Size-tunable silicon nanoparticles synthesized in solution <i>via</i> a redox reaction.
Parker, Megan A.; De Marco, Maria Letizia; Castro-Grijalba, Alexander; Ghoridi, Anissa; Portehault, David; Pechev, Stanislav; Hillard, Elizabeth A.; Lacomme, Sabrina; Bessière, Aurélie; Cunin, Frédérique; Rosa, Patrick; Gonidec, Mathieu; Drisko, Glenna L.; Nanoscale 16 (2024) 7958–7964; doi:10.1039/d3nr05793c

data_1571355
_publ_section_title
;
 Size-tunable silicon nanoparticles synthesized in solution <i>via</i> a
 redox reaction.
;
_journal_issue                   16
_journal_name_full               Nanoscale
_journal_page_first              7958
_journal_page_last               7964
_journal_paper_doi               10.1039/d3nr05793c
_journal_volume                  16
_journal_year                    2024
_chemical_formula_moiety         '2(Cl), C22 H46 N4 Si'
_chemical_formula_sum            'C22 H46 Cl2 N4 Si'
_chemical_formula_weight         465.62
_chemical_name_common            'silicon bisamidinate'
_chemical_name_systematic        (N,N'-dimethylbutylamidinate)dichlorosilane
_chemical_properties_physical    Air-sensitive
_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     dual
_audit_creation_date             2022-03-08
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-03-08 deposited with the CCDC.	2024-03-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.199(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.1108(12)
_cell_length_b                   12.0581(11)
_cell_length_c                   18.0846(16)
_cell_measurement_reflns_used    7099
_cell_measurement_temperature    120
_cell_measurement_theta_max      27.33
_cell_measurement_theta_min      2.35
_cell_volume                     2716.0(4)
_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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Kappa APEX II'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0490
_diffrn_reflns_av_unetI/netI     0.0372
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            13089
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.282
_diffrn_reflns_theta_min         2.351
_diffrn_source                   'sealed X-ray tube'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.298
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.6984
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2012/1 (Bruker,2012)'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.139
_exptl_crystal_description       plate
_exptl_crystal_F_000             1016
_exptl_crystal_size_max          0.169
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.041
_refine_diff_density_max         0.311
_refine_diff_density_min         -0.223
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     137
_refine_ls_number_reflns         3365
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0550
_refine_ls_R_factor_gt           0.0330
_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^)+(0.0390P)^2^+0.9628P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0734
_refine_ls_wR_factor_ref         0.0810
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2551
_reflns_number_total             3365
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nr05793c2.cif
_cod_data_source_block           ml19_0m
_cod_depositor_comments          'Adding full bibliography for 1571355.cif.'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               1571355
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.988
_shelx_estimated_absorpt_t_min   0.951
_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.a Ternary CH refined with riding coordinates:
 C006(H006), C007(H007)
2.b Secondary CH2 refined with riding coordinates:
 C008(H00A,H00B), C009(H00C,H00D), C00C(H00K,H00L)
2.c Idealised Me refined as rotating group:
 C00A(H00E,H00F,H00G), C00B(H00H,H00I,H00J), C00D(H00M,H00N,H00O), C00E(H00P,
 H00Q,H00R), C00F(H00S,H00T,H00U)
;
_shelx_res_checksum              97475
_olex2_date_sample_data_collection 2018-09-06
_olex2_date_sample_submission    2022-03-07
_olex2_submission_original_sample_id ml19
_olex2_submission_special_instructions 'No special instructions were received'