Ruthenium, copper and ruthenium-copper complexes of an unsymmetrical phosphino pyridyl 1,8-naphthyridine PNNN ligand.
Wu, Jingyun; Stevens, Michael A.; Gardiner, Michael G.; Colebatch, Annie L.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 18037–18046; doi:10.1039/d4dt02755h

data_7717234
_publ_section_title
;
 Ruthenium, copper and ruthenium-copper complexes of an unsymmetrical
 phosphino pyridyl 1,8-naphthyridine PNNN ligand.
;
_journal_issue                   44
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              18037
_journal_page_last               18046
_journal_paper_doi               10.1039/d4dt02755h
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C22 H28 Cl2 Cu2 N3 P, C H2 Cl2'
_chemical_formula_sum            'C23 H30 Cl4 Cu2 N3 P'
_chemical_formula_weight         648.35
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-09-22
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-09-26 deposited with the CCDC.	2024-10-15 downloaded from the CCDC.
;
_cell_angle_alpha                64.567(3)
_cell_angle_beta                 68.136(3)
_cell_angle_gamma                75.453(3)
_cell_formula_units_Z            2
_cell_length_a                   9.7176(3)
_cell_length_b                   13.0045(5)
_cell_length_c                   13.0393(4)
_cell_measurement_reflns_used    6575
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      77.2040
_cell_measurement_theta_min      3.7750
_cell_volume                     1372.87(9)
_computing_cell_refinement       'CrysAlisPro 1.171.42.85a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.85a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.85a (Rigaku OD, 2023)'
_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_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -78.00 -52.00   0.50   12.00    --  -46.45 113.00 -86.00   52
  2  \w     30.00  80.00   0.50   12.00    --   46.45-113.00-178.00  100
  3  \w    105.00 139.00   0.50   35.33    --  106.49 113.00 -86.00   68
  4  \w     60.00 108.00   0.50   35.33    --  106.49-113.00-178.00   96
  5  \w    -70.00 -14.00   0.50   12.00    --  -46.45  77.00 -90.00  112
  6  \w   -119.00 -24.00   0.50   12.00    --  -46.45 -77.00-180.00  190
  7  \w    -10.00  16.00   0.50   12.00    --  -46.45  77.00 -90.00   52
  8  \w     -4.00  23.00   0.50   12.00    --  -46.45  19.00-150.00   54
  9  \w    -22.00  48.00   0.50   12.00    --   46.45 -57.00  30.00  140
 10  \w     38.00  96.00   0.50   12.00    --   46.45  38.00 150.00  116
 11  \w    -25.00  17.00   0.50   12.00    --   46.45 -57.00 -30.00   84
 12  \w     28.00  62.00   0.50   12.00    --   46.45 -57.00 -30.00   68
 13  \w     71.00 108.00   0.50   35.33    --  106.49-125.00  60.00   74
 14  \w     31.00  56.00   0.50   35.33    --  106.49 -30.00 120.00   50
 15  \w     38.00  73.00   0.50   35.33    --  106.49 -45.00-150.00   70
 16  \w     41.00  67.00   0.50   35.33    --  106.49-125.00  60.00   52
 17  \w    100.00 128.00   0.50   35.33    --  106.49 125.00-150.00   56
 18  \w     54.00  92.00   0.50   35.33    --  106.49 -61.00 -60.00   76
 19  \w     42.00  71.00   0.50   35.33    --  106.49 -45.00  60.00   58
 20  \w     33.00  59.00   0.50   35.33    --  106.49 -30.00 -90.00   52
 21  \w     33.00  59.00   0.50   35.33    --  106.49 -30.00-120.00   52
 22  \w     64.00 106.00   0.50   35.33    --  106.49 -95.00 -90.00   84
 23  \w     32.00  58.00   0.50   35.33    --  106.49 -30.00-150.00   52
 24  \w     31.00  56.00   0.50   35.33    --  106.49 -30.00  60.00   50
 25  \w     42.00 104.00   0.50   35.33    --  106.49 -95.00-180.00  124
 26  \w     36.00  72.00   0.50   35.33    --  106.49 -45.00 -90.00   72
 27  \w     32.00  57.00   0.50   35.33    --  106.49 -30.00   0.00   50
 28  \w     66.00 105.00   0.50   35.33    --  106.49 -95.00 -60.00   78
 29  \w     31.00  57.00   0.50   35.33    --  106.49 -30.00  90.00   52
 30  \w    132.00 176.00   0.50   35.33    --  106.49  30.00   0.00   88
 31  \w     44.00  73.00   0.50   35.33    --  106.49 -45.00   0.00   58
 32  \w    104.00 130.00   0.50   35.33    --  106.49  30.00   0.00   52
 33  \w     32.00  58.00   0.50   35.33    --  106.49 -30.00 150.00   52
 34  \w     31.00  56.00   0.50   35.33    --  106.49 -30.00 -60.00   50
 35  \w     36.00  61.00   0.50   35.33    --  106.49 -45.00-120.00   50
 36  \w     38.00  65.00   0.50   35.33    --  106.49 -45.00-180.00   54
 37  \w     41.00  85.00   0.50   35.33    --  106.49 -95.00  90.00   88
 38  \w     33.00  58.00   0.50   35.33    --  106.49 -30.00-180.00   50
 39  \w     31.00  59.00   0.50   35.33    --  106.49 -30.00  30.00   56
 40  \w     96.00 138.00   0.50   35.33    --  106.49 125.00-120.00   84
 41  \w    142.00 171.00   0.50   35.33    --  106.49  30.00-150.00   58
 42  \w     65.00 106.00   0.50   35.33    --  106.49 -95.00  60.00   82
 43  \w     97.00 122.00   0.50   35.33    --  106.49  30.00-150.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0694262000
_diffrn_orient_matrix_UB_12      -0.0880258000
_diffrn_orient_matrix_UB_13      0.1243378000
_diffrn_orient_matrix_UB_21      0.0522467000
_diffrn_orient_matrix_UB_22      -0.0952600000
_diffrn_orient_matrix_UB_23      -0.0509438000
_diffrn_orient_matrix_UB_31      0.1482550000
_diffrn_orient_matrix_UB_32      -0.0243024000
_diffrn_orient_matrix_UB_33      0.0280324000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0402
_diffrn_reflns_av_unetI/netI     0.0441
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            14511
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.454
_diffrn_reflns_theta_min         3.786
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.175
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64942
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.85a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.568
_exptl_crystal_description       block
_exptl_crystal_F_000             660
_exptl_crystal_size_max          0.216
_exptl_crystal_size_mid          0.093
_exptl_crystal_size_min          0.071
_refine_diff_density_max         0.990
_refine_diff_density_min         -0.322
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     304
_refine_ls_number_reflns         5606
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0579
_refine_ls_R_factor_gt           0.0476
_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^)+(0.0636P)^2^+0.9182P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1190
_refine_ls_wR_factor_ref         0.1241
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4753
_reflns_number_total             5606
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02755h2.cif
_cod_data_source_block           jw208_auto
_cod_depositor_comments
'Adding full bibliography for 7717232--7717238.cif.'
_cod_database_code               7717234
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C22H28N3PCu2Cl2
_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:
 C10(H10A,H10B), C24(H24A,H24B)
2.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C4(H4), C23(H23), C22(H22), C3(H3), C21(H21), C20(H20)
2.c Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C15(H15A,H15B,H15C), C17(H17A,H17B,H17C), C18(H18A,H18B,
 H18C), C14(H14A,H14B,H14C), C16(H16A,H16B,H16C)
;
_shelx_res_checksum              43275
_shelx_hkl_checksum              10400
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.116
_oxdiff_exptl_absorpt_empirical_full_min 0.575