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_4323158
_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 H49 Cl O6 P4 W'
_chemical_formula_weight         1113.09
_chemical_name_systematic
; 
trans-hydroxooxo-bis(diphenylphosphinoethane)tungsten(IV)perchlorate.
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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 12 in the manuscript.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 102.256(18)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.864(3)
_cell_length_b                   16.639(4)
_cell_length_c                   17.114(4)
_cell_measurement_temperature    122(2)
_cell_volume                     4692.7(18)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      122(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_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    0.0346
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            17389
_diffrn_reflns_theta_full        32.96
_diffrn_reflns_theta_max         32.96
_diffrn_reflns_theta_min         1.73
_exptl_absorpt_coefficient_mu    2.706
_exptl_crystal_density_diffrn    1.576
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2240
_refine_diff_density_max         1.746
_refine_diff_density_min         -2.335
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     581
_refine_ls_number_reflns         17389
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0358
_refine_ls_R_factor_gt           0.0278
_refine_ls_shift/su_max          0.656
_refine_ls_shift/su_mean         0.011
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0147P)^2^+4.6308P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0587
_refine_ls_wR_factor_ref         0.0622
_reflns_number_gt                15295
_reflns_number_total             17389
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic980342u_3.cif
_cod_data_source_block           fh465
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0147P)^2^+4.6308P] 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^)+(0.0147P)^2^+4.6308P] 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        4692.5(18)
_cod_database_code               4323158