Multimetal Fischer carbene complexes of Group VI transition metals: synthesis, structure and substituent effect investigation.
Bezuidenhout, Daniela I.; Barnard, Werner; van der Westhuizen, Belinda; van der Watt, Elisia; Liles, David C.; Dalton transactions (Cambridge, England : 2003) 40 (2011) 6711–6721; doi:10.1039/c1dt10183h

data_7016080
_publ_section_title
;
 Multimetal Fischer carbene complexes of Group VI transition metals:
 synthesis, structure and substituent effect investigation.
;
_journal_issue                   25
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6711
_journal_page_last               6721
_journal_paper_doi               10.1039/c1dt10183h
_journal_volume                  40
_journal_year                    2011
_chemical_formula_moiety         'C24 H15 Cl O6 S Ti W, C H2 Cl2'
_chemical_formula_sum            'C25 H17 Cl3 O6 S Ti W'
_chemical_formula_weight         783.55
_chemical_name_common
;
((Chloro-bis(eta$5!-pentadienyl)-titanium-oxy)-(benzo(b)thien-
2-yl)-methylidene) -(pentacarbonyl)-tungsten dichloromethane solvate
;
_chemical_name_systematic
;
((Chloro-bis(\h^5^-pentadienyl)-titanium-oxy)-(benzo[b]thien-2-yl)-methylidene)
-(pentacarbonyl)-tungsten dichloromethane solvate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                66.392(1)
_cell_angle_beta                 88.689(1)
_cell_angle_gamma                66.317(1)
_cell_formula_units_Z            2
_cell_length_a                   11.3533(6)
_cell_length_b                   11.6696(6)
_cell_length_c                   12.3627(7)
_cell_measurement_reflns_used    6906
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.570
_cell_measurement_theta_min      2.908
_cell_volume                     1355.73(13)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        SAINT
_computing_molecular_graphics
' ORTEP-3 for Windows (Farrugia, 1997), POV-Ray (Cason, 2004)'
_computing_structure_refinement  'SHELXTL and SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXTL (Bruker, 2001)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'SMART 1000 CCD'
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.865
_diffrn_measurement_device_type  'Bruker (Siemens) P4'
_diffrn_measurement_method       '\f and \w 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  0.0165
_diffrn_reflns_av_sigmaI/netI    0.0270
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            7350
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.57
_diffrn_reflns_theta_min         2.46
_exptl_absorpt_coefficient_mu    4.945
_exptl_absorpt_correction_T_max  0.276
_exptl_absorpt_correction_T_min  0.212
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2001)'
_exptl_crystal_colour            dark-red
_exptl_crystal_density_diffrn    1.919
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rectangular-prism
_exptl_crystal_F_000             756
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.26
_refine_diff_density_max         1.311
_refine_diff_density_min         -1.015
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         4908
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0270
_refine_ls_R_factor_gt           0.0264
_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^)+(0.0472P)^2^+1.0141P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0704
_refine_ls_wR_factor_ref         0.0709
_reflns_number_gt                4739
_reflns_number_total             4908
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c1dt10183h.txt
_cod_data_source_block           EvdW09_Complex_2b
_cod_database_code               7016080