Efficient Demetalation of Fischer Alkoxy- and Amino-Biscarbene Complexes of Chromium via CO-Promoted Sulfuration and Selenylation
Zheng, Zhaoyan; Chen, Jinzhu; Luo, Ning; Yu, Zhengkun; Han, Xiuwen; Organometallics 25 (2006) 5301–5310; doi:10.1021/om060288m

data_4075446
_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_page_last               5310
_journal_paper_doi               10.1021/om060288m
_journal_volume                  25
_journal_year                    2006
_chemical_formula_sum            'C28 H29 N O3 Se2'
_chemical_formula_weight         585.44
_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                107.768(2)
_cell_angle_beta                 103.307(2)
_cell_angle_gamma                100.490(2)
_cell_formula_units_Z            2
_cell_length_a                   9.8424(12)
_cell_length_b                   10.0858(13)
_cell_length_c                   14.5902(18)
_cell_measurement_reflns_used    2255
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      53.975
_cell_measurement_theta_min      5.325
_cell_volume                     1291.5(3)
_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  0.0652
_diffrn_reflns_av_sigmaI/netI    0.0849
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            7635
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         2.18
_exptl_absorpt_coefficient_mu    2.892
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.47562
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.505
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             592
_exptl_crystal_size_max          0.516
_exptl_crystal_size_mid          0.455
_exptl_crystal_size_min          0.347
_refine_diff_density_max         0.789
_refine_diff_density_min         -0.736
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.862
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     310
_refine_ls_number_reflns         5477
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.862
_refine_ls_R_factor_all          0.0824
_refine_ls_R_factor_gt           0.0513
_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^)+(0.0642P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1194
_refine_ls_wR_factor_ref         0.1285
_reflns_number_gt                3226
_reflns_number_total             5477
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om060288msi20060822_072948.cif
_cod_data_source_block           cd25249_for_compound_6b
_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               4075446