_exptl_crystal_description       'nearly isometric with broken edge'
_exptl_crystal_F_000             1160
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.26
_refine_diff_density_max         2.237
_refine_diff_density_min         -0.958
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.136
_refine_ls_goodness_of_fit_obs   1.160
_refine_ls_matrix_type           full
_refine_ls_number_parameters     205
_refine_ls_number_reflns         2625
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.136
_refine_ls_restrained_S_obs      1.159
_refine_ls_R_factor_all          0.0314
_refine_ls_R_factor_obs          .0284
_refine_ls_shift/esd_max         0.083
_refine_ls_shift/esd_mean        0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²)+(0.0402P)²+3.8P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0747
_refine_ls_wR_factor_obs         .0733
_reflns_number_observed          2446
_reflns_number_total             2625
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            jz1195.cif
_cod_data_source_block           C~17~H~16~W~2~O~3~
_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 'calc w =
1/[\s^2^(Fo^2^)+(0.0402P)^2^+3.8P] 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^)+(0.0402P)^2^+3.8P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        '[W2 O (CO)2 (C5 H5)2 (C5 H6)]'
_cod_database_code               2006397
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_group
_atom_site_type_symbol
W1 .24068(3) .05561(3) .37823(2) .02389(12) Uani d . 1 . W
W2 .26868(3) .08131(3) .19676(2) .02368(11) Uani d . 1 . W
O1 .3268(7) -.1962(5) .4644(4) .0472(14) Uani d . 1 . O
O2 .5947(7) .0622(7) .3597(4) .054(2) Uani d . 1 . O
O3 .2762(5) .2355(5) .2044(3) .0286(11) Uani d . 1 . O
C1 .2953(8) -.1049(9) .4326(5) .041(2) Uani d . 1 . C
C2 .4616(9) .0550(7) .3588(5) .031(2) Uani d . 1 . C
C11 .2785(11) .1821(8) .4934(5) .045(2) Uani d . 1 . C
C12 .2676(10) .2590(7) .4218(6) .047(2) Uani d . 1 . C
C13 .1170(9) .2478(8) .3825(4) .036(2) Uani d . 1 . C
C14 .0340(9) .1626(8) .4277(4) .042(2) Uani d . 1 . C
C15 .1350(11) .1251(9) .4981(5) .049(2) Uani d . 1 . C
C21 .5178(9) .0159(10) .1767(5) .048(2) Uani d . 1 . C
C22 .4421(12) .0492(10) .0979(6) .055(3) Uani d . 1 . C
C23 .3303(14) -.0399(12) .0791(6) .073(4) Uani d . 1 . C
C24 .3386(11) -.1252(11) .1433(8) .070(4) Uani d . 1 . C
C25 .4518(10) -.0905(9) .2059(5) .047(2) Uani d . 1 . C
C31 .0594(10) .0861(7) .1153(5) .038(2) Uani d . 1 . C
C32 -.0762(9) .0797(8) .1475(5) .040(2) Uani d . 1 . C
C33 -.0707(9) .0525(8) .2395(5) .037(2) Uani d . 1 . C
C34 .0902(8) .0076(7) .2643(4) .030(2) Uani d . 1 . C
C35 .1166(9) -.1048(7) .3071(5) .031(2) Uani d D 1 . C
H11 .3664(11) .1712(8) .5310(5) .054 Uiso calc R 1 . H
H12 .3464(10) .3082(7) .4040(6) .057 Uiso calc R 1 . H
H13 .0777(9) .2898(8) .3343(4) .043 Uiso calc R 1 . H
H14 -.0676(9) .1361(8) .4139(4) .050 Uiso calc R 1 . H
H15 .1100(11) .0717(9) .5403(5) .059 Uiso calc R 1 . H
H21 .6000(9) .0588(10) .2049(5) .058 Uiso calc R 1 . H
H22 .4631(12) .1171(10) .0653(6) .066 Uiso calc R 1 . H
H23 .2607(14) -.0420(12) .0309(6) .088 Uiso calc R 1 . H
H24 .2772(11) -.1955(11) .1443(8) .084 Uiso calc R 1 . H
H25 .4782(10) -.1302(9) .2570(5) .056 Uiso calc R 1 . H
H31 .0629(10) .0928(7) .0575(5) .045 Uiso calc R 1 . H
H32 -.1696(9) .0914(8) .1145(5) .048 Uiso calc R 1 . H
H331 -.1464(9) -.0102(8) .2502(5) .049 Uiso calc R 1 . H
H332 -.0922(9) .1262(8) .2708(5) .049 Uiso calc R 1 . H
H351 .039(7) -.143(7) .338(5) .044 Uiso d D 1 . H
H352 .181(8) -.170(6) .289(5) .044 Uiso d D 1 . H
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'
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_publ_flag
C1 W1 C2 82.6(3) yes
C1 W1 C11 99.5(4) ?
C1 W1 C12 133.8(4) ?
C1 W1 C13 149.1(3) ?
C1 W1 C14 116.6(3) ?
C1 W1 C15 91.2(3) ?
C1 W1 C34 104.6(3) ?
C1 W1 C35 68.3(3) ?
C2 W1 C11 93.6(3) ?
C2 W1 C12 88.8(3) ?
C2 W1 C13 117.4(3) ?
C2 W1 C14 147.5(3) ?
C2 W1 C15 126.6(3) ?
C2 W1 C34 112.1(3) ?
C2 W1 C35 109.6(3) ?
C11 W1 C34 146.6(3) ?
C11 W1 C35 151.3(3) ?
C12 W1 C34 120.6(3) ?
C12 W1 C35 154.4(3) ?
C13 W1 C34 90.0(3) ?
C13 W1 C35 119.8(3) ?
C14 W1 C34 89.2(3) ?
C14 W1 C35 102.0(3) ?
C15 W1 C34 120.7(3) ?
C15 W1 C35 116.9(3) ?
C1 W1 W2 118.4(3) ?
C2 W1 W2 70.9(2) yes
C11 W1 W2 135.5(2) ?
C12 W1 W2 100.9(2) ?
C13 W1 W2 91.4(2) ?
C14 W1 W2 115.1(2) ?
C15 W1 W2 148.8(2) ?
O3 W2 C21 106.6(3) ?
O3 W2 C22 100.2(3) ?
O3 W2 C23 126.5(4) ?
O3 W2 C24 155.8(3) ?
O3 W2 C25 137.4(3) ?
O3 W2 C31 92.5(3) ?
O3 W2 C34 111.4(3) ?
C21 W2 C31 132.1(3) ?
C21 W2 C34 133.2(3) ?
C22 W2 C31 99.0(4) ?
C22 W2 C34 147.5(3) ?
C23 W2 C31 77.0(3) ?
C23 W2 C34 114.7(4) ?
C24 W2 C34 92.7(3) ?
C24 W2 C31 91.9(3) ?
C25 W2 C34 100.4(3) ?
C25 W2 C31 124.4(3) ?
C31 W2 C34 72.6(3) ?
O3 W2 W1 91.69(15) ?
C21 W2 W1 105.8(2) ?
C22 W2 W1 141.2(3) ?
C23 W2 W1 140.0(3) ?
C24 W2 W1 107.3(3) ?
C25 W2 W1 89.0(2) ?
C31 W2 W1 117.3(2) ?
W1 C1 O1 179.3(8) yes
W1 C2 W2 70.2(2) yes
W1 C2 O2 169.5(7) yes
C15 C11 C12 108.3(8) ?
C11 C12 C13 107.4(7) ?
C12 C13 C14 109.1(7) ?
C13 C14 C15 106.7(8) ?
C14 C15 C11 108.4(8) ?
C25 C21 C22 110.0(8) ?
C21 C22 C23 105.7(10) ?
C22 C23 C24 108.9(9) ?
C23 C24 C25 109.7(10) ?
C24 C25 C21 105.5(8) ?
C32 C31 W2 119.7(6) yes
C31 C32 C33 116.4(7) yes
C32 C33 C34 105.4(6) yes
W1 C34 W2 85.9(3) ?
W1 C34 C33 127.3(5) ?
W2 C34 C33 116.6(5) yes
W2 C34 C35 118.8(5) yes
C33 C34 C35 121.1(7) yes
C34 C35 H351 122.(5) ?
W1 C35 H351 113.(5) ?
C34 C35 H352 124.(5) ?
W1 C35 H352 117.(5) ?
H351 C35 H352 107.(7) ?
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
W1 W2 . 2.9426(5) yes
W1 C1 . 1.982(9) yes
W1 C2 . 1.964(8) yes
W1 C11 . 2.292(7) yes
W1 C12 . 2.319(7) yes
W1 C13 . 2.347(8) yes
W1 C14 . 2.331(8) yes
W1 C15 . 2.323(8) yes
W1 C34 . 2.196(7) yes
W1 C35 . 2.289(7) yes
W2 O3 . 1.678(5) yes
W2 C2 . 2.955(7) yes
W2 C21 . 2.319(8) yes
W2 C22 . 2.304(8) yes
W2 C23 . 2.394(9) yes
W2 C24 . 2.492(10) yes
W2 C25 . 2.441(8) yes
W2 C31 . 2.125(8) yes
W2 C34 . 2.121(7) yes
O1 C1 . 1.135(10) yes
O2 C2 . 1.152(10) yes
C11 C12 . 1.411(13) n
C12 C13 . 1.396(12) n
C13 C14 . 1.410(12) n
C14 C15 . 1.415(12) n
C11 C15 . 1.395(13) n
C21 C22 . 1.408(14) n
C22 C23 . 1.38(2) n
C23 C24 . 1.38(2) n
C24 C25 . 1.383(14) n
C21 C25 . 1.388(14) n
C31 C32 . 1.325(12) yes
C32 C33 . 1.495(11) yes
C33 C34 . 1.491(10) yes
C34 C35 . 1.406(11) yes
C11 H11 . .93 ?
C12 H12 . .93 ?
C13 H13 . .93 ?
C14 H14 . .93 ?
C15 H15 . .93 ?
C21 H21 . .93 ?
C22 H22 . .93 ?
C23 H23 . .93 ?
C24 H24 . .93 ?
C25 H25 . .93 ?
C31 H31 . .93 ?
C32 H32 . .93 ?
C33 H331 . .97 ?
C33 H332 . .97 ?
C35 H351 . .96(2) ?
C35 H352 . .96(2) ?
