#------------------------------------------------------------------------------
#$Date: 2021-06-05 21:22:54 +0200 (Sat 05 de Jun de 2021) $
#$Revision: 266148 $
#$URL: svn://www.crystallography.net/cod/cif/7/06/04/7060498.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_7060498
loop_
_publ_author_name
'Mikhailov, Artem A.'
'Komarov, Vladislav Yu.'
'Pishchur, Denis P.'
'Schaniel, Dominik'
'Kostin, Gennadiy A.'
_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         '2(C5 H11 F N5 O4 Ru), F6 Si, 2(H2 O)'
_chemical_formula_sum            'C10 H26 F8 N10 O10 Ru2 Si'
_chemical_formula_weight         828.64
_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             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                103.780(2)
_cell_angle_beta                 101.152(2)
_cell_angle_gamma                103.764(2)
_cell_formula_units_Z            1
_cell_length_a                   6.7669(3)
_cell_length_b                   9.2867(4)
_cell_length_c                   11.4450(6)
_cell_measurement_reflns_used    6138
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.51
_cell_measurement_theta_min      2.37
_cell_volume                     654.19(5)
_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 (Sheldrick, 2015)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.947
_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  0.0312
_diffrn_reflns_av_unetI/netI     0.0368
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.947
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            12459
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.947
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.720
_diffrn_reflns_theta_min         1.900
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.323
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6478
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0573 before and 0.0413 after correction.
The Ratio of minimum to maximum transmission is 0.8682.
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.103
_exptl_crystal_description       block
_exptl_crystal_F_000             410
_exptl_crystal_size_max          0.137
_exptl_crystal_size_mid          0.107
_exptl_crystal_size_min          0.059
_refine_diff_density_max         0.481
_refine_diff_density_min         -0.661
_refine_diff_density_rms         0.098
_refine_ls_extinction_coef       0.0017(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     193
_refine_ls_number_reflns         3865
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0285
_refine_ls_R_factor_gt           0.0238
_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)+(0.0080P)²+0.4554P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0442
_refine_ls_wR_factor_ref         0.0458
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3496
_reflns_number_total             3865
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1nj01038g2.cif
_cod_data_source_block           py2nh32sif6_150k
_cod_depositor_comments
'Adding full bibliography for 7060496--7060499.cif.'
_cod_database_code               7060498
_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   0.926
_shelx_estimated_absorpt_t_min   0.840
_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,H) groups
2.a Free rotating group:
 O5(H5A,H5B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C1(H1), C4(H4), C5(H5), C3(H3)
2.c Idealised Me refined as rotating group:
 N3(H3A,H3B,H3C), N2(H2A,H2B,H2C)
;
_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
Ru1 Ru 0.57886(2) 0.23300(2) 0.21677(2) 0.00936(5) Uani 1 1 d . . . . .
Si1 Si 1.000000 0.500000 0.000000 0.01497(15) Uani 1 2 d S T P . .
F1 F 0.38641(16) 0.02940(12) 0.11872(10) 0.0164(2) Uani 1 1 d . . . . .
F4 F 1.20449(18) 0.66389(13) 0.06176(11) 0.0221(3) Uani 1 1 d . . . . .
F3 F 1.10174(17) 0.42547(13) 0.11082(11) 0.0208(2) Uani 1 1 d . . . . .
F2 F 0.86136(18) 0.57625(13) 0.09344(11) 0.0228(3) Uani 1 1 d . . . . .
O1 O 0.8586(2) 0.54097(15) 0.34280(14) 0.0227(3) Uani 1 1 d . . . . .
O2 O 0.3210(2) 0.25089(14) 0.28470(13) 0.0160(3) Uani 1 1 d . . . . .
O5 O 0.9668(2) 0.90046(16) 0.13991(15) 0.0234(3) Uani 1 1 d . . . . .
H5A H 0.952104 0.802961 0.133315 0.035 Uiso 1 1 d G . . . .
H5B H 1.092872 0.944834 0.135817 0.035 Uiso 1 1 d G . . . .
O3 O 0.1464(2) 0.37076(19) 0.39119(15) 0.0288(4) Uani 1 1 d . . . . .
N3 N 0.8003(2) 0.16774(17) 0.13117(14) 0.0126(3) Uani 1 1 d . . . . .
H3A H 0.734755 0.106593 0.051463 0.015 Uiso 1 1 calc GR . . . .
H3B H 0.866168 0.113943 0.174104 0.015 Uiso 1 1 calc GR . . . .
H3C H 0.897184 0.253999 0.130315 0.015 Uiso 1 1 calc GR . . . .
N1 N 0.7486(2) 0.41681(17) 0.29619(14) 0.0135(3) Uani 1 1 d . . . . .
O4 O 0.4358(2) 0.50500(17) 0.36488(17) 0.0338(4) Uani 1 1 d . . . . .
N5 N 0.3024(3) 0.3819(2) 0.34965(16) 0.0197(4) Uani 1 1 d . . . . .
N4 N 0.6668(2) 0.12966(17) 0.35479(15) 0.0129(3) Uani 1 1 d . . . . .
N2 N 0.4568(2) 0.30644(19) 0.06683(15) 0.0164(3) Uani 1 1 d . . . . .
H2A H 0.356657 0.224689 0.007528 0.020 Uiso 1 1 calc GR . . . .
H2B H 0.562568 0.344278 0.033716 0.020 Uiso 1 1 calc GR . . . .
H2C H 0.398045 0.382326 0.093986 0.020 Uiso 1 1 calc GR . . . .
C2 C 0.7858(3) 0.1453(3) 0.5690(2) 0.0245(5) Uani 1 1 d . . . . .
H2 H 0.831907 0.205931 0.654198 0.029 Uiso 1 1 calc R . . . .
C1 C 0.7334(3) 0.2121(2) 0.47638(18) 0.0178(4) Uani 1 1 d . . . . .
H1 H 0.744762 0.319641 0.499196 0.021 Uiso 1 1 calc R . . . .
C4 C 0.7012(3) -0.0953(2) 0.4118(2) 0.0259(5) Uani 1 1 d . . . . .
H4 H 0.688089 -0.203098 0.387198 0.031 Uiso 1 1 calc R . . . .
C5 C 0.6509(3) -0.0228(2) 0.3230(2) 0.0187(4) Uani 1 1 d . . . . .
H5 H 0.603901 -0.081789 0.237391 0.022 Uiso 1 1 calc R . . . .
C3 C 0.7704(3) -0.0110(3) 0.5362(2) 0.0274(5) Uani 1 1 d . . . . .
H3 H 0.806905 -0.059280 0.598271 0.033 Uiso 1 1 calc R . . . .
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'
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'
Si Si 0.0817 0.0704 '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 O2 81.94(5) . . ?
F1 Ru1 N3 86.36(5) . . ?
F1 Ru1 N4 86.92(5) . . ?
F1 Ru1 N2 85.07(6) . . ?
O2 Ru1 N3 168.17(5) . . ?
O2 Ru1 N4 87.79(5) . . ?
O2 Ru1 N2 89.69(6) . . ?
N3 Ru1 N4 89.83(6) . . ?
N3 Ru1 N2 91.05(6) . . ?
N1 Ru1 F1 176.76(6) . . ?
N1 Ru1 O2 99.15(6) . . ?
N1 Ru1 N3 92.62(6) . . ?
N1 Ru1 N4 96.16(7) . . ?
N1 Ru1 N2 91.88(7) . . ?
N2 Ru1 N4 171.87(6) . . ?
F4 Si1 F4 180.0 2_765 . ?
F4 Si1 F3 89.95(6) . 2_765 ?
F4 Si1 F3 90.05(6) 2_765 2_765 ?
F4 Si1 F3 89.95(6) 2_765 . ?
F4 Si1 F3 90.05(6) . . ?
F4 Si1 F2 90.46(6) 2_765 2_765 ?
F4 Si1 F2 89.54(6) 2_765 . ?
F4 Si1 F2 89.54(6) . 2_765 ?
F4 Si1 F2 90.46(6) . . ?
F3 Si1 F3 180.0 2_765 . ?
F2 Si1 F3 90.00(6) 2_765 2_765 ?
F2 Si1 F3 90.00(6) 2_765 . ?
F2 Si1 F3 90.00(6) . 2_765 ?
F2 Si1 F3 90.00(6) . . ?
F2 Si1 F2 180.0 2_765 . ?
N5 O2 Ru1 124.13(11) . . ?
O1 N1 Ru1 176.15(15) . . ?
O3 N5 O2 115.90(16) . . ?
O4 N5 O2 119.80(16) . . ?
O4 N5 O3 124.30(17) . . ?
C1 N4 Ru1 121.09(12) . . ?
C1 N4 C5 118.71(16) . . ?
C5 N4 Ru1 120.17(13) . . ?
C1 C2 C3 119.2(2) . . ?
N4 C1 C2 122.03(19) . . ?
C3 C4 C5 119.8(2) . . ?
N4 C5 C4 121.6(2) . . ?
C4 C3 C2 118.67(19) . . ?
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 1.9449(10) . ?
Ru1 O2 2.0685(12) . ?
Ru1 N3 2.0710(14) . ?
Ru1 N1 1.7272(15) . ?
Ru1 N4 2.0978(15) . ?
Ru1 N2 2.0903(15) . ?
Si1 F4 1.6846(11) 2_765 ?
Si1 F4 1.6846(11) . ?
Si1 F3 1.6938(11) 2_765 ?
Si1 F3 1.6938(11) . ?
Si1 F2 1.6937(11) . ?
Si1 F2 1.6937(11) 2_765 ?
O1 N1 1.1461(19) . ?
O2 N5 1.314(2) . ?
O3 N5 1.231(2) . ?
O4 N5 1.227(2) . ?
N4 C1 1.346(2) . ?
N4 C5 1.347(2) . ?
C2 C1 1.381(3) . ?
C2 C3 1.383(3) . ?
C4 C5 1.380(3) . ?
C4 C3 1.377(3) . ?
