A combined experimental‒theoretical study on the lithiation/electrophilic quench reaction of benzylic position of (η5-tetramethylcyclohexadienyl)-Mn(CO)3
Rose, Eric; Dubarle-Offner, Julien; Rose-Munch, Françoise; Gérard, Hélène; New Journal of Chemistry 35 (2011) 2375–; doi:10.1039/c1nj20178f

data_7052727
_publ_section_title
;
 A combined experimental--theoretical study on the
 lithiation/electrophilic quench reaction of benzylic position of
 (\h5-tetramethylcyclohexadienyl)-Mn(CO)3
;
_journal_issue                   10
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              2375
_journal_paper_doi               10.1039/c1nj20178f
_journal_volume                  35
_journal_year                    2011
_chemical_formula_moiety         'C13 H15 Mn1 O3'
_chemical_formula_sum            'C13 H15 Mn O3'
_chemical_formula_weight         274.19
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 108.932(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.8868(10)
_cell_length_b                   9.2279(9)
_cell_length_c                   12.5852(7)
_cell_measurement_reflns_used    157
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      24
_cell_measurement_theta_min      4
_cell_volume                     1305.80(19)
_computing_cell_refinement
'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1999)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR-92 (Giacovazzo, 1993)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_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  0.0303
_diffrn_reflns_av_sigmaI/netI    0.0438
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            10505
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         3.62
_exptl_absorpt_coefficient_mu    1.004
_exptl_absorpt_correction_T_max  0.904
_exptl_absorpt_correction_T_min  0.529
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.395
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             568
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.297
_refine_diff_density_min         -0.234
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     158
_refine_ls_number_reflns         3772
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0593
_refine_ls_R_factor_gt           0.0333
_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^)+(0.0356P)^2^+0.1675P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0727
_refine_ls_wR_factor_ref         0.0801
_reflns_number_gt                2731
_reflns_number_total             3772
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c1nj20178f.txt
_cod_data_source_block           jdo-tetrah
_cod_original_cell_volume        1305.80(18)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7052727