Evidence of proton-coupled mixed-valency by electrochemical behavior on transition metal complex dimers bridged by two Ag<sup>+</sup> ions.
Tadokoro, Makoto; Isogai, Kazuo; Harada, Shohei; Kouchi, Takaya; Yamane, Takeshi; Sugaya, Tomoaki; Kamebuchi, Hajime; Dalton transactions (Cambridge, England : 2003) 48 (2019) 535–546; doi:10.1039/c8dt03962c

data_7048325
_publ_section_title
;
 Evidence of proton-coupled mixed-valency by electrochemical behavior on
 transition metal complex dimers bridged by two Ag<sup>+</sup> ions.
;
_journal_issue                   2
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              535
_journal_page_last               546
_journal_paper_doi               10.1039/c8dt03962c
_journal_volume                  48
_journal_year                    2019
_chemical_formula_sum            'C96 H184 Ag4 Cl8 N16 P8 Re4'
_chemical_formula_weight         3270.22
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2018-10-01 deposited with the CCDC.
2018-11-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.1348(13)
_cell_length_b                   37.674(3)
_cell_length_c                   23.0683(19)
_cell_measurement_reflns_used    9605
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      24.90
_cell_measurement_theta_min      2.24
_cell_volume                     14022(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'Bruker Helios multilayer confocal mirror'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0899
_diffrn_reflns_av_unetI/netI     0.1053
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       48
_diffrn_reflns_limit_k_min       -48
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            161225
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.494
_diffrn_reflns_theta_min         1.081
_diffrn_source                   'Bruker TXS fine-focus rotating anode'
_exptl_absorpt_coefficient_mu    4.270
_exptl_absorpt_correction_T_max  0.78
_exptl_absorpt_correction_T_min  0.69
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS V2014/2 (Bruker AXS Inc.)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.549
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             6464
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.060
_refine_diff_density_max         2.532
_refine_diff_density_min         -1.482
_refine_diff_density_rms         0.135
_refine_ls_abs_structure_details
; 
 Refined as an inversion twin. 
;
_refine_ls_abs_structure_Flack   0.198(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.936
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1214
_refine_ls_number_reflns         32143
_refine_ls_number_restraints     170
_refine_ls_restrained_S_all      0.940
_refine_ls_R_factor_all          0.1034
_refine_ls_R_factor_gt           0.0528
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0400P)^2^+0.8592P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1003
_refine_ls_wR_factor_ref         0.1100
_reflns_Friedel_coverage         0.948
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                17985
_reflns_number_total             32143
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03962c2.cif
_cod_data_source_block           RePPr3Cl2Agbim_dimer_400a_sq
_cod_depositor_comments
'Adding full bibliography for 7048323--7048326.cif.'
_cod_database_code               7048325
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.548
_shelx_estimated_absorpt_t_max   0.784
_shelx_res_checksum              48466
_shelx_fab_checksum              23178