Mixed-Valence Manganese Carbonyl Complexes with Supersilyl Thiolate Ligands: [(OC)4Mn(μ-SSitBu3)2Mn(THF)X] (X = Br, SSitBu3) and Na(THF)6[(OC)3Mn(μ-SSitBu3)3MnSSitBu3]
Kückmann, Theresa I.; Schödel, Frauke; Sänger, Inge; Bolte, Michael; Wagner, Matthias; Lerner, Hans-Wolfram; Organometallics 27 (2008) 3272–; doi:10.1021/om800211k

data_4071537
_publ_section_title
;
 Mixed-Valence Manganese Carbonyl Complexes with Supersilyl Thiolate
 Ligands: [(OC)4Mn(\m-SSitBu3)2Mn(THF)X] (X = Br, SSitBu3) and
 Na(THF)6[(OC)3Mn(\m-SSitBu3)3MnSSitBu3]
;
_journal_issue                   13
_journal_name_full               Organometallics
_journal_page_first              3272
_journal_paper_doi               10.1021/om800211k
_journal_volume                  27
_journal_year                    2008
_chemical_formula_sum            'C99 H210 Mn2 Na O9 S7 Si6'
_chemical_formula_weight         2070.50
_chemical_name_systematic        ?
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   14.6380(5)
_cell_length_b                   14.6380(5)
_cell_length_c                   101.570(7)
_cell_measurement_reflns_used    19824
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      24.4
_cell_measurement_theta_min      2.1
_cell_volume                     18847.8(16)
_computing_cell_refinement       'X-Area (Stoe & Cie, 2001)'
_computing_data_collection       'X-Area (Stoe & Cie, 2001)'
_computing_data_reduction        'X-Area (Stoe & Cie, 2001)'
_computing_molecular_graphics    'XP in SHELXTL-Plus (Sheldrick, 1991)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997) '
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990) '
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'STOE IPDS II two-circle-diffractometer'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1004
_diffrn_reflns_av_sigmaI/netI    0.1339
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       120
_diffrn_reflns_limit_l_min       -120
_diffrn_reflns_number            70191
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.13
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.423
_exptl_absorpt_correction_T_max  0.9431
_exptl_absorpt_correction_T_min  0.8942
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'MULABS (Spek, 2003; Blessing, 1995)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.095
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             6798
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.077
_refine_diff_density_min         -0.873
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     392
_refine_ls_number_reflns         7364
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.1766
_refine_ls_R_factor_gt           0.1075
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1780P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2847
_refine_ls_wR_factor_ref         0.3175
_reflns_number_gt                3849
_reflns_number_total             7364
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om800211k-file001.cif
_cod_data_source_block           wa520
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal'
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        18847.7(16)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4071537