#------------------------------------------------------------------------------
#$Date: 2025-11-29 22:00:32 +0100 (Sat 29 de Nov de 2025) $
#$Revision: 303810 $
#$URL: svn://www.crystallography.net/cod/cif/7/71/94/7719454.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7719454
loop_
_publ_author_name
'Quillian, Brandon'
'Marks, Allison'
'Musso, Kennedy'
'Durrell, George'
'Bazemore, Joseph'
'Padgett, Clifford W.'
'Fields, Alexis'
'Zurwell, Dane'
_publ_section_title
;
 On the chemistry of p-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  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     15.00  61.00   0.50    0.20    --   42.11 -54.00-180.00   92
  2  ω    -21.00   4.00   0.50    0.20    --   42.11 -54.00-180.00   50
  3  ω    -25.00  12.00   0.50    0.20    --   42.11 -32.00 -90.00   74
  4  ω    -29.00  24.00   0.50    0.20    --   42.11 -11.00 -30.00  106
  5  ω    -19.00  28.00   0.50    0.20    --   42.11 -21.00   0.00   94
  6  ω    -23.00  18.00   0.50    0.20    --   42.11 -21.00  30.00   82
  7  ω     -9.00  34.00   0.50    0.20    --   42.11 -32.00  30.00   86
  8  ω    -25.00  44.00   0.50    0.20    --   42.11 -80.00 -21.00  138
  9  ω     80.00 127.00   0.50    0.47    --   98.65-145.00   0.00   94
 10  ω     31.00  84.00   0.50    0.47    --   98.65-145.00 150.00  106
 11  ω     31.00  63.00   0.50    0.47    --   98.65-145.00   0.00   64
 12  ω     44.00 109.00   0.50    0.47    --   98.65-117.00   0.00  130
 13  ω     28.00  76.00   0.50    0.20    --   42.11-138.00 -30.00   96
 14  ω     38.00 107.00   0.50    0.47    --   98.65-117.00-180.00  138
 15  ω     36.00  90.00   0.50    0.47    --   98.65-117.00-150.00  108
 16  ω     78.00 107.00   0.50    0.47    --   98.65-117.00-120.00   58
 17  ω     42.00  67.00   0.50    0.47    --   98.65 -80.00 -21.00   50
 18  ω     35.00  61.00   0.50    0.47    --   98.65 -59.00   0.00   52
 19  ω     39.00 103.00   0.50    0.47    --   98.65 -77.00-180.00  128
 20  ω    109.00 135.00   0.50    0.47    --   98.65  33.00 -30.00   52
 21  ω     83.00 139.00   0.50    0.47    --   98.65  42.00 -90.00  112
 22  ω     96.00 166.00   0.50    0.47    --   98.65  80.00 102.00  140
 23  ω    121.00 162.00   0.50    0.47    --   98.65  68.00 150.00   82
 24  ω     92.00 118.00   0.50    0.47    --   98.65  68.00 150.00   52
 25  ω     74.00 107.00   0.50    0.20    --   42.11 138.00   0.00   66
 26  ω     64.00  99.00   0.50    0.20    --   42.11 138.00  60.00   70
 27  ω     89.00 158.00   0.50    0.47    --   98.65 117.00-180.00  138
 28  ω    -66.00 -12.00   0.50    0.20    --  -41.49  80.00 102.00  108
 29  ω     -7.00  26.00   0.50    0.20    --  -41.49  80.00 102.00   66
 30  ω    -36.00 -11.00   0.50    0.20    --  -41.49  32.00-150.00   50
 31  ω     -9.00  17.00   0.50    0.20    --  -41.49  32.00-150.00   52
 32  ω    -57.00 -32.00   0.50    0.47    --  -98.03  50.00  90.00   50
 33  ω    -64.00 -29.00   0.50    0.47    --  -98.03  80.00 102.00   70
 34  ω   -106.00 -77.00   0.50    0.47    --  -98.03  80.00 102.00   58
 35  ω    -78.00 -30.00   0.50    0.47    --  -98.03  68.00 -60.00   96
 36  ω    -56.00 -31.00   0.50    0.47    --  -98.03  50.00 -60.00   50
 37  ω    -57.00 -31.00   0.50    0.47    --  -98.03  50.00-120.00   52
 38  ω    -67.00 -32.00   0.50    0.47    --  -98.03  77.00-120.00   70
 39  ω   -110.00 -38.00   0.50    0.47    --  -98.03 117.00 -30.00  144
 40  ω    -90.00 -43.00   0.50    0.20    --  -41.49 138.00 -90.00   94
 41  ω   -121.00 -75.00   0.50    0.47    --  -98.03 136.00  25.07   92
 42  ω   -110.00 -56.00   0.50    0.47    --  -98.03 117.00  90.00  108
 43  ω    -95.00 -53.00   0.50    0.20    --  -41.49 138.00 150.00   84
 44  ω    -49.00 -19.00   0.50    0.20    --  -41.49 138.00 150.00   60
 45  ω    -59.00 -33.00   0.50    0.20    --  -41.49 -32.00 -30.00   52
 46  ω   -104.00 -63.00   0.50    0.20    --  -41.49 -32.00 -30.00   82
 47  ω    -52.00 -20.00   0.50    0.20    --  -41.49 -65.00 120.00   64
 48  ω   -103.00 -61.00   0.50    0.20    --  -41.49 -65.00 120.00   84
 49  ω   -165.00-113.00   0.50    0.47    --  -98.03 -50.00  30.00  104
 50  ω   -154.00-126.00   0.50    0.47    --  -98.03 -80.00 -21.00   56
 51  ω   -165.00 -78.00   0.50    0.47    --  -98.03 -68.00   0.00  174
 52  ω   -159.00 -85.00   0.50    0.47    --  -98.03 -77.00  90.00  148
 53  ω   -161.00 -90.00   0.50    0.47    --  -98.03 -87.00  60.00  142
 54  ω   -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       'ω 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/[σ²(Fo²)+(0.0405P)²+0.2093P] where P=(Fo²+2Fc²)/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 > 2σ(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_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_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)
;
_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
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.1065(3) 0.2930(3) 0.6753(3) 0.0431(8) Uani 1 1 d . . . . .
C2 C 0.0380(3) 0.1800(3) 0.6151(4) 0.0488(8) Uani 1 1 d . . . . .
H2 H 0.071782 0.116224 0.562644 0.059 Uiso 1 1 calc R U . . .
C3 C -0.0784(4) 0.1587(4) 0.6301(4) 0.0583(10) Uani 1 1 d . . . . .
H3 H -0.121024 0.082384 0.586852 0.070 Uiso 1 1 calc R U . . .
C4 C -0.1307(4) 0.2502(4) 0.7088(5) 0.0658(12) Uani 1 1 d . . . . .
H4 H -0.207654 0.236138 0.720739 0.079 Uiso 1 1 calc R U . . .
C5 C -0.0662(4) 0.3630(4) 0.7695(4) 0.0636(11) Uani 1 1 d . . . . .
H5 H -0.100730 0.425991 0.822016 0.076 Uiso 1 1 calc R U . . .
C6 C 0.0490(4) 0.3840(3) 0.7537(4) 0.0505(9) Uani 1 1 d . . . . .
H6 H 0.090070 0.461206 0.796424 0.061 Uiso 1 1 calc R U . . .
C7 C 0.3403(4) 0.5125(4) 0.9259(4) 0.0532(9) Uani 1 1 d . . . . .
C8 C 0.3629(5) 0.5956(5) 1.0538(4) 0.0824(16) Uani 1 1 d . . . . .
H8A H 0.292714 0.639398 1.068382 0.124 Uiso 1 1 calc R U . . .
H8B H 0.431481 0.652492 1.070197 0.124 Uiso 1 1 calc R U . . .
H8C H 0.379267 0.549676 1.107265 0.124 Uiso 1 1 calc R U . . .
C9 C 0.1512(3) 0.5716(3) 0.6035(4) 0.0452(8) Uani 1 1 d . . . . .
C10 C 0.0924(5) 0.6760(4) 0.5901(5) 0.0677(12) Uani 1 1 d . . . . .
H10A H 0.089344 0.675734 0.508567 0.102 Uiso 1 1 calc R U . . .
H10B H 0.137375 0.749646 0.649877 0.102 Uiso 1 1 calc R U . . .
H10C H 0.011453 0.672182 0.603089 0.102 Uiso 1 1 calc R U . . .
C11 C 0.1785(4) 0.1730(4) 0.3666(4) 0.0518(9) Uani 1 1 d . . . . .
C12 C 0.1259(5) 0.0951(5) 0.2383(4) 0.0794(15) Uani 1 1 d . . . . .
H12A H 0.160220 0.122981 0.183773 0.119 Uiso 1 1 calc R U . . .
H12B H 0.039613 0.099208 0.221609 0.119 Uiso 1 1 calc R U . . .
H12C H 0.143531 0.012135 0.225558 0.119 Uiso 1 1 calc R U . . .
C13 C 0.5378(4) 0.4267(4) 0.6149(4) 0.0507(9) Uani 1 1 d . . . . .
C14 C 0.6581(4) 0.4649(5) 0.6077(5) 0.0744(13) Uani 1 1 d . . . . .
H14A H 0.651670 0.492939 0.540053 0.112 Uiso 1 1 calc R U . . .
H14B H 0.707088 0.396903 0.595189 0.112 Uiso 1 1 calc R U . . .
H14C H 0.695034 0.529952 0.683295 0.112 Uiso 1 1 calc R U . . .
C17 C 0.5442(4) 0.0614(4) 0.7008(5) 0.0667(12) Uani 1 1 d . . . . .
H17A H 0.616592 0.090400 0.766192 0.080 Uiso 1 1 calc R U . . .
H17B H 0.567710 0.006861 0.627416 0.080 Uiso 1 1 calc R U . . .
C20 C 0.4562(4) -0.0074(4) 0.7383(6) 0.0751(16) Uani 1 1 d D . . . .
I1 I 0.20034(3) 0.84453(3) 0.94673(3) 0.07014(11) Uani 1 1 d . . . . .
N1 N 0.3215(3) 0.4470(3) 0.8268(3) 0.0457(7) Uani 1 1 d . . . . .
N2 N 0.1961(3) 0.4880(3) 0.6115(3) 0.0462(7) Uani 1 1 d . . . . .
N3 N 0.2172(3) 0.2320(3) 0.4660(3) 0.0444(7) Uani 1 1 d . . . . .
N4 N 0.4447(3) 0.3963(3) 0.6205(3) 0.0509(7) Uani 1 1 d . . . . .
O1 O 0.4916(3) 0.1646(3) 0.6759(3) 0.0704(9) Uani 1 1 d . . . . .
P1 P 0.35314(8) 0.18126(8) 0.68787(9) 0.0437(2) Uani 1 1 d D . . . .
Ru1 Ru 0.27401(2) 0.33619(2) 0.64673(2) 0.03862(9) Uani 1 1 d . . . . .
C18 C 0.434(2) 0.0901(16) 0.8550(13) 0.076(5) Uani 0.519(12) 1 d D U P A 1
H18A H 0.380247 0.054863 0.890800 0.091 Uiso 0.519(12) 1 calc R U P A 1
H18B H 0.510305 0.119245 0.914875 0.091 Uiso 0.519(12) 1 calc R U P A 1
C19 C 0.3622(9) -0.0581(7) 0.6064(10) 0.059(3) Uani 0.519(12) 1 d D U P A 1
H19A H 0.403733 -0.103170 0.542275 0.071 Uiso 0.519(12) 1 calc R U P A 1
H19B H 0.297923 -0.112633 0.608028 0.071 Uiso 0.519(12) 1 calc R U P A 1
C21 C 0.5302(8) -0.1225(9) 0.7411(12) 0.061(3) Uani 0.519(12) 1 d D U P A 1
H21A H 0.563730 -0.152512 0.667863 0.073 Uiso 0.519(12) 1 calc R U P A 1
H21B H 0.597458 -0.096052 0.812390 0.073 Uiso 0.519(12) 1 calc R U P A 1
C22 C 0.4542(11) -0.2247(9) 0.7467(14) 0.079(3) Uani 0.519(12) 1 d D U P A 1
H22A H 0.411191 -0.193161 0.811835 0.118 Uiso 0.519(12) 1 calc R U P A 1
H22B H 0.505473 -0.284631 0.762334 0.118 Uiso 0.519(12) 1 calc R U P A 1
H22C H 0.397105 -0.261838 0.669434 0.118 Uiso 0.519(12) 1 calc R U P A 1
O2 O 0.3798(13) 0.1929(13) 0.8276(9) 0.063(3) Uani 0.519(12) 1 d D U P A 1
O3 O 0.3121(8) 0.0461(6) 0.5819(8) 0.062(2) Uani 0.519(12) 1 d D U P A 1
C18A C 0.406(2) 0.0728(18) 0.8459(15) 0.079(6) Uani 0.481(12) 1 d D U P A 2
H18C H 0.350020 0.023970 0.866012 0.094 Uiso 0.481(12) 1 calc R U P A 2
H18D H 0.472241 0.108537 0.917682 0.094 Uiso 0.481(12) 1 calc R U P A 2
C19A C 0.3224(8) -0.0448(8) 0.6679(12) 0.056(3) Uani 0.481(12) 1 d D U P A 2
H19C H 0.318275 -0.116417 0.593945 0.067 Uiso 0.481(12) 1 calc R U P A 2
H19D H 0.275926 -0.065644 0.719515 0.067 Uiso 0.481(12) 1 calc R U P A 2
C21A C 0.5013(11) -0.1020(8) 0.8008(10) 0.056(3) Uani 0.481(12) 1 d D U P A 2
H21C H 0.580257 -0.072864 0.855825 0.067 Uiso 0.481(12) 1 calc R U P A 2
H21D H 0.444631 -0.114016 0.848081 0.067 Uiso 0.481(12) 1 calc R U P A 2
C22A C 0.5090(14) -0.2208(10) 0.6966(12) 0.082(4) Uani 0.481(12) 1 d D U P A 2
H22D H 0.548594 -0.203864 0.639007 0.122 Uiso 0.481(12) 1 calc R U P A 2
H22E H 0.428704 -0.258786 0.655232 0.122 Uiso 0.481(12) 1 calc R U P A 2
H22F H 0.554626 -0.274736 0.729802 0.122 Uiso 0.481(12) 1 calc R U P A 2
O2A O 0.3446(14) 0.1699(16) 0.8145(12) 0.074(4) Uani 0.481(12) 1 d D U P A 2
O3A O 0.2703(8) 0.0542(7) 0.6343(11) 0.067(3) Uani 0.481(12) 1 d D U P A 2
C24 C 0.1121(5) 0.1822(5) 0.9377(5) 0.0794(14) Uani 1 1 d . . . B 1
H24A H 0.129300 0.175806 0.859766 0.119 Uiso 1 1 calc R U . B 1
H24B H 0.030898 0.204822 0.940017 0.119 Uiso 1 1 calc R U . B 1
H24C H 0.119848 0.104818 0.948040 0.119 Uiso 1 1 calc R U . B 1
C23 C 0.1939(7) 0.2711(6) 1.0328(6) 0.0971(19) Uani 1 1 d . . . B 1
N5 N 0.2619(8) 0.3411(7) 1.1101(8) 0.176(4) Uani 1 1 d . . . B 1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.3257 6.8362 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ru Ru 0.0552 3.2960 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 C6 114.8(3) . . ?
C2 C1 Ru1 125.3(3) . . ?
C6 C1 Ru1 119.8(3) . . ?
C1 C2 H2 118.5 . . ?
C3 C2 C1 123.0(4) . . ?
C3 C2 H2 118.5 . . ?
C2 C3 H3 119.9 . . ?
C4 C3 C2 120.3(4) . . ?
C4 C3 H3 119.9 . . ?
C3 C4 H4 120.8 . . ?
C5 C4 C3 118.4(4) . . ?
C5 C4 H4 120.8 . . ?
C4 C5 H5 119.4 . . ?
C4 C5 C6 121.1(4) . . ?
C6 C5 H5 119.4 . . ?
C1 C6 H6 118.8 . . ?
C5 C6 C1 122.4(4) . . ?
C5 C6 H6 118.8 . . ?
N1 C7 C8 179.1(5) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N2 C9 C10 178.5(4) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N3 C11 C12 178.7(5) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N4 C13 C14 179.4(5) . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
H17A C17 H17B 108.0 . . ?
C20 C17 H17A 109.4 . . ?
C20 C17 H17B 109.4 . . ?
O1 C17 H17A 109.4 . . ?
O1 C17 H17B 109.4 . . ?
O1 C17 C20 111.4(4) . . ?
C17 C20 C18 101.7(10) . . ?
C17 C20 C19 96.1(6) . . ?
C17 C20 C21 100.1(5) . . ?
C17 C20 C18A 113.1(11) . . ?
C17 C20 C19A 123.0(6) . . ?
C17 C20 C21A 120.5(6) . . ?
C18 C20 C19 125.8(10) . . ?
C18 C20 C21 122.3(8) . . ?
C21 C20 C19 103.7(6) . . ?
C18A C20 C19A 86.4(12) . . ?
C18A C20 C21A 94.5(8) . . ?
C19A C20 C21A 109.6(6) . . ?
C7 N1 Ru1 175.0(3) . . ?
C9 N2 Ru1 173.2(3) . . ?
C11 N3 Ru1 175.7(3) . . ?
C13 N4 Ru1 174.9(3) . . ?
C17 O1 P1 116.2(3) . . ?
O1 P1 Ru1 115.69(11) . . ?
O1 P1 O3 90.0(4) . . ?
O2 P1 O1 94.1(5) . . ?
O2 P1 Ru1 116.5(5) . . ?
O2 P1 O3 118.2(7) . . ?
O3 P1 Ru1 116.5(3) . . ?
O2A P1 O1 106.3(6) . . ?
O2A P1 Ru1 117.8(6) . . ?
O2A P1 O3A 81.8(9) . . ?
O3A P1 O1 113.0(4) . . ?
O3A P1 Ru1 117.3(3) . . ?
C1 Ru1 N2 86.56(13) . . ?
C1 Ru1 N4 175.36(13) . . ?
C1 Ru1 P1 92.60(10) . . ?
N1 Ru1 C1 89.00(13) . . ?
N1 Ru1 N2 87.01(12) . . ?
N1 Ru1 N4 88.95(13) . . ?
N1 Ru1 P1 91.71(9) . . ?
N2 Ru1 N4 89.18(12) . . ?
N2 Ru1 P1 178.48(9) . . ?
N3 Ru1 C1 88.95(13) . . ?
N3 Ru1 N1 176.27(12) . . ?
N3 Ru1 N2 89.76(12) . . ?
N3 Ru1 N4 92.87(12) . . ?
N3 Ru1 P1 91.49(9) . . ?
N4 Ru1 P1 91.62(9) . . ?
C20 C18 H18A 109.5 . . ?
C20 C18 H18B 109.5 . . ?
H18A C18 H18B 108.1 . . ?
O2 C18 C20 110.7(10) . . ?
O2 C18 H18A 109.5 . . ?
O2 C18 H18B 109.5 . . ?
C20 C19 H19A 110.2 . . ?
C20 C19 H19B 110.2 . . ?
H19A C19 H19B 108.5 . . ?
O3 C19 C20 107.7(6) . . ?
O3 C19 H19A 110.2 . . ?
O3 C19 H19B 110.2 . . ?
C20 C21 H21A 108.9 . . ?
C20 C21 H21B 108.9 . . ?
H21A C21 H21B 107.8 . . ?
C22 C21 C20 113.2(8) . . ?
C22 C21 H21A 108.9 . . ?
C22 C21 H21B 108.9 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C18 O2 P1 116.3(10) . . ?
C19 O3 P1 117.9(6) . . ?
C20 C18A H18C 109.7 . . ?
C20 C18A H18D 109.7 . . ?
H18C C18A H18D 108.2 . . ?
O2A C18A C20 109.8(12) . . ?
O2A C18A H18C 109.7 . . ?
O2A C18A H18D 109.7 . . ?
C20 C19A H19C 109.5 . . ?
C20 C19A H19D 109.5 . . ?
H19C C19A H19D 108.1 . . ?
O3A C19A C20 110.6(6) . . ?
O3A C19A H19C 109.5 . . ?
O3A C19A H19D 109.5 . . ?
C20 C21A H21C 110.4 . . ?
C20 C21A H21D 110.4 . . ?
H21C C21A H21D 108.6 . . ?
C22A C21A C20 106.4(8) . . ?
C22A C21A H21C 110.4 . . ?
C22A C21A H21D 110.4 . . ?
C21A C22A H22D 109.5 . . ?
C21A C22A H22E 109.5 . . ?
C21A C22A H22F 109.5 . . ?
H22D C22A H22E 109.5 . . ?
H22D C22A H22F 109.5 . . ?
H22E C22A H22F 109.5 . . ?
C18A O2A P1 117.5(12) . . ?
C19A O3A P1 116.2(6) . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
N5 C23 C24 178.5(9) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.398(5) . ?
C1 C6 1.407(5) . ?
C1 Ru1 2.075(4) . ?
C2 H2 0.9300 . ?
C2 C3 1.393(6) . ?
C3 H3 0.9300 . ?
C3 C4 1.378(7) . ?
C4 H4 0.9300 . ?
C4 C5 1.378(6) . ?
C5 H5 0.9300 . ?
C5 C6 1.383(6) . ?
C6 H6 0.9300 . ?
C7 C8 1.454(6) . ?
C7 N1 1.131(5) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 C10 1.441(5) . ?
C9 N2 1.133(5) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 C12 1.467(6) . ?
C11 N3 1.128(5) . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 C14 1.454(6) . ?
C13 N4 1.128(5) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C17 C20 1.499(7) . ?
C17 O1 1.449(5) . ?
C20 C18 1.522(14) . ?
C20 C19 1.611(9) . ?
C20 C21 1.601(9) . ?
C20 C18A 1.510(14) . ?
C20 C19A 1.549(9) . ?
C20 C21A 1.575(9) . ?
N1 Ru1 2.027(3) . ?
N2 Ru1 2.128(3) . ?
N3 Ru1 2.022(3) . ?
N4 Ru1 2.162(3) . ?
O1 P1 1.605(3) . ?
P1 Ru1 2.1958(9) . ?
P1 O2 1.580(9) . ?
P1 O3 1.630(6) . ?
P1 O2A 1.575(11) . ?
P1 O3A 1.602(7) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C18 O2 1.464(11) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C19 O3 1.449(10) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C21 C22 1.495(12) . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C18A H18C 0.9700 . ?
C18A H18D 0.9700 . ?
C18A O2A 1.461(12) . ?
C19A H19C 0.9700 . ?
C19A H19D 0.9700 . ?
C19A O3A 1.449(10) . ?
C21A H21C 0.9700 . ?
C21A H21D 0.9700 . ?
C21A C22A 1.519(12) . ?
C22A H22D 0.9600 . ?
C22A H22E 0.9600 . ?
C22A H22F 0.9600 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C24 C23 1.395(9) . ?
C23 N5 1.131(9) . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 C3 C4 -1.2(7) . . . . ?
C2 C1 C6 C5 -0.1(6) . . . . ?
C2 C3 C4 C5 1.4(7) . . . . ?
C3 C4 C5 C6 -0.9(7) . . . . ?
C4 C5 C6 C1 0.3(7) . . . . ?
C6 C1 C2 C3 0.6(6) . . . . ?
C17 C20 C18 O2 61.8(16) . . . . ?
C17 C20 C19 O3 -64.1(8) . . . . ?
C17 C20 C21 C22 -166.2(11) . . . . ?
C17 C20 C18A O2A 59.1(19) . . . . ?
C17 C20 C19A O3A -42.2(12) . . . . ?
C17 C20 C21A C22A -82.7(11) . . . . ?
C17 O1 P1 Ru1 -179.0(3) . . . . ?
C17 O1 P1 O2 59.0(6) . . . . ?
C17 O1 P1 O3 -59.3(4) . . . . ?
C17 O1 P1 O2A 48.1(8) . . . . ?
C17 O1 P1 O3A -39.8(6) . . . . ?
C20 C17 O1 P1 -2.2(5) . . . . ?
C20 C18 O2 P1 1(2) . . . . ?
C20 C19 O3 P1 -2.8(11) . . . . ?
C20 C18A O2A P1 -6(2) . . . . ?
C20 C19A O3A P1 -6.5(12) . . . . ?
O1 C17 C20 C18 -61.0(8) . . . . ?
O1 C17 C20 C19 67.5(6) . . . . ?
O1 C17 C20 C21 172.7(6) . . . . ?
O1 C17 C20 C18A -54.3(10) . . . . ?
O1 C17 C20 C19A 47.0(8) . . . . ?
O1 C17 C20 C21A -164.9(6) . . . . ?
O1 P1 O2 C18 -57.8(14) . . . . ?
O1 P1 O3 C19 61.3(8) . . . . ?
O1 P1 O2A C18A -43.1(16) . . . . ?
O1 P1 O3A C19A 44.4(10) . . . . ?
Ru1 C1 C2 C3 -174.6(3) . . . . ?
Ru1 C1 C6 C5 175.4(3) . . . . ?
Ru1 P1 O2 C18 -179.2(12) . . . . ?
Ru1 P1 O3 C19 -179.7(6) . . . . ?
Ru1 P1 O2A C18A -174.8(14) . . . . ?
Ru1 P1 O3A C19A -177.0(7) . . . . ?
C18 C20 C19 O3 45.1(14) . . . . ?
C18 C20 C21 C22 82.8(16) . . . . ?
C19 C20 C18 O2 -45(2) . . . . ?
C19 C20 C21 C22 -67.4(14) . . . . ?
C21 C20 C18 O2 171.9(11) . . . . ?
C21 C20 C19 O3 -166.1(7) . . . . ?
O2 P1 O3 C19 -33.3(11) . . . . ?
O3 P1 O2 C18 34.4(16) . . . . ?
C18A C20 C19A O3A 73.1(11) . . . . ?
C18A C20 C21A C22A 157.0(14) . . . . ?
C19A C20 C18A O2A -65.5(17) . . . . ?
C19A C20 C21A C22A 69.2(14) . . . . ?
C21A C20 C18A O2A -174.9(16) . . . . ?
C21A C20 C19A O3A 166.7(9) . . . . ?
O2A P1 O3A C19A -59.9(10) . . . . ?
O3A P1 O2A C18A 68.6(16) . . . . ?
