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_7720348
_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         'C22 H25 Cl3 Mo N O, 0.5[CH2Cl2]'
_chemical_formula_sum            'C45 H52 Cl8 Mo2 N2 O2'
_chemical_formula_weight         1128.36
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -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                81.729(5)
_cell_angle_beta                 88.599(5)
_cell_angle_gamma                69.331(6)
_cell_formula_units_Z            1
_cell_length_a                   9.7090(5)
_cell_length_b                   9.9534(7)
_cell_length_c                   13.4743(9)
_cell_measurement_reflns_used    8208
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      74.2780
_cell_measurement_theta_min      3.3200
_cell_volume                     1205.15(14)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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    -49.00 -20.00   0.50    0.15    --  -96.00  45.00 150.00   58
  2  \w    -46.00 -21.00   0.50    0.15    --  -96.00  45.00 120.00   50
  3  \w    -49.00 -20.00   0.50    0.15    --  -96.00  45.00  60.00   58
  4  \w    -50.00 -21.00   0.50    0.15    --  -96.00  45.00  90.00   58
  5  \w    -50.00 -20.00   0.50    0.15    --  -96.00  45.00 -30.00   60
  6  \w    -50.00 -25.00   0.50    0.15    --  -96.00  45.00 -60.00   50
  7  \w    -49.00 -21.00   0.50    0.15    --  -96.00  45.00-180.00   56
  8  \w    -19.00  36.00   0.50    0.05    --  -43.12  19.00   0.00  110
  9  \w    -17.00  58.00   0.50    0.05    --   43.12 -88.00   0.00  150
 10  \w     51.00  78.00   0.50    0.05    --   43.12-125.00  90.00   54
 11  \w     38.00  95.00   0.50    0.05    --   43.12-125.00-150.00  114
 12  \w    115.00 173.00   0.50    0.15    --  106.61  88.00 116.00  116
 13  \w    150.00 175.00   0.50    0.15    --  106.61 125.00  60.00   50
 14  \w     98.00 136.00   0.50    0.15    --  106.61 125.00  60.00   76
 15  \w     97.00 170.00   0.50    0.15    --  106.61 125.00 -30.00  146
 16  \w     89.00 114.00   0.50    0.05    --   43.12  77.00  60.00   50
 17  \w     89.00 114.00   0.50    0.05    --   43.12  77.00   0.00   50
 18  \w     33.00  69.00   0.50    0.15    --  106.61 -61.00-150.00   72
 19  \w     41.00  66.00   0.50    0.15    --  106.61 -61.00-120.00   50
 20  \w     35.00  72.00   0.50    0.15    --  106.61 -61.00   0.00   74
 21  \w     38.00  63.00   0.50    0.15    --  106.61 -61.00 150.00   50
 22  \w     92.00 118.00   0.50    0.15    --  106.61 -88.00   0.00   52
 23  \w     75.00 116.00   0.50    0.15    --  106.61-125.00   0.00   82
 24  \w     44.00 107.00   0.50    0.15    --  106.61 -94.00  60.00  126
 25  \w     46.00 104.00   0.50    0.15    --  106.61 -94.00 120.00  116
 26  \w     37.00 105.00   0.50    0.15    --  106.61 -94.00 -30.00  136
 27  \w     58.00  85.00   0.50    0.15    --  106.61 -94.00 -90.00   54
 28  \w     33.00 110.00   0.50    0.15    --  106.61-125.00-120.00  154
 29  \w   -114.00 -89.00   0.50    0.05    --  -43.12 -77.00 120.00   50
 30  \w   -116.00 -90.00   0.50    0.05    --  -43.12 -77.00  60.00   52
 31  \w   -115.00 -90.00   0.50    0.05    --  -43.12 -77.00  30.00   50
 32  \w   -170.00 -92.00   0.50    0.15    --  -96.00 -77.00 120.00  156
 33  \w   -149.00 -89.00   0.50    0.15    --  -96.00 -77.00  90.00  120
 34  \w   -170.00 -93.00   0.50    0.15    --  -96.00 -77.00  30.00  154
 35  \w   -149.00-122.00   0.50    0.15    --  -96.00 -77.00-120.00   54
 36  \w   -165.00 -76.00   0.50    0.15    --  -96.00 -88.00   0.00  178
 37  \w   -106.00 -80.00   0.50    0.05    --  -43.12-125.00 150.00   52
 38  \w    -76.00 -51.00   0.50    0.15    --  -96.00  88.00 116.00   50
 39  \w    -50.00 -23.00   0.50    0.15    --  -96.00 125.00  30.00   54
 40  \w    -60.00  11.00   0.50    0.05    --  -43.12  88.00 116.00  142
;
_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      -0.0020915000
_diffrn_orient_matrix_UB_12      -0.1236579000
_diffrn_orient_matrix_UB_13      -0.0561266000
_diffrn_orient_matrix_UB_21      0.0786299000
_diffrn_orient_matrix_UB_22      0.0559254000
_diffrn_orient_matrix_UB_23      -0.0882937000
_diffrn_orient_matrix_UB_31      0.1503183000
_diffrn_orient_matrix_UB_32      -0.0976365000
_diffrn_orient_matrix_UB_33      0.0491225000
_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  0.0480
_diffrn_reflns_av_unetI/netI     0.0492
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            12274
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        66.593
_diffrn_reflns_theta_max         66.593
_diffrn_reflns_theta_min         3.316
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.642
_exptl_absorpt_correction_T_max  0.954
_exptl_absorpt_correction_T_min  0.206
_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            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.555
_exptl_crystal_description       prism
_exptl_crystal_F_000             572
_exptl_crystal_size_max          0.324
_exptl_crystal_size_mid          0.206
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.419
_refine_diff_density_min         -0.689
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     257
_refine_ls_number_reflns         4259
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0352
_refine_ls_R_factor_gt           0.0333
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0460P)^2^+0.3081P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0848
_refine_ls_wR_factor_ref         0.0863
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3969
_reflns_number_total             4259
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d6dt00469e2.cif
_cod_data_source_block           ksk576-gg
_cod_depositor_comments
'Adding full bibliography for 7720347--7720357.cif.'
_cod_database_code               7720348
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C45 H52 Cl8 Mo2 N2 O2'
_diffrn_oxdiff_digest_hkl
;
439dc86b0cd251c2f433b1dfe353ec08083380
;
_diffrn_oxdiff_digest_od_ed
;

;
_diffrn_oxdiff_measurement_exp_name KSK576.par
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
2. Restrained distances
 C22A-C23
 1.47 with sigma of 0.02
 C22B-C23
 1.47 with sigma of 0.02
 C22B-C21
 1.47 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C22A) = Uanis(C22B)
4. Rigid body (RIGU) restrains
 C21, C22B, C23, C24, C22A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(H21A)=Sof(H21B)=Sof(H23A)=Sof(H23B)=Sof(C22A)=Sof(H22A)=Sof(H22B)=1-FVAR(1)
 Sof(H21C)=Sof(H21D)=Sof(H23C)=Sof(H23D)=Sof(C22B)=Sof(H22C)=Sof(H22D)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C14(H14)
6.b Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C15(H15A,H15B), C24(H24A,H24B), C17(H17A,H17B), C21(H21A,
 H21B), C21(H21C,H21D), C16(H16A,H16B), C23(H23A,H23B), C23(H23C,H23D),
 C22A(H22A,H22B), C22B(H22C,H22D)
6.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C4(H4), C9(H9), C2(H2), C3(H3), C12(H12), C10(H10), C11(H11)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 44 electrons were 
found in a volume of 148\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
1[CH2Cl2] per Unit Cell 
which account for 42 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              12998
_shelx_hkl_checksum              69308
_shelx_fab_checksum              70514
_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 1.492
_oxdiff_exptl_absorpt_empirical_full_min 0.750