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_4071448
_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         'C19 H10 Cr2 O9 S'
_chemical_formula_sum            'C19 H10 Cr2 O9 S'
_chemical_formula_weight         518.33
_chemical_name_systematic
; 
 (Ethoxy-(\h^6^-tricarbonylchromium-benzo[b]thien-2-yl)-methylidene)-
(pentacarbonyl)-chromium 
;
_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                109.519(2)
_cell_angle_beta                 108.371(2)
_cell_angle_gamma                95.519(2)
_cell_formula_units_Z            2
_cell_length_a                   8.3523(11)
_cell_length_b                   10.7547(15)
_cell_length_c                   13.0118(17)
_cell_measurement_reflns_used    4002
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.506
_cell_measurement_theta_min      2.581
_cell_volume                     1018.6(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 0.977
_diffrn_measured_fraction_theta_max 0.876
_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  0.0212
_diffrn_reflns_av_sigmaI/netI    0.0353
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            5597
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.53
_diffrn_reflns_theta_min         2.58
_exptl_absorpt_coefficient_mu    1.219
_exptl_absorpt_correction_T_max  0.941
_exptl_absorpt_correction_T_min  0.795
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2001)'
_exptl_crystal_colour            dark-purple
_exptl_crystal_density_diffrn    1.690
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rectangular-plate
_exptl_crystal_F_000             520
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.408
_refine_diff_density_min         -0.355
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         3714
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0411
_refine_ls_R_factor_gt           0.0370
_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^)+(0.0612P)^2^+0.2800P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0992
_refine_ls_wR_factor_ref         0.1040
_reflns_number_gt                3317
_reflns_number_total             3714
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om8001735-file004.cif
_cod_data_source_block           evdw10_abs
_cod_database_code               4071448