New insights in the progressive ligand replacement from [Ru2Cl(O2CCH3)4]: synthetic strategies and variation of redox potentials and paramagnetic shifts
Inchausti, Almudena; Terán, Aarón; Manchado-Parra, Alberto; de Marcos-Galán, Alessandra; Perles, Josefina; Cortijo, Miguel; González-Prieto, Rodrigo; HERRERO (DOMINGUEZ), SANTIAGO; Jimenez-Aparicio, Reyes; Dalton Transactions  (2022) –; doi:10.1039/D2DT00909A

data_7710368
_publ_section_title
;
 New insights in the progressive ligand replacement from [Ru2Cl(O2CCH3)4]:
 synthetic strategies and variation of redox potentials and paramagnetic
 shifts
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT00909A
_journal_year                    2022
_chemical_formula_moiety         'C21 H24 Cl F2 N2 O7 Ru2 S, 2(C H2 Cl2)'
_chemical_formula_sum            'C23 H28 Cl5 F2 N2 O7 Ru2 S'
_chemical_formula_weight         893.92
_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     dual
_audit_creation_date             2022-02-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-05-03 deposited with the CCDC.	2022-05-27 downloaded from the CCDC.
;
_cell_angle_alpha                73.119(4)
_cell_angle_beta                 86.441(4)
_cell_angle_gamma                82.059(4)
_cell_formula_units_Z            2
_cell_length_a                   11.4157(13)
_cell_length_b                   11.6710(12)
_cell_length_c                   13.1768(12)
_cell_measurement_reflns_used    2284
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      20.114
_cell_measurement_theta_min      2.392
_cell_volume                     1663.4(3)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       'Bruker Instrument Service v2010.9.0.0'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_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      199.99
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0972
_diffrn_reflns_av_unetI/netI     0.0985
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            26102
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         2.564
_exptl_absorpt_coefficient_mu    1.425
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6440
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0745 before and 0.0645 after correction. The Ratio of minimum to maximum transmission is 0.8640. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.785
_exptl_crystal_description       ribbon
_exptl_crystal_F_000             886
_exptl_crystal_size_max          0.233
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.013
_refine_diff_density_max         0.595
_refine_diff_density_min         -0.582
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.968
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     384
_refine_ls_number_reflns         6066
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.968
_refine_ls_R_factor_all          0.0953
_refine_ls_R_factor_gt           0.0438
_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^)+(0.0262P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0715
_refine_ls_wR_factor_ref         0.0853
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3786
_reflns_number_total             6066
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00909a2.cif
_cod_data_source_block           atm210
_cod_database_code               7710368
_shelx_shelxl_version_number     2018/1
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C22(H22A,H22B), C23(H23A,H23B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C7(H7), C1(H1), C4(H4), C6(H6), C9(H9), C12(H12), C10(H10), C13(H13)
2.c Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C19(H19A,H19B,H19C), C15(H15A,H15B,H15C), C20(H20A,H20B,
 H20C), C21(H21A,H21B,H21C)
;
_olex2_submission_special_instructions 'No special instructions were received'