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_7704554
_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         'C72 H66 B Fe Na O5 P2 Pt S2'
_chemical_formula_sum            'C72 H66 B Fe Na O5 P2 Pt S2'
_chemical_formula_weight         1422.04
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     intrinsic
_atom_sites_solution_secondary   difmap
_audit_creation_date             2019-09-17
_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                 106.0570(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.8886(6)
_cell_length_b                   33.2871(17)
_cell_length_c                   17.9102(9)
_cell_measurement_reflns_used    9780
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      50.358
_cell_measurement_theta_min      3.984
_cell_volume                     6238.3(6)
_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      150.0
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0834
_diffrn_reflns_av_unetI/netI     0.0522
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            59803
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        50.485
_diffrn_reflns_theta_max         50.485
_diffrn_reflns_theta_min         2.890
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.587
_exptl_absorpt_correction_T_max  0.7500
_exptl_absorpt_correction_T_min  0.5387
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.1232 before and 0.0859 after correction.
The Ratio of minimum to maximum transmission is 0.7183.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.514
_exptl_crystal_description       thin
_exptl_crystal_F_000             2880
_exptl_crystal_size_max          0.176
_exptl_crystal_size_mid          0.153
_exptl_crystal_size_min          0.109
_refine_diff_density_max         1.120
_refine_diff_density_min         -3.703
_refine_diff_density_rms         0.184
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.306
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     787
_refine_ls_number_reflns         6471
_refine_ls_number_restraints     365
_refine_ls_restrained_S_all      1.271
_refine_ls_R_factor_all          0.1125
_refine_ls_R_factor_gt           0.0961
_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^)+242.3684P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1992
_refine_ls_wR_factor_ref         0.2065
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5681
_reflns_number_total             6471
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01678k2.cif
_cod_data_source_block           lw089_3rdxtal_p21_c_acopy
_cod_depositor_comments
'Adding full bibliography for 7704546--7704563.cif.'
_cod_database_code               7704554
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.492
_shelx_estimated_absorpt_t_min   0.349
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C14-O5 \\sim C14A-O5 \\sim C13-O4 \\sim C13A-O4
 with sigma of 0.02
 C13-C14 \\sim C13A-C14A
 with sigma of 0.02
 C12-O4 \\sim C12A-O4 \\sim C11-O3 \\sim C11A-O3
 with sigma of 0.02
 C12-C11 \\sim C12A-C11A
 with sigma of 0.02
 O3-C10 \\sim O3-C10A \\sim O2-C9 \\sim O2-C9A
 with sigma of 0.02
 C10-C9 \\sim C10A-C9A
 with sigma of 0.02
3. Rigid bond restraints
 All non-hydrogen atoms
 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) \\sim Ueq, Uanis(C9A) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
Uanis(C14) = Uanis(C14A)
Uanis(C13) = Uanis(C13A)
Uanis(C12) = Uanis(C12A)
Uanis(C11) = Uanis(C11A)
Uanis(C9) = Uanis(C9A)
Uanis(C10) = Uanis(C10A)
5. Others
 Sof(C13A)=Sof(H13C)=Sof(H13D)=Sof(C14A)=Sof(H14C)=Sof(H14D)=1-FVAR(1)
 Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(C14)=Sof(H14A)=Sof(H14B)=FVAR(1)
 Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(C10A)=Sof(H10C)=Sof(H10D)=1-FVAR(2)
 Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(C10)=Sof(H10A)=Sof(H10B)=FVAR(2)
 Sof(C11A)=Sof(H11C)=Sof(H11D)=Sof(C12A)=Sof(H12C)=Sof(H12D)=1-FVAR(3)
 Sof(C11)=Sof(H11A)=Sof(H11B)=Sof(C12)=Sof(H12A)=Sof(H12B)=FVAR(3)
6.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C9A(H9AA,H9AB),
 C10A(H10C,H10D), C11(H11A,H11B), C12(H12A,H12B), C11A(H11C,H11D), C12A(H12C,
 H12D), C13(H13A,H13B), C14(H14A,H14B), C13A(H13C,H13D), C14A(H14C,H14D)
6.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C5(H5), C16(H16), C17(H17), C18(H18), C19(H19), C21(H21), C22(H22),
 C23(H23), C24(H24), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30), C32(H32),
  C33(H33), C34(H34), C35(H35), C36(H36), C38(H38), C39(H39), C40(H40),
 C41(H41), C42(H42), C44(H44), C45(H45), C46(H46), C47(H47), C48(H48), C50(H50),
  C51(H51), C52(H52), C53(H53), C54(H54), C56(H56), C57(H57), C58(H58),
 C59(H59), C60(H60), C62(H62), C63(H63), C64(H64), C65(H65), C66(H66), C68(H68),
  C69(H69), C70(H70), C71(H71), C72(H72)
;
_olex2_submission_special_instructions 'No special instructions were received'