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_1556877
_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         'C56 H64 Fe2 O2 S8 Sn2, 2(C32 H12 B F24)'
_chemical_formula_sum            'C120 H88 B2 F48 Fe2 O2 S8 Sn2'
_chemical_formula_weight         3101.08
_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     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                90
_cell_angle_beta                 107.358(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.734(2)
_cell_length_b                   31.568(5)
_cell_length_c                   18.543(3)
_cell_measurement_reflns_used    9904
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      13.95
_cell_measurement_theta_min      2.30
_cell_volume                     7115(2)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2016)'
_computing_data_collection       'APEX3 v.2015.9-0 (Bruker AXS Inc., 2015)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 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    'XT 2014/5 (Sheldrick, 2015a)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Pilatus1M(CdTe) pixel array detector'
_diffrn_detector_area_resol_mean 30
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'three-circle diffractometer'
_diffrn_measurement_method       'phi rotation'
_diffrn_radiation_collimation    '0.2 mm sinlge-pinhole'
_diffrn_radiation_monochromator  'Si(111) & Si(311)'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.41328
_diffrn_reflns_av_R_equivalents  0.1297
_diffrn_reflns_av_unetI/netI     0.0798
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            150144
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        14.357
_diffrn_reflns_theta_max         14.380
_diffrn_reflns_theta_min         0.750
_diffrn_source                   synchrotron
_diffrn_source_type
'Insertion Device, Station 15 ID-B, APS, Argonne Nat'l Lab'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.562
_exptl_absorpt_correction_T_max  0.7438
_exptl_absorpt_correction_T_min  0.5786
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. 
wR2(int) was 0.1262 before and 0.0804 after correction. 
The Ratio of minimum to maximum transmission is 0.7779. 
;
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.448
_exptl_crystal_description       block
_exptl_crystal_F_000             3092
_exptl_crystal_size_max          0.001
_exptl_crystal_size_mid          0.001
_exptl_crystal_size_min          0.001
_refine_diff_density_max         1.074
_refine_diff_density_min         -0.742
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     991
_refine_ls_number_reflns         12839
_refine_ls_number_restraints     728
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.1035
_refine_ls_R_factor_gt           0.0678
_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^)+(0.0740P)^2^+14.7827P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1719
_refine_ls_wR_factor_ref         0.1966
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8348
_reflns_number_total             12839
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc04381k2.cif
_cod_data_source_block           1
_cod_depositor_comments
;Adding full bibliography for 1556876--1556883.cif.

 Adding full bibliography for 1556876--1556883.cif.
;
_cod_original_cell_volume        7114(2)
_cod_database_code               1556877
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.999
_shelx_estimated_absorpt_t_min   0.999
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C22-C21 \\sim C23-C22 \\sim C23-C24 \\sim C20-C24 \\sim C20-C21
 with sigma of 0.02
 C23A-C24A \\sim C24A-C20A \\sim C23A-C22A \\sim C20A-C21A \\sim C22A-C21A
 with sigma of 0.02
3. Restrained planarity
 C20, C21, C22, C23, C24
 with sigma of 0.1
 C20A, C21A, C22A, C23A, C24A
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
O1 \\sim C12 \\sim C19 \\sim C18 \\sim C17 \\sim C16 \\sim C15 \\sim C14 \\sim
C20 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25 \\sim C26 \\sim C27 \\sim
C28 \\sim C29 \\sim Fe1: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
Fe1A \\sim O1A \\sim C12A \\sim C14A \\sim C15A \\sim C16A \\sim C17A \\sim
C18A \\sim C19A \\sim C20A \\sim C21A \\sim C22A \\sim C23A \\sim C24A \\sim
C25A \\sim C26A \\sim C27A \\sim C28A \\sim C29A: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08
Uanis(Fe1A) = Uanis(Fe1)
Uanis(O1A) = Uanis(O1)
5. Rigid body (RIGU) restrains
 O1, C12, C19, C18, C17, C16, C15, C14, C20, C21, C22, C23, C24, C25, C26, C27,
  C28, C29, Fe1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Fe1A, O1A, C12A, C14A, C15A, C16A, C17A, C18A, C19A, C20A, C21A, C22A, C23A,
 C24A, C25A, C26A, C27A, C28A, C29A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(Fe1A)=Sof(O1A)=Sof(C12A)=Sof(C14A)=Sof(H14A)=Sof(C15A)=Sof(H15A)=
 Sof(C16A)=Sof(H16A)=Sof(C17A)=Sof(H17A)=Sof(C18A)=Sof(H18A)=Sof(C19A)=
 Sof(C20A)=Sof(H20A)=Sof(C21A)=Sof(H21A)=Sof(C22A)=Sof(H22A)=Sof(C23A)=
 Sof(H23A)=Sof(C24A)=Sof(C25A)=Sof(H25A)=Sof(C26A)=Sof(H26A)=Sof(C27A)=
 Sof(H27A)=Sof(C28A)=Sof(H28A)=Sof(C29A)=Sof(H29A)=1-FVAR(1)
 Sof(Fe1)=Sof(O1)=Sof(C12)=Sof(C19)=Sof(C18)=Sof(H18)=Sof(C17)=Sof(H17)=
 Sof(C16)=Sof(H16)=Sof(C15)=Sof(H15)=Sof(C14)=Sof(H14)=Sof(C20)=Sof(C21)=
 Sof(H21)=Sof(C22)=Sof(H22)=Sof(C23)=Sof(H23)=Sof(C24)=Sof(H24)=Sof(C25)=
 Sof(H25)=Sof(C26)=Sof(H26)=Sof(C27)=Sof(H27)=Sof(C28)=Sof(H28)=Sof(C29)=
 Sof(H29)=FVAR(1)
7.a Ternary CH refined with riding coordinates:
 C24(H24), C20A(H20A), C21A(H21A)
7.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B)
7.c Aromatic/amide H refined with riding coordinates:
 C31(H31), C33(H33), C35(H35), C39(H39), C41(H41), C43(H43), C47(H47),
 C49(H49), C51(H51), C55(H55), C57(H57), C59(H59), C18(H18), C17(H17), C16(H16),
  C15(H15), C14(H14), C21(H21), C22(H22), C23(H23), C25(H25), C26(H26),
 C27(H27), C28(H28), C29(H29), C14A(H14A), C15A(H15A), C16A(H16A), C17A(H17A),
 C18A(H18A), C22A(H22A), C23A(H23A), C25A(H25A), C26A(H26A), C27A(H27A),
 C28A(H28A), C29A(H29A)
7.d Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C8(H8A,H8B,H8C)
;
_shelx_res_checksum              70504
_shelx_fab_checksum              41289
_olex2_submission_special_instructions 'No special instructions were received'