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_7717236
_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         'C26 H36 Cu2 N3 O P'
_chemical_formula_sum            'C26 H36 Cu2 N3 O P'
_chemical_formula_weight         564.63
_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     iterative
_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                96.178(2)
_cell_angle_beta                 98.598(2)
_cell_angle_gamma                108.172(3)
_cell_formula_units_Z            2
_cell_length_a                   8.2661(3)
_cell_length_b                   11.0365(3)
_cell_length_c                   15.4542(4)
_cell_measurement_reflns_used    4121
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      72.9880
_cell_measurement_theta_min      4.7860
_cell_volume                     1306.52(7)
_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    'olex2.solve 1.3 (Bourhis et al., 2015)'
_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 0.992
_diffrn_measured_fraction_theta_max 0.966
_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    -94.00 -27.00   1.00    1.00    --  -36.18 -57.00   0.00   67
  2  \w     34.00  90.00   1.00    1.00    --   36.18-125.00-180.00   56
  3  \w     21.00 105.00   1.00    1.00    --   36.18  38.00 -30.00   84
  4  \w    -29.00  53.00   1.00    1.00    --   36.18 -57.00  60.00   82
  5  \w     29.00  82.00   1.00    1.00    --   36.18-125.00  30.00   53
  6  \w    -33.00  41.00   1.00    1.00    --   36.18 -38.00 150.00   74
  7  \w    -23.00  52.00   1.00    1.00    --   36.18 -57.00-150.00   75
  8  \w     51.00 109.00   1.00    2.34    --  109.99-111.00   0.00   58
  9  \w     58.00 131.00   1.00    2.34    --  109.99 -30.00-150.00   73
 10  \w     77.00 128.00   1.00    2.34    --  109.99 -77.00-150.00   51
 11  \w     44.00 122.00   1.00    2.34    --  109.99 -45.00 150.00   78
 12  \w    120.00 162.00   1.00    2.34    --  109.99  77.00 -90.00   42
 13  \w     56.00 106.00   1.00    2.34    --  109.99 -95.00-150.00   50
 14  \w     52.00 123.00   1.00    2.34    --  109.99 -45.00 -60.00   71
 15  \w     41.00 106.00   1.00    2.34    --  109.99 -95.00 150.00   65
 16  \w    120.00 172.00   1.00    2.34    --  109.99 111.00-150.00   52
 17  \w    114.00 176.00   1.00    2.34    --  109.99  77.00 -60.00   62
 18  \w     48.00 178.00   1.00    2.34    --  109.99   0.00  90.00  130
 19  \w     55.00 105.00   1.00    2.34    --  109.99 -95.00  60.00   50
;
_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      0.1089089000
_diffrn_orient_matrix_UB_12      -0.0622342000
_diffrn_orient_matrix_UB_13      -0.0505632000
_diffrn_orient_matrix_UB_21      -0.1519463000
_diffrn_orient_matrix_UB_22      -0.0516165000
_diffrn_orient_matrix_UB_23      -0.0801610000
_diffrn_orient_matrix_UB_31      0.0709156000
_diffrn_orient_matrix_UB_32      0.1250791000
_diffrn_orient_matrix_UB_33      -0.0382567000
_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  0.0194
_diffrn_reflns_av_unetI/netI     0.0329
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            7947
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.229
_diffrn_reflns_theta_min         4.274
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.756
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92310
_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            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.435
_exptl_crystal_description       prism
_exptl_crystal_F_000             588
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.413
_refine_diff_density_min         -0.439
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         5072
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0381
_refine_ls_R_factor_gt           0.0341
_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^)+(0.0498P)^2^+0.5203P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0897
_refine_ls_wR_factor_ref         0.0937
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4561
_reflns_number_total             5072
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02755h2.cif
_cod_data_source_block           jw063
_cod_depositor_comments
'Adding full bibliography for 7717232--7717238.cif.'
_cod_database_code               7717236
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         P1O1Cu2N3C26H36
_reflns_odcompleteness_completeness 94.61
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C10(H10), C4(H4), C6(H6), C7(H7), C20(H20), C23(H23), C22(H22),
 C21(H21)
2.b Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C13(H13A,H13B,H13C), C18(H18A,H18B,H18C), C16(H16A,H16B,
 H16C), C25(H25A,H25B,H25C), C27(H27A,H27B,H27C), C14(H14A,H14B,H14C), C26(H26A,
 H26B,H26C), C15(H15A,H15B,H15C)
;
_shelx_res_checksum              32220
_shelx_hkl_checksum              84875
_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 1.375
_oxdiff_exptl_absorpt_empirical_full_min 0.854