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_1575005
_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         'C17 H15 N3 O'
_chemical_formula_sum            'C17 H15 N3 O'
_chemical_formula_weight         277.32
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-05-12
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2024-02-02 deposited with the CCDC.	2025-03-04 downloaded from the CCDC.
;
_cell_angle_alpha                116.535(4)
_cell_angle_beta                 108.263(5)
_cell_angle_gamma                100.865(4)
_cell_formula_units_Z            2
_cell_length_a                   9.4605(5)
_cell_length_b                   9.5615(4)
_cell_length_c                   9.9418(4)
_cell_measurement_reflns_used    3050
_cell_measurement_temperature    298
_cell_measurement_theta_max      72.1460
_cell_measurement_theta_min      5.3630
_cell_volume                     704.62(8)
_computing_cell_refinement       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_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      298
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.941
_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    -25.00  26.00   0.50    0.05    --   47.45 -19.00 -90.00  102
  2  \w     28.00  54.00   0.50    0.10    --   98.15 -57.00 -30.00   52
  3  \w     26.00  51.00   0.50    0.10    --   98.15 -57.00  30.00   50
  4  \w     35.00 105.00   0.50    0.10    --   98.15 -77.00  60.00  140
  5  \w     76.00 114.00   0.50    0.10    --   98.15-125.00  60.00   76
  6  \w     70.00 106.00   0.50    0.10    --   98.15 -99.00 -30.00   72
  7  \w     31.00 112.00   0.50    0.10    --   98.15-125.00 -30.00  162
  8  \w     33.00  73.00   0.50    0.10    --   98.15-125.00  60.00   80
  9  \w     27.00  65.00   0.50    0.10    --   98.15 -99.00 -30.00   76
 10  \w     89.00 117.00   0.50    0.10    --   98.15-125.00-180.00   56
 11  \w     70.00 105.00   0.50    0.10    --   98.15 -77.00-180.00   70
 12  \w     32.00  76.00   0.50    0.10    --   98.15-125.00-180.00   88
 13  \w     27.00  66.00   0.50    0.10    --   98.15 -77.00-180.00   78
 14  \w     88.00 162.00   0.50    0.10    --   98.15  37.00-150.00  148
 15  \w    102.00 168.00   0.50    0.10    --   98.15  91.00 -68.00  132
 16  \w     83.00 167.00   0.50    0.10    --   98.15  57.00-120.00  168
 17  \w     92.00 146.00   0.50    0.10    --   98.15 125.00 120.00  108
 18  \w     16.00  42.00   0.50    0.05    --   47.45 -37.00 150.00   52
 19  \w      2.00  43.00   0.50    0.05    --   47.45 -91.00 177.00   82
 20  \w     52.00  77.00   0.50    0.10    --   98.15 -91.00 177.00   50
 21  \w    -24.00   8.00   0.50    0.05    --   47.45 -37.00 150.00   64
 22  \w     -5.00  21.00   0.50    0.05    --  -47.45  91.00 -68.00   52
 23  \w      2.00  27.00   0.50    0.05    --  -47.45  19.00-150.00   50
 24  \w    -41.00 -16.00   0.50    0.10    --  -86.25  37.00-120.00   50
 25  \w    -63.00 -38.00   0.50    0.10    --  -86.25  57.00 -90.00   50
 26  \w    -75.00  -8.00   0.50    0.05    --  -47.45  91.00 -68.00  134
 27  \w    -42.00 -17.00   0.50    0.10    --  -86.25  37.00   0.00   50
 28  \w    -39.00 -14.00   0.50    0.10    --  -86.25  37.00  60.00   50
 29  \w    -39.00 -14.00   0.50    0.10    --  -86.25  37.00  90.00   50
 30  \w    -38.00 -13.00   0.50    0.10    --  -86.25  37.00 150.00   50
 31  \w    -41.00 -16.00   0.50    0.10    --  -86.25  37.00 120.00   50
 32  \w   -123.00 -98.00   0.50    0.10    --  -86.25 -91.00 177.00   50
 33  \w   -159.00 -83.00   0.50    0.10    --  -86.25 -99.00 150.00  152
 34  \w   -111.00 -70.00   0.50    0.05    --  -47.45-125.00  30.00   82
 35  \w   -110.00 -83.00   0.50    0.05    --  -47.45-125.00 -60.00   54
 36  \w   -100.00 -70.00   0.50    0.05    --  -47.45-125.00-120.00   60
;
_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      -0.0960577000
_diffrn_orient_matrix_UB_12      -0.0257363000
_diffrn_orient_matrix_UB_13      -0.1718893000
_diffrn_orient_matrix_UB_21      -0.1405493000
_diffrn_orient_matrix_UB_22      -0.1484202000
_diffrn_orient_matrix_UB_23      -0.0415357000
_diffrn_orient_matrix_UB_31      -0.0747837000
_diffrn_orient_matrix_UB_32      0.1242701000
_diffrn_orient_matrix_UB_33      0.0803264000
_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  0.0620
_diffrn_reflns_av_unetI/netI     0.0653
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.941
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            7133
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.941
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.893
_diffrn_reflns_theta_min         5.339
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.670
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58299
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.68a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic light black'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.307
_exptl_crystal_description       trapezoid
_exptl_crystal_F_000             292
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.121
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.254
_refine_diff_density_min         -0.369
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     200
_refine_ls_number_reflns         2643
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0770
_refine_ls_R_factor_gt           0.0644
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1387P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1808
_refine_ls_wR_factor_ref         0.1971
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2097
_reflns_number_total             2643
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc02360a2.cif
_cod_data_source_block           exp_1978
_cod_original_cell_volume        704.62(6)
_cod_database_code               1575005
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.924
_shelx_estimated_absorpt_t_min   0.918
_reflns_odcompleteness_completeness 99.09
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     64.99
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N2(H2), C1(H1), C2(H2A), C17(H17), C16(H16), C15(H15), C3(H3)
2.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C11(H11A,H11B,H11C)
;
_shelx_res_checksum              27413
_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 2.573
_oxdiff_exptl_absorpt_empirical_full_min 0.362