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_7719452
_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         'C16 H25 I2 O3 P Ru, 0.417[H2O]'
_chemical_formula_sum            'C16 H25.83 I2 O3.42 P Ru'
_chemical_formula_weight         658.76
_space_group_crystal_system      hexagonal
_space_group_IT_number           170
_space_group_name_Hall           'P 65'
_space_group_name_H-M_alt        'P 65'
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   16.7253(2)
_cell_length_b                   16.7253(2)
_cell_length_c                   13.1053(2)
_cell_measurement_reflns_used    15939
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      69.6020
_cell_measurement_theta_min      3.0210
_cell_volume                     3174.87(7)
_computing_cell_refinement       'CrysAlisPro 1.171.42.84a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.84a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.84a (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      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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      0.00  81.00   0.50    1.00    --   42.11-109.00-138.00  162
  2  \w     84.00 165.00   0.50    3.00    --   98.65  36.00  78.00  162
  3  \w     31.00  83.00   0.50    3.00    --   98.65 -68.00  -8.00  104
  4  \w     31.00 109.00   0.50    3.00    --   98.65-109.00-138.00  156
  5  \w     80.00 165.00   0.50    3.00    --   98.65  49.00 112.00  170
  6  \w   -109.00 -64.00   0.50    1.00    --  -41.49-138.00 -90.00   90
  7  \w   -109.00 -64.00   0.50    1.00    --  -41.49-138.00 -30.00   90
  8  \w    -48.00  26.00   0.50    1.00    --  -41.49  43.00-180.00  148
  9  \w     64.00 109.00   0.50    1.00    --   42.11 138.00-180.00   90
 10  \w     64.00 109.00   0.50    1.00    --   42.11 138.00 -60.00   90
 11  \w     64.00 109.00   0.50    1.00    --   42.11 138.00  90.00   90
 12  \w    -34.00  24.00   0.50    1.00    --   42.11 -11.00 -90.00  116
 13  \w    -34.00  24.00   0.50    1.00    --   42.11 -11.00  60.00  116
 14  \w    -68.00 -30.00   0.50    3.00    --  -98.03  59.00  30.00   76
 15  \w    -57.00 -31.00   0.50    3.00    --  -98.03  50.00  60.00   52
 16  \w   -106.00 -25.00   0.50    3.00    --  -98.03  96.00 -30.00  162
 17  \w    -57.00 -31.00   0.50    3.00    --  -98.03  50.00  90.00   52
 18  \w   -165.00 -83.00   0.50    3.00    --  -98.03 -36.00 -77.00  164
 19  \w     31.00  68.00   0.50    3.00    --   98.65 -59.00-120.00   74
 20  \w     31.00  68.00   0.50    3.00    --   98.65 -59.00 -90.00   74
 21  \w     35.00 109.00   0.50    3.00    --   98.65-117.00-180.00  148
 22  \w     26.00 108.00   0.50    1.00    --   42.11  41.00  38.00  164
 23  \w    -26.00  37.00   0.50    1.00    --   42.11 -32.00-150.00  126
 24  \w     22.00 109.00   0.50    1.00    --   42.11  54.00-150.00  174
 25  \w     18.00 110.00   0.50    1.00    --   42.11  68.00 124.00  184
 26  \w     19.00 110.00   0.50    1.00    --   42.11  65.00-120.00  182
 27  \w     15.00 111.00   0.50    1.00    --   42.11  77.00  60.00  192
 28  \w     15.00 111.00   0.50    1.00    --   42.11  77.00 150.00  192
 29  \w     15.00 111.00   0.50    1.00    --   42.11  77.00 -60.00  192
 30  \w     75.00 155.00   0.50    3.00    --   98.65  68.00   0.00  160
;
_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      0.0432308000
_diffrn_orient_matrix_UB_12      0.0441849000
_diffrn_orient_matrix_UB_13      0.1035053000
_diffrn_orient_matrix_UB_21      -0.0345924000
_diffrn_orient_matrix_UB_22      0.0692066000
_diffrn_orient_matrix_UB_23      -0.0130939000
_diffrn_orient_matrix_UB_31      -0.0907616000
_diffrn_orient_matrix_UB_32      -0.0674658000
_diffrn_orient_matrix_UB_33      0.0543327000
_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  0.0593
_diffrn_reflns_av_unetI/netI     0.0346
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            21266
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.123
_diffrn_reflns_theta_min         3.051
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    29.723
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.16165
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.84a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear reddish violet'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    2.067
_exptl_crystal_description       plate
_exptl_crystal_F_000             1885
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.638
_refine_diff_density_min         -0.660
_refine_diff_density_rms         0.155
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   -0.014(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     212
_refine_ls_number_reflns         3832
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0422
_refine_ls_R_factor_gt           0.0408
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0862P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1069
_refine_ls_wR_factor_ref         0.1080
_reflns_Friedel_coverage         0.884
_reflns_Friedel_fraction_full    0.974
_reflns_Friedel_fraction_max     0.972
_reflns_number_gt                3680
_reflns_number_total             3832
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01437a2.cif
_cod_data_source_block           i119
_cod_depositor_comments
'Adding full bibliography for 7719452--7719457.cif.'
_cod_original_cell_volume        3174.87(9)
_cod_database_code               7719452
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H I O P Ru'
_shelx_estimated_absorpt_t_max   0.383
_shelx_estimated_absorpt_t_min   0.075
_diffrn_oxdiff_digest_hkl
;
01e33cf08f3446270d86d9e36d1ddd1492448c
;
_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:
 C7(H7)
2.b Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B), C15(H15A,H15B)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6)
2.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C16(H16A,H16B,H16C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 25 electrons were 
found in a volume of 308\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
0.417[H2O] per Unit Cell 
which account for 25 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              21999
_shelx_hkl_checksum              99333
_shelx_fab_checksum              22335
_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 4.355
_oxdiff_exptl_absorpt_empirical_full_min 0.598