Interconversion between square-planar palladium(ii) and octahedral palladium(iv) centres in a sulfur-bridged trinuclear structure.
Kouno, Masahiro; Kuwamura, Naoto; Konno, Takumi; Chemical communications (Cambridge, England) 57 (2021) 1336–1339; doi:10.1039/d0cc07490j

data_7127714
_publ_section_title
;
 Interconversion between square-planar palladium(ii) and octahedral
 palladium(iv) centres in a sulfur-bridged trinuclear structure.
;
_journal_issue                   11
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              1336
_journal_page_last               1339
_journal_paper_doi               10.1039/d0cc07490j
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C18 H48 N6 Ni Rh2 S6, 4(N O3), 4(O)'
_chemical_formula_sum            'C18 H48 N10 O16 Pd Rh2 S6'
_chemical_formula_weight         1165.24
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2020-11-13 deposited with the CCDC.	2020-12-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.207(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.8176(3)
_cell_length_b                   12.4115(2)
_cell_length_c                   23.4669(4)
_cell_measurement_reflns_used    16448
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      35.77
_cell_measurement_theta_min      3.20
_cell_volume                     3992.71(14)
_computing_cell_refinement       'RAPID-AUTO (Rigaku Corporation)'
_computing_data_collection       'RAPID-AUTO (Rigaku Corporation)'
_computing_data_reduction        'RAPID-AUTO (Rigaku Corporation)'
_computing_molecular_graphics
'Yadokari-XG 2009 (Wakita Nemoto et al., 2009)'
_computing_publication_material
'Yadokari-XG 2009 (Wakita,Nemoto et al., 2009)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.924
_diffrn_measurement_device_type  'Rigaku R-AXIS VII'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0220
_diffrn_reflns_av_unetI/netI     0.0363
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.924
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            26493
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.924
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         35.844
_diffrn_reflns_theta_min         3.255
_exptl_absorpt_coefficient_mu    1.652
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7204
_exptl_absorpt_correction_type   multi-scans
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.938
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2344
_exptl_crystal_size_max          0.330
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.130
_refine_diff_density_max         0.955
_refine_diff_density_min         -1.339
_refine_diff_density_rms         0.131
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.363(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     479
_refine_ls_number_reflns         15431
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0258
_refine_ls_R_factor_gt           0.0239
_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^)+(0.0274P)^2^+5.9069P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0606
_refine_ls_wR_factor_ref         0.0632
_reflns_Friedel_coverage         0.999
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.924
_reflns_number_gt                14852
_reflns_number_total             15431
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc07490j2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7127714--7127717.cif.'
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               7127714
_shelx_estimated_absorpt_t_min   0.612
_shelx_estimated_absorpt_t_max   0.814
_shelxl_version_number           2013-4
_shelx_res_checksum              30685
_shelx_hkl_checksum              16456