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_7717235
_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         'C32 H42 Cl3 Cu N3 P Ru, 2(C2 H3 N)'
_chemical_formula_sum            'C36 H48 Cl3 Cu N5 P Ru'
_chemical_formula_weight         852.72
_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                87.736(2)
_cell_angle_beta                 83.713(2)
_cell_angle_gamma                77.647(2)
_cell_formula_units_Z            2
_cell_length_a                   11.0189(2)
_cell_length_b                   12.5547(2)
_cell_length_c                   14.1481(3)
_cell_measurement_reflns_used    14286
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.6740
_cell_measurement_theta_min      4.7420
_cell_volume                     1900.16(6)
_computing_cell_refinement       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1297
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_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    -75.00 -49.00   1.00    1.00    --  -36.95 -38.00   0.00   26
  2  \w    -97.00 -71.00   1.00    1.00    --  -36.95-153.00  51.00   26
  3  \w     51.00 104.00   1.00    1.00    --   36.95  57.00 -90.00   53
  4  \w     56.00  82.00   1.00    1.00    --   36.95  57.00 -30.00   26
  5  \w     34.00  88.00   1.00    1.00    --   36.95-121.00-149.00   54
  6  \w     43.00  73.00   1.00    1.00    --   36.95 -99.00 150.00   30
  7  \w      7.00  38.00   1.00    1.00    --   36.95 -99.00 150.00   31
  8  \w     26.00  51.00   1.00    1.00    --   36.95 -57.00  30.00   25
  9  \w    -20.00   6.00   1.00    1.00    --   36.95 -77.00 120.00   26
 10  \w     56.00 105.00   1.00    1.00    --   36.95  38.00 -30.00   49
 11  \w    -32.00  56.00   1.00    1.00    --   36.95 -38.00   0.00   88
 12  \w    -29.00  14.00   1.00    1.00    --   36.95 -57.00-120.00   43
 13  \w      8.00  35.00   1.00    1.00    --   36.95 -77.00 120.00   27
 14  \w    -19.00  63.00   1.00    1.00    --   36.95 -77.00-120.00   82
 15  \w      9.00  76.00   1.00    1.00    --   36.95 -99.00   0.00   67
 16  \w     48.00 107.00   1.00    1.00    --   36.95  19.00-150.00   59
 17  \w     98.00 126.00   1.00    1.00    --  111.00 -38.00 -90.00   28
 18  \w    135.00 176.00   1.00    1.00    --  111.00  12.00  60.00   41
 19  \w     50.00  79.00   1.00    1.00    --  111.00 -38.00 -90.00   29
 20  \w    107.00 137.00   1.00    1.00    --  111.00  64.00  60.00   30
 21  \w     42.00  77.00   1.00    1.00    --  111.00-111.00  30.00   35
 22  \w     83.00 109.00   1.00    1.00    --  111.00-111.00-120.00   26
 23  \w    147.00 172.00   1.00    1.00    --  111.00  12.00-180.00   25
 24  \w     84.00 109.00   1.00    1.00    --  111.00-111.00  30.00   25
 25  \w    145.00 177.00   1.00    1.00    --  111.00  64.00  60.00   32
 26  \w     66.00 115.00   1.00    1.00    --  111.00  12.00  60.00   49
 27  \w     68.00  94.00   1.00    1.00    --  111.00 -92.00   0.00   26
 28  \w     82.00 107.00   1.00    1.00    --  111.00-111.00 120.00   25
 29  \w     72.00  98.00   1.00    1.00    --  111.00-111.00 -30.00   26
 30  \w     58.00 101.00   1.00    1.00    --  111.00 -64.00  60.00   43
 31  \w     89.00 115.00   1.00    1.00    --  111.00 -64.00  90.00   26
 32  \w     43.00 106.00   1.00    1.00    --  111.00 -92.00  90.00   63
 33  \w     43.00  69.00   1.00    1.00    --  111.00 -77.00-150.00   26
 34  \w     62.00 105.00   1.00    1.00    --  111.00 -92.00-120.00   43
 35  \w    125.00 167.00   1.00    1.00    --  111.00  77.00 -90.00   42
 36  \w    103.00 128.00   1.00    1.00    --  111.00 -50.00  60.00   25
 37  \w    128.00 177.00   1.00    1.00    --  111.00  77.00-180.00   49
 38  \w    116.00 142.00   1.00    1.00    --  111.00  12.00-180.00   26
 39  \w     47.00  83.00   1.00    1.00    --  111.00 -50.00  60.00   36
 40  \w     43.00 104.00   1.00    1.00    --  111.00 -92.00-150.00   61
 41  \w    116.00 142.00   1.00    1.00    --  111.00 178.00 150.00   26
 42  \w     85.00 111.00   1.00    1.00    --  111.00 178.00 150.00   26
 43  \w    101.00 162.00   1.00    1.00    --  111.00  25.00 120.00   61
 44  \w     67.00  92.00   1.00    1.00    --  111.00-121.00-149.00   25
 45  \w     92.00 137.00   1.00    1.00    --  111.00 -77.00-150.00   45
 46  \w     54.00 125.00   1.00    1.00    --  111.00 -38.00 150.00   71
 47  \w     72.00  97.00   1.00    1.00    --  111.00 -92.00-180.00   25
 48  \w     80.00 109.00   1.00    1.00    --  111.00-111.00   0.00   29
 49  \w    131.00 177.00   1.00    1.00    --  111.00 111.00-180.00   46
 50  \w    121.00 146.00   1.00    1.00    --  111.00 178.00 -60.00   25
 51  \w     80.00 130.00   1.00    1.00    --  111.00 -25.00  90.00   50
 52  \w     49.00  74.00   1.00    1.00    --  111.00 -25.00  90.00   25
 53  \w     48.00  73.00   1.00    1.00    --  111.00 -64.00   0.00   25
 54  \w    114.00 139.00   1.00    1.00    --  111.00  77.00-120.00   25
 55  \w     83.00 109.00   1.00    1.00    --  111.00-111.00  90.00   26
 56  \w     45.00 107.00   1.00    1.00    --  111.00-111.00-180.00   62
 57  \w    108.00 134.00   1.00    1.00    --  111.00  77.00-150.00   26
 58  \w    152.00 177.00   1.00    1.00    --  111.00  77.00 -60.00   25
 59  \w     71.00 122.00   1.00    1.00    --  111.00 -50.00   0.00   51
 60  \w     93.00 166.00   1.00    1.00    --  111.00  38.00 -30.00   73
 61  \w     60.00 106.00   1.00    1.00    --  111.00 -50.00-150.00   46
 62  \w     91.00 150.00   1.00    1.00    --  111.00  25.00 -60.00   59
 63  \w     86.00 137.00   1.00    1.00    --  111.00 -80.00 -96.08   51
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1117582000
_diffrn_orient_matrix_UB_12      0.0835181000
_diffrn_orient_matrix_UB_13      -0.0332907000
_diffrn_orient_matrix_UB_21      0.0594077000
_diffrn_orient_matrix_UB_22      -0.0140472000
_diffrn_orient_matrix_UB_23      -0.1037117000
_diffrn_orient_matrix_UB_31      -0.0684644000
_diffrn_orient_matrix_UB_32      -0.0927956000
_diffrn_orient_matrix_UB_33      -0.0118074000
_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  0.0238
_diffrn_reflns_av_unetI/netI     0.0243
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            22982
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.766
_diffrn_reflns_theta_min         3.604
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.494
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75296
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.82a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.490
_exptl_crystal_description       block
_exptl_crystal_F_000             876
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.178
_exptl_crystal_size_min          0.139
_refine_diff_density_max         1.364
_refine_diff_density_min         -0.627
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     435
_refine_ls_number_reflns         7655
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0287
_refine_ls_R_factor_gt           0.0278
_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^)+(0.0306P)^2^+1.9628P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0692
_refine_ls_wR_factor_ref         0.0698
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7418
_reflns_number_total             7655
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02755h2.cif
_cod_data_source_block           jw092
_cod_depositor_comments
'Adding full bibliography for 7717232--7717238.cif.'
_cod_database_code               7717235
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C31H46N10Cu1Ru1P1Cl3
_reflns_odcompleteness_completeness 98.48
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_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:
 C31(H31)
2.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B)
2.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C29(H29), C7(H7), C27(H27), C20(H20), C23(H23), C3(H3),
 C26(H26), C28(H28), C22(H22), C21(H21)
2.d Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C14(H14A,H14B,
 H14C), C15(H15A,H15B,H15C), C13(H13A,H13B,H13C), C16(H16A,H16B,H16C), C33(H33A,
 H33B,H33C), C32(H32A,H32B,H32C), C35(H35A,H35B,H35C), C37(H37A,H37B,H37C)
;
_shelx_res_checksum              66915
_shelx_hkl_checksum              57206
_olex2_date_sample_data_collection 2022-04-08
_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 1.629
_oxdiff_exptl_absorpt_empirical_full_min 0.786