Surprising Acid/Base and Ion-Sequestration Chemistry of Sn94-: HSn93-, Ni@HSn93-, and the Sn93- Ion Revisited
F. Sanem Kocak; Domonique O. Downing; Peter Zavalij; Yiu-Fai Lam; Andrei N. Vedernikov; Bryan Eichhorn; Journal of the American Chemical Society 134 (2012) 9733–9740; doi:10.1021/ja3018797

data_4118047
_publ_section_title
;
 Surprising Acid/Base and Ion-Sequestration Chemistry of Sn94-: HSn93-,
 Ni@HSn93-, and the Sn93- Ion Revisited
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9733
_journal_page_last               9740
_journal_paper_doi               10.1021/ja3018797
_journal_volume                  134
_journal_year                    2012
_chemical_formula_moiety         '3(C18 H36 K N2 O6), Sn9, 1.5(C2 H8 N2)'
_chemical_formula_sum            'C57 H120 K3 N9 O18 Sn9'
_chemical_formula_weight         2405.13
_chemical_name_common            S9-cluster
_chemical_name_systematic
;
S9-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                89.391(2)
_cell_angle_beta                 79.589(2)
_cell_angle_gamma                78.861(2)
_cell_formula_units_Z            2
_cell_length_a                   13.9891(15)
_cell_length_b                   14.8896(16)
_cell_length_c                   22.004(2)
_cell_measurement_reflns_used    35037
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.2
_cell_measurement_theta_min      2.2
_cell_volume                     4421.5(8)
_computing_cell_refinement       Apex2
_computing_data_collection       'Apex2 (Bruker, 2005)'
_computing_data_reduction        Apex2
_computing_molecular_graphics    'XSHEL (Bruker, 2004)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 11.198
_diffrn_detector_type            'Bruker Smart Apex II'
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details      610,610,610,437
_diffrn_measurement_device_type  'three-circle diffractometer'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_measurement_specimen_support 'MiTeGen loop'
_diffrn_orient_matrix_type       standard
_diffrn_orient_matrix_UB_11      -0.0022070
_diffrn_orient_matrix_UB_12      -0.0058516
_diffrn_orient_matrix_UB_13      -0.0449331
_diffrn_orient_matrix_UB_21      0.0529592
_diffrn_orient_matrix_UB_22      0.0370973
_diffrn_orient_matrix_UB_23      -0.0102719
_diffrn_orient_matrix_UB_31      0.0517744
_diffrn_orient_matrix_UB_32      -0.0572536
_diffrn_orient_matrix_UB_33      -0.0034540
_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  0.0201
_diffrn_reflns_av_sigmaI/netI    0.0265
_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       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            59313
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.18
_diffrn_source_current           30.00
_diffrn_source_voltage           50.00
_exptl_absorpt_coefficient_mu    2.697
_exptl_absorpt_correction_T_max  0.496
_exptl_absorpt_correction_T_min  0.301
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.807
_exptl_crystal_description       plate
_exptl_crystal_F_000             2352
_exptl_crystal_id
'Eichhorn/Sanem 10/08/10 Sn9H #10 needles & some plates'
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.26
_refine_diff_density_max         4.036
_refine_diff_density_min         -1.672
_refine_diff_density_rms         0.128
_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     897
_refine_ls_number_reflns         25571
_refine_ls_number_restraints     101
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0450
_refine_ls_R_factor_gt           0.0345
_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^)+(0.01P)^2^+20.5P], P=(max(Fo^2^,0)+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0699
_refine_ls_wR_factor_ref         0.0728
_reflns_number_gt                21241
_reflns_number_total             25571
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja3018797_si_002.cif
_cod_data_source_block           2012
_cod_database_code               4118047
_diffrn_measurement_frame_width-ccd -0.30
_diffrn_measurement_total_frames-ccd 2267
_diffrn_measurement_frame_time-ccd 5
_diffrn_measurement_total_time-ccd 6.9
_diffrn_detector_distance-ccd    5.000
_diffrn_measurement_frame_size-ccd 512