New Sterically Hindered Tin(IV) Siloxane Precursors to Tinsilicate Materials: Synthesis, Spectral, Structural and Photocatalytic Studies
Mohan, Gopalakrishnan; Nallasamy, Palanisami; RSC Adv.  (2015) –; doi:10.1039/C5RA23424G

data_7223559
_publ_section_title
;
 New Sterically Hindered Tin(IV) Siloxane Precursors to Tinsilicate
 Materials: Synthesis, Spectral, Structural and Photocatalytic Studies
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C5RA23424G
_journal_year                    2015
_chemical_formula_moiety         'C32 H72 O8 Si2 Sn'
_chemical_formula_sum            'C32 H72 O8 Si2 Sn'
_chemical_formula_weight         759.76
_chemical_name_systematic        'Tin (IV) siloxanes'
_chemical_properties_physical    Moisture-sensitive
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-05-15
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2014.10.22 svn.r3046 for OlexSys, GUI svn.r4928)
;
_audit_update_record
;
2015-12-01 deposited with the CCDC.
2015-12-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.697(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.505(2)
_cell_length_b                   16.483(4)
_cell_length_c                   27.196(6)
_cell_measurement_reflns_used    9902
_cell_measurement_temperature    150.15
_cell_measurement_theta_max      27.389
_cell_measurement_theta_min      2.384
_cell_volume                     4222.4(16)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0460
_diffrn_reflns_av_unetI/netI     0.0335
_diffrn_reflns_laue_measured_fraction_full 0.999
_diffrn_reflns_laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            47953
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         1.511
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.701
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4171
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/3 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.1269 before and 0.0561 after correction.
The Ratio of minimum to maximum transmission is 0.5594.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.195
_exptl_crystal_description       block
_exptl_crystal_F_000             1624
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: hexane'
_exptl_crystal_size_max          0.57
_exptl_crystal_size_mid          0.53
_exptl_crystal_size_min          0.5
_refine_diff_density_max         0.953
_refine_diff_density_min         -0.701
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     412
_refine_ls_number_reflns         9618
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.118
_refine_ls_R_factor_all          0.0398
_refine_ls_R_factor_gt           0.0331
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0233P)^2^+3.6854P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0729
_refine_ls_wR_factor_ref         0.0758
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8613
_reflns_number_total             9618
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ra23424g2.cif
_cod_data_source_block           gp10
_cod_original_cell_volume        4222.8(16)
_cod_database_code               7223559
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.721
_shelx_estimated_absorpt_t_min   0.691
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2.a Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C27(H27A,H27B,H27C), C7(H7A,H7B,H7C), C2(H2A,H2B,H2C),
 C6(H6A,H6B,H6C), C8(H8A,H8B,H8C), C4(H4A,H4B,H4C), C28(H28A,H28B,H28C), C3(H3A,
 H3B,H3C), C24(H24A,H24B,H24C), C14(H14A,H14B,H14C), C20(H20A,H20B,H20C),
 C22(H22A,H22B,H22C), C26(H26A,H26B,H26C), C19(H19A,H19B,H19C), C11(H11A,H11B,
 H11C), C12(H12A,H12B,H12C), C31(H31A,H31B,H31C), C10(H10A,H10B,H10C), C23(H23A,
 H23B,H23C), C16(H16A,H16B,H16C), C32(H32A,H32B,H32C), C15(H15A,H15B,H15C),
 C30(H30A,H30B,H30C)
;
_shelx_res_checksum              85389
_olex2_submission_special_instructions 'No special instructions were received'