Ferrocenyl-Substituted (η5-Hydroxyalkylcyclohexadienyl)tricarbonylmanganese Complexes: Synthesis, Structural Determinations, and Formation of Carbenium Ions
Eloi, Antoine; Poizat, Mael; Hautecoeur, Albin; Panossian, Armen; Rose-Munch, Françoise; Rose, Eric; Organometallics 30 (2011) 5564–; doi:10.1021/om200905p

data_4065529
_publ_section_title
;
 Ferrocenyl-Substituted
 (\h5-Hydroxyalkylcyclohexadienyl)tricarbonylmanganese Complexes:
 Synthesis, Structural Determinations, and Formation of Carbenium Ions
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              5564
_journal_paper_doi               10.1021/om200905p
_journal_volume                  30
_journal_year                    2011
_chemical_formula_moiety         'C27 H22 B1 F4 Fe1 Mn1 O4'
_chemical_formula_sum            'C27 H22 B F4 Fe Mn O4'
_chemical_formula_weight         608.05
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             11-03-18
_audit_creation_method           CRYSTALS_ver_14.11
_cell_angle_alpha                90
_cell_angle_beta                 101.746(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.274(2)
_cell_length_b                   9.2958(9)
_cell_length_c                   20.041(3)
_cell_measurement_reflns_used    173
_cell_measurement_temperature    200
_cell_measurement_theta_max      23
_cell_measurement_theta_min      3
_cell_volume                     2603.5(6)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_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      200
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.000
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            25909
_diffrn_reflns_theta_full        25.204
_diffrn_reflns_theta_max         30.005
_diffrn_reflns_theta_min         1.608
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.103
_exptl_absorpt_correction_T_max  0.92
_exptl_absorpt_correction_T_min  0.92
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.551
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1232
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.080
_refine_diff_density_max         1.98
_refine_diff_density_min         -1.11
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9465
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     345
_refine_ls_number_reflns         7381
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0910
_refine_ls_R_factor_gt           0.0528
_refine_ls_shift/su_max          0.0010722
_refine_ls_shift/su_mean         0.0000306
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.08P)^2^ + 3.57P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1545
_refine_ls_wR_factor_gt          0.1338
_refine_ls_wR_factor_ref         0.1545
_reflns_limit_h_max              19
_reflns_limit_h_min              -20
_reflns_limit_k_max              13
_reflns_limit_k_min              0
_reflns_limit_l_max              28
_reflns_limit_l_min              0
_reflns_number_gt                4916
_reflns_number_total             7393
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.17
_oxford_diffrn_Wilson_scale      6.29
_oxford_refine_ls_r_factor_ref   0.0910
_oxford_refine_ls_scale          0.4200(7)
_oxford_reflns_number_all        7381
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_cod_data_source_file            om200905p_si_002.cif
_cod_data_source_block           15
_cod_original_sg_symbol_H-M      'P 2/n '
_cod_original_formula_sum        'C27 H22 B1 F4 Fe1 Mn1 O4'
_cod_database_code               4065529
_iucr_refine_instruction_details_constraints
;
FULL MN(1,X'S,U'S) UNTIL F(22) H(21,U[ISO]) UNTIL LAST 
EQUIV H(21,U[ISO]) UNTIL LAST 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
NO 
END                                                                             
;