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_4323156
_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            'C54 H56 O4 P4 W'
_chemical_formula_weight         1076.72
_chemical_name_systematic
; 
trans-dioxo-bis(diphenylphosphinoethane)tungsten(IV) dimethanol solvate.
;
_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-97
_audit_update_record
;
98-03-15   edited for submission to Inorg. Chem. These data pertains to the 
compound labeled 11 in the manuscript.
;
_cell_angle_alpha                110.864(19)
_cell_angle_beta                 99.05(2)
_cell_angle_gamma                110.244(19)
_cell_formula_units_Z            1
_cell_length_a                   9.464(2)
_cell_length_b                   11.429(2)
_cell_length_c                   13.126(3)
_cell_measurement_temperature    122(2)
_cell_volume                     1179.3(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      122(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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    0.0295
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6857
_diffrn_reflns_theta_full        29.97
_diffrn_reflns_theta_max         29.97
_diffrn_reflns_theta_min         1.75
_exptl_absorpt_coefficient_mu    2.631
_exptl_crystal_density_diffrn    1.516
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             546
_refine_diff_density_max         0.851
_refine_diff_density_min         -1.117
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     398
_refine_ls_number_reflns         6857
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0174
_refine_ls_R_factor_gt           0.0173
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0195P)^2^+0.2698P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0433
_refine_ls_wR_factor_ref         0.0434
_reflns_number_gt                6845
_reflns_number_total             6857
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic980342u_1.cif
_cod_data_source_block           fh454_abs
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0195P)^2^+0.2698P] 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^)+(0.0195P)^2^+0.2698P] 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        1179.4(5)
_cod_database_code               4323156