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_7715919
_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         'C36 H76 N4 O12 Si4'
_chemical_formula_sum            'C36 H76 N4 O12 Si4'
_chemical_formula_weight         869.36
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 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                 95.304(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.6119(2)
_cell_length_b                   22.4858(4)
_cell_length_c                   23.6228(4)
_cell_measurement_reflns_used    13393
_cell_measurement_temperature    213.00
_cell_measurement_theta_max      73.7630
_cell_measurement_theta_min      3.7490
_cell_volume                     5083.76(16)
_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 1.000
_diffrn_measured_fraction_theta_max 0.972
_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    -18.00  55.00   0.50    0.77    --    0.00  19.00 -30.00  146
  2  \w    -57.00  17.00   0.50    0.77    --    0.00 -37.00 -30.00  148
  3  \w     15.00  84.00   0.50    0.77    --    0.00  37.00   0.00  138
  4  \w     85.00 180.00   0.50    3.07    --   94.90  45.00-180.00  190
  5  \w      5.00 111.00   0.50    3.07    --   94.90 -30.00  30.00  212
  6  \w     33.00 120.00   0.50    3.07    --   94.90 -82.00 -30.00  174
  7  \w    135.00 160.00   0.50    3.07    --   94.90  15.00-150.00   50
  8  \w     71.00 116.00   0.50    3.07    --   94.90  15.00-150.00   90
  9  \w     70.00  96.00   0.50    3.07    --   94.90 -45.00   0.00   52
 10  \w      5.00 111.00   0.50    3.07    --   94.90 -61.00 -30.00  212
 11  \w     99.00 184.00   0.50    3.07    --   94.90  30.00 150.00  170
;
_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      -0.0504233000
_diffrn_orient_matrix_UB_12      0.0316712000
_diffrn_orient_matrix_UB_13      0.0522071000
_diffrn_orient_matrix_UB_21      0.1275162000
_diffrn_orient_matrix_UB_22      -0.0242805000
_diffrn_orient_matrix_UB_23      0.0371366000
_diffrn_orient_matrix_UB_31      0.0842201000
_diffrn_orient_matrix_UB_32      0.0557287000
_diffrn_orient_matrix_UB_33      -0.0135146000
_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  0.0305
_diffrn_reflns_av_unetI/netI     0.0297
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            30731
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.532
_diffrn_reflns_theta_min         2.719
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.535
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88204
_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    1.136
_exptl_crystal_description       block
_exptl_crystal_F_000             1888
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.415
_refine_diff_density_min         -0.513
_refine_diff_density_rms         0.039
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     559
_refine_ls_number_reflns         10101
_refine_ls_number_restraints     63
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0557
_refine_ls_R_factor_gt           0.0478
_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^)+(0.0614P)^2^+1.4407P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1297
_refine_ls_wR_factor_ref         0.1353
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8471
_reflns_number_total             10101
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00062e2.cif
_cod_data_source_block           exp_4145
_cod_depositor_comments
'Adding full bibliography for 7715919--7715920.cif.'
_cod_database_code               7715919
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHONSiFS
_shelx_estimated_absorpt_t_max   0.749
_shelx_estimated_absorpt_t_min   0.749
_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
 Si5-C01D \\sim Si5-C2
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C01L \\sim C01J \\sim C1 \\sim C01K \\sim Si5: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
4. Rigid body (RIGU) restrains
 Si5, C01L, C1, C01K, C01J
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C01D
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(HI)=Sof(HJ)=Sof(O11A)=Sof(C01L)=Sof(H11)=Sof(HU)=Sof(C1)=Sof(H1A)=
 Sof(H1B)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(H2C)=1-FVAR(1)
 Sof(O11)=Sof(C01D)=Sof(H3)=Sof(HF)=Sof(HG)=Sof(H4)=Sof(HH)=Sof(C01J)=Sof(H9)=
 Sof(HS)=Sof(C01K)=Sof(H10)=Sof(HT)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C00N(H00A,H00B), C00O(H00C,H00D), C00R(H00E,H00F), C00S(H00I,H00J), C00T(H00K,
 H00L), C00V(H00M,H00N), C011(H01A,H01B), C013(H01F,H01G), C014(H01H,H01I),
 C01E(H4,HH), C01E(HI,HJ), C01J(H9,HS), C01K(H10,HT), C01L(H11,HU), C1(H1A,H1B)
6.b Aromatic/amide H refined with riding coordinates:
 N00G(H00G), N00H(H00H), N1(H1), N2(H2)
6.c Idealised Me refined as rotating group:
 C00Y(H00O,H00P,H00Q), C00Z(H00R,H00S,H00T), C012(H01C,H01D,H01E), C015(H01J,
 H01K,H01L), C016(H01M,H01N,H01O), C017(H01P,H01Q,H01R), C018(H01S,H01T,H01U),
 C019(H01V,H01W,H01X), C01A(H01Y,H,HA), C01B(H01Z,HB,HC), C01C(H01,HD,HE),
 C01D(H3,HF,HG), C01F(H5,HK,HL), C01G(H6,HM,HN), C01H(H7,HO,HP), C01I(H8,HQ,HR),
  C2(H2A,H2B,H2C)
;
_shelx_res_checksum              93873
_shelx_hkl_checksum              68990
_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 1.158
_oxdiff_exptl_absorpt_empirical_full_min 0.815