Broadband near-IR absorbing Au-dithiolene complexes bearing redox-active oligothiophene ligands.
Wright, Iain A.; Wilson, Claire; Coles, Simon J.; Skabara, Peter J.; Dalton transactions (Cambridge, England : 2003) 48 (2018) 107–116; doi:10.1039/c8dt03915a

data_7048119
_publ_section_title
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 Broadband near-IR absorbing Au-dithiolene complexes bearing redox-active
 oligothiophene ligands.
;
_journal_issue                   1
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              107
_journal_page_last               116
_journal_paper_doi               10.1039/c8dt03915a
_journal_volume                  48
_journal_year                    2018
_chemical_formula_moiety         'C52 H68 Ni1 O2.76 S10, 2(C8 H20 N)'
_chemical_formula_sum            'C68 H108 N2 Ni O2.7 S10'
_chemical_formula_weight         1376.07
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-11-06
_audit_creation_method
;
  Olex2 1.2
  (compiled Oct 26 2012 17:09:49, GUI svn.r4371)
;
_audit_update_record
;
2018-08-13 deposited with the CCDC.
2018-11-15 downloaded from the CCDC.
;
_cell_angle_alpha                76.076(6)
_cell_angle_beta                 76.307(4)
_cell_angle_gamma                89.934(7)
_cell_formula_units_Z            2
_cell_length_a                   12.2157(13)
_cell_length_b                   14.6041(13)
_cell_length_c                   21.186(2)
_cell_measurement_reflns_used    104609
_cell_measurement_temperature    120
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_volume                     3558.0(6)
_computing_cell_refinement
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_data_collection       'COLLECT (Hooft, R.W.W., 1998)'
_computing_data_reduction
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean '4096x4096pixels / 62x62mm'
_diffrn_measured_fraction_theta_full 0.943
_diffrn_measured_fraction_theta_max 0.943
_diffrn_measurement_device_type
'Bruker-Nonius APEX II CCD camera on \k-goniostat'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  '10cm confocal mirrors'
_diffrn_radiation_source         'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1743
_diffrn_reflns_av_unetI/netI     0.2726
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            38810
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.94
_exptl_absorpt_coefficient_mu    0.611
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.602
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2007/2 (Sheldrick, G.M., 2007)'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.284
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1479
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.939
_refine_diff_density_min         -0.698
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     737
_refine_ls_number_reflns         11833
_refine_ls_number_restraints     61
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.3281
_refine_ls_R_factor_gt           0.1625
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+88.5304P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2712
_refine_ls_wR_factor_ref         0.3599
_reflns_number_gt                4924
_reflns_number_total             11833
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c8dt03915a2.cif
_cod_data_source_block           2011src0164
_cod_depositor_comments          'Adding full bibliography for 7048119.cif.'
_cod_original_formula_sum        'C68 H108 N2 Ni O2.70 S10'
_cod_database_code               7048119
_olex2_refinement_description
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1. Fixed Uiso
 At 1.2 times of:
  {H7NA,H7NB} of C7N, {H5NA,H5NB} of C5N, {H3NA,H3NB} of C3N, {H24A,H24B} of
  C24A, {H25A,H25B} of C25A, {H9NA,H9NB} of C9N, {H11A,H11B} of C11N, {H13A,
  H13B} of C13N, {H15G,H15H} of C15N, {H1NA,H1NB} of C1N, {H23A,H23B} of C23A,
  {H15E,H15F} of C15, H7 of C7, {H17E,H17F} of C17, H12 of C12, {H16E,H16F} of
  C16, {H18E,H18F} of C18, {H19E,H19F} of C19, {H22A,H22B} of C22A, {H21A,H21B}
  of C21A, {H19C,H19D} of C19C, {H19A,H19B} of C19A, {H18C,H18D} of C18C, {H18A,
  H18B} of C18A, {H17C,H17D} of C17C, {H17A,H17B} of C17A, {H16C,H16D} of C16C,
  {H16A,H16B} of C16A, {H15C,H15D} of C15C, {H15A,H15B} of C15A, H12A of C12A,
  H7A of C7A, {H25C,H25D,H25E,H25F} of C25, {H24C,H24D} of C24, {H23C,H23D} of
  C23, {H22C,H22D} of C22, {H21C,H21D} of C21
 At 1.5 times of:
  {H8NA,H8NB,H8NC} of C8N, {H6NA,H6NB,H6NC} of C6N, {H4NA,H4NB,H4NC} of C4N,
  {H2NA,H2NB,H2NC} of C2N, {H26A,H26B,H26C} of C26A, {H10A,H10B,H10C} of C10N,
  {H12B,H12C,H12D} of C12N, {H14G,H14H,H14I} of C14N, {H16G,H16H,H16I} of C16N,
  {H14D,H14E,H14F} of C14, {H9A,H9B,H9C} of C9, {H20D,H20E,H20F} of C20C, {H20A,
  H20B,H20C} of C20A, {H14A,H14B,H14C} of C14A, {H9AA,H9AB,H9AC} of C9A, {H26G,
  H26H,H26I} of C26B, {H26D,H26E,H26F} of C26, {H20G,H20H,H20I} of C20
2. Restrained distances
 C6-C15 = C16-C15 = C17-C16 = C18-C17 = C19-C18 = C20-C19
 1.51 with sigma of 0.02
 C6A-C15A = C16A-C15A = C17A-C16A = C18A-C17A = C19A-C18A = C20A-C19A
 1.51 with sigma of 0.02
 C11A-C21A = C21A-C22A = C22A-C23A = C23A-C24A = C24A-C25A = C25A-C26A
 1.51 with sigma of 0.02
 C6A-C15C = C16C-C15C = C17C-C16C = C18C-C17C = C18C-C19C = C19C-C20C
 1.51 with sigma of 0.02
 C21-C11 = C22-C21 = C23-C22 = C24-C23 = C25-C24 = C26-C25 = C25-C26B
 1.51 with sigma of 0.02
 C6-C16 ~ C15-C17 ~ C17-C19 ~ C16-C18 ~ C18-C20
 with sigma of 0.02
 C6A-C16C ~ C15C-C17C ~ C16C-C18C ~ C17C-C19C ~ C18C-C20C
 with sigma of 0.02
 C11-C22 ~ C22-C24 ~ C24-C26 ~ C21-C23 ~ C23-C25
 with sigma of 0.02
3. Others
 Sof(C15A)=Sof(H15A)=Sof(H15B)=1-Sof(H15A)=1-Sof(H15A)=1-Sof(H15A)=Sof(C16A)=
 Sof(H16A)=Sof(H16B)=1-Sof(H15A)=1-Sof(H15A)=1-Sof(H15A)=Sof(C17A)=Sof(H17A)=
 Sof(H17B)=1-Sof(H15A)=1-Sof(H15A)=1-Sof(H15A)=Sof(C18A)=Sof(H18A)=Sof(H18B)=1-
 Sof(H15A)=1-Sof(H15A)=1-Sof(H15A)=Sof(C19A)=Sof(H19A)=Sof(H19B)=1-Sof(H15A)=1-
 Sof(H15A)=1-Sof(H15A)=Sof(C20A)=Sof(H20A)=Sof(H20B)=Sof(H20C)=1-Sof(H15A)=1-
 Sof(H15A)=1-Sof(H15A)=1-Sof(H15A)
 Sof(O1)=Sof(O2)
 Sof(O3)=Sof(O4)
 Sof(O1A)=Sof(O2A)
 Sof(O3A)=Sof(O4A)
 Uiso(C15C)=Uiso(C16C)=Uiso(C17C)=Uiso(C18C)=Uiso(C19C)=Uiso(C20C)
 Sof(H25C)=Sof(H25D)=1-Sof(H25D)=1-Sof(H25D)=Sof(C26)=Sof(H26D)=Sof(H26E)=
 Sof(H26F)=1-Sof(H25D)=1-Sof(H25D)=1-Sof(H25D)=1-Sof(H25D)
4.a Secondary CH2 refined with riding coordinates:
 C15(H15E,H15F), C16(H16E,H16F), C17(H17E,H17F), C18(H18E,H18F), C19(H19E,
 H19F), C21(H21C,H21D), C22(H22C,H22D), C23(H23C,H23D), C24(H24C,H24D),
 C25(H25C,H25D), C25(H25E,H25F), C15A(H15A,H15B), C15C(H15C,H15D), C16A(H16A,
 H16B), C16C(H16C,H16D), C17A(H17A,H17B), C17C(H17C,H17D), C18A(H18A,H18B),
 C18C(H18C,H18D), C19A(H19A,H19B), C19C(H19C,H19D), C21A(H21A,H21B), C22A(H22A,
 H22B), C23A(H23A,H23B), C24A(H24A,H24B), C25A(H25A,H25B), C9N(H9NA,H9NB),
 C11N(H11A,H11B), C13N(H13A,H13B), C15N(H15G,H15H), C1N(H1NA,H1NB), C3N(H3NA,
 H3NB), C5N(H5NA,H5NB), C7N(H7NA,H7NB)
4.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C12(H12), C7A(H7A), C12A(H12A)
4.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C14(H14D,H14E,H14F), C20(H20G,H20H,H20I), C26(H26D,H26E,
 H26F), C26B(H26G,H26H,H26I), C9A(H9AA,H9AB,H9AC), C14A(H14A,H14B,H14C),
 C20A(H20A,H20B,H20C), C20C(H20D,H20E,H20F), C26A(H26A,H26B,H26C), C10N(H10A,
 H10B,H10C), C12N(H12B,H12C,H12D), C14N(H14G,H14H,H14I), C16N(H16G,H16H,H16I),
 C2N(H2NA,H2NB,H2NC), C4N(H4NA,H4NB,H4NC), C6N(H6NA,H6NB,H6NC), C8N(H8NA,H8NB,
 H8NC)
;