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_7717232
_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_absolute_configuration rm
_chemical_formula_moiety         '2(C22 H28 N3 P), C H Cl3'
_chemical_formula_sum            'C45 H57 Cl3 N6 P2'
_chemical_formula_weight         850.25
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-10-31
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2024-09-26 deposited with the CCDC.	2024-10-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.9800(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   18.4963(2)
_cell_length_b                   6.17950(10)
_cell_length_c                   20.5648(3)
_cell_measurement_reflns_used    8407
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      73.5740
_cell_measurement_theta_min      5.0060
_cell_volume                     2235.72(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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1297
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_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    -76.00 -50.00   1.00    5.25    --  -36.95 125.00-180.00   26
  2  \w    -44.00 -16.00   1.00    5.25    --  -36.95 125.00-180.00   28
  3  \w    -21.00  44.00   1.00    5.25    --   36.95 -38.00   0.00   65
  4  \w     29.00  63.00   1.00    5.25    --   36.95-125.00  30.00   34
  5  \w    -32.00  51.00   1.00    5.25    --   36.95 -38.00-150.00   83
  6  \w     59.00  89.00   1.00    5.25    --   36.95-125.00 -30.00   30
  7  \w     11.00  37.00   1.00    5.25    --   36.95 -99.00-180.00   26
  8  \w     45.00  76.00   1.00    5.25    --   36.95 -99.00-180.00   31
  9  \w     35.00  64.00   1.00    5.25    --   36.95 -99.00  90.00   29
 10  \w     29.00  93.00   1.00    5.25    --   36.95  38.00-150.00   64
 11  \w     42.00  75.00   1.00   21.00    --  111.00-111.00 -30.00   33
 12  \w    101.00 127.00   1.00   21.00    --  111.00 -38.00 -60.00   26
 13  \w     92.00 118.00   1.00   21.00    --  111.00 -77.00   0.00   26
 14  \w     81.00 109.00   1.00   21.00    --  111.00-111.00 -30.00   28
 15  \w     79.00 107.00   1.00   21.00    --  111.00-111.00   0.00   28
 16  \w     60.00 100.00   1.00   21.00    --  111.00 -38.00 -60.00   40
 17  \w    108.00 148.00   1.00   21.00    --  111.00  64.00  30.00   40
 18  \w     51.00  79.00   1.00   21.00    --  111.00-111.00-120.00   28
 19  \w     43.00 102.00   1.00   21.00    --  111.00 -92.00   0.00   59
 20  \w     96.00 124.00   1.00   21.00    --  111.00 -25.00   0.00   28
 21  \w     63.00 104.00   1.00   21.00    --  111.00 -92.00-120.00   41
 22  \w     43.00  73.00   1.00   21.00    --  111.00-111.00   0.00   30
 23  \w     69.00 101.00   1.00   21.00    --  111.00 -92.00-180.00   32
 24  \w    104.00 137.00   1.00   21.00    --  111.00  77.00 -90.00   33
 25  \w    152.00 177.00   1.00   21.00    --  111.00  77.00 -90.00   25
 26  \w     49.00  80.00   1.00   21.00    --  111.00 -77.00   0.00   31
 27  \w     48.00  77.00   1.00   21.00    --  111.00 -25.00   0.00   29
 28  \w    109.00 171.00   1.00   21.00    --  111.00 111.00  26.00   62
 29  \w     44.00  88.00   1.00   21.00    --  111.00 -50.00  60.00   44
 30  \w    124.00 177.00   1.00   21.00    --  111.00  25.00 120.00   53
 31  \w    115.00 142.00   1.00   21.00    --  111.00  77.00 120.00   27
 32  \w     81.00 106.00   1.00   21.00    --  111.00 -92.00-150.00   25
 33  \w     91.00 124.00   1.00   21.00    --  111.00 -77.00 -90.00   33
 34  \w     52.00 114.00   1.00   21.00    --  111.00 -50.00  90.00   62
 35  \w     76.00 101.00   1.00   21.00    --  111.00 -92.00  30.00   25
 36  \w     64.00  90.00   1.00   21.00    --  111.00 -92.00  90.00   26
 37  \w     99.00 129.00   1.00   21.00    --  111.00  64.00 -90.00   30
 38  \w     99.00 137.00   1.00   21.00    --  111.00 -77.00 -46.81   38
 39  \w     60.00  85.00   1.00   21.00    --  111.00 -77.00 -46.81   25
;
_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      -0.0218592000
_diffrn_orient_matrix_UB_12      -0.2291290000
_diffrn_orient_matrix_UB_13      0.0168179000
_diffrn_orient_matrix_UB_21      -0.0083078000
_diffrn_orient_matrix_UB_22      0.0842397000
_diffrn_orient_matrix_UB_23      0.0678460000
_diffrn_orient_matrix_UB_31      -0.0843448000
_diffrn_orient_matrix_UB_32      0.0510866000
_diffrn_orient_matrix_UB_33      -0.0363386000
_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  0.0314
_diffrn_reflns_av_unetI/netI     0.0452
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            15589
_diffrn_reflns_point_group_measured_fraction_full 0.883
_diffrn_reflns_point_group_measured_fraction_max 0.866
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.856
_diffrn_reflns_theta_min         3.863
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.827
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73142
_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            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.263
_exptl_crystal_description       needle
_exptl_crystal_F_000             900
_exptl_crystal_size_max          0.494
_exptl_crystal_size_mid          0.064
_exptl_crystal_size_min          0.042
_refine_diff_density_max         0.393
_refine_diff_density_min         -0.242
_refine_diff_density_rms         0.046
_refine_ls_abs_structure_details
;
 Flack x determined using 2541 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.065(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     517
_refine_ls_number_reflns         7852
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0389
_refine_ls_R_factor_gt           0.0358
_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^)+(0.0554P)^2^+0.0477P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0913
_refine_ls_wR_factor_ref         0.0934
_reflns_Friedel_coverage         0.582
_reflns_Friedel_fraction_full    0.741
_reflns_Friedel_fraction_max     0.706
_reflns_number_gt                7325
_reflns_number_total             7852
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02755h2.cif
_cod_data_source_block           jw105
_cod_depositor_comments
'Adding full bibliography for 7717232--7717238.cif.'
_cod_database_code               7717232
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N P Cl Ru'
_shelx_estimated_absorpt_t_max   0.890
_shelx_estimated_absorpt_t_min   0.336
_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:
 C24(H24)
2.b Secondary CH2 refined with riding coordinates:
 C10(H10C,H10D), C10A(H10A,H10B)
2.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C4(H4), C6A(H6A), C20A(H20A), C3(H3), C3A(H3A), C7A(H7A),
 C4A(H4A), C20(H20), C21A(H21A), C22(H22), C23(H23), C22A(H22A), C21(H21),
 C23A(H23A)
2.d Idealised Me refined as rotating group:
 C14(H14D,H14E,H14F), C13(H13D,H13E,H13F), C15(H15D,H15E,H15F), C17(H17D,H17E,
 H17F), C18(H18D,H18E,H18F), C18A(H18A,H18B,H18C), C16(H16D,H16E,H16F),
 C14A(H14A,H14B,H14C), C13A(H13A,H13B,H13C), C15A(H15A,H15B,H15C), C16A(H16A,
 H16B,H16C), C17A(H17A,H17B,H17C)
;
_shelx_res_checksum              21174
_shelx_hkl_checksum              77822
_olex2_date_sample_data_collection 2022-06-02
_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 1.512
_oxdiff_exptl_absorpt_empirical_full_min 0.654