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_7060498
_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       '\f and \w 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 \l/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+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.056
_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/[\s^2^(Fo^2^)+(0.0080P)^2^+0.4554P] where P=(Fo^2^+2Fc^2^)/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 > 2\s(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_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)
;
_shelx_res_checksum              847
_olex2_submission_special_instructions 'No special instructions were received'