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_1556880
_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         'C58 H48 Ni2 P4 S8, C32 H12 B F24'
_chemical_formula_sum            'C90 H60 B F24 Ni2 P4 S8'
_chemical_formula_weight         2105.97
_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                94.073(2)
_cell_angle_beta                 103.397(2)
_cell_angle_gamma                106.515(2)
_cell_formula_units_Z            2
_cell_length_a                   14.1624(15)
_cell_length_b                   18.3974(19)
_cell_length_c                   20.189(2)
_cell_measurement_reflns_used    9361
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      15.83
_cell_measurement_theta_min      2.43
_cell_volume                     4852.9(9)
_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 2018/2 (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 0.964
_diffrn_measured_fraction_theta_max 0.960
_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  0.0384
_diffrn_reflns_av_unetI/netI     0.0261
_diffrn_reflns_Laue_measured_fraction_full 0.964
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            141909
_diffrn_reflns_point_group_measured_fraction_full 0.964
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        14.357
_diffrn_reflns_theta_max         15.826
_diffrn_reflns_theta_min         0.843
_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    0.169
_exptl_absorpt_correction_T_max  0.7439
_exptl_absorpt_correction_T_min  0.6645
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. 
wR2(int) was 0.1535 before and 0.0482 after correction. 
The Ratio of minimum to maximum transmission is 0.8933. 
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.441
_exptl_crystal_description       plate
_exptl_crystal_F_000             2130
_exptl_crystal_size_max          0.002
_exptl_crystal_size_mid          0.002
_exptl_crystal_size_min          0.001
_refine_diff_density_max         0.956
_refine_diff_density_min         -0.578
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1200
_refine_ls_number_reflns         22441
_refine_ls_number_restraints     174
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0416
_refine_ls_R_factor_gt           0.0352
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0401P)^2^+3.7431P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0910
_refine_ls_wR_factor_ref         0.0963
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19223
_reflns_number_total             22441
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc04381k2.cif
_cod_data_source_block           076
_cod_depositor_comments
;Adding full bibliography for 1556876--1556883.cif.

 Adding full bibliography for 1556876--1556883.cif.
;
_cod_original_cell_volume        4852.8(9)
_cod_database_code               1556880
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   1.000
_shelx_estimated_absorpt_t_min   1.000
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 F1-C65 \\sim F2A-C65 \\sim F2-C65 \\sim F3A-C65 \\sim F3-C65 \\sim F1A-C65
 with sigma of 0.01
 F24A-C89 \\sim F23-C89 \\sim F24-C89 \\sim F22A-C89 \\sim F22-C89 \\sim
F23A-C89
 with sigma of 0.005
 F22A-F23A \\sim F23A-F24A \\sim F22A-F24A
 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
C61 \\sim C65 \\sim F1 \\sim F2 \\sim F3 \\sim F2A \\sim F1A \\sim F3A: within
2A with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F22A) = Uanis(F23)
Uanis(F23A) = Uanis(F24)
Uanis(F24A) = Uanis(F22)
4. Rigid body (RIGU) restrains
 C61, C65, F1, F2, F3, F2A, F1A, F3A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Others
 Sof(F2A)=Sof(F1A)=Sof(F3A)=1-FVAR(1)
 Sof(F1)=Sof(F2)=Sof(F3)=FVAR(1)
 Sof(F24A)=Sof(F22A)=Sof(F23A)=1-FVAR(2)
 Sof(F22)=Sof(F23)=Sof(F24)=FVAR(2)
6.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C14(H14A,H14B), C45(H45A,H45B), C46(H46A,H46B)
6.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C22(H22), C23(H23),
  C24(H24), C25(H25), C26(H26), C34(H34), C35(H35), C36(H36), C37(H37),
 C38(H38), C40(H40), C41(H41), C42(H42), C43(H43), C44(H44), C48(H48), C49(H49),
  C50(H50), C51(H51), C52(H52), C54(H54), C55(H55), C56(H56), C57(H57),
 C58(H58), C60(H60), C62(H62), C64(H64), C68(H68), C70(H70), C72(H72), C76(H76),
  C78(H78), C80(H80), C84(H84), C86(H86), C88(H88)
;
_shelx_res_checksum              63360
_shelx_fab_checksum              72189
_olex2_submission_special_instructions 'No special instructions were received'