Clicking [Mo(CO)<sub>3</sub>(triphos)] to an azide-terminated alkylthiol SAM: structural, spectroscopic and electrochemical investigations.
Michaelis, Niels; Engesser, Tobias A.; Krahmer, Jan; Strunskus, Thomas; Näther, Christian; Le Poul, Nicolas; Tuczek, Felix; Dalton transactions (Cambridge, England : 2003) 54 (2025) 14286–14303; doi:10.1039/d5dt01217a

data_7719171
_publ_section_title
;
 Clicking [Mo(CO)<sub>3</sub>(triphos)] to an azide-terminated alkylthiol
 SAM: structural, spectroscopic and electrochemical investigations.
;
_journal_issue                   38
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14286
_journal_page_last               14303
_journal_paper_doi               10.1039/d5dt01217a
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C39 H50 B3 P3 Si'
_chemical_formula_sum            'C39 H50 B3 P3 Si'
_chemical_formula_weight         672.22
_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             2022-02-17
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2020.11.27 svn.r5f609507 for Rigaku Oxford Diffraction, GUI svn.r6214)
;
_audit_update_record
;
2025-05-21 deposited with the CCDC.	2025-07-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.341(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.3368(4)
_cell_length_b                   16.4165(3)
_cell_length_c                   12.2136(2)
_cell_measurement_reflns_used    20608
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      78.9410
_cell_measurement_theta_min      3.5000
_cell_volume                     3950.56(13)
_computing_cell_refinement       'CrysAlisPro 1.171.42.40a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.42.40a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.42.40a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -25.00  54.00   0.50   25.00    --   43.22 -63.00 -85.00  158
  2  \w    -54.00 -22.00   0.50  100.00    --  -96.00  63.00  51.00   64
  3  \w   -170.00 -92.00   0.50  100.00    --  -96.00 -63.00 -85.00  156
  4  \w    114.00 178.00   0.50  100.00    --  117.50  63.00  51.00  128
  5  \w    -54.00  31.00   0.50   25.00    --  -43.22  63.00  51.00  170
  6  \w    -75.00 -13.00   0.50   25.00    --  -43.22 125.00 150.00  124
  7  \w    -19.00  34.00   0.50   25.00    --  -43.22  38.00 -60.00  106
  8  \w    -75.00 -13.00   0.50   25.00    --  -43.22 125.00 -60.00  124
  9  \w    -34.00  19.00   0.50   25.00    --   43.22 -38.00 150.00  106
 10  \w      1.00  66.00   0.50   25.00    --   43.22 -77.00-180.00  130
 11  \w   -171.00-102.00   0.50  100.00    --  -96.00 -95.00-150.00  138
 12  \w    -51.00 -22.00   0.50  100.00    --  -96.00  61.00 -90.00   58
 13  \w   -171.00-102.00   0.50  100.00    --  -96.00 -95.00  90.00  138
 14  \w     44.00  75.00   0.50  100.00    --  117.50 -77.00   0.00   62
 15  \w     44.00  75.00   0.50  100.00    --  117.50 -77.00  60.00   62
 16  \w    103.00 136.00   0.50  100.00    --  117.50  15.00 -30.00   66
 17  \w     44.00  92.00   0.50  100.00    --  117.50 -95.00 120.00   96
 18  \w    103.00 136.00   0.50  100.00    --  117.50  15.00   0.00   66
 19  \w    103.00 136.00   0.50  100.00    --  117.50  15.00 150.00   66
 20  \w    103.00 136.00   0.50  100.00    --  117.50  15.00-180.00   66
 21  \w    103.00 136.00   0.50  100.00    --  117.50  15.00-120.00   66
 22  \w    124.00 178.00   0.50  100.00    --  117.50  77.00 -30.00  108
 23  \w     44.00  75.00   0.50  100.00    --  117.50 -77.00 120.00   62
 24  \w     44.00  92.00   0.50  100.00    --  117.50 -95.00 -90.00   96
 25  \w    103.00 136.00   0.50  100.00    --  117.50  15.00  60.00   66
 26  \w    124.00 178.00   0.50  100.00    --  117.50  77.00 -60.00  108
 27  \w     44.00  92.00   0.50  100.00    --  117.50 -95.00   0.00   96
 28  \w    124.00 178.00   0.50  100.00    --  117.50  77.00 150.00  108
 29  \w    103.00 136.00   0.50  100.00    --  117.50  15.00 -90.00   66
 30  \w    103.00 136.00   0.50  100.00    --  117.50  15.00  30.00   66
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0391595000
_diffrn_orient_matrix_UB_12      -0.0660474000
_diffrn_orient_matrix_UB_13      -0.0474099000
_diffrn_orient_matrix_UB_21      -0.0405433000
_diffrn_orient_matrix_UB_22      0.0208579000
_diffrn_orient_matrix_UB_23      -0.1208185000
_diffrn_orient_matrix_UB_31      0.0541989000
_diffrn_orient_matrix_UB_32      0.0633436000
_diffrn_orient_matrix_UB_33      -0.0096567000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0269
_diffrn_reflns_av_unetI/netI     0.0194
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.955
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            32315
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.245
_diffrn_reflns_theta_min         2.242
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.850
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85977
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.40a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.130
_exptl_crystal_description       block
_exptl_crystal_F_000             1432
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.452
_refine_diff_density_min         -0.434
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     454
_refine_ls_number_reflns         8258
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0409
_refine_ls_R_factor_gt           0.0373
_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^)+(0.0502P)^2^+1.6926P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0997
_refine_ls_wR_factor_ref         0.1017
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7423
_reflns_number_total             8258
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01217a2.cif
_cod_data_source_block           felix238
_cod_depositor_comments
'Adding full bibliography for 7719171--7719173.cif.'
_cod_database_code               7719171
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         C39H50B3P3Si
_chemical_oxdiff_usercomment     'Niels Michaelis NM89 kris'
_reflns_odcompleteness_completeness 97.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_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 Secondary CH2 refined with riding coordinates:
 C1(H1D,H1E), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B)
2.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C12(H12), C13(H13), C14(H14),
 C15(H15), C16(H16), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C24(H24),
  C25(H25), C26(H26), C27(H27), C28(H28), C30(H30), C31(H31), C33(H33), C34(H34)
2.c Idealised Me refined as rotating group:
 C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C)
;
_shelx_res_checksum              99892
_shelx_hkl_checksum              48915
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.564
_oxdiff_exptl_absorpt_empirical_full_min 0.703