Cobalt, Rhodium, Iridium, and Ruthenium Carbonyl Complexes with Stanna-closo-dodecaborate:103Rh NMR,119Sn Mössbauer Spectroscopy, and Solid-State119Sn NMR
Fleischhauer, Sebastian; Eichele, Klaus; Schellenberg, Inga; Pöttgen, Rainer; Wesemann, Lars; Organometallics 30 (2011) 3200–; doi:10.1021/om200301v

data_4064737
_publ_section_title
;
 Cobalt, Rhodium, Iridium, and Ruthenium Carbonyl Complexes with
 Stanna-closo-dodecaborate:103Rh NMR,119Sn M\"ossbauer Spectroscopy, and
 Solid-State119Sn NMR
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              3200
_journal_paper_doi               10.1021/om200301v
_journal_volume                  30
_journal_year                    2011
_chemical_formula_sum            'C50 H145 B33 Ir N9 O2 Sn3'
_chemical_formula_weight         1809.75
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.7901(5)
_cell_length_b                   19.9695(10)
_cell_length_c                   32.4045(14)
_cell_measurement_reflns_used    43011
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.20
_cell_measurement_theta_min      2.65
_cell_volume                     8923.6(7)
_computing_cell_refinement       'Stoe X-Area'
_computing_data_collection       'Stoe WinXpose'
_computing_data_reduction        'Stoe X-Area'
_computing_molecular_graphics    ORTEP3
_computing_publication_material  SHELX97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Stoe IPDS 2T'
_diffrn_measurement_method       'OMEGA SCANS'
_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  0.1046
_diffrn_reflns_av_sigmaI/netI    0.0679
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            60567
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         5.69
_exptl_absorpt_coefficient_mu    2.356
_exptl_absorpt_correction_T_max  0.7782
_exptl_absorpt_correction_T_min  0.4790
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Stoe XRED, XSHAPE'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.347
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3664
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.462
_refine_diff_density_min         -1.324
_refine_diff_density_rms         0.105
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.518(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     817
_refine_ls_number_reflns         16149
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.0568
_refine_ls_R_factor_gt           0.0488
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0264P)^2^+45.3986P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1086
_refine_ls_wR_factor_ref         0.1123
_reflns_number_gt                14586
_reflns_number_total             16149
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om200301v_si_002.cif
_cod_data_source_block           sf61
_cod_database_code               4064737