Synthesis of Mixed Tin-Ruthenium and Tin-Germanium-Ruthenium Carbonyl Clusters from [Ru3(CO)12] and Diaminometalenes (M = Sn, Ge)
Javier A. Cabeza; Pablo García-Álvarez; Diego Polo; Inorganic Chemistry 51 (2012) 2569–2576; doi:10.1021/ic202532u

data_4328425
_publ_section_title
;
 Synthesis of Mixed Tin-Ruthenium and Tin-Germanium-Ruthenium Carbonyl
 Clusters from [Ru3(CO)12] and Diaminometalenes (M = Sn, Ge)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2569
_journal_page_last               2576
_journal_paper_doi               10.1021/ic202532u
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C45 H108 N6 O9 Ru3 Si12 Sn3'
_chemical_formula_sum            'C45 H108 N6 O9 Ru3 Si12 Sn3'
_chemical_formula_weight         1873.73
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           176
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-P 6c'
_symmetry_space_group_name_H-M   'P 63/m'
_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            2
_cell_length_a                   14.9240(2)
_cell_length_b                   14.9240(2)
_cell_length_c                   20.7550(4)
_cell_measurement_reflns_used    6032
_cell_measurement_temperature    297(2)
_cell_measurement_theta_max      74.3268
_cell_measurement_theta_min      3.4168
_cell_volume                     4003.35(11)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Aug  2 2010,13:00:58)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Aug  2 2010,13:00:58)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Aug  2 2010,13:00:58)
;
_computing_molecular_graphics    'PLATON (Spek, 2008)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR-97 (Giacovazzo, 1999)'
_diffrn_ambient_temperature      297(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0618
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2455
_diffrn_reflns_theta_full        66.96
_diffrn_reflns_theta_max         66.96
_diffrn_reflns_theta_min         3.42
_exptl_absorpt_coefficient_mu    13.880
_exptl_absorpt_correction_T_max  0.0107
_exptl_absorpt_correction_T_min  0.0018
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
;
Parkin S,Moezzi B & Hope H, (1995) J. Appl. Cryst. 28, 53-56
cubic fit to sin(theta)/lambda - 24 parameters
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.554
_exptl_crystal_description       prism
_exptl_crystal_F_000             1884
_exptl_crystal_size_max          0.3365
_exptl_crystal_size_mid          0.1546
_exptl_crystal_size_min          0.0954
_refine_diff_density_max         0.805
_refine_diff_density_min         -0.818
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     210
_refine_ls_number_reflns         2455
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0493
_refine_ls_R_factor_gt           0.0458
_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^)+(0.0706P)^2^+1.7266P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1279
_refine_ls_wR_factor_ref         0.1319
_reflns_number_gt                2284
_reflns_number_total             2455
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic202532u_si_002.cif
_cod_data_source_block           pc9b_rt
_cod_database_code               4328425