Assembly of discrete and oligomeric structures of organotin double-decker silsesquioxanes: inherent stability studies
Loganathan, Pushparaj; Pillai, Renjith S.; Jeevananthan, Velusamy; David, Ezhumalai; Palanisami, Nallasamy; Bhuvanesh, Nattamai S. P.; Shanmugan, Swaminathan; New Journal of Chemistry 45 (2021) 20144–20154; doi:10.1039/D1NJ03128G

data_7060973
_publ_section_title
;
 Assembly of discrete and oligomeric structures of organotin double-decker
 silsesquioxanes: inherent stability studies
;
_journal_issue                   43
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              20144
_journal_page_last               20154
_journal_paper_doi               10.1039/D1NJ03128G
_journal_volume                  45
_journal_year                    2021
_chemical_formula_moiety         'C80 H76 O16 Si8 Sn2'
_chemical_formula_sum            'C80 H76 O16 Si8 Sn2'
_chemical_formula_weight         1755.50
_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     direct
_audit_creation_date             2019-12-19
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-05-23 deposited with the CCDC.	2021-09-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.902(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.419(2)
_cell_length_b                   13.5736(10)
_cell_length_c                   24.9877(18)
_cell_measurement_reflns_used    9136
_cell_measurement_temperature    110.0
_cell_measurement_theta_max      25.077
_cell_measurement_theta_min      2.390
_cell_volume                     7942.1(11)
_computing_cell_refinement
'SAINT V8.38 Bruker AXS Inc., Madison, WI, USA.'
_computing_data_reduction
'SAINT V8.38 Bruker AXS Inc., Madison, WI, USA.'
_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      110.0
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker PHOTON II'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0291
_diffrn_reflns_av_unetI/netI     0.0089
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            147722
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.076
_diffrn_reflns_theta_max         25.076
_diffrn_reflns_theta_min         2.371
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.815
_exptl_absorpt_correction_T_max  0.4286
_exptl_absorpt_correction_T_min  0.3619
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1206 before and 0.0451 after correction. The Ratio of minimum to maximum transmission is 0.8444. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.468
_exptl_crystal_description       block
_exptl_crystal_F_000             3584
_exptl_crystal_size_max          0.418
_exptl_crystal_size_mid          0.374
_exptl_crystal_size_min          0.241
_refine_diff_density_max         0.753
_refine_diff_density_min         -0.719
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     632
_refine_ls_number_reflns         7019
_refine_ls_number_restraints     820
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0246
_refine_ls_R_factor_gt           0.0228
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0228P)^2^+20.7958P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0549
_refine_ls_wR_factor_ref         0.0564
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6651
_reflns_number_total             7019
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj03128g2.cif
_cod_data_source_block           lp10a
_cod_depositor_comments
'Adding full bibliography for 7060973--7060974.cif.'
_cod_original_cell_volume        7942.0(11)
_cod_database_code               7060973
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.828
_shelx_estimated_absorpt_t_min   0.727
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Shared sites
{O8, O8A}
{C7, C7A}
3. Restrained distances
 Si2-C7A \\sim Si2-C7
 with sigma of 0.02
 Si3-C13 \\sim Si3-C13A
 with sigma of 0.02
 Sn1-O8 \\sim Sn1-O8A
 with sigma of 0.02
 O8-C40 \\sim O8A-C40A \\sim O8-C37 \\sim O8A-C37A
 with sigma of 0.02
 Sn1-C25 \\sim Sn1-C25A
 with sigma of 0.02
 O8A-C37A \\sim O8-C37 \\sim O8-C40 \\sim O8A-C40A
 with sigma of 0.005
 C38A-C37A \\sim C38-C37 \\sim C40-C39 \\sim C40A-C39A
 with sigma of 0.005
 C39A-C38A \\sim C39-C38
 with sigma of 0.005
4. Uiso/Uaniso restraints and constraints
C7 \\sim C8 \\sim C9 \\sim C10 \\sim C11 \\sim C12 \\sim C7A \\sim C8A \\sim
C9A \\sim C10A \\sim C11A \\sim C12A: within 2A with sigma of 0.02 and sigma
for terminal atoms of 0.04
C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17 \\sim C18 \\sim C13A \\sim C14A
\\sim C15A \\sim C16A \\sim C17A \\sim C18A: within 2A with sigma of 0.02 and
sigma for terminal atoms of 0.04
O8 \\sim C37 \\sim C38 \\sim C39 \\sim C40 \\sim O8A \\sim C37A \\sim C38A
\\sim C39A \\sim C40A: within 2A with sigma of 0.005 and sigma for terminal
atoms of 0.01
Uanis(C7) = Uanis(C7A)
Uanis(C14) = Uanis(C14A)
Uanis(C13) = Uanis(C13A)
Uanis(O8) = Uanis(O8A)
Uanis(C37) = Uanis(C37A)
Uanis(C39A) = Uanis(C39)
Uanis(C38) = Uanis(C38A)
Uanis(C25) = Uanis(C25A)
5. Rigid body (RIGU) restrains
 C7, C8, C9, C10, C11, C12, C7A, C8A, C9A, C10A, C11A, C12A
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C13, C14, C15, C16, C17, C18, C13A, C14A, C15A, C16A, C17A, C18A
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 O8, C37, C38, C39, C40, O8A, C37A, C38A, C39A, C40A
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 C25, C26, C27, C28, C29, C30, C25A, C26A, C27A, C28A, C29A, C30A
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
6. Same fragment restrains
{O8, C37, C38, C39, C40} sigma for 1-2: 0.005, 1-3: 0.04
as
{O8A, C37A, C38A, C39A, C40A}
7. Others
 Sof(C7A)=Sof(C8A)=Sof(H8A)=Sof(C9A)=Sof(H9A)=Sof(C10A)=Sof(H10A)=Sof(C11A)=
 Sof(H11A)=Sof(C12A)=Sof(H12A)=Sof(C13A)=Sof(C14A)=Sof(H14A)=Sof(C15A)=
 Sof(H15A)=Sof(C16A)=Sof(H16A)=Sof(C17A)=Sof(H17A)=Sof(C18A)=Sof(H18A)=
 Sof(C25A)=Sof(C26A)=Sof(H26A)=Sof(C27A)=Sof(H27A)=Sof(C28A)=Sof(H28A)=
 Sof(C29A)=Sof(H29A)=Sof(C30A)=Sof(H30A)=Sof(O8A)=Sof(C37A)=Sof(H37C)=Sof(H37D)=
 Sof(C38A)=Sof(H38C)=Sof(H38D)=Sof(C39A)=Sof(H39C)=Sof(H39D)=Sof(C40A)=
 Sof(H40C)=Sof(H40D)=1-FVAR(1)
 Sof(C7)=Sof(C8)=Sof(H8)=Sof(C9)=Sof(H9)=Sof(C10)=Sof(H10)=Sof(C11)=Sof(H11)=
 Sof(C12)=Sof(H12)=Sof(C13)=Sof(C14)=Sof(H14)=Sof(C15)=Sof(H15)=Sof(C16)=
 Sof(H16)=Sof(C17)=Sof(H17)=Sof(C18)=Sof(H18)=Sof(C25)=Sof(C26)=Sof(H26)=
 Sof(C27)=Sof(H27)=Sof(C28)=Sof(H28)=Sof(C29)=Sof(H29)=Sof(C30)=Sof(H30)=
 Sof(O8)=Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(C38)=Sof(H38A)=Sof(H38B)=Sof(C39)=
 Sof(H39A)=Sof(H39B)=Sof(C40)=Sof(H40A)=Sof(H40B)=FVAR(1)
8.a Secondary CH2 refined with riding coordinates:
 C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B), C40(H40A,H40B), C37A(H37C,
 H37D), C38A(H38C,H38D), C39A(H39C,H39D), C40A(H40C,H40D)
8.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C8A(H8A), C9A(H9A), C10A(H10A), C11A(H11A), C12A(H12A), C14(H14),
 C15(H15), C16(H16), C17(H17), C18(H18), C14A(H14A), C15A(H15A), C16A(H16A),
 C17A(H17A), C18A(H18A), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24),
 C26(H26), C27(H27), C28(H28), C29(H29), C30(H30), C26A(H26A), C27A(H27A),
 C28A(H28A), C29A(H29A), C30A(H30A), C32(H32), C33(H33), C34(H34), C35(H35),
 C36(H36)
;
_shelx_res_checksum              98088
_olex2_submission_special_instructions 'No special instructions were received'