Phosphine control of the oxidative addition chemistry of tetrathiocins to palladium(0): characterization of mono-, di-, and hexanuclear palladium(II) dithiolate complexes.
Wrixon, Justin D.; Hayward, John J.; Rawson, Jeremy M.; Inorganic chemistry 54 (2015) 9384–9386; doi:10.1021/acs.inorgchem.5b01555

data_4346468
_publ_section_title
;
 Phosphine control of the oxidative addition chemistry of tetrathiocins to
 palladium(0): characterization of mono-, di-, and hexanuclear
 palladium(II) dithiolate complexes.
;
_journal_issue                   19
_journal_name_full               'Inorganic chemistry'
_journal_page_first              9384
_journal_page_last               9386
_journal_paper_doi               10.1021/acs.inorgchem.5b01555
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C42 H36 Fe O2 P2 Pd S2'
_chemical_formula_sum            'C42 H36 Fe O2 P2 Pd S2'
_chemical_formula_weight         861.02
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                64.850(4)
_cell_angle_beta                 76.688(4)
_cell_angle_gamma                76.738(4)
_cell_formula_units_Z            6
_cell_length_a                   15.232(5)
_cell_length_b                   21.963(7)
_cell_length_c                   22.470(7)
_cell_measurement_reflns_used    6717
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      20.18
_cell_measurement_theta_min      2.20
_cell_volume                     6547(4)
_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-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.531
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0751
_diffrn_reflns_av_unetI/netI     0.0790
_diffrn_reflns_Laue_measured_fraction_full 0.531
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            38788
_diffrn_reflns_point_group_measured_fraction_full 0.531
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         20.254
_diffrn_reflns_theta_min         1.533
_diffrn_source                   'fine focus sealed tube'
_exptl_absorpt_coefficient_mu    0.944
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_correction_T_min  0.582
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.310
_exptl_crystal_description       plate
_exptl_crystal_F_000             2628
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.020
_platon_squeeze_details
;
TITL JW010_preSP -1         R = 0.19
CELL   15.2320   21.9630   22.4700     64.85     76.69     76.74
SPGR P-1
C101 0.790 0.532 0.485 !      18.76 eA-3
C102 0.317 0.579 0.470 !      17.30 eA-3
C103 0.930 1.001 0.329 !      15.14 eA-3
C104 0.971 0.939 0.462 !      13.70 eA-3
C105 0.867 0.335 0.109 !      10.98 eA-3
C106 0.774 0.064 0.194 !       9.87 eA-3
C107 0.882 0.202 0.219 !       8.89 eA-3
C108 0.421 0.639 0.228 !       8.80 eA-3
C109 0.517 0.529 0.327 !       7.90 eA-3
C110 0.729 0.181 0.079 !       6.60 eA-3
C111 0.744 0.478 0.464 !       5.03 eA-3
C112 0.991 0.940 0.383 !       4.67 eA-3
C113 0.915 0.278 0.179 !       4.42 eA-3
C114 0.723 0.140 0.174 !       3.87 eA-3
C115 0.433 0.611 0.296 !       3.15 eA-3
C116 0.315 0.735 0.076 !       2.95 eA-3
C117 0.218 0.931 0.046 !       2.85 eA-3
C118 0.236 0.783 0.118 !       2.62 eA-3
C119 0.175 0.833 0.099 !       2.60 eA-3
C120 0.268 0.758 0.120 !       2.51 eA-3
C121 0.280 0.750 0.100 !       2.39 eA-3
C122 0.795 0.194 0.162 !       2.39 eA-3
C123 0.130 0.867 0.048 !       1.86 eA-3
C124 0.981 0.227 0.151 !       1.63 eA-3
C125 0.195 0.877 0.017 !       1.47 eA-3
C126 0.316 0.733 0.179 !       1.47 eA-3
C127 0.859 0.095 0.143 !       1.43 eA-3
Q128 0.588 0.591 0.204 !       1.43 eA-3
Q129 0.535 0.392 0.032 !       1.38 eA-3
C130 0.751 0.165 0.009 !       1.34 eA-3
C131 0.144 0.905 0.056 !       1.33 eA-3
C132 0.848 0.157 0.203 !       1.32 eA-3
Q133 0.529 0.843 0.221 !       1.31 eA-3
Q134 0.805 0.890 0.192 !       1.30 eA-3
Q135 0.592 0.803 0.257 !       1.30 eA-3
C136 0.987 0.196 0.225 !       1.29 eA-3
Q137 0.299 0.146 0.264 !       1.28 eA-3
Q138 0.871 0.829 0.212 !       1.24 eA-3
Q139 0.191 0.156 0.500 !       1.24 eA-3
C140 0.893 0.079 0.015 !       1.22 eA-3
C141 0.877 0.133 0.022 !       1.22 eA-3
Q142 0.032 0.474 0.287 !       1.22 eA-3
Q143 0.719 0.593 0.485 !       1.21 eA-3
C144 0.104 0.953 0.008 !       1.20 eA-3
C145 0.968 0.077 0.038 !       1.20 eA-3
C146 0.361 0.593 0.396 !       1.20 eA-3
Q147 0.067 0.983 0.118 !       1.19 eA-3
C148 0.293 0.850 0.093 !       1.19 eA-3
Q149 0.968 0.046 0.343 !       1.18 eA-3
C150 0.801 0.120 0.073 !       1.17 eA-3
Q151 0.532 0.084 0.118 !       1.17 eA-3
Q152 0.160 0.093 0.113 !       1.17 eA-3
Q153 0.428 0.163 0.249 !       1.17 eA-3
Q154 0.101 0.548 0.124 !       1.16 eA-3
C155 0.930 0.142 0.235 !       1.16 eA-3
C156 0.028 1.000 0.327 !       1.16 eA-3
Q157 0.666 0.829 0.078 !       1.16 eA-3
Q158 0.270 0.874 0.235 !       1.15 eA-3
Q159 0.781 0.071 0.276 !       1.15 eA-3
C160 0.786 0.306 0.121 !       1.14 eA-3
Q161 0.298 0.155 0.422 !       1.14 eA-3
Q162 0.719 0.828 0.302 !       1.14 eA-3
Q163 0.598 0.219 0.373 !       1.13 eA-3
C164 0.310 0.686 0.039 !       1.13 eA-3
Q165 1.006 0.966 0.093 !       1.13 eA-3
Q166 0.645 0.373 0.286 !       1.13 eA-3
C167 0.716 0.219 0.205 !       1.12 eA-3
Q168 0.118 0.386 0.057 !       1.12 eA-3
Q169 0.614 0.303 0.452 !       1.12 eA-3
Q170 0.548 0.112 0.368 !       1.11 eA-3
Q171 0.856 0.814 0.165 !       1.10 eA-3
C172 0.740 0.156 0.235 !       1.10 eA-3
Q173 0.655 0.398 0.065 !       1.10 eA-3
C174 0.351 0.641 0.415 !       1.09 eA-3
Q175 0.633 0.318 0.489 !       1.09 eA-3
Q176 0.843 0.343 0.046 !       1.09 eA-3
C177 0.037 0.951 0.492 !       1.09 eA-3
C178 0.587 0.491 0.297 !       1.09 eA-3
Q179 0.855 0.039 0.367 !       1.09 eA-3
Q180 0.679 0.172 0.334 !       1.08 eA-3
Q181 0.671 0.146 0.383 !       1.08 eA-3
C182 0.344 0.632 0.195 !       1.08 eA-3
C183 0.825 0.470 0.468 !       1.08 eA-3
Q184 0.061 0.953 0.188 !       1.08 eA-3
C185 0.058 1.001 0.016 !       1.07 eA-3
Q186 0.238 0.742 0.405 !       1.07 eA-3
Q187 0.012 0.954 0.322 !       1.07 eA-3
Q188 0.880 0.180 0.296 !       1.06 eA-3
C189 0.404 0.727 0.189 !       1.06 eA-3
Q190 0.885 0.384 0.335 !       1.06 eA-3
Q191 0.588 0.443 0.427 !       1.05 eA-3
C192 0.902 0.109 0.069 !       1.05 eA-3
C193 0.944 0.061 0.251 !       1.05 eA-3
Q194 0.922 0.976 0.212 !       1.04 eA-3
C195 0.323 0.788 0.054 !       1.04 eA-3
C196 0.284 0.781 0.016 !       1.04 eA-3
Q197 0.025 0.415 0.301 !       1.04 eA-3
C198 0.419 0.682 0.148 !       1.03 eA-3
C199 0.880 0.936 0.459 !       1.03 eA-3
;
_refine_diff_density_max         1.026
_refine_diff_density_min         -0.676
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     817
_refine_ls_number_reflns         12574
_refine_ls_number_restraints     646
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0956
_refine_ls_R_factor_gt           0.0759
_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^)+(0.0475P)^2^+81.3813P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1564
_refine_ls_wR_factor_ref         0.1651
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10043
_reflns_number_total             12574
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b01555_si_002.cif
_cod_data_source_block           jw010_presq_sq
_cod_original_cell_volume        6547(3)
_cod_database_code               4346468
_shelx_estimated_absorpt_t_min   0.785
_shelx_estimated_absorpt_t_max   0.981
_shelxl_version_number           2013-3
_shelx_res_checksum              73520
_shelx_hkl_checksum              97696
_platon_squeeze_void_probe_radius 1.20
_shelx_fab_checksum              38606