Crystal structure of a mixed-valence μ-oxide Sn~12~ cluster
Kireenko, Marina M.; Zaitsev, Kirill V.; Karlov, Sergey S.; Egorov, Mikhail P.; Churakov, Andrei V.; Acta Crystallographica Section E 70 (2014) m378–m379; doi:10.1107/S1600536814023460

data_2240143
_publ_section_title
;
 Crystal structure of a mixed-valence \m-oxide Sn~12~ cluster
;
_journal_coeditor_code           RZ5135
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m378
_journal_page_last               m379
_journal_paper_doi               10.1107/S1600536814023460
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac
'[Mo2 Sn12 (C33 H27 N O2)4 O10 (C O)10], 7C7 H8'
_chemical_formula_moiety         'C142 H108 Mo2 N4 O28 Sn12, 7(C7 H8)'
_chemical_formula_sum            'C191 H164 Mo2 N4 O28 Sn12'
_chemical_formula_weight         4579.42
_chemical_name_systematic
;Decacarbonyltetra-\m~4~-oxido-hexa-\m~3~-oxido-tetrakis[\m-2,2'-(pyridine-2,6-diyl)bis(1,1-diphenylethanolato)]
decatin(II)ditin(IV)dimolybdenum(O)(2 <i>Mo</i>---<i>Sn</i>) toluene
heptasolvate
;
_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                94.833(2)
_cell_angle_beta                 95.014(2)
_cell_angle_gamma                110.605(2)
_cell_formula_units_Z            1
_cell_length_a                   15.8218(17)
_cell_length_b                   15.9933(17)
_cell_length_c                   18.806(2)
_cell_measurement_reflns_used    9901
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      30.484
_cell_measurement_theta_min      2.372
_cell_volume                     4403.4(8)
_computing_cell_refinement
;
SAINT (Bruker, 2008)
;
_computing_data_collection
;
<i>APEX2</i> (Bruker, 2008)
;
_computing_data_reduction
;
SAINT (Bruker, 2008)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXTL (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXTL (Sheldrick, 2008)
;
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker SMART APEX II'
_diffrn_measurement_method       \w
_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  0.0282
_diffrn_reflns_av_sigmaI/netI    0.0410
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            32165
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         2.28
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.876
_exptl_absorpt_correction_T_max  0.8644
_exptl_absorpt_correction_T_min  0.6513
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2008)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.727
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2246
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.053
_refine_diff_density_min         -0.861
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     939
_refine_ls_number_reflns         15393
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0428
_refine_ls_R_factor_gt           0.0325
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0327P)^2^+7.0359P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0757
_refine_ls_wR_factor_ref         0.0813
_reflns_number_gt                12647
_reflns_number_total             15393
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            rz5135sup1.cf
_cod_data_source_block           I
_cod_original_cell_volume        4403.5(8)
_cod_database_code               2240143
_cod_database_fobs_code          2240143