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_1556881
_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         'C38 H68 O4 S8 Sn2, 2(C32 H12 B F24)'
_chemical_formula_sum            'C102 H92 B2 F48 O4 S8 Sn2'
_chemical_formula_weight         2809.23
_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             2019-08-01
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-08-29 deposited with the CCDC.	2019-12-04 downloaded from the CCDC.
;
_cell_angle_alpha                88.537(3)
_cell_angle_beta                 88.979(3)
_cell_angle_gamma                69.195(3)
_cell_formula_units_Z            1
_cell_length_a                   12.9111(17)
_cell_length_b                   15.863(2)
_cell_length_c                   16.368(2)
_cell_measurement_reflns_used    9921
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.97
_cell_measurement_theta_min      2.49
_cell_volume                     3132.6(7)
_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 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  mirrors
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1152
_diffrn_reflns_av_unetI/netI     0.1068
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            32479
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.199
_diffrn_reflns_theta_max         25.199
_diffrn_reflns_theta_min         2.179
_diffrn_source                   'micro-focus X-ray tube'
_diffrn_source_type              'INCOATEC ImuS'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.649
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6298
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. 
wR2(int) was 0.0926 before and 0.0675 after correction. 
The Ratio of minimum to maximum transmission is 0.8451.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.489
_exptl_crystal_description       plate
_exptl_crystal_F_000             1406
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.397
_refine_diff_density_min         -0.982
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     815
_refine_ls_number_reflns         11153
_refine_ls_number_restraints     487
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.1437
_refine_ls_R_factor_gt           0.0977
_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^)+(0.0334P)^2^+40.6801P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2003
_refine_ls_wR_factor_ref         0.2241
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7626
_reflns_number_total             11153
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc04381k2.cif
_cod_data_source_block           mo_0792_jiaze__0m
_cod_depositor_comments
;Adding full bibliography for 1556876--1556883.cif.

 Adding full bibliography for 1556876--1556883.cif.
;
_cod_original_cell_volume        3132.5(7)
_cod_database_code               1556881
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.975
_shelx_estimated_absorpt_t_min   0.834
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C12-C13
 1.45 with sigma of 0.02
 C15-C14
 1.55 with sigma of 0.02
 C15A-C14A
 1.54 with sigma of 0.02
 F15A-C42
 1.34 with sigma of 0.02
 F4-C35
 1.34 with sigma of 0.02
 F5A-C35A = F4A-C35A = F6A-C35A
 1.34 with sigma of 0.02
 F14-C42
 1.34 with sigma of 0.02
 F13A-C42
 1.34 with sigma of 0.02
 Sn1-C12 \\sim Sn1-C4
 with sigma of 0.02
 C13-C14 \\sim C12-C13
 with sigma of 0.02
 C12-C13 \\sim C5-C4
 with sigma of 0.02
 C13-C14 \\sim C5-C6
 with sigma of 0.02
 C7-C6 \\sim C15-C14
 with sigma of 0.02
 Sn1-C12A \\sim Sn1-C12
 with sigma of 0.02
 C13A-C12A \\sim C12-C13
 with sigma of 0.02
 C13-C14 \\sim C13A-C14A
 with sigma of 0.02
 C15-C14 \\sim C15A-C14A
 with sigma of 0.02
 F13-C42 \\sim F13A-C42 \\sim F15-C42 \\sim F15A-C42 \\sim F14-C42 \\sim
F14A-C42
 with sigma of 0.02
 F4-C35 \\sim F5-C35 \\sim F6-C35
 with sigma of 0.02
 F4A-C35A \\sim F6A-C35A \\sim F5A-C35A
 with sigma of 0.02
 F13-F15 \\sim F15-F14 \\sim F13-F14
 with sigma of 0.02
 F14A-C42 \\sim F15A-C42 \\sim F13A-C42
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
F4 \\sim F5 \\sim F6 \\sim C35 \\sim F4 \\sim F5 \\sim F6 \\sim C35A \\sim F4A
\\sim F5A \\sim F6A \\sim C35A: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C12 \\sim C13 \\sim C14 \\sim C15 \\sim C12A \\sim C13A \\sim C14A \\sim C15A:
within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
O2 \\sim C16 \\sim C18 \\sim C19 \\sim C17A \\sim C17: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08
Uanis(F13A) = Uanis(F13)
Uanis(C35) = Uanis(C35A)
Uanis(C12A) = Uanis(C12)
Uanis(C15) = Uanis(C15A)
Uanis(F14A) = Uanis(F15)
Uanis(F14) = Uanis(F13A)
Uanis(F13) = Uanis(F15A)
Uanis(C14) = Uanis(C14A)
4. Rigid body (RIGU) restrains
 C42, F13, F14, F15, F13A, F14A, F15A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F4, F5, F6, C35, F4, F5, F6, C35A, F4A, F5A, F6A, C35A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C12, C13, C14, C15, C12A, C13A, C14A, C15A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O2, C16, C18, C19, C17A, C17
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O1, C8, C9, C10, C11
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C12A)=Sof(H12C)=Sof(H12D)=Sof(C13A)=Sof(H13C)=Sof(H13D)=Sof(C14A)=
 Sof(H14C)=Sof(H14D)=Sof(C15A)=Sof(H15D)=Sof(H15E)=Sof(H15F)=1-FVAR(1)
 Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(C14)=Sof(H14A)=
 Sof(H14B)=Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(H15C)=FVAR(1)
 Sof(C35A)=Sof(F4A)=Sof(F5A)=Sof(F6A)=1-FVAR(2)
 Sof(C35)=Sof(F4)=Sof(F5)=Sof(F6)=FVAR(2)
 Sof(F13A)=Sof(F14A)=Sof(F15A)=1-FVAR(3)
 Sof(F13)=Sof(F14)=Sof(F15)=FVAR(3)
 Sof(H16C)=Sof(H16D)=Sof(H18C)=Sof(H18D)=Sof(C17A)=Sof(H17C)=Sof(H17D)=1-FVAR(4)
 Sof(H16A)=Sof(H16B)=Sof(H18A)=Sof(H18B)=Sof(C17)=Sof(H17A)=Sof(H17B)=FVAR(4)
6.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,
 H10B), C11(H11A,H11B), C16(H16A,H16B), C16(H16C,H16D), C18(H18A,H18B),
 C18(H18C,H18D), C17(H17A,H17B), C17A(H17C,H17D), C19(H19A,H19B), C12(H12A,
 H12B), C13(H13A,H13B), C14(H14A,H14B), C12A(H12C,H12D), C13A(H13C,H13D),
 C14A(H14C,H14D)
6.b Aromatic/amide H refined with riding coordinates:
 C21(H21), C23(H23), C25(H25), C29(H29), C31(H31), C33(H33), C37(H37),
 C39(H39), C41(H41), C45(H45), C47(H47), C49(H49)
6.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C15(H15A,H15B,H15C), C15A(H15D,H15E,H15F)
;
_shelx_res_checksum              64055
_shelx_fab_checksum              25709
_olex2_submission_special_instructions 'No special instructions were received'