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_4322294
_publ_section_title
;
 Structural and Spectroscopic Studies of 16-Electron, Unsaturated
 Derivatives of Low-Valent, Group 6 Carbonyl Complexes Containing \p-Donor
 Ligands
;
_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            'C85 H70 N4 O4 P4 S W'
_chemical_formula_weight         1551.24
_chemical_name_systematic
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;
_space_group_IT_number           2
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_symmetry_space_group_name_Hall  '-P 1'
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_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                76.441(13)
_cell_angle_beta                 75.981(15)
_cell_angle_gamma                70.978(12)
_cell_formula_units_Z            2
_cell_length_a                   12.236(2)
_cell_length_b                   14.419(2)
_cell_length_c                   22.748(4)
_cell_measurement_temperature    193(2)
_cell_volume                     3628.0(11)
_computing_cell_refinement       'XSCANS (SIEMENS, 1995)'
_computing_data_collection       'XSCANS (SIEMENS, 1995)'
_computing_molecular_graphics    'XP (SIEMENS, 1990)'
_computing_publication_material  'CIFTAB (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoKa
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0996
_diffrn_reflns_av_sigmaI/netI    0.1651
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -3
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            13395
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.16
_diffrn_standards_decay_%        <<1
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.764
_exptl_absorpt_correction_T_max  0.5973
_exptl_absorpt_correction_T_min  0.4614
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.420
_exptl_crystal_description       plate
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_refine_diff_density_max         1.454
_refine_diff_density_min         -1.480
_refine_diff_density_rms         0.156
_refine_ls_extinction_method     none
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_refine_ls_goodness_of_fit_obs   1.057
_refine_ls_hydrogen_treatment    riding
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_refine_ls_number_parameters     862
_refine_ls_number_reflns         12730
_refine_ls_number_restraints     0
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_refine_ls_restrained_S_obs      1.057
_refine_ls_R_factor_all          0.1336
_refine_ls_R_factor_obs          0.0713
_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^)+( 0.0548P)^2^+2.5714P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1672
_refine_ls_wR_factor_obs         0.1357
_reflns_number_observed          8130
_reflns_number_total             12743
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9804216_01.cif
_cod_data_source_block           dd265
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w=1/[s^2^(Fo^2^)+(
0.0548P)^2^+2.5714P] 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^)+( 0.0548P)^2^+2.5714P] 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        3628.0(10)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4322294