#------------------------------------------------------------------------------
#$Date: 2024-10-09 00:51:42 +0200 (Wed 09 de Oct de 2024) $
#$Revision: 295365 $
#$URL: svn://www.crystallography.net/cod/cif/7/71/71/7717182.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7717182
loop_
_publ_author_name
'Yakovlev, Ivan A.'
'Golubeva, Yuliya A.'
'Klyushova, Lyubov'
'Kostin, Gennadiy'
'Mikhailov, Artem A.'
_publ_section_title
;
 Photoinduced cytotoxic activity of a rare ruthenium nitrosyl
 phenanthroline complex showing NO generation in human cells
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D4DT02653E
_journal_year                    2024
_chemical_formula_moiety         'C12 H9 N5 O6 Ru C3 H7 N O'
_chemical_formula_sum            'C15 H16 N6 O7 Ru'
_chemical_formula_weight         986.81
_chemical_name_systematic        Block
_chemical_properties_physical    Light-sensitive,Photo-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-02-05
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-02-05 deposited with the CCDC.	2024-10-01 downloaded from the CCDC.
;
_cell_angle_alpha                92.9480(10)
_cell_angle_beta                 93.6620(10)
_cell_angle_gamma                103.6120(10)
_cell_formula_units_Z            1
_cell_length_a                   7.08750(10)
_cell_length_b                   10.3691(2)
_cell_length_c                   12.6632(3)
_cell_measurement_reflns_used    9876
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      31.34
_cell_measurement_theta_min      2.50
_cell_volume                     900.52(3)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.927
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0245
_diffrn_reflns_av_unetI/netI     0.0263
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.927
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            19476
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.927
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.550
_diffrn_reflns_theta_min         1.615
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.926
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.6835
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1340 before and 0.0404 after correction.
The Ratio of minimum to maximum transmission is 0.9160.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear greenish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.820
_exptl_crystal_description       block
_exptl_crystal_F_000             496
_exptl_crystal_preparation       DMF
_exptl_crystal_recrystallization_method evoparation
_exptl_crystal_size_max          1
_exptl_crystal_size_mid          0.8
_exptl_crystal_size_min          0.4
_refine_diff_density_max         0.444
_refine_diff_density_min         -0.544
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     265
_refine_ls_number_reflns         5590
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0258
_refine_ls_R_factor_gt           0.0219
_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/[σ²(Fo²)+(0.0132P)²+0.6048P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0470
_refine_ls_wR_factor_ref         0.0485
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5151
_reflns_number_total             5590
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4dt02653e2.cif
_cod_data_source_block           mo_ccu_zargarova_0m
_cod_database_code               7717182
_shelx_shelxl_version_number     2018/3
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.708
_shelx_estimated_absorpt_t_min   0.458
_olex2_refinement_description
;
1.a Rotating group:
 O002(H002)
1.b Aromatic/amide H refined with riding coordinates:
 C00J(H00J), C00K(H00K), C00L(H00L), C00M(H00M), C00N(H00N), C00O(H00O),
 C00P(H00P), C00Q(H00Q), C00R(H00R)
1.c Idealised Me refined as rotating group:
 C00S(H00A,H00B,H00C), C00T(H00D,H00E,H00F)
;
_olex2_exptl_crystal_mounting_method -
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ru01 Ru 0.73474(2) 0.61393(2) 0.22705(2) 0.01428(3) Uani 1 1 d . . . . .
O002 O 1.01493(15) 0.67608(11) 0.24107(8) 0.0207(2) Uani 1 1 d . . . . .
H002 H 1.049289 0.757475 0.272164 0.031 Uiso 1 1 d R U . . .
O003 O 0.31255(16) 0.53381(12) 0.19004(9) 0.0272(2) Uani 1 1 d . . . . .
O004 O 0.33661(18) 0.32187(11) 0.33340(10) 0.0292(3) Uani 1 1 d . . . . .
O005 O 0.8251(2) 0.84622(11) 0.10201(10) 0.0319(3) Uani 1 1 d . . . . .
N006 N 0.75794(17) 0.49832(11) 0.35610(9) 0.0144(2) Uani 1 1 d . . . . .
N007 N 0.78511(17) 0.44180(11) 0.14929(9) 0.0157(2) Uani 1 1 d . . . . .
O008 O 0.8659(2) 0.84786(12) 0.37076(10) 0.0348(3) Uani 1 1 d . . . . .
N009 N 0.73621(19) 0.72817(12) 0.09533(10) 0.0206(2) Uani 1 1 d . . . . .
O00A O 0.64701(19) 0.67619(12) 0.01061(9) 0.0319(3) Uani 1 1 d . . . . .
N00B N 0.7174(2) 0.77872(12) 0.32161(10) 0.0220(3) Uani 1 1 d . . . . .
O00C O 0.5588(2) 0.80554(13) 0.33124(12) 0.0413(3) Uani 1 1 d . . . . .
N00D N 0.3346(2) 0.11093(13) 0.27211(11) 0.0239(3) Uani 1 1 d . . . . .
N00E N 0.47855(18) 0.56023(12) 0.20677(9) 0.0178(2) Uani 1 1 d . . . . .
C00F C 0.8086(2) 0.34826(13) 0.21753(11) 0.0154(2) Uani 1 1 d . . . . .
C00G C 0.7932(2) 0.37805(13) 0.32759(11) 0.0146(2) Uani 1 1 d . . . . .
C00H C 0.8420(2) 0.22523(14) 0.18290(12) 0.0183(3) Uani 1 1 d . . . . .
C00I C 0.8098(2) 0.28382(14) 0.40110(11) 0.0171(3) Uani 1 1 d . . . . .
C00J C 0.7394(2) 0.52808(14) 0.45771(11) 0.0177(3) Uani 1 1 d . . . . .
H00J H 0.715123 0.611856 0.477884 0.021 Uiso 1 1 calc R U . . .
C00K C 0.8425(2) 0.15869(14) 0.36408(12) 0.0211(3) Uani 1 1 d . . . . .
H00K H 0.853928 0.094419 0.413409 0.025 Uiso 1 1 calc R U . . .
C00L C 0.3349(2) 0.23860(15) 0.26088(13) 0.0239(3) Uani 1 1 d . . . . .
H00L H 0.333683 0.267057 0.190772 0.029 Uiso 1 1 calc R U . . .
C00M C 0.8576(2) 0.13058(14) 0.25942(13) 0.0213(3) Uani 1 1 d . . . . .
H00M H 0.878800 0.046759 0.236645 0.026 Uiso 1 1 calc R U . . .
C00N C 0.7546(2) 0.43944(15) 0.53585(12) 0.0204(3) Uani 1 1 d . . . . .
H00N H 0.741571 0.463522 0.607944 0.025 Uiso 1 1 calc R U . . .
C00O C 0.7969(2) 0.41651(15) 0.04638(11) 0.0194(3) Uani 1 1 d . . . . .
H00O H 0.778779 0.481130 -0.001311 0.023 Uiso 1 1 calc R U . . .
C00P C 0.7883(2) 0.31815(15) 0.50803(12) 0.0207(3) Uani 1 1 d . . . . .
H00P H 0.797150 0.257237 0.560586 0.025 Uiso 1 1 calc R U . . .
C00Q C 0.8567(2) 0.20223(15) 0.07346(12) 0.0226(3) Uani 1 1 d . . . . .
H00Q H 0.881284 0.120968 0.046712 0.027 Uiso 1 1 calc R U . . .
C00R C 0.8353(2) 0.29784(16) 0.00565(12) 0.0235(3) Uani 1 1 d . . . . .
H00R H 0.846377 0.283685 -0.068176 0.028 Uiso 1 1 calc R U . . .
C00S C 0.3269(3) 0.05798(17) 0.37598(14) 0.0305(4) Uani 1 1 d . . . . .
H00A H 0.355181 0.131514 0.430863 0.046 Uiso 1 1 calc R U . . .
H00B H 0.423728 0.004857 0.384637 0.046 Uiso 1 1 calc R U . . .
H00C H 0.196707 0.001778 0.382619 0.046 Uiso 1 1 calc R U . . .
C00T C 0.3246(3) 0.01906(18) 0.18017(16) 0.0368(4) Uani 1 1 d . . . . .
H00D H 0.201233 -0.048522 0.175922 0.055 Uiso 1 1 calc R U . . .
H00E H 0.433343 -0.024201 0.186820 0.055 Uiso 1 1 calc R U . . .
H00F H 0.332520 0.067948 0.115758 0.055 Uiso 1 1 calc R U . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O002 Ru01 N006 88.20(4) . . ?
O002 Ru01 N007 85.30(5) . . ?
O002 Ru01 N009 87.33(5) . . ?
O002 Ru01 N00B 88.80(5) . . ?
N006 Ru01 N007 79.29(4) . . ?
N009 Ru01 N006 174.97(5) . . ?
N009 Ru01 N007 98.04(5) . . ?
N00B Ru01 N006 93.73(5) . . ?
N00B Ru01 N007 170.98(5) . . ?
N00B Ru01 N009 88.47(5) . . ?
N00E Ru01 O002 176.72(5) . . ?
N00E Ru01 N006 94.93(5) . . ?
N00E Ru01 N007 94.27(5) . . ?
N00E Ru01 N009 89.51(5) . . ?
N00E Ru01 N00B 92.00(5) . . ?
Ru01 O002 H002 110.3 . . ?
C00G N006 Ru01 113.17(9) . . ?
C00J N006 Ru01 127.99(10) . . ?
C00J N006 C00G 118.83(12) . . ?
C00F N007 Ru01 112.75(9) . . ?
C00O N007 Ru01 128.43(10) . . ?
C00O N007 C00F 118.82(12) . . ?
O005 N009 Ru01 120.31(10) . . ?
O005 N009 O00A 120.26(13) . . ?
O00A N009 Ru01 119.43(10) . . ?
O008 N00B Ru01 119.66(10) . . ?
O00C N00B Ru01 120.14(11) . . ?
O00C N00B O008 120.17(13) . . ?
C00L N00D C00S 120.70(14) . . ?
C00L N00D C00T 120.99(15) . . ?
C00S N00D C00T 118.09(14) . . ?
O003 N00E Ru01 174.99(12) . . ?
N007 C00F C00G 117.41(12) . . ?
N007 C00F C00H 122.46(13) . . ?
C00H C00F C00G 120.11(13) . . ?
N006 C00G C00F 117.37(12) . . ?
N006 C00G C00I 122.68(12) . . ?
C00I C00G C00F 119.94(12) . . ?
C00F C00H C00M 118.87(13) . . ?
C00F C00H C00Q 117.34(13) . . ?
C00Q C00H C00M 123.79(13) . . ?
C00G C00I C00K 119.07(13) . . ?
C00G C00I C00P 117.07(13) . . ?
C00P C00I C00K 123.84(13) . . ?
N006 C00J H00J 119.1 . . ?
N006 C00J C00N 121.88(13) . . ?
C00N C00J H00J 119.1 . . ?
C00I C00K H00K 119.5 . . ?
C00M C00K C00I 120.94(13) . . ?
C00M C00K H00K 119.5 . . ?
O004 C00L N00D 125.50(16) . . ?
O004 C00L H00L 117.3 . . ?
N00D C00L H00L 117.3 . . ?
C00H C00M H00M 119.5 . . ?
C00K C00M C00H 121.07(13) . . ?
C00K C00M H00M 119.5 . . ?
C00J C00N H00N 120.1 . . ?
C00P C00N C00J 119.78(13) . . ?
C00P C00N H00N 120.1 . . ?
N007 C00O H00O 118.8 . . ?
N007 C00O C00R 122.30(14) . . ?
C00R C00O H00O 118.8 . . ?
C00I C00P H00P 120.1 . . ?
C00N C00P C00I 119.76(13) . . ?
C00N C00P H00P 120.1 . . ?
C00H C00Q H00Q 120.2 . . ?
C00R C00Q C00H 119.67(14) . . ?
C00R C00Q H00Q 120.2 . . ?
C00O C00R H00R 120.3 . . ?
C00Q C00R C00O 119.38(14) . . ?
C00Q C00R H00R 120.3 . . ?
N00D C00S H00A 109.5 . . ?
N00D C00S H00B 109.5 . . ?
N00D C00S H00C 109.5 . . ?
H00A C00S H00B 109.5 . . ?
H00A C00S H00C 109.5 . . ?
H00B C00S H00C 109.5 . . ?
N00D C00T H00D 109.5 . . ?
N00D C00T H00E 109.5 . . ?
N00D C00T H00F 109.5 . . ?
H00D C00T H00E 109.5 . . ?
H00D C00T H00F 109.5 . . ?
H00E C00T H00F 109.5 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ru01 O002 1.9316(10) . ?
Ru01 N006 2.0964(11) . ?
Ru01 N007 2.1087(11) . ?
Ru01 N009 2.0940(12) . ?
Ru01 N00B 2.0679(12) . ?
Ru01 N00E 1.7671(13) . ?
O002 H002 0.8851 . ?
O003 N00E 1.1466(16) . ?
O004 C00L 1.2253(19) . ?
O005 N009 1.2336(17) . ?
N006 C00G 1.3637(17) . ?
N006 C00J 1.3296(18) . ?
N007 C00F 1.3634(18) . ?
N007 C00O 1.3278(18) . ?
O008 N00B 1.2348(18) . ?
N009 O00A 1.2388(17) . ?
N00B O00C 1.2315(18) . ?
N00D C00L 1.338(2) . ?
N00D C00S 1.450(2) . ?
N00D C00T 1.453(2) . ?
C00F C00G 1.4285(19) . ?
C00F C00H 1.4048(19) . ?
C00G C00I 1.4031(19) . ?
C00H C00M 1.432(2) . ?
C00H C00Q 1.409(2) . ?
C00I C00K 1.432(2) . ?
C00I C00P 1.409(2) . ?
C00J H00J 0.9500 . ?
C00J C00N 1.401(2) . ?
C00K H00K 0.9500 . ?
C00K C00M 1.359(2) . ?
C00L H00L 0.9500 . ?
C00M H00M 0.9500 . ?
C00N H00N 0.9500 . ?
C00N C00P 1.367(2) . ?
C00O H00O 0.9500 . ?
C00O C00R 1.401(2) . ?
C00P H00P 0.9500 . ?
C00Q H00Q 0.9500 . ?
C00Q C00R 1.373(2) . ?
C00R H00R 0.9500 . ?
C00S H00A 0.9800 . ?
C00S H00B 0.9800 . ?
C00S H00C 0.9800 . ?
C00T H00D 0.9800 . ?
C00T H00E 0.9800 . ?
C00T H00F 0.9800 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ru01 N006 C00G C00F -0.09(15) . . . . ?
Ru01 N006 C00G C00I -178.61(11) . . . . ?
Ru01 N006 C00J C00N 178.61(10) . . . . ?
Ru01 N007 C00F C00G 0.96(16) . . . . ?
Ru01 N007 C00F C00H 179.42(11) . . . . ?
Ru01 N007 C00O C00R 178.67(11) . . . . ?
N006 C00G C00I C00K 178.61(13) . . . . ?
N006 C00G C00I C00P 0.0(2) . . . . ?
N006 C00J C00N C00P -0.4(2) . . . . ?
N007 C00F C00G N006 -0.60(19) . . . . ?
N007 C00F C00G C00I 177.96(12) . . . . ?
N007 C00F C00H C00M -177.64(13) . . . . ?
N007 C00F C00H C00Q 1.9(2) . . . . ?
N007 C00O C00R C00Q 1.7(2) . . . . ?
C00F N007 C00O C00R -0.9(2) . . . . ?
C00F C00G C00I C00K 0.1(2) . . . . ?
C00F C00G C00I C00P -178.44(13) . . . . ?
C00F C00H C00M C00K -0.6(2) . . . . ?
C00F C00H C00Q C00R -1.0(2) . . . . ?
C00G N006 C00J C00N -0.1(2) . . . . ?
C00G C00F C00H C00M 0.8(2) . . . . ?
C00G C00F C00H C00Q -179.69(13) . . . . ?
C00G C00I C00K C00M 0.0(2) . . . . ?
C00G C00I C00P C00N -0.6(2) . . . . ?
C00H C00F C00G N006 -179.09(12) . . . . ?
C00H C00F C00G C00I -0.5(2) . . . . ?
C00H C00Q C00R C00O -0.7(2) . . . . ?
C00I C00K C00M C00H 0.3(2) . . . . ?
C00J N006 C00G C00F 178.83(13) . . . . ?
C00J N006 C00G C00I 0.3(2) . . . . ?
C00J C00N C00P C00I 0.8(2) . . . . ?
C00K C00I C00P C00N -179.08(14) . . . . ?
C00M C00H C00Q C00R 178.50(15) . . . . ?
C00O N007 C00F C00G -179.42(13) . . . . ?
C00O N007 C00F C00H -1.0(2) . . . . ?
C00P C00I C00K C00M 178.48(15) . . . . ?
C00Q C00H C00M C00K 179.85(15) . . . . ?
C00S N00D C00L O004 3.0(3) . . . . ?
C00T N00D C00L O004 177.49(16) . . . . ?
