Steric and Electronic Effects of Metal-Containing Substituents in Fischer Carbene Complexes of Chromium
Bezuidenhout, Daniela I.; van der Watt, Elisia; Liles, David C.; Landman, Marilé; Lotz, Simon; Organometallics 27 (2008) 2447–; doi:10.1021/om8001735

data_4071449
_publ_section_title
;
 Steric and Electronic Effects of Metal-Containing Substituents in Fischer
 Carbene Complexes of Chromium
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              2447
_journal_paper_doi               10.1021/om8001735
_journal_volume                  27
_journal_year                    2008
_chemical_formula_moiety         'C27 H15 Cl Cr2 O9 S Ti, C H2 Cl2'
_chemical_formula_sum            'C28 H17 Cl3 Cr2 O9 S Ti'
_chemical_formula_weight         787.73
_chemical_name_systematic
; 
((Chloro-bis(\h^5^-pentadienyl)-titanium-oxy)-(\h^6^-tricarbonylchromium-
benzo[b]thien-2-yl)-methylidene)-(pentacarbonyl)-chromium dichloromethane 
solvate 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 101.009(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.260(2)
_cell_length_b                   12.083(2)
_cell_length_c                   23.804(4)
_cell_measurement_reflns_used    4753
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.357
_cell_measurement_theta_min      2.425
_cell_volume                     3179.0(9)
_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 (The POV-Ray Team, 2004)'
_computing_publication_material  SHELXL-97
_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 0.998
_diffrn_measured_fraction_theta_max 0.914
_diffrn_measurement_device_type  'Bruker (Seimens) 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  0.0501
_diffrn_reflns_av_sigmaI/netI    0.0581
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            17002
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.54
_diffrn_reflns_theta_min         2.42
_exptl_absorpt_coefficient_mu    1.285
_exptl_absorpt_correction_T_max  0.981
_exptl_absorpt_correction_T_min  0.690
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2001)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.646
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blade
_exptl_crystal_F_000             1576
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.015
_refine_diff_density_max         0.676
_refine_diff_density_min         -0.645
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     447
_refine_ls_number_reflns         6045
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0946
_refine_ls_R_factor_gt           0.0525
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0815P)^2^+2.1850P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1355
_refine_ls_wR_factor_ref         0.1623
_reflns_number_gt                3866
_reflns_number_total             6045
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om8001735-file005.cif
_cod_data_source_block           evdw02_abs
_cod_original_cell_volume        3178.9(10)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4071449