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_4071450
_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         'C32 H18 Cr2 Fe O12 Ti'
_chemical_formula_sum            'C32 H18 Cr2 Fe O12 Ti'
_chemical_formula_weight         802.21
_chemical_name_systematic
; 
 (\m~2~-(ferrocen-1,1'-diyl)-(bis(\h^5^-cyclopentadienyl)-dioxy-titanium-
O,O')-dimethylidene-C,C')-bis(pentacarbonyl-chromium)
;
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 101.7230(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.9813(4)
_cell_length_b                   15.8650(7)
_cell_length_c                   20.1457(9)
_cell_measurement_reflns_used    9597
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.458
_cell_measurement_theta_min      2.431
_cell_volume                     3123.6(2)
_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 0.916
_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  0.0290
_diffrn_reflns_av_sigmaI/netI    0.0296
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            16699
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.53
_diffrn_reflns_theta_min         2.43
_exptl_absorpt_coefficient_mu    1.444
_exptl_absorpt_correction_T_max  0.841
_exptl_absorpt_correction_T_min  0.725
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2001)'
_exptl_crystal_colour            dark-brown
_exptl_crystal_density_diffrn    1.706
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       square-prism
_exptl_crystal_F_000             1608
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.407
_refine_diff_density_min         -0.286
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         5958
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0409
_refine_ls_R_factor_gt           0.0314
_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^)+(0.0462P)^2^+1.0764P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0825
_refine_ls_wR_factor_ref         0.0911
_reflns_number_gt                4975
_reflns_number_total             5958
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om8001735-file006.cif
_cod_data_source_block           db52a3n_abs
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4071450