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_4314812
_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            'C28.5 H69.25 Cl8 P8 W2'
_chemical_formula_weight         1311.15
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.733(3)
_cell_length_b                   16.348(3)
_cell_length_c                   19.759(4)
_cell_measurement_reflns_used    1024
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      1.62
_cell_volume                     5082.1(17)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(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  0.0460
_diffrn_reflns_av_sigmaI/netI    0.0405
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            49429
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.62
_exptl_absorpt_coefficient_mu    5.216
_exptl_absorpt_correction_T_max  0.7805
_exptl_absorpt_correction_T_min  0.2625
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
absorption corrections were made based on correspondance of
equivalent intensities usingprogram SADABS (G. Sheldrick, Bruker 
Analytical X-ray Systems, Madison, WI)
;
_exptl_crystal_density_diffrn    1.714
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2579
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.845
_refine_diff_density_min         -0.865
_refine_diff_density_rms         0.138
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.017(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     436
_refine_ls_number_reflns         8972
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0404
_refine_ls_R_factor_gt           0.0376
_refine_ls_shift/su_max          1.017
_refine_ls_shift/su_mean         0.096
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0488P)^2^+0.6378P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0862
_refine_ls_wR_factor_ref         0.0878
_reflns_number_gt                8496
_reflns_number_total             8972
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic902088x_si_002_1.cif
_cod_data_source_block           Cl(dmpe)2WCCW(dmpe)2Cl+3CH2Cl2
_cod_original_cell_volume        5082.2(16)
_cod_original_formula_sum        'C28.50 H69.25 Cl8 P8 W2'
_cod_database_code               4314812