The [Sn9Pt2(PPh3)]2- and [Sn9Ni2(CO)]3- Complexes: Two Markedly Different Sn9M2L Transition Metal Zintl Ion Clusters and Their Dynamic Behavior
Banu Kesanli; James Fettinger; Donna R. Gardner; Bryan Eichhorn; Journal of the American Chemical Society 124 (2002) 4779–4786; doi:10.1021/ja012528p

data_4114752
_publ_section_title
;
 The [Sn9Pt2(PPh3)]2- and [Sn9Ni2(CO)]3- Complexes: Two Markedly Different
 Sn9M2L Transition Metal Zintl Ion Clusters and Their Dynamic Behavior
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4779
_journal_page_last               4786
_journal_paper_doi               10.1021/ja012528p
_journal_volume                  124
_journal_year                    2002
_chemical_formula_sum            'C112 H190 K4 N12 O24 P2 Pt4 Sn18'
_chemical_formula_weight         5223.88
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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                79.4450(10)
_cell_angle_beta                 76.0670(10)
_cell_angle_gamma                83.7260(10)
_cell_formula_units_Z            1
_cell_length_a                   13.1703(6)
_cell_length_b                   13.3120(6)
_cell_length_c                   24.3236(10)
_cell_measurement_temperature    193(2)
_cell_volume                     4059.5(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and 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  0.0595
_diffrn_reflns_av_sigmaI/netI    0.0631
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            53909
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.60
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    6.322
_exptl_absorpt_correction_type   'empirical, Sadabs'
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    2.137
_exptl_crystal_description       Block
_exptl_crystal_F_000             2456
_exptl_crystal_size_max          0.105
_exptl_crystal_size_mid          0.083
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.858
_refine_diff_density_min         -1.078
_refine_diff_density_rms         0.130
_refine_ls_extinction_coef       0.000036(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     875
_refine_ls_number_reflns         14288
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0790
_refine_ls_R_factor_gt           0.0398
_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^)+(0.0180P)^2^+10.4114P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0684
_refine_ls_wR_factor_ref         0.0819
_reflns_number_gt                9417
_reflns_number_total             14288
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja012528p_1.cif
_cod_data_source_block           '[Sn9Pt2(PPh3)][K(crypt)]2-en'
_cod_database_code               4114752