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_4322298
_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            'C84 H68 Cr N3 O5 P4 S'
_chemical_formula_weight         1407.35
_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                104.84(3)
_cell_angle_beta                 106.91(3)
_cell_angle_gamma                95.29(3)
_cell_formula_units_Z            2
_cell_length_a                   13.869(3)
_cell_length_b                   23.128(5)
_cell_length_c                   12.056(2)
_cell_measurement_temperature    193(2)
_cell_volume                     3517.9(16)
_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  0.0978
_diffrn_reflns_av_sigmaI/netI    0.2109
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            9636
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         1.56
_exptl_absorpt_coefficient_mu    0.340
_exptl_crystal_density_diffrn    1.329
_exptl_crystal_F_000             1466
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.637
_refine_diff_density_min         -0.844
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.003
_refine_ls_goodness_of_fit_obs   1.159
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     883
_refine_ls_number_reflns         9151
_refine_ls_number_restraints     272
_refine_ls_restrained_S_all      0.997
_refine_ls_restrained_S_obs      1.127
_refine_ls_R_factor_all          0.2001
_refine_ls_R_factor_obs          0.0815
_refine_ls_shift/esd_max         0.302
_refine_ls_shift/esd_mean        0.014
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1146P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2404
_refine_ls_wR_factor_obs         0.1878
_reflns_number_observed          4641
_reflns_number_total             9174
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9804216_05.cif
_cod_data_source_block           dd332
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1146P)^2^+0.0000P] 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^)+(0.1146P)^2^+0.0000P] 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        3517.5(12)
_cod_database_code               4322298