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_7064331
_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         'C12 H11 Cl N4 O Pd S, C3 H7 N O'
_chemical_formula_sum            'C15 H18 Cl N5 O2 Pd S'
_chemical_formula_weight         474.28
_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             2021-03-19
_audit_creation_method
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Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-12-28 deposited with the CCDC.	2025-12-22 downloaded from the CCDC.
;
_cell_angle_alpha                111.827(3)
_cell_angle_beta                 109.312(3)
_cell_angle_gamma                93.968(3)
_cell_formula_units_Z            2
_cell_length_a                   8.4878(8)
_cell_length_b                   11.0977(11)
_cell_length_c                   11.1379(11)
_cell_measurement_reflns_used    5302
_cell_measurement_temperature    273
_cell_measurement_theta_max      27.131
_cell_measurement_theta_min      2.244
_cell_volume                     896.74(16)
_computing_cell_refinement       'SAINT V8.40A (?, 2016)'
_computing_data_reduction        'SAINT V8.40A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      273
_diffrn_measured_fraction_theta_full 0.9811
_diffrn_measured_fraction_theta_max 0.9811
_diffrn_measurement_device_type  'Bruker D8'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0591
_diffrn_reflns_av_unetI/netI     0.0560
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            13634
_diffrn_reflns_theta_full        27.1372
_diffrn_reflns_theta_max         27.14
_diffrn_reflns_theta_min         2.03
_exptl_absorpt_coefficient_mu    1.320
_exptl_absorpt_correction_T_max  0.912
_exptl_absorpt_correction_T_min  0.912
_exptl_absorpt_correction_type   gaussian
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.7564
_exptl_crystal_description       block
_exptl_crystal_F_000             474.7124
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.1665
_refine_diff_density_min         -0.7508
_refine_diff_density_rms         0.1613
_refine_ls_d_res_high            0.7791
_refine_ls_d_res_low             10.0512
_refine_ls_goodness_of_fit_ref   1.0319
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    29
_refine_ls_number_parameters     230
_refine_ls_number_reflns         3900
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0319
_refine_ls_R_factor_all          0.0553
_refine_ls_R_factor_gt           0.0355
_refine_ls_shift/su_max          0.0004
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0446P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0798
_refine_ls_wR_factor_ref         0.0876
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              10
_reflns_limit_h_min              -10
_reflns_limit_k_max              12
_reflns_limit_k_min              -14
_reflns_limit_l_max              14
_reflns_limit_l_min              0
_reflns_number_gt                3110
_reflns_number_total             3900
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d5nj02138c2.cif
_cod_data_source_block           mo_GP_8MOBT_0m_a
_cod_database_code               7064331
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Rotating group:
 N3(H3a,H3b)
2.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C7(H7), C6(H6), C4(H4a), N4(H4), C2(H2), C13(H13)
2.c Idealised Me refined as rotating group:
 C12(H12a,H12b,H12c), C14(H14a,H14b,H14c), C15(H15a,H15b,H15c)
;
_olex2_submission_special_instructions 'No special instructions were received'