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_7720352
_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 H20 O6'
_chemical_formula_sum            'C20 H20 O6'
_chemical_formula_weight         356.36
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 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                90
_cell_angle_beta                 105.593(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.2982(2)
_cell_length_b                   11.5691(3)
_cell_length_c                   10.7137(3)
_cell_measurement_reflns_used    5088
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      74.5790
_cell_measurement_theta_min      5.7280
_cell_volume                     871.30(4)
_computing_cell_refinement       'CrysAlisPro 1.171.44.117a (Rigaku OD, 2025)'
_computing_data_collection
'CrysAlisPro system (CCD 44.113a 64-bit (release 02-06-2025))'
_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 0.999
_diffrn_measured_fraction_theta_max 0.960
_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     93.00 118.00   0.50    0.08    --   44.59  77.00 120.00   50
  2  \w     89.00 114.00   0.50    0.08    --   44.59  77.00  60.00   50
  3  \w     89.00 117.00   0.50    0.08    --   44.59  77.00-120.00   56
  4  \w     89.00 118.00   0.50    0.08    --   44.59  77.00-150.00   58
  5  \w     93.00 122.00   0.50    0.32    --  105.77 125.00 -90.00   58
  6  \w    130.00 165.00   0.50    0.32    --  105.77 125.00 -90.00   70
  7  \w    138.00 169.00   0.50    0.32    --  105.77 125.00   0.00   62
  8  \w    100.00 133.00   0.50    0.32    --  105.77 125.00   0.00   66
  9  \w    146.00 175.00   0.50    0.32    --  105.77  45.00  60.00   58
 10  \w    104.00 174.00   0.50    0.32    --  105.77  61.00 120.00  140
 11  \w     85.00 124.00   0.50    0.32    --  105.77  45.00  60.00   78
 12  \w     52.00  93.00   0.50    0.08    --   44.59-125.00 120.00   82
 13  \w     35.00  95.00   0.50    0.08    --   44.59-125.00  90.00  120
 14  \w     74.00 105.00   0.50    0.32    --  105.77 -94.00 -60.00   62
 15  \w     38.00  70.00   0.50    0.32    --  105.77 -94.00 -60.00   64
 16  \w     51.00  76.00   0.50    0.32    --  105.77-125.00-120.00   50
 17  \w     90.00 117.00   0.50    0.32    --  105.77-125.00-120.00   54
 18  \w     35.00 115.00   0.50    0.32    --  105.77-125.00-180.00  160
 19  \w     59.00  93.00   0.50    0.32    --  105.77 -94.00  60.00   68
 20  \w     32.00 120.00   0.50    0.32    --  105.77 -77.00 -60.00  176
 21  \w    -31.00  31.00   0.50    0.08    --   44.59 -37.00-150.00  124
 22  \w    -32.00  23.00   0.50    0.08    --   44.59 -19.00   0.00  110
 23  \w   -118.00 -93.00   0.50    0.08    --  -44.59 -77.00 150.00   50
 24  \w   -118.00 -93.00   0.50    0.08    --  -44.59 -77.00  90.00   50
 25  \w    -95.00 -23.00   0.50    0.32    --  -96.00 139.00 145.00  144
 26  \w   -165.00-137.00   0.50    0.32    --  -96.00 -61.00   0.00   56
 27  \w   -132.00 -79.00   0.50    0.32    --  -96.00 -61.00   0.00  106
 28  \w   -154.00 -99.00   0.50    0.32    --  -96.00 -94.00 -30.00  110
 29  \w   -118.00 -93.00   0.50    0.08    --  -44.59-125.00-180.00   50
 30  \w   -150.00 -95.00   0.50    0.32    --  -96.00-125.00 -90.00  110
 31  \w    -47.00 -21.00   0.50    0.32    --  -96.00  45.00 120.00   52
 32  \w    -48.00 -21.00   0.50    0.32    --  -96.00  45.00  90.00   54
 33  \w    -50.00 -25.00   0.50    0.32    --  -96.00  45.00  30.00   50
 34  \w    -48.00 -22.00   0.50    0.32    --  -96.00  45.00   0.00   52
 35  \w    -50.00 -21.00   0.50    0.32    --  -96.00  45.00 -30.00   58
 36  \w    -50.00 -22.00   0.50    0.32    --  -96.00  45.00 -90.00   56
 37  \w    -50.00 -25.00   0.50    0.32    --  -96.00  45.00-150.00   50
;
_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      0.1942570000
_diffrn_orient_matrix_UB_12      0.0560521000
_diffrn_orient_matrix_UB_13      0.0078450000
_diffrn_orient_matrix_UB_21      0.0919338000
_diffrn_orient_matrix_UB_22      -0.1207023000
_diffrn_orient_matrix_UB_23      0.0095719000
_diffrn_orient_matrix_UB_31      -0.0427910000
_diffrn_orient_matrix_UB_32      -0.0047498000
_diffrn_orient_matrix_UB_33      -0.1487531000
_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  0.0622
_diffrn_reflns_av_unetI/netI     0.0595
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            7953
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.036
_diffrn_reflns_theta_min         5.745
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.834
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.235
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.358
_exptl_crystal_description       irregular
_exptl_crystal_F_000             376
_exptl_crystal_size_max          0.472
_exptl_crystal_size_mid          0.285
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.306
_refine_diff_density_min         -0.414
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.131
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     120
_refine_ls_number_reflns         1725
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.131
_refine_ls_R_factor_all          0.0611
_refine_ls_R_factor_gt           0.0582
_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^)+(0.0826P)^2^+0.1797P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1417
_refine_ls_wR_factor_ref         0.1452
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1572
_reflns_number_total             1725
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d6dt00469e2.cif
_cod_data_source_block           ksk590d2-4-gg
_cod_depositor_comments
'Adding full bibliography for 7720347--7720357.cif.'
_cod_database_code               7720352
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C10 H10 O3'
_diffrn_oxdiff_digest_hkl
;
4309c62a721cf427b2bed41571463aa35141d5
;
_diffrn_oxdiff_digest_od_ed
;

;
_diffrn_oxdiff_measurement_exp_name KSK590D2-4.par
_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.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C7(H7), C6(H6)
2.b Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C8(H8A,H8B,H8C)
;
_shelx_res_checksum              11490
_shelx_hkl_checksum              44011
_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 2.245
_oxdiff_exptl_absorpt_empirical_full_min 0.546