Trindenyl Trimolybdenum and Tritungsten Complexes: Crystal Structure of (trindenyl)[(OC)3W‒W(CO)3]W(CO)3Bn
Lynch, Thomas J.; Carroll, James M.; Helvenston, Merritt C.; Tisch, Theodore L.; Rheingold, Arnold L.; Staley, Donna L.; Mahmoudkhani, Amir; Organometallics 31 (2012) 3300–; doi:10.1021/om3001263

data_4078113
_publ_section_title
;
 Trindenyl Trimolybdenum and Tritungsten Complexes: Crystal Structure of
 (trindenyl)[(OC)3W--W(CO)3]W(CO)3Bn
;
_journal_issue                   8
_journal_name_full               Organometallics
_journal_page_first              3300
_journal_paper_doi               10.1021/om3001263
_journal_volume                  31
_journal_year                    2012
_chemical_formula_sum            'C31 H16 O9 W3'
_chemical_formula_weight         1083.99
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           33
_symmetry_space_group_name_Hall  'P -2ac -2n'
_symmetry_space_group_name_H-M   'P n 21 a'
_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                   29.188(8)
_cell_length_b                   10.387(3)
_cell_length_c                   9.599(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      20
_cell_volume                     2910.2(15)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.846
_diffrn_measured_fraction_theta_max 0.846
_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    0.0954
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2045
_diffrn_reflns_theta_full        24.00
_diffrn_reflns_theta_max         24.00
_diffrn_reflns_theta_min         2.23
_exptl_absorpt_coefficient_mu    11.884
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.474
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1984
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.297
_refine_diff_density_min         -1.248
_refine_diff_density_rms         0.251
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.742
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     188
_refine_ls_number_reflns         2045
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.742
_refine_ls_R_factor_all          0.0393
_refine_ls_R_factor_gt           0.0393
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1132
_refine_ls_wR_factor_ref         0.1132
_reflns_number_gt                2045
_reflns_number_total             2045
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om3001263_si_002.cif
_cod_data_source_block           Td[(OC)3W-W(CO)3][W(CO)3Bn]
_cod_original_sg_symbol_H-M      Pn21a
_cod_database_code               4078113