Photochemical Reactions of Transition Metal Organyl Complexes with Olefins. 18. Dicarbonylbis(η^5^-cyclopentadienyl)(μ-1,4-η:4,5-η-1,4-pentadien-1,4-diyl)oxoditungsten(<i>W</i>—<i>W</i>)
Kreiter, Cornelius G.; Schwarz, C. Bettina; Frank, Walter; Reiß, Guido J.; Acta Crystallographica Section C 53 (1997) 1018–1020; doi:10.1107/S0108270197004393

data_2006397
_publ_contact_author
;
      Walter Frank
      Fachbereich Chemie
      Universit\"at Kaiserslautern
      Erwin-Schr\"odinger-Stra\&se
      67663 Kaiserslautern
      Germany
;
_publ_section_title
;Photochemical Reactions of Transition Metal Organyl Complexes with Olefins.
 18.
 Dicarbonylbis(\h^5^-cyclopentadienyl)(\m-1,4-\h:4,5-\h-1,4-pentadien-1,4-diyl)oxoditungsten(<i>W</i>---<i>W</i>)
;
_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(\h^5^-cyclopentadienyl)-(\m-1,4-\h:4,5-\h-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       '\w/\q 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/[\s^2^(Fo^2^)+(0.0402P)^2^+3.8P] where P=(Fo^2^+2Fc^2^)/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