#------------------------------------------------------------------------------
#$Date: 2021-03-05 03:56:12 +0200 (Fri, 05 Mar 2021) $
#$Revision: 262609 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/64/7706454.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_7706454
loop_
_publ_author_name
'Mikhailov, Artem A.'
'Sukhikh, Taisiya S.'
'Kuratieva, Natalia V.'
'Pishchur, Denis P.'
'Kostin, Gennadiy A.'
_publ_section_title
;
 Remarkable thermal stability of light-induced Ru-ON linkage isomers in
 mixed salts of a ruthenium amine complex with a trans-ON-Ru-F
 coordinate.
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2864
_journal_page_last               2871
_journal_paper_doi               10.1039/d0dt04323k
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety
'F H12 N5 O Ru, 1.5(F), 1.5(N O3), (H3 O), 0.5(H2 O)'
_chemical_formula_sum            'F2.5 H16 N6.5 O7 Ru'
_chemical_formula_weight         367.73
_space_group_crystal_system      tetragonal
_space_group_IT_number           87
_space_group_name_Hall           '-I 4'
_space_group_name_H-M_alt        'I 4/m'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-09-08
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-09-08 deposited with the CCDC.	2021-01-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.8917(6)
_cell_length_b                   16.8917(6)
_cell_length_c                   7.7823(5)
_cell_measurement_reflns_used    9888
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.76
_cell_measurement_theta_min      2.41
_cell_volume                     2220.52(18)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 8.33
_diffrn_detector_type            'Bruker APEXII CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0287
_diffrn_reflns_av_unetI/netI     0.0133
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            16232
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.784
_diffrn_reflns_theta_min         2.411
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    1.488
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6394
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0688 before and 0.0458 after correction.
The Ratio of minimum to maximum transmission is 0.8573.
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.176
_exptl_crystal_description       prism
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.084
_refine_diff_density_min         -1.465
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.248
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     94
_refine_ls_number_reflns         1550
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.248
_refine_ls_R_factor_all          0.0466
_refine_ls_R_factor_gt           0.0459
_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)+(0.0306P)²+29.9232P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1130
_refine_ls_wR_factor_ref         0.1134
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1510
_reflns_number_total             1550
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0dt04323k2.cif
_cod_data_source_block           artma4f3_2_pl
_cod_depositor_comments
'Adding full bibliography for 7706454--7706455.cif.'
_cod_original_cell_volume        2220.5(2)
_cod_original_formula_sum        'F2.50 H16 N6.50 O7 Ru'
_cod_database_code               7706454
_shelx_shelxl_version_number     2017/1
_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   0.808
_shelx_estimated_absorpt_t_min   0.624
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H,H,H) groups
2. Shared sites
{O6A, O6B}
3. Uiso/Uaniso restraints and constraints
Uiso(O7B) = Uiso(O7A)
Uiso(O6A) = Uiso(O6B)
4. Others
 Fixed Sof: O6B(0.25) O7B(0.25) O4(0.25) O5(0.25) O6A(0.25) N5(0.25) O7A(0.25)
 Fixed Z: O6B(-0.5) O4(-0.5) O5(-0.5) O6A(-0.5) N5(-0.5)
5.a Idealised Me refined as rotating group:
 N2(H2A,H2B,H2C), N3(H3A,H3B,H3C)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x, z'
'-x, -y, z'
'y, -x, z'
'x+1/2, y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-x, -y, -z'
'y, -x, -z'
'x, y, -z'
'-y, x, -z'
'-x+1/2, -y+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
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
Ru1 Ru 0.07634(3) 0.23386(3) 0.000000 0.01701(16) Uani 1 2 d S T P . .
F1 F -0.0188(2) 0.1706(2) 0.000000 0.0268(8) Uani 1 2 d S T P . .
O1 O 0.2189(3) 0.3269(4) 0.000000 0.0444(15) Uani 1 2 d S T P . .
N1 N 0.1612(3) 0.2902(4) 0.000000 0.0292(12) Uani 1 2 d S T P . .
N2 N 0.1169(3) 0.1558(2) -0.1886(5) 0.0295(9) Uani 1 1 d . . . . .
H2A H 0.162898 0.138291 -0.160220 0.035 Uiso 1 1 calc GR . . . .
H2B H 0.120076 0.180201 -0.285341 0.035 Uiso 1 1 calc GR . . . .
H2C H 0.084467 0.116803 -0.197820 0.035 Uiso 1 1 calc GR . . . .
N3 N 0.0197(2) 0.3009(2) 0.1892(5) 0.0257(8) Uani 1 1 d . . . . .
H3A H 0.037816 0.287926 0.288576 0.031 Uiso 1 1 calc GR . . . .
H3B H -0.030396 0.291892 0.185743 0.031 Uiso 1 1 calc GR . . . .
H3C H 0.028359 0.350334 0.171109 0.031 Uiso 1 1 calc GR . . . .
F3 F 0.000000 0.000000 -0.1954(13) 0.081(3) Uani 1 4 d S T P . .
F2 F -0.0297(4) 0.1715(4) -0.500000 0.088(3) Uani 1 2 d S T P A 1
O2 O 0.2006(2) 0.3383(2) -0.3610(5) 0.0378(9) Uani 1 1 d . . . . .
O3 O 0.1189(3) 0.2644(3) -0.500000 0.0293(10) Uani 1 2 d S T P . .
N4 N 0.1739(3) 0.3139(3) -0.500000 0.0235(11) Uani 1 2 d S T P . .
O6B O -0.0571(5) 0.3890(5) -0.500000 0.075(2) Uiso 0.5 2 d S T P B 2
O7B O 0.049(2) 0.082(2) -0.573(5) 0.074(5) Uiso 0.25 1 d . . . C -2
O4 O 0.0596(10) 0.4400(11) -0.500000 0.067(4) Uiso 0.25 1 d S T P D -1
O5 O -0.0426(14) 0.5152(16) -0.500000 0.096(7) Uiso 0.25 1 d S T P D -1
O6A O -0.0571(5) 0.3890(5) -0.500000 0.075(2) Uiso 0.25 1 d S T P D -1
N5 N -0.0139(11) 0.4542(11) -0.500000 0.054(4) Uiso 0.25 1 d S T P D -1
O7A O 0.038(2) 0.066(2) -0.415(5) 0.074(5) Uiso 0.25 1 d . . . E -1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
F F 0.0171 0.0103 '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
F1 Ru1 N2 85.62(15) . . ?
F1 Ru1 N2 85.62(15) . 11 ?
F1 Ru1 N3 85.33(14) . . ?
F1 Ru1 N3 85.33(14) . 11 ?
N1 Ru1 F1 180.0(2) . . ?
N1 Ru1 N2 94.3(2) . . ?
N1 Ru1 N2 94.3(2) . 11 ?
N1 Ru1 N3 94.70(19) . 11 ?
N1 Ru1 N3 94.70(19) . . ?
N2 Ru1 N2 89.3(2) . 11 ?
N2 Ru1 N3 89.83(16) 11 . ?
N2 Ru1 N3 89.83(16) . 11 ?
N2 Ru1 N3 170.95(17) . . ?
N2 Ru1 N3 170.95(17) 11 11 ?
N3 Ru1 N3 89.6(2) 11 . ?
O1 N1 Ru1 178.9(7) . . ?
O2 N4 O2 121.1(6) 11_554 . ?
O2 N4 O3 119.4(3) 11_554 . ?
O2 N4 O3 119.4(3) . . ?
O4 N5 O6A 112.5(18) . . ?
O5 N5 O4 126(3) . . ?
O5 N5 O6A 121(2) . . ?
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
Ru1 F1 1.930(4) . ?
Ru1 N1 1.721(6) . ?
Ru1 N2 2.088(4) 11 ?
Ru1 N2 2.088(4) . ?
Ru1 N3 2.089(4) 11 ?
Ru1 N3 2.089(4) . ?
O1 N1 1.154(8) . ?
O2 N4 1.242(5) . ?
O3 N4 1.250(7) . ?
O4 N5 1.27(3) . ?
O5 N5 1.14(3) . ?
O6A N5 1.32(2) . ?
