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_1572684
_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         'C42 H31 N9 Ru, 2(F6 P), 0.5(C H4 O)'
_chemical_formula_sum            'C42.5 H33 F12 N9 O0.5 P2 Ru'
_chemical_formula_weight         1068.79
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-12-01
_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                70.753(5)
_cell_angle_beta                 76.873(4)
_cell_angle_gamma                69.270(4)
_cell_formula_units_Z            2
_cell_length_a                   10.1007(8)
_cell_length_b                   13.3932(16)
_cell_length_c                   17.7896(19)
_cell_measurement_reflns_used    4627
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      30.546
_cell_measurement_theta_min      2.173
_cell_volume                     2108.3(4)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_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  (Sheldrick, 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type
'Bruker SMART APEX II diffractometer with CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1168
_diffrn_reflns_av_unetI/netI     0.1541
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            11747
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.690
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.548
_exptl_absorpt_correction_T_max  0.5645
_exptl_absorpt_correction_T_min  0.4604
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1150 before and 0.0703 after correction.
The Ratio of minimum to maximum transmission is 0.8156.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.684
_exptl_crystal_description       block
_exptl_crystal_F_000             1074
_exptl_crystal_size_max          0.103
_exptl_crystal_size_mid          0.099
_exptl_crystal_size_min          0.081
_refine_diff_density_max         1.317
_refine_diff_density_min         -1.147
_refine_diff_density_rms         0.180
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     615
_refine_ls_number_reflns         7207
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.1448
_refine_ls_R_factor_gt           0.1009
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2775
_refine_ls_wR_factor_ref         0.3136
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4517
_reflns_number_total             7207
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02067g2.cif
_cod_data_source_block           q
_cod_depositor_comments
'Adding full bibliography for 1572684--1572687.cif.'
_cod_original_formula_sum        'C42.50 H33 F12 N9 O0.50 P2 Ru'
_cod_database_code               1572684
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.812(3)
 0.188(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(C40) \\sim Ueq, Uanis(C39) \\sim Ueq: with sigma of 0.003 and sigma for
terminal atoms of 0.006
Uanis(N7) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C28) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(O1S) \\sim Ueq, Uanis(C1S) \\sim Ueq: with sigma of 0.003 and sigma for
terminal atoms of 0.006
Uanis(C14) \\sim Ueq: with sigma of 0.003 and sigma for terminal atoms of 0.006
Uanis(C16) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
4. Others
 Fixed Sof: O1S(0.5) H1S(0.5) C1S(0.5) H1SA(0.5) H1SB(0.5) H1SC(0.5)
5.a Riding coordinates:
 O1S(H1S)
5.b Aromatic/amide H refined with riding coordinates:
 C14(H14), C3(H3), C2(H2), C6(H6), C1(H1), C26(H26), C16(H16), C9(H9),
 C10(H10), C23(H23), C42(H42), C19(H19), C36(H36), C29(H29), C20(H20), C25(H25),
  C8(H8), C30(H30), C32(H32), C33(H33), C17(H17), C31(H31), C41(H41), C34(H34),
 C24(H24), C21(H21), C35(H35), C22(H22), C15(H15), C39(H39), C40(H40)
5.c Idealised Me refined as rotating group:
 C1S(H1SA,H1SB,H1SC)
;
_shelx_res_checksum              60823
_shelx_hkl_checksum              89067
_olex2_submission_special_instructions 'No special instructions were received'