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_7720350
_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         'C18 H17 N3'
_chemical_formula_sum            'C18 H17 N3'
_chemical_formula_weight         275.34
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 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                 94.456(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.3007(3)
_cell_length_b                   14.2372(3)
_cell_length_c                   10.7745(3)
_cell_measurement_reflns_used    4826
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      73.6510
_cell_measurement_theta_min      3.0980
_cell_volume                     1422.40(7)
_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 0.993
_diffrn_measured_fraction_theta_max 0.929
_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     45.00  72.00   0.50    0.16    --  106.61 -61.00 -60.00   54
  2  \w     47.00  72.00   0.50    0.16    --  106.61 -61.00  30.00   50
  3  \w     39.00  68.00   0.50    0.16    --  106.61 -61.00  60.00   58
  4  \w     41.00  66.00   0.50    0.16    --  106.61 -61.00 120.00   50
  5  \w     37.00  62.00   0.50    0.16    --  106.61 -61.00 150.00   50
  6  \w     33.00  61.00   0.50    0.16    --  106.61 -55.00 -80.00   56
  7  \w    117.00 142.00   0.50    0.16    --  106.61  55.00  62.00   50
  8  \w     92.00 117.00   0.50    0.16    --  106.61 125.00-120.00   50
  9  \w    139.00 177.00   0.50    0.16    --  106.61 125.00-120.00   76
 10  \w    -59.00  30.00   0.50    0.05    --  -43.12  55.00  62.00  178
 11  \w    -62.00 -25.00   0.50    0.16    --  -96.00  55.00  62.00   74
 12  \w    -50.00 -24.00   0.50    0.16    --  -96.00  45.00  30.00   52
 13  \w    -50.00 -25.00   0.50    0.16    --  -96.00  45.00  60.00   50
 14  \w    -66.00 -25.00   0.50    0.16    --  -96.00  61.00 -90.00   82
 15  \w    -48.00 -21.00   0.50    0.16    --  -96.00  45.00-120.00   54
 16  \w    -50.00 -21.00   0.50    0.16    --  -96.00  45.00-150.00   58
 17  \w    -50.00 -21.00   0.50    0.16    --  -96.00  45.00-180.00   58
 18  \w    -53.00 -23.00   0.50    0.16    --  -96.00 125.00 -90.00   60
 19  \w   -117.00 -78.00   0.50    0.16    --  -96.00 -55.00 -80.00   78
 20  \w   -170.00-122.00   0.50    0.16    --  -96.00 -55.00 -80.00   96
 21  \w   -161.00-102.00   0.50    0.16    --  -96.00 -77.00-150.00  118
 22  \w   -114.00 -21.00   0.50    0.05    --  -43.12 -55.00 -80.00  186
 23  \w   -169.00 -89.00   0.50    0.16    --  -96.00 -77.00   0.00  160
 24  \w   -117.00 -83.00   0.50    0.05    --  -43.12-125.00  60.00   68
 25  \w   -111.00 -85.00   0.50    0.05    --  -43.12-125.00  30.00   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      -0.0982275000
_diffrn_orient_matrix_UB_12      0.0696248000
_diffrn_orient_matrix_UB_13      0.0629925000
_diffrn_orient_matrix_UB_21      -0.1156122000
_diffrn_orient_matrix_UB_22      -0.0110378000
_diffrn_orient_matrix_UB_23      -0.1093207000
_diffrn_orient_matrix_UB_31      -0.0677383000
_diffrn_orient_matrix_UB_32      -0.0820831000
_diffrn_orient_matrix_UB_33      0.0681839000
_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  0.0531
_diffrn_reflns_av_unetI/netI     0.0503
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.929
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8174
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.929
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.455
_diffrn_reflns_theta_min         5.158
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.604
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.153
_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    1.286
_exptl_crystal_description       prism
_exptl_crystal_F_000             584
_exptl_crystal_size_max          0.95
_exptl_crystal_size_mid          0.53
_exptl_crystal_size_min          0.29
_refine_diff_density_max         0.259
_refine_diff_density_min         -0.304
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         2709
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0600
_refine_ls_R_factor_gt           0.0563
_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^)+(0.1033P)^2^+0.1397P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1492
_refine_ls_wR_factor_ref         0.1538
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2407
_reflns_number_total             2709
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d6dt00469e2.cif
_cod_data_source_block           ksk575-gg
_cod_depositor_comments
'Adding full bibliography for 7720347--7720357.cif.'
_cod_database_code               7720350
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C18 H17 N3'
_shelx_estimated_absorpt_t_max   0.844
_shelx_estimated_absorpt_t_min   0.598
_diffrn_oxdiff_digest_hkl
;
43c4f9b0787877b702c8e852ad9b8fa2c42bbb
;
_diffrn_oxdiff_digest_od_ed
;

;
_diffrn_oxdiff_measurement_exp_name KSK575.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:
 C14(H14)
2.b Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C18(H18A,H18B), C16(H16A,H16B), C17(H17A,H17B)
2.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C12(H12), C11(H11), C2(H2), C3(H3), C9(H9), C4(H4), C10(H10)
;
_shelx_res_checksum              4153
_shelx_hkl_checksum              66916
_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 1.292
_oxdiff_exptl_absorpt_empirical_full_min 0.802