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#$Date: 2019-11-07 22:19:49 +0200 (Thu, 07 Nov 2019) $
#$Revision: 223756 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/03/7700344.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_7700344
loop_
_publ_author_name
'Roveda, Jr, Antonio C'
'Santos, Willy G.'
'Souza, Maykon L.'
'Adelson, Charles N.'
'Gonçalves, Felipe S'
'Castellano, Eduardo E.'
'Garino, Claudio'
'Franco, Douglas W.'
'Cardoso, Daniel R.'
_publ_section_title
;
 Light-activated generation of nitric oxide (NO) and sulfite anion
 radicals (SO₃˙⁻) from a ruthenium(ii)
 nitrosylsulphito complex.
;
_journal_issue                   29
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10812
_journal_page_last               10823
_journal_paper_doi               10.1039/c9dt01432b
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C6 H18 N7 O2 Ru,3(B F4)'
_chemical_formula_sum            'C6 H18 B3 F12 N7 O2 Ru'
_chemical_formula_weight         581.77
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/6
_audit_update_record
;
2019-06-13 deposited with the CCDC.    2019-06-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.6469(14)
_cell_length_b                   8.6875(5)
_cell_length_c                   9.7514(5)
_cell_measurement_reflns_used    6189
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      32.7040
_cell_measurement_theta_min      3.1070
_cell_volume                     2088.0(2)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini (ROW)'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0429
_diffrn_reflns_av_unetI/netI     0.0391
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.952
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            19332
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.952
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         34.533
_diffrn_reflns_theta_min         2.664
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.874
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.99119
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.35c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.851
_exptl_crystal_description       needle
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.190
_refine_diff_density_min         -1.140
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     166
_refine_ls_number_reflns         4454
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0656
_refine_ls_R_factor_gt           0.0416
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0528P)²+1.2336P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0983
_refine_ls_wR_factor_ref         0.1085
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3350
_reflns_number_total             4454
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9dt01432b2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 7700343--7700344.cif.'
_cod_database_code               7700344
_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.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.952
_oxdiff_exptl_absorpt_empirical_full_max 1.033
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelxl_version_number           2014/6
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'x, -y-1/2, 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
Ru Ru 0.15973(2) 0.7500 -0.01209(2) 0.02216(8) Uani 1 2 d S T P
O1 O 0.20068(13) 0.7500 -0.2874(3) 0.0613(10) Uani 1 2 d S T P
O2 O 0.08068(12) 0.7500 0.6796(3) 0.0503(8) Uani 1 2 d S T P
N1 N 0.18678(12) 0.7500 -0.1781(3) 0.0328(6) Uani 1 2 d S T P
N2 N 0.10250(8) 0.9166(2) -0.0692(2) 0.0297(4) Uani 1 1 d . . .
H2A H 0.0817 0.9395 0.0026 0.036 Uiso 1 1 d R U .
H2B H 0.1196 1.0011 -0.0976 0.036 Uiso 1 1 d R U .
H2C H 0.0819 0.8801 -0.1368 0.036 Uiso 1 1 d R U .
N4 N 0.21435(8) 0.5823(2) 0.0616(2) 0.0305(4) Uani 1 1 d . . .
H4A H 0.2075 0.5635 0.1496 0.037 Uiso 1 1 d R U .
H4B H 0.2104 0.4959 0.0134 0.037 Uiso 1 1 d R U .
H4C H 0.2482 0.6166 0.0527 0.037 Uiso 1 1 d R U .
N6 N 0.12375(11) 0.7500 0.1830(3) 0.0237(5) Uani 1 2 d S T P
N7 N -0.00222(14) 0.7500 0.5860(4) 0.0612(12) Uani 1 2 d S T P
H7A H -0.0184 0.7500 0.6642 0.073 Uiso 1 2 d R U P
H7B H -0.0209 0.7500 0.5115 0.073 Uiso 1 2 d R U P
C1 C 0.11132(11) 0.6177(3) 0.2468(2) 0.0328(5) Uani 1 1 d . . .
H1 H 0.1190 0.5250 0.2031 0.039 Uiso 1 1 calc R U .
C2 C 0.08769(12) 0.6142(3) 0.3745(3) 0.0388(6) Uani 1 1 d . . .
H2 H 0.0803 0.5206 0.4169 0.047 Uiso 1 1 calc R U .
C3 C 0.07503(14) 0.7500 0.4387(3) 0.0302(7) Uani 1 2 d S T P
C6 C 0.05075(16) 0.7500 0.5804(3) 0.0365(8) Uani 1 2 d S T P
F11 F 0.12193(12) 0.2500 0.3186(4) 0.0754(10) Uani 1 2 d S T P
F12 F 0.20116(8) 0.1210(2) 0.3263(3) 0.0708(6) Uani 1 1 d . . .
F13 F 0.1737(2) 0.2500 0.5057(3) 0.1027(17) Uani 1 2 d S T P
B1 B 0.17310(19) 0.2500 0.3651(5) 0.0409(9) Uani 1 2 d S T P
F21 F 0.31485(9) 0.6193(2) 0.3009(2) 0.0619(5) Uani 1 1 d . . .
F22 F 0.29735(15) 0.7500 0.4928(2) 0.0588(8) Uani 1 2 d S T P
F23 F 0.23756(12) 0.7500 0.3177(3) 0.0671(8) Uani 1 2 d S T P
B2 B 0.2912(2) 0.7500 0.3528(5) 0.0383(9) Uani 1 2 d S T P
F31 F 0.08088(12) 0.2500 -0.0332(4) 0.0672(9) Uani 1 2 d S T P
F32 F 0.02688(8) 0.1203(2) 0.11277(19) 0.0521(4) Uani 1 1 d . . .
F33 F -0.00865(12) 0.2500 -0.0646(3) 0.0624(8) Uani 1 2 d S T P
B3 B 0.03139(18) 0.2500 0.0313(4) 0.0338(8) Uani 1 2 d S T P
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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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
N1 Ru N2 90.62(9) . 8_575
N1 Ru N2 90.62(9) . .
N2 Ru N2 87.33(11) 8_575 .
N1 Ru N6 177.39(12) . .
N2 Ru N6 87.50(8) 8_575 .
N2 Ru N6 87.50(8) . .
N1 Ru N4 94.12(9) . .
N2 Ru N4 92.45(8) 8_575 .
N2 Ru N4 175.27(8) . .
N6 Ru N4 87.77(8) . .
N1 Ru N4 94.12(9) . 8_575
N2 Ru N4 175.27(8) 8_575 8_575
N2 Ru N4 92.45(8) . 8_575
N6 Ru N4 87.77(8) . 8_575
N4 Ru N4 87.37(11) . 8_575
O1 N1 Ru 175.4(3) . .
Ru N2 H2A 109.5 . .
Ru N2 H2B 109.5 . .
H2A N2 H2B 109.5 . .
Ru N2 H2C 109.5 . .
H2A N2 H2C 109.5 . .
H2B N2 H2C 109.5 . .
Ru N4 H4A 109.5 . .
Ru N4 H4B 109.5 . .
H4A N4 H4B 109.5 . .
Ru N4 H4C 109.5 . .
H4A N4 H4C 109.5 . .
H4B N4 H4C 109.5 . .
C1 N6 C1 117.8(3) . 8_575
C1 N6 Ru 121.10(14) . .
C1 N6 Ru 121.10(14) 8_575 .
C6 N7 H7A 120.0 . .
C6 N7 H7B 120.0 . .
H7A N7 H7B 120.0 . .
N6 C1 C2 122.3(2) . .
N6 C1 H1 118.8 . .
C2 C1 H1 118.8 . .
C3 C2 C1 119.4(2) . .
C3 C2 H2 120.3 . .
C1 C2 H2 120.3 . .
C2 C3 C2 118.6(3) . 8_575
C2 C3 C6 120.64(15) . .
C2 C3 C6 120.64(15) 8_575 .
O2 C6 N7 124.9(3) . .
O2 C6 C3 119.2(3) . .
N7 C6 C3 115.8(3) . .
F11 B1 F12 112.4(3) . .
F11 B1 F12 112.5(3) . 8_565
F12 B1 F12 109.8(4) . 8_565
F11 B1 F13 110.4(5) . .
F12 B1 F13 105.7(3) . .
F12 B1 F13 105.7(3) 8_565 .
F23 B2 F21 108.5(2) . .
F23 B2 F21 108.5(2) . 8_575
F21 B2 F21 111.6(4) . 8_575
F23 B2 F22 110.8(4) . .
F21 B2 F22 108.7(2) . .
F21 B2 F22 108.7(2) 8_575 .
F33 B3 F31 109.2(4) . .
F33 B3 F32 109.7(2) . 8_565
F31 B3 F32 109.6(2) . 8_565
F33 B3 F32 109.7(2) . .
F31 B3 F32 109.6(2) . .
F32 B3 F32 109.1(3) 8_565 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ru N1 1.750(3) .
Ru N2 2.0964(19) 8_575
Ru N2 2.0964(19) .
Ru N6 2.099(3) .
Ru N4 2.1097(19) .
Ru N4 2.1097(19) 8_575
O1 N1 1.119(4) .
O2 C6 1.216(4) .
N2 H2A 0.8900 .
N2 H2B 0.8901 .
N2 H2C 0.8900 .
N4 H4A 0.8900 .
N4 H4B 0.8900 .
N4 H4C 0.8901 .
N6 C1 1.343(3) .
N6 C1 1.343(3) 8_575
N7 C6 1.307(5) .
N7 H7A 0.8600 .
N7 H7B 0.8600 .
C1 C2 1.374(3) .
C1 H1 0.9300 .
C2 C3 1.372(3) .
C2 H2 0.9300 .
C3 C2 1.372(3) 8_575
C3 C6 1.505(5) .
F11 B1 1.340(5) .
F12 B1 1.370(3) .
F13 B1 1.371(6) .
B1 F12 1.370(3) 8_565
F21 B2 1.373(3) .
F22 B2 1.373(5) .
F23 B2 1.367(5) .
B2 F21 1.373(3) 8_575
F31 B3 1.372(5) .
F32 B3 1.383(3) .
F33 B3 1.360(5) .
B3 F32 1.383(3) 8_565
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_4
C1 N6 C1 C2 -1.3(5) 8_575 .
Ru N6 C1 C2 -179.9(2) . .
N6 C1 C2 C3 1.5(5) . .
C1 C2 C3 C2 -1.6(6) . 8_575
C1 C2 C3 C6 -178.1(3) . .
C2 C3 C6 O2 88.2(3) . .
C2 C3 C6 O2 -88.2(3) 8_575 .
C2 C3 C6 N7 -91.8(3) . .
C2 C3 C6 N7 91.8(3) 8_575 .
