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_7704546
_publ_section_title
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 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         'C35 H32 O2 P2 Pt S2'
_chemical_formula_sum            'C35 H32 O2 P2 Pt S2'
_chemical_formula_weight         805.75
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-08-02
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.4938(4)
_cell_length_b                   12.8694(4)
_cell_length_c                   21.4788(6)
_cell_measurement_reflns_used    9870
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      27.544
_cell_measurement_theta_min      3.041
_cell_volume                     3177.11(17)
_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 (Sheldrick, 2015)'
_diffrn_ambient_temperature      170.0
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_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  0.0276
_diffrn_reflns_av_unetI/netI     0.0343
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            36129
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.544
_diffrn_reflns_theta_min         3.040
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.680
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4836
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.1306 before and 0.0699 after correction.
The Ratio of minimum to maximum transmission is 0.6486.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.685
_exptl_crystal_description       block
_exptl_crystal_F_000             1592
_exptl_crystal_size_max          0.420
_exptl_crystal_size_mid          0.254
_exptl_crystal_size_min          0.241
_refine_diff_density_max         0.692
_refine_diff_density_min         -0.767
_refine_diff_density_rms         0.089
_refine_ls_abs_structure_details
;
 Flack x determined using 2868 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.010(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     409
_refine_ls_number_reflns         7216
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0263
_refine_ls_R_factor_gt           0.0233
_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^)+(0.0191P)^2^+2.7323P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0511
_refine_ls_wR_factor_ref         0.0524
_reflns_Friedel_coverage         0.771
_reflns_Friedel_fraction_full    0.970
_reflns_Friedel_fraction_max     0.971
_reflns_number_gt                6868
_reflns_number_total             7216
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01678k2.cif
_cod_data_source_block           lw069_1_0m
_cod_depositor_comments
'Adding full bibliography for 7704546--7704563.cif.'
_cod_database_code               7704546
_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
2. Uiso/Uaniso restraints and constraints
C12 \\sim C12A: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
C13 \\sim C13A \\sim C17 \\sim C17A: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C14 \\sim C14A \\sim C16 \\sim C16A: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C15 \\sim C15A: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
3. Same fragment restrains
{C12, C13, C14, C15, C16, C17} sigma for 1-2: 0.02, 1-3: 0.04
as
{C12A, C13A, C14A, C15A, C16A, C17A}
4. Others
 Fixed Sof: C12(0.5) C13(0.5) H13(0.5) C14(0.5) H14(0.5) C15(0.5) H15(0.5)
 C16(0.5) H16(0.5) C17(0.5) H17(0.5) C12A(0.5) C13A(0.5) H13A(0.5) C14A(0.5)
 H14A(0.5) C15A(0.5) H15A(0.5) C16A(0.5) H16A(0.5) C17A(0.5) H17A(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C10(H10A,H10B), C8(H8A,H8B), C9(H9A,H9B), C7(H7A,H7B)
5.b Aromatic/amide H refined with riding coordinates:
 C25(H25), C31(H31), C22(H22), C23(H23), C19(H19), C2(H2), C35(H35), C33(H33),
 C34(H34), C21(H21), C32(H32), C5(H5), C29(H29), C20(H20), C26(H26), C27(H27),
 C28(H28), C13(H13), C14(H14), C15(H15), C16(H16), C17(H17), C13A(H13A),
 C14A(H14A), C15A(H15A), C16A(H16A), C17A(H17A)
5.c Fitted hexagon refined as free rotating group:
 C12(C13,C14,C15,C16,C17), C12A(C13A,C14A,C15A,C16A,C17A)
;
_olex2_submission_special_instructions 'No special instructions were received'