Di(pyridin-2-yl)amino-substituted 1,10-phenanthrolines and their Ru(II)-Pd(II) dinuclear complexes: synthesis, characterization and application in Cu-free Sonogashira reaction.
Ionova, Violetta A.; Dmitrieva, Alena V.; Abel, Anton S.; Sergeev, Aleksandr D.; Evko, Grigory S.; Yakushev, Alexei A.; Gontcharenko, Victoria E.; Nefedov, Sergei E.; Roznyatovsky, Vitaly A.; Cheprakov, Andrey V.; Averin, Alexei D.; Magdesieva, Tatiana V.; Beletskaya, Irina P.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 17021–17035; doi:10.1039/d4dt02067g

data_1572685
_publ_section_title
;
 Di(pyridin-2-yl)amino-substituted 1,10-phenanthrolines and their
 Ru(II)-Pd(II) dinuclear complexes: synthesis, characterization and
 application in Cu-free Sonogashira reaction.
;
_journal_issue                   41
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              17021
_journal_page_last               17035
_journal_paper_doi               10.1039/d4dt02067g
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C13 H15 Cl2 N3 O Pd'
_chemical_formula_sum            'C13 H15 Cl2 N3 O Pd'
_chemical_formula_weight         406.58
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-11-16
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2024-01-23 deposited with the CCDC.	2024-09-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.0324(10)
_cell_length_b                   15.1880(13)
_cell_length_c                   16.2973(14)
_cell_measurement_reflns_used    5156
_cell_measurement_temperature    120.00
_cell_measurement_theta_max      30.44
_cell_measurement_theta_min      2.50
_cell_volume                     2978.3(4)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      120.00
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker D8 Quest with Photon III detector'
_diffrn_measurement_method       'phi and omega shutterless scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0871
_diffrn_reflns_av_unetI/netI     0.0525
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            19389
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.998
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         2.495
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.603
_exptl_absorpt_correction_T_max  0.6478
_exptl_absorpt_correction_T_min  0.4555
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1743 before and 0.0856 after correction.
The Ratio of minimum to maximum transmission is 0.7031.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.813
_exptl_crystal_description       block
_exptl_crystal_F_000             1616
_exptl_crystal_size_max          0.089
_exptl_crystal_size_mid          0.076
_exptl_crystal_size_min          0.072
_refine_diff_density_max         2.392
_refine_diff_density_min         -0.738
_refine_diff_density_rms         0.158
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     182
_refine_ls_number_reflns         2618
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0520
_refine_ls_R_factor_gt           0.0429
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0691P)^2^+2.2266P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1070
_refine_ls_wR_factor_ref         0.1159
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2172
_reflns_number_total             2618
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02067g2.cif
_cod_data_source_block           q_CCDC1
_cod_depositor_comments
'Adding full bibliography for 1572684--1572687.cif.'
_cod_database_code               1572685
_shelx_shelxl_version_number     2018/3
_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 Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C12(H12A,H12B)
2.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C4(H4), C9(H9), C1(H1), C2(H2), C7(H7), C3(H3), C8(H8)
2.c Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C)
;
_shelx_res_checksum              64174
_shelx_hkl_checksum              1957
_olex2_submission_special_instructions 'No special instructions were received'