Resolution of Planar Chiral Cationic (η6-Arene)tricarbonylmanganese Complexes
Antoine Eloi; Françoise Rose-Munch; Eric Rose; Journal of the American Chemical Society 131 (2009) 14178–14179; doi:10.1021/ja905712k

data_4105109
_publ_contact_author_address
; 
Laboratoire de Chimie Organique, Equipe Synthese Organique et 
Organometallique, Universite Pierre et Marie Curie, UMR 7611
4 place Jussieu, 75252 Paris cedex 05, France
;
_publ_contact_author_email       francoise.rose@upmc.fr
_publ_contact_author_fax         '00 33 (0) 1 44 27 55 04 '
_publ_contact_author_name        'F. Rose-Munch'
_publ_contact_author_phone       '00 33 (0) 1 44 27 62 35'
_publ_section_title
;
 Resolution of Planar Chiral Cationic (\h6-Arene)tricarbonylmanganese
 Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14178
_journal_page_last               14179
_journal_paper_doi               10.1021/ja905712k
_journal_volume                  131
_journal_year                    2009
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C11 H10 Mn1 O4,B1 F4'
_chemical_formula_sum            'C11 H10 B F4 Mn O4'
_chemical_formula_weight         347.93
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             08-02-07
_audit_creation_method           CRYSTALS_ver_12.85
_cell_angle_alpha                90
_cell_angle_beta                 100.152(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.0577(19)
_cell_length_b                   10.8143(10)
_cell_length_c                   13.1328(19)
_cell_measurement_reflns_used    49
_cell_measurement_temperature    200
_cell_measurement_theta_max      21
_cell_measurement_theta_min      3
_cell_volume                     1406.1(4)
_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      200
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.945
_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  0.049
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            20445
_diffrn_reflns_theta_full        28.207
_diffrn_reflns_theta_max         30.008
_diffrn_reflns_theta_min         1.575
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.994
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_correction_T_min  0.93
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.644
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             696
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.00
_refine_diff_density_min         -0.73
_refine_ls_abs_structure_details 'Flack (1983), 3315 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.17(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.0744
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     380
_refine_ls_number_reflns         5076
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0960
_refine_ls_R_factor_gt           0.0727
_refine_ls_shift/su_max          0.004157
_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: 
 1.79 0.974 1.17 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1149
_refine_ls_wR_factor_gt          0.0831
_refine_ls_wR_factor_ref         0.0797
_reflns_limit_h_max              13
_reflns_limit_h_min              -14
_reflns_limit_k_max              15
_reflns_limit_k_min              -14
_reflns_limit_l_max              18
_reflns_limit_l_min              0
_reflns_number_gt                5593
_reflns_number_total             7389
_reflns_threshold_expression     I>2.0\s(I)
_oxford_refine_ls_r_factor_ref   0.0686
_oxford_reflns_number_all        7386
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            ja905712k_si_001.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_hydrogen_treatment' value 'refu' changed to 'refU'
according to the built-in table from CIF Core 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 1 '
_cod_original_formula_sum        'C11 H10 B1 F4 Mn1 O4'
_cod_database_code               4105109