Structure and reactivity of a seven-coordinate ruthenium acylperoxo complex.
Wang, Rui; Pan, Yunling; Feng, Sushan; Liang, Chenyi; Xie, Jianhui; Lau, Tai-Chu; Liu, Yingying; Chemical communications (Cambridge, England) 60 (2024) 312–315; doi:10.1039/d3cc04751b

data_7132425
_publ_section_title
;
 Structure and reactivity of a seven-coordinate ruthenium acylperoxo
 complex.
;
_journal_issue                   3
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              312
_journal_page_last               315
_journal_paper_doi               10.1039/d3cc04751b
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C55 H44 Cl N4 O5 Ru, F6 P, 0.5(C3 H6 O)'
_chemical_formula_sum            'C56.5 H47 Cl F6 N4 O5.5 P Ru'
_chemical_formula_weight         1151.47
_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
_audit_creation_date             2023-05-11
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-08-29 deposited with the CCDC.	2023-12-05 downloaded from the CCDC.
;
_cell_angle_alpha                86.1900(10)
_cell_angle_beta                 81.9140(10)
_cell_angle_gamma                67.7720(10)
_cell_formula_units_Z            4
_cell_length_a                   13.75640(10)
_cell_length_b                   17.46850(10)
_cell_length_c                   25.0576(2)
_cell_measurement_reflns_used    109579
_cell_measurement_temperature    105(8)
_cell_measurement_theta_max      79.1820
_cell_measurement_theta_min      4.1140
_cell_volume                     5517.96(8)
_computing_cell_refinement       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.41.123a (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 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      105.15
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.983
_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    -32.00  20.00   0.50    0.50    --    0.00 -82.00-150.00  104
  2  \w    -86.00  29.00   0.50    0.50    --    0.00 -22.00 143.69  230
  3  \w    -43.00 -13.00   0.50    0.50    --    0.00 -77.00 -30.00   60
  4  \w    -50.00  32.00   0.50    0.50    --    0.00 -19.00 -30.00  164
  5  \w    -24.00  10.00   0.50    0.50    --    0.00  57.00   0.00   68
  6  \w    -87.00 -55.00   0.50    0.50    --    0.00 -37.00-150.00   64
  7  \w    -88.00 -46.00   0.50    0.50    --    0.00 -37.00 -60.00   84
  8  \w    -58.00 -18.00   0.50    0.50    --    0.00 -37.00  60.00   80
  9  \w    -44.00  22.00   0.50    0.50    --    0.00 -37.00-150.00  132
 10  \w    -25.00  10.00   0.50    0.50    --    0.00  57.00-120.00   70
 11  \w     -4.00  30.00   0.50    0.50    --    0.00 -77.00 -30.00   68
 12  \w    -32.00  22.00   0.50    0.50    --    0.00 -82.00-120.00  108
 13  \w    -84.00  -6.00   0.50    0.50    --    0.00 -19.00  60.00  156
 14  \w      5.00  32.00   0.50    0.50    --    0.00 -19.00  60.00   54
 15  \w    -10.00  23.00   0.50    0.50    --    0.00 -37.00  60.00   66
 16  \w    -23.00  23.00   0.50    0.50    --    0.00 -37.00 -60.00   92
 17  \w     31.00  64.00   0.50    0.50    --    0.00  57.00-120.00   66
 18  \w     25.00  82.00   0.50    0.50    --    0.00  57.00   0.00  114
 19  \w     76.00 103.00   0.50    0.50    --  105.20  70.00   0.51   54
 20  \w     82.00 193.00   0.50    0.50    --  105.20  34.00   1.72  222
 21  \w     81.00 194.00   0.50    0.50    --  105.20  30.00-113.42  226
 22  \w    129.00 191.00   0.50    0.50    --  105.20  33.00 130.89  124
 23  \w     76.00 103.00   0.50    0.50    --  105.20  72.00 177.83   54
 24  \w    155.00 182.00   0.50    0.50    --  105.20  76.00 -57.02   54
 25  \w     76.00 102.00   0.50    0.50    --  105.20  70.00 -23.45   52
 26  \w     79.00 106.00   0.50    0.50    --  105.20  62.00 124.74   54
 27  \w    170.00 195.00   0.50    0.50    --  105.20  62.00 124.74   50
 28  \w     79.00 107.00   0.50    0.50    --  105.20  61.00  83.99   56
 29  \w     78.00 104.00   0.50    0.50    --  105.20  64.00  43.25   52
 30  \w    115.00 142.00   0.50    0.50    --  105.20  64.00  43.25   54
 31  \w     83.00 114.00   0.50    0.50    --  105.20  33.00 130.89   62
 32  \w    153.00 178.00   0.50    0.50    --  105.20  28.00 -20.83   50
 33  \w    116.00 153.00   0.50    0.50    --  105.20  42.00  45.11   74
 34  \w     74.00 101.00   0.50    0.50    --  105.20  76.00 -57.02   54
 35  \w    138.00 186.00   0.50    0.50    --  105.20  75.00   1.19   96
 36  \w     81.00 195.00   0.50    0.50    --  105.20  53.00  46.50  228
 37  \w     74.00 100.00   0.50    0.50    --  105.20  75.00   1.19   52
 38  \w     75.00 194.00   0.50    0.50    --  105.20  73.00-120.48  238
 39  \w     78.00 104.00   0.50    0.50    --  105.20  65.00-164.10   52
 40  \w    106.00 193.00   0.50    0.50    --  105.20  68.00 106.35  174
 41  \w     75.00 101.00   0.50    0.50    --  105.20  74.00 -78.16   52
 42  \w     74.00 100.00   0.50    0.50    --  105.20  76.00-152.17   52
 43  \w     83.00 114.00   0.50    0.50    --  105.20  52.00 150.15   62
 44  \w     74.00 100.00   0.50    0.50    --  105.20  75.00  13.81   52
 45  \w     78.00 104.00   0.50    0.50    --  105.20  64.00 -24.19   52
 46  \w     76.00 102.00   0.50    0.50    --  105.20  71.00  87.57   52
 47  \w     75.00 102.00   0.50    0.50    --  105.20  73.00-164.24   54
 48  \w     74.00 101.00   0.50    0.50    --  105.20  76.00 -35.10   54
 49  \w    125.00 193.00   0.50    0.50    --  105.20  76.00 -35.10  136
 50  \w     76.00 103.00   0.50    0.50    --  105.20  72.00  40.77   54
 51  \w     75.00 102.00   0.50    0.50    --  105.20  74.00 115.65   54
 52  \w     74.00 100.00   0.50    0.50    --  105.20  76.00 -97.07   52
 53  \w    112.00 194.00   0.50    0.50    --  105.20  76.00 -97.07  164
 54  \w     77.00 103.00   0.50    0.50    --  105.20  68.00 -60.66   52
 55  \w     75.00 101.00   0.50    0.50    --  105.20  73.00-131.64   52
 56  \w     74.00 100.00   0.50    0.50    --  105.20  76.00-159.59   52
 57  \w     76.00 102.00   0.50    0.50    --  105.20  71.00  65.71   52
 58  \w    135.00 194.00   0.50    0.50    --  105.20  71.00  65.71  118
 59  \w     74.00 100.00   0.50    0.50    --  105.20  76.00 164.15   52
 60  \w    113.00 195.00   0.50    0.50    --  105.20  76.00 164.15  164
 61  \w     75.00 101.00   0.50    0.50    --  105.20  74.00  34.72   52
 62  \w     18.00 138.00   0.50    0.50    --  105.20 -82.00 -90.00  240
 63  \w     79.00 151.00   0.50    0.50    --  105.20  59.00  62.18  144
 64  \w    118.00 147.00   0.50    0.50    --  105.20  28.00 -20.83   58
 65  \w    127.00 190.00   0.50    0.50    --  105.20  67.00 -81.64  126
 66  \w     78.00 106.00   0.50    0.50    --  105.20  67.00 -81.64   56
 67  \w     77.00 103.00   0.50    0.50    --  105.20  68.00 106.35   52
 68  \w     77.00 103.00   0.50    0.50    --  105.20  69.00  28.58   52
 69  \w    138.00 165.00   0.50    0.50    --  105.20  61.00  90.00   54
 70  \w     79.00 106.00   0.50    0.50    --  105.20  61.00  90.00   54
 71  \w     78.00 106.00   0.50    0.50    --  105.20  63.00 106.92   56
 72  \w    166.00 193.00   0.50    0.50    --  105.20  54.00 163.94   54
 73  \w     32.00  57.00   0.50    0.50    --  105.20 -82.00 -30.00   50
 74  \w     72.00 137.00   0.50    0.50    --  105.20 -82.00 -30.00  130
 75  \w    153.00 185.00   0.50    0.50    --  105.20  49.00  12.38   64
 76  \w     78.00 104.00   0.50    0.50    --  105.20  64.00 160.64   52
 77  \w     79.00 105.00   0.50    0.50    --  105.20  61.00 150.00   52
 78  \w     77.00 103.00   0.50    0.50    --  105.20  69.00 158.63   52
 79  \w     79.00 105.00   0.50    0.50    --  105.20  61.00 -90.00   52
 80  \w     82.00 110.00   0.50    0.50    --  105.20  45.00 -60.00   56
 81  \w    170.00 195.00   0.50    0.50    --  105.20  45.00 -60.00   50
 82  \w     83.00 114.00   0.50    0.50    --  105.20  45.00-169.13   62
 83  \w     55.00 139.00   0.50    0.50    --  105.20 -82.00  30.00  168
 84  \w    139.00 164.00   0.50    0.50    --  105.20  53.00 -36.18   50
 85  \w     81.00 140.00   0.50    0.50    --  105.20  54.00 163.94  118
 86  \w     18.00  51.00   0.50    0.50    --  105.20 -82.00  30.00   66
 87  \w     81.00 107.00   0.50    0.50    --  105.20  53.00 -36.18   52
 88  \w     80.00 106.00   0.50    0.50    --  105.20  58.00 -95.10   52
 89  \w     79.00 105.00   0.50    0.50    --  105.20  61.00   0.00   52
 90  \w     79.00 106.00   0.50    0.50    --  105.20  61.00 120.00   54
 91  \w     77.00 129.00   0.50    0.50    --  105.20  67.00-131.96  104
 92  \w    146.00 192.00   0.50    0.50    --  105.20  67.00-131.96   92
 93  \w     82.00 109.00   0.50    0.50    --  105.20  45.00-150.00   54
 94  \w    116.00 154.00   0.50    0.50    --  105.20  45.00-150.00   76
 95  \w    161.00 194.00   0.50    0.50    --  105.20  45.00-150.00   66
 96  \w     81.00 108.00   0.50    0.50    --  105.20  52.00 -15.66   54
 97  \w     83.00 110.00   0.50    0.50    --  105.20  52.00  -0.00   54
 98  \w     80.00 107.00   0.50    0.50    --  105.20  77.00 120.00   54
 99  \w    141.00 195.00   0.50    0.50    --  105.20  77.00 120.00  108
100  \w     53.00 137.00   0.50    0.50    --  105.20 -82.00-180.00  168
101  \w    167.00 192.00   0.50    0.50    --  105.20  64.00  43.25   50
102  \w     82.00 109.00   0.50    0.50    --  105.20  45.00  30.00   54
103  \w     19.00  46.00   0.50    0.50    --  105.20 -82.00-150.00   54
104  \w     62.00  92.00   0.50    0.50    --  105.20 -82.00-150.00   60
105  \w    102.00 137.00   0.50    0.50    --  105.20 -82.00-150.00   70
106  \w     54.00 115.00   0.50    0.50    --  105.20 -82.00 120.00  122
107  \w     76.00 102.00   0.50    0.50    --  105.20  70.00  58.29   52
108  \w     82.00 112.00   0.50    0.50    --  105.20  49.00  12.38   60
109  \w     80.00 107.00   0.50    0.50    --  105.20  28.00 -20.83   54
110  \w     24.00  89.00   0.50    0.50    --  105.20 -82.00  60.00  130
111  \w    103.00 135.00   0.50    0.50    --  105.20 -82.00  60.00   64
112  \w     82.00 108.00   0.50    0.50    --  105.20  42.00  45.11   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0569
_diffrn_reflns_av_unetI/netI     0.0279
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            192909
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.497
_diffrn_reflns_theta_min         3.748
_exptl_absorpt_coefficient_mu    3.630
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.105
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.123a (Rigaku Oxford Diffraction, 2022)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark brown'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.386
_exptl_crystal_description       block
_exptl_crystal_F_000             2352
_exptl_crystal_size_max          0.66
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.915
_refine_diff_density_min         -1.908
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1357
_refine_ls_number_reflns         23561
_refine_ls_number_restraints     297
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0699
_refine_ls_R_factor_gt           0.0670
_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^)+(0.1106P)^2^+13.1521P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1859
_refine_ls_wR_factor_ref         0.1888
_reflns_Friedel_coverage         0.000
_reflns_number_gt                21874
_reflns_number_total             23561
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc04751b2.cif
_cod_data_source_block           220721-ru1
_cod_depositor_comments          'Adding full bibliography for 7132425.cif.'
_cod_original_formula_sum        'C56.50 H47 Cl F6 N4 O5.50 P Ru'
_cod_database_code               7132425
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.899
_shelx_estimated_absorpt_t_min   0.198
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Cl1B-C52B
 1.74 with sigma of 0.02
 C52B-C53B = C52B-C51B = C50B-C51B
 1.39 with sigma of 0.02
 C53B-C48B = C49B-C50B
 1.4 with sigma of 0.02
 C48B-C49B
 1.36 with sigma of 0.02
 C47B-C48B
 1.49 with sigma of 0.02
 C52B-C48B = C53B-C49B
 2.4 with sigma of 0.04
 Cl1B-C53B
 2.7 with sigma of 0.04
 C48B-C50B
 2.39 with sigma of 0.04
 Cl1B-C51B
 2.71 with sigma of 0.04
 C52B-C50B
 2.38 with sigma of 0.04
 C49B-C51B
 2.43 with sigma of 0.04
 C52B-C53B \\sim C53B-C48B \\sim C48B-C49B \\sim C49B-C50B \\sim C50B-C51B
\\sim C51B-C52B
 with sigma of 0.02
 C52B-C48B \\sim C48B-C50B \\sim C53B-C51B \\sim C53B-C49B \\sim C49B-C51B
\\sim C52B-C50B
 with sigma of 0.02
 Cl1B-C53B \\sim Cl1B-C51B
 with sigma of 0.02
 F1-F2 \\sim F1-F4 \\sim F1-F5 \\sim F1-F6 \\sim F2-F3 \\sim F2-F5 \\sim F2-F6
\\sim F3-F4 \\sim F3-F5 \\sim F3-F6
 \\sim F4-F5 \\sim F4-F6
 with sigma of 0.04
 P2-F7 \\sim P2-F8 \\sim P2-F9 \\sim P2-F10 \\sim P2-F11 \\sim P2-F12
 with sigma of 0.02
 F7-F8 \\sim F7-F10 \\sim F7-F11 \\sim F7-F12 \\sim F8-F9 \\sim F8-F11 \\sim
F8-F12 \\sim F9-F10 \\sim F9-F11
 \\sim F9-F12 \\sim F10-F11 \\sim F10-F12
 with sigma of 0.04
 P1-F1 \\sim P1-F2 \\sim P1-F3 \\sim P1-F4 \\sim P1-F5 \\sim P1-F6
 with sigma of 0.02
3. Restrained planarity
 Cl1B, C48B, C49B, C50B, C51B, C52B, C53B
 with sigma of 0.1
 O4B, O5B, C47B, C48B
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Cl1B \\sim C48B \\sim C49B \\sim C50B \\sim C51B \\sim C52B \\sim C53B: within
2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
5. Rigid body (RIGU) restrains
 Cl1B, C48B, C49B, C50B, C51B, C52B, C53B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C13(H13), C14(H14), C15(H15),
 C16(H16), C17(H17), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C26(H26),
  C27(H27), C28(H28), C29(H29), C30(H30), C32(H32), C33(H33), C34(H34),
 C35(H35), C36(H36), C37(H37), C38(H38), C40(H40), C41(H41), C43(H43), C44(H44),
  C47(H47), C48(H48), C51(H51), C53(H53), C54(H54), C55(H55), C2B(H2B),
 C02O(H02O), C3B(H3B), C03C(H03C), C4B(H4B), C7B(H7B), C8B(H8B), C9B(H9B),
 C13B(H13B), C14B(H14B), C15B(H15B), C16B(H16B), C17B(H17B), C19B(H19B),
 C20B(H20B), C21B(H21B), C22B(H22B), C25B(H25B), C26B(H26B), C27B(H27B),
 C28B(H28B), C29B(H29B), C31B(H31B), C32B(H32B), C33B(H33B), C34B(H34B),
 C35B(H35B), C36B(H36B), C37B(H37B), C39B(H39B), C40B(H40B), C42B(H42D),
 C45B(H45B), C46B(H46D), C49B(H49B), C50B(H50B), C51B(H51B), C53B(H53B)
6.b Idealised Me refined as rotating group:
 C42(H42A,H42B,H42C), C46(H46A,H46B,H46C), C41B(H41A,H41B,H41C), C44B(H44A,
 H44B,H44C), C1S(H1SA,H1SB,H1SC), C3S(H3SA,H3SB,H3SC)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 219 electrons were 
found in a volume of 862\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 
1[C3H6O], 0.75[C3H6O] per Unit Cell 
which account for 224 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              42400
_shelx_hkl_checksum              82383
_shelx_fab_checksum              27173
_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
;