Nitrosyl linkage photoisomerization in heteroleptic fluoride ruthenium complexes derived from labile nitrate precursors
Mikhailov, Artem A.; Komarov, Vladislav Yu.; Pishchur, Denis P.; Schaniel, Dominik; Kostin, Gennadiy A.; New Journal of Chemistry 45 (2021) 8192–8202; doi:10.1039/D1NJ01038G

data_7060499
_publ_section_title
;
 Nitrosyl linkage photoisomerization in heteroleptic fluoride ruthenium
 complexes derived from labile nitrate precursors
;
_journal_issue                   18
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              8192
_journal_page_last               8202
_journal_paper_doi               10.1039/D1NJ01038G
_journal_volume                  45
_journal_year                    2021
_chemical_formula_moiety
'C5 H12 F N4 O2 Ru, C5 H13 F N4 O2 Ru, 3(Cl O4)'
_chemical_formula_sum            'C10 H25 Cl3 F2 N8 O16 Ru2'
_chemical_formula_weight         859.87
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2020-12-14
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-12-14 deposited with the CCDC.	2021-03-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.730(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.6327(8)
_cell_length_b                   13.8821(5)
_cell_length_c                   10.4352(5)
_cell_measurement_reflns_used    10100
_cell_measurement_temperature    100
_cell_measurement_theta_max      32.6500
_cell_measurement_theta_min      2.3620
_cell_volume                     2680.6(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100
_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 0.942
_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    -94.00  10.00   1.00   25.00    --  -19.97 -57.00 -30.00  104
  2  \w    -53.00  50.00   1.00   25.00    --   20.91 -57.00-120.00  103
  3  \w    -53.00  50.00   1.00   25.00    --   20.91 -57.00   0.00  103
  4  \w    -53.00  50.00   1.00   25.00    --   20.91 -57.00-180.00  103
  5  \w    -94.00 -66.00   1.00   25.00    --  -19.97 -57.00  90.00   28
  6  \w    -94.00  10.00   1.00   25.00    --  -19.97 -57.00-150.00  104
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0296255000
_diffrn_orient_matrix_UB_12      0.0258794000
_diffrn_orient_matrix_UB_13      0.0322166000
_diffrn_orient_matrix_UB_21      -0.0073589000
_diffrn_orient_matrix_UB_22      0.0388918000
_diffrn_orient_matrix_UB_23      -0.0436561000
_diffrn_orient_matrix_UB_31      -0.0231746000
_diffrn_orient_matrix_UB_32      0.0206908000
_diffrn_orient_matrix_UB_33      0.0417473000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0597
_diffrn_reflns_av_unetI/netI     0.0543
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.942
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            44028
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.942
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.915
_diffrn_reflns_theta_min         2.201
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.526
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65756
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.131
_exptl_crystal_description       block
_exptl_crystal_F_000             1704
_exptl_crystal_size_max          0.036
_exptl_crystal_size_mid          0.021
_exptl_crystal_size_min          0.012
_refine_diff_density_max         1.928
_refine_diff_density_min         -1.395
_refine_diff_density_rms         0.173
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     380
_refine_ls_number_reflns         9455
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0701
_refine_ls_R_factor_gt           0.0395
_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^)+(0.0262P)^2^+3.8829P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0758
_refine_ls_wR_factor_ref         0.0924
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6755
_reflns_number_total             9455
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj01038g2.cif
_cod_data_source_block           gs
_cod_depositor_comments
;
Adding full bibliography for 7060496--7060499.cif.

2025-03-04
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum         'C6.67 H16.67 Cl2 F1.33 N5.33 O10.67 Ru1.33'
_cod_original_formula_weight         573.25
_cod_original_formula_moiety
'0.67(C5 H12 F N4 O2 Ru), 0.67(C5 H13 F N4 O2 Ru), 2(Cl O4)'
_cod_original_formula_units_Z            6
_cod_database_code               7060499
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Ru1 N4 O9 C10 H16 F1 Cl2'
_shelx_estimated_absorpt_t_max   0.982
_shelx_estimated_absorpt_t_min   0.947
_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) groups, All N(H,H,H) groups
 At 1.5 times of:
  All O(H) groups
2. Restrained distances
 O21-H21B
 0.85 with sigma of 0.02
3.a Rotating group:
 O21(H21A), O22(H22)
3.b Aromatic/amide H refined with riding coordinates:
 C31(H31), C52(H52), C11(H11), C12(H12), C51(H51), C41(H41), C21(H21),
 C42(H42), C32(H32), C22(H22D)
3.c Idealised Me refined as rotating group:
 N21(H21C,H21D,H21E), N22(H22A,H22B,H22C), N31(H31A,H31B,H31C), N32(H32A,H32B,
 H32C)
;
_shelx_res_checksum              2314
_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 1.461
_oxdiff_exptl_absorpt_empirical_full_min 0.698