Bromoamination of α,β-unsaturated keto alkenes by palladium(ii) metalallocycles: experimental and theoretical approaches
Nandhini, S.; Dharani, S.; Mugesh, B.; Prabusankar, G.; Mohanapriya, S.; Shankar, R.; Prabhakaran, R.; New Journal of Chemistry 50 (2026) 1602–1612; doi:10.1039/D5NJ02138C

data_7064333
_publ_section_title
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 Bromoamination of \a,\b-unsaturated keto alkenes by palladium(ii)
 metalallocycles: experimental and theoretical approaches
;
_journal_issue                   3
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              1602
_journal_page_last               1612
_journal_paper_doi               10.1039/D5NJ02138C
_journal_volume                  50
_journal_year                    2026
_chemical_formula_moiety         'C13 H13 Cl N4 O Pd S, C3 H7 N O'
_chemical_formula_sum            'C16 H20 Cl N5 O2 Pd S'
_chemical_formula_weight         488.304
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_atom_sites_solution_primary     iterative
_audit_creation_date             2024-01-13
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-01-13 deposited with the CCDC.	2025-12-22 downloaded from the CCDC.
;
_cell_angle_alpha                69.710(1)
_cell_angle_beta                 68.738(1)
_cell_angle_gamma                89.247(1)
_cell_formula_units_Z            2
_cell_length_a                   8.6492(3)
_cell_length_b                   10.9746(4)
_cell_length_c                   11.5173(4)
_cell_measurement_reflns_used    9907
_cell_measurement_temperature    273
_cell_measurement_theta_max      27.124
_cell_measurement_theta_min      2.998
_cell_volume                     947.64(6)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5 (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      273
_diffrn_measured_fraction_theta_full 0.9977
_diffrn_measured_fraction_theta_max 0.9957
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0632
_diffrn_reflns_av_unetI/netI     0.0338
_diffrn_reflns_Laue_measured_fraction_full 0.9977
_diffrn_reflns_Laue_measured_fraction_max 0.9957
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            28425
_diffrn_reflns_point_group_measured_fraction_full 0.9977
_diffrn_reflns_point_group_measured_fraction_max 0.9957
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         27.16
_diffrn_reflns_theta_min         2.04
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.252
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.5955
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1378 before and 0.0747 after correction.
The Ratio of minimum to maximum transmission is 0.7988.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.711
_exptl_crystal_description       needle
_exptl_crystal_F_000             490.816
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.065
_exptl_crystal_size_min          0.065
_refine_diff_density_max         0.4541
_refine_diff_density_min         -0.6020
_refine_diff_density_rms         0.0751
_refine_ls_d_res_high            0.7785
_refine_ls_d_res_low             9.9843
_refine_ls_goodness_of_fit_ref   1.0563
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    32
_refine_ls_number_parameters     239
_refine_ls_number_reflns         4184
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0563
_refine_ls_R_factor_all          0.0301
_refine_ls_R_factor_gt           0.0253
_refine_ls_shift/su_max          -0.0003
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0293P)^2^+0.3634P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0656
_refine_ls_wR_factor_ref         0.0683
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              11
_reflns_limit_h_min              -10
_reflns_limit_k_max              14
_reflns_limit_k_min              -13
_reflns_limit_l_max              14
_reflns_limit_l_min              0
_reflns_number_gt                3801
_reflns_number_total             4184
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d5nj02138c2.cif
_cod_data_source_block           mo_GP8MODM_0m_a
_cod_database_code               7064333
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N4(H4), N1(H1), C3(H3), C7(H7), C8(H8), C9(H9), C5(H5), C14(H14)
2.b Idealised Me refined as rotating group:
 C2(H2a,H2b,H2c), C11(H11a,H11b,H11c), C15(H15a,H15b,H15c), C16(H16a,H16b,H16c)
;
_olex2_submission_special_instructions 'No special instructions were received'