Bimetallic Zwitterionic Complexes with an Ambident Stanna-closo-dodecaborate Ligand: [1-{M(CO)5}-2,7,8-(μ-H)3-{Fe(triphos)}-SnB11H11] (M = Cr, Mo, W)
Gädt, Torben; Eichele, Klaus; Wesemann, Lars; Organometallics 25 (2006) 3904–; doi:10.1021/om060328m

data_4075504
_publ_section_title
;
 Bimetallic Zwitterionic Complexes with an Ambident
 Stanna-closo-dodecaborate Ligand:&#x00A0;
 [1-{M(CO)5}-2,7,8-(\m-H)3-{Fe(triphos)}-SnB11H11] (M = Cr, Mo, W)
;
_journal_issue                   16
_journal_name_full               Organometallics
_journal_page_first              3904
_journal_paper_doi               10.1021/om060328m
_journal_volume                  25
_journal_year                    2006
_chemical_formula_moiety         'C46 H50 B11 Fe Mo O5 P3 Sn, 2(C H2 Cl2)'
_chemical_formula_sum            'C48 H54 B11 Cl4 Fe Mo O5 P3 Sn'
_chemical_formula_weight         1335.01
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 112.210(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   23.1640(8)
_cell_length_b                   20.2790(9)
_cell_length_c                   27.1721(10)
_cell_measurement_reflns_used    54031
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      62.23
_cell_measurement_theta_min      5.90
_cell_volume                     11816.9(8)
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2004)'
_computing_data_collection       'X-AREA (Stoe & Cie, 2004)'
_computing_data_reduction        'X-AREA (Stoe & Cie, 2004)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXL97 and WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.918
_diffrn_measurement_device_type  'Stoe IPDS 2T'
_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  0.0979
_diffrn_reflns_av_sigmaI/netI    0.1091
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            131701
_diffrn_reflns_theta_full        26.30
_diffrn_reflns_theta_max         31.20
_diffrn_reflns_theta_min         2.95
_exptl_absorpt_coefficient_mu    1.175
_exptl_absorpt_correction_T_max  0.8767
_exptl_absorpt_correction_T_min  0.7460
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
The absorption correction (X-RED; Stoe & Cie, 2004) 
was performed after optimizing the crystal shape 
using X-SHAPE (Stoe & Cie, 2004).
;
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.501
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             5344
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.319
_refine_diff_density_min         -0.921
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1384
_refine_ls_number_reflns         35188
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.1622
_refine_ls_R_factor_gt           0.0808
_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^)+(0.0323P)^2^+44.7190P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1256
_refine_ls_wR_factor_ref         0.1511
_reflns_number_gt                19759
_reflns_number_total             35188
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om060328msi20060418_035617.cif
_cod_data_source_block           tg34
_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.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

2026-02-27
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C96 H108 B22 Cl8 Fe2 Mo2 O10 P6 Sn2'
_cod_original_formula_weight         2670.02
_cod_original_formula_moiety      '2(C46 H50 B11 Fe Mo O5 P3 Sn), 4(C H2 Cl2)'
_cod_original_formula_units_Z            4
_cod_original_sg_symbol_H-M      P21/a
_cod_database_code               4075504