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_7718669
_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, H2 O, 2(N O3)'
_chemical_formula_sum            'C4 H19 N7 O9 Ru'
_chemical_formula_weight         410.33
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-02-02
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-11-14 deposited with the CCDC.	2025-05-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.997(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.4249(3)
_cell_length_b                   17.5864(5)
_cell_length_c                   9.3788(2)
_cell_measurement_reflns_used    19355
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      32.2470
_cell_measurement_theta_min      2.2680
_cell_volume                     1389.39(7)
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_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_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4508
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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    -42.00  14.00   1.00    7.50    --  -19.66 -77.00-120.00   56
  2  \w    -42.00  14.00   1.00    7.50    --  -19.66 -77.00  90.00   56
  3  \w   -110.00 -61.00   1.00    7.50    --  -19.66-178.00 120.00   49
  4  \w   -108.00 -58.00   1.00    7.50    --  -19.66 178.00 -60.00   50
  5  \w    -68.00 110.00   1.00    7.50    --   20.91   0.00-180.00  178
  6  \w    -25.00 102.00   1.00    7.50    --   20.91  19.00  90.00  127
  7  \w    -53.00  21.00   1.00    7.50    --  -19.66  77.00  30.00   74
  8  \w   -108.00 -58.00   1.00    7.50    --  -19.66 178.00-120.00   50
  9  \w    -96.00   7.00   1.00    7.50    --  -19.66 -37.00 -90.00  103
 10  \w    -15.00  63.00   1.00    7.50    --   20.91 -99.00 120.00   78
 11  \w     -5.00  97.00   1.00    7.50    --   20.91  37.00 -90.00  102
 12  \w    -42.00  14.00   1.00    7.50    --  -19.66 -77.00  30.00   56
 13  \w    -88.00 -36.00   1.00    7.50    --  -19.66 143.00-131.00   52
 14  \w    -96.00   7.00   1.00    7.50    --  -19.66 -37.00-180.00  103
 15  \w    -15.00  63.00   1.00    7.50    --   20.91 -99.00-150.00   78
 16  \w    -42.00  55.00   1.00    7.50    --   20.91 -77.00   0.00   97
 17  \w    -15.00  63.00   1.00    7.50    --   20.91 -99.00  60.00   78
 18  \w     39.00 111.00   1.00    7.50    --   20.91 178.00-150.00   72
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0271689000
_diffrn_orient_matrix_UB_12      0.0377587000
_diffrn_orient_matrix_UB_13      -0.0108127000
_diffrn_orient_matrix_UB_21      0.0775529000
_diffrn_orient_matrix_UB_22      0.0138883000
_diffrn_orient_matrix_UB_23      0.0148994000
_diffrn_orient_matrix_UB_31      0.0182430000
_diffrn_orient_matrix_UB_32      -0.0027650000
_diffrn_orient_matrix_UB_33      -0.0734027000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0941
_diffrn_reflns_av_unetI/netI     0.0319
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            43223
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         2.316
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.188
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  1.00000
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Spherical absorption correction
using equivalent radius and absorption coefficient.
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    1.962
_exptl_crystal_description       block
_exptl_crystal_F_000             832
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_exptl_crystal_size_rad          0.400
_refine_diff_density_max         1.084
_refine_diff_density_min         -0.585
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     194
_refine_ls_number_reflns         2838
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0354
_refine_ls_R_factor_gt           0.0271
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0148P)^2^+3.0030P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0590
_refine_ls_wR_factor_ref         0.0633
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2431
_reflns_number_total             2838
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00549c2.cif
_cod_data_source_block           gs2
_cod_depositor_comments
'Adding full bibliography for 7718667--7718675.cif.'
_cod_database_code               7718669
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Ru1 N7 O8 C4 H17'
_shelx_estimated_absorpt_t_max   0.943
_shelx_estimated_absorpt_t_min   0.797
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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, All O(H,H) groups
2.a Free rotating group:
 O3(H3E,H3F)
2.b Rotating group:
 O2(H2)
2.c Secondary CH2 refined with riding coordinates:
 N3(H3A,H3B), N5(H5A,H5B), N2(H2A,H2B), N4(H4A,H4B), C1(H1A,H1B), C2(H2C,H2D),
 C3(H3C,H3D), C4(H4C,H4D)
;
_shelx_res_checksum              63800
_shelx_hkl_checksum              84845
_olex2_date_sample_data_collection 2023-03-15
_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 3.841
_oxdiff_exptl_absorpt_empirical_full_min 0.256