Redox, transmetalation, and stacking properties of tetrathiafulvalene-2,3,6,7-tetrathiolate bridged tin, nickel, and palladium compounds
Xie, Jiaze; Boyn, Jan-Niklas; Filatov, Alexander S.; McNeece, Andrew J.; Mazziotti, David A.; Anderson, John S.; Chemical Science 11 (2020) 1066–1078; doi:10.1039/C9SC04381K

data_1556882
_publ_section_title
;
 Redox, transmetalation, and stacking properties of
 tetrathiafulvalene-2,3,6,7-tetrathiolate bridged tin, nickel, and
 palladium compounds
;
_journal_issue                   4
_journal_name_full               'Chemical Science'
_journal_page_first              1066
_journal_page_last               1078
_journal_paper_doi               10.1039/C9SC04381K
_journal_volume                  11
_journal_year                    2020
_chemical_formula_moiety         'C74 H56 Fe2 P4 Pd2 S8, C32 H12 B F24'
_chemical_formula_sum            'C106 H68 B F24 Fe2 P4 Pd2 S8'
_chemical_formula_weight         2513.27
_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
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2019-10-17
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-12-10 deposited with the CCDC.	2019-12-13 downloaded from the CCDC.
;
_cell_angle_alpha                105.082(5)
_cell_angle_beta                 91.975(4)
_cell_angle_gamma                90.730(5)
_cell_formula_units_Z            2
_cell_length_a                   13.503(3)
_cell_length_b                   19.054(4)
_cell_length_c                   28.239(6)
_cell_measurement_reflns_used    9888
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22.31
_cell_measurement_theta_min      2.23
_cell_volume                     7009(3)
_computing_cell_refinement       'SAINT V.8.35A (Bruker AXS Inc., 2013)'
_computing_data_collection       'APEX3 v.2015.9-0 (Bruker AXS Inc., 2015)'
_computing_data_reduction        'SAINT V.8.35A (Bruker AXS Inc., 2013)'
_computing_molecular_graphics
;
OLEX2: a complete structure solution, refinement and analysis program 
Dolomanov et al., 2009

Mercury: visualization and analysis of crystal structures
Macrae, et al., 2006

O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann.
J. Appl. Cryst. (2009). 42, 339-341;

C. F. Macrae, P. R. Edgington, P. McCabe, E. Pidcock, G. P. Shields, R. Taylor,
M. Towler and J. van de Streek, J. Appl. Cryst. (2006). 39, 453-457.
;
_computing_publication_material
;
 APEX3 v.2015.5-2 (Bruker AXS Inc., 2015)
 OLEX2 (Dolomanov et al., 2009)
;
_computing_structure_refinement  'XL-2018/3 (Sheldrick, 2015b)'
_computing_structure_solution    'XT 2018/2 (Sheldrick, 2015a)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Bruker PHOTON 100'
_diffrn_detector_area_resol_mean 10.4167
_diffrn_detector_type            CMOS
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  mirrors
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1086
_diffrn_reflns_av_unetI/netI     0.1360
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            59637
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        22.364
_diffrn_reflns_theta_max         22.364
_diffrn_reflns_theta_min         2.145
_diffrn_source                   'micro-focus X-ray tube'
_diffrn_source_type              'INCOATEC ImuS'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.688
_exptl_absorpt_correction_T_max  0.7447
_exptl_absorpt_correction_T_min  0.5471
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. 
wR2(int) was 0.1169 before and 0.0751 after correction. 
The Ratio of minimum to maximum transmission is 0.7347. 
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.191
_exptl_crystal_description       plate
_exptl_crystal_F_000             2514
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.252
_refine_diff_density_min         -1.040
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1458
_refine_ls_number_reflns         17875
_refine_ls_number_restraints     754
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.1467
_refine_ls_R_factor_gt           0.0914
_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^)+(0.0120P)^2^+85.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1827
_refine_ls_wR_factor_ref         0.2038
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10448
_reflns_number_total             17875
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc04381k3.cif
_cod_data_source_block           mo_0835_jiaze_0m
_cod_depositor_comments
;Adding full bibliography for 1556876--1556883.cif.

 Adding full bibliography for 1556876--1556883.cif.
;
_cod_database_code               1556882
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.986
_shelx_estimated_absorpt_t_min   0.831
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C82-C79 \\sim C77-C81 \\sim C87-C90 \\sim C85-C89 \\sim C97-C95 \\sim C98-C93
\\sim C105-C103 \\sim C106-
 C101
 with sigma of 0.02
 F13-C106 \\sim F15-C106 \\sim F14-C106
 with sigma of 0.02
 F13-F15 \\sim F15-F14
 with sigma of 0.02
 F4-C82 \\sim F6-C82 \\sim F5-C82
 with sigma of 0.02
 F4-F6 \\sim F6-F5
 with sigma of 0.02
 C69-C68 \\sim C68-C67 \\sim C67-C66 \\sim C66-C65 \\sim C69-C65
 with sigma of 0.02
 C74-C70 \\sim C71-C70 \\sim C72-C71 \\sim C74-C73 \\sim C73-C72
 with sigma of 0.02
 F21A-C98 \\sim F21-C98 \\sim F19A-C98 \\sim F19-C98 \\sim F20A-C98 \\sim
F20-C98
 with sigma of 0.02
 F7A-C89 \\sim F7-C89 \\sim F9A-C89 \\sim F9-C89 \\sim F8A-C89 \\sim F8-C89
 with sigma of 0.02
 F4A-C82 \\sim F4-C82 \\sim F6A-C82 \\sim F6-C82 \\sim F5A-C82 \\sim F5-C82
 with sigma of 0.02
 F6A-F4A \\sim F4A-F5A
 with sigma of 0.02
 F6A-F4A \\sim F5A-F4A \\sim F5A-F6A
 with sigma of 0.02
 F13-C106 \\sim F13A-C106 \\sim F14-C106 \\sim F14A-C106 \\sim F15-C106 \\sim
F15A-C106
 with sigma of 0.02
 F15-F13 \\sim F13-F14
 with sigma of 0.02
 F13-F14 \\sim F13-F15 \\sim F14-F15
 with sigma of 0.02
 F18-C105 \\sim F16A-C105 \\sim F16-C105 \\sim F17A-C105 \\sim F17-C105 \\sim
F18A-C105
 with sigma of 0.02
 F18-F16 \\sim F16-F17
 with sigma of 0.02
 F16-F17 \\sim F16-F18 \\sim F17-F18
 with sigma of 0.02
 C99-B1 \\sim C75-B1 \\sim C91-B1 \\sim C83-B1
 with sigma of 0.02
3. Rigid bond restraints
 F7A, F8A, F9A, C89
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 F13, F14, F15, C106
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 F13A, F14A, F15A, C106
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
F7 \\sim F8 \\sim F9 \\sim F7A \\sim F8A \\sim F9A \\sim C89: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
F16A \\sim F17A \\sim F18A \\sim C105: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
F4A \\sim F5A \\sim F6A \\sim C82: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
F16 \\sim F18 \\sim C105 \\sim F17: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
F13 \\sim F14 \\sim F15 \\sim C106: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
F13A \\sim F14A \\sim F15A \\sim C106: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
Uanis(C25) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(F9A) = Uanis(F8)
5. Rigid body (RIGU) restrains
 F7A, F8A, F9A, C89
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F7A, F8A, F9A, C89, C85
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F13, F14, F15, C106
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F13A, F14A, F15A, C106
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F16, F17, F18, C105
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F4A, F5A, F6A, C82
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F4, F5, F6, C82
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C67, C68, C69, C65, C66
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C74, C70, C71, C72, C73
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C48, C47, C51, C52, C50, C49
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F16, F17, F18, C103, C105
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F16A, F17A, F18A, C103, C105
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F19, F20, F21, C98
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F19A, F20A, F21A, C98
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F16A, F17A, F18A, C105
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C40, C39, C38, C37, C36
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C25, C27, C29, C30, C28, C26
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C31, C33, C35, C34, C32
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C25, C26, C27, C28, C29, C30, P2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C99, C100, C101, C102, C103, C104
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(F19A)=Sof(F20A)=Sof(F21A)=1-FVAR(1)
 Sof(F19)=Sof(F20)=Sof(F21)=FVAR(1)
 Sof(F7A)=Sof(F8A)=Sof(F9A)=1-FVAR(2)
 Sof(F7)=Sof(F8)=Sof(F9)=FVAR(2)
 Sof(F4A)=Sof(F5A)=Sof(F6A)=1-FVAR(3)
 Sof(F4)=Sof(F5)=Sof(F6)=FVAR(3)
 Sof(F13A)=Sof(F14A)=Sof(F15A)=1-FVAR(4)
 Sof(F13)=Sof(F14)=Sof(F15)=FVAR(4)
 Sof(F16A)=Sof(F17A)=Sof(F18A)=1-FVAR(5)
 Sof(F16)=Sof(F17)=Sof(F18)=FVAR(5)
7.a Ternary CH refined with riding coordinates:
 C66(H66)
7.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C10(H10), C11(H11), C12(H12), C14(H14), C15(H15), C16(H16),
 C17(H17), C18(H18), C20(H20), 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), C37(H37), C38(H38), C40(H40), C42(H42), C43(H43), C44(H44),
  C45(H45), C46(H46), C47(H47), 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), C65(H65), C67(H67), C69(H69), C70(H70), C71(H71),
 C72(H72), C74(H74), C76(H76), C78(H78), C80(H80), C84(H84), C86(H86), C88(H88),
  C92(H92), C94(H94), C96(H96), C100(H100), C102(H102), C104(H104)
;
_shelx_res_checksum              17172
_shelx_fab_checksum              92481
_olex2_submission_special_instructions 'No special instructions were received'