Synthesis of organic (trimethylsilyl)chalcogenolate salts Cat[TMS-E] (E = S, Se, Te): the methylcarbonate anion as a desilylating agent.
Finger, Lars H.; Scheibe, Benjamin; Sundermeyer, Jörg; Inorganic chemistry 54 (2015) 9568–9575; doi:10.1021/acs.inorgchem.5b01665

data_4346552
_publ_section_title
;
 Synthesis of organic (trimethylsilyl)chalcogenolate salts Cat[TMS-E] (E =
 S, Se, Te): the methylcarbonate anion as a desilylating agent.
;
_journal_issue                   19
_journal_name_full               'Inorganic chemistry'
_journal_page_first              9568
_journal_page_last               9575
_journal_paper_doi               10.1021/acs.inorgchem.5b01665
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C6 H14 N, C3 H9 Se Si'
_chemical_formula_sum            'C9 H23 N Se Si'
_chemical_formula_weight         252.33
_chemical_name_common            '[DMPyr][TMS-Se], 5'
_chemical_name_systematic
;
N,N-Dimethylpyrrolidinium-trimethylsilylselenolate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90.166(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.2500(8)
_cell_length_b                   10.8215(7)
_cell_length_c                   19.3331(12)
_cell_measurement_reflns_used    1490
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.2466
_cell_measurement_theta_min      2.6907
_cell_volume                     2562.9(3)
_computing_cell_refinement
;
Bruker: APEX2 v2013.10-0, Bruker AXS Inc., 
Madison, Wisconsin, USA, 2012.
;
_computing_data_collection
;
Bruker: Bruker Instrument Service v3.0.26, Bruker AXS Inc., 
Madison, Wisconsin, USA, 2012.
;
_computing_data_reduction
;
Bruker: SAINT V8.27B, Bruker AXS Inc., 
Madison, Wisconsin, USA, 2012.
;
_computing_molecular_graphics
;
Mercury (C. F. Macrae, P. R. Edgington, P. McCabe, E. Pidcock, G. P. 
Shields, R. Taylor, M. Towler, 
J. van de Streek, J. Appl. Cryst. 2006,  39, 453-457.)
Ortep-3 for Windows (L.J. Farrugia, J. Appl. Cryst. 2012, 45, 849-854)
DIAMOND 4 (H. Putz, K. Brandenburg, Crystal Impact GbR, Kreuzherrenstr. 
102, 53227 Bonn, Germany)
;
_computing_publication_material
;
WinGX 2014.1 (L.J. Farrugia, J. Appl. Cryst. 2012, 45, 849-854)
enCIFer (F. H. Allen, O. Johnson, G. P. Shields, B. R. Smith, M. Towler,
 J. Appl. Cryst. 2004, 37, 335-338.)
;
_computing_structure_refinement
;
SHELXL-2014/7 (G. M. Sheldrick, Acta Cryst. A 2008, 64, 112-122)
;
_computing_structure_solution
;
SIR2011 (M. C. Burla, R. Caliandro, M. Camalli, B. Carrozzini,
G. L. Cascarano, C. Giacovazzo, M. Mallamo, A. Mazzone, G. Polidori, 
R. Spagna, J. Appl. Cryst. 2012, 45, 357-361)
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'D8 Quest (Bruker AXS Inc.)'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0730
_diffrn_reflns_av_unetI/netI     0.0361
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            38995
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.374
_diffrn_reflns_theta_min         2.157
_diffrn_source                   'I\mS Microfocus Source'
_exptl_absorpt_coefficient_mu    2.983
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6204
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.308
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.521
_refine_diff_density_min         -0.550
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     228
_refine_ls_number_reflns         4683
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.117
_refine_ls_R_factor_all          0.0360
_refine_ls_R_factor_gt           0.0306
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0284P)^2^+2.3901P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0674
_refine_ls_wR_factor_ref         0.0692
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4335
_reflns_number_total             4683
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b01665_si_001.cif
_cod_data_source_block           FINJG11
_cod_depositor_comments
;

2020-08-14
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_moiety
;
 2(C6 H14 N), 2(C3 H9 Se Si)
;
_cod_original_formula_sum        'C18 H46 N2 Se2 Si2'
_cod_original_formula_units_Z    4
_cod_original_formula_weight     504.67
_cod_database_code               4346552
_audit_contact_author            'Joerg Sundermeyer'
_shelx_shelxl_version_number     2014/7
_exptl_absorpt_special_details
;
Bruker: SADABS v2012/1, Bruker AXS Inc., 
Madison, Wisconsin, USA, 2012.
;
_shelx_res_checksum              23983
_shelx_hkl_checksum              48596