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_7060497
_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         'C5 H13 F N4 O2 Ru, 2(Cl O4)'
_chemical_formula_sum            'C5 H13 Cl2 F N4 O10 Ru'
_chemical_formula_weight         480.16
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 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                90
_cell_angle_beta                 104.729(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.3073(8)
_cell_length_b                   8.3396(3)
_cell_length_c                   10.2007(4)
_cell_measurement_reflns_used    7258
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      31.45
_cell_measurement_theta_min      2.30
_cell_volume                     1506.22(10)
_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      150.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_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  0.0513
_diffrn_reflns_av_unetI/netI     0.0442
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            22377
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.501
_diffrn_reflns_theta_min         2.301
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.465
_exptl_absorpt_correction_T_max  0.9706
_exptl_absorpt_correction_T_min  0.7730
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0868 before and 0.0625 after correction.
The Ratio of minimum to maximum transmission is 0.7964.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.117
_exptl_crystal_description       plate
_exptl_crystal_F_000             952
_exptl_crystal_size_max          0.284
_exptl_crystal_size_mid          0.145
_exptl_crystal_size_min          0.091
_refine_diff_density_max         0.611
_refine_diff_density_min         -0.745
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         5005
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.123
_refine_ls_R_factor_all          0.0489
_refine_ls_R_factor_gt           0.0404
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0133P)^2^+2.9918P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0785
_refine_ls_wR_factor_ref         0.0821
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4251
_reflns_number_total             5005
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj01038g2.cif
_cod_data_source_block           ru
_cod_depositor_comments
'Adding full bibliography for 7060496--7060499.cif.'
_cod_database_code               7060497
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.878
_shelx_estimated_absorpt_t_min   0.681
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H,H) groups, All O(H,H) groups
2. Others
 Sof(O7)=Sof(O9)=Sof(O8)=1-FVAR(1)
 Sof(O12)=Sof(O11)=Sof(O13)=FVAR(1)
3.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C5(H5), C4(H4), C3(H3), C2(H2)
3.b Idealised Me refined as rotating group:
 N3(H3A,H3B,H3C), N2(H2C,H2D,H2E)
;
_shelx_res_checksum              18494
_olex2_submission_special_instructions 'No special instructions were received'