Electronically-Coupled Tungsten-Tungsten Quadruple Bonds: Comparisons of Electron Delocalization in 3,6-Dioxypyridazine and Oxalate-Bridged Compounds
Malcolm H. Chisholm; Robin J. H. Clark; Judith Gallucci; Christopher M. Hadad; Nathan J. Patmore; Journal of the American Chemical Society 126 (2004) 8303–8313; doi:10.1021/ja048768x

data_4112735
_publ_section_title
;
 Electronically-Coupled Tungsten-Tungsten Quadruple Bonds: Comparisons of
 Electron Delocalization in 3,6-Dioxypyridazine and Oxalate-Bridged
 Compounds
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8303
_journal_page_last               8313
_journal_paper_doi               10.1021/ja048768x
_journal_volume                  126
_journal_year                    2004
_chemical_formula_sum            'C50 H88 F6 N2 O18 P W4'
_chemical_formula_weight         1885.59
_chemical_name_systematic
;
 ?
;
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_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 109.895(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   19.915(1)
_cell_length_b                   34.809(2)
_cell_length_c                   20.334(1)
_cell_measurement_temperature    200(2)
_cell_volume                     13254.7(12)
_computing_cell_refinement       'DENZO (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1999)'
_computing_data_reduction        'DENZO (Otwinowski & Minor, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       'phi and omega scans'
_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  0.058
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_k_min       -45
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            224111
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.05
_exptl_absorpt_coefficient_mu    7.024
_exptl_absorpt_correction_type   empirical
_exptl_crystal_density_diffrn    1.890
_exptl_crystal_description       chunk
_exptl_crystal_F_000             7288
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.19
_refine_diff_density_max         2.021
_refine_diff_density_min         -1.156
_refine_diff_density_rms         0.152
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1312
_refine_ls_number_reflns         30374
_refine_ls_number_restraints     106
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0995
_refine_ls_R_factor_gt           0.0443
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0562P)^2^+20.8700P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1085
_refine_ls_wR_factor_ref         0.1279
_reflns_number_gt                16834
_reflns_number_total             30374
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja048768xsi20040303_023916.cif
_cod_data_source_block           I+PF6-
_cod_database_code               4112735