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_7704562
_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         'C33 H28 O2 P2 Pt S2'
_chemical_formula_sum            'C33 H28 O2 P2 Pt S2'
_chemical_formula_weight         777.70
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-07-26
_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                 97.1010(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.1176(4)
_cell_length_b                   12.7702(5)
_cell_length_c                   20.8750(9)
_cell_measurement_reflns_used    9962
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      25.43
_cell_measurement_theta_min      3.19
_cell_volume                     2941.0(2)
_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      169.99
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_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  0.0650
_diffrn_reflns_av_unetI/netI     0.0314
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            49441
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.433
_diffrn_reflns_theta_min         2.987
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.052
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5869
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.0921 before and 0.0697 after correction.
The Ratio of minimum to maximum transmission is 0.7876.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.756
_exptl_crystal_description       'thin needle'
_exptl_crystal_F_000             1528
_exptl_crystal_size_max          0.387
_exptl_crystal_size_mid          0.086
_exptl_crystal_size_min          0.016
_refine_diff_density_max         1.227
_refine_diff_density_min         -0.869
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         5420
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.116
_refine_ls_R_factor_all          0.0392
_refine_ls_R_factor_gt           0.0268
_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^)+(0.0042P)^2^+8.3249P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0478
_refine_ls_wR_factor_ref         0.0519
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4581
_reflns_number_total             5420
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01678k2.cif
_cod_data_source_block           lw070_p21_n_a
_cod_depositor_comments
'Adding full bibliography for 7704546--7704563.cif.'
_cod_database_code               7704562
_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.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C8(H8A,H8B), C7(H7A,H7B)
2.b Aromatic/amide H refined with riding coordinates:
 C33(H33), C15(H15), C21(H21), C32(H32), C11(H11), C2(H2), C17(H17), C5(H5),
 C13(H13), C20(H20), C18(H18), C29(H29), C14(H14), C12(H12), C23(H23), C31(H31),
  C19(H19), C27(H27), C30(H30), C25(H25), C26(H26), C24(H24)
;
_olex2_submission_special_instructions 'No special instructions were received'