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_4118046
_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
'6(C18 H36 K N2 O6), 2(Ni Sn9), C7 H8, 3(C2 H8 N2)'
_chemical_formula_sum            'C121 H248 K6 N18 Ni2 O36 Sn18'
_chemical_formula_weight         5019.81
_chemical_name_common            NiSn9-cluster
_chemical_name_systematic
;
NiSn9-cluster
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                90.00
_cell_angle_beta                 93.5886(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   28.212(3)
_cell_length_b                   23.516(3)
_cell_length_c                   27.828(3)
_cell_measurement_reflns_used    39294
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.1
_cell_measurement_theta_min      2.3
_cell_volume                     18426(4)
_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      150(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 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details      610,610,384
_diffrn_measurement_device_type  'three-circle diffractometer'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'MiTeGen loop'
_diffrn_orient_matrix_type       standard
_diffrn_orient_matrix_UB_11      -0.0035829
_diffrn_orient_matrix_UB_12      -0.0014012
_diffrn_orient_matrix_UB_13      -0.0354718
_diffrn_orient_matrix_UB_21      -0.0199689
_diffrn_orient_matrix_UB_22      0.0353675
_diffrn_orient_matrix_UB_23      -0.0002450
_diffrn_orient_matrix_UB_31      0.0297452
_diffrn_orient_matrix_UB_32      0.0235680
_diffrn_orient_matrix_UB_33      -0.0017468
_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  0.0301
_diffrn_reflns_av_sigmaI/netI    0.0293
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            119472
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.73
_diffrn_source_current           30.00
_diffrn_source_voltage           50.00
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    2.789
_exptl_absorpt_correction_T_max  0.889
_exptl_absorpt_correction_T_min  0.379
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.810
_exptl_crystal_description       plate
_exptl_crystal_F_000             9832
_exptl_crystal_id                'Eichhorn/Kocak Sn9Ni-cluster red plate 150K'
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.319
_exptl_crystal_size_min          0.042
_refine_diff_density_max         2.519
_refine_diff_density_min         -1.805
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2156
_refine_ls_number_reflns         32295
_refine_ls_number_restraints     1102
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0619
_refine_ls_R_factor_gt           0.0417
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.03P)^2^+69.P], P=(max(Fo^2^,0)+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0902
_refine_ls_wR_factor_ref         0.0961
_reflns_number_gt                24639
_reflns_number_total             32295
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja3018797_si_001.cif
_cod_data_source_block           1897
_cod_original_cell_volume        18426(3)
_cod_database_code               4118046
_diffrn_measurement_frame_width-ccd -0.30
_diffrn_measurement_total_frames-ccd 1604
_diffrn_measurement_frame_time-ccd 40
_diffrn_measurement_total_time-ccd 20.5
_diffrn_detector_distance-ccd    6.000
_diffrn_measurement_frame_size-ccd 1024