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_1550917
_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         '2(O2 S10 Sn5)'
_chemical_formula_sum            'O4 S20 Sn10'
_chemical_formula_weight         1892.10
_space_group_crystal_system      cubic
_space_group_IT_number           227
_space_group_name_Hall           '-F 4vw 2vw 3'
_space_group_name_H-M_alt        'F d -3 m'
_symmetry_space_group_name_Hall  '-F 4vw 2vw 3'
_symmetry_space_group_name_H-M   'F d -3 m :2'
_atom_sites_solution_primary     dual
_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            8
_cell_length_a                   27.248(3)
_cell_length_b                   27.248(3)
_cell_length_c                   27.248(3)
_cell_measurement_reflns_used    148
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      19.4
_cell_measurement_theta_min      2.08
_cell_volume                     20230(4)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Stoe IPDS-2'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1198
_diffrn_reflns_av_unetI/netI     0.0486
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            2622
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        17.977
_diffrn_reflns_theta_max         17.977
_diffrn_reflns_theta_min         2.114
_exptl_absorpt_coefficient_mu    2.842
_exptl_absorpt_correction_T_max  0.7667
_exptl_absorpt_correction_T_min  0.6250
_exptl_absorpt_correction_type   sphere
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.242
_exptl_crystal_description       octahedral
_exptl_crystal_F_000             6816
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_exptl_crystal_size_rad          0.0363
_refine_diff_density_max         0.550
_refine_diff_density_min         -1.456
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     21
_refine_ls_number_reflns         368
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0887
_refine_ls_R_factor_gt           0.0543
_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^)+(0.0344P)^2^+890.8331P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1127
_refine_ls_wR_factor_ref         0.1205
_reflns_Friedel_coverage         0.000
_reflns_number_gt                213
_reflns_number_total             368
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc01358j2.cif
_cod_data_source_block           bp009a
_cod_original_cell_volume        20230(7)
_cod_database_code               1550917
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.871
_shelx_estimated_absorpt_t_min   0.805
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Uanis(S2) = Uanis(S1)
;
_shelx_res_checksum              58695
_shelx_fab_checksum              82271
_olex2_submission_special_instructions 'No special instructions were received'