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_7245458
_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         'C26 H29 Cl2 N8 O3.5 Ru'
_chemical_formula_sum            'C26 H29 Cl2 N8 O3.5 Ru'
_chemical_formula_weight         681.54
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2022-08-01 deposited with the CCDC.	2022-08-21 downloaded from the CCDC.
;
_cell_angle_alpha                99.448(2)
_cell_angle_beta                 102.616(2)
_cell_angle_gamma                99.741(2)
_cell_formula_units_Z            2
_cell_length_a                   9.1020(2)
_cell_length_b                   10.5348(3)
_cell_length_c                   17.4020(4)
_cell_measurement_reflns_used    8789
_cell_measurement_temperature    173
_cell_measurement_theta_max      74.78
_cell_measurement_theta_min      4.37
_cell_volume                     1569.40(7)
_computing_cell_refinement       'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)'
_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 5.811
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_device_type  'Rigaku XtaLAB PRO'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0880
_diffrn_reflns_av_unetI/netI     0.0758
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            15666
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.287
_diffrn_reflns_theta_min         4.355
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.967
_exptl_absorpt_correction_T_max  0.742
_exptl_absorpt_correction_T_min  0.472
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.20a (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.442
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             694.00
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_refine_diff_density_max         2.11
_refine_diff_density_min         -2.37
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_parameters     349
_refine_ls_number_reflns         6216
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0832
_refine_ls_R_factor_gt           0.0787
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.1211P)^2^+4.8886P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2069
_refine_ls_wR_factor_ref         0.2118
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5625
_reflns_number_total             6216
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            d2ra03593f2.cif
_cod_data_source_block           '[Ru(Hdpa)2(H2pia)]Cl2'
_cod_database_code               7245458
_shelx_res_checksum              90118
_shelx_fab_checksum              54017