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_1543617
_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_absolute_configuration ad
_chemical_formula_sum            'C48 H60 K2 N8 O7.5 Se6 Sn2'
_chemical_formula_weight         1658.38
_chemical_name_systematic        '[K2(DMF)3][Se6Sn2(mBDCA-5t)]'
_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'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/6
_audit_update_record
;
2016-03-20 deposited with the CCDC.
2016-07-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 113.704(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.2183(19)
_cell_length_b                   18.536(3)
_cell_length_c                   16.295(2)
_cell_measurement_reflns_used    9910
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.20
_cell_volume                     3655.7(9)
_computing_cell_refinement       'SAINT 7.46A (Bruker-AXS, 2015)'
_computing_data_collection       'APEX2 v2011.4.0 (Bruker-AXS, 2015)'
_computing_data_reduction        'SAINT 7.46A (Bruker-AXS, 2015)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2015 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0807
_diffrn_reflns_av_unetI/netI     0.0766
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            62975
_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         26.372
_diffrn_reflns_theta_min         1.365
_diffrn_source
'I\mS micro-focus sealed tube, multilayer optics'
_exptl_absorpt_coefficient_mu    3.828
_exptl_absorpt_correction_T_max  0.1524
_exptl_absorpt_correction_T_min  0.1025
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2009)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.507
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1612
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.030
_refine_diff_density_max         1.928
_refine_diff_density_min         -1.128
_refine_diff_density_rms         0.179
_refine_ls_abs_structure_details
; 
 Refined as an inversion twin. 
;
_refine_ls_abs_structure_Flack   0.27(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1264
_refine_ls_number_reflns         14765
_refine_ls_number_restraints     5504
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.1017
_refine_ls_R_factor_gt           0.0718
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1252P)^2^+10.9744P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1873
_refine_ls_wR_factor_ref         0.2100
_reflns_Friedel_coverage         0.938
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                10913
_reflns_number_total             14765
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6sc01754a2.cif
_cod_data_source_block           x13160_sq
_cod_original_formula_sum        'C48 H60 K2 N8 O7.50 Se6 Sn2'
_cod_database_code               1543617
_shelx_estimated_absorpt_t_min   0.546
_shelx_estimated_absorpt_t_max   0.894
_shelxl_version_number           2014/6
_shelx_res_checksum              95182
_shelx_fab_checksum              95353
_solvent_exptl_crystal_recrystallization_method 'DMF, Et2O'