Methyldisulfide groups enable the direct connection of air-stable metal bis(terpyridine) complexes to gold surfaces
Trang, Christina D. M.; Saal, Thomas; Inkpen , Michael Stephen; Dalton Transactions  (2023) –; doi:10.1039/D3DT00955F

data_7713027
_publ_section_title
;
 Methyldisulfide groups enable the direct connection of air-stable metal
 bis(terpyridine) complexes to gold surfaces
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT00955F
_journal_year                    2023
_chemical_formula_moiety         'C32 H26 Fe N6 S4, 2(F6 P),C2 H3 N [+ solvent]'
_chemical_formula_sum            'C34 H29 F12 Fe N7 P2 S4'
_chemical_formula_weight         1009.67
_chemical_name_common            'FeSS, [Fe(tpySS)2](PF6)2'
_chemical_name_systematic
Iron(II)-bis(4?-(methyldisulfide)-2,2?:6?,2??-terpyridine)
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_update_record
;
2022-11-18 deposited with the CCDC.	2023-05-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.314(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.7953(2)
_cell_length_b                   33.8428(8)
_cell_length_c                   14.0963(3)
_cell_measurement_reflns_used    5578
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      69.4580
_cell_measurement_theta_min      3.3988
_cell_volume                     4192.45(16)
_computing_cell_refinement       'APEX2 v2014.11-0 (Bruker AXS, 2014)'
_computing_data_collection
'Bruker Instrument Service v2012.12.0.3 (Bruker AXS, 2012'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS, 2013)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 882)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Bruker APEX II CCD'
_diffrn_measurement_method       'omega- and phi-scans'
_diffrn_radiation_monochromator  'multi-layer optics'
_diffrn_radiation_type           'CuK\a '
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1455
_diffrn_reflns_av_unetI/netI     0.1081
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7951
_diffrn_reflns_theta_full        70.07
_diffrn_reflns_theta_max         70.07
_diffrn_reflns_theta_min         2.61
_diffrn_source                   'IuS microsource'
_exptl_absorpt_coefficient_mu    6.322
_exptl_absorpt_correction_T_max  0.753299
_exptl_absorpt_correction_T_min  0.527141
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/5 (Bruker AXS)'
_exptl_crystal_colour            'clear red'
_exptl_crystal_density_diffrn    1.600
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2128
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.183
_exptl_crystal_size_min          0.044
_platon_squeeze_details
;
The unit cell contains 4 acetonitrile molecules which have been treated as a 
diffuse contribution to the overall scattering without specific atom positions by 
SQUEEZE/PLATON.
;
_refine_diff_density_max         0.540
_refine_diff_density_min         -0.453
_refine_ls_abs_structure_details
;

Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.490(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1118
_refine_ls_number_reflns         7951
_refine_ls_number_restraints     101
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0807
_refine_ls_R_factor_gt           0.0618
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0535P)^2^+11.3694P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1342
_refine_ls_wR_factor_ref         0.1416
_reflns_number_gt                6858
_reflns_number_total             7951
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00955f2.cif
_cod_data_source_block           C32H26F12FeN6P2S4
_cod_database_code               7713027
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              68590
_shelx_fab_checksum              68325