Chemoselective Stepwise Demetalation of Unusually Stable Fischer Biscarbene Complexes by Domino [4+2]/[2+2] Cycloaddition of 2-Isopropenyl-2-oxazoline to 1-Alkynyl Fischer Carbene Complexes of Chromium and Tungsten
Jinzhu Chen; Zhengkun Yu; Zhaoyan Zheng; Kaichun Gu; Sizhong Wu; Fanlong Zeng; Weiqiang Tan; Xiaowei Wu; Wenjing Xiao; Organometallics 24 (2005) 302–308; doi:10.1021/om049213d

data_4060057
_publ_section_title
;
 Chemoselective Stepwise Demetalation of Unusually Stable Fischer
 Biscarbene Complexes by Domino [4+2]/[2+2] Cycloaddition of
 2-Isopropenyl-2-oxazoline to 1-Alkynyl Fischer Carbene Complexes of
 Chromium and Tungsten
;
_journal_name_full               Organometallics
_journal_page_first              302
_journal_page_last               308
_journal_paper_doi               10.1021/om049213d
_journal_volume                  24
_journal_year                    2005
_chemical_formula_sum            'C28 H29 N O5'
_chemical_formula_weight         459.52
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 92.733(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   38.242(9)
_cell_length_b                   7.1774(17)
_cell_length_c                   17.705(4)
_cell_measurement_reflns_used    763
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      34.636
_cell_measurement_theta_min      4.983
_cell_volume                     4854.1(19)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0837
_diffrn_reflns_av_sigmaI/netI    0.1708
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            12758
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.13
_exptl_absorpt_coefficient_mu    0.086
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76367
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.258
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1952
_exptl_crystal_size_max          0.378
_exptl_crystal_size_mid          0.153
_exptl_crystal_size_min          0.068
_refine_diff_density_max         0.572
_refine_diff_density_min         -0.276
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.707
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     300
_refine_ls_number_reflns         4754
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.723
_refine_ls_R_factor_all          0.1657
_refine_ls_R_factor_gt           0.0583
_refine_ls_shift/su_max          0.081
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0576P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1318
_refine_ls_wR_factor_ref         0.1543
_reflns_number_gt                1433
_reflns_number_total             4754
_reflns_threshold_expression     >2sigma(I)
_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_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4060057