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_7719453
_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         'C22 H30 I O3 P Ru'
_chemical_formula_sum            'C22 H30 I O3 P Ru'
_chemical_formula_weight         601.40
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2025-06-02
_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                 93.2955(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.46970(10)
_cell_length_b                   7.90641(5)
_cell_length_c                   15.80923(9)
_cell_measurement_reflns_used    17642
_cell_measurement_temperature    295.53(17)
_cell_measurement_theta_max      69.5620
_cell_measurement_theta_min      2.3930
_cell_volume                     2304.79(2)
_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  (Sheldrick, 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      295.53(17)
_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 0.994
_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    -29.00  28.00   0.50    0.20    --   42.11 -21.00 150.00  114
  2  \w    -25.00  62.00   0.50    0.20    --   42.11 -54.00  90.00  174
  3  \w    -28.00  30.00   0.50    0.20    --   42.11 -24.00  80.00  116
  4  \w    -34.00  24.00   0.50    0.20    --   42.11 -11.00  30.00  116
  5  \w    -29.00  28.00   0.50    0.20    --   42.11 -21.00 -30.00  114
  6  \w    -25.00  62.00   0.50    0.20    --   42.11 -54.00-150.00  174
  7  \w     19.00 101.00   0.50    0.20    --   42.11-138.00-180.00  164
  8  \w     31.00  83.00   0.50    0.40    --   98.65 -68.00-180.00  104
  9  \w     35.00 109.00   0.50    0.40    --   98.65-117.00-150.00  148
 10  \w     25.00 106.00   0.50    0.40    --   98.65 -96.00 -90.00  162
 11  \w     31.00  68.00   0.50    0.40    --   98.65 -59.00-120.00   74
 12  \w     31.00  68.00   0.50    0.40    --   98.65 -59.00 -90.00   74
 13  \w     31.00  68.00   0.50    0.40    --   98.65 -59.00 -60.00   74
 14  \w     31.00  83.00   0.50    0.40    --   98.65 -68.00 150.00  104
 15  \w     82.00 166.00   0.50    0.40    --   98.65  42.00 -30.00  168
 16  \w     83.00 169.00   0.50    0.40    --   98.65  24.00-114.00  172
 17  \w     85.00 166.00   0.50    0.40    --   98.65  33.00 -90.00  162
 18  \w     19.00 110.00   0.50    0.20    --   42.11  65.00 -60.00  182
 19  \w     19.00 110.00   0.50    0.20    --   42.11  65.00   0.00  182
 20  \w     15.00 111.00   0.50    0.20    --   42.11  77.00  60.00  192
 21  \w     26.00 113.00   0.50    0.20    --   42.11  24.00-114.00  174
 22  \w   -110.00 -14.00   0.50    0.20    --  -41.49 -77.00-150.00  192
 23  \w   -110.00 -14.00   0.50    0.20    --  -41.49 -77.00-180.00  192
 24  \w   -110.00 -14.00   0.50    0.20    --  -41.49 -77.00-120.00  192
 25  \w   -110.00 -14.00   0.50    0.20    --  -41.49 -77.00 -60.00  192
 26  \w   -110.00 -14.00   0.50    0.20    --  -41.49 -77.00  60.00  192
 27  \w   -110.00 -14.00   0.50    0.20    --  -41.49 -77.00  90.00  192
 28  \w   -110.00 -14.00   0.50    0.20    --  -41.49 -77.00 120.00  192
 29  \w   -110.00 -14.00   0.50    0.20    --  -41.49 -77.00 150.00  192
 30  \w   -112.00 -26.00   0.50    0.20    --  -41.49 -24.00  80.00  172
 31  \w   -108.00 -24.00   0.50    0.20    --  -41.49 -43.00 -30.00  168
 32  \w   -109.00 -64.00   0.50    0.20    --  -41.49-138.00 -90.00   90
 33  \w   -109.00 -64.00   0.50    0.20    --  -41.49-138.00-150.00   90
 34  \w   -166.00 -84.00   0.50    0.40    --  -98.03 -33.00  30.00  164
 35  \w   -169.00 -83.00   0.50    0.40    --  -98.03 -24.00  80.00  172
 36  \w   -165.00 -76.00   0.50    0.40    --  -98.03 -59.00 150.00  178
 37  \w   -105.00 -29.00   0.50    0.40    --  -98.03  77.00  30.00  152
 38  \w    -65.00  26.00   0.50    0.20    --  -41.49  65.00 150.00  182
 39  \w    -57.00 -31.00   0.50    0.40    --  -98.03  50.00 120.00   52
 40  \w    -68.00 -30.00   0.50    0.40    --  -98.03  59.00  90.00   76
 41  \w    -57.00 -31.00   0.50    0.40    --  -98.03  50.00  30.00   52
 42  \w    -30.00  29.00   0.50    0.20    --  -41.49  24.00-114.00  118
 43  \w   -106.00 -25.00   0.50    0.40    --  -98.03  96.00 -60.00  162
 44  \w   -100.00 -19.00   0.50    0.20    --  -41.49 138.00-180.00  162
 45  \w    -79.00   4.00   0.50    0.20    --  -41.49 104.00  30.00  166
;
_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      -0.0257191000
_diffrn_orient_matrix_UB_12      0.0580269000
_diffrn_orient_matrix_UB_13      -0.0897739000
_diffrn_orient_matrix_UB_21      -0.0794898000
_diffrn_orient_matrix_UB_22      -0.0177588000
_diffrn_orient_matrix_UB_23      0.0233376000
_diffrn_orient_matrix_UB_31      0.0004168000
_diffrn_orient_matrix_UB_32      0.1851707000
_diffrn_orient_matrix_UB_33      0.0303663000
_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  0.0341
_diffrn_reflns_av_unetI/netI     0.0223
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            24704
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.744
_diffrn_reflns_theta_min         2.396
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    16.833
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.39212
_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 orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.733
_exptl_crystal_description       'rect. Prism'
_exptl_crystal_F_000             1192
_exptl_crystal_size_max          0.244
_exptl_crystal_size_mid          0.095
_exptl_crystal_size_min          0.062
_refine_diff_density_max         0.538
_refine_diff_density_min         -0.660
_refine_diff_density_rms         0.060
_refine_ls_extinction_coef       0.00024(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     258
_refine_ls_number_reflns         4326
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0273
_refine_ls_R_factor_gt           0.0248
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0271P)^2^+1.2860P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0599
_refine_ls_wR_factor_ref         0.0612
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3982
_reflns_number_total             4326
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01437a2.cif
_cod_data_source_block           i1167_auto
_cod_depositor_comments
'Adding full bibliography for 7719452--7719457.cif.'
_cod_database_code               7719453
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H O P I Ru'
_chemical_oxdiff_usercomment     'BQAM 38'
_shelx_estimated_absorpt_t_max   0.422
_shelx_estimated_absorpt_t_min   0.105
_diffrn_oxdiff_digest_hkl
;
01fceb51a09d8fc18638655061ba009bf363e9
;
_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:
 C13(H13)
2.b Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B), C21(H21A,H21B)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C11(H11), C12(H12)
2.d Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C22(H22A,H22B,
 H22C)
;
_shelx_res_checksum              24956
_shelx_hkl_checksum              65060
_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 2.029
_oxdiff_exptl_absorpt_empirical_full_min 0.738