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_1550918
_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         '1(O4 S20 Sn10)'
_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'
_audit_creation_date             2019-02-21
_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            136
_cell_length_a                   73.6160(17)
_cell_length_b                   73.6160(17)
_cell_length_c                   73.6160(17)
_cell_measurement_reflns_used    1748
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.395
_cell_measurement_theta_min      11.625
_cell_volume                     398948(16)
_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 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Stoe StadiVari'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_R_equivalents  0.1740
_diffrn_reflns_av_unetI/netI     0.1508
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       77
_diffrn_reflns_limit_h_min       -74
_diffrn_reflns_limit_k_max       75
_diffrn_reflns_limit_k_min       -46
_diffrn_reflns_limit_l_max       64
_diffrn_reflns_limit_l_min       -86
_diffrn_reflns_number            171427
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        64.986
_diffrn_reflns_theta_max         64.986
_diffrn_reflns_theta_min         7.612
_exptl_absorpt_coefficient_mu    19.998
_exptl_absorpt_correction_T_max  0.0163
_exptl_absorpt_correction_T_min  0.0013
_exptl_absorpt_correction_type   sphere
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.071
_exptl_crystal_description       octahedral
_exptl_crystal_F_000             115872
_exptl_crystal_size_max          0.174
_exptl_crystal_size_mid          0.137
_exptl_crystal_size_min          0.116
_exptl_crystal_size_rad          0.086
_refine_diff_density_max         0.491
_refine_diff_density_min         -0.470
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.643
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     261
_refine_ls_number_reflns         15027
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.643
_refine_ls_R_factor_all          0.0942
_refine_ls_R_factor_gt           0.0353
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0178P)^2^+0.0092P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0582
_refine_ls_wR_factor_ref         0.0609
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4134
_reflns_number_total             15027
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc01358j2.cif
_cod_data_source_block           bp079e
_cod_original_cell_volume        398948(28)
_cod_database_code               1550918
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.205
_shelx_estimated_absorpt_t_min   0.129
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Uanis(S3A) = Uanis(S4A)
;
_shelx_res_checksum              14697
_shelx_fab_checksum              10150
_olex2_submission_special_instructions 'No special instructions were received'