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_7717237
_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
'C64 H84 Cl4 Cu2 N6 P2 Ru2, 2.526(F3.932 P0.655), 2(C2 H3 N), Cl0.689 Cu0.345'
_chemical_formula_sum            'C68 H90 Cl4.69 Cu2.35 F9.93 N8 P3.66 Ru2'
_chemical_formula_weight         1839.21
_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             2024-09-26
_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                113.508(3)
_cell_angle_beta                 100.048(3)
_cell_angle_gamma                96.419(3)
_cell_formula_units_Z            1
_cell_length_a                   8.3879(3)
_cell_length_b                   16.3160(6)
_cell_length_c                   16.3624(5)
_cell_measurement_reflns_used    5570
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      71.7610
_cell_measurement_theta_min      5.1090
_cell_volume                     1980.74(13)
_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 1.5 (Bourhis et al., 2015)'
_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 0.994
_diffrn_measured_fraction_theta_max 0.974
_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   -104.00 -25.00   1.00    2.98    --  -37.17 -57.00 -90.00   79
  2  \w     38.00 104.00   1.00    2.98    --   37.17  57.00  60.00   66
  3  \w     27.00  81.00   1.00    2.98    --   37.17-125.00 -90.00   54
  4  \w    -30.00   0.00   1.00    2.98    --   37.17 -57.00 120.00   30
  5  \w     27.00  86.00   1.00    2.98    --   37.17-125.00  30.00   59
  6  \w      2.00  54.00   1.00    2.98    --   37.17 -57.00 120.00   52
  7  \w    -29.00 102.00   1.00    2.98    --   37.17   0.00  90.00  131
  8  \w     17.00  72.00   1.00    2.98    --   37.17 -99.00 120.00   55
  9  \w     99.00 130.00   1.00   11.93    --  111.00 -64.00 120.00   31
 10  \w     42.00 119.00   1.00   11.93    --  111.00 -38.00 150.00   77
 11  \w     49.00  82.00   1.00   11.93    --  111.00 -64.00 120.00   33
 12  \w     56.00 109.00   1.00   11.93    --  111.00-111.00-150.00   53
 13  \w     53.00 109.00   1.00   11.93    --  111.00-111.00 -60.00   56
 14  \w     42.00 106.00   1.00   11.93    --  111.00 -92.00 -30.00   64
 15  \w     42.00 128.00   1.00   11.93    --  111.00 -38.00 -30.00   86
 16  \w    126.00 174.00   1.00   11.93    --  111.00 111.00  60.00   48
 17  \w    105.00 178.00   1.00   11.93    --  111.00  77.00 120.00   73
 18  \w     77.00 109.00   1.00   11.93    --  111.00-111.00 150.00   32
 19  \w    114.00 178.00   1.00   11.93    --  111.00  77.00  90.00   64
 20  \w    110.00 158.00   1.00   11.93    --  111.00  77.00 150.00   48
 21  \w     49.00 106.00   1.00   11.93    --  111.00 -92.00  30.00   57
 22  \w     42.00 129.00   1.00   11.93    --  111.00 -38.00  60.00   87
 23  \w     57.00 113.00   1.00   11.93    --  111.00 -64.00  30.00   56
 24  \w     70.00 178.00   1.00   11.93    --  111.00   0.00  90.00  108
;
_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      0.1723235000
_diffrn_orient_matrix_UB_12      -0.0239766000
_diffrn_orient_matrix_UB_13      -0.0013111000
_diffrn_orient_matrix_UB_21      -0.0495276000
_diffrn_orient_matrix_UB_22      -0.0761731000
_diffrn_orient_matrix_UB_23      0.0292087000
_diffrn_orient_matrix_UB_31      -0.0640819000
_diffrn_orient_matrix_UB_32      -0.0683416000
_diffrn_orient_matrix_UB_33      -0.1016542000
_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  0.0228
_diffrn_reflns_av_unetI/netI     0.0405
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            14037
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.722
_diffrn_reflns_theta_min         5.115
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.453
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72485
_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    1.542
_exptl_crystal_description       block
_exptl_crystal_F_000             934
_exptl_crystal_size_max          0.304
_exptl_crystal_size_mid          0.163
_exptl_crystal_size_min          0.142
_refine_diff_density_max         1.463
_refine_diff_density_min         -1.001
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     474
_refine_ls_number_reflns         7822
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0585
_refine_ls_R_factor_gt           0.0470
_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^)+(0.0686P)^2^+1.8428P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1226
_refine_ls_wR_factor_ref         0.1318
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6494
_reflns_number_total             7822
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02755h2.cif
_cod_data_source_block           jw090
_cod_depositor_comments
'Adding full bibliography for 7717232--7717238.cif.'
_cod_database_code               7717237
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N P Ru Cu F'
_shelx_estimated_absorpt_t_max   0.461
_shelx_estimated_absorpt_t_min   0.244
_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. Shared sites
{P3, Cu3}
3. Restrained distances
 P3-F7 \\sim Cu3-F7
 with sigma of 0.02
 P3-F5 \\sim Cu3-F5
 with sigma of 0.02
 P3-F4 \\sim Cu3-F4
 with sigma of 0.02
 P3-Cl3 \\sim Cu3-Cl3
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Cl3: within 2A with sigma of 0.005 and sigma for terminal atoms of 0.01 within
2A
Uanis(Cl3) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(F5) \\sim Ueq, Uanis(F5) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(F4) \\sim Ueq, Uanis(F4) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(P3) = Uanis(Cu3)
5. Others
 Sof(Cl3)=1-FVAR(1)
 Sof(Cu3)=0.5*(1-FVAR(2))
 Sof(P3)=0.5*FVAR(2)
 Sof(F7)=Sof(F5)=Sof(F4)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C31(H31)
6.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B)
6.c Aromatic/amide H refined with riding coordinates:
 C26(H26), C29(H29), C7(H7), C4(H4), C20(H20), C6(H6), C27(H27), C3(H3),
 C23(H23), C21(H21), C28(H28), C22(H22)
6.d Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,
 H15C), C17(H17A,H17B,H17C), C24(H24A,H24B,H24C), C16(H16A,H16B,H16C), C35(H35A,
 H35B,H35C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C)
;
_shelx_res_checksum              8855
_shelx_hkl_checksum              8779
_olex2_date_sample_data_collection 2022-04-12
_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 1.721
_oxdiff_exptl_absorpt_empirical_full_min 0.717