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_4112734
_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            'C77 H94 N2 O14 P2 W4'
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_symmetry_cell_setting           monoclinic
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_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 107.295(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.790(1)
_cell_length_b                   17.993(1)
_cell_length_c                   19.885(1)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      18
_cell_measurement_theta_min      12
_cell_volume                     4027.6(5)
_computing_cell_refinement       'DENZO (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1999)'
_computing_data_reduction        'DENZO (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'ORTEX (P.McArdle, 1995)'
_computing_publication_material  'SHELXL-97/2 (Sheldrick,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  0.062
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            69012
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.13
_exptl_absorpt_coefficient_mu    5.793
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            Blue
_exptl_crystal_density_diffrn    1.706
_exptl_crystal_description       'triangular plate'
_exptl_crystal_F_000             2016
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.316
_refine_diff_density_min         -0.725
_refine_diff_density_rms         0.104
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.016(5)
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
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_refine_ls_number_reflns         18469
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_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0355
_refine_ls_R_factor_gt           0.0286
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0344P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
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_refine_ls_wR_factor_ref         0.0614
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_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja048768xsi20040303_023854.cif
_cod_data_source_block           I(PPh3)2
_cod_original_cell_volume        4027.6(4)
_cod_database_code               4112734