Multi-electron reactivity of a cofacial di-tin(II) cryptand: Partial reduction of sulfur and selenium and reversible generation of S3●−
Stauber, Julia; Mueller, Peter; Dai, Yizhe; Wu, Gang; Nocera, Daniel G.; Cummins, Christopher; Chem. Sci.  (2016) –; doi:10.1039/C6SC01754A

data_1543616
_publ_section_title
;
 Multi-electron reactivity of a cofacial di-tin(II) cryptand: Partial
 reduction of sulfur and selenium and reversible generation of
 S3&#x25CF;&#x2212;
;
_journal_name_full               'Chem. Sci.'
_journal_paper_doi               10.1039/C6SC01754A
_journal_year                    2016
_chemical_formula_sum            'C84 H132 K2 N12 O18 Sn2'
_chemical_formula_weight         1913.59
_chemical_name_systematic        '[K(Kryptofix-2,2,2]2[Sn2(mBDCA-5t)]'
_space_group_crystal_system      hexagonal
_space_group_IT_number           176
_space_group_name_Hall           '-P 6c'
_space_group_name_H-M_alt        'P 63/m'
_symmetry_space_group_name_Hall  '-P 6c'
_symmetry_space_group_name_H-M   'P 63/m'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-03-26 deposited with the CCDC.
2016-07-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   13.1963(19)
_cell_length_b                   13.1963(19)
_cell_length_c                   29.806(5)
_cell_measurement_reflns_used    9780
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.56
_cell_measurement_theta_min      2.25
_cell_volume                     4495.1(12)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Smart APEX2 CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0604
_diffrn_reflns_av_unetI/netI     0.0181
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            186032
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.504
_diffrn_reflns_theta_min         1.366
_diffrn_source
'I\mS micro-focus sealed tube, multilayer optics'
_exptl_absorpt_coefficient_mu    0.723
_exptl_absorpt_correction_T_max  0.6483
_exptl_absorpt_correction_T_min  0.5888
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2009)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.420
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2012
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.257
_exptl_crystal_size_mid          0.177
_exptl_crystal_size_min          0.086
_refine_diff_density_max         1.307
_refine_diff_density_min         -1.035
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     274
_refine_ls_number_reflns         5098
_refine_ls_number_restraints     546
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0481
_refine_ls_R_factor_gt           0.0372
_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^)+(0.0490P)^2^+4.9624P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0931
_refine_ls_wR_factor_ref         0.1008
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4179
_reflns_number_total             5098
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6sc01754a2.cif
_cod_data_source_block           Sn2
_cod_original_cell_volume        4495.0(15)
_cod_database_code               1543616
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.836
_shelx_estimated_absorpt_t_max   0.940
_shelx_res_checksum              40178
_solvent_exptl_crystal_recrystallization_method DMF/Et2O