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_7720351
_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 N2'
_chemical_formula_sum            'C15 H10 N2'
_chemical_formula_weight         218.25
_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                 106.898(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.9972(2)
_cell_length_b                   17.3076(4)
_cell_length_c                   8.2800(2)
_cell_measurement_reflns_used    4753
_cell_measurement_temperature    99.98(10)
_cell_measurement_theta_max      74.8090
_cell_measurement_theta_min      5.0840
_cell_volume                     1096.57(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      99.98(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.922
_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     33.00  58.00   0.50    0.38    --  104.64 -57.00-180.00   50
  2  \w     34.00  60.00   0.50    0.38    --  104.64 -57.00-150.00   52
  3  \w     34.00  60.00   0.50    0.38    --  104.64 -57.00 -90.00   52
  4  \w     37.00  62.00   0.50    0.38    --  104.64 -57.00 -60.00   50
  5  \w    -17.00  36.00   0.50    0.10    --   49.47 -35.00 105.00  106
  6  \w     36.00  63.00   0.50    0.38    --  104.64 -57.00 120.00   54
  7  \w     33.00  63.00   0.50    0.38    --  104.64 -57.00  90.00   60
  8  \w     45.00  81.00   0.50    0.10    --   49.47  35.00 -96.00   72
  9  \w    100.00 126.00   0.50    0.38    --  104.64  19.00-150.00   52
 10  \w    138.00 164.00   0.50    0.38    --  104.64  19.00-150.00   52
 11  \w    110.00 166.00   0.50    0.38    --  104.64  35.00 -96.00  112
 12  \w    -39.00  20.00   0.50    0.10    --  -49.47  35.00 -96.00  118
 13  \w   -110.00 -27.00   0.50    0.38    --  -90.00  77.00-150.00  166
 14  \w    -65.00 -18.00   0.50    0.38    --  -90.00  57.00 -30.00   94
 15  \w    -56.00 -29.00   0.50    0.38    --  -90.00  57.00   0.00   54
 16  \w    -57.00 -19.00   0.50    0.38    --  -90.00  57.00  30.00   76
 17  \w    -51.00 -19.00   0.50    0.38    --  -90.00  77.00  60.00   64
 18  \w   -104.00 -61.00   0.50    0.38    --  -90.00  77.00  60.00   86
 19  \w    -64.00 -19.00   0.50    0.38    --  -90.00  57.00  60.00   90
 20  \w    -83.00 -42.00   0.50    0.10    --  -49.47 -37.00  30.00   82
 21  \w   -115.00 -45.00   0.50    0.10    --  -49.47 -35.00 105.00  140
 22  \w   -122.00 -82.00   0.50    0.38    --  -90.00 -35.00 105.00   80
;
_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      0.1778087000
_diffrn_orient_matrix_UB_12      0.0397272000
_diffrn_orient_matrix_UB_13      0.0227994000
_diffrn_orient_matrix_UB_21      -0.0359750000
_diffrn_orient_matrix_UB_22      0.0028412000
_diffrn_orient_matrix_UB_23      -0.1930494000
_diffrn_orient_matrix_UB_31      -0.0872782000
_diffrn_orient_matrix_UB_32      0.0796160000
_diffrn_orient_matrix_UB_33      -0.0043192000
_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  0.0445
_diffrn_reflns_av_unetI/netI     0.0415
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.922
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            7200
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.922
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.707
_diffrn_reflns_theta_min         5.111
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.620
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.492
_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    1.322
_exptl_crystal_description       prism
_exptl_crystal_F_000             456
_exptl_crystal_size_max          0.242
_exptl_crystal_size_mid          0.239
_exptl_crystal_size_min          0.118
_refine_diff_density_max         0.160
_refine_diff_density_min         -0.156
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     154
_refine_ls_number_reflns         2130
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0455
_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^)+(0.0554P)^2^+0.1746P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1113
_refine_ls_wR_factor_ref         0.1148
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1890
_reflns_number_total             2130
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d6dt00469e2.cif
_cod_data_source_block           ksk551-gg
_cod_depositor_comments
'Adding full bibliography for 7720347--7720357.cif.'
_cod_original_cell_volume        1096.58(5)
_cod_database_code               7720351
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C15 H10 N2 '
_diffrn_oxdiff_digest_hkl
;
4339468b4ad05376dbc2abcdc11bc9892d523a
;
_diffrn_oxdiff_digest_od_ed
;

;
_diffrn_oxdiff_measurement_exp_name KSK551.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:
 C3(H3), C15(H15), C8(H8), C14(H14), C5(H5), C6(H6), C7(H7), C12(H12),
 C11(H11), C13(H13)
;
_shelx_res_checksum              72773
_shelx_hkl_checksum              97943
_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 1.294
_oxdiff_exptl_absorpt_empirical_full_min 0.831