Synthesis, Structures, Bonding, and Redox Chemistry of Ditungsten Butadiyne Complexes with W\τbC-C\τbW Backbones
Jibin Sun; Sarah E. Shaner; Marya K. Jones; Daniel C. O'Hanlon; Jeffrey S. Mugridge; Michael D. Hopkins; Inorganic Chemistry 49 (2010) 1687–1698; doi:10.1021/ic902088x

data_4314813
_publ_section_title
;
 Synthesis, Structures, Bonding, and Redox Chemistry of Ditungsten
 Butadiyne Complexes with W\\tbC-C\\tbW Backbones
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1687
_journal_page_last               1698
_journal_paper_doi               10.1021/ic902088x
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'C35 H0 Cl4 O39 P16 W4'
_chemical_formula_weight         2417.07
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           7
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P -2yc'
_symmetry_space_group_name_H-M   'P 1 c 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                 113.440(18)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.112(6)
_cell_length_b                   19.464(10)
_cell_length_c                   27.235(13)
_cell_measurement_temperature    100(2)
_cell_volume                     5404(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_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  0.0451
_diffrn_reflns_av_sigmaI/netI    0.0623
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            50350
_diffrn_reflns_theta_full        25.40
_diffrn_reflns_theta_max         25.40
_diffrn_reflns_theta_min         1.33
_exptl_absorpt_coefficient_mu    4.639
_exptl_crystal_density_diffrn    1.485
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2252
_refine_diff_density_max         7.433
_refine_diff_density_min         -3.961
_refine_diff_density_rms         0.371
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.51(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.126
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     566
_refine_ls_number_reflns         19249
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.126
_refine_ls_R_factor_all          0.1073
_refine_ls_R_factor_gt           0.0971
_refine_ls_shift/su_max          2.988
_refine_ls_shift/su_mean         0.082
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0625P)^2^+369.2311P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2375
_refine_ls_wR_factor_ref         0.2453
_reflns_number_gt                17008
_reflns_number_total             19249
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic902088x_si_002_2.cif
_cod_data_source_block           Cl(P(OMe)3)4WCCW(P(OMe)3)4Cl
_cod_database_code               4314813