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_7718668
_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 H18 N5 O2 Ru, 3(N O3)'
_chemical_formula_sum            'C4 H18 N8 O11 Ru'
_chemical_formula_weight         455.33
_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
_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                   9.3314(2)
_cell_length_b                   11.8505(3)
_cell_length_c                   13.4342(3)
_cell_measurement_reflns_used    19322
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      32.7000
_cell_measurement_theta_min      2.2250
_cell_volume                     1485.58(6)
_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_temperature      100.15
_diffrn_detector_area_resol_mean 10.4508
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.958
_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    -49.00  54.00   1.00    7.50    --  -19.50  57.00 120.00  103
  2  \w    -49.00  54.00   1.00    7.50    --  -19.50  57.00   0.00  103
  3  \w     -9.00  95.00   1.00    7.50    --   20.91  57.00 -90.00  104
  4  \w    -49.00  54.00   1.00    7.50    --  -19.50  57.00-120.00  103
  5  \w     -9.00  95.00   1.00    7.50    --   20.91  57.00 150.00  104
  6  \w     -9.00  95.00   1.00    7.50    --   20.91  57.00  60.00  104
;
_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           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0318
_diffrn_reflns_av_unetI/netI     0.0217
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            28532
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.939
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.895
_diffrn_reflns_theta_min         2.292
_exptl_absorpt_coefficient_mu    1.134
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76068
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
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    2.036
_exptl_crystal_description       block
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.805
_refine_diff_density_min         -0.568
_refine_diff_density_rms         0.073
_refine_ls_abs_structure_details
;
 Flack x determined using 2132 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.016(8)
_refine_ls_extinction_coef       0.0034(3)
_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   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     231
_refine_ls_number_reflns         5212
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0193
_refine_ls_R_factor_gt           0.0183
_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^)+(0.0197P)^2^+0.6508P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0425
_refine_ls_wR_factor_ref         0.0433
_reflns_Friedel_coverage         0.740
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.914
_reflns_number_gt                5086
_reflns_number_total             5212
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00549c2.cif
_cod_data_source_block           appolinaire_xtal1
_cod_depositor_comments
'Adding full bibliography for 7718667--7718675.cif.'
_cod_database_code               7718668
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.895
_shelx_estimated_absorpt_t_min   0.805
_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,H) groups
2. Restrained distances
 O9A-N8 = O10A-N8 = O11A-N8
 1.25 with sigma of 0.002
 O11A-O9A
 2.15 with sigma of 0.004
 O9A-O10A
 2.15 with sigma of 0.004
 O11A-O10A
 2.15 with sigma of 0.004
 Ru1-H2A \\sim Ru1-H2B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O10A) = Uanis(O10)
Uanis(O11) = Uanis(O11A)
Uanis(O9A) = Uanis(O9)
4. Others
 Sof(O11A)=Sof(O10A)=Sof(O9A)=1-FVAR(1)
 Sof(O9)=Sof(O10)=Sof(O11)=FVAR(1)
5.a Free rotating group:
 O2(H2A,H2B)
5.b Secondary CH2 refined with riding coordinates:
 N5(H5A,H5B), N2(H2C,H2D), N4(H4A,H4B), N3(H3A,H3B), C4(H4C,H4D), C1(H1A,H1B),
 C2(H2E,H2F), C3(H3C,H3D)
;
_shelx_res_checksum              95202
_shelx_hkl_checksum              72082
_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
;