Synthesis and Reactivity of (η5-Hydroxyalkylcyclohexadienyl)Mn(CO)3Complexes
Cetiner, Derya; Norel, Lucie; Tranchier, Jean-Philippe; Rose-Munch, Françoise; Rose, Eric; Herson, Patrick; Organometallics 29 (2010) 1778–; doi:10.1021/om100062m

data_4065678
_publ_section_title
;
 Synthesis and Reactivity of
 (\h5-Hydroxyalkylcyclohexadienyl)Mn(CO)3Complexes
;
_journal_issue                   7
_journal_name_full               Organometallics
_journal_page_first              1778
_journal_paper_doi               10.1021/om100062m
_journal_volume                  29
_journal_year                    2010
_chemical_formula_moiety         'C21 H16 B1 F4 Mn1 O5 S1'
_chemical_formula_sum            'C21 H16 B F4 Mn O5 S'
_chemical_formula_weight         522.15
_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                 97.09(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   10.583(6)
_cell_length_b                   39.81(3)
_cell_length_c                   10.614(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    295
_cell_measurement_theta_max      13
_cell_measurement_theta_min      12
_cell_volume                     4438(5)
_computing_cell_refinement       'CAD4 EXPRESS, (Straver, 1992)'
_computing_data_collection       'CAD4 EXPRESS, (Straver, 1992)'
_computing_data_reduction        'RC93 (Watkin et al., 1994)'
_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      295
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'Enraf-Nonius CAD4'
_diffrn_measurement_device_type  Serial
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.096
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       50
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            10046
_diffrn_reflns_theta_full        76.747
_diffrn_reflns_theta_max         76.747
_diffrn_reflns_theta_min         2.220
_diffrn_standards_decay_%        8.18
_diffrn_standards_interval_time  3600
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    6.314
_exptl_absorpt_correction_T_max  0.41
_exptl_absorpt_correction_T_min  0.25
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North et al., 1968)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.563
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             2112
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.99
_refine_diff_density_min         -0.73
_refine_ls_extinction_coef       330
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   1.0938
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     597
_refine_ls_number_reflns         3866
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.2027
_refine_ls_R_factor_gt           0.0932
_refine_ls_shift/su_max          0.007940
_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: 
 7.32 4.03 5.38 1.42 -0.322 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2616
_refine_ls_wR_factor_gt          0.0995
_refine_ls_wR_factor_ref         0.0995
_reflns_limit_h_max              13
_reflns_limit_h_min              -13
_reflns_limit_k_max              50
_reflns_limit_k_min              0
_reflns_limit_l_max              13
_reflns_limit_l_min              0
_reflns_number_gt                3866
_reflns_number_total             9376
_reflns_threshold_expression     I>2.0\s(I)
_oxford_refine_ls_r_factor_ref   0.0932
_oxford_reflns_number_all        9341
_oxford_reflns_threshold_expression_ref I>2.0\s(I)
_cod_data_source_file            om100062m_si_001.cif
_cod_data_source_block           1
_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        'C21 H16 B1 F4 Mn1 O5 S1'
_cod_database_code               4065678