Molybdenum(VI) borano-imido complexes and their application as Lewis acid catalysts in homocoupling of diazo compounds
Škoch, Karel; Buziková, Michaela; Jakubczyk, Michal; Pattanamcheril Anilkumar, Krishna; Demel, Jan; Litecká, Miroslava; Dalton Transactions  (2026) –; doi:10.1039/D6DT00469E

data_7720354
_publ_section_title
;
 Molybdenum(VI) borano-imido complexes and their application as Lewis acid
 catalysts in homocoupling of diazo compounds.
;
_journal_issue                   12
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4997
_journal_page_last               5003
_journal_paper_doi               10.1039/d6dt00469e
_journal_volume                  55
_journal_year                    2026
_chemical_formula_moiety         'C20 H25 B Cl4 Mo N2 O'
_chemical_formula_sum            'C20 H25 B Cl4 Mo N2 O'
_chemical_formula_weight         557.97
_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             2025-12-04
_audit_creation_method
;
Olex2 1.5-ac7-016
(compiled 2025.05.29 svn.r8cd99b3d for Rigaku Oxford Diffraction, GUI svn.r7254)
;
_audit_update_record
;
2026-01-05 deposited with the CCDC.	2026-02-26 downloaded from the CCDC.
;
_cell_angle_alpha                75.817(6)
_cell_angle_beta                 89.591(4)
_cell_angle_gamma                76.111(5)
_cell_formula_units_Z            2
_cell_length_a                   9.4421(5)
_cell_length_b                   10.6384(9)
_cell_length_c                   12.3347(3)
_cell_measurement_reflns_used    9260
_cell_measurement_temperature    100.00(12)
_cell_measurement_theta_max      70.2830
_cell_measurement_theta_min      3.7070
_cell_volume                     1164.36(13)
_computing_cell_refinement       'CrysAlisPro 1.171.43.105a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 43.104a 64-bit (release 22-12-2023))'
_computing_data_reduction        'CrysAlisPro 1.171.43.105a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.5-ac7-016 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac7-016 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(12)
_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 0.994
_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    -98.00 -73.00   0.50   16.00    --  -49.30 -48.00 137.00   50
  2  \w    -19.00   8.00   0.50   16.00    --   49.30 -48.00 137.00   54
  3  \w     67.00 119.00   0.50   16.00    --   49.30  48.00 -75.00  104
  4  \w     16.00  47.00   0.50   16.00    --   49.30 -48.00 137.00   62
  5  \w    -50.00 -20.00   0.50   64.00    --  -90.00  48.00 -75.00   60
  6  \w   -161.00-109.00   0.50   64.00    --  -90.00 -48.00 137.00  104
  7  \w    122.00 148.00   0.50   64.00    --  107.39  48.00 -75.00   52
  8  \w    -33.00  -8.00   0.50   16.00    --    6.00 119.00  90.59   50
  9  \w    -71.00 -42.00   0.50   16.00    --  -14.00 157.00 134.97   58
 10  \w    -11.00  14.00   0.50   16.00    --   18.00  95.00  18.15   50
 11  \w     -5.00  20.00   0.50   16.00    --   22.00  91.00-135.40   50
 12  \w     14.00  39.00   0.50   16.00    --   34.00  75.00 120.93   50
 13  \w     18.00  43.00   0.50   16.00    --   34.00  73.00 -42.03   50
 14  \w     14.00  39.00   0.50   16.00    --   34.00  75.00-120.10   50
 15  \w     20.00  45.00   0.50   16.00    --   38.00  70.00 -71.45   50
 16  \w     21.00  46.00   0.50   16.00    --   38.00  69.00 139.21   50
 17  \w     21.00  46.00   0.50   16.00    --   38.00  69.00  24.76   50
 18  \w     30.00  56.00   0.50   16.00    --   46.00  65.00  90.93   52
 19  \w     78.00 105.00   0.50   16.00    --   46.00  65.00  90.93   54
 20  \w     30.00  63.00   0.50   16.00    --   46.00  66.00 173.12   66
 21  \w    -38.00   1.00   0.50   16.00    --  -49.30  48.00 -75.00   78
 22  \w     42.00  93.00   0.50   16.00    --   49.30-125.00 -60.00  102
 23  \w     34.00  88.00   0.50   16.00    --   50.00  66.00 -65.21  108
 24  \w     34.00  60.00   0.50   16.00    --   50.00  66.00  22.40   52
 25  \w     38.00  67.00   0.50   16.00    --   54.00  66.00  46.54   58
 26  \w     42.00  68.00   0.50   16.00    --   58.00  65.00-147.81   52
 27  \w     42.00  67.00   0.50   16.00    --   58.00  67.00 172.64   50
 28  \w     81.00 107.00   0.50   16.00    --   58.00  67.00  99.43   52
 29  \w     42.00  68.00   0.50   16.00    --   58.00  67.00  83.62   52
 30  \w     42.00  75.00   0.50   16.00    --   58.00  67.00-129.83   66
 31  \w     45.00  72.00   0.50   16.00    --   58.00  65.00 131.23   54
 32  \w     42.00  68.00   0.50   16.00    --   58.00  67.00 -35.42   52
 33  \w     43.00  68.00   0.50   16.00    --   58.00  67.00  99.43   50
 34  \w     82.00 107.00   0.50   16.00    --   58.00  67.00 172.64   50
 35  \w     85.00 110.00   0.50   16.00    --   58.00  65.00-147.81   50
 36  \w     48.00  73.00   0.50   16.00    --   62.00  66.00 -21.14   50
 37  \w    -79.00 -50.00   0.50   16.00    --  -66.00 -66.00 -42.14   58
 38  \w    -79.00 -54.00   0.50   16.00    --  -70.00 -66.00 161.56   50
 39  \w   -139.00-105.00   0.50   16.00    --  -70.00 -66.00  94.40   68
 40  \w   -141.00-115.00   0.50   16.00    --  -70.00 -63.00-125.64   52
 41  \w    -81.00 -55.00   0.50   16.00    --  -70.00 -66.00  20.90   52
 42  \w    -85.00 -55.00   0.50   16.00    --  -70.00 -63.00-125.64   60
 43  \w    -81.00 -54.00   0.50   16.00    --  -70.00 -66.00  94.40   54
 44  \w    -84.00 -58.00   0.50   16.00    --  -74.00 -64.00-101.05   52
 45  \w    -85.00 -59.00   0.50   16.00    --  -74.00 -65.00 153.19   52
 46  \w    -85.00 -58.00   0.50   16.00    --  -74.00 -64.00  68.15   54
 47  \w    -83.00 -58.00   0.50   16.00    --  -74.00 -66.00 -84.04   50
 48  \w    -85.00 -59.00   0.50   16.00    --  -74.00 -63.00  -4.81   52
 49  \w    -89.00 -63.00   0.50   16.00    --  -78.00 -64.00 122.90   52
 50  \w    -91.00 -62.00   0.50   16.00    --  -78.00 -64.00-131.09   58
 51  \w    -87.00 -62.00   0.50   16.00    --  -78.00 -65.00  47.09   50
 52  \w    -90.00 -64.00   0.50   16.00    --  -78.00 -59.00 -56.64   52
 53  \w   -150.00-125.00   0.50   64.00    --  -82.00 -63.00-168.25   50
 54  \w    -97.00 -67.00   0.50   64.00    --  -82.00 -63.00-168.25   60
 55  \w    -94.00 -69.00   0.50   64.00    --  -82.00 -59.00 134.55   50
 56  \w    -93.00 -66.00   0.50   64.00    --  -82.00 -64.00 -32.62   54
 57  \w    -98.00 -72.00   0.50   64.00    --  -86.00 -62.00 120.98   52
 58  \w   -158.00-118.00   0.50   64.00    --  -86.00 -62.00 120.98   80
 59  \w   -148.00-117.00   0.50   64.00    --  -86.00 -66.00  65.54   62
 60  \w    -98.00 -72.00   0.50   64.00    --  -86.00 -64.00  84.96   52
 61  \w    -96.00 -70.00   0.50   64.00    --  -86.00 -66.00  65.54   52
 62  \w   -144.00-119.00   0.50   64.00    --  -90.00 -61.00 -67.54   50
 63  \w   -111.00 -86.00   0.50   64.00    --  -90.00  77.00  90.00   50
 64  \w   -108.00 -75.00   0.50   64.00    --  -90.00 -62.00 155.85   66
 65  \w   -158.00-127.00   0.50   64.00    --  -90.00 -63.00 103.46   62
 66  \w   -106.00 -81.00   0.50   64.00    --  -90.00 -59.00  -7.40   50
 67  \w   -115.00 -76.00   0.50   64.00    --  -90.00 -63.00 103.46   78
 68  \w   -160.00-128.00   0.50   64.00    --  -90.00 -59.00  -7.40   64
 69  \w   -156.00-121.00   0.50   64.00    --  -90.00 -65.00  29.74   70
 70  \w   -105.00 -80.00   0.50   64.00    --  -90.00 -59.00  47.75   50
 71  \w   -151.00-125.00   0.50   64.00    --  -90.00 -64.00  20.53   52
 72  \w   -161.00-126.00   0.50   64.00    --  -90.00 -59.00  47.75   70
 73  \w   -106.00 -75.00   0.50   64.00    --  -90.00 -63.00  11.80   62
 74  \w   -161.00-125.00   0.50   64.00    --  -90.00 -63.00  11.80   72
 75  \w   -106.00 -75.00   0.50   64.00    --  -90.00 -62.00 -86.87   62
 76  \w   -109.00 -75.00   0.50   64.00    --  -90.00 -62.00 170.87   68
 77  \w   -150.00-124.00   0.50   64.00    --  -90.00 -62.00 170.87   52
 78  \w   -104.00 -78.00   0.50   64.00    --  -90.00 -68.00-131.89   52
 79  \w   -140.00-111.00   0.50   64.00    --  -90.00 -68.00-131.89   58
 80  \w    -49.00 -23.00   0.50   64.00    --  -90.00  57.00-150.00   52
 81  \w   -112.00 -74.00   0.50   64.00    --  -90.00 -65.00 -36.01   76
 82  \w   -100.00 -75.00   0.50   64.00    --  -90.00 -63.00-129.69   50
 83  \w   -158.00-126.00   0.50   64.00    --  -90.00 -59.00-155.67   64
 84  \w   -159.00-116.00   0.50   64.00    --  -90.00 -63.00-129.69   86
 85  \w   -160.00-134.00   0.50   64.00    --  -90.00 -65.00 -36.01   52
 86  \w    -99.00 -74.00   0.50   64.00    --  -90.00 -64.00  20.53   50
 87  \w   -102.00 -77.00   0.50   64.00    --  -90.00 -57.00 -60.00   50
 88  \w   -105.00 -76.00   0.50   64.00    --  -90.00 -59.00-155.67   58
 89  \w   -161.00-113.00   0.50   64.00    --  -90.00 -57.00 -60.00   96
 90  \w   -138.00 -78.00   0.50   64.00    --  -90.00 -54.00 133.65  120
 91  \w    -99.00 -74.00   0.50   64.00    --  -90.00 -65.00  29.74   50
 92  \w   -107.00 -77.00   0.50   64.00    --  -90.00 -58.00  72.40   60
 93  \w   -159.00-114.00   0.50   64.00    --  -90.00 -58.00  72.40   90
 94  \w    -62.00 -18.00   0.50   64.00    --  -90.00  57.00  90.00   88
 95  \w   -117.00 -76.00   0.50   64.00    --  -90.00 -63.00-105.93   82
 96  \w   -146.00-121.00   0.50   64.00    --  -90.00 -63.00-105.93   50
 97  \w   -115.00 -77.00   0.50   64.00    --  -90.00 -61.00 -67.54   76
 98  \w    -70.00 -22.00   0.50   64.00    --  -90.00  77.00  90.00   96
 99  \w     42.00  86.00   0.50   64.00    --  107.39 -99.00 -60.00   88
100  \w     36.00  66.00   0.50   64.00    --  107.39 -57.00 -30.00   60
101  \w     37.00  62.00   0.50   64.00    --  107.39 -57.00  90.00   50
102  \w     40.00  65.00   0.50   64.00    --  107.39 -57.00   0.00   50
103  \w     80.00 116.00   0.50   64.00    --  107.39-125.00   0.00   72
104  \w     39.00  65.00   0.50   64.00    --  107.39 -57.00 -60.00   52
105  \w     41.00  68.00   0.50   64.00    --  107.39-125.00   0.00   54
106  \w     51.00 110.00   0.50   64.00    --  107.39 -99.00-120.00  118
107  \w     43.00 109.00   0.50   64.00    --  107.39 -99.00  30.00  132
108  \w     38.00  64.00   0.50   64.00    --  107.39 -57.00 -90.00   52
109  \w     36.00  61.00   0.50   64.00    --  107.39 -57.00-150.00   50
110  \w     95.00 164.00   0.50   64.00    --  107.39  57.00-150.00  138
111  \w     36.00  65.00   0.50   64.00    --  107.39 -57.00-180.00   58
112  \w     41.00 116.00   0.50   64.00    --  107.39-125.00-180.00  150
113  \w     69.00 109.00   0.50   64.00    --  107.39-125.00 150.00   80
114  \w     45.00 109.00   0.50   64.00    --  107.39 -99.00-180.00  128
;
_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      -0.1094809000
_diffrn_orient_matrix_UB_12      0.1277176000
_diffrn_orient_matrix_UB_13      -0.0660180000
_diffrn_orient_matrix_UB_21      0.1275077000
_diffrn_orient_matrix_UB_22      0.0639601000
_diffrn_orient_matrix_UB_23      -0.0396350000
_diffrn_orient_matrix_UB_31      0.0094806000
_diffrn_orient_matrix_UB_32      -0.0578039000
_diffrn_orient_matrix_UB_33      -0.1035194000
_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  0.1551
_diffrn_reflns_av_unetI/netI     0.0697
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            27278
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        66.593
_diffrn_reflns_theta_max         66.593
_diffrn_reflns_theta_min         3.702
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.943
_exptl_absorpt_correction_T_max  0.859
_exptl_absorpt_correction_T_min  0.652
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.105a (Rigaku Oxford Diffraction, 2024)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.591
_exptl_crystal_description       plate
_exptl_crystal_F_000             564
_exptl_crystal_size_max          0.075
_exptl_crystal_size_mid          0.058
_exptl_crystal_size_min          0.035
_refine_diff_density_max         0.904
_refine_diff_density_min         -1.818
_refine_diff_density_rms         0.164
_refine_ls_extinction_coef       0.0077(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.153
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     282
_refine_ls_number_reflns         4091
_refine_ls_number_restraints     61
_refine_ls_restrained_S_all      1.145
_refine_ls_R_factor_all          0.1351
_refine_ls_R_factor_gt           0.0922
_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^)+(0.1525P)^2^+2.7268P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2416
_refine_ls_wR_factor_ref         0.2995
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2716
_reflns_number_total             4091
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d6dt00469e2.cif
_cod_data_source_block           ksk457-gg
_cod_depositor_comments
'Adding full bibliography for 7720347--7720357.cif.'
_cod_original_cell_volume        1164.36(12)
_cod_database_code               7720354
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'B C20 Cl4 Mo N2 O'
_diffrn_oxdiff_digest_hkl
;
0131048aaf4350d6962927370328d2c0c09b27
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C14A-C13A
 1.521 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C12A) = Uanis(C12B)
Uanis(C16A) = Uanis(C16B)
Uanis(C15B) = Uanis(C15A)
Uanis(C13A) = Uanis(C13B)
Uanis(C14A) = Uanis(C14B)
Uanis(C12B) = Uanis(C12A)
4. Rigid body (RIGU) restrains
 C12A, C12B, C13B, C13A, C14B, C14A, C15A, C15B, C16A, C16B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C12A)=Sof(H12A)=1-FVAR(1)
 Sof(C12B)=Sof(H12B)=FVAR(1)
 Sof(C16B)=Sof(H16C)=Sof(H16D)=1-FVAR(2)
 Sof(C16A)=Sof(H16A)=Sof(H16B)=FVAR(2)
 Sof(C15B)=Sof(H15C)=Sof(H15D)=1-FVAR(3)
 Sof(C15A)=Sof(H15A)=Sof(H15B)=FVAR(3)
 Sof(C13A)=Sof(H13A)=Sof(H13B)=1-FVAR(4)
 Sof(C13B)=Sof(H13C)=Sof(H13D)=FVAR(4)
 Fixed Sof: C14B(0.5) H14A(0.5) H14B(0.5) C14A(0.5) H14C(0.5) H14D(0.5)
6.a Ternary CH refined with riding coordinates:
 C12A(H12A), C12B(H12B)
6.b Secondary CH2 refined with riding coordinates:
 C23(H23A,H23B), C24(H24A,H24B), C21(H21A,H21B), C22(H22A,H22B), C13A(H13A,
 H13B), C16A(H16A,H16B), C15A(H15A,H15B), C13B(H13C,H13D), C16B(H16C,H16D),
 C14B(H14A,H14B), C15B(H15C,H15D), C14A(H14C,H14D)
6.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C11(H11), C10(H10), C5(H5), C3(H3), C4(H4), C8(H8), C9(H9)
;
_shelx_res_checksum              59141
_shelx_hkl_checksum              70928
_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 3.488
_oxdiff_exptl_absorpt_empirical_full_min 0.324