Nitrosyl linkage photoisomerization in heteroleptic fluoride ruthenium complexes derived from labile nitrate precursors
Mikhailov, Artem A.; Komarov, Vladislav Yu.; Pishchur, Denis P.; Schaniel, Dominik; Kostin, Gennadiy A.; New Journal of Chemistry 45 (2021) 8192–8202; doi:10.1039/D1NJ01038G

data_7060496
_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       '\f and \w 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 \l/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+0.001xFc^2^\l^3^/sin(2\q)]^-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/[\s^2^(Fo^2^)+(0.0064P)^2^+1.8934P] where P=(Fo^2^+2Fc^2^)/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 > 2\s(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_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)
;
_shelx_res_checksum              69594
_olex2_submission_special_instructions 'No special instructions were received'