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_4078780
_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         'C17 H15 Cr N O6 S'
_chemical_formula_sum            'C17 H15 Cr N O6 S'
_chemical_formula_weight         413.36
_chemical_name_systematic
; 
[2,3-Di(ethoxymethylidenyl)-4-methyl-4-<i>H</i>-thienopyrrole](tetracarbonyl)
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                85.341(3)
_cell_angle_beta                 89.251(3)
_cell_angle_gamma                83.935(3)
_cell_formula_units_Z            6
_cell_length_a                   7.2443(3)
_cell_length_b                   18.7946(9)
_cell_length_c                   20.0564(5)
_cell_measurement_reflns_used    12040
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      27.46
_cell_measurement_theta_min      1.02
_cell_volume                     2706.47(19)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'COLLECT (Nonius B.V. 1998)'
_computing_data_reduction
' HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics
' ORTEP-3 for Windows (Farrugia, 1997), POV-Ray (Cason, 2004)'
_computing_publication_material  ' SHELXL-97, PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      183(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Nonius Kappa 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  0.0780
_diffrn_reflns_av_sigmaI/netI    0.1245
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            23805
_diffrn_reflns_theta_full        25.24
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_min         1.02
_exptl_absorpt_coefficient_mu    0.783
_exptl_absorpt_correction_T_max  0.932
_exptl_absorpt_correction_T_min  0.914
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sortav (Blessing 1995)'
_exptl_crystal_colour            red-orange
_exptl_crystal_density_diffrn    1.522
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1272
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.748
_refine_diff_density_min         -0.527
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.856
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     706
_refine_ls_number_reflns         12040
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.856
_refine_ls_R_factor_all          0.0935
_refine_ls_R_factor_gt           0.0451
_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^)+(0.0321P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0930
_refine_ls_wR_factor_ref         0.1006
_reflns_number_gt                6344
_reflns_number_total             12040
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om300414y_si_002.cif
_cod_data_source_block           complex_10a_fo1430
_cod_original_cell_volume        2706.47(18)
_cod_database_code               4078780