Colorimetric fluoride detection in dimethyl sulfoxide using a heteroleptic ruthenium(ii) complex with amino and amide groups: X-ray crystallographic and spectroscopic analyses
Toyama, Mari; Hasegawa, Tomoki; Nagao, Noriharu; RSC Advances 12 (2022) 25227–25239; doi:10.1039/D2RA03593F

data_7245457
_publ_section_title
;
 Colorimetric fluoride detection in dimethyl sulfoxide using a
 heteroleptic ruthenium(ii) complex with amino and amide groups: X-ray
 crystallographic and spectroscopic analyses
;
_journal_issue                   39
_journal_name_full               'RSC Advances'
_journal_page_first              25227
_journal_page_last               25239
_journal_paper_doi               10.1039/D2RA03593F
_journal_volume                  12
_journal_year                    2022
_chemical_formula_moiety         'C30 H36 F2 N8 O3 Ru'
_chemical_formula_sum            'C30 H36 F2 N8 O3 Ru'
_chemical_formula_weight         695.73
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2022-04-19 deposited with the CCDC.	2022-08-21 downloaded from the CCDC.
;
_cell_angle_alpha                90.0000
_cell_angle_beta                 103.492(2)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   9.09482(19)
_cell_length_b                   23.8546(5)
_cell_length_c                   16.9383(4)
_cell_measurement_reflns_used    28137
_cell_measurement_temperature    173
_cell_measurement_theta_max      30.57
_cell_measurement_theta_min      2.10
_cell_volume                     3573.40(14)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'CrystalStructure 4.3'
_computing_publication_material  'CrystalStructure 4.3 (Rigaku, 2019)'
_computing_structure_refinement  'SHELXL Version 2014/7 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2014 (Burla, et al., 2014)'
_diffrn_ambient_temperature      173
_diffrn_detector_area_resol_mean 14.629
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.910
_diffrn_measurement_device_type  'Rigaku Mercury70'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0284
_diffrn_reflns_av_unetI/netI     0.0251
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.910
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            44447
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.910
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.351
_diffrn_reflns_theta_min         2.108
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.489
_exptl_absorpt_correction_T_max  0.976
_exptl_absorpt_correction_T_min  0.880
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.293
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1432.00
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.62
_refine_diff_density_min         -0.60
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_parameters     417
_refine_ls_number_reflns         9765
_refine_ls_number_restraints     8
_refine_ls_R_factor_all          0.0439
_refine_ls_R_factor_gt           0.0322
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0404P)^2^+2.3806P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0759
_refine_ls_wR_factor_ref         0.0807
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8060
_reflns_number_total             9765
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            d2ra03593f2.cif
_cod_data_source_block           '[Ru(Hdpa)2(H2pia)]F2_2(EtOH)'
_cod_database_code               7245457
_shelx_res_checksum              73
_shelx_fab_checksum              56974