Effect of the cation on the stability of cation-glyme complexes and their interactions with the [TFSA]- anion
Tsuzuki, Seiji; MANDAI, Toshihiko; Suzuki, Soma; Shinoda, Wataru; Nakamura, Takenobu; Morishita, Tetsuya; Ueno, Kazuhide; Seki, Shiro; Umebayashi, Yasuhiro; Dokko, Kaoru; Watanabe, Masayoshi; Phys. Chem. Chem. Phys.  (2017) –; doi:10.1039/C7CP02779F

data_7228639
_publ_section_title
;
 Effect of the cation on the stability of cation-glyme complexes and their
 interactions with the [TFSA]- anion
;
_journal_name_full               'Phys. Chem. Chem. Phys.'
_journal_paper_doi               10.1039/C7CP02779F
_journal_year                    2017
_chemical_formula_moiety         'C12 H18 F12 Mg N2 O12 S4'
_chemical_formula_sum            'C12 H18 F12 Mg N2 O12 S4'
_chemical_formula_weight         762.83
_chemical_properties_physical    ', Hygroscopic'
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-03-01
_audit_creation_method
;
Olex2 1.2
(compiled 2017.02.23 svn.r3390 for OlexSys, GUI svn.r5320)
;
_audit_update_record
;
2017-04-04 deposited with the CCDC.
2017-07-05 downloaded from the CCDC.
;
_cell_angle_alpha                97.006(5)
_cell_angle_beta                 95.727(4)
_cell_angle_gamma                100.012(5)
_cell_formula_units_Z            1
_cell_length_a                   8.7021(4)
_cell_length_b                   9.1183(6)
_cell_length_c                   9.2356(5)
_cell_measurement_reflns_used    3130
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      29.8540
_cell_measurement_theta_min      3.6060
_cell_volume                     710.77(7)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_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      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.860
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \f    -80.00 100.00   0.50    6.00   0.00  20.00   0.00    --   360
  2  \w    -20.00  28.00   0.50    6.00    --   20.00 -90.00   0.00   96
  3  \w    -20.00  28.00   0.50    6.00    --   20.00 -90.00  90.00   96
  4  \w    -20.00  28.00   0.50    6.00    --   20.00 -90.00 180.00   96
  5  \w    -20.00  28.00   0.50    6.00    --   20.00 -90.00 270.00   96
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0467212000
_diffrn_orient_matrix_UB_12      -0.0614739000
_diffrn_orient_matrix_UB_13      -0.0484685000
_diffrn_orient_matrix_UB_21      -0.0355937000
_diffrn_orient_matrix_UB_22      0.0507850000
_diffrn_orient_matrix_UB_23      -0.0382495000
_diffrn_orient_matrix_UB_31      0.0592258000
_diffrn_orient_matrix_UB_32      0.0031961000
_diffrn_orient_matrix_UB_33      -0.0476273000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0376
_diffrn_reflns_av_unetI/netI     0.0560
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.860
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5938
_diffrn_reflns_point_group_measured_fraction_full 0.599
_diffrn_reflns_point_group_measured_fraction_max 0.497
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.190
_diffrn_reflns_theta_min         3.425
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.491
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70935
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.782
_exptl_crystal_description       plate
_exptl_crystal_F_000             384
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.409
_refine_diff_density_min         -0.410
_refine_diff_density_rms         0.068
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.05(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.891
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     390
_refine_ls_number_reflns         4187
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.890
_refine_ls_R_factor_all          0.0573
_refine_ls_R_factor_gt           0.0473
_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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1163
_refine_ls_wR_factor_ref         0.1294
_reflns_Friedel_coverage         0.156
_reflns_Friedel_fraction_full    0.217
_reflns_Friedel_fraction_max     0.134
_reflns_number_gt                3649
_reflns_number_total             8422
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cp02779f2.cif
_cod_data_source_block           160721_mgg3tfsa
_cod_database_code               7228639
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C12H18F12Mg1N2O12S4
_reflns_odcompleteness_completeness 85.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.12
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B)
2.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C8(H8A,H8B,H8C)
;
_shelx_res_checksum              9372
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.554
_oxdiff_exptl_absorpt_empirical_full_min 0.546