Oxidative addition of tetrathiocins to palladium(0) and platinum(0): a route to dithiolate coordination complexes.
Watanabe, Lara K.; Wrixon, Justin D.; Ahmed, Zeinab S.; Hayward, John J.; Abbasi, Parisa; Pilkington, Melanie; Macdonald, Charles L. B.; Rawson, Jeremy M.; Dalton transactions (Cambridge, England : 2003) 49 (2020) 9086–9093; doi:10.1039/d0dt01678k

data_7704550
_publ_section_title
;
 Oxidative addition of tetrathiocins to palladium(0) and platinum(0): a
 route to dithiolate coordination complexes.
;
_journal_issue                   26
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9086
_journal_page_last               9093
_journal_paper_doi               10.1039/d0dt01678k
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety
'C40 H42 Na O5 P2 Pt S2, C24 H20 B, 2(C H2 Cl2)'
_chemical_formula_sum            'C66 H66 B Cl4 Na O5 P2 Pt S2'
_chemical_formula_weight         1435.93
_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
_audit_creation_date             2019-09-06
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-12-13 deposited with the CCDC.	2020-05-25 downloaded from the CCDC.
;
_cell_angle_alpha                80.747(4)
_cell_angle_beta                 78.054(2)
_cell_angle_gamma                66.431(3)
_cell_formula_units_Z            2
_cell_length_a                   13.0406(8)
_cell_length_b                   16.0671(16)
_cell_length_c                   16.7995(11)
_cell_measurement_reflns_used    9432
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.532
_cell_measurement_theta_min      3.146
_cell_volume                     3144.4(4)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      149.99
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0250
_diffrn_reflns_av_unetI/netI     0.0330
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            37422
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.530
_diffrn_reflns_theta_min         2.941
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.575
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6014
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.0644 before and 0.0409 after correction.
The Ratio of minimum to maximum transmission is 0.8066.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.517
_exptl_crystal_description       block
_exptl_crystal_F_000             1452
_exptl_crystal_size_max          0.237
_exptl_crystal_size_mid          0.228
_exptl_crystal_size_min          0.118
_refine_diff_density_max         2.209
_refine_diff_density_min         -1.181
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.131
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     762
_refine_ls_number_reflns         14041
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      1.133
_refine_ls_R_factor_all          0.0416
_refine_ls_R_factor_gt           0.0319
_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^)+(0.0193P)^2^+6.3009P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0658
_refine_ls_wR_factor_ref         0.0712
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12356
_reflns_number_total             14041
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01678k2.cif
_cod_data_source_block           lw088_1_p1
_cod_depositor_comments
'Adding full bibliography for 7704546--7704563.cif.'
_cod_database_code               7704550
_shelx_shelxl_version_number     2018/1
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
2. Restrained distances
 O2-C9 \\sim O2A-C9A \\sim O3-C10 \\sim O3-C10A \\sim O3-C11 \\sim O3A-C11A
\\sim O4-C12 \\sim O4-C12A
 with sigma of 0.02
 C11-C12 \\sim C11A-C12A \\sim C9-C10 \\sim C9A-C10A \\sim C11-C12 \\sim
C11A-C12A
 with sigma of 0.02
 C65-Cl2 \\sim C65-Cl2A
 with sigma of 0.02
3. Rigid bond restraints
 C41, C42, C43, C44, C45, C46
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(C9) = Uanis(C9A)
Uanis(C10) = Uanis(C10A)
Uanis(C11) = Uanis(C11A)
Uanis(C12) = Uanis(C12A)
Uanis(C8) = Uanis(C8A)
Uanis(Cl2) = Uanis(Cl2A)
Uanis(C65) = Uanis(C65A)
Uanis(C9) = Uanis(C9A) = Uanis(C10) = Uanis(C10A)
Uanis(O2) = Uanis(O2A)
Uanis(O3) = Uanis(O3A)
5. Others
 Sof(H7BC)=Sof(H7BD)=Sof(C8A)=Sof(H8AA)=Sof(H8AB)=Sof(O2A)=Sof(C9A)=Sof(H9AA)=
 Sof(H9AB)=Sof(C10A)=Sof(H10C)=Sof(H10D)=Sof(O3A)=Sof(C11A)=Sof(H11C)=Sof(H11D)=
 Sof(C12A)=Sof(H12C)=Sof(H12D)=1-FVAR(1)
 Sof(H7AA)=Sof(H7AB)=Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(O2)=Sof(C9)=Sof(H9A)=
 Sof(H9B)=Sof(C10)=Sof(H10A)=Sof(H10B)=Sof(O3)=Sof(C11)=Sof(H11A)=Sof(H11B)=
 Sof(C12)=Sof(H12A)=Sof(H12B)=FVAR(1)
 Sof(C65A)=Sof(H65C)=Sof(H65D)=Sof(Cl2A)=1-FVAR(2)
 Sof(C65)=Sof(H65A)=Sof(H65B)=Sof(Cl2)=FVAR(2)
6.a Secondary CH2 refined with riding coordinates:
 C7(H7AA,H7AB), C7(H7BC,H7BD), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B),
 C11(H11A,H11B), C12(H12A,H12B), C8A(H8AA,H8AB), C9A(H9AA,H9AB), C10A(H10C,
 H10D), C11A(H11C,H11D), C12A(H12C,H12D), C13(H13A,H13B), C14(H14A,H14B),
 C15(H15A,H15B), C16(H16A,H16B), C65(H65A,H65B), C65A(H65C,H65D), C66(H66A,H66B)
6.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C5(H5), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C24(H24),
 C25(H25), C26(H26), C27(H27), C28(H28), C30(H30), C31(H31), C32(H32), C33(H33),
  C34(H34), C36(H36), C37(H37), C38(H38), C39(H39), C40(H40), C42(H42),
 C43(H43), C44(H44), C45(H45), C46(H46), C48(H48), C49(H49), C50(H50), C51(H51),
  C52(H52), C54(H54), C55(H55), C56(H56), C57(H57), C58(H58), C60(H60),
 C61(H61), C62(H62), C63(H63), C64(H64)
;
_olex2_submission_special_instructions 'No special instructions were received'