Host guest chemistry of a bidentate silyl-triflate bis-Lewis-acid – complex complexation behaviour unravelled by diffusion NMR spectroscopy
Schäfer, Fabian; Mix, Andreas; Cati, Ninive; Lamm, Jan-Hendrik; Neumann, Beate; Stammler, Georg; Mitzel, Norbert Werner; Dalton Transactions  (2022) –; doi:10.1039/D2DT00583B

data_7710043
_publ_section_title
;
 Host guest chemistry of a bidentate silyl-triflate bis-Lewis-acid --
 complex complexation behaviour unravelled by diffusion NMR spectroscopy
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT00583B
_journal_year                    2022
_chemical_formula_moiety         'C20 H36 N2 Si3, 2(C F3 O3 S), C H2 Cl2'
_chemical_formula_sum            'C23 H38 Cl2 F6 N2 O6 S2 Si3'
_chemical_formula_weight         771.84
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-08-06
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_audit_update_record
;
2021-04-30 deposited with the CCDC.	2022-04-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 113.808(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   25.5005(7)
_cell_length_b                   10.5126(2)
_cell_length_c                   29.3823(7)
_cell_measurement_reflns_used    12519
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      76.3090
_cell_measurement_theta_min      3.2440
_cell_volume                     7206.4(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_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_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3114
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -115.00  -5.00   1.00    1.00    --  -38.50 -19.00-150.00  110
  2  \w    -50.00  -6.00   1.00    1.00    --  -38.50 125.00 120.00   44
  3  \w    -46.00  33.00   1.00    1.00    --  -38.50  38.00  30.00   79
  4  \w     56.00  81.00   1.00    1.00    --   42.70 -99.00 120.00   25
  5  \w      6.00  32.00   1.00    1.00    --   42.70 -99.00 120.00   26
  6  \w     40.00  86.00   1.00    1.00    --   42.70-125.00 120.00   46
  7  \w     41.00  92.00   1.00    1.00    --   42.70-125.00 -60.00   51
  8  \w     45.00  83.00   1.00    3.00    --  111.00 -45.00-150.00   38
  9  \w     52.00 107.00   1.00    3.00    --  111.00 -94.00  60.00   55
 10  \w     44.00 121.00   1.00    3.00    --  111.00 -61.00  60.00   77
 11  \w     79.00 125.00   1.00    3.00    --  111.00 -61.00 -90.00   46
 12  \w    113.00 150.00   1.00    3.00    --  111.00  45.00 150.00   37
 13  \w     44.00  70.00   1.00    3.00    --  111.00-125.00 150.00   26
 14  \w     94.00 131.00   1.00    3.00    --  111.00 -45.00-150.00   37
 15  \w     47.00  84.00   1.00    3.00    --  111.00-125.00-120.00   37
 16  \w     37.00 102.00   1.00    3.00    --  111.00 -94.00-120.00   65
 17  \w     88.00 113.00   1.00    3.00    --  111.00-125.00-180.00   25
 18  \w     36.00 149.00   1.00    3.00    --  111.00 -15.00 120.00  113
 19  \w     43.00  69.00   1.00    3.00    --  111.00-125.00-180.00   26
 20  \w     77.00 106.00   1.00    3.00    --  111.00 -94.00   0.00   29
 21  \w     90.00 176.00   1.00    3.00    --  111.00  30.00 120.00   86
 22  \w     88.00 113.00   1.00    3.00    --  111.00-125.00 150.00   25
 23  \w     38.00 132.00   1.00    3.00    --  111.00 -30.00 -60.00   94
 24  \w     38.00  63.00   1.00    3.00    --  111.00 -94.00-180.00   25
 25  \w     66.00 107.00   1.00    3.00    --  111.00 -94.00-180.00   41
 26  \w     35.00 107.00   1.00    3.00    --  111.00-102.00 -49.46   72
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0525420500
_diffrn_orient_matrix_UB_12      0.0887148500
_diffrn_orient_matrix_UB_13      -0.0193451000
_diffrn_orient_matrix_UB_21      -0.0377180500
_diffrn_orient_matrix_UB_22      -0.1082928500
_diffrn_orient_matrix_UB_23      0.0055231000
_diffrn_orient_matrix_UB_31      0.0133359000
_diffrn_orient_matrix_UB_32      0.0431520000
_diffrn_orient_matrix_UB_33      0.0536485000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0326
_diffrn_reflns_av_unetI/netI     0.0262
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            29113
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.448
_diffrn_reflns_theta_min         3.288
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.283
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.729
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.82a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.423
_exptl_crystal_description       block
_exptl_crystal_F_000             3200
_exptl_crystal_size_max          0.208
_exptl_crystal_size_mid          0.184
_exptl_crystal_size_min          0.102
_refine_diff_density_max         0.842
_refine_diff_density_min         -0.819
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     432
_refine_ls_number_reflns         7471
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0677
_refine_ls_R_factor_gt           0.0615
_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^)+(0.0736P)^2^+27.4795P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1638
_refine_ls_wR_factor_ref         0.1691
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6621
_reflns_number_total             7471
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00583b2.cif
_cod_data_source_block           compound_2_2Py
_cod_database_code               7710043
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C23H38Cl2F6N2O6S2Si3
_diffrn_oxdiff_digest_frames
;
0101830bfa2898784e6343c3eb8e371a9901391a08b
;
_diffrn_oxdiff_digest_hkl
;
018b5c1049b8d01f5dd8842a33301e25b2327a
;
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.98
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Cl2B-C23B \\sim Cl1A-C23A \\sim Cl2A-C23A \\sim Cl1B-C23B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C23B) = Uanis(C23A)
Uanis(O4B) = Uanis(O4A)
Uanis(O6B) = Uanis(O6A)
Uanis(O5A) = Uanis(O5B)
Uanis(F4A) = Uanis(F4B)
Uanis(F5B) = Uanis(F5A)
Uanis(F6A) = Uanis(F6B)
Uanis(Cl2A) = Uanis(Cl1B)
Uanis(Cl2B) = Uanis(Cl1A)
4. Others
 Sof(Cl1B)=Sof(Cl2B)=Sof(C23B)=Sof(H23C)=Sof(H23D)=1-FVAR(1)
 Sof(Cl1A)=Sof(Cl2A)=Sof(C23A)=Sof(H23A)=Sof(H23B)=FVAR(1)
 Sof(F4B)=Sof(F5B)=Sof(F6B)=Sof(O4B)=Sof(O5B)=Sof(O6B)=1-FVAR(2)
 Sof(F4A)=Sof(F5A)=Sof(F6A)=Sof(O4A)=Sof(O5A)=Sof(O6A)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B), C7(H7A,H7B), C8(H8A,H8B), C23A(H23A,H23B),
 C23B(H23C,H23D)
5.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C12(H12), C13(H13), C14(H14), C15(H15), C16(H16), C17(H17),
 C18(H18), C19(H19), C20(H20)
5.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C9(H9A,
 H9B,H9C), C10(H10A,H10B,H10C)
;
_shelx_res_checksum              27459
_olex2_date_sample_data_collection 2020-08-06
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.230
_oxdiff_exptl_absorpt_empirical_full_min 0.813