A Combined Experimental−Theoretical Study on the Lithiation/Electrophilic Quench Sequence of (η5-Cyclohexadienyl)Mn(CO)3Complexes
Jacques, Béatrice; Chanaewa, Alina; Chavarot-Kerlidou, Murielle; Rose-Munch, Françoise; Rose, Eric; Gérard, Hélène; Organometallics 27 (2008) 626–; doi:10.1021/om7010529

data_4070820
_publ_section_title
;
 A Combined Experimental&#x2212;Theoretical Study on the
 Lithiation/Electrophilic Quench Sequence of
 (\h5-Cyclohexadienyl)Mn(CO)3Complexes
;
_journal_issue                   4
_journal_name_full               Organometallics
_journal_page_first              626
_journal_paper_doi               10.1021/om7010529
_journal_volume                  27
_journal_year                    2008
_chemical_formula_moiety         'C29 H23 Mn1 O5'
_chemical_formula_sum            'C29 H23 Mn O5'
_chemical_formula_weight         506.43
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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
_audit_creation_date             07-03-08
_audit_creation_method           CRYSTALS_ver_12.84
_cell_angle_alpha                90
_cell_angle_beta                 98.163(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.864(3)
_cell_length_b                   11.6069(18)
_cell_length_c                   17.1408(8)
_cell_measurement_reflns_used    153
_cell_measurement_temperature    250
_cell_measurement_theta_max      22
_cell_measurement_theta_min      3
_cell_volume                     2533.4(7)
_computing_cell_refinement
'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_collection       'COLLECT (Nonius, 1997-2001).'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SHELXS 86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      250
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.066
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            42698
_diffrn_reflns_theta_full        32.007
_diffrn_reflns_theta_max         32.007
_diffrn_reflns_theta_min         1.599
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.557
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.95
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.328
_exptl_crystal_description       stick
_exptl_crystal_F_000             1048
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.31
_refine_diff_density_min         -0.24
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1243
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         3259
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1160
_refine_ls_R_factor_gt           0.0303
_refine_ls_shift/su_max          0.001048
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 0.381 0.153E-01 0.115 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0967
_refine_ls_wR_factor_gt          0.0307
_refine_ls_wR_factor_ref         0.0307
_reflns_limit_h_max              18
_reflns_limit_h_min              -19
_reflns_limit_k_max              17
_reflns_limit_k_min              0
_reflns_limit_l_max              25
_reflns_limit_l_min              0
_reflns_number_gt                3259
_reflns_number_total             8783
_reflns_threshold_expression     I>3.0\s(I)
_oxford_structure_analysis_title '3080952 Compound X'
_cod_data_source_file            om7010529-file003.cif
_cod_data_source_block           CRYSTALS_cif
_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.

'_refine_ls_hydrogen_treatment' value 'refu' changed to
'refU' 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      'P 1 21/c 1 '
_cod_original_formula_sum        'C29 H23 Mn1 O5'
_cod_database_code               4070820