Sulfur functionalized diamondoid phosphines enable building nanocomposites interfacing sp<sup>3</sup>-carbon and gold nanolayers.
Bouzid, Moad; Poinsot, Didier; Mboyi, Clève D; Ochmann, Lukas; Domenichini, Bruno; Schreiner, Peter R.; Hierso, Jean-Cyrille; Nanoscale 17 (2025) 4123–4131; doi:10.1039/d4nr03511a

data_1573528
_publ_section_title
;
 Sulfur functionalized diamondoid phosphines enable building
 nanocomposites interfacing sp<sup>3</sup>-carbon and gold nanolayers.
;
_journal_issue                   7
_journal_name_full               Nanoscale
_journal_page_first              4123
_journal_page_last               4131
_journal_paper_doi               10.1039/d4nr03511a
_journal_volume                  17
_journal_year                    2025
_chemical_formula_moiety         'C14 H21 P S'
_chemical_formula_sum            'C14 H21 P S'
_chemical_formula_weight         252.34
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-08-06
_audit_creation_method
;FinalCif V139 by Daniel Kratzert, Freiburg 2024, 
https://dkratzert.de/finalcif.html
;
_audit_update_record
;
2024-08-06 deposited with the CCDC.	2024-12-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.820(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.7405(4)
_cell_length_b                   13.6302(7)
_cell_length_c                   12.6387(6)
_cell_measurement_reflns_used    5410
_cell_measurement_temperature    110.0(1)
_cell_measurement_theta_max      27.33
_cell_measurement_theta_min      2.72
_cell_volume                     1289.08(11)
_computing_cell_refinement       'SAINT V8.40B (Bruker, 2016)'
_computing_data_collection       'APEX5 (Bruker, 2023)'
_computing_data_reduction        'SAINT V8.40B (Bruker, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      110.0(1)
_diffrn_detector                 'CCD Plate'
_diffrn_detector_area_resol_mean 8.3
_diffrn_detector_type            APEX2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Nonius Kappa Apex II'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_radiation_collimation    '0.6 mm'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a~1~'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0474
_diffrn_reflns_av_unetI/netI     0.0314
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            25147
_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         27.498
_diffrn_reflns_theta_min         2.239
_diffrn_source                   'X-ray tube'
_diffrn_source_current           5.0
_diffrn_source_power             0.1
_diffrn_source_target            Mo
_diffrn_source_type              'Siemens KFF Mo 2K-180'
_diffrn_source_voltage           20.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.346
_exptl_absorpt_correction_T_max  0.9583
_exptl_absorpt_correction_T_min  0.8623
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.0543 before and 0.0500 after correction.
The Ratio of minimum to maximum transmission is 0.8998.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.300
_exptl_crystal_description       needle
_exptl_crystal_F_000             544
_exptl_crystal_recrystallization_method
'The material was recrystallised from DCM by slow evaporation'
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.136
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.382
_refine_diff_density_min         -0.519
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     155
_refine_ls_number_reflns         2954
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0613
_refine_ls_R_factor_gt           0.0375
_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^)+(0.0450P)^2^+1.0270P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0913
_refine_ls_wR_factor_ref         0.1051
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2209
_reflns_number_total             2954
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nr03511a2.cif
_cod_data_source_block           Compound_3
_cod_depositor_comments
'Adding full bibliography for 1573527--1573528.cif.'
_cod_database_code               1573528
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder oil'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All P(H,H) groups, All S(H) groups
2. Others
 Fixed Sof: S1A(0.54) H1A(0.54) P1A(0.54) H1AA(0.54) H1AB(0.54) S1(0.46)
 H1(0.46) P1(0.46) H1B(0.46) H1C(0.46)
3.a Everything fixed:
 H1AA, H1AB, H1B, H1C
3.b Ternary CH refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C8(H8), C9(H9), C11(H11)
3.c Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C6(H6A,H6B), C7(H7A,H7B), C10(H10A,H10B), C12(H12A,H12B),
 C14(H14A,H14B)
3.d Idealised tetrahedral OH refined as rotating group:
 S1A(H1A), S1(H1)
;
_olex2_submission_special_instructions 'No special instructions were received'
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.891
_shelx_estimated_absorpt_t_max   0.976
_diffrn_measurement_ambient_temperature_device_make 'Oxford Cryostream 600'
_shelx_res_checksum              49180
_shelx_hkl_checksum              62062