Structural and Spectroscopic Studies of 16-Electron, Unsaturated Derivatives of Low-Valent, Group 6 Carbonyl Complexes Containing π-Donor Ligands
Donald J. Darensbourg; Jennifer D. Draper; Brian J. Frost; Joseph H. Reibenspies; Inorganic Chemistry 38 (1999) 4705–4714; doi:10.1021/ic9804216

data_4322297
_publ_section_title
;
 Structural and Spectroscopic Studies of 16-Electron, Unsaturated
 Derivatives of Low-Valent, Group 6 Carbonyl Complexes Containing \p-Donor
 Ligands
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4705
_journal_page_last               4714
_journal_paper_doi               10.1021/ic9804216
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C82 H64 N2 O4 P4 S2 W'
_chemical_formula_weight         1513.20
_chemical_name_systematic
; 

 ? 

;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                77.182(7)
_cell_angle_beta                 78.334(7)
_cell_angle_gamma                66.579(7)
_cell_formula_units_Z            2
_cell_length_a                   12.6497(10)
_cell_length_b                   14.8095(13)
_cell_length_c                   21.053(2)
_cell_measurement_temperature    193(2)
_cell_volume                     3500.1(6)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0242
_diffrn_reflns_av_sigmaI/netI    0.0499
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            12863
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.77
_exptl_absorpt_coefficient_mu    1.855
_exptl_crystal_density_diffrn    1.436
_exptl_crystal_F_000             1536
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.637
_refine_diff_density_min         -0.547
_refine_diff_density_rms         0.076
_refine_ls_extinction_coef       0.00000(10)
_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   1.070
_refine_ls_goodness_of_fit_obs   1.055
_refine_ls_matrix_type           full
_refine_ls_number_parameters     857
_refine_ls_number_reflns         12257
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_restrained_S_obs      1.055
_refine_ls_R_factor_all          0.0459
_refine_ls_R_factor_obs          0.0346
_refine_ls_shift/esd_max         -0.955
_refine_ls_shift/esd_mean        0.019
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0329P)^2^+2.6773P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0903
_refine_ls_wR_factor_obs         0.0819
_reflns_number_observed          10506
_reflns_number_total             12257
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9804216_04.cif
_cod_data_source_block           dd331
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0329P)^2^+2.6773P] 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^)+(0.0329P)^2^+2.6773P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3500.0(5)
_cod_database_code               4322297