Unprecedented (η5-Formylcyclohexadienyl)Mn(CO)3Complexes: Synthesis, Structural and Theoretical Characterizations, and Resolution of the Planar Chirality
Jacques, Béatrice; Eloi, Antoine; Chavarot-Kerlidou, Murielle; Rose-Munch, Françoise; Rose, Eric; Gérard, Hélène; Herson, Patrick; Organometallics 27 (2008) 2505–; doi:10.1021/om7012666

data_4071114
_publ_section_title
;
 Unprecedented (\h5-Formylcyclohexadienyl)Mn(CO)3Complexes: Synthesis,
 Structural and Theoretical Characterizations, and Resolution of the
 Planar Chirality
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              2505
_journal_paper_doi               10.1021/om7012666
_journal_volume                  27
_journal_year                    2008
_chemical_formula_moiety         'C23 H19 Mn1 O5'
_chemical_formula_sum            'C23 H19 Mn O5'
_chemical_formula_weight         430.33
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                72.273(8)
_cell_angle_beta                 80.503(11)
_cell_angle_gamma                88.397(8)
_cell_formula_units_Z            2
_cell_length_a                   8.9297(8)
_cell_length_b                   10.7940(10)
_cell_length_c                   11.1264(13)
_cell_measurement_reflns_used    133
_cell_measurement_temperature    200
_cell_measurement_theta_max      23
_cell_measurement_theta_min      3
_cell_volume                     1007.24(18)
_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 0.994
_diffrn_measured_fraction_theta_max 0.992
_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  0.031
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            19938
_diffrn_reflns_theta_full        27.300
_diffrn_reflns_theta_max         30.000
_diffrn_reflns_theta_min         1.948
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.687
_exptl_absorpt_correction_T_max  0.93
_exptl_absorpt_correction_T_min  0.92
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.419
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             444
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.46
_refine_diff_density_min         -0.40
_refine_ls_extinction_coef       80.590
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   1.3664
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     263
_refine_ls_number_reflns         5832
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0434
_refine_ls_R_factor_gt           0.0326
_refine_ls_shift/su_max          0.001186
_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: 
 8.75 8.34 1.76 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0506
_refine_ls_wR_factor_gt          0.0473
_refine_ls_wR_factor_ref         0.0506
_reflns_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              15
_reflns_limit_k_min              -14
_reflns_limit_l_max              15
_reflns_limit_l_min              0
_reflns_number_gt                4782
_reflns_number_total             5835
_reflns_threshold_expression     I>2.0\s(I)
_oxford_refine_ls_r_factor_ref   0.0434
_oxford_reflns_number_all        5832
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_cod_data_source_file            om7012666-file002.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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_cell_volume        1007.23(18)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C23 H19 Mn1 O5'
_cod_database_code               4071114