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_7720357
_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         'C45 H30 N4 O3'
_chemical_formula_sum            'C45 H30 N4 O3'
_chemical_formula_weight         674.73
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.79123(8)
_cell_length_b                   16.54087(14)
_cell_length_c                   19.00846(16)
_cell_measurement_reflns_used    38095
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      74.3290
_cell_measurement_theta_min      2.6550
_cell_volume                     3392.94(5)
_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 1.000
_diffrn_measured_fraction_theta_max 0.984
_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   -116.00 -45.00   0.50    3.00    --  -43.12-164.00 137.00  142
  2  \w    -86.00  -3.00   0.50    3.00    --  -43.12 116.00  14.00  166
  3  \w   -118.00 -29.00   0.50    3.00    --  -43.12 164.00 162.00  178
  4  \w     25.00  92.00   0.50    3.00    --   43.12-116.00 -74.00  134
  5  \w     68.00 115.00   0.50    3.00    --   43.12 164.00 162.00   94
  6  \w     51.00 123.00   0.50    3.00    --   43.12-164.00 137.00  144
  7  \w   -144.00 -45.00   0.50   12.00    --  -96.00-164.00 137.00  198
  8  \w    -87.00 -21.00   0.50   12.00    --  -96.00 116.00  14.00  132
  9  \w   -171.00 -76.00   0.50   12.00    --  -96.00-116.00 -74.00  190
 10  \w   -118.00 -29.00   0.50   12.00    --  -96.00 164.00 162.00  178
 11  \w     67.00 161.00   0.50   12.00    --  106.61 164.00 162.00  188
 12  \w     51.00 144.00   0.50   12.00    --  106.61-164.00 137.00  186
 13  \w     98.00 178.00   0.50   12.00    --  106.61 116.00  14.00  160
 14  \w     32.00 112.00   0.50   12.00    --  106.61-116.00 -74.00  160
 15  \w   -116.00 -89.00   0.50    3.00    --  -43.12 -77.00  90.00   54
 16  \w   -116.00 -89.00   0.50    3.00    --  -43.12 -77.00 120.00   54
 17  \w   -116.00 -89.00   0.50    3.00    --  -43.12 -77.00  30.00   54
 18  \w   -116.00 -89.00   0.50    3.00    --  -43.12 -77.00-180.00   54
 19  \w    -23.00  38.00   0.50    3.00    --  -43.12  19.00 -90.00  122
 20  \w   -117.00 -80.00   0.50    3.00    --  -43.12-125.00   0.00   74
 21  \w   -116.00 -89.00   0.50    3.00    --  -43.12 -77.00 -30.00   54
 22  \w   -117.00 -80.00   0.50    3.00    --  -43.12-125.00 -30.00   74
 23  \w     89.00 116.00   0.50    3.00    --   43.12  77.00 -90.00   54
 24  \w     89.00 116.00   0.50    3.00    --   43.12  77.00 -60.00   54
 25  \w     89.00 116.00   0.50    3.00    --   43.12  77.00-120.00   54
 26  \w     89.00 116.00   0.50    3.00    --   43.12  77.00 -30.00   54
 27  \w   -170.00 -89.00   0.50   12.00    --  -96.00 -77.00  30.00  162
 28  \w   -170.00 -80.00   0.50   12.00    --  -96.00-125.00 -30.00  180
 29  \w    -50.00 -20.00   0.50   12.00    --  -96.00  45.00-180.00   60
 30  \w    -50.00 -20.00   0.50   12.00    --  -96.00  45.00 -30.00   60
 31  \w   -170.00 -89.00   0.50   12.00    --  -96.00 -77.00 -60.00  162
 32  \w    -50.00 -20.00   0.50   12.00    --  -96.00  45.00  60.00   60
 33  \w    -50.00 -20.00   0.50   12.00    --  -96.00  45.00-150.00   60
 34  \w   -172.00 -74.00   0.50   12.00    --  -96.00 -45.00-150.00  196
 35  \w    -50.00 -20.00   0.50   12.00    --  -96.00  45.00   0.00   60
 36  \w   -170.00 -72.00   0.50   12.00    --  -96.00 -61.00   0.00  196
 37  \w   -172.00 -74.00   0.50   12.00    --  -96.00 -45.00-150.00  196
 38  \w     33.00  72.00   0.50   12.00    --  106.61 -61.00 -30.00   78
 39  \w     33.00 109.00   0.50   12.00    --  106.61 -94.00  30.00  152
 40  \w     33.00 116.00   0.50   12.00    --  106.61-125.00-120.00  166
 41  \w     33.00 109.00   0.50   12.00    --  106.61 -94.00 120.00  152
 42  \w     92.00 177.00   0.50   12.00    --  106.61 125.00  90.00  170
 43  \w     42.00  72.00   0.50   12.00    --  106.61 -61.00 -90.00   60
 44  \w     85.00 111.00   0.50   12.00    --  106.61  45.00 -60.00   52
 45  \w     92.00 132.00   0.50   12.00    --  106.61 125.00  90.00   80
 46  \w     92.00 149.00   0.50   12.00    --  106.61 125.00-120.00  114
 47  \w    143.00 178.00   0.50   12.00    --  106.61 125.00 -30.00   70
 48  \w     96.00 126.00   0.50   12.00    --  106.61 125.00 -30.00   60
 49  \w    125.00 152.00   0.50   12.00    --  106.61  45.00 -60.00   54
 50  \w     39.00  71.00   0.50   12.00    --  106.61 -61.00 -60.00   64
 51  \w     68.00 102.00   0.50   12.00    --  106.61 -94.00 -90.00   68
 52  \w     34.00  85.00   0.50   12.00    --  106.61 -94.00 150.00  102
 53  \w     40.00  66.00   0.50   12.00    --  106.61 -61.00 150.00   52
;
_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      -0.0255987000
_diffrn_orient_matrix_UB_12      0.0465142000
_diffrn_orient_matrix_UB_13      0.0687025000
_diffrn_orient_matrix_UB_21      0.0008848000
_diffrn_orient_matrix_UB_22      0.0803191000
_diffrn_orient_matrix_UB_23      -0.0410516000
_diffrn_orient_matrix_UB_31      -0.1404148000
_diffrn_orient_matrix_UB_32      -0.0079343000
_diffrn_orient_matrix_UB_33      -0.0127819000
_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  0.0397
_diffrn_reflns_av_unetI/netI     0.0160
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            61590
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.725
_diffrn_reflns_theta_min         3.542
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.668
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.232
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.321
_exptl_crystal_description       prism
_exptl_crystal_F_000             1408
_exptl_crystal_size_max          0.353
_exptl_crystal_size_mid          0.288
_exptl_crystal_size_min          0.214
_refine_diff_density_max         0.129
_refine_diff_density_min         -0.130
_refine_diff_density_rms         0.025
_refine_ls_abs_structure_details
;
 Flack x determined using 2660 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.06(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     469
_refine_ls_number_reflns         6805
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0334
_refine_ls_R_factor_gt           0.0307
_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^)+(0.0469P)^2^+0.3111P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0834
_refine_ls_wR_factor_ref         0.0871
_reflns_Friedel_coverage         0.770
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.963
_reflns_number_gt                6363
_reflns_number_total             6805
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d6dt00469e2.cif
_cod_data_source_block           ksk578a-yell-prism-gg
_cod_depositor_comments
'Adding full bibliography for 7720347--7720357.cif.'
_cod_database_code               7720357
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C45 H30 N4 O3'
_diffrn_oxdiff_digest_hkl
;
436074310452e30824b46aa45cdea9cecb8b6a
;
_diffrn_oxdiff_digest_od_ed
;

;
_diffrn_oxdiff_measurement_exp_name KSK578A-yell-hex3-baby-orange_prism.par
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C26(H26), C52(H52), C32(H32), C16(H16), C36(H36), C42(H42), C33(H33),
 C25(H25), C12(H12), C54(H54), C62(H62), C63(H63), C46(H46), C66(H66), C53(H53),
  C44(H44), C22(H22), C14(H14), C56(H56), C43(H43), C13(H13), C15(H15),
 C55(H55), C35(H35), C45(H45), C34(H34), C24(H24), C65(H65), C64(H64), C23(H23)
;
_shelx_res_checksum              4922
_shelx_hkl_checksum              91580
_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 1.619
_oxdiff_exptl_absorpt_empirical_full_min 0.714