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_4346465
_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         'C48 H48 O12 Pd6 S12'
_chemical_formula_sum            'C48 H48 O12 Pd6 S12'
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_space_group_name_Hall           'P 2 2ab'
_space_group_name_H-M_alt        'P 21 21 2'
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_cell_length_a                   21.721(6)
_cell_length_b                   22.370(6)
_cell_length_c                   16.448(4)
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_cell_measurement_temperature    150(2)
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_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
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_diffrn_measurement_device_type  'Bruker APEX-II CCD'
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_diffrn_reflns_Laue_measured_fraction_full 0.996
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_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
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_diffrn_reflns_limit_k_min       -29
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_diffrn_source                   'fine focus sealed tube'
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_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5951
_exptl_absorpt_correction_type   multi-scan
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;
TITL JW016preSQP 21 21 2    R = 0.09
CELL   21.7210   22.3700   16.4480     90.00     90.00     90.00
SPGR P21212
C101 0.736 0.072 0.221 !      19.91 eA-3
C102 0.173 0.832 0.209 !      19.40 eA-3
C103 0.226 0.410 0.249 !      15.04 eA-3
C104 0.655 0.987 0.763 !      12.69 eA-3
C105 0.810 0.762 0.327 !       9.53 eA-3
C106 0.806 0.902 0.347 !       8.62 eA-3
C107 1.000 0.502 0.234 !       8.36 eA-3
C108 0.344 0.212 0.342 !       7.84 eA-3
C109 0.766 0.131 0.271 !       7.30 eA-3
C110 0.419 0.108 0.324 !       6.20 eA-3
C111 0.937 0.528 0.776 !       5.58 eA-3
C112 0.962 0.403 0.153 !       5.55 eA-3
C113 0.695 0.027 0.704 !       5.15 eA-3
C114 0.880 0.838 0.107 !       4.50 eA-3
C115 0.473 0.571 0.875 !       4.02 eA-3
C116 0.545 0.345 0.905 !       3.82 eA-3
C117 0.455 0.577 0.894 !       3.67 eA-3
C118 0.413 0.170 0.362 !       3.56 eA-3
C119 0.068 0.263 0.143 !       3.48 eA-3
C120 0.994 0.831 0.175 !       3.37 eA-3
C121 0.304 0.671 0.611 !       3.37 eA-3
C122 0.938 0.343 0.232 !       3.06 eA-3
C123 0.947 0.322 0.235 !       3.05 eA-3
C124 0.039 0.711 0.220 !       2.89 eA-3
C125 0.984 0.768 0.203 !       2.77 eA-3
C126 0.999 0.678 0.169 !       2.71 eA-3
C127 0.399 0.675 0.654 !       2.62 eA-3
C128 0.094 0.101 0.125 !       2.55 eA-3
C129 0.970 0.137 0.158 !       2.50 eA-3
C130 0.506 0.842 0.813 !       2.49 eA-3
C131 0.486 0.345 0.856 !       2.48 eA-3
C132 0.431 0.271 0.765 !       2.46 eA-3
C133 0.494 0.641 0.865 !       2.42 eA-3
C134 0.344 0.299 0.754 !       2.26 eA-3
C135 0.946 0.790 0.145 !       2.19 eA-3
C136 0.987 0.470 0.140 !       2.18 eA-3
C137 0.577 0.314 0.658 !       2.15 eA-3
C138 0.811 0.126 0.216 !       2.11 eA-3
C139 0.111 0.688 0.716 !       2.07 eA-3
C140 0.743 0.328 0.623 !       2.06 eA-3
Q141 0.032 0.480 0.564 !       2.00 eA-3
C142 0.016 0.170 0.254 !       1.99 eA-3
C143 0.430 0.641 0.688 !       1.99 eA-3
C144 0.233 0.924 0.170 !       1.94 eA-3
Q145 0.022 0.972 0.214 !       1.91 eA-3
C146 0.563 0.380 0.670 !       1.91 eA-3
C147 0.836 0.340 0.618 !       1.84 eA-3
C148 0.031 0.115 0.200 !       1.84 eA-3
C149 0.853 0.140 0.171 !       1.80 eA-3
C150 0.540 0.347 0.653 !       1.79 eA-3
C151 0.054 0.522 0.809 !       1.79 eA-3
C152 0.157 0.831 0.143 !       1.78 eA-3
C153 0.030 0.821 0.193 !       1.77 eA-3
Q154 0.344 0.377 0.756 !       1.77 eA-3
C155 0.016 0.098 0.223 !       1.77 eA-3
C156 0.039 0.621 0.231 !       1.75 eA-3
C157 0.383 0.618 0.842 !       1.75 eA-3
C158 0.721 0.594 0.748 !       1.74 eA-3
Q159 0.953 0.057 0.169 !       1.72 eA-3
Q160 0.062 0.537 0.875 !       1.71 eA-3
C161 0.155 0.099 0.177 !       1.70 eA-3
C162 0.994 0.784 0.263 !       1.70 eA-3
C163 0.640 0.332 0.748 !       1.70 eA-3
C164 0.766 0.540 0.831 !       1.70 eA-3
C165 0.892 0.467 0.815 !       1.68 eA-3
C166 0.538 0.895 0.747 !       1.68 eA-3
C167 0.976 0.467 0.814 !       1.68 eA-3
C168 0.486 0.990 0.315 !       1.67 eA-3
C169 0.017 0.753 0.231 !       1.66 eA-3
Q170 0.149 0.512 0.827 !       1.65 eA-3
C171 0.380 0.633 0.808 !       1.65 eA-3
Q172 0.585 0.221 0.736 !       1.65 eA-3
C173 0.062 0.881 0.201 !       1.65 eA-3
C174 0.788 0.963 0.328 !       1.64 eA-3
C175 0.829 0.516 0.823 !       1.62 eA-3
C176 0.021 0.061 0.212 !       1.62 eA-3
C177 0.367 0.605 0.734 !       1.60 eA-3
C178 0.576 0.939 0.781 !       1.60 eA-3
Q179 0.267 0.899 0.813 !       1.59 eA-3
Q180 0.987 0.071 0.215 !       1.58 eA-3
C181 0.477 0.731 0.861 !       1.58 eA-3
C182 0.892 0.447 0.172 !       1.57 eA-3
Q183 0.179 0.081 0.227 !       1.56 eA-3
C184 0.594 0.806 0.751 !       1.56 eA-3
C185 0.788 0.056 0.204 !       1.56 eA-3
C186 0.961 0.226 0.203 !       1.56 eA-3
C187 0.752 0.929 0.312 !       1.56 eA-3
C188 0.752 0.796 0.285 !       1.55 eA-3
C189 0.357 0.583 0.803 !       1.55 eA-3
C190 0.040 0.109 0.269 !       1.55 eA-3
C191 0.079 0.837 0.201 !       1.54 eA-3
C192 0.624 0.285 0.753 !       1.54 eA-3
C193 0.062 0.387 0.177 !       1.54 eA-3
C194 1.001 0.120 0.246 !       1.54 eA-3
C195 0.532 0.300 0.701 !       1.54 eA-3
C196 0.979 0.636 0.159 !       1.54 eA-3
C197 0.692 0.064 0.249 !       1.53 eA-3
C198 0.136 0.511 0.871 !       1.53 eA-3
C199 0.868 0.921 0.159 !       1.52 eA-3
;
_refine_diff_density_max         1.166
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_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.04(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     686
_refine_ls_number_reflns         18285
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0339
_refine_ls_R_factor_gt           0.0310
_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^)+(0.0525P)^2^+8.4559P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0852
_refine_ls_wR_factor_ref         0.0871
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_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                17294
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_reflns_threshold_expression     'I > 2\s(I)'
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_cod_data_source_block           jw016presq_sq
_cod_database_code               4346465
_shelx_estimated_absorpt_t_min   0.576
_shelx_estimated_absorpt_t_max   0.752
_shelxl_version_number           2013-3
_shelx_res_checksum              47537
_shelx_hkl_checksum              27214
_platon_squeeze_void_probe_radius 1.20
_shelx_fab_checksum              97472