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_7717233
_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 H43 Cl N3 P Ru, Cl'
_chemical_formula_sum            'C32 H43 Cl2 N3 P Ru'
_chemical_formula_weight         672.63
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a :2'
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   32.5802(3)
_cell_length_b                   32.5802(3)
_cell_length_c                   12.6410(3)
_cell_measurement_reflns_used    8563
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      76.9720
_cell_measurement_theta_min      3.7380
_cell_volume                     13418.0(4)
_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 0.997
_diffrn_measured_fraction_theta_max 0.963
_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   -116.00 -75.00   0.50    0.50    --  -46.45 -45.00 -54.00   82
  2  \w    -71.00 -33.00   0.50    0.50    --  -46.45 -45.00 -54.00   76
  3  \w     35.00  63.00   0.50    0.50    --  107.75 -45.00 -54.00   56
  4  \w    128.00 154.00   0.50    0.50    --  107.75  45.00  96.00   52
  5  \w      1.00  26.00   0.50    0.50    --  -46.45  19.00-150.00   50
  6  \w     -3.00  23.00   0.50    0.50    --  -46.45  19.00 120.00   52
  7  \w      0.00  25.00   0.50    0.50    --  -46.45  19.00-120.00   50
  8  \w     37.00  81.00   0.50    0.50    --  107.75 -61.00   0.00   88
  9  \w     39.00  75.00   0.50    0.50    --  107.75 -61.00-120.00   72
 10  \w     38.00  73.00   0.50    0.50    --  107.75 -45.00-120.00   70
 11  \w     33.00  59.00   0.50    0.50    --  107.75 -30.00  30.00   52
 12  \w     41.00  97.00   0.50    0.50    --  107.75-125.00 -90.00  112
 13  \w    104.00 163.00   0.50    0.50    --  107.75 105.00 -42.00  118
;
_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      0.0402578000
_diffrn_orient_matrix_UB_12      -0.0247077000
_diffrn_orient_matrix_UB_13      -0.0056520000
_diffrn_orient_matrix_UB_21      -0.0083020000
_diffrn_orient_matrix_UB_22      -0.0093831000
_diffrn_orient_matrix_UB_23      -0.1175022000
_diffrn_orient_matrix_UB_31      0.0234014000
_diffrn_orient_matrix_UB_32      0.0392113000
_diffrn_orient_matrix_UB_33      -0.0317000000
_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  0.0640
_diffrn_reflns_av_unetI/netI     0.0642
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            21093
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.997
_diffrn_reflns_theta_min         3.751
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.877
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56130
_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            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.332
_exptl_crystal_description       block
_exptl_crystal_F_000             5584
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.129
_exptl_crystal_size_min          0.067
_refine_diff_density_max         0.510
_refine_diff_density_min         -0.661
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         6925
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0584
_refine_ls_R_factor_gt           0.0457
_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^)+(0.0546P)^2^+5.1814P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1167
_refine_ls_wR_factor_ref         0.1241
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5380
_reflns_number_total             6925
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02755h2.cif
_cod_data_source_block           jw167_auto
_cod_depositor_comments
'Adding full bibliography for 7717232--7717238.cif.'
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               7717233
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C32H42N3PCl2Ru
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(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:
 N1(H1), C28(H28), C29(H29), C3(H3), C22(H22), C4(H4), C23(H23), C20(H20),
 C21(H21), C7(H7), C6(H6), C26(H26), C27(H27)
2.d Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C17(H17A,H17B,H17C), C32(H32A,H32B,H32C), C33(H33A,H33B,
 H33C), C14(H14A,H14B,H14C), C16(H16A,H16B,H16C), C24(H24A,H24B,H24C), C13(H13A,
 H13B,H13C), C15(H15A,H15B,H15C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              23815
_shelx_hkl_checksum              61148
_shelx_fab_checksum              65795
_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 1.851
_oxdiff_exptl_absorpt_empirical_full_min 0.659