Pyranylidene Carbene Complexes from 1-Lithio 1,3-Dienes and M(CO)6(M = Cr, Mo, W): Novel Synthesis and Demetalation Reaction
Wang, Qifeng; Zhang, Wen-Xiong; Xi, Zhenfeng; Organometallics 27 (2008) 3627–; doi:10.1021/om800565r

data_4072069
_publ_section_title
;
 Pyranylidene Carbene Complexes from 1-Lithio 1,3-Dienes and M(CO)6(M =
 Cr, Mo, W): Novel Synthesis and Demetalation Reaction
;
_journal_issue                   15
_journal_name_full               Organometallics
_journal_page_first              3627
_journal_paper_doi               10.1021/om800565r
_journal_volume                  27
_journal_year                    2008
_chemical_formula_sum            'C22 H28 O6 S W'
_chemical_formula_weight         604.35
_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                83.70(3)
_cell_angle_beta                 66.19(3)
_cell_angle_gamma                72.92(3)
_cell_formula_units_Z            2
_cell_length_a                   10.667(2)
_cell_length_b                   11.590(2)
_cell_length_c                   11.644(2)
_cell_measurement_reflns_used    15592
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      54.93
_cell_measurement_theta_min      3.82
_cell_volume                     1258.9(5)
_computing_cell_refinement       'Rapid Auto(Rigaku 2001)'
_computing_data_collection       'Rapid Auto(Rigaku 2001)'
_computing_data_reduction        'Rapid Auto(Rigaku 2001)'
_computing_molecular_graphics    'XP in Siemens SHELXTL (Sheldrick, 1994)'
_computing_publication_material  'SHELX97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku raxis Rapid IP Area Detector'
_diffrn_measurement_method       '\w scans at fixed \c = 45\%'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0437
_diffrn_reflns_av_sigmaI/netI    0.0624
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8272
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.17
_exptl_absorpt_coefficient_mu    4.703
_exptl_absorpt_correction_T_max  0.6506
_exptl_absorpt_correction_T_min  0.5200
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR by T.Higashi    8 March, 1995'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.595
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             596
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.912
_refine_diff_density_min         -0.902
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         4435
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0630
_refine_ls_R_factor_gt           0.0468
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0318P)^2^+0.4292P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0801
_refine_ls_wR_factor_ref         0.0842
_reflns_number_gt                3733
_reflns_number_total             4435
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800565r-file006.cif
_cod_data_source_block           sx2245
_cod_original_cell_volume        1258.7(4)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4072069