Chromium catalyzed acceptorless dehydrogenative (cross)coupling of primary amines to secondary imines.
Anand, Aman; Regina, Anitta; Jalwal, Sachin; Prodhan, Soumojyati; Sil, Debangsu; Paranjothy, Manikandan; Chakraborty, Subrata; Dalton transactions (Cambridge, England : 2003) 54 (2025) 6432–6442; doi:10.1039/d4dt03460k

data_7718365
_publ_section_title
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 Chromium catalyzed acceptorless dehydrogenative (cross)coupling of
 primary amines to secondary imines.
;
_journal_issue                   16
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6432
_journal_page_last               6442
_journal_paper_doi               10.1039/d4dt03460k
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C15 H6 Cr N2 O5'
_chemical_formula_sum            'C15 H6 Cr N2 O5'
_chemical_formula_weight         346.22
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yac'
_space_group_name_H-M_alt        'P 1 2/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2025-03-13
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2025-03-13 deposited with the CCDC.	2025-03-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.937(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.9252(11)
_cell_length_b                   12.898(2)
_cell_length_c                   15.288(3)
_cell_measurement_reflns_used    9941
_cell_measurement_temperature    150
_cell_measurement_theta_max      25.67
_cell_measurement_theta_min      2.66
_cell_volume                     1365.4(4)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0319
_diffrn_reflns_av_unetI/netI     0.0162
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            21604
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.749
_diffrn_reflns_theta_min         2.066
_exptl_absorpt_coefficient_mu    0.867
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6495
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1621 before and 0.0728 after correction.
The Ratio of minimum to maximum transmission is 0.8715.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'metallic reddish red'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.684
_exptl_crystal_description       irregular
_exptl_crystal_F_000             696
_exptl_crystal_size_max          0.572
_exptl_crystal_size_mid          0.238
_exptl_crystal_size_min          0.136
_refine_diff_density_max         0.335
_refine_diff_density_min         -0.420
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         2605
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0298
_refine_ls_R_factor_gt           0.0272
_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^)+(0.0361P)^2^+1.0739P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0717
_refine_ls_wR_factor_ref         0.0736
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2440
_reflns_number_total             2605
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03460k2.cif
_cod_data_source_block           mo_cr_1_aa_blkl_0m
_cod_depositor_comments
'Adding full bibliography for 7718364--7718365.cif.'
_cod_original_cell_volume        1365.3(4)
_cod_database_code               7718365
_shelx_shelxl_version_number     2019/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C15(H15), C5(H5), C14(H14), C13(H13), C6(H6), C7(H7)
;
_shelx_res_checksum              39317
_shelx_hkl_checksum              16269
_olex2_submission_special_instructions 'No special instructions were received'