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_7720349
_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         'C30 H20 N2'
_chemical_formula_sum            'C30 H20 N2'
_chemical_formula_weight         408.48
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 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                   16.0842(2)
_cell_length_b                   5.47310(10)
_cell_length_c                   23.5249(3)
_cell_measurement_reflns_used    18583
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      75.4590
_cell_measurement_theta_min      3.7710
_cell_volume                     2070.91(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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.99(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   -118.00 -80.00   0.50    5.00    --  -46.16-125.00  90.00   76
  2  \w    -91.00 -10.00   0.50    5.00    --  -46.16 125.00  60.00  162
  3  \w     89.00 118.00   0.50    5.00    --   46.16  77.00  60.00   58
  4  \w     89.00 118.00   0.50    5.00    --   46.16  77.00 -60.00   58
  5  \w    -26.00  64.00   0.50    5.00    --   46.16 -57.00-150.00  180
  6  \w     89.00 118.00   0.50    5.00    --   46.16  77.00-180.00   58
  7  \w     89.00 118.00   0.50    5.00    --   46.16  77.00-150.00   58
  8  \w    -28.00  41.00   0.50    5.00    --   46.16 -37.00 -90.00  138
  9  \w     31.00  96.00   0.50    5.00    --   46.16-125.00  90.00  130
 10  \w     89.00 118.00   0.50    5.00    --   46.16  77.00 150.00   58
 11  \w   -119.00 -20.00   0.50   20.00    --  -93.75  77.00  60.00  198
 12  \w    -72.00 -20.00   0.50   20.00    --  -93.75  61.00 120.00  104
 13  \w   -171.00 -72.00   0.50   20.00    --  -93.75 -15.00  60.00  198
 14  \w    -50.00 -20.00   0.50   20.00    --  -93.75  45.00 -30.00   60
 15  \w    -50.00 -20.00   0.50   20.00    --  -93.75  45.00 150.00   60
 16  \w    -50.00 -20.00   0.50   20.00    --  -93.75  45.00 -60.00   60
 17  \w    -50.00 -20.00   0.50   20.00    --  -93.75  45.00  90.00   60
 18  \w   -119.00 -20.00   0.50   20.00    --  -93.75  77.00  60.00  198
 19  \w    -72.00 -20.00   0.50   20.00    --  -93.75  61.00 150.00  104
 20  \w    -50.00 -20.00   0.50   20.00    --  -93.75  45.00   0.00   60
 21  \w    -72.00 -20.00   0.50   20.00    --  -93.75  61.00-120.00  104
 22  \w    -72.00 -20.00   0.50   20.00    --  -93.75  61.00 -60.00  104
 23  \w   -171.00 -72.00   0.50   20.00    --  -93.75 -15.00 -30.00  198
 24  \w    -72.00 -20.00   0.50   20.00    --  -93.75  61.00 -90.00  104
 25  \w     92.00 178.00   0.50   20.00    --  105.45 125.00   0.00  172
 26  \w     32.00 108.00   0.50   20.00    --  105.45 -94.00-180.00  152
 27  \w     32.00  72.00   0.50   20.00    --  105.45 -61.00   0.00   80
 28  \w     32.00 108.00   0.50   20.00    --  105.45 -94.00  30.00  152
 29  \w     84.00 178.00   0.50   20.00    --  105.45  15.00-150.00  188
 30  \w     32.00 108.00   0.50   20.00    --  105.45 -94.00 -60.00  152
 31  \w     32.00 108.00   0.50   20.00    --  105.45 -94.00  90.00  152
 32  \w     32.00 108.00   0.50   20.00    --  105.45 -94.00-120.00  152
 33  \w     32.00 108.00   0.50   20.00    --  105.45 -94.00 150.00  152
 34  \w     29.00 102.00   0.50    5.00    --   46.16  57.00 -60.00  146
 35  \w     29.00 118.00   0.50    5.00    --   46.16  57.00 150.00  178
;
_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      -0.0225135000
_diffrn_orient_matrix_UB_12      0.0029863000
_diffrn_orient_matrix_UB_13      0.0652621000
_diffrn_orient_matrix_UB_21      0.0377449000
_diffrn_orient_matrix_UB_22      0.0949095000
_diffrn_orient_matrix_UB_23      -0.0012899000
_diffrn_orient_matrix_UB_31      -0.2779222000
_diffrn_orient_matrix_UB_32      0.0126353000
_diffrn_orient_matrix_UB_33      -0.0054501000
_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  0.0412
_diffrn_reflns_av_unetI/netI     0.0239
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            29264
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.724
_diffrn_reflns_theta_min         3.758
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.590
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85641
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.44.117a (Rigaku Oxford Diffraction, 2025)
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    1.310
_exptl_crystal_description       plate
_exptl_crystal_F_000             856
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.339
_refine_diff_density_min         -0.179
_refine_diff_density_rms         0.046
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.7(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         4114
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0436
_refine_ls_R_factor_gt           0.0416
_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^)+(0.0869P)^2^+0.0954P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1095
_refine_ls_wR_factor_ref         0.1119
_reflns_Friedel_coverage         0.892
_reflns_Friedel_fraction_full    0.980
_reflns_Friedel_fraction_max     0.925
_reflns_number_gt                3877
_reflns_number_total             4114
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d6dt00469e2.cif
_cod_data_source_block           ksk551r-newfm-gg
_cod_depositor_comments
'Adding full bibliography for 7720347--7720357.cif.'
_cod_database_code               7720349
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C30 H20 N2'
_shelx_estimated_absorpt_t_max   0.965
_shelx_estimated_absorpt_t_min   0.852
_diffrn_oxdiff_digest_hkl
;
43a4218317a9b4ac104c6d1791227b70d9a3f1
;
_diffrn_oxdiff_digest_od_ed
;

;
_diffrn_oxdiff_measurement_exp_name KSK551R-newFM.par
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.3(8)
 0.7(8)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C32(H32), C8(H8), C10(H10), C27(H27), C7(H7), C12(H12), C31(H31),
 C9(H9), C11(H11), C15(H15), C24(H24), C33(H33), C30(H30), C13(H13), C35(H35),
 C28(H28), C29(H29), C14(H14), C34(H34)
;
_shelx_res_checksum              30455
_shelx_hkl_checksum              15892
_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 2.329
_oxdiff_exptl_absorpt_empirical_full_min 0.562