A catalytic study of water dispersed gold nanoparticles for the hydrolytic oxidation of diorganosilanes - <i>en route</i> formation of a Pickering catalyst and synthesis of tetraorganodisiloxane-1,3-diols.
Shankar, Ravi; Mahavar, Nidhi; Dalton transactions (Cambridge, England : 2003) 49 (2020) 16633–16637; doi:10.1039/d0dt03252b

data_7705873
_publ_section_title
;
 A catalytic study of water dispersed gold nanoparticles for the
 hydrolytic oxidation of diorganosilanes - <i>en route</i> formation of a
 Pickering catalyst and synthesis of tetraorganodisiloxane-1,3-diols.
;
_journal_issue                   46
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16633
_journal_page_last               16637
_journal_paper_doi               10.1039/d0dt03252b
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         '1(C24 H22 O3 Si2)'
_chemical_formula_sum            'C24 H22 O3 Si2'
_chemical_formula_weight         414.59
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-10-05
_audit_creation_method
;
Olex2 1.3-dev
(compiled 2020.09.11 svn.rc89507dd for OlexSys, GUI svn.r5830)
;
_audit_update_record
;
2020-10-07 deposited with the CCDC.	2020-10-26 downloaded from the CCDC.
;
_cell_angle_alpha                98.906(2)
_cell_angle_beta                 99.541(2)
_cell_angle_gamma                113.364(2)
_cell_formula_units_Z            6
_cell_length_a                   13.4751(8)
_cell_length_b                   14.2528(9)
_cell_length_c                   20.2962(14)
_cell_measurement_reflns_used    9867
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      28.08
_cell_measurement_theta_min      2.31
_cell_volume                     3422.6(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 1.3-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-III CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0427
_diffrn_reflns_av_unetI/netI     0.0347
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            55779
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.500
_diffrn_reflns_theta_min         1.700
_exptl_absorpt_coefficient_mu    0.177
_exptl_absorpt_correction_T_max  0.983
_exptl_absorpt_correction_T_min  0.978
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2008/1 - Bruker AXS area detector scaling and absorption correction'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.207
_exptl_crystal_description       Blocks
_exptl_crystal_F_000             1308
_exptl_crystal_size_max          0.132
_exptl_crystal_size_mid          0.106
_exptl_crystal_size_min          0.098
_refine_diff_density_max         0.302
_refine_diff_density_min         -0.333
_refine_diff_density_rms         0.037
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1009
_refine_ls_number_reflns         12754
_refine_ls_number_restraints     104
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0687
_refine_ls_R_factor_gt           0.0479
_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^)+(0.0656P)^2^+1.3031P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1257
_refine_ls_wR_factor_ref         0.1452
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9451
_reflns_number_total             12754
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03252b2.cif
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-scan' was
changed to 'multi-scan' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_database_code               7705873
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups
2. Restrained distances
 C70-C71 \\sim C70A-C71A
 with sigma of 0.02
 C67-C68 \\sim C67A-C68A
 with sigma of 0.02
 C68-C69 \\sim C68A-C69A
 with sigma of 0.02
 C71-C72 \\sim C71A-C72A
 with sigma of 0.02
 C67-C72 \\sim C67A-C72A
 with sigma of 0.02
 C70-C72 \\sim C70A-C72A
 with sigma of 0.04
 C67-C69 \\sim C67A-C69A
 with sigma of 0.04
 C68-C70 \\sim C68A-C70A
 with sigma of 0.04
 C68-C72 \\sim C68A-C72A
 with sigma of 0.04
 C67-Si6 \\sim C67A-Si6
 with sigma of 0.02
 C72-Si6 \\sim C72A-Si6
 with sigma of 0.04
 C67-C71 \\sim C67A-C71A
 with sigma of 0.04
 C69-C70 \\sim C69A-C70A
 with sigma of 0.02
 C69-C71 \\sim C69A-C71A
 with sigma of 0.04
 C68-Si6 \\sim C68A-Si6
 with sigma of 0.04
 C25-C30 \\sim C25A-C30A
 with sigma of 0.02
 C25-Si3 \\sim C25A-Si3
 with sigma of 0.02
 C27-C29 \\sim C27A-C29A
 with sigma of 0.04
 C26-C27 \\sim C26A-C27A
 with sigma of 0.02
 C27-C28 \\sim C27A-C28A
 with sigma of 0.02
 C28-C29 \\sim C28A-C29A
 with sigma of 0.02
 C29-C30 \\sim C29A-C30A
 with sigma of 0.02
 C25-C27 \\sim C25A-C27A
 with sigma of 0.04
 C28-C30 \\sim C28A-C30A
 with sigma of 0.04
 C25-C29 \\sim C25A-C29A
 with sigma of 0.04
 C26-C28 \\sim C26A-C28A
 with sigma of 0.04
 C30-Si3 \\sim C30A-Si3
 with sigma of 0.04
 C26-C30 \\sim C26A-C30A
 with sigma of 0.04
 C26-Si3 \\sim C26A-Si3
 with sigma of 0.04
 C25-C26 \\sim C25A-C26A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C28A \\sim C29A \\sim C30A: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.002 within 2A
4. Rigid body (RIGU) restrains
 C31A, C36A, C35A, C34A, C33A, C32A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C31, C36, C35, C34, C33, C32
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Sof(C31A)=Sof(C32A)=Sof(H32A)=Sof(C33A)=Sof(H33A)=Sof(C34A)=Sof(H34A)=
 Sof(C35A)=Sof(H35A)=Sof(C36A)=Sof(H36A)=1-FVAR(1)
 Sof(C31)=Sof(C32)=Sof(H32)=Sof(C33)=Sof(H33)=Sof(C34)=Sof(H34)=Sof(C35)=
 Sof(H35)=Sof(C36)=Sof(H36)=FVAR(1)
 Sof(C13A)=Sof(C14A)=Sof(H14A)=Sof(C15A)=Sof(H15A)=Sof(C16A)=Sof(H16A)=
 Sof(C17A)=Sof(H17A)=Sof(C18A)=Sof(H18A)=1-FVAR(2)
 Sof(C13)=Sof(C14)=Sof(H14)=Sof(C15)=Sof(H15)=Sof(C16)=Sof(H16)=Sof(C17)=
 Sof(H17)=Sof(C18)=Sof(H18)=FVAR(2)
 Sof(C19A)=Sof(C20A)=Sof(H20A)=Sof(C21A)=Sof(H21A)=Sof(C22A)=Sof(H22A)=
 Sof(C23A)=Sof(H23A)=Sof(C24A)=Sof(H24A)=1-FVAR(3)
 Sof(C19)=Sof(C20)=Sof(H20)=Sof(C21)=Sof(H21)=Sof(C22)=Sof(H22)=Sof(C23)=
 Sof(H23)=Sof(C24)=Sof(H24)=FVAR(3)
 Sof(C43A)=Sof(C44A)=Sof(H44A)=Sof(C45A)=Sof(H45A)=Sof(C46A)=Sof(H46A)=
 Sof(C47A)=Sof(H47A)=Sof(C48A)=Sof(H48A)=1-FVAR(4)
 Sof(C43)=Sof(C44)=Sof(H44)=Sof(C45)=Sof(H45)=Sof(C46)=Sof(H46)=Sof(C47)=
 Sof(H47)=Sof(C48)=Sof(H48)=FVAR(4)
 Sof(C7A)=Sof(C8A)=Sof(H8A)=Sof(C9A)=Sof(H9A)=Sof(C10A)=Sof(H10A)=Sof(C11A)=
 Sof(H11A)=Sof(C12A)=Sof(H12A)=1-FVAR(5)
 Sof(C7)=Sof(C8)=Sof(H8)=Sof(C9)=Sof(H9)=Sof(C10)=Sof(H10)=Sof(C11)=Sof(H11)=
 Sof(C12)=Sof(H12)=FVAR(5)
 Sof(C49A)=Sof(C50A)=Sof(H50A)=Sof(C51A)=Sof(H51A)=Sof(C52A)=Sof(H52A)=
 Sof(C53A)=Sof(H53A)=Sof(C54A)=Sof(H54A)=1-FVAR(6)
 Sof(C49)=Sof(C50)=Sof(H50)=Sof(C51)=Sof(H51)=Sof(C52)=Sof(H52)=Sof(C53)=
 Sof(H53)=Sof(C54)=Sof(H54)=FVAR(6)
 Sof(C67A)=Sof(C68A)=Sof(H68A)=Sof(C69A)=Sof(H69A)=Sof(C70A)=Sof(H70A)=
 Sof(C71A)=Sof(H71A)=Sof(C72A)=Sof(H72A)=1-FVAR(7)
 Sof(C67)=Sof(C68)=Sof(H68)=Sof(C69)=Sof(H69)=Sof(C70)=Sof(H70)=Sof(C71)=
 Sof(H71)=Sof(C72)=Sof(H72)=FVAR(7)
 Fixed Sof: C25(0.9) C26(0.9) H26(0.9) C27(0.9) H27(0.9) C28(0.9) H28(0.9)
 C29(0.9) H29(0.9) C30(0.9) H30(0.9) C25A(0.1) C26A(0.1) H26A(0.1) C27A(0.1)
 H27A(0.1) C28A(0.1) H28A(0.1) C29A(0.1) H29A(0.1) C30A(0.1) H30A(0.1)
6.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C73(H73), 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),
 C20A(H20A), C21A(H21A), C22A(H22A), C23A(H23A), C24A(H24A), C26(H26), C27(H27),
  C28(H28), C29(H29), C30(H30), C32(H32), C33(H33), C34(H34), C35(H35),
 C36(H36), C32A(H32A), C33A(H33A), C34A(H34A), C35A(H35A), C36A(H36A), C38(H38),
  C39(H39), C40(H40), C41(H41), C42(H42), C44(H44), C45(H45), C46(H46),
 C47(H47), C48(H48), C44A(H44A), C45A(H45A), C46A(H46A), C47A(H47A), C48A(H48A),
  C50(H50), C51(H51), C52(H52), C53(H53), C54(H54), C50A(H50A), C51A(H51A),
 C52A(H52A), C53A(H53A), C54A(H54A), C56(H56), C57(H57), C58(H58), C59(H59),
 C60(H60), C62(H62), C63(H63), C64(H64), C65(H65), C66(H66), C68(H68), C69(H69),
  C70(H70), C71(H71), C72(H72), C68A(H68A), C69A(H69A), C70A(H70A), C71A(H71A),
 C72A(H72A), C26A(H26A), C27A(H27A), C28A(H28A), C29A(H29A), C30A(H30A)
6.b Fitted hexagon refined as free rotating group:
 C7(C8,C9,C10,C11,C12), C7A(C8A,C9A,C10A,C11A,C12A), C13(C14,C15,C16,C17,C18),
 C13A(C14A,C15A,C16A,C17A,C18A), C19(C20,C21,C22,C23,C24), C19A(C20A,C21A,C22A,
 C23A,C24A), C31(C32,C33,C34,C35,C36), C31A(C32A,C33A,C34A,C35A,C36A), C43(C44,
 C45,C46,C47,C48), C43A(C44A,C45A,C46A,C47A,C48A), C49(C50,C51,C52,C53,C54),
 C49A(C50A,C51A,C52A,C53A,C54A), C67A(C68A,C69A,C70A,C71A,C72A)
6.c Tetrahedral OH refined with riding coordinates:
 O3(H3A), O4(H4), O6(H6A), O7(H7)
6.d Idealised tetrahedral OH refined as rotating group:
 O1(H1), O9(H9B)
;
_shelx_res_checksum              3867
_olex2_submission_special_instructions 'No special instructions were received'