Efficient Demetalation of Fischer Alkoxy- and Amino-Biscarbene Complexes of Chromium via CO-Promoted Sulfuration and Selenylation
Zheng,; Chen, Jinzhu; Luo, Ning; Yu,; Han, Xiuwen; Organometallics 25 (2006) 5301–; doi:10.1021/om060288m

data_4075448
_publ_section_title
;
 Efficient Demetalation of Fischer Alkoxy- and Amino-Biscarbene Complexes
 of Chromium via CO-Promoted Sulfuration and Selenylation
;
_journal_issue                   22
_journal_name_full               Organometallics
_journal_page_first              5301
_journal_paper_doi               10.1021/om060288m
_journal_volume                  25
_journal_year                    2006
_chemical_formula_sum            'C14 H6 Cr O6 S'
_chemical_formula_weight         354.25
_chemical_name_systematic
; 
 ? 
;
_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                95.864(2)
_cell_angle_beta                 100.443(2)
_cell_angle_gamma                101.288(2)
_cell_formula_units_Z            2
_cell_length_a                   6.9915(8)
_cell_length_b                   9.2960(10)
_cell_length_c                   11.6505(12)
_cell_measurement_reflns_used    2502
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      56.075
_cell_measurement_theta_min      4.514
_cell_volume                     722.78(14)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0483
_diffrn_reflns_av_sigmaI/netI    0.0434
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            4272
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         1.80
_exptl_absorpt_coefficient_mu    0.961
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76110
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.628
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             356
_exptl_crystal_size_max          0.489
_exptl_crystal_size_mid          0.457
_exptl_crystal_size_min          0.301
_refine_diff_density_max         0.294
_refine_diff_density_min         -0.364
_refine_diff_density_rms         0.065
_refine_ls_extinction_coef       0.084(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     200
_refine_ls_number_reflns         3056
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0392
_refine_ls_R_factor_gt           0.0343
_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^)+(0.0527P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0943
_refine_ls_wR_factor_ref         0.0970
_reflns_number_gt                2602
_reflns_number_total             3056
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om060288msi20060822_072948.cif
_cod_data_source_block           cd26291_for_complex_21
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4075448