Synthesis of New Selenium- and Oxygen-Containing Tungsten Acetylide Complexes [(η5-C5Me5)W(O)(Se2)(CCPh)] and [(η5-C5Me5)W(Se5CCPh)]
Mathur, Pradeep; Ahmed, Moawia O.; Dash, Aswini K.; Kaldis, John H.; Organometallics 19 (2000) 941–; doi:10.1021/om990775k

data_4077676
_publ_section_title
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 Synthesis of New Selenium- and Oxygen-Containing Tungsten Acetylide
 Complexes [(\h5-C5Me5)W(O)(Se2)(CCPh)] and [(\h5-C5Me5)W(Se5CCPh)]
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_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              941
_journal_paper_doi               10.1021/om990775k
_journal_volume                  19
_journal_year                    2000
_chemical_formula_sum            'C18 H20 O Se2 W'
_chemical_formula_weight         594.11
_chemical_name_systematic
; 
 ? 
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_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 92.1210(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.6251(3)
_cell_length_b                   14.4492(4)
_cell_length_c                   13.3573(5)
_cell_measurement_reflns_used    4267
_cell_measurement_temperature    299(2)
_cell_measurement_theta_max      27.55
_cell_measurement_theta_min      2.08
_cell_volume                     1856.39(10)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-V.5.03 (Sheldrick, 1994)'
_computing_structure_solution    'SHELXTL-V.5.03 (Sheldrick, 1994)'
_diffrn_ambient_temperature      299(2)
_diffrn_measurement_device       'Siemems Smart CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0404
_diffrn_reflns_av_sigmaI/netI    0.0399
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            16888
_diffrn_reflns_theta_max         27.55
_diffrn_reflns_theta_min         2.08
_exptl_absorpt_coefficient_mu    10.143
_exptl_absorpt_correction_T_max  0.261696
_exptl_absorpt_correction_T_min  0.137627
_exptl_absorpt_correction_type   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    2.126
_exptl_crystal_description       plate
_exptl_crystal_F_000             1112
_exptl_crystal_size_max          .32
_exptl_crystal_size_mid          .16
_exptl_crystal_size_min          .08
_refine_diff_density_max         0.911
_refine_diff_density_min         -0.753
_refine_diff_density_rms         0.103
_refine_ls_extinction_coef       0.00122(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.009
_refine_ls_goodness_of_fit_obs   1.093
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     200
_refine_ls_number_reflns         4267
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.009
_refine_ls_restrained_S_obs      1.093
_refine_ls_R_factor_all          0.0609
_refine_ls_R_factor_obs          0.0338
_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/[\s^2^(Fo^2^)+(0.0372P)^2^+1.1499P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0815
_refine_ls_wR_factor_obs         0.0733
_reflns_number_observed          2999
_reflns_number_total             4267
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            om990775k.cif
_cod_data_source_block           compound_1
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_hydrogen_treatment' value 'no ref' changed to 'noref'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0372P)^2^+1.1499P] 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^)+(0.0372P)^2^+1.1499P] 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      P2(1)/n
_cod_database_code               4077676