Synthesis and Characterization of a Stable trans-Dioxo Tungsten(IV) Complex and Series of Mono-Oxo Molybdenum(IV) and Tungsten(IV) Complexes. Structural and Electronic Effects of π-Bonding in trans-[M(O)(X)(dppe)2]+/0 Systems
Jesper Bendix; Anders Bøgevig; Inorganic Chemistry 37 (1998) 5992–6001; doi:10.1021/ic980342u

data_4323157
_publ_section_title
;
 Synthesis and Characterization of a Stable trans-Dioxo Tungsten(IV)
 Complex and Series of Mono-Oxo Molybdenum(IV) and Tungsten(IV) Complexes.
 Structural and Electronic Effects of \p-Bonding in
 trans-[M(O)(X)(dppe)2]+/0 Systems
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5992
_journal_page_last               6001
_journal_paper_doi               10.1021/ic980342u
_journal_volume                  37
_journal_year                    1998
_chemical_formula_sum            'C52 H48 B F5 O P4 W'
_chemical_formula_weight         1102.44
_chemical_name_systematic
; 
trans-fluorooxo-bis(diphenylphosphinoethane)tungsten(IV)tetrafluoroborate.
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
98-03-15   edited for submission to Inorg. Chem. These data pertains to the 
compound labeled 10 in the manuscript.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 92.522(17)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.814(5)
_cell_length_b                   22.472(3)
_cell_length_c                   21.1029(17)
_cell_measurement_temperature    122(2)
_cell_volume                     4650(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      122(2)
_diffrn_measured_fraction_theta_full 0.500
_diffrn_measured_fraction_theta_max 0.500
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0431
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            9928
_diffrn_reflns_theta_full        33.96
_diffrn_reflns_theta_max         33.96
_diffrn_reflns_theta_min         1.81
_exptl_absorpt_coefficient_mu    2.681
_exptl_crystal_density_diffrn    1.575
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2208
_refine_diff_density_max         0.888
_refine_diff_density_min         -1.430
_refine_diff_density_rms         0.111
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.554(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.178
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     607
_refine_ls_number_reflns         9928
_refine_ls_number_restraints     65
_refine_ls_restrained_S_all      1.177
_refine_ls_R_factor_all          0.0343
_refine_ls_R_factor_gt           0.0306
_refine_ls_shift/su_max          0.076
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+4.1573P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0620
_refine_ls_wR_factor_ref         0.0636
_reflns_number_gt                9473
_reflns_number_total             9928
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic980342u_2.cif
_cod_data_source_block           fh460
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+4.1573P] 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^)+(0.0000P)^2^+4.1573P] 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        4649(2)
_cod_database_code               4323157