Monolayers of a thiacalix[3]pyridine-supported molybdenum(0) tricarbonyl complex on Au(111): characterisation with surface spectroscopy and scanning tunneling microscopy.
Clausen, Kai Uwe; Meng, Xiangzhi; Reisig, Katrin; Näther, Christian; Strunskus, Thomas; Berndt, Richard; Tuczek, Felix; Dalton transactions (Cambridge, England : 2003) 53 (2024) 18304–18312; doi:10.1039/d4dt02521k

data_7717281
_publ_section_title
;
 Monolayers of a thiacalix[3]pyridine-supported molybdenum(0) tricarbonyl
 complex on Au(111): characterisation with surface spectroscopy and
 scanning tunneling microscopy.
;
_journal_issue                   45
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              18304
_journal_page_last               18312
_journal_paper_doi               10.1039/d4dt02521k
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C18 H9 Mo N3 O3 S3, C H3 O0.5 S0.5'
_chemical_formula_sum            'C19 H12 Mo N3 O3.5 S3.5'
_chemical_formula_weight         546.47
_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             2021-08-16
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2020.03.28 svn.rd84adfe8 for Rigaku Oxford Diffraction, GUI svn.r6032)
;
_audit_update_record
;
2024-06-27 deposited with the CCDC.	2024-10-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.4270(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   33.1665(2)
_cell_length_b                   10.32120(10)
_cell_length_c                   12.45270(10)
_cell_measurement_reflns_used    46113
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      79.7880
_cell_measurement_theta_min      2.8160
_cell_volume                     4020.09(6)
_computing_cell_refinement       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.112a (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      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 1.000
_diffrn_measured_fraction_theta_max 0.993
_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    -72.00 -35.00   0.50    3.00    --  -47.79 -38.00  90.00   74
  2  \w    -68.00 -25.00   0.50    3.00    --  -47.79 -77.00  30.00   86
  3  \w    -67.00 -35.00   0.50    3.00    --  -47.79 -38.00   0.00   64
  4  \w   -117.00 -91.00   0.50    3.00    --  -47.79 -38.00   0.00   52
  5  \w    -66.00 -25.00   0.50    3.00    --  -47.79 -77.00-180.00   82
  6  \w    -80.00 -25.00   0.50    3.00    --  -47.79 -77.00-120.00  110
  7  \w    -62.00  24.00   0.50    3.00    --  -47.79  57.00-180.00  172
  8  \w    -68.00 -26.00   0.50    3.00    --  -47.79 -77.00 -60.00   84
  9  \w   -106.00 -81.00   0.50    3.00    --  -47.79 -77.00 120.00   50
 10  \w    -95.00 -69.00   0.50    3.00    --  -47.79 -77.00-180.00   52
 11  \w    -93.00 -37.00   0.50    3.00    --  -47.79 -38.00-180.00  112
 12  \w   -120.00 -40.00   0.50    3.00    --  -47.79 -38.00  60.00  160
 13  \w    -62.00 -26.00   0.50    3.00    --  -47.79 -77.00  90.00   72
 14  \w    -81.00 -25.00   0.50    3.00    --  -47.79 -77.00 -30.00  112
 15  \w   -117.00 -76.00   0.50    3.00    --  -47.79 -38.00  90.00   82
 16  \w    -55.00 -25.00   0.50    3.00    --  -47.79 -77.00 120.00   60
 17  \w     35.00  93.00   0.50    3.00    --   47.79-125.00  60.00  116
 18  \w     37.00  62.00   0.50    3.00    --   47.79  38.00   0.00   50
 19  \w     33.00  59.00   0.50    3.00    --   47.79  57.00 120.00   52
 20  \w     39.00 109.00   0.50    3.00    --   47.79  19.00-120.00  140
 21  \w     33.00  68.00   0.50    3.00    --   47.79  57.00-120.00   70
 22  \w     85.00 121.00   0.50    3.00    --   47.79  38.00   0.00   72
 23  \w     32.00  89.00   0.50    3.00    --   47.79-122.00 -28.00  114
 24  \w    -95.00 -69.00   0.50    9.00    --  -91.75 -77.00  30.00   52
 25  \w   -160.00-134.00   0.50    9.00    --  -91.75 -68.00-151.52   52
 26  \w    -97.00 -71.00   0.50    9.00    --  -91.75 -71.00  66.16   52
 27  \w   -155.00-129.00   0.50    9.00    --  -91.75 -71.00  66.16   52
 28  \w    -96.00 -70.00   0.50    9.00    --  -91.75 -77.00   0.00   52
 29  \w    -95.00 -69.00   0.50    9.00    --  -91.75 -77.00 150.00   52
 30  \w   -120.00 -69.00   0.50    9.00    --  -91.75 -77.00 -90.00  102
 31  \w   -100.00 -74.00   0.50    9.00    --  -91.75 -63.00  79.73   52
 32  \w    -96.00 -70.00   0.50    9.00    --  -91.75 -75.00 164.70   52
 33  \w    -95.00 -69.00   0.50    9.00    --  -91.75 -77.00  90.00   52
 34  \w    -95.00 -69.00   0.50    9.00    --  -91.75 -77.00  60.00   52
 35  \w    -97.00 -72.00   0.50    9.00    --  -91.75 -70.00-115.05   50
 36  \w    -95.00 -69.00   0.50    9.00    --  -91.75 -77.00 -60.00   52
 37  \w   -154.00-128.00   0.50    9.00    --  -91.75 -70.00-115.05   52
 38  \w    -97.00 -71.00   0.50    9.00    --  -91.75 -74.00 -25.00   52
 39  \w   -163.00-138.00   0.50    9.00    --  -91.75 -68.00 179.11   50
 40  \w    -98.00 -73.00   0.50    9.00    --  -91.75 -67.00  93.02   50
 41  \w   -162.00-136.00   0.50    9.00    --  -91.75 -74.00 -25.00   52
 42  \w    -95.00 -70.00   0.50    9.00    --  -91.75 -74.00 128.33   50
 43  \w    -98.00 -72.00   0.50    9.00    --  -91.75 -73.00  13.28   52
 44  \w    -99.00 -73.00   0.50    9.00    --  -91.75 -68.00 179.11   52
 45  \w    -95.00 -69.00   0.50    9.00    --  -91.75 -77.00 -37.61   52
 46  \w    -95.00 -70.00   0.50    9.00    --  -91.75 -74.00 115.26   50
 47  \w    -99.00 -73.00   0.50    9.00    --  -91.75 -68.00-170.50   52
 48  \w    -95.00 -69.00   0.50    9.00    --  -91.75 -77.00-150.00   52
 49  \w   -162.00-134.00   0.50    9.00    --  -91.75 -65.00  -6.09   56
 50  \w    -95.00 -69.00   0.50    9.00    --  -91.75 -77.00-120.00   52
 51  \w   -104.00 -78.00   0.50    9.00    --  -91.75 -60.00  21.19   52
 52  \w   -100.00 -74.00   0.50    9.00    --  -91.75 -65.00  -6.09   52
 53  \w   -100.00 -71.00   0.50    9.00    --  -91.75 -73.00 -80.47   58
 54  \w    -94.00 -69.00   0.50    9.00    --  -91.75 -77.00-180.00   50
 55  \w   -101.00 -75.00   0.50    9.00    --  -91.75 -61.00 -33.88   52
 56  \w   -157.00-131.00   0.50    9.00    --  -91.75 -73.00 -80.47   52
 57  \w    -96.00 -70.00   0.50    9.00    --  -91.75 -74.00 154.60   52
 58  \w   -101.00 -70.00   0.50    9.00    --  -91.75 -74.00 -70.92   62
 59  \w   -152.00-126.00   0.50    9.00    --  -91.75 -70.00 -54.72   52
 60  \w    -96.00 -71.00   0.50    9.00    --  -91.75 -73.00-136.02   50
 61  \w    -98.00 -73.00   0.50    9.00    --  -91.75 -68.00-151.52   50
 62  \w   -163.00-124.00   0.50    9.00    --  -91.75 -63.00  79.73   78
 63  \w    -97.00 -72.00   0.50    9.00    --  -91.75 -70.00 -54.72   50
 64  \w   -116.00 -72.00   0.50    9.00    --  -91.75 -69.00  37.53   88
 65  \w    -97.00 -71.00   0.50    9.00    --  -91.75 -72.00 116.73   52
 66  \w   -162.00-124.00   0.50    9.00    --  -91.75 -74.00 115.26   76
 67  \w     94.00 124.00   0.50    9.00    --  113.25  77.00 -30.00   60
 68  \w    100.00 152.00   0.50    9.00    --  113.25  61.00 150.00  104
 69  \w    100.00 166.00   0.50    9.00    --  113.25  61.00  60.00  132
 70  \w    128.00 161.00   0.50    9.00    --  113.25 125.00 -60.00   66
 71  \w     98.00 125.00   0.50    9.00    --  113.25 125.00 -60.00   54
 72  \w     81.00 106.00   0.50    9.00    --  113.25-102.00-107.92   50
 73  \w     42.00 106.00   0.50    9.00    --  113.25 -95.00  90.00  128
 74  \w    136.00 170.00   0.50    9.00    --  113.25  61.00-180.00   68
 75  \w     45.00  74.00   0.50    9.00    --  113.25-102.00-107.92   58
 76  \w     98.00 132.00   0.50    9.00    --  113.25  61.00-180.00   68
 77  \w    100.00 159.00   0.50    9.00    --  113.25  61.00 -60.00  118
 78  \w     99.00 169.00   0.50    9.00    --  113.25  61.00-150.68  140
 79  \w     48.00 108.00   0.50    9.00    --  113.25-125.00   0.00  120
 80  \w     92.00 176.00   0.50    9.00    --  113.25  77.00  30.00  168
 81  \w     66.00 106.00   0.50    9.00    --  113.25 -98.00 -17.25   80
 82  \w     98.00 177.00   0.50    9.00    --  113.25  61.00   0.00  158
 83  \w    139.00 168.00   0.50    9.00    --  113.25  61.00-120.00   58
 84  \w     99.00 135.00   0.50    9.00    --  113.25  61.00-120.00   72
 85  \w     81.00 106.00   0.50    9.00    --  113.25 -95.00 150.00   50
 86  \w     42.00  69.00   0.50    9.00    --  113.25 -95.00 150.00   54
 87  \w     42.00  90.00   0.50    9.00    --  113.25 -77.00 -90.00   96
 88  \w    103.00 148.00   0.50    9.00    --  113.25  61.00  30.00   90
 89  \w     46.00  71.00   0.50    9.00    --  113.25 -61.00 120.00   50
 90  \w    101.00 168.00   0.50    9.00    --  113.25  61.00 120.00  134
 91  \w    126.00 177.00   0.50    9.00    --  113.25  77.00 150.00  102
 92  \w     93.00 119.00   0.50    9.00    --  113.25  77.00 150.00   52
 93  \w     97.00 171.00   0.50    9.00    --  113.25  61.00 -90.00  148
 94  \w     92.00 148.00   0.50    9.00    --  113.25  77.00  90.00  112
 95  \w     92.00 170.00   0.50    9.00    --  113.25  77.00 -60.00  156
 96  \w     80.00 106.00   0.50    9.00    --  113.25 -95.00  60.00   52
 97  \w    139.00 178.00   0.50    9.00    --  113.25  77.00-180.00   78
 98  \w     43.00  74.00   0.50    9.00    --  113.25 -95.00  60.00   62
 99  \w     94.00 123.00   0.50    9.00    --  113.25  77.00-180.00   58
100  \w     79.00 106.00   0.50    9.00    --  113.25 -95.00-180.00   54
101  \w     93.00 133.00   0.50    9.00    --  113.25  77.00  60.00   80
102  \w    152.00 178.00   0.50    9.00    --  113.25  77.00  60.00   52
103  \w     51.00  76.00   0.50    9.00    --  113.25 -95.00-180.00   50
104  \w     95.00 136.00   0.50    9.00    --  113.25  77.00 -90.00   82
105  \w     42.00  68.00   0.50    9.00    --  113.25-125.00 -60.00   52
106  \w     63.00 106.00   0.50    9.00    --  113.25 -95.00  30.00   86
107  \w    136.00 178.00   0.50    9.00    --  113.25  61.00  90.00   84
108  \w     42.00  94.00   0.50    9.00    --  113.25 -95.00-120.00  104
109  \w    105.00 130.00   0.50    9.00    --  113.25  61.00 -30.00   50
110  \w     97.00 131.00   0.50    9.00    --  113.25  61.00  90.00   68
111  \w     92.00 144.00   0.50    9.00    --  113.25  77.00   0.00  104
112  \w    142.00 177.00   0.50    9.00    --  113.25  77.00-150.00   70
113  \w     91.00 127.00   0.50    9.00    --  113.25  77.00-150.00   72
114  \w    131.00 177.00   0.50    9.00    --  113.25  77.00 120.00   92
115  \w     92.00 126.00   0.50    9.00    --  113.25  77.00 120.00   68
116  \w     46.00  71.00   0.50    9.00    --  113.25 -77.00   0.00   50
117  \w     56.00 103.00   0.50    9.00    --  113.25 -95.00-150.00   94
118  \w     43.00 105.00   0.50    9.00    --  113.25 -95.00 -90.00  124
119  \w     77.00 104.00   0.50    9.00    --  113.25 -95.00   0.00   54
120  \w     78.00 106.00   0.50    9.00    --  113.25 -95.00 120.00   56
121  \w     42.00  73.00   0.50    9.00    --  113.25 -95.00   0.00   62
122  \w     96.00 177.00   0.50    9.00    --  113.25  77.00-120.00  162
123  \w     42.00  72.00   0.50    9.00    --  113.25 -95.00 120.00   60
124  \w    144.00 176.00   0.50    9.00    --  113.25  77.00 -30.00   64
;
_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      0.0232003000
_diffrn_orient_matrix_UB_12      0.0055968000
_diffrn_orient_matrix_UB_13      -0.0478702000
_diffrn_orient_matrix_UB_21      -0.1166772000
_diffrn_orient_matrix_UB_22      0.0432136000
_diffrn_orient_matrix_UB_23      -0.0104102000
_diffrn_orient_matrix_UB_31      0.0344631000
_diffrn_orient_matrix_UB_32      0.1427702000
_diffrn_orient_matrix_UB_33      0.0050163000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0227
_diffrn_reflns_av_unetI/netI     0.0079
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            61942
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         80.032
_diffrn_reflns_theta_min         2.825
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.014
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54987
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.112a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.806
_exptl_crystal_description       needle
_exptl_crystal_F_000             2184
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.409
_refine_diff_density_min         -0.587
_refine_diff_density_rms         0.067
_refine_ls_extinction_coef       0.000091(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         4358
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0201
_refine_ls_R_factor_gt           0.0199
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0270P)^2^+8.7791P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0528
_refine_ls_wR_factor_ref         0.0530
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4324
_reflns_number_total             4358
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02521k2.cif
_cod_data_source_block           felix218
_cod_depositor_comments          'Adding full bibliography for 7717281.cif.'
_cod_original_formula_sum        'C19 H12 Mo N3 O3.50 S3.50'
_cod_database_code               7717281
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         C18H9N3S3MoO3
_chemical_oxdiff_usercomment     'KU Clausen  KR019'
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid body (RIGU) restrains
 S51, C51, C52
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 S51', C51', C52'
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3. Same fragment restrains
{S51, C51, C52} sigma for 1-2: 0.02, 1-3: 0.04
as in
{S51', C51', C52'}
4. Others
 Fixed Sof: S51(0.25) C51(0.25) H51A(0.25) H51B(0.25) H51C(0.25) C52(0.25)
 H52A(0.25) H52B(0.25) H52C(0.25) S51'(0.25) C51'(0.25) H51D(0.25) H51E(0.25)
 H51F(0.25) C52'(0.25) H52D(0.25) H52E(0.25) H52F(0.25)
5.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C12(H12), C13(H13), C14(H14)
5.b Idealised Me refined as rotating group:
 C51(H51A,H51B,H51C), C52(H52A,H52B,H52C), C51'(H51D,H51E,H51F), C52'(H52D,
 H52E,H52F)
;
_shelx_res_checksum              99766
_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 1.614
_oxdiff_exptl_absorpt_empirical_full_min 0.785