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_4328424
_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         'C49 H98 Ge N6 O9 Ru3 Si8 Sn2, 0.5(C6 H14)'
_chemical_formula_sum            'C52 H105 Ge N6 O9 Ru3 Si8 Sn2'
_chemical_formula_weight         1796.32
_chemical_name_systematic
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 ?
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_space_group_IT_number           2
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_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                104.017(2)
_cell_angle_beta                 93.241(2)
_cell_angle_gamma                94.865(2)
_cell_formula_units_Z            2
_cell_length_a                   11.7533(3)
_cell_length_b                   14.3899(4)
_cell_length_c                   23.7850(6)
_cell_measurement_reflns_used    16917
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      73.7992
_cell_measurement_theta_min      3.1792
_cell_volume                     3876.51(18)
_computing_cell_refinement
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Aug  2 2010,13:00:58)
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_computing_data_collection
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Aug  2 2010,13:00:58)
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_computing_data_reduction
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Aug  2 2010,13:00:58)
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_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      100(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Xcalibur, Onyx, Nova'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'Nova (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.0564
_diffrn_reflns_av_sigmaI/netI    0.0630
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            26287
_diffrn_reflns_theta_full        67.49
_diffrn_reflns_theta_max         67.49
_diffrn_reflns_theta_min         3.18
_exptl_absorpt_coefficient_mu    11.669
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.43630
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Aug  2 2010,13:00:58)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
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_exptl_crystal_colour            dark-green
_exptl_crystal_density_diffrn    1.539
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1814
_exptl_crystal_size_max          0.1102
_exptl_crystal_size_mid          0.0741
_exptl_crystal_size_min          0.0457
_refine_diff_density_max         1.240
_refine_diff_density_min         -1.542
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     761
_refine_ls_number_reflns         13691
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0475
_refine_ls_R_factor_gt           0.0397
_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^)+(0.0512P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0962
_refine_ls_wR_factor_ref         0.1010
_reflns_number_gt                11767
_reflns_number_total             13691
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic202532u_si_001.cif
_cod_data_source_block           dp81
_cod_database_code               4328424