(η6-Bromoarene)Mn(CO)3+Complexes: Synthesis and Applications to the Functionalization of (η5-Cyclohexadienyl)Mn(CO)3Complexes by Halogen−Metal Exchange Reaction
Eloi, Antoine; Rose-Munch, Françoise; Rose, Eric; Lennartz, Petra; Organometallics 28 (2009) 5757–; doi:10.1021/om9006517

data_4070206
_publ_section_title
;
 (\h6-Bromoarene)Mn(CO)3+Complexes: Synthesis and Applications to the
 Functionalization of (\h5-Cyclohexadienyl)Mn(CO)3Complexes by
 Halogen&#x2212;Metal Exchange Reaction
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              5757
_journal_paper_doi               10.1021/om9006517
_journal_volume                  28
_journal_year                    2009
_chemical_formula_moiety         'C10 H7 Br1 Mn1 O4, B F4'
_chemical_formula_sum            'C10 H7 B Br F4 Mn O4'
_chemical_formula_weight         412.80
_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
_cell_angle_alpha                90
_cell_angle_beta                 100.105(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.5888(16)
_cell_length_b                   7.6169(10)
_cell_length_c                   20.189(2)
_cell_measurement_reflns_used    72
_cell_measurement_temperature    200
_cell_measurement_theta_max      21
_cell_measurement_theta_min      3
_cell_volume                     2814.2(5)
_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 0.995
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_device_type  Area
_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       26
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            8139
_diffrn_reflns_theta_full        25.516
_diffrn_reflns_theta_max         30.019
_diffrn_reflns_theta_min         2.049
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.833
_exptl_absorpt_correction_T_max  0.46
_exptl_absorpt_correction_T_min  0.34
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.949
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1600
_exptl_crystal_size_max          0.380
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.200
_refine_diff_density_max         1.45
_refine_diff_density_min         -2.40
_refine_ls_extinction_coef       36.6(18)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   1.0263
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     381
_refine_ls_number_reflns         8138
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0776
_refine_ls_R_factor_gt           0.0354
_refine_ls_shift/su_max          0.0008142
_refine_ls_shift/su_mean         9.8991337
_refine_ls_structure_factor_coef Fsqd
_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: 
 7.56 7.68 2.14 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0623
_refine_ls_wR_factor_gt          0.0436
_refine_ls_wR_factor_ref         0.0623
_reflns_limit_h_max              25
_reflns_limit_h_min              -26
_reflns_limit_k_max              10
_reflns_limit_k_min              0
_reflns_limit_l_max              28
_reflns_limit_l_min              0
_reflns_number_gt                5208
_reflns_number_total             8139
_reflns_threshold_expression     I>2.0\s(I)
_oxford_refine_ls_r_factor_ref   0.0776
_oxford_refine_ls_scale          0.20912(8)
_oxford_reflns_number_all        8138
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_cod_data_source_file            om9006517_si_002.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'P 21/c '
_cod_original_formula_sum        'C10 H7 B1 Br1 F4 Mn1 O4'
_cod_database_code               4070206