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_7719173
_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 H33 Mo O3 P3'
_chemical_formula_sum            'C39 H33 Mo O3 P3'
_chemical_formula_weight         738.50
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2023-05-05
_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                76.7060(10)
_cell_angle_beta                 88.7958(8)
_cell_angle_gamma                80.6135(8)
_cell_formula_units_Z            4
_cell_length_a                   8.99800(7)
_cell_length_b                   17.1690(2)
_cell_length_c                   24.1397(3)
_cell_measurement_reflns_used    32983
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      79.5530
_cell_measurement_theta_min      2.9060
_cell_volume                     3580.21(7)
_computing_cell_refinement       'CrysAlisPro 1.171.42.87a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.87a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.87a (Rigaku OD, 2023)'
_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 0.967
_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    -69.00 -36.00   0.50   10.00    --  -41.97 120.00 131.00   66
  2  \w     42.00  68.00   0.50   10.00    --   41.97-120.00  47.00   52
  3  \w    -73.00 -48.00   0.50   40.00    --  -96.00 120.00 131.00   50
  4  \w   -150.00-125.00   0.50   40.00    --  -96.00-120.00  47.00   50
  5  \w     71.00  97.00   0.50   40.00    --  117.50-120.00  47.00   52
  6  \w    115.00 158.00   0.50   40.00    --  117.50 120.00 131.00   86
  7  \w    -19.00  23.00   0.50   10.00    --  -41.97  38.00-120.00   84
  8  \w    -62.00  21.00   0.50   10.00    --  -41.97  77.00 -30.00  166
  9  \w    -19.00  32.00   0.50   10.00    --  -41.97  38.00 -90.00  102
 10  \w    -19.00  22.00   0.50   10.00    --  -41.97  38.00-150.00   82
 11  \w     19.00  75.00   0.50   10.00    --   41.97 -99.00  30.00  112
 12  \w     20.00  75.00   0.50   10.00    --   41.97 -99.00 120.00  110
 13  \w     92.00 118.00   0.50   10.00    --   41.97  38.00   0.00   52
 14  \w     24.00  75.00   0.50   10.00    --   41.97 -99.00-180.00  102
 15  \w    -35.00  19.00   0.50   10.00    --   41.97 -38.00  90.00  108
 16  \w    -34.00   8.00   0.50   10.00    --   41.97 -38.00  60.00   84
 17  \w    -33.00  -5.00   0.50   10.00    --   41.97 -38.00 -30.00   56
 18  \w     29.00  66.00   0.50   10.00    --   41.97  38.00   0.00   74
 19  \w    -49.00 -24.00   0.50   40.00    --  -96.00  61.00-120.00   50
 20  \w   -135.00 -82.00   0.50   40.00    --  -96.00 -15.00 150.00  106
 21  \w    -50.00 -22.00   0.50   40.00    --  -96.00  61.00 -90.00   56
 22  \w    -66.00 -41.00   0.50   40.00    --  -96.00  77.00 -90.00   50
 23  \w   -112.00 -82.00   0.50   40.00    --  -96.00 -15.00  90.00   60
 24  \w    103.00 129.00   0.50   40.00    --  117.50  15.00 -60.00   52
 25  \w    103.00 128.00   0.50   40.00    --  117.50  15.00  90.00   50
 26  \w     45.00  92.00   0.50   40.00    --  117.50 -95.00 150.00   94
 27  \w     53.00  93.00   0.50   40.00    --  117.50 -94.00 -90.30   80
 28  \w     50.00  92.00   0.50   40.00    --  117.50 -95.00 120.00   84
 29  \w     47.00 101.00   0.50   40.00    --  117.50-125.00   0.00  108
 30  \w    128.00 177.00   0.50   40.00    --  117.50 125.00-120.00   98
 31  \w     44.00  69.00   0.50   40.00    --  117.50 -77.00 -90.00   50
 32  \w     53.00  92.00   0.50   40.00    --  117.50 -95.00-180.00   78
 33  \w    153.00 178.00   0.50   40.00    --  117.50 125.00 120.00   50
 34  \w    103.00 129.00   0.50   40.00    --  117.50  15.00  30.00   52
 35  \w     45.00  72.00   0.50   40.00    --  117.50 -77.00  60.00   54
 36  \w    134.00 160.00   0.50   40.00    --  117.50  30.00 -60.00   52
 37  \w    104.00 130.00   0.50   40.00    --  117.50  15.00 -90.00   52
 38  \w     44.00  69.00   0.50   40.00    --  117.50 -77.00 -60.00   50
 39  \w    151.00 177.00   0.50   40.00    --  117.50  61.00-120.00   52
 40  \w     46.00  71.00   0.50   40.00    --  117.50-125.00  90.00   50
 41  \w    103.00 132.00   0.50   40.00    --  117.50  15.00-180.00   58
 42  \w    104.00 136.00   0.50   40.00    --  117.50  15.00-120.00   64
 43  \w     44.00  69.00   0.50   40.00    --  117.50 -77.00  30.00   50
 44  \w     65.00  91.00   0.50   40.00    --  117.50 -95.00  90.00   52
 45  \w     64.00  92.00   0.50   40.00    --  117.50 -95.00   0.00   56
 46  \w     46.00  72.00   0.50   40.00    --  117.50 -77.00 -30.00   52
 47  \w    128.00 171.00   0.50   40.00    --  117.50  77.00-150.00   86
 48  \w    112.00 145.00   0.50   40.00    --  117.50  61.00-120.00   66
 49  \w     61.00  92.00   0.50   40.00    --  117.50 -95.00-120.00   62
 50  \w    127.00 175.00   0.50   40.00    --  117.50 125.00 -90.00   96
 51  \w     66.00  92.00   0.50   40.00    --  117.50 -95.00  60.00   52
 52  \w    114.00 148.00   0.50   40.00    --  117.50 125.00  -9.59   68
 53  \w    124.00 176.00   0.50   40.00    --  117.50  45.00-180.00  104
 54  \w     57.00  91.00   0.50   40.00    --  117.50 -95.00  30.00   68
 55  \w     62.00  92.00   0.50   40.00    --  117.50 -95.00 -60.00   60
 56  \w    104.00 136.00   0.50   40.00    --  117.50  15.00  60.00   64
 57  \w     44.00  69.00   0.50   40.00    --  117.50 -77.00-120.00   50
 58  \w    124.00 170.00   0.50   40.00    --  117.50  77.00 -60.00   92
 59  \w     63.00 100.00   0.50   40.00    --  117.50-125.00 -60.00   74
 60  \w    113.00 145.00   0.50   40.00    --  117.50 125.00 120.00   64
 61  \w     65.00  90.00   0.50   40.00    --  117.50 -95.00 -30.00   50
 62  \w     67.00  92.00   0.50   40.00    --  117.50 -92.00  34.55   50
 63  \w     44.00  90.00   0.50   40.00    --  117.50 -88.00-141.83   92
 64  \w    109.00 165.00   0.50   40.00    --  117.50  30.00 120.00  112
 65  \w    153.00 178.00   0.50   40.00    --  117.50 125.00 -60.00   50
 66  \w    119.00 148.00   0.50   40.00    --  117.50 125.00 -60.00   58
 67  \w    134.00 177.00   0.50   40.00    --  117.50  77.00  60.00   86
 68  \w    116.00 178.00   0.50   40.00    --  117.50 125.00-150.00  124
 69  \w    104.00 135.00   0.50   40.00    --  117.50  15.00   0.00   62
 70  \w    103.00 136.00   0.50   40.00    --  117.50  15.00 -30.00   66
 71  \w     46.00  92.00   0.50   40.00    --  117.50 -95.00-150.00   92
;
_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      0.0443282000
_diffrn_orient_matrix_UB_12      0.0825543000
_diffrn_orient_matrix_UB_13      0.0012390000
_diffrn_orient_matrix_UB_21      0.0220831000
_diffrn_orient_matrix_UB_22      -0.0272881000
_diffrn_orient_matrix_UB_23      0.0651085000
_diffrn_orient_matrix_UB_31      0.1663450000
_diffrn_orient_matrix_UB_32      -0.0342352000
_diffrn_orient_matrix_UB_33      -0.0077987000
_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  0.0284
_diffrn_reflns_av_unetI/netI     0.0241
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            48755
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.378
_diffrn_reflns_theta_min         2.680
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.545
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76341
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.87a (Rigaku Oxford Diffraction, 2023)
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    1.370
_exptl_crystal_description       block
_exptl_crystal_F_000             1512
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.391
_refine_diff_density_min         -0.921
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     829
_refine_ls_number_reflns         15168
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0394
_refine_ls_R_factor_gt           0.0378
_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^)+(0.0556P)^2^+4.1867P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1025
_refine_ls_wR_factor_ref         0.1035
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14363
_reflns_number_total             15168
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01217a2.cif
_cod_data_source_block           felix264
_cod_depositor_comments
'Adding full bibliography for 7719171--7719173.cif.'
_cod_original_cell_volume        3580.19(7)
_cod_database_code               7719173
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         C41H37MoO3.5P3
_chemical_oxdiff_usercomment     'Nils Michaelis NM125'
_reflns_odcompleteness_completeness 98.68
_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
2.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B), C51(H51A,
 H51B), C52(H52A,H52B), C53(H53A,H53B), C54(H54A,H54B)
2.b Aromatic/amide H refined with riding coordinates:
 C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C22(H22), C23(H23),
 C24(H24), C25(H25), C26(H26), C28(H28), C29(H29), C31(H31), C32(H32), C36(H36),
  C37(H37), C38(H38), C39(H39), C40(H40), C42(H42), C43(H43), C44(H44),
 C45(H45), C46(H46), C56(H56), C57(H57), C58(H58), C59(H59), C60(H60), C62(H62),
  C63(H63), C64(H64), C65(H65), C66(H66), C68(H68), C69(H69), C71(H71),
 C72(H72), C76(H76), C77(H77), C78(H78), C79(H79), C80(H80), C82(H82), C83(H83),
  C84(H84), C85(H85), C86(H86)
2.c :
 C34(H34), C74(H74)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              95083
_shelx_hkl_checksum              50815
_shelx_fab_checksum              30320
_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 1.537
_oxdiff_exptl_absorpt_empirical_full_min 0.638