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_4075445
_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            'C33 H29 Cr N O8 Se'
_chemical_formula_weight         698.53
_chemical_name_systematic        ?
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 107.215(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.045(4)
_cell_length_b                   23.888(10)
_cell_length_c                   12.305(5)
_cell_measurement_reflns_used    604
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.393
_cell_measurement_theta_min      4.358
_cell_volume                     3101(2)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.1634
_diffrn_reflns_av_sigmaI/netI    0.3018
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            15876
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         1.93
_exptl_absorpt_coefficient_mu    1.595
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86289
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.496
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1424
_exptl_crystal_size_max          0.176
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.047
_refine_diff_density_max         0.264
_refine_diff_density_min         -0.376
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.844
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     400
_refine_ls_number_reflns         5774
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.844
_refine_ls_R_factor_all          0.2042
_refine_ls_R_factor_gt           0.0499
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; calc 
 [0.00000+1.00000exp(3.00(sin\q/\l)^2^)]/ 
   [\s^2^(Fo^2^)+0.0000+0.0000*P+(0.0000P)^2^+0.0000sin\q/\l] 
 where P = 0.33333Fo^2^ + 0.66667Fc^2^ 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0674
_refine_ls_wR_factor_ref         0.1129
_reflns_number_gt                1762
_reflns_number_total             5774
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om060288msi20060822_072948.cif
_cod_data_source_block           cd25262_for_complex_5b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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      P2(1)/n
_cod_database_code               4075445