An unusual Pd(III) oxidation state in the Pd-Cl chain complex with high thermal stability and electrical conductivity.
Mian, Mohammad Rasel; Wakizaka, Masanori; Yoshida, Takefumi; Iguchi, Hiroaki; Takaishi, Shinya; Afrin, Unjila; Miyamoto, Tatsuya; Okamoto, Hiroshi; Tanaka, Hisaaki; Kuroda, Shin-Ichi; Breedlove, Brian K.; Yamashita, Masahiro; Dalton transactions (Cambridge, England : 2003) 50 (2021) 1614–1619; doi:10.1039/d0dt03848b

data_7705963
_publ_section_title
;
 An unusual Pd(III) oxidation state in the Pd-Cl chain complex with high
 thermal stability and electrical conductivity.
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1614
_journal_page_last               1619
_journal_paper_doi               10.1039/d0dt03848b
_journal_volume                  50
_journal_year                    2021
_chemical_absolute_configuration rmad
_chemical_formula_sum            'C8 H24 Cl3 N4 O4 Pd'
_chemical_formula_weight         453.06
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2020-10-14 deposited with the CCDC.	2020-12-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.900(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   22.3546(18)
_cell_length_b                   4.9468(4)
_cell_length_c                   7.1164(6)
_cell_measurement_reflns_used    2696
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      34.12
_cell_measurement_theta_min      2.91
_cell_volume                     772.76(11)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Yadokari-XG (Wakita, Nemoto et al., 2009)'
_computing_publication_material  'Yadokari-XG (Wakita, Nemoto et al., 2009)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_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  0.0269
_diffrn_reflns_av_unetI/netI     0.0554
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            4273
_diffrn_reflns_point_group_measured_fraction_full 0.946
_diffrn_reflns_point_group_measured_fraction_max 0.842
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         34.127
_diffrn_reflns_theta_min         1.855
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.736
_exptl_absorpt_correction_T_max  0.950
_exptl_absorpt_correction_T_min  0.855
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2014/5
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.947
_exptl_crystal_description       needle
_exptl_crystal_F_000             458
_exptl_crystal_size_max          0.580
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.751
_refine_diff_density_min         -0.910
_refine_diff_density_rms         0.157
_refine_ls_abs_structure_details
;
 Flack x determined using 864 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.07(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     94
_refine_ls_number_reflns         2683
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0389
_refine_ls_R_factor_gt           0.0333
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0104P)^2^+1.6639P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0558
_refine_ls_wR_factor_ref         0.0576
_reflns_Friedel_coverage         0.599
_reflns_Friedel_fraction_full    0.885
_reflns_Friedel_fraction_max     0.697
_reflns_number_gt                2502
_reflns_number_total             2683
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03848b2.cif
_cod_data_source_block           20170923pdcldabdohcl2_100k_00m
_cod_depositor_comments
'Adding full bibliography for 7705963--7705964.cif.'
_cod_original_sg_symbol_H-M      'C 2'
_cod_database_code               7705963
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.432
_shelx_estimated_absorpt_t_max   0.950
_exptl_absorpt_special_details
;
SADABS-2014/5 - Bruker AXS area detector scaling and absorption correction.
wR2(int) was 0.0517 before and 0.0448 after correction.
;
_shelx_res_checksum              97887