Ruthenium nitrosyl complexes with the molecular framework [RuII(dmdptz)(bpy)(NO)]n+ (dmdptz: N,N-dimethyl-4,6-di(pyridin-2-yl)-1,3,5-triazin-2-amine and bpy: 2,2′-bipyridine). Electronic structure, reactivity aspects, photorelease, and scavenging of NO
Giri, Bishnubasu; Kumbhakar, Sadananda; Selvan K, Kalai; Muley, Arabinda; Maji, Somnath; New Journal of Chemistry 44 (2020) 18732–18744; doi:10.1039/D0NJ03923C

data_7060039
_publ_section_title
;
 Ruthenium nitrosyl complexes with the molecular framework
 [RuII(dmdptz)(bpy)(NO)]n+ (dmdptz:
 N,N-dimethyl-4,6-di(pyridin-2-yl)-1,3,5-triazin-2-amine and bpy:
 2,2&#x2032;-bipyridine). Electronic structure, reactivity aspects,
 photorelease, and scavenging of NO
;
_journal_issue                   43
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              18732
_journal_page_last               18744
_journal_paper_doi               10.1039/D0NJ03923C
_journal_volume                  44
_journal_year                    2020
_chemical_formula_moiety         'C25 H22 N9 O2 Ru, Cl O4, H2 O'
_chemical_formula_sum            'C25 H24 Cl N9 O7 Ru'
_chemical_formula_weight         699.05
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_Int_Tables_number      61
_atom_sites_solution_primary     iterative
_audit_creation_date             2020-01-27
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-10-05 deposited with the CCDC.	2020-10-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.07395(18)
_cell_length_b                   16.71663(17)
_cell_length_c                   20.7947(2)
_cell_measurement_reflns_used    9677
_cell_measurement_temperature    290
_cell_measurement_theta_max      69.6980
_cell_measurement_theta_min      4.2530
_cell_volume                     5587.58(10)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      290
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1293
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.9947
_diffrn_measured_fraction_theta_max 0.9947
_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    -18.00   8.00   1.00    1.88    --    0.00 -57.00-120.00   26
  2  \w    -40.00   0.00   1.00    1.88    --    0.00 116.00 -58.00   40
  3  \w    -58.00 -23.00   1.00    1.88    --    0.00 -57.00-120.00   35
  4  \w     24.00 109.00   1.00    7.50    --   54.00-125.00-150.00   85
  5  \w      0.00  27.00   1.00    7.50    --   54.00 -57.00-150.00   27
  6  \w     50.00 117.00   1.00    7.50    --   54.00  38.00  60.00   67
  7  \w     68.00 100.00   1.00    7.50    --   54.00 164.00  90.00   32
  8  \w     75.00 112.00   1.00    7.50    --  108.00-111.00 -90.00   37
  9  \w     82.00 111.00   1.00    7.50    --  108.00-111.00  30.00   29
 10  \w    134.00 175.00   1.00    7.50    --  108.00  63.00  90.00   41
 11  \w    146.00 175.00   1.00    7.50    --  108.00  50.00-150.00   29
 12  \w     56.00  89.00   1.00    7.50    --  108.00 -38.00 -30.00   33
 13  \w     44.00  95.00   1.00    7.50    --  108.00 -77.00   0.00   51
 14  \w    114.00 139.00   1.00    7.50    --  108.00 -77.00   0.00   25
 15  \w    153.00 178.00   1.00    7.50    --  108.00  50.00-120.00   25
 16  \w     37.00  63.00   1.00    7.50    --  108.00-111.00  30.00   26
 17  \w     98.00 129.00   1.00    7.50    --  108.00  50.00-120.00   31
 18  \w    150.00 175.00   1.00    7.50    --  108.00  63.00 150.00   25
 19  \w    104.00 133.00   1.00    7.50    --  108.00  63.00 150.00   29
 20  \w    118.00 150.00   1.00    7.50    --  108.00 178.00 -60.00   32
 21  \w     46.00  72.00   1.00    7.50    --  108.00 -63.00 -30.00   26
 22  \w     48.00  73.00   1.00    7.50    --  108.00 -63.00  60.00   25
 23  \w     95.00 127.00   1.00    7.50    --  108.00 -63.00  60.00   32
 24  \w     92.00 117.00   1.00    7.50    --  108.00  25.00-180.00   25
 25  \w     57.00 101.00   1.00    7.50    --  108.00 178.00 -60.00   44
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0198065000
_diffrn_orient_matrix_UB_12      -0.0665306000
_diffrn_orient_matrix_UB_13      -0.0489642000
_diffrn_orient_matrix_UB_21      -0.0925978000
_diffrn_orient_matrix_UB_22      0.0040019000
_diffrn_orient_matrix_UB_23      0.0189086000
_diffrn_orient_matrix_UB_31      -0.0148988000
_diffrn_orient_matrix_UB_32      0.0636477000
_diffrn_orient_matrix_UB_33      -0.0522636000
_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  0.0259
_diffrn_reflns_av_unetI/netI     0.0200
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            19322
_diffrn_reflns_theta_full        69.9951
_diffrn_reflns_theta_max         70.00
_diffrn_reflns_theta_min         4.25
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.969
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84234
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dull reddish black'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.6618
_exptl_crystal_description       cube
_exptl_crystal_F_000             2844.2798
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.6264
_refine_diff_density_min         -1.0760
_refine_diff_density_rms         0.0855
_refine_ls_d_res_high            0.8204
_refine_ls_d_res_low             10.3974
_refine_ls_goodness_of_fit_ref   1.0490
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    43
_refine_ls_number_parameters     393
_refine_ls_number_reflns         5265
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0490
_refine_ls_R_factor_all          0.0413
_refine_ls_R_factor_gt           0.0380
_refine_ls_shift/su_max          0.0001
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0661P)^2^+4.1287P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1037
_refine_ls_wR_factor_ref         0.1078
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              19
_reflns_limit_h_min              0
_reflns_limit_k_max              20
_reflns_limit_k_min              0
_reflns_limit_l_max              25
_reflns_limit_l_min              0
_reflns_number_gt                4756
_reflns_number_total             5265
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d0nj03923c2.cif
_cod_data_source_block           exp_9452
_cod_depositor_comments
;
Adding full bibliography for 7060037--7060039.cif.

2025-03-29
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum          'C28.571 H27.429 Cl1.143 N10.286 O8 Ru1.143'
_cod_original_formula_weight         798.91
_cod_original_formula_moiety
'1.14(C25 H22 N9 O2 Ru), 1.14(Cl O4), 1.14(H2 O)'
_cod_original_formula_units_Z            7
_cod_original_cell_volume        5587.59(10)
_cod_database_code               7060039
_chemical_oxdiff_formula         C25H22ClN9O6Ru
_reflns_odcompleteness_completeness 92.52
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2.a Free rotating group:
 O5aa(H5aa,H5ab)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C22(H22), C2(H2), C3(H3), C10(H10), C4(H4), C11(H11), C12(H12),
 C16(H16), C20(H20), C14(H14), C23(H23), C15(H15), C13(H13), C21(H21), C17(H17)
2.c Idealised Me refined as rotating group:
 C24(H24a,H24b,H24c), C25(H25a,H25b,H25c)
;
_olex2_date_sample_data_collection 2019-02-01
_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 1.527
_oxdiff_exptl_absorpt_empirical_full_min 0.795