Ionic liquid cations as methylation agent for extremely weak chalcogenido metalate nucleophiles
Dehnen, Stefanie Susanne; Peters, Bertram; Santner, Silke; Donsbach, Carsten; Smarsly, Bernd; Voepel, Pascal; Chemical Science  (2019) –; doi:10.1039/C9SC01358J

data_1550921
_publ_section_title
;
 Ionic liquid cations as methylation agent for extremely weak chalcogenido
 metalate nucleophiles
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C9SC01358J
_journal_year                    2019
_chemical_formula_moiety
'0.08(C20 H60 O40 S200 Sn100), 0.17(C4 H12 O4 S20 Sn10), 0.33(C5 H5 N2), 0.33(C3 H2 N2)'
_chemical_formula_sum            'C5 H9.33 N1.33 O4 S20 Sn10'
_chemical_formula_weight         1980.24
_space_group_crystal_system      tetragonal
_space_group_IT_number           120
_space_group_name_Hall           'I -4 -2c'
_space_group_name_H-M_alt        'I -4 c 2'
_symmetry_space_group_name_Hall  'I -4 -2c'
_symmetry_space_group_name_H-M   'I -4 c 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-03-06
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-03-13 deposited with the CCDC.    2019-04-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            24
_cell_length_a                   29.1874(4)
_cell_length_b                   29.1874(4)
_cell_length_c                   57.5222(14)
_cell_measurement_reflns_used    575
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      36.74
_cell_measurement_theta_min      6.87
_cell_volume                     49003.4(15)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Stoe StadiVari'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_R_equivalents  0.1785
_diffrn_reflns_av_unetI/netI     0.0954
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            44492
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        39.990
_diffrn_reflns_theta_max         39.990
_diffrn_reflns_theta_min         2.635
_exptl_absorpt_coefficient_mu    28.764
_exptl_absorpt_correction_T_max  0.1595
_exptl_absorpt_correction_T_min  0.0547
_exptl_absorpt_correction_type   sphere
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.610
_exptl_crystal_description       block
_exptl_crystal_F_000             21616
_exptl_crystal_size_max          0.157
_exptl_crystal_size_mid          0.139
_exptl_crystal_size_min          0.1
_exptl_crystal_size_rad          0.078
_refine_diff_density_max         0.880
_refine_diff_density_min         -0.692
_refine_diff_density_rms         0.155
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.86(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     505
_refine_ls_number_reflns         7341
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0757
_refine_ls_R_factor_gt           0.0650
_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^)+(0.1289P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1687
_refine_ls_wR_factor_ref         0.1776
_reflns_Friedel_coverage         0.886
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                6030
_reflns_number_total             7341
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc01358j2.cif
_cod_data_source_block           ed086b_pl_sq
_cod_original_cell_volume        49003.4(18)
_cod_database_code               1550921
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.161
_shelx_estimated_absorpt_t_min   0.093
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.14(3)
 0.86(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(S1A) = Uanis(S7A)
4. Others
 Fixed Sof: C25(0.5) N32(0.5) C12(0.5) H12(0.5) C6AA(0.5) H6AA(0.5) N9(0.5)
 C15(0.5) N13(0.5) C2AA(0.5) H2AA(0.5) C8(0.5) H8(0.5) N1AA(0.5) C3(0.5)
 C33(0.5) H33A(0.5) H33B(0.5) H33C(0.5) C10(0.5) H10A(0.5) H10B(0.5) H10C(0.5)
5.a Me refined with riding coordinates:
 C33(H33A,H33B,H33C), C10(H10A,H10B,H10C)
5.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C6AA(H6AA), C2AA(H2AA), C8(H8)
5.c Fitted pentagon refined as free rotating group:
 C25(N32,C12,C6AA,N9), N13(C2AA,C8,N1AA,C3)
5.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C14(H14A,H14B,H14C), C40(H40A,H40B,H40C)
;
_shelx_res_checksum              12446
_shelx_fab_checksum              43908
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'