On the chemistry of <i>p</i>-cymene ruthenium iodide complexes: entry into octahedral phenylated ruthenium(II) complexes supported by chelating bidentate N,N'-donor ligands.
Quillian, Brandon; Marks, Allison; Musso, Kennedy; Durrell, George; Bazemore, Joseph; Padgett, Clifford W.; Fields, Alexis; Zurwell, Dane; Dalton transactions (Cambridge, England : 2003) 54 (2025) 15025–15042; doi:10.1039/d5dt01437a

data_7719454
_publ_section_title
;
 On the chemistry of <i>p</i>-cymene ruthenium iodide complexes: entry
 into octahedral phenylated ruthenium(II) complexes supported by chelating
 bidentate N,N'-donor ligands.
;
_journal_issue                   40
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15025
_journal_page_last               15042
_journal_paper_doi               10.1039/d5dt01437a
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C20 H28 N4 O3 P Ru, I, 1[C2NH3]'
_chemical_formula_sum            'C22 H31 I N5 O3 P Ru'
_chemical_formula_weight         672.46
_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             2025-05-29
_audit_creation_method
;
Olex2 1.5
(compiled 2025.05.22 svn.r631f81ec for OlexSys, GUI svn.r7248)
;
_audit_update_record
;
2025-06-10 deposited with the CCDC.	2025-09-05 downloaded from the CCDC.
;
_cell_angle_alpha                110.6300(10)
_cell_angle_beta                 101.5250(10)
_cell_angle_gamma                90.5820(10)
_cell_formula_units_Z            2
_cell_length_a                   11.2894(2)
_cell_length_b                   11.72880(10)
_cell_length_c                   11.8593(2)
_cell_measurement_reflns_used    8519
_cell_measurement_temperature    278(4)
_cell_measurement_theta_max      69.5100
_cell_measurement_theta_min      4.0140
_cell_volume                     1434.41(4)
_computing_cell_refinement       'CrysAlisPro 1.171.42.70a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.70a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.70a (Rigaku OD, 2022)'
_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      air
_diffrn_ambient_temperature      278(4)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.988
_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     15.00  61.00   0.50    0.20    --   42.11 -54.00-180.00   92
  2  \w    -21.00   4.00   0.50    0.20    --   42.11 -54.00-180.00   50
  3  \w    -25.00  12.00   0.50    0.20    --   42.11 -32.00 -90.00   74
  4  \w    -29.00  24.00   0.50    0.20    --   42.11 -11.00 -30.00  106
  5  \w    -19.00  28.00   0.50    0.20    --   42.11 -21.00   0.00   94
  6  \w    -23.00  18.00   0.50    0.20    --   42.11 -21.00  30.00   82
  7  \w     -9.00  34.00   0.50    0.20    --   42.11 -32.00  30.00   86
  8  \w    -25.00  44.00   0.50    0.20    --   42.11 -80.00 -21.00  138
  9  \w     80.00 127.00   0.50    0.47    --   98.65-145.00   0.00   94
 10  \w     31.00  84.00   0.50    0.47    --   98.65-145.00 150.00  106
 11  \w     31.00  63.00   0.50    0.47    --   98.65-145.00   0.00   64
 12  \w     44.00 109.00   0.50    0.47    --   98.65-117.00   0.00  130
 13  \w     28.00  76.00   0.50    0.20    --   42.11-138.00 -30.00   96
 14  \w     38.00 107.00   0.50    0.47    --   98.65-117.00-180.00  138
 15  \w     36.00  90.00   0.50    0.47    --   98.65-117.00-150.00  108
 16  \w     78.00 107.00   0.50    0.47    --   98.65-117.00-120.00   58
 17  \w     42.00  67.00   0.50    0.47    --   98.65 -80.00 -21.00   50
 18  \w     35.00  61.00   0.50    0.47    --   98.65 -59.00   0.00   52
 19  \w     39.00 103.00   0.50    0.47    --   98.65 -77.00-180.00  128
 20  \w    109.00 135.00   0.50    0.47    --   98.65  33.00 -30.00   52
 21  \w     83.00 139.00   0.50    0.47    --   98.65  42.00 -90.00  112
 22  \w     96.00 166.00   0.50    0.47    --   98.65  80.00 102.00  140
 23  \w    121.00 162.00   0.50    0.47    --   98.65  68.00 150.00   82
 24  \w     92.00 118.00   0.50    0.47    --   98.65  68.00 150.00   52
 25  \w     74.00 107.00   0.50    0.20    --   42.11 138.00   0.00   66
 26  \w     64.00  99.00   0.50    0.20    --   42.11 138.00  60.00   70
 27  \w     89.00 158.00   0.50    0.47    --   98.65 117.00-180.00  138
 28  \w    -66.00 -12.00   0.50    0.20    --  -41.49  80.00 102.00  108
 29  \w     -7.00  26.00   0.50    0.20    --  -41.49  80.00 102.00   66
 30  \w    -36.00 -11.00   0.50    0.20    --  -41.49  32.00-150.00   50
 31  \w     -9.00  17.00   0.50    0.20    --  -41.49  32.00-150.00   52
 32  \w    -57.00 -32.00   0.50    0.47    --  -98.03  50.00  90.00   50
 33  \w    -64.00 -29.00   0.50    0.47    --  -98.03  80.00 102.00   70
 34  \w   -106.00 -77.00   0.50    0.47    --  -98.03  80.00 102.00   58
 35  \w    -78.00 -30.00   0.50    0.47    --  -98.03  68.00 -60.00   96
 36  \w    -56.00 -31.00   0.50    0.47    --  -98.03  50.00 -60.00   50
 37  \w    -57.00 -31.00   0.50    0.47    --  -98.03  50.00-120.00   52
 38  \w    -67.00 -32.00   0.50    0.47    --  -98.03  77.00-120.00   70
 39  \w   -110.00 -38.00   0.50    0.47    --  -98.03 117.00 -30.00  144
 40  \w    -90.00 -43.00   0.50    0.20    --  -41.49 138.00 -90.00   94
 41  \w   -121.00 -75.00   0.50    0.47    --  -98.03 136.00  25.07   92
 42  \w   -110.00 -56.00   0.50    0.47    --  -98.03 117.00  90.00  108
 43  \w    -95.00 -53.00   0.50    0.20    --  -41.49 138.00 150.00   84
 44  \w    -49.00 -19.00   0.50    0.20    --  -41.49 138.00 150.00   60
 45  \w    -59.00 -33.00   0.50    0.20    --  -41.49 -32.00 -30.00   52
 46  \w   -104.00 -63.00   0.50    0.20    --  -41.49 -32.00 -30.00   82
 47  \w    -52.00 -20.00   0.50    0.20    --  -41.49 -65.00 120.00   64
 48  \w   -103.00 -61.00   0.50    0.20    --  -41.49 -65.00 120.00   84
 49  \w   -165.00-113.00   0.50    0.47    --  -98.03 -50.00  30.00  104
 50  \w   -154.00-126.00   0.50    0.47    --  -98.03 -80.00 -21.00   56
 51  \w   -165.00 -78.00   0.50    0.47    --  -98.03 -68.00   0.00  174
 52  \w   -159.00 -85.00   0.50    0.47    --  -98.03 -77.00  90.00  148
 53  \w   -161.00 -90.00   0.50    0.47    --  -98.03 -87.00  60.00  142
 54  \w   -134.00 -78.00   0.50    0.47    --  -98.03-117.00 150.00  112
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at home/near, HyPix3000'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0906091000
_diffrn_orient_matrix_UB_12      0.0180047000
_diffrn_orient_matrix_UB_13      -0.1069109000
_diffrn_orient_matrix_UB_21      -0.0778536000
_diffrn_orient_matrix_UB_22      0.0697708000
_diffrn_orient_matrix_UB_23      0.0907887000
_diffrn_orient_matrix_UB_31      0.0726317000
_diffrn_orient_matrix_UB_32      0.1210733000
_diffrn_orient_matrix_UB_33      0.0234286000
_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  0.0366
_diffrn_reflns_av_unetI/netI     0.0428
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            13344
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.718
_diffrn_reflns_theta_min         4.012
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    13.644
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.50367
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.70a (Rigaku Oxford Diffraction, 2022)
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    1.557
_exptl_crystal_description       prism
_exptl_crystal_F_000             668
_exptl_crystal_size_max          0.327
_exptl_crystal_size_mid          0.051
_exptl_crystal_size_min          0.046
_refine_diff_density_max         1.031
_refine_diff_density_min         -0.780
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     360
_refine_ls_number_reflns         5352
_refine_ls_number_restraints     127
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0389
_refine_ls_R_factor_gt           0.0346
_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^)+(0.0405P)^2^+0.2093P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0890
_refine_ls_wR_factor_ref         0.0917
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4692
_reflns_number_total             5352
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01437a2.cif
_cod_data_source_block           i1009_auto
_cod_depositor_comments
'Adding full bibliography for 7719452--7719457.cif.'
_cod_database_code               7719454
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N O P I Ru'
_shelx_estimated_absorpt_t_max   0.573
_shelx_estimated_absorpt_t_min   0.095
_diffrn_oxdiff_digest_hkl
;
0113eee59148582755557ec7346ffa13db8ae5
;
_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. Restrained distances
 C19-C20 \\sim C19A-C20
 with sigma of 0.02
 O3-P1 \\sim O3A-P1
 with sigma of 0.02
 C19-P1 \\sim C19A-P1
 with sigma of 0.04
 C19-O3 \\sim C19A-O3A
 with sigma of 0.02
 C20-O3 \\sim C20-O3A
 with sigma of 0.04
 C20-C22 \\sim C20-C22A
 with sigma of 0.04
 C20-C21 \\sim C20-C21A
 with sigma of 0.02
 C21-C22 \\sim C21A-C22A
 with sigma of 0.02
 O2-P1 \\sim O2A-P1
 with sigma of 0.02
 C20-O2 \\sim C20-O2A
 with sigma of 0.04
 C18-P1 \\sim C18A-P1
 with sigma of 0.04
 C18-C20 \\sim C18A-C20
 with sigma of 0.02
 C18-O2 \\sim C18A-O2A
 with sigma of 0.02
3. Rigid bond restraints
 O2, O3, C18, C19, C21, C22, O2A, O3A, C18A, C19A, C21A, C22A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
O2 \\sim O3 \\sim C18 \\sim C19 \\sim C21 \\sim C22 \\sim O2A \\sim O3A \\sim
C18A \\sim C19A \\sim C21A \\sim C22A: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
5. Others
 Sof(C18A)=Sof(H18C)=Sof(H18D)=Sof(C19A)=Sof(H19C)=Sof(H19D)=Sof(C21A)=
 Sof(H21C)=Sof(H21D)=Sof(C22A)=Sof(H22D)=Sof(H22E)=Sof(H22F)=Sof(O2A)=Sof(O3A)=
 1-FVAR(1)
 Sof(C18)=Sof(H18A)=Sof(H18B)=Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(C21)=Sof(H21A)=
 Sof(H21B)=Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(H22C)=Sof(O2)=Sof(O3)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B), C21(H21A,H21B), C18A(H18C,
 H18D), C19A(H19C,H19D), C21A(H21C,H21D)
6.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6)
6.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C10(H10A,H10B,H10C), C12(H12A,H12B,H12C), C14(H14A,H14B,
 H14C), C22(H22A,H22B,H22C), C22A(H22D,H22E,H22F), C24(H24A,H24B,H24C)
;
_shelx_res_checksum              70471
_shelx_hkl_checksum              67021
_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 1.787
_oxdiff_exptl_absorpt_empirical_full_min 0.605