Imine Palladacycles: Synthesis, Structural Analysis and Application in Suzuki–Miyaura Cross Coupling in Semi-Aqueous Media
Bermúdez-Puente, Brais; Adrio, Luis A.; Lucio-Martínez, Fátima; Reigosa, Francisco; Ortigueira, Juan M.; Vila, José M.; Molecules 27 (2022) 3146–; doi:10.3390/molecules27103146

data_1567074
_publ_section_title
;
 Imine Palladacycles: Synthesis, Structural Analysis and Application in
 Suzuki--Miyaura Cross Coupling in Semi-Aqueous Media
;
_journal_issue                   10
_journal_name_full               Molecules
_journal_page_first              3146
_journal_paper_doi               10.3390/molecules27103146
_journal_volume                  27
_journal_year                    2022
_chemical_formula_moiety         'C32 H30 Br2 Cl2 N2 O6 Pd2'
_chemical_formula_sum            'C32 H30 Br2 Cl2 N2 O6 Pd2'
_chemical_formula_weight         982.147
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_Int_Tables_number      14
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-03-22
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_cell_angle_alpha                90
_cell_angle_beta                 102.0378(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.9156(3)
_cell_length_b                   3.92009(8)
_cell_length_c                   30.0833(6)
_cell_measurement_reflns_used    4951
_cell_measurement_temperature    99.99
_cell_measurement_theta_max      26.482
_cell_measurement_theta_min      2.24
_cell_volume                     1604.97(6)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_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      99.99
_diffrn_measured_fraction_theta_full 0.9997
_diffrn_measured_fraction_theta_max 0.9919
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0501
_diffrn_reflns_av_unetI/netI     0.0387
_diffrn_reflns_Laue_measured_fraction_full 0.9997
_diffrn_reflns_Laue_measured_fraction_max 0.9919
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            21117
_diffrn_reflns_point_group_measured_fraction_full 0.9997
_diffrn_reflns_point_group_measured_fraction_max 0.9919
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         26.61
_diffrn_reflns_theta_min         1.50
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.825
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6264
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0655 before and 0.0482 after correction.
The Ratio of minimum to maximum transmission is 0.8404.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.032
_exptl_crystal_description       prism
_exptl_crystal_F_000             956.318
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.8099
_refine_diff_density_min         -0.8814
_refine_diff_density_rms         0.2063
_refine_ls_d_res_high            0.7933
_refine_ls_d_res_low             13.6096
_refine_ls_goodness_of_fit_ref   1.0355
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    24
_refine_ls_number_parameters     211
_refine_ls_number_reflns         3313
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0355
_refine_ls_R_factor_all          0.0448
_refine_ls_R_factor_gt           0.0283
_refine_ls_shift/su_max          -0.0007
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0206P)^2^+1.5237P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0501
_refine_ls_wR_factor_ref         0.0541
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              17
_reflns_limit_h_min              -17
_reflns_limit_k_max              4
_reflns_limit_k_min              0
_reflns_limit_l_max              37
_reflns_limit_l_min              0
_reflns_number_gt                2674
_reflns_number_total             3313
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            2011vi11bbp10_0m.cif
_cod_data_source_block           2011vi11bbp10_0m
_cod_depositor_comments
;

2025-07-10
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C64 H60 Br4 Cl4 N4 O12 Pd4'
_cod_original_formula_weight         1964.295
_cod_original_formula_moiety         '2(C32 H30 Br2 Cl2 N2 O6 Pd2)'
_cod_original_formula_units_Z            1
_cod_database_code               1567074
_olex2_refinement_description
;
1.a Aromatic/amide H refined with riding coordinates:
 C9(H4), C12(H9), C7(H10), C5(H13), C13(H14), C10(H16)
1.b Idealised Me refined as rotating group:
 C15(H8a,H8b,H8c), C16(H15a,H15b,H15c), C14(H1a,H1b,H1c)
;
_olex2_submission_special_instructions 'No special instructions were received'