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_4322296
_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            'C89 H76 N7 O3 P4 S W'
_chemical_formula_weight         1631.36
_chemical_name_systematic
; 

 ? 

;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 90.583(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.054(2)
_cell_length_b                   28.140(6)
_cell_length_c                   12.566(2)
_cell_measurement_temperature    293(2)
_cell_volume                     3908.6(13)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(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  0.0446
_diffrn_reflns_av_sigmaI/netI    0.0603
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7395
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.17
_exptl_absorpt_coefficient_mu    3.283
_exptl_crystal_density_diffrn    2.772
_exptl_crystal_F_000             3332
_refine_diff_density_max         1.235
_refine_diff_density_min         -0.664
_refine_diff_density_rms         0.092
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.012(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.051
_refine_ls_goodness_of_fit_obs   1.031
_refine_ls_matrix_type           full
_refine_ls_number_parameters     950
_refine_ls_number_reflns         7007
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.103
_refine_ls_restrained_S_obs      1.031
_refine_ls_R_factor_all          0.0471
_refine_ls_R_factor_obs          0.0362
_refine_ls_shift/esd_max         0.444
_refine_ls_shift/esd_mean        0.010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0443P)^2^+2.6884P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0975
_refine_ls_wR_factor_obs         0.0854
_reflns_number_observed          6288
_reflns_number_total             7017
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9804216_03.cif
_cod_data_source_block           dd319
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0443P)^2^+2.6884P] 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^)+(0.0443P)^2^+2.6884P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 

2020-09-02
Z value changed to be consistent with given formula
                 miguel
;
_cod_original_formula_units_Z            4
_cod_original_cell_volume        3908.6(12)
_cod_database_code               4322296