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_4064738
_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            'C30 H105 B33 Co N9 O2 Sn3'
_chemical_formula_weight         1395.96
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P -2n -2ac'
_symmetry_space_group_name_H-M   'P c 21 n'
_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                   12.4299(6)
_cell_length_b                   17.8892(8)
_cell_length_c                   31.7370(16)
_cell_measurement_reflns_used    36246
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      54.50
_cell_measurement_theta_min      4.90
_cell_volume                     7057.1(6)
_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  0.0638
_diffrn_reflns_av_sigmaI/netI    0.0360
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            73755
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         5.67
_exptl_absorpt_coefficient_mu    1.316
_exptl_absorpt_correction_T_max  0.8676
_exptl_absorpt_correction_T_min  0.7799
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'stoe xred, xshape'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.314
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2824
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.620
_refine_diff_density_min         -0.613
_refine_diff_density_rms         0.077
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.47(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     581
_refine_ls_number_reflns         13100
_refine_ls_number_restraints     185
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0574
_refine_ls_R_factor_gt           0.0449
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0511P)^2^+13.0244P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1077
_refine_ls_wR_factor_ref         0.1142
_reflns_number_gt                10803
_reflns_number_total             13100
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om200301v_si_002.cif
_cod_data_source_block           sf62
_cod_original_sg_symbol_H-M      Pc21n
_cod_database_code               4064738