[2 + 2] Cross Coupling of Benzene and Tropylium Ligands in Reductively Activated Piano Stool Complexes of Mn, Cr, and W
Li Shao; Steven J. Geib; Paul D. Badger; N. John Cooper; Journal of the American Chemical Society 124 (2002) 14812–14813; doi:10.1021/ja027081e

data_4115378
_publ_section_title
;
 [2 + 2] Cross Coupling of Benzene and Tropylium Ligands in Reductively
 Activated Piano Stool Complexes of Mn, Cr, and W
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14812
_journal_page_last               14813
_journal_paper_doi               10.1021/ja027081e
_journal_volume                  124
_journal_year                    2002
_chemical_formula_sum            'C26 H21 Mn O6 W'
_chemical_formula_weight         668.22
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.809(5)
_cell_length_b                   9.5230(19)
_cell_length_c                   11.144(2)
_cell_measurement_temperature    200(2)
_cell_volume                     2420.6(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.854
_diffrn_measured_fraction_theta_max 0.854
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0286
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1449
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         1.79
_exptl_absorpt_coefficient_mu    5.309
_exptl_absorpt_correction_T_max  0.6188
_exptl_absorpt_correction_T_min  0.1006
_exptl_crystal_density_diffrn    1.834
_exptl_crystal_F_000             1296
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.947
_refine_diff_density_min         -1.604
_refine_diff_density_rms         0.155
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.210
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         1449
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.210
_refine_ls_R_factor_all          0.0470
_refine_ls_R_factor_gt           0.0375
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0671P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1001
_refine_ls_wR_factor_ref         0.1045
_reflns_number_gt                1246
_reflns_number_total             1449
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja027081e-2_s2.cif
_cod_data_source_block           li1199c
_cod_database_code               4115378