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_7720356
_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         '2(C7.5 H7 N)'
_chemical_formula_sum            'C15 H14 N2'
_chemical_formula_weight         222.28
_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_Hall           'P 2 2ab'
_space_group_name_H-M_alt        'P 21 21 2'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.4374(3)
_cell_length_b                   14.1906(4)
_cell_length_c                   11.8015(3)
_cell_measurement_reflns_used    15481
_cell_measurement_temperature    100.00(11)
_cell_measurement_theta_max      36.0010
_cell_measurement_theta_min      2.2230
_cell_volume                     1245.54(7)
_computing_cell_refinement       'CrysAlisPro 1.171.44.117a (Rigaku OD, 2025)'
_computing_data_collection
'CrysAlisPro system (CCD 44.108a 64-bit (release 25-04-2025))'
_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      100.00(11)
_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 0.999
_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    -45.00  49.00   0.50  196.00    --   24.86 -84.00-168.00  188
  2  \w    -51.00  18.00   0.50  196.00    --  -25.18  84.00 -48.00  138
  3  \w    -49.00  -1.00   0.50  196.00    --   24.86 -19.00 -60.00   96
  4  \w    -44.00   1.00   0.50  196.00    --   24.86 -19.00  90.00   90
  5  \w      6.00  37.00   0.50  196.00    --   24.86  77.00-120.00   62
  6  \w    -37.00  48.00   0.50  196.00    --   24.86 -77.00  30.00  170
  7  \w    -48.00   2.00   0.50  196.00    --   24.86 -19.00 -90.00  100
  8  \w     10.00  96.00   0.50  196.00    --   24.86  57.00 120.00  172
  9  \w    -47.00  -4.00   0.50  196.00    --   24.86 -19.00  60.00   86
 10  \w      5.00  37.00   0.50  196.00    --   24.86  77.00  30.00   64
 11  \w     13.00  95.00   0.50  196.00    --   24.86  37.00-120.00  164
 12  \w    -65.00 -22.00   0.50  196.00    --  -25.18 110.00  51.89   86
 13  \w    -65.00 -20.00   0.50  196.00    --  -25.18 110.00 163.41   90
 14  \w    -99.00 -13.00   0.50  196.00    --  -25.18 -19.00   0.00  172
 15  \w    -94.00 -13.00   0.50  196.00    --  -25.18 -37.00-150.00  162
 16  \w    -68.00 -32.00   0.50  196.00    --  -25.18 115.00  80.09   72
 17  \w    -96.00 -11.00   0.50  196.00    --  -25.18 -57.00 -30.00  170
 18  \w    -65.00 -22.00   0.50  196.00    --  -25.18 110.00-120.02   86
 19  \w    -49.00 -16.00   0.50  196.00    --  -25.18 -70.00 -92.23   66
 20  \w    -34.00  -7.00   0.50  196.00    --  -25.18 -77.00  60.00   54
 21  \w    -37.00  -2.00   0.50  196.00    --  -25.18 -77.00 120.00   70
 22  \w    -68.00 -24.00   0.50  196.00    --  -25.18 115.00  -5.69   88
 23  \w    -68.00 -25.00   0.50  196.00    --  -25.18 115.00 179.69   86
;
_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      0.0917908000
_diffrn_orient_matrix_UB_12      -0.0117696000
_diffrn_orient_matrix_UB_13      0.0080593000
_diffrn_orient_matrix_UB_21      -0.0258639000
_diffrn_orient_matrix_UB_22      -0.0426187000
_diffrn_orient_matrix_UB_23      0.0268988000
_diffrn_orient_matrix_UB_31      0.0008515000
_diffrn_orient_matrix_UB_32      -0.0233122000
_diffrn_orient_matrix_UB_33      -0.0531398000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0780
_diffrn_reflns_av_unetI/netI     0.0231
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            43794
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.991
_diffrn_reflns_theta_min         2.245
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.071
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.355
_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            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.185
_exptl_crystal_description       prism
_exptl_crystal_F_000             472
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.305
_refine_diff_density_min         -0.135
_refine_diff_density_rms         0.051
_refine_ls_abs_structure_details
;
 Flack x determined using 1228 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.4(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.993
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     159
_refine_ls_number_reflns         3978
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.993
_refine_ls_R_factor_all          0.0652
_refine_ls_R_factor_gt           0.0560
_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^)+(0.1241P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1571
_refine_ls_wR_factor_ref         0.1650
_reflns_Friedel_coverage         0.746
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                3232
_reflns_number_total             3978
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d6dt00469e2.cif
_cod_data_source_block           ptol2cn2_moly-gg
_cod_depositor_comments
'Adding full bibliography for 7720347--7720357.cif.'
_cod_database_code               7720356
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C15 H14 N2'
_shelx_estimated_absorpt_t_max   0.988
_shelx_estimated_absorpt_t_min   0.979
_diffrn_oxdiff_digest_hkl
;
43e2c2a0ca200a2d94f5a933a11494f51a5cb0
;
_diffrn_oxdiff_digest_od_ed
;

;
_diffrn_oxdiff_measurement_exp_name pTol2CN2_moly.par
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C6B(H6B), C7B(H7B), C3B(H3B), C6A(H6A), C4B(H4B), C7A(H7A), C3A(H3A), C4A(H4A)
2.b Idealised Me refined as rotating group:
 C8B(H8BA,H8BB,H8BC), C8A(H8AA,H8AB,H8AC)
;
_shelx_res_checksum              89596
_shelx_hkl_checksum              88574
_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 3.153
_oxdiff_exptl_absorpt_empirical_full_min 0.695