Cluster Growth and Fragmentation in the Highly Fluxional Platinum Derivatives of Sn94-: Synthesis, Characterization, and Solution Dynamics of Pt2@Sn174- and Pt@Sn9H3-
Banu Kesanli; Jordan E. Halsig; Peter Zavalij; James C. Fettinger; Yiu-Fai Lam; Bryan W. Eichhorn; Journal of the American Chemical Society 129 (2007) 4567–4574; doi:10.1021/ja065764e

data_4109296
_publ_section_title
;
 Cluster Growth and Fragmentation in the Highly Fluxional Platinum
 Derivatives of Sn94-: Synthesis, Characterization, and Solution Dynamics
 of Pt2@Sn174- and Pt@Sn9H3-
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4567
_journal_page_last               4574
_journal_paper_doi               10.1021/ja065764e
_journal_volume                  129
_journal_year                    2007
_chemical_formula_moiety         'Pt2 Sn17, 4(C18 H36 K N2 O6), 3(C2 H8 N2)'
_chemical_formula_sum            'C78 H168 K4 N14 O24 P0 Pt2 Sn17'
_chemical_formula_weight         4250.57
_chemical_name_common            'Platinum Tin cluster'
_chemical_name_systematic
;
Platinum Tin cluster
;
_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 & ZCIF'
_cell_angle_alpha                116.874(4)
_cell_angle_beta                 96.699(4)
_cell_angle_gamma                100.299(4)
_cell_formula_units_Z            1
_cell_length_a                   14.710(3)
_cell_length_b                   15.829(4)
_cell_length_c                   16.253(4)
_cell_measurement_reflns_used    8090
_cell_measurement_temperature    220(2)
_cell_measurement_theta_max      28.3
_cell_measurement_theta_min      2.3
_cell_volume                     3236.2(13)
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'XSHEL (Bruker, 1999)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      220(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 8.33
_diffrn_detector_type            'Bruker Smart1000'
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_details      606,606,606,1206
_diffrn_measurement_device_type  'three-circle diffractometer'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_measurement_specimen_support 'glass capillary'
_diffrn_orient_matrix_type       standard
_diffrn_orient_matrix_UB_11      0.0358728
_diffrn_orient_matrix_UB_12      0.0267198
_diffrn_orient_matrix_UB_13      -0.0354206
_diffrn_orient_matrix_UB_21      0.0580874
_diffrn_orient_matrix_UB_22      -0.0150818
_diffrn_orient_matrix_UB_23      0.0225117
_diffrn_orient_matrix_UB_31      -0.0191622
_diffrn_orient_matrix_UB_32      -0.0666495
_diffrn_orient_matrix_UB_33      -0.0570065
_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  0.0398
_diffrn_reflns_av_sigmaI/netI    0.0418
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            40278
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.53
_diffrn_source_current           30
_diffrn_source_voltage           50
_diffrn_standards_decay_%        0.00
_exptl_absorpt_coefficient_mu    5.553
_exptl_absorpt_correction_T_max  0.500
_exptl_absorpt_correction_T_min  0.292
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            dark-red
_exptl_crystal_density_diffrn    2.181
_exptl_crystal_density_method    not-measured
_exptl_crystal_description       prism
_exptl_crystal_F_000             2008
_exptl_crystal_id                Eichhorn
_exptl_crystal_size_max          0.290
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.125
_refine_diff_density_max         1.596
_refine_diff_density_min         -1.519
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     911
_refine_ls_number_reflns         14639
_refine_ls_number_restraints     670
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0553
_refine_ls_R_factor_gt           0.0372
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.02P)^2^+8.78P], P=(max(Fo^2^,0)+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0812
_refine_ls_wR_factor_ref         0.0879
_reflns_number_gt                11410
_reflns_number_total             14639
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja065764esi20060808_055854.cif
_cod_data_source_block           1337
_cod_original_cell_volume        3236.4(12)
_cod_database_code               4109296
_diffrn_measurement_total_frames-ccd 3024
_diffrn_measurement_frame_width-ccd 0.3
_diffrn_detector_distance-ccd    4.940
_diffrn_measurement_frame_time-ccd 20
_diffrn_measurement_total_time-ccd 22.81
_diffrn_measurement_frame_size-ccd 512