Fischer Dinuclear and Mononuclear Bis-Carbene Complexes of Thiophene and Thiophene Derivatives
Lotz, Simon; van Jaarsveld, Nina A.; Liles, David C.; Crause, Chantelle; Görls, Helmar; Terblans, Yvette M.; Organometallics 31 (2012) 5371–; doi:10.1021/om300414y

data_4078776
_publ_section_title
;
 Fischer Dinuclear and Mononuclear Bis-Carbene Complexes of Thiophene and
 Thiophene Derivatives
;
_journal_issue                   15
_journal_name_full               Organometallics
_journal_page_first              5371
_journal_paper_doi               10.1021/om300414y
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C18 H14 Cr O6 S'
_chemical_formula_sum            'C18 H14 Cr O6 S'
_chemical_formula_weight         410.35
_chemical_name_systematic
; 
[2,3-Di(ethoxymethylidenyl)-benzothiophene](tetracarbonyl)
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                 103.1890(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.2106(5)
_cell_length_b                   26.1162(16)
_cell_length_c                   9.9037(6)
_cell_measurement_reflns_used    8613
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.28
_cell_measurement_theta_min      3.12
_cell_volume                     1815.8(2)
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        SAINT
_computing_molecular_graphics
' ORTEP-3 for Windows (Farrugia, 1997), POV-Ray (Cason, 2004)'
_computing_publication_material  ' SHELXL-97 and PLATON (Spek, 2009) '
_computing_structure_refinement
'SHELXTL (Bruker, 2001) and SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTS (Bruker, 2001)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_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  0.0361
_diffrn_reflns_av_sigmaI/netI    0.0229
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            28769
_diffrn_reflns_theta_full        28.42
_diffrn_reflns_theta_max         28.42
_diffrn_reflns_theta_min         1.56
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.776
_exptl_absorpt_correction_T_max  0.947
_exptl_absorpt_correction_T_min  0.851
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2005)'
_exptl_crystal_colour            red-orange
_exptl_crystal_density_diffrn    1.501
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             840
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.337
_refine_diff_density_min         -0.295
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     237
_refine_ls_number_reflns         4549
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0324
_refine_ls_R_factor_gt           0.0274
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0381P)^2^+0.5268P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0727
_refine_ls_wR_factor_ref         0.0751
_reflns_number_gt                4013
_reflns_number_total             4549
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om300414y_si_002.cif
_cod_data_source_block           complex_7a_nina0666
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4078776