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_7048326
_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 Os4 P8'
_chemical_formula_weight         3286.22
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_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                77.147(2)
_cell_angle_beta                 72.7960(10)
_cell_angle_gamma                89.845(2)
_cell_formula_units_Z            2
_cell_length_a                   16.5298(16)
_cell_length_b                   18.9862(19)
_cell_length_c                   24.131(2)
_cell_measurement_reflns_used    8774
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.43
_cell_measurement_theta_min      2.35
_cell_volume                     7036.9(11)
_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      100(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0288
_diffrn_reflns_av_unetI/netI     0.0600
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            37414
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         0.908
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    4.425
_exptl_absorpt_correction_T_max  0.64
_exptl_absorpt_correction_T_min  0.35
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS V2014/2 (Bruker AXS Inc.)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.551
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3240
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.110
_refine_diff_density_max         1.872
_refine_diff_density_min         -1.594
_refine_diff_density_rms         0.161
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1225
_refine_ls_number_reflns         24555
_refine_ls_number_restraints     29
_refine_ls_restrained_S_all      0.964
_refine_ls_R_factor_all          0.0689
_refine_ls_R_factor_gt           0.0475
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.8134P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1371
_refine_ls_wR_factor_ref         0.1545
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18117
_reflns_number_total             24555
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03962c2.cif
_cod_data_source_block           OsPPr3Cl2Agbim_dimer_100_sq
_cod_depositor_comments
'Adding full bibliography for 7048323--7048326.cif.'
_cod_original_cell_volume        7036.8(12)
_cod_database_code               7048326
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.332
_shelx_estimated_absorpt_t_max   0.642
_shelx_res_checksum              88533
_shelx_fab_checksum              6955