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_7720347
_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         'C15 H10 N4 O'
_chemical_formula_sum            'C15 H10 N4 O'
_chemical_formula_weight         262.27
_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                 99.628(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.5623(8)
_cell_length_b                   17.4548(12)
_cell_length_c                   7.0682(4)
_cell_measurement_reflns_used    4057
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      75.7740
_cell_measurement_theta_min      4.9100
_cell_volume                     1284.76(15)
_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 0.992
_diffrn_measured_fraction_theta_max 0.992
_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   -120.00 -94.00   0.50    0.50    --  -49.47 -77.00 -90.00   52
  2  \w    -62.00  20.00   0.50    0.50    --  -49.47  57.00 -60.00  164
  3  \w    -20.00  19.00   0.50    0.50    --  -49.47  19.00  60.00   78
  4  \w    -20.00  24.00   0.50    0.50    --  -49.47  19.00-180.00   88
  5  \w    -47.00 -15.00   0.50    0.50    --  -49.47 125.00 150.00   64
  6  \w    -88.00 -62.00   0.50    0.50    --  -49.47 125.00 150.00   52
  7  \w    -23.00   2.00   0.50    0.50    --  -49.47  19.00 120.00   50
  8  \w     -5.00  23.00   0.50    0.50    --   49.47 -19.00  90.00   56
  9  \w   -114.00 -77.00   0.50    2.00    --  -90.00 -57.00 120.00   74
 10  \w    -53.00 -20.00   0.50    2.00    --  -90.00  57.00 -90.00   66
 11  \w    -64.00 -20.00   0.50    2.00    --  -90.00  57.00  90.00   88
 12  \w   -159.00-102.00   0.50    2.00    --  -90.00 -77.00-120.00  114
 13  \w    -91.00 -42.00   0.50    2.00    --  -90.00 125.00 150.00   98
 14  \w   -118.00 -89.00   0.50    2.00    --  -90.00 -77.00   0.00   58
 15  \w   -160.00-123.00   0.50    2.00    --  -90.00 -77.00   0.00   74
 16  \w   -161.00-119.00   0.50    2.00    --  -90.00 -57.00 120.00   84
 17  \w   -161.00-111.00   0.50    2.00    --  -90.00   0.00 -30.00  100
 18  \w    -92.00 -64.00   0.50    2.00    --  -90.00   0.00 -30.00   56
 19  \w     73.00 106.00   0.50    2.00    --  104.64 -99.00 -60.00   66
 20  \w     34.00  65.00   0.50    2.00    --  104.64 -57.00   0.00   62
 21  \w     36.00  61.00   0.50    2.00    --  104.64 -99.00 -60.00   50
 22  \w     81.00 120.00   0.50    2.00    --  104.64 -77.00   0.00   78
 23  \w     33.00  62.00   0.50    2.00    --  104.64 -57.00 150.00   58
 24  \w     97.00 172.00   0.50    2.00    --  104.64  37.00  90.00  150
 25  \w     36.00  66.00   0.50    2.00    --  104.64 -57.00 -60.00   60
 26  \w     37.00  70.00   0.50    2.00    --  104.64 -99.00-180.00   66
 27  \w     36.00 107.00   0.50    2.00    --  104.64 -99.00-120.00  142
 28  \w     41.00  66.00   0.50    2.00    --  104.64 -57.00 -90.00   50
 29  \w     61.00 117.00   0.50    2.00    --  104.64-125.00 150.00  112
 30  \w     33.00  66.00   0.50    2.00    --  104.64 -57.00 -30.00   66
 31  \w     66.00 117.00   0.50    2.00    --  104.64-125.00  60.00  102
;
_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      0.0633514000
_diffrn_orient_matrix_UB_12      0.0778627000
_diffrn_orient_matrix_UB_13      0.0574258000
_diffrn_orient_matrix_UB_21      0.1335540000
_diffrn_orient_matrix_UB_22      -0.0363881000
_diffrn_orient_matrix_UB_23      0.0066171000
_diffrn_orient_matrix_UB_31      -0.0045013000
_diffrn_orient_matrix_UB_32      0.0202159000
_diffrn_orient_matrix_UB_33      -0.2133940000
_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  0.0874
_diffrn_reflns_av_unetI/netI     0.0699
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            9496
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        66.587
_diffrn_reflns_theta_max         66.587
_diffrn_reflns_theta_min         4.246
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.732
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.711
_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            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.356
_exptl_crystal_description       needle
_exptl_crystal_F_000             544
_exptl_crystal_size_max          0.204
_exptl_crystal_size_mid          0.075
_exptl_crystal_size_min          0.069
_refine_diff_density_max         0.208
_refine_diff_density_min         -0.216
_refine_diff_density_rms         0.053
_refine_ls_extinction_coef       0.0078(12)
_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   0.998
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     182
_refine_ls_number_reflns         2267
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.0719
_refine_ls_R_factor_gt           0.0513
_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^)+(0.0868P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1311
_refine_ls_wR_factor_ref         0.1472
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1639
_reflns_number_total             2267
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d6dt00469e2.cif
_cod_data_source_block           ksk578a-orange_prism3_mod-gg
_cod_depositor_comments
'Adding full bibliography for 7720347--7720357.cif.'
_cod_database_code               7720347
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C15 H10 N4 O'
_diffrn_oxdiff_digest_hkl
;
43101fca3bcdc0473d7d93da84f42bbf584931
;
_diffrn_oxdiff_digest_od_ed
;

;
_diffrn_oxdiff_measurement_exp_name KSK578A-orange_prism3.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:
 C16(H16), C12(H12), C15(H15), C22(H22), C14(H14), C26(H26), C13(H13),
 C23(H23), C24(H24), C25(H25)
;
_shelx_res_checksum              33035
_shelx_hkl_checksum              65655
_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 2.635
_oxdiff_exptl_absorpt_empirical_full_min 0.669