Stereoselective synthesis of different cyclic tetrasiloxane isomers depending on the superacid catalyst employed.
Sonoda, Kanako; Tohnai, Norimitsu; Kaneko, Yoshiro; Dalton transactions (Cambridge, England : 2003) 53 (2024) 8709–8715; doi:10.1039/d4dt00062e

data_7715920
_publ_section_title
;
 Stereoselective synthesis of different cyclic tetrasiloxane isomers
 depending on the superacid catalyst employed.
;
_journal_issue                   20
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8709
_journal_page_last               8715
_journal_paper_doi               10.1039/d4dt00062e
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C18 H38 N2 O6 Si2'
_chemical_formula_sum            'C18 H38 N2 O6 Si2'
_chemical_formula_weight         434.68
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2024-03-07
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2024-03-09 deposited with the CCDC.	2024-04-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.5930(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.2917(2)
_cell_length_b                   14.8352(2)
_cell_length_c                   9.99670(10)
_cell_measurement_reflns_used    6577
_cell_measurement_temperature    213.00
_cell_measurement_theta_max      74.0730
_cell_measurement_theta_min      3.8810
_cell_volume                     2563.42(5)
_computing_cell_refinement       'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      213.00
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.961
_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    -85.00 -55.00   0.50    0.76    --    0.00 -37.00   0.00   60
  2  \w    -88.00  18.00   0.50    0.76    --    0.00 -19.00-120.00  212
  3  \w     33.00  59.00   0.50    0.76    --    0.00  37.00 -90.00   52
  4  \w    -18.00  14.00   0.50    0.76    --    0.00 -37.00   0.00   64
  5  \w     76.00 103.00   0.50    3.02    --   94.90  45.00  30.00   54
  6  \w    122.00 166.00   0.50    3.02    --   94.90  45.00  30.00   88
  7  \w     75.00 169.00   0.50    3.02    --   94.90  45.00  60.00  188
  8  \w      6.00 118.00   0.50    3.02    --   94.90 -61.00 -60.00  224
  9  \w     34.00  73.00   0.50    3.02    --   94.90 -77.00 -90.00   78
 10  \w     13.00  46.00   0.50    3.02    --   94.90 -77.00   0.00   66
 11  \w     66.00  91.00   0.50    3.02    --   94.90 -77.00   0.00   50
 12  \w     19.00 105.00   0.50    3.02    --   94.90 -77.00 -60.00  172
 13  \w      6.00 100.00   0.50    3.02    --   94.90 -30.00  90.00  188
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Pro: Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0357141000
_diffrn_orient_matrix_UB_12      0.0941627000
_diffrn_orient_matrix_UB_13      -0.0179914000
_diffrn_orient_matrix_UB_21      0.0777981000
_diffrn_orient_matrix_UB_22      -0.0349189000
_diffrn_orient_matrix_UB_23      0.0581953000
_diffrn_orient_matrix_UB_31      0.0247117000
_diffrn_orient_matrix_UB_32      -0.0263002000
_diffrn_orient_matrix_UB_33      -0.1417233000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0324
_diffrn_reflns_av_unetI/netI     0.0345
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            14591
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.466
_diffrn_reflns_theta_min         3.927
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.522
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81706
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.20a (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.126
_exptl_crystal_description       plate
_exptl_crystal_F_000             944
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.314
_refine_diff_density_min         -0.280
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         5051
_refine_ls_number_restraints     45
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0551
_refine_ls_R_factor_gt           0.0485
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0701P)^2^+0.7119P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1342
_refine_ls_wR_factor_ref         0.1391
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4343
_reflns_number_total             5051
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00062e2.cif
_cod_data_source_block           exp_4146
_cod_depositor_comments
'Adding full bibliography for 7715919--7715920.cif.'
_cod_database_code               7715920
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHNOSiFS
_shelx_estimated_absorpt_t_max   0.863
_shelx_estimated_absorpt_t_min   0.751
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C3-C00D
 1.54 with sigma of 0.01
 Si01-C00N \\sim Si02-C00O \\sim Si-C6 \\sim Si1-C5
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Si1 \\sim C4 \\sim C1: within 2A with sigma of 0.02 and sigma for terminal
atoms of 0.04 within 2A
C3 \\sim C2 \\sim Si: within 2A with sigma of 0.01 and sigma for terminal atoms
of 0.02 within 2A
4. Rigid body (RIGU) restrains
 Si1, C4, C1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Si, C2, C3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(H00C)=Sof(H00D)=Sof(H00I)=Sof(H00J)=Sof(Si)=Sof(Si1)=Sof(O10A)=Sof(C2)=
 Sof(H2A)=Sof(H2B)=Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(C3)=
 Sof(H3A)=Sof(H3B)=Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(H5C)=Sof(C6)=Sof(H6A)=Sof(H6B)=
 Sof(H6C)=1-FVAR(1)
 Sof(Si01)=Sof(Si02)=Sof(O10)=Sof(H00A)=Sof(H00B)=Sof(C00E)=Sof(H00E)=
 Sof(H00F)=Sof(H00G)=Sof(H00H)=Sof(C00H)=Sof(H00K)=Sof(H00L)=Sof(C00I)=
 Sof(H00M)=Sof(H00N)=Sof(C00K)=Sof(H00O)=Sof(H00P)=Sof(C00N)=Sof(H00W)=
 Sof(H00X)=Sof(H00Y)=Sof(C00O)=Sof(H00Z)=Sof(H)=Sof(HA)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C00D(H00A,H00B), C00D(H00C,H00D), C00E(H00E,H00F), C00G(H00G,H00H), C00G(H00I,
 H00J), C00H(H00K,H00L), C00I(H00M,H00N), C00K(H00O,H00P), C2(H2A,H2B), C4(H4A,
 H4B), C1(H1A,H1B), C3(H3A,H3B)
6.b Me refined with riding coordinates:
 C5(H5A,H5B,H5C), C6(H6A,H6B,H6C)
6.c Aromatic/amide H refined with riding coordinates:
 N007(H007), N008(H008)
6.d Idealised Me refined as rotating group:
 C00L(H00Q,H00R,H00S), C00M(H00T,H00U,H00V), C00N(H00W,H00X,H00Y), C00O(H00Z,H,
 HA), C00P(H00,HB,HC), C00Q(H1,HD,HE), C00R(H2,HF,HG), C00S(H3,HH,HI)
;
_shelx_res_checksum              59644
_shelx_hkl_checksum              68115
_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 1.308
_oxdiff_exptl_absorpt_empirical_full_min 0.836