Understanding the factors governing the ammonia oxidation reaction by a mononuclear ruthenium complex
Chen, Guo; Ding, Xiao-Lv; He, Piao; Cheng, Tao; Chen, Yang; Lin, Jian; Zhang, Xi; Zhao, Shan; Qiao, Na; Yi, Xiao-Yi; Chemical Science 16 (2025) 7573–7578; doi:10.1039/D4SC02360A

data_1575004
_publ_section_title
;
 Understanding the factors governing the ammonia oxidation reaction by a
 mononuclear ruthenium complex
;
_journal_issue                   17
_journal_name_full               'Chemical Science'
_journal_page_first              7573
_journal_page_last               7578
_journal_paper_doi               10.1039/D4SC02360A
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety         'C27 H22 Cl N5 O Ru'
_chemical_formula_sum            'C27 H22 Cl N5 O Ru'
_chemical_formula_weight         569.01
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-05-29
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2024-01-30 deposited with the CCDC.	2025-03-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.4383(4)
_cell_length_b                   15.9847(7)
_cell_length_c                   18.7749(8)
_cell_measurement_reflns_used    18840
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      32.7070
_cell_measurement_theta_min      2.3040
_cell_volume                     2832.5(2)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.886
_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  47.00   0.50    3.99    --  -14.57  26.00 -75.00  152
  2  \w      2.00  48.00   0.50    3.99    --  -14.57  37.00-180.00   92
  3  \w     40.00  71.00   0.50    3.99    --   13.79 178.00 -90.00   62
  4  \w    -16.00  20.00   0.50    3.99    --  -14.57 -99.00  60.00   72
  5  \w     34.00  62.00   0.50    3.99    --   13.79-155.00 113.00   56
  6  \w    -22.00  12.00   0.50    3.99    --  -14.57 -99.00 120.00   68
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0229982000
_diffrn_orient_matrix_UB_12      0.0293364000
_diffrn_orient_matrix_UB_13      -0.0259175000
_diffrn_orient_matrix_UB_21      0.0098539000
_diffrn_orient_matrix_UB_22      0.0303367000
_diffrn_orient_matrix_UB_23      0.0270864000
_diffrn_orient_matrix_UB_31      0.0708848000
_diffrn_orient_matrix_UB_32      -0.0137231000
_diffrn_orient_matrix_UB_33      0.0045909000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0536
_diffrn_reflns_av_unetI/netI     0.0706
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.886
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            23862
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.847
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.709
_diffrn_reflns_theta_min         2.169
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.674
_exptl_absorpt_correction_T_max  0.936
_exptl_absorpt_correction_T_min  0.689
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'clear reddish red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.334
_exptl_crystal_description       prism
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.954
_refine_diff_density_min         -1.266
_refine_diff_density_rms         0.094
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.49(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.922
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     318
_refine_ls_number_reflns         9572
_refine_ls_number_restraints     63
_refine_ls_restrained_S_all      0.922
_refine_ls_R_factor_all          0.0886
_refine_ls_R_factor_gt           0.0541
_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^)+(0.0878P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1343
_refine_ls_wR_factor_ref         0.1502
_reflns_Friedel_coverage         0.733
_reflns_Friedel_fraction_full    0.983
_reflns_Friedel_fraction_max     0.799
_reflns_number_gt                6009
_reflns_number_total             9572
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc02360a2.cif
_cod_data_source_block           exp_526
_cod_database_code               1575004
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHONIrCl
_shelx_estimated_absorpt_t_max   0.936
_shelx_estimated_absorpt_t_min   0.688
_reflns_odcompleteness_completeness 99.75
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.51(5)
 0.49(5)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Rigid body (RIGU) restrains
 C11, C10, O1, C9, C7, C8, C6, C12, N2
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
4.a Riding coordinates:
 C8(H8A,H8B,H8C)
4.b Aromatic/amide H refined with riding coordinates:
 C27(H27), C18(H18), C26(H26), C21(H21), C24(H24), C19(H19), C25(H25), C2(H2),
 C20(H20), C1(H1), C17(H17), C15(H15), C3(H3), C16(H16), C14(H14), C4(H4)
4.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              36347
_shelx_fab_checksum              79390
_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 2.655
_oxdiff_exptl_absorpt_empirical_full_min 0.463