Hexanuclear tin(ii) and mixed valence tin(ii,iv) oxide clusters within polyoxometalates.
Suzuki, Kosuke; Hanaya, Takumi; Sato, Rinta; Minato, Takuo; Yamaguchi, Kazuya; Mizuno, Noritaka; Chemical communications (Cambridge, England) 52 (2016) 10688–10691; doi:10.1039/c6cc05284c

data_7124875
_publ_section_title
;
 Hexanuclear tin(ii) and mixed valence tin(ii,iv) oxide clusters within
 polyoxometalates.
;
_journal_issue                   70
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              10688
_journal_page_last               10691
_journal_paper_doi               10.1039/c6cc05284c
_journal_volume                  52
_journal_year                    2016
_chemical_formula_sum            'C124 Cl12 N7 O73 Si2 Sn6 W18'
_chemical_formula_weight         7258.33
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   none
_audit_creation_method           SHELXL-2014/6
_audit_update_record
;
2016-06-20 deposited with the CCDC.
2016-08-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 115.1216(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   18.75170(10)
_cell_length_b                   28.4384(3)
_cell_length_c                   21.5390(2)
_cell_measurement_reflns_used    26128
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      29.483
_cell_measurement_theta_min      1.895
_cell_volume                     10399.59(16)
_computing_cell_refinement       HKL2000
_computing_data_collection       'Rigaku CrystalClear'
_computing_data_reduction        HKL2000
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      113(2)
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  CCD
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_unetI/netI     0.0278
_diffrn_reflns_Laue_measured_fraction_full 0.967
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_number            28615
_diffrn_reflns_point_group_measured_fraction_full 0.494
_diffrn_reflns_point_group_measured_fraction_max 0.495
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         29.483
_diffrn_reflns_theta_min         1.895
_exptl_absorpt_coefficient_mu    10.850
_exptl_absorpt_correction_T_max  0.337
_exptl_absorpt_correction_T_min  0.093
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'HKL2000 DENZO SCALEPACK'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.318
_exptl_crystal_description       plate
_exptl_crystal_F_000             6482
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         4.140
_refine_diff_density_min         -4.874
_refine_diff_density_rms         0.274
_refine_ls_abs_structure_details
;
No quotients, so Flack parameter determined by classical intensity fit
;
_refine_ls_abs_structure_Flack   0.069(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1340
_refine_ls_number_reflns         28615
_refine_ls_number_restraints     221
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0875
_refine_ls_R_factor_gt           0.0724
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+160.6876P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1845
_refine_ls_wR_factor_ref         0.2046
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    0.000
_reflns_Friedel_fraction_max     0.000
_reflns_number_gt                24462
_reflns_number_total             28615
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc05284c2.cif
_cod_data_source_block           I
_cod_original_cell_volume        10399.58(16)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7124875
_shelx_estimated_absorpt_t_min   0.410
_shelx_estimated_absorpt_t_max   0.410
_shelxl_version_number           2014/6
_shelx_res_checksum              96893
_shelx_hkl_checksum              32867