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_7720355
_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         'C34 H32 B Cl3 Mo N2 P'
_chemical_formula_sum            'C34 H32 B Cl3 Mo N2 P'
_chemical_formula_weight         712.68
_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             2025-12-05
_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                91.7045(5)
_cell_angle_beta                 97.5172(7)
_cell_angle_gamma                118.0068(10)
_cell_formula_units_Z            2
_cell_length_a                   9.72725(10)
_cell_length_b                   10.29523(9)
_cell_length_c                   18.78662(10)
_cell_measurement_reflns_used    37946
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      76.3740
_cell_measurement_theta_min      2.3540
_cell_volume                     1637.81(3)
_computing_cell_refinement       'CrysAlisPro 1.171.44.117a (Rigaku OD, 2025)'
_computing_data_collection
'CrysAlisPro system (CCD 44.108a 64-bit (release 25-04-2025))'
_computing_data_reduction        'CrysAlisPro 1.171.44.117a (Rigaku OD, 2025)'
_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(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.940
_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   -103.00 -18.00   0.50    2.00    --  -49.50 140.00   2.00  170
  2  \w   -121.00 -68.00   0.50    2.00    --  -49.50-129.00 116.00  106
  3  \w   -121.00 -60.00   0.50    2.00    --  -49.50-140.00 -56.00  122
  4  \w    -77.00 -52.00   0.50    2.00    --  -49.50 129.00-170.00   50
  5  \w     40.00 104.00   0.50    2.00    --   49.50-140.00 -56.00  128
  6  \w     34.00  95.00   0.50    2.00    --   49.50-129.00 116.00  122
  7  \w    -81.00 -47.00   0.50    8.00    --  -90.00 140.00   2.00   68
  8  \w    -76.00 -51.00   0.50    8.00    --  -90.00 129.00-170.00   50
  9  \w   -161.00-136.00   0.50    8.00    --  -90.00-140.00 -56.00   50
 10  \w   -139.00-114.00   0.50    8.00    --  -90.00-129.00 116.00   50
 11  \w     98.00 128.00   0.50    8.00    --  104.61-140.00 -56.00   60
 12  \w    109.00 134.00   0.50    8.00    --  104.61 129.00-170.00   50
 13  \w    104.00 140.00   0.50    8.00    --  104.61 140.00   2.00   72
 14  \w     42.00 107.00   0.50    8.00    --  104.61-129.00 116.00  130
 15  \w    -90.00 -42.00   0.50    2.00    --  -49.50 -37.00 150.00   96
 16  \w    -80.00 -37.00   0.50    2.00    --  -49.50 -57.00 150.00   86
 17  \w   -121.00 -96.00   0.50    2.00    --  -49.50 -57.00  90.00   50
 18  \w    -84.00 -38.00   0.50    2.00    --  -49.50 -57.00  90.00   92
 19  \w    -63.00 -37.00   0.50    2.00    --  -49.50 -57.00-180.00   52
 20  \w   -108.00 -37.00   0.50    2.00    --  -49.50 -57.00  30.00  142
 21  \w   -111.00 -39.00   0.50    2.00    --  -49.50 -57.00-150.00  144
 22  \w    -84.00 -37.00   0.50    2.00    --  -49.50 -57.00 -30.00   94
 23  \w   -115.00 -89.00   0.50    2.00    --  -49.50 -57.00 150.00   52
 24  \w    -65.00 -40.00   0.50    2.00    --  -49.50 -46.00  85.31   50
 25  \w   -120.00 -94.00   0.50    2.00    --  -49.50 -57.00  60.00   52
 26  \w    -79.00 -37.00   0.50    2.00    --  -49.50 -57.00  60.00   84
 27  \w    -86.00 -37.00   0.50    2.00    --  -49.50 -57.00-120.00   98
 28  \w    -96.00 -43.00   0.50    2.00    --  -49.50 -37.00 -90.00  106
 29  \w     37.00  72.00   0.50    2.00    --   49.50  57.00  90.00   70
 30  \w     37.00  77.00   0.50    2.00    --   49.50  57.00 -30.00   80
 31  \w     37.00  75.00   0.50    2.00    --   49.50  57.00  60.00   76
 32  \w     38.00  64.00   0.50    2.00    --   49.50  57.00 -60.00   52
 33  \w     37.00  74.00   0.50    2.00    --   49.50  57.00   0.00   74
 34  \w     37.00  66.00   0.50    2.00    --   49.50  57.00 -90.00   58
 35  \w     44.00  71.00   0.50    2.00    --   49.50  37.00 -30.00   54
 36  \w     43.00  87.00   0.50    2.00    --   49.50  19.00 -30.00   88
 37  \w     37.00  62.00   0.50    2.00    --   49.50  57.00-180.00   50
 38  \w   -101.00 -74.00   0.50    8.00    --  -90.00 -64.00-136.45   54
 39  \w   -109.00 -74.00   0.50    8.00    --  -90.00 -65.00-162.19   70
 40  \w   -161.00 -75.00   0.50    8.00    --  -90.00 -62.00-125.81  172
 41  \w   -103.00 -77.00   0.50    8.00    --  -90.00 -57.00 150.00   52
 42  \w   -159.00-117.00   0.50    8.00    --  -90.00 -64.00-136.45   84
 43  \w   -161.00 -75.00   0.50    8.00    --  -90.00 -62.00  81.17  172
 44  \w   -102.00 -76.00   0.50    8.00    --  -90.00 -63.00 -51.24   52
 45  \w    -99.00 -74.00   0.50    8.00    --  -90.00 -66.00  15.09   50
 46  \w   -115.00 -75.00   0.50    8.00    --  -90.00 -62.00  86.76   80
 47  \w   -157.00 -78.00   0.50    8.00    --  -90.00 -55.00 -48.90  158
 48  \w   -132.00 -74.00   0.50    8.00    --  -90.00 -64.00  -8.16  116
 49  \w   -107.00 -76.00   0.50    8.00    --  -90.00 -62.00   2.47   62
 50  \w   -100.00 -74.00   0.50    8.00    --  -90.00 -64.00 133.99   52
 51  \w   -108.00 -78.00   0.50    8.00    --  -90.00 -61.00-100.27   60
 52  \w   -161.00-121.00   0.50    8.00    --  -90.00 -66.00  15.09   80
 53  \w   -100.00 -74.00   0.50    8.00    --  -90.00 -66.00  48.56   52
 54  \w   -100.00 -74.00   0.50    8.00    --  -90.00 -66.00-103.84   52
 55  \w   -119.00 -76.00   0.50    8.00    --  -90.00 -59.00 -32.59   86
 56  \w   -154.00-125.00   0.50    8.00    --  -90.00 -59.00 -32.59   58
 57  \w   -161.00-116.00   0.50    8.00    --  -90.00 -63.00 169.97   90
 58  \w   -160.00 -75.00   0.50    8.00    --  -90.00 -63.00 -84.75  170
 59  \w   -108.00 -77.00   0.50    8.00    --  -90.00 -59.00 101.51   62
 60  \w   -121.00 -76.00   0.50    8.00    --  -90.00 -59.00-159.67   90
 61  \w   -161.00 -74.00   0.50    8.00    --  -90.00 -66.00  58.62  174
 62  \w   -161.00-129.00   0.50    8.00    --  -90.00 -66.00  48.56   64
 63  \w   -149.00-119.00   0.50    8.00    --  -90.00 -64.00 116.07   60
 64  \w   -111.00 -75.00   0.50    8.00    --  -90.00 -64.00 116.07   72
 65  \w   -157.00-116.00   0.50    8.00    --  -90.00 -66.00-165.83   82
 66  \w   -109.00 -74.00   0.50    8.00    --  -90.00 -66.00-165.83   70
 67  \w   -103.00 -78.00   0.50    8.00    --  -90.00 -55.00 136.45   50
 68  \w   -126.00 -74.00   0.50    8.00    --  -90.00 -65.00  68.69  104
 69  \w   -161.00 -76.00   0.50    8.00    --  -90.00 -62.00 -67.05  170
 70  \w   -101.00 -75.00   0.50    8.00    --  -90.00 -62.00 123.51   52
 71  \w   -160.00-131.00   0.50    8.00    --  -90.00 -57.00 150.00   58
 72  \w   -149.00-123.00   0.50    8.00    --  -90.00 -62.00 123.51   52
 73  \w   -153.00-112.00   0.50    8.00    --  -90.00 -59.00 101.51   82
 74  \w   -161.00-134.00   0.50    8.00    --  -90.00 -66.00  39.63   54
 75  \w   -119.00 -74.00   0.50    8.00    --  -90.00 -66.00  39.63   90
 76  \w   -107.00 -75.00   0.50    8.00    --  -90.00 -63.00 169.97   64
 77  \w     33.00 105.00   0.50    8.00    --  104.61 -99.00-150.00  144
 78  \w     66.00 110.00   0.50    8.00    --  104.61 -99.00   0.00   88
 79  \w     33.00  60.00   0.50    8.00    --  104.61 -99.00   0.00   54
 80  \w     33.00  63.00   0.50    8.00    --  104.61 -57.00 -90.00   60
 81  \w     34.00  66.00   0.50    8.00    --  104.61 -57.00   0.00   64
 82  \w     73.00 105.00   0.50    8.00    --  104.61 -77.00 -90.00   64
 83  \w     67.00 106.00   0.50    8.00    --  104.61 -99.00 -90.00   78
 84  \w     33.00  66.00   0.50    8.00    --  104.61 -57.00  60.00   66
 85  \w     68.00 105.00   0.50    8.00    --  104.61 -99.00 120.00   74
 86  \w     36.00  62.00   0.50    8.00    --  104.61 -99.00 120.00   52
 87  \w     33.00  68.00   0.50    8.00    --  104.61 -77.00 -90.00   70
 88  \w     35.00  65.00   0.50    8.00    --  104.61 -57.00 -30.00   60
 89  \w     65.00 104.00   0.50    8.00    --  104.61 -77.00 120.00   78
 90  \w     33.00  61.00   0.50    8.00    --  104.61 -77.00 120.00   56
 91  \w     33.00  63.00   0.50    8.00    --  104.61 -57.00 120.00   60
;
_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      -0.0517163000
_diffrn_orient_matrix_UB_12      -0.0292317000
_diffrn_orient_matrix_UB_13      0.0745670000
_diffrn_orient_matrix_UB_21      -0.1694616000
_diffrn_orient_matrix_UB_22      -0.1092530000
_diffrn_orient_matrix_UB_23      -0.0367235000
_diffrn_orient_matrix_UB_31      0.0409466000
_diffrn_orient_matrix_UB_32      -0.1274762000
_diffrn_orient_matrix_UB_33      0.0027938000
_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  0.0365
_diffrn_reflns_av_unetI/netI     0.0158
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.940
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            45508
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.940
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.780
_diffrn_reflns_theta_min         2.385
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.187
_exptl_absorpt_correction_T_max  0.906
_exptl_absorpt_correction_T_min  0.353
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.44.117a (Rigaku Oxford Diffraction, 2025)
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            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.445
_exptl_crystal_description       plate
_exptl_crystal_F_000             726
_exptl_crystal_size_max          0.319
_exptl_crystal_size_mid          0.138
_exptl_crystal_size_min          0.118
_refine_diff_density_max         0.301
_refine_diff_density_min         -0.623
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         6496
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0276
_refine_ls_R_factor_gt           0.0270
_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^)+(0.0424P)^2^+0.8448P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0734
_refine_ls_wR_factor_ref         0.0738
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6309
_reflns_number_total             6496
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d6dt00469e2.cif
_cod_data_source_block           ksk527-gg
_cod_depositor_comments
'Adding full bibliography for 7720347--7720357.cif.'
_cod_database_code               7720355
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C34 H32 B Cl3 Mo N2 P'
_diffrn_oxdiff_digest_hkl
;
43cfcabcbe7add7fe20f8d0e3785bfc27b71ee
;
_diffrn_oxdiff_digest_od_ed
;

;
_diffrn_oxdiff_measurement_exp_name KSK527.par
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Ternary CH refined with riding coordinates:
 C12(H12)
2.b Secondary CH2 refined with riding coordinates:
 C13(H13a,H13b), C16(H16a,H16b), C14(H14a,H14b), C15(H15a,H15b)
2.c Aromatic/amide H refined with riding coordinates:
 C22(H22), C26(H26), C36(H36), C46(H46), C23(H23), C32(H32), C25(H25),
 C42(H42), C35(H35), C8(H8), C24(H24), C2(H2), C44(H44), C9(H9), C11(H11),
 C34(H34), C33(H33), C10(H10), C5(H5), C43(H43), C45(H45), C3(H3), C4(H4)
;
_shelx_res_checksum              1122
_shelx_hkl_checksum              41151
_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 1.746
_oxdiff_exptl_absorpt_empirical_full_min 0.688