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_7705872
_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         'C14 H30 O3 Si2'
_chemical_formula_sum            'C14 H30 O3 Si2'
_chemical_formula_weight         302.56
_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   mixed
_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                90
_cell_angle_beta                 102.749(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.8568(7)
_cell_length_b                   6.6114(3)
_cell_length_c                   21.7760(11)
_cell_measurement_reflns_used    9972
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      27.75
_cell_measurement_theta_min      3.23
_cell_volume                     1805.36(16)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0521
_diffrn_reflns_av_unetI/netI     0.0281
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            31060
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.997
_diffrn_reflns_theta_min         3.227
_exptl_absorpt_coefficient_mu    0.199
_exptl_absorpt_correction_T_max  0.937
_exptl_absorpt_correction_T_min  0.903
_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    1.113
_exptl_crystal_description       Needles
_exptl_crystal_F_000             664
_exptl_crystal_size_max          0.928
_exptl_crystal_size_mid          0.428
_exptl_crystal_size_min          0.326
_refine_diff_density_max         0.226
_refine_diff_density_min         -0.172
_refine_diff_density_rms         0.034
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         3941
_refine_ls_number_restraints     527
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0685
_refine_ls_R_factor_gt           0.0479
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0511P)^2^+0.7488P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1213
_refine_ls_wR_factor_ref         0.1388
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2981
_reflns_number_total             3941
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03252b2.cif
_cod_data_source_block           2
_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               7705872
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O1-H1A
 0.92 with sigma of 0.02
 O3-H3
 0.92 with sigma of 0.02
 C1_1-C2_1 = C1_1-C6_1 = C2_1-C3_1 = C3_1-C4_1 = C4_1-C5_1 = C5_1-C6_1
 1.54 with sigma of 0.02
 C1_2-C2_2 = C1_2-C6_2 = C2_2-C3_2 = C3_2-C4_2 = C4_2-C5_2 = C5_2-C6_2
 1.54 with sigma of 0.02
 C1_3-C2_3 = C1_3-C6_3 = C2_3-C3_3 = C3_3-C4_3 = C4_3-C5_3 = C5_3-C6_3
 1.54 with sigma of 0.02
 C1_1-C3_1 = C1_1-C5_1 = C2_1-C4_1 = C3_1-C5_1 = C4_1-C6_1
 2.54 with sigma of 0.04
 C1_2-C3_2 = C1_2-C5_2 = C2_2-C4_2 = C3_2-C5_2 = C4_2-C6_2
 2.54 with sigma of 0.04
 C1_3-C3_3 = C1_3-C5_3 = C2_3-C4_3 = C3_3-C5_3 = C4_3-C6_3
 2.54 with sigma of 0.04
 C1_1-C5_1 \\sim C3_1-C5_1 \\sim C2_1-C6_1 \\sim C2_1-C4_1 \\sim C4_1-C6_1
\\sim C1_1-C3_1
 C1_2-C5_2 \\sim C3_2-C5_2 \\sim C2_2-C6_2 \\sim C2_2-C4_2 \\sim C4_2-C6_2
\\sim C1_2-C3_2
 C1_3-C5_3 \\sim C3_3-C5_3 \\sim C2_3-C6_3 \\sim C2_3-C4_3 \\sim C4_3-C6_3
\\sim C1_3-C3_3
 with sigma of 0.04
 C1_1-C2_1 \\sim C2_1-C3_1 \\sim C3_1-C4_1 \\sim C4_1-C5_1 \\sim C5_1-C6_1
\\sim C6_1-C1_1
 C1_2-C2_2 \\sim C2_2-C3_2 \\sim C3_2-C4_2 \\sim C4_2-C5_2 \\sim C5_2-C6_2
\\sim C6_2-C1_2
 C1_3-C2_3 \\sim C2_3-C3_3 \\sim C3_3-C4_3 \\sim C4_3-C5_3 \\sim C5_3-C6_3
\\sim C6_3-C1_3
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 1A
4. Rigid body (RIGU) restrains
 C1_1, C2_1, C3_1, C4_1, C5_1, C6_1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C1_2, C2_2, C3_2, C4_2, C5_2, C6_2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C1_3, C2_3, C3_3, C4_3, C5_3, C6_3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C1_3, C5_3, C6_3, C2_3, C4_3, C3_3
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
5. Others
 Fixed Sof: C1(0.55) H1A(0.55) H1B(0.55) C2(0.55) H2A(0.55) H2B(0.55) C3(0.55)
 H3A(0.55) H3B(0.55) C4(0.55) H4A(0.55) H4B(0.55) C5(0.55) H5(0.55) C6(0.55)
 H6A(0.55) H6B(0.55) C1(0.3) H1A(0.3) H1B(0.3) C2(0.3) H2A(0.3) H2B(0.3)
 C3(0.3) H3A(0.3) H3B(0.3) C4(0.3) H4A(0.3) H4B(0.3) C5(0.3) H5(0.3) C6(0.3)
 H6A(0.3) H6B(0.3) C1(0.15) H1A(0.15) H1B(0.15) C2(0.15) H2A(0.15) H2B(0.15)
 C3(0.15) H3A(0.15) H3B(0.15) C4(0.15) H4A(0.15) H4B(0.15) C5(0.15) H5(0.15)
 C6(0.15) H6A(0.15) H6B(0.15)
6.a Ternary CH refined with riding coordinates:
 C1(H1), C5(H5), C5(H5), C5(H5)
6.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C1(H1A,H1B),
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C6(H6A,H6B), C1(H1A,H1B), C2(H2A,H2B),
 C3(H3A,H3B), C4(H4A,H4B), C6(H6A,H6B), C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B),
 C4(H4A,H4B), C6(H6A,H6B)
6.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C)
;
_shelx_res_checksum              2076
_olex2_submission_special_instructions 'No special instructions were received'