Exploring the photoswitching pathways and efficiency of NO isomerization in ethylenediamine ruthenium nitrosyl complexes.
Mikhailov, Artem A.; Tiognou, Appolinaire Tchoutchoua; Brovko, Anastasiya O.; Kostin, Gennadiy A.; Schaniel, Dominik; Dalton transactions (Cambridge, England : 2003) 54 (2025) 8918–8931; doi:10.1039/d5dt00549c

data_7718671
_publ_section_title
;
 Exploring the photoswitching pathways and efficiency of NO isomerization
 in ethylenediamine ruthenium nitrosyl complexes.
;
_journal_issue                   22
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8918
_journal_page_last               8931
_journal_paper_doi               10.1039/d5dt00549c
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C4 H17 N5 O2 Ru, 2(N O3)'
_chemical_formula_sum            'C4 H17 N7 O8 Ru'
_chemical_formula_weight         392.32
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2025-04-23
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2025-04-23 deposited with the CCDC.	2025-05-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.2856(5)
_cell_length_b                   16.8095(6)
_cell_length_c                   8.8220(4)
_cell_measurement_reflns_used    6168
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      76.0250
_cell_measurement_theta_min      5.2640
_cell_volume                     1376.99(11)
_computing_cell_refinement       'CrysAlisPro 1.171.43.90 (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.43.90 (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.43.90 (Rigaku OD, 2023)'
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.4508
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.957
_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    -67.00  36.00   1.00    6.00    --  -40.63  37.00 150.00  103
  2  \w    -87.00  -6.00   1.00    6.00    --  -40.63 125.00-150.00   81
  3  \w   -117.00 -14.00   1.00    6.00    --  -40.63 -37.00 -30.00  103
  4  \w    -74.00  38.00   1.00    6.00    --  -40.63  77.00  60.00  112
  5  \w   -115.00 -11.00   1.00    6.00    --  -40.63 -57.00  90.00  104
  6  \w   -115.00 -11.00   1.00    6.00    --  -40.63 -57.00-150.00  104
  7  \w   -117.00 -14.00   1.00    6.00    --  -40.63 -37.00 120.00  103
  8  \w    -87.00  -6.00   1.00    6.00    --  -40.63 125.00 150.00   81
  9  \w   -117.00 -14.00   1.00    6.00    --  -40.63 -37.00-120.00  103
 10  \w    -36.00  67.00   1.00    6.00    --   40.63 -37.00 -60.00  103
 11  \w      2.00  29.00   1.00    6.00    --   40.63  90.00-148.32   27
 12  \w      3.00  30.00   1.00    6.00    --   40.63  89.00  67.30   27
 13  \w      4.00  31.00   1.00    6.00    --   40.63  87.00 126.66   27
 14  \w      7.00  42.00   1.00    6.00    --   40.63  78.00 -46.37   35
 15  \w      3.00  30.00   1.00    6.00    --   40.63  89.00  24.79   27
 16  \w     83.00 178.00   1.00    1.00    --  113.00  61.00-120.00   95
 17  \w     83.00 178.00   1.00    1.00    --  113.00  61.00-180.00   95
 18  \w     38.00 109.00   1.00    1.00    --  113.00-111.00 -90.00   71
 19  \w     83.00 178.00   1.00    1.00    --  113.00  61.00 -60.00   95
 20  \w     83.00 178.00   1.00    1.00    --  113.00  61.00 150.00   95
 21  \w     85.00 178.00   1.00    1.00    --  113.00  45.00 -30.00   93
 22  \w     83.00 108.00   1.00    1.00    --  113.00  61.00   0.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0461
_diffrn_reflns_av_unetI/netI     0.0323
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            11078
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.428
_diffrn_reflns_theta_min         5.263
_exptl_absorpt_coefficient_mu    9.735
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.35720
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.90 (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.892
_exptl_crystal_description       block
_exptl_crystal_F_000             792
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.675
_refine_diff_density_min         -0.679
_refine_diff_density_rms         0.095
_refine_ls_extinction_coef       0.00024(9)
_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   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     145
_refine_ls_number_reflns         1431
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_gt           0.0377
_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^)+(0.0573P)^2^+0.8884P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0911
_refine_ls_wR_factor_ref         0.0997
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1186
_reflns_number_total             1431
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00549c2.cif
_cod_data_source_block           rt_auto
_cod_depositor_comments
'Adding full bibliography for 7718667--7718675.cif.'
_cod_database_code               7718671
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.642
_shelx_estimated_absorpt_t_min   0.246
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H) groups
2. Restrained distances
 N2-C2A
 1.44 with sigma of 0.005
 N3-C1A
 1.44 with sigma of 0.005
 C2A-C1A
 1.44 with sigma of 0.005
 O5-N4 = O4-N4 = O3-N4
 1.25 with sigma of 0.01
 O5A-N4 = O3A-N4 = O4A-N4
 1.25 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(O4) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.02
Uanis(C2A) \\sim Ueq, Uanis(C1A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O5A) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.02
Uanis(O3A) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.02
4. Others
 Sof(O4A)=Sof(O3A)=Sof(O5A)=1-FVAR(1)
 Sof(O5)=Sof(O3)=Sof(O4)=FVAR(1)
 Fixed Sof: H2(0.5) C2(0.8) H2C(0.8) H2D(0.8) C1(0.8) H1A(0.8) H1B(0.8)
 C1A(0.2) H1AA(0.2) H1AB(0.2) C2A(0.2) H2AA(0.2) H2AB(0.2)
5.a Rotating group:
 O2(H2)
5.b Secondary CH2 refined with riding coordinates:
 N3(H3A,H3B), N2(H2A,H2B), C2(H2C,H2D), C1(H1A,H1B), C1A(H1AA,H1AB), C2A(H2AA,
 H2AB)
;
_shelx_res_checksum              63794
_shelx_hkl_checksum              15337
_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
;