Electron-rich pyridines with <i>para</i>-N-heterocyclic imine substituents: ligand properties and coordination to CO<sub>2</sub>, SO<sub>2</sub>, BCl<sub>3</sub> and Pd<sup>II</sup> complexes.
Franzen, Jonas H.; Wilm, Lukas F. B.; Rotering, Philipp; Wurst, Klaus; Seidl, Michael; Dielmann, Fabian; Dalton transactions (Cambridge, England : 2003) 53 (2024) 11876–11883; doi:10.1039/d4dt01399a

data_7716422
_publ_section_title
;
 Electron-rich pyridines with <i>para</i>-N-heterocyclic imine
 substituents: ligand properties and coordination to CO<sub>2</sub>,
 SO<sub>2</sub>, BCl<sub>3</sub> and Pd<sup>II</sup> complexes.
;
_journal_issue                   28
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11876
_journal_page_last               11883
_journal_paper_doi               10.1039/d4dt01399a
_journal_volume                  53
_journal_year                    2024
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C29 H44 Br2 N6 Pd, C H2 Cl2'
_chemical_formula_sum            'C30 H46 Br2 Cl2 N6 Pd'
_chemical_formula_weight         827.85
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-05-08
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-05-08 deposited with the CCDC.	2024-06-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.7755(4)
_cell_length_b                   18.4999(4)
_cell_length_c                   10.9830(2)
_cell_measurement_reflns_used    9856
_cell_measurement_temperature    183.00
_cell_measurement_theta_max      27.479
_cell_measurement_theta_min      2.292
_cell_volume                     3611.70(13)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection       'Bruker Apex 4 v2021.4-0'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXD  (Sheldrick, 2008)'
_diffrn_ambient_temperature      183.00
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 QUEST PHOTON III C14'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0411
_diffrn_reflns_av_unetI/netI     0.0219
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            87916
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.523
_diffrn_reflns_theta_min         2.292
_exptl_absorpt_coefficient_mu    2.902
_exptl_absorpt_correction_T_max  0.6032
_exptl_absorpt_correction_T_min  0.4718
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0959 before and 0.0500 after correction.
The Ratio of minimum to maximum transmission is 0.7822.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.522
_exptl_crystal_description       prism
_exptl_crystal_F_000             1672
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.702
_refine_diff_density_min         -0.487
_refine_diff_density_rms         0.048
_refine_ls_abs_structure_details
;
 Flack x determined using 3467 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.001(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     380
_refine_ls_number_reflns         8120
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0219
_refine_ls_R_factor_gt           0.0205
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0236P)^2^+1.9563P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0485
_refine_ls_wR_factor_ref         0.0492
_reflns_Friedel_coverage         0.859
_reflns_Friedel_fraction_full    0.975
_reflns_Friedel_fraction_max     0.954
_reflns_number_gt                7835
_reflns_number_total             8120
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01399a2.cif
_cod_data_source_block           compound_8
_cod_depositor_comments
'Adding full bibliography for 7716413--7716422.cif.'
_cod_database_code               7716422
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.780
_shelx_estimated_absorpt_t_min   0.581
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C27(H27), C24(H24)
2.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C7(H7A,H7B), C30(H30A,H30B)
2.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C5(H5), C4(H4), C19(H19), C21(H21), C22(H22), C20(H20)
2.d Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C29(H29A,H29B,H29C), C26(H26A,H26B,H26C), C16(H16A,H16B,
 H16C), C28(H28A,H28B,H28C), C11(H11A,H11B,H11C), C10(H10A,H10B,H10C), C25(H25A,
 H25B,H25C), C12(H12A,H12B,H12C), C15(H15A,H15B,H15C)
;
_shelx_res_checksum              5074
_olex2_submission_special_instructions 'No special instructions were received'