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_7719172
_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         'C42 H41 Mo O3 P3 Si'
_chemical_formula_sum            'C42 H41 Mo O3 P3 Si'
_chemical_formula_weight         810.69
_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             2022-05-18
_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                75.4307(6)
_cell_angle_beta                 84.8563(6)
_cell_angle_gamma                79.6243(6)
_cell_formula_units_Z            4
_cell_length_a                   10.20427(7)
_cell_length_b                   14.90425(11)
_cell_length_c                   27.02750(19)
_cell_measurement_reflns_used    62829
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      79.4430
_cell_measurement_theta_min      3.0930
_cell_volume                     3909.05(5)
_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 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.99(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 0.971
_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    -68.00   1.00   0.50    3.00    --  -43.21 103.00 126.00  138
  2  \w     20.00  79.00   0.50    3.00    --   43.21-103.00  24.00  118
  3  \w    -68.00 -21.00   0.50   14.00    --  -96.00 103.00 126.00   94
  4  \w   -160.00-103.00   0.50   14.00    --  -96.00-103.00  24.00  114
  5  \w    125.00 178.00   0.50   14.00    --  117.50 103.00 126.00  106
  6  \w     43.00  94.00   0.50   14.00    --  117.50-103.00  24.00  102
  7  \w    -66.00  21.00   0.50    3.00    --  -43.21  77.00  60.00  174
  8  \w    -66.00  21.00   0.50    3.00    --  -43.21  77.00 -90.00  174
  9  \w     27.00  54.00   0.50    3.00    --   43.21  61.00-160.92   54
 10  \w    -34.00  19.00   0.50    3.00    --   43.21 -38.00 -30.00  106
 11  \w     28.00  59.00   0.50    3.00    --   43.21  58.00 -49.71   62
 12  \w     29.00  60.00   0.50    3.00    --   43.21  55.00 124.99   62
 13  \w     28.00  59.00   0.50    3.00    --   43.21  59.00 -91.66   62
 14  \w    -34.00  19.00   0.50    3.00    --   43.21 -38.00 -60.00  106
 15  \w     27.00  54.00   0.50    3.00    --   43.21  61.00 -26.38   54
 16  \w     27.00  54.00   0.50    3.00    --   43.21  61.00  42.74   54
 17  \w     29.00  60.00   0.50    3.00    --   43.21  53.00 155.64   62
 18  \w     18.00  77.00   0.50    3.00    --   43.21 -99.00-150.00  118
 19  \w     29.00  60.00   0.50    3.00    --   43.21  57.00 174.97   62
 20  \w     28.00  59.00   0.50    3.00    --   43.21  58.00 132.96   62
 21  \w     28.00  57.00   0.50    3.00    --   43.21  60.00  -8.41   58
 22  \w     29.00  60.00   0.50    3.00    --   43.21  54.00  91.48   62
 23  \w     29.00  60.00   0.50    3.00    --   43.21  53.00 -61.20   62
 24  \w   -136.00 -81.00   0.50   14.00    --  -96.00 -15.00-180.00  110
 25  \w   -169.00 -83.00   0.50   14.00    --  -96.00 -54.00 103.34  172
 26  \w    -67.00 -22.00   0.50   14.00    --  -96.00  77.00  90.00   90
 27  \w     44.00  92.00   0.50   14.00    --  117.50 -95.00 -30.00   96
 28  \w    109.00 178.00   0.50   14.00    --  117.50  61.00  90.00  138
 29  \w    103.00 136.00   0.50   14.00    --  117.50  15.00  60.00   66
 30  \w     44.00  92.00   0.50   14.00    --  117.50 -95.00  90.00   96
 31  \w    103.00 136.00   0.50   14.00    --  117.50  15.00  30.00   66
 32  \w    109.00 178.00   0.50   14.00    --  117.50  61.00 -30.00  138
 33  \w     44.00  95.00   0.50   14.00    --  117.50 -91.00 100.98  102
 34  \w     44.00  92.00   0.50   14.00    --  117.50 -95.00 150.00   96
 35  \w     44.00  92.00   0.50   14.00    --  117.50 -95.00-180.00   96
 36  \w     44.00  92.00   0.50   14.00    --  117.50 -92.00 153.85   96
 37  \w    103.00 136.00   0.50   14.00    --  117.50  15.00 -90.00   66
 38  \w     44.00  75.00   0.50   14.00    --  117.50 -77.00 -60.00   62
 39  \w    104.00 170.00   0.50   14.00    --  117.50  34.00-152.83  132
 40  \w    103.00 136.00   0.50   14.00    --  117.50  15.00 -60.00   66
 41  \w    124.00 178.00   0.50   14.00    --  117.50  77.00-120.00  108
 42  \w     44.00 102.00   0.50   14.00    --  117.50-125.00  30.00  116
 43  \w     43.00  97.00   0.50   14.00    --  117.50-115.00 -61.17  108
 44  \w     44.00 102.00   0.50   14.00    --  117.50-125.00 -60.00  116
 45  \w    103.00 136.00   0.50   14.00    --  117.50  15.00 -30.00   66
 46  \w    103.00 136.00   0.50   14.00    --  117.50  15.00-180.00   66
 47  \w     44.00  92.00   0.50   14.00    --  117.50 -95.00  60.00   96
 48  \w     44.00  92.00   0.50   14.00    --  117.50 -95.00 120.00   96
 49  \w     44.00 102.00   0.50   14.00    --  117.50-125.00 -30.00  116
 50  \w    124.00 178.00   0.50   14.00    --  117.50  77.00  90.00  108
 51  \w    103.00 136.00   0.50   14.00    --  117.50  15.00 120.00   66
 52  \w    103.00 136.00   0.50   14.00    --  117.50  15.00 150.00   66
 53  \w    109.00 178.00   0.50   14.00    --  117.50  61.00 120.00  138
 54  \w     44.00  95.00   0.50   14.00    --  117.50 -91.00  42.18  102
 55  \w    105.00 178.00   0.50   14.00    --  117.50  45.00-120.00  146
 56  \w    104.00 166.00   0.50   14.00    --  117.50  30.00-180.00  124
 57  \w     44.00  75.00   0.50   14.00    --  117.50 -77.00  60.00   62
 58  \w     44.00  75.00   0.50   14.00    --  117.50 -77.00-150.00   62
 59  \w     44.00  95.00   0.50   14.00    --  117.50 -88.00 178.01  102
 60  \w    104.00 166.00   0.50   14.00    --  117.50  30.00  60.00  124
 61  \w    112.00 178.00   0.50   14.00    --  117.50 125.00  90.00  132
 62  \w     44.00 102.00   0.50   14.00    --  117.50-125.00  90.00  116
 63  \w     44.00  75.00   0.50   14.00    --  117.50 -77.00 120.00   62
 64  \w     44.00 102.00   0.50   14.00    --  117.50-125.00  60.00  116
 65  \w     44.00  75.00   0.50   14.00    --  117.50 -77.00 -90.00   62
 66  \w    124.00 178.00   0.50   14.00    --  117.50  77.00-180.00  108
 67  \w     44.00  92.00   0.50   14.00    --  117.50 -95.00 -90.00   96
 68  \w     44.00  95.00   0.50   14.00    --  117.50 -90.00-144.50  102
 69  \w     44.00  92.00   0.50   14.00    --  117.50 -95.00-150.00   96
 70  \w    103.00 136.00   0.50   14.00    --  117.50  15.00  90.00   66
 71  \w     44.00  92.00   0.50   14.00    --  117.50 -95.00 -60.00   96
 72  \w     44.00  75.00   0.50   14.00    --  117.50 -77.00-120.00   62
 73  \w    -19.00  34.00   0.50    3.00    --  -43.21  38.00-150.00  106
 74  \w    -19.00  34.00   0.50    3.00    --  -43.21  38.00 120.00  106
 75  \w    -19.00  34.00   0.50    3.00    --  -43.21  38.00-180.00  106
 76  \w     28.00  59.00   0.50    3.00    --   43.21  59.00  62.91   62
 77  \w     27.00  54.00   0.50    3.00    --   43.21  61.00 103.79   54
 78  \w     27.00  54.00   0.50    3.00    --   43.21  61.00-119.29   54
 79  \w     27.00  54.00   0.50    3.00    --   43.21  61.00  14.36   54
;
_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      -0.1180557000
_diffrn_orient_matrix_UB_12      0.0711672000
_diffrn_orient_matrix_UB_13      0.0137898000
_diffrn_orient_matrix_UB_21      0.0478991000
_diffrn_orient_matrix_UB_22      -0.0221316000
_diffrn_orient_matrix_UB_23      0.0548770000
_diffrn_orient_matrix_UB_31      0.0858865000
_diffrn_orient_matrix_UB_32      0.0785132000
_diffrn_orient_matrix_UB_33      -0.0165635000
_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  0.0190
_diffrn_reflns_av_unetI/netI     0.0110
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            78576
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.972
_diffrn_reflns_theta_min         3.105
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.495
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62531
_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            colorless
_exptl_crystal_density_diffrn    1.377
_exptl_crystal_description       block
_exptl_crystal_F_000             1672
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.637
_refine_diff_density_min         -0.880
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     907
_refine_ls_number_reflns         16540
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0280
_refine_ls_R_factor_gt           0.0276
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0379P)^2^+3.4223P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0751
_refine_ls_wR_factor_ref         0.0754
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16229
_reflns_number_total             16540
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01217a2.cif
_cod_data_source_block           felix246
_cod_depositor_comments
'Adding full bibliography for 7719171--7719173.cif.'
_cod_database_code               7719172
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         C42H41MoO3P3Si
_chemical_oxdiff_usercomment     'niels michaelis  NM112'
_reflns_odcompleteness_completeness 98.70
_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(H1A,H1B), C2(H2A,H2B), C15(H15A,H15B), C16(H16A,H16B), C51(H51A,H51B),
 C52(H52A,H52B), C65(H65A,H65B), C66(H66A,H66B)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C10(H10), C11(H11), C12(H12),
 C13(H13), C14(H14), 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), C54(H54), C55(H55), C56(H56), C57(H57), C58(H58), C60(H60), C61(H61),
  C62(H62), C63(H63), C64(H64), C68(H68), C69(H69), C70(H70), C71(H71),
 C72(H72), C74(H74), C75(H75), C76(H76), C77(H77), C78(H78), C80(H80), C81(H81),
  C83(H83), C84(H84)
2.c Idealised Me refined as rotating group:
 C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C87(H87A,H87B,
 H87C), C88(H88A,H88B,H88C), C89(H89A,H89B,H89C)
;
_shelx_res_checksum              12109
_shelx_hkl_checksum              20015
_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 1.311
_oxdiff_exptl_absorpt_empirical_full_min 0.845