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_7720353
_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         'C26 H25 B Cl3 Mo N4, C H2 Cl2'
_chemical_formula_sum            'C27 H27 B Cl5 Mo N4'
_chemical_formula_weight         691.52
_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                 92.883(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.9751(4)
_cell_length_b                   10.6445(2)
_cell_length_c                   19.6815(5)
_cell_measurement_reflns_used    10267
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      75.9900
_cell_measurement_theta_min      3.1440
_cell_volume                     2924.07(12)
_computing_cell_refinement       'CrysAlisPro 1.171.44.117a (Rigaku OD, 2025)'
_computing_data_collection
'CrysAlisPro system (CCD 43.143a 64-bit (release 25-10-2024))'
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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   -121.00 -14.00   0.50    2.17    --  -49.42   0.00-180.00  214
  2  \w   -121.00 -95.00   0.50    2.17    --  -49.42 -77.00-150.00   52
  3  \w     -5.00  21.00   0.50    2.17    --  -49.42  19.00 -30.00   52
  4  \w   -121.00 -96.00   0.50    2.17    --  -49.42 -77.00-120.00   50
  5  \w   -118.00 -80.00   0.50    2.17    --  -49.42-125.00-150.00   76
  6  \w   -119.00 -93.00   0.50    2.17    --  -49.42 -77.00 -60.00   52
  7  \w   -125.00 -93.00   0.50    8.69    --  -90.00 -99.00 -60.00   64
  8  \w   -160.00-128.00   0.50    8.69    --  -90.00 -99.00 -60.00   64
  9  \w    -65.00 -21.00   0.50    8.69    --  -90.00 125.00  90.00   88
 10  \w    -66.00 -21.00   0.50    8.69    --  -90.00  57.00 -30.00   90
 11  \w    -66.00 -29.00   0.50    8.69    --  -90.00  57.00   0.00   74
 12  \w     98.00 174.00   0.50    8.69    --  104.56  38.00  90.00  152
 13  \w     93.00 176.00   0.50    8.69    --  104.56  57.00   0.00  166
 14  \w     73.00 102.00   0.50    8.69    --  104.56 -75.00-151.00   58
 15  \w     33.00  62.00   0.50    8.69    --  104.56 -57.00 -60.00   58
 16  \w     36.00  66.00   0.50    8.69    --  104.56 -57.00-150.00   60
 17  \w     39.00  66.00   0.50    8.69    --  104.56 -57.00-180.00   54
 18  \w     61.00 110.00   0.50    8.69    --  104.56 -99.00  60.00   98
 19  \w     33.00  64.00   0.50    8.69    --  104.56 -57.00-120.00   62
 20  \w    103.00 168.00   0.50    8.69    --  104.56  38.00  30.00  130
 21  \w     40.00  65.00   0.50    8.69    --  104.56 -57.00 -90.00   50
;
_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      -0.1092525000
_diffrn_orient_matrix_UB_12      0.0024323000
_diffrn_orient_matrix_UB_13      -0.0153223000
_diffrn_orient_matrix_UB_21      0.0074685000
_diffrn_orient_matrix_UB_22      -0.1199722000
_diffrn_orient_matrix_UB_23      -0.0431652000
_diffrn_orient_matrix_UB_31      -0.0144403000
_diffrn_orient_matrix_UB_32      -0.0807635000
_diffrn_orient_matrix_UB_33      0.0635808000
_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  0.0461
_diffrn_reflns_av_unetI/netI     0.0423
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            17665
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        66.596
_diffrn_reflns_theta_max         66.596
_diffrn_reflns_theta_min         3.166
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.068
_exptl_absorpt_correction_T_max  0.802
_exptl_absorpt_correction_T_min  0.539
_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    1.571
_exptl_crystal_description       plate
_exptl_crystal_F_000             1396
_exptl_crystal_size_max          0.159
_exptl_crystal_size_mid          0.117
_exptl_crystal_size_min          0.102
_refine_diff_density_max         1.167
_refine_diff_density_min         -0.702
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     375
_refine_ls_number_reflns         5166
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0455
_refine_ls_R_factor_gt           0.0403
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0635P)^2^+2.1672P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1049
_refine_ls_wR_factor_ref         0.1083
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4541
_reflns_number_total             5166
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d6dt00469e2.cif
_cod_data_source_block           ksk495-gg
_cod_depositor_comments
'Adding full bibliography for 7720347--7720357.cif.'
_cod_database_code               7720353
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Mo Cl5 C27 B H27 N4'
_diffrn_oxdiff_digest_hkl
;
43dc4d0b0bb3b2a235f26e131226b54e50dcd0
;
_diffrn_oxdiff_digest_od_ed
;

;
_diffrn_oxdiff_measurement_exp_name KSK495.par
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C15B) = Uanis(C15A)
Uanis(C14A) = Uanis(C14B)
Uanis(C12A) = Uanis(C12B)
3. Others
 Sof(C12B)=Sof(H12B)=1-FVAR(1)
 Sof(C12A)=Sof(H12A)=FVAR(1)
 Sof(C16B)=Sof(H16C)=Sof(H16D)=1-FVAR(2)
 Sof(C16A)=Sof(H16A)=Sof(H16B)=FVAR(2)
 Sof(C15A)=Sof(H15A)=Sof(H15B)=1-FVAR(3)
 Sof(C15B)=Sof(H15C)=Sof(H15D)=FVAR(3)
 Sof(C13A)=Sof(H13A)=Sof(H13B)=1-FVAR(4)
 Sof(C13B)=Sof(H13C)=Sof(H13D)=FVAR(4)
 Sof(C14B)=Sof(H14C)=Sof(H14D)=1-FVAR(5)
 Sof(C14A)=Sof(H14A)=Sof(H14B)=FVAR(5)
4.a Ternary CH refined with riding coordinates:
 C12A(H12A), C12B(H12B)
4.b Secondary CH2 refined with riding coordinates:
 C31(H31A,H31B), C15A(H15A,H15B), C13A(H13A,H13B), C16A(H16A,H16B), C14A(H14A,
 H14B), C16B(H16C,H16D), C14B(H14C,H14D), C13B(H13C,H13D), C15B(H15C,H15D)
4.c Aromatic/amide H refined with riding coordinates:
 C29(H29), C21(H21), C8(H8), C27(H27), C9(H9), C3(H3), C30(H30), C4(H4),
 C23(H23), C22(H22), C5(H5), C28(H28), C11(H11), C10(H10), C2(H2), C24(H24)
;
_shelx_res_checksum              7689
_shelx_hkl_checksum              1974
_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 1.840
_oxdiff_exptl_absorpt_empirical_full_min 0.483