Sn12O8(OH)4(OEt)28(HOEt)4: an Additional Member in the Family of Dodecameric Oxo Clusters
François Ribot; Eugenia Martínez-Ferrero; Kamal Boubekeur; Peter M. S. Hendrickx; Jose C. Martins; Luk Van Lokeren; Rudolph Willem; Monique Biesemans; Inorganic Chemistry 47 (2008) 5831–5840; doi:10.1021/ic800123z

data_4305261
_publ_contact_author
;
Francois Ribot
UPMC Univ Paris 06, UMR CNRS 7574, CMCP
Tour 54, 5e etage
4, place Jussieu - 75252 PARIS cedex 05 - FRANCE
;
_publ_contact_author_email       francois.ribot@courriel.upmc.fr
_publ_contact_author_fax         '(33) 1 4427 4769'
_publ_contact_author_phone       '(33) 1 4427 4135'
_publ_section_title
;
Sn12O8(OH)4(OEt)28(HOEt)4: an Additional Member in the Family of
Dodecameric Oxo Clusters
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5831
_journal_page_last               5840
_journal_paper_doi               10.1021/ic800123z
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'C64 H166 O44 Sn12'
_chemical_formula_sum            'C64 H166 O44 Sn12'
_chemical_formula_weight         3064.24
_chemical_name_systematic
;
 ?
;
_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                93.83(8)
_cell_angle_beta                 102.77(6)
_cell_angle_gamma                104.39(4)
_cell_formula_units_Z            1
_cell_length_a                   11.979(6)
_cell_length_b                   13.562(8)
_cell_length_c                   18.618(9)
_cell_measurement_reflns_used    32
_cell_measurement_temperature    250(2)
_cell_measurement_theta_max      9.44
_cell_measurement_theta_min      3.36
_cell_volume                     2833(3)
_computing_cell_refinement
'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1999)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      250(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_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  0.0597
_diffrn_reflns_av_sigmaI/netI    0.0769
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            56695
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.05
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.667
_exptl_absorpt_correction_T_max  0.819
_exptl_absorpt_correction_T_min  0.542
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.796
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate-like
_exptl_crystal_F_000             1502
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.805
_refine_diff_density_min         -1.425
_refine_diff_density_rms         0.289
_refine_ls_extinction_coef       0.0018(5)
_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   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     506
_refine_ls_number_reflns         16410
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.1279
_refine_ls_R_factor_gt           0.0684
_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^)+(0.1603P)^2^+5.2716P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0809
_refine_ls_wR_factor_ref         0.1342
_reflns_number_gt                9119
_reflns_number_total             16410
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic800123z-file013.cif
_cod_data_source_block           fra24blt
_cod_original_cell_volume        2834(3)
_cod_database_code               4305261