#------------------------------------------------------------------------------
#$Date: 2021-06-05 21:22:54 +0200 (Sat 05 de Jun de 2021) $
#$Revision: 266148 $
#$URL: svn://www.crystallography.net/cod/cif/7/06/04/7060496.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_7060496
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         'F H10 N3 O3 Ru, F6 Si'
_chemical_formula_sum            'F7 H10 N3 O3 Ru Si'
_chemical_formula_weight         362.27
_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'
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.2150(5)
_cell_length_b                   7.7578(3)
_cell_length_c                   6.2397(2)
_cell_measurement_reflns_used    3247
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.63
_cell_measurement_theta_min      3.38
_cell_volume                     930.13(5)
_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 (Sheldrick, 2015)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_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  0.0238
_diffrn_reflns_av_unetI/netI     0.0248
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            4440
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.659
_diffrn_reflns_theta_min         2.120
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.924
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.5969
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0776 before and 0.0348 after correction.
The Ratio of minimum to maximum transmission is 0.8002.
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.587
_exptl_crystal_description       block
_exptl_crystal_F_000             704
_exptl_crystal_size_max          0.388
_exptl_crystal_size_mid          0.369
_exptl_crystal_size_min          0.194
_refine_diff_density_max         0.418
_refine_diff_density_min         -0.889
_refine_diff_density_rms         0.105
_refine_ls_extinction_coef       0.0028(4)
_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   1.262
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     82
_refine_ls_number_reflns         1406
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.262
_refine_ls_R_factor_all          0.0284
_refine_ls_R_factor_gt           0.0272
_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)+(0.0064P)²+1.8934P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0542
_refine_ls_wR_factor_ref         0.0546
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1370
_reflns_number_total             1406
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1nj01038g2.cif
_cod_data_source_block           artam2f32hf_150k
_cod_depositor_comments
'Adding full bibliography for 7060496--7060499.cif.'
_cod_database_code               7060496
_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   0.707
_shelx_estimated_absorpt_t_min   0.522
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H,H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Rotating group:
 O2(H2A,H2B)
2.b Idealised Me refined as rotating group:
 N2(H2C,H2D,H2E)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-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 0.14824(2) 0.750000 0.65153(4) 0.00823(9) Uani 1 2 d S T P . .
Si1 Si 0.40105(4) 0.750000 0.77827(14) 0.00843(17) Uani 1 2 d S T P . .
F5 F 0.34691(10) 0.750000 0.9971(3) 0.0129(4) Uani 1 2 d S T P . .
F1 F 0.19900(10) 0.750000 0.9158(3) 0.0149(4) Uani 1 2 d S T P . .
F4 F 0.45339(10) 0.750000 0.5628(3) 0.0146(4) Uani 1 2 d S T P . .
F2 F 0.35011(7) 0.9034(2) 0.6651(2) 0.0186(3) Uani 1 1 d . . . . .
F3 F 0.44902(7) 0.9027(2) 0.8925(2) 0.0176(3) Uani 1 1 d . . . . .
O2 O 0.21917(8) 0.9365(2) 0.5442(3) 0.0159(4) Uani 1 1 d . . . . .
H2A H 0.256497 0.939018 0.627695 0.024 Uiso 1 1 d GR . . . .
H2B H 0.201227 1.041097 0.559201 0.024 Uiso 1 1 d GR . . . .
O1 O 0.07088(14) 0.750000 0.2561(4) 0.0193(5) Uani 1 2 d S T P . .
N2 N 0.08700(10) 0.5618(3) 0.7859(3) 0.0126(4) Uani 1 1 d . . . . .
H2C H 0.079888 0.476085 0.688781 0.015 Uiso 1 1 calc GR . . . .
H2D H 0.045335 0.607931 0.824888 0.015 Uiso 1 1 calc GR . . . .
H2E H 0.108638 0.517958 0.903652 0.015 Uiso 1 1 calc GR . . . .
N1 N 0.10169(14) 0.750000 0.4121(5) 0.0125(5) 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
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'
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 86.79(6) . 7_575 ?
F1 Ru1 O2 86.79(6) . . ?
F1 Ru1 N2 86.58(7) . 7_575 ?
F1 Ru1 N2 86.58(7) . . ?
O2 Ru1 O2 87.24(10) 7_575 . ?
N2 Ru1 O2 173.15(7) . . ?
N2 Ru1 O2 173.15(7) 7_575 7_575 ?
N2 Ru1 O2 90.70(8) 7_575 . ?
N2 Ru1 O2 90.70(8) . 7_575 ?
N2 Ru1 N2 90.60(12) 7_575 . ?
N1 Ru1 F1 179.69(11) . . ?
N1 Ru1 O2 93.43(8) . 7_575 ?
N1 Ru1 O2 93.43(8) . . ?
N1 Ru1 N2 93.21(8) . . ?
N1 Ru1 N2 93.21(8) . 7_575 ?
F4 Si1 F5 179.49(11) . . ?
F4 Si1 F2 90.70(8) . . ?
F4 Si1 F2 90.70(8) . 7_575 ?
F2 Si1 F5 88.93(7) . . ?
F2 Si1 F5 88.93(8) 7_575 . ?
F2 Si1 F2 89.19(12) 7_575 . ?
F3 Si1 F5 89.71(7) 7_575 . ?
F3 Si1 F5 89.71(7) . . ?
F3 Si1 F4 90.65(8) 7_575 . ?
F3 Si1 F4 90.65(8) . . ?
F3 Si1 F2 178.39(9) . 7_575 ?
F3 Si1 F2 89.92(8) 7_575 7_575 ?
F3 Si1 F2 178.39(9) 7_575 . ?
F3 Si1 F2 89.92(8) . . ?
F3 Si1 F3 90.93(12) . 7_575 ?
O1 N1 Ru1 179.6(3) . . ?
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 1.9160(19) . ?
Ru1 O2 2.0977(17) 7_575 ?
Ru1 O2 2.0977(17) . ?
Ru1 N2 2.0543(19) 7_575 ?
Ru1 N2 2.0543(19) . ?
Ru1 N1 1.741(3) . ?
Si1 F5 1.717(2) . ?
Si1 F4 1.679(2) . ?
Si1 F2 1.6949(16) 7_575 ?
Si1 F2 1.6950(16) . ?
Si1 F3 1.6616(15) 7_575 ?
Si1 F3 1.6616(15) . ?
O1 N1 1.139(4) . ?
