Extreme red shifted SERS nanotags
Bedics, Matthew A.; Kearns, Hayleigh; Cox, Jordan M.; Mabbott, Sam; Ali, Fatima; Shand, Neil C.; Faulds, Karen; Benedict, Jason B.; Graham, Duncan; Detty, Michael R.; Chem. Sci. 6 (2015) 2302–; doi:10.1039/C4SC03917C

data_1518609
_publ_section_title
;
 Extreme red shifted SERS nanotags
;
_journal_issue                   4
_journal_name_full               'Chem. Sci.'
_journal_page_first              2302
_journal_paper_doi               10.1039/C4SC03917C
_journal_volume                  6
_journal_year                    2015
_chemical_formula_moiety         'C29 H19 S2 Se4, F6 P, 3(C2 H3 N)'
_chemical_formula_sum            'C35 H28 F6 N3 P S2 Se4'
_chemical_formula_weight         1015.53
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2014-11-26
_audit_creation_method
;
Olex2 1.2
(compiled 2014.11.25 svn.r3098 for OlexSys, GUI svn.r4951)
;
_audit_update_record
;
2014-12-17 deposited with the CCDC.
2015-01-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.7263(19)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.6176(12)
_cell_length_b                   7.5992(5)
_cell_length_c                   25.2231(15)
_cell_measurement_reflns_used    6686
_cell_measurement_temperature    90
_cell_measurement_theta_max      23.270
_cell_measurement_theta_min      2.552
_cell_volume                     3752.3(4)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      90
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1034
_diffrn_reflns_av_unetI/netI     0.0651
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            69197
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.151
_diffrn_reflns_theta_min         1.618
_diffrn_source                   'microfocus rotating anode'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.126
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6005
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/2 (Bruker,2014/2) was used for absorption correction. wR2(int) was 
0.1028 before and 0.0541 after correction. The Ratio of minimum to maximum 
transmission is 0.8055. The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.798
_exptl_crystal_description       needle
_exptl_crystal_F_000             1984
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetonitrile'
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.549
_refine_diff_density_min         -0.641
_refine_diff_density_rms         0.125
_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     502
_refine_ls_number_reflns         8308
_refine_ls_number_restraints     22
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0911
_refine_ls_R_factor_gt           0.0513
_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^)+(0.0359P)^2^+9.2036P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0967
_refine_ls_wR_factor_ref         0.1075
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5735
_reflns_number_total             8308
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4sc03917c2.cif
_cod_data_source_block           dye_14
_cod_depositor_comments          'Adding full bibliography for 1518609.cif.'
_cod_database_code               1518609
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Se3-C17 \\sim Se3A-C17A
 with sigma of 0.02
 Se4-C26 \\sim Se4A-C26
 with sigma of 0.02
 C27-C26 \\sim C27A-C26
 with sigma of 0.02
 Se4A-C29A \\sim Se4-C29
 with sigma of 0.02
 C28-C27 \\sim C28A-C27A
 with sigma of 0.02
 C28-C29 \\sim C28A-C29A
 with sigma of 0.02
 C10-C11 \\sim C10-C11A
 with sigma of 0.02
 Se2A-C10 \\sim Se2-C10
 with sigma of 0.02
 Se2-C13 \\sim Se2A-C13A
 with sigma of 0.02
 C12A-C11A \\sim C12-C11
 with sigma of 0.02
 C13-C12 \\sim C13A-C12A
 with sigma of 0.02
 Se3A-C20 \\sim Se3-C20
 with sigma of 0.02
 C18-C17 \\sim C18A-C17A
 with sigma of 0.02
 Se2A-C12A \\sim Se2A-C11A
 with sigma of 0.02
 C19-C20 \\sim C19A-C20
 with sigma of 0.02
 C19-C18 \\sim C19A-C18A
 with sigma of 0.02
3. Restrained planarity
 C26, Se4A, C27A, C28A, C29A
 with sigma of 0.1
 C10, C11A, C12A, C13A, Se2A
 with sigma of 0.1
 C20, Se3A, C17A, C18A, C19A
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(Se3) = Uanis(Se3A)
Uanis(C18) = Uanis(C18A)
Uanis(C17A) = Uanis(C17)
Uanis(C27) = Uanis(C27A)
Uanis(C28) = Uanis(C28A)
Uanis(C29A) = Uanis(C29)
Uanis(Se4A) = Uanis(Se4)
Uanis(Se2) = Uanis(Se2A)
Uanis(C11) = Uanis(C11A)
Uanis(C12) = Uanis(C12A)
Uanis(C13A) = Uanis(C13)
Uanis(C19A) = Uanis(C19)
5. Others
 Sof(Se3A)=Sof(C17A)=Sof(H17A)=Sof(C18A)=Sof(H18A)=Sof(C19A)=Sof(H19A)=1-FVAR(1)
 Sof(Se3)=Sof(C17)=Sof(H17)=Sof(C18)=Sof(H18)=Sof(C19)=Sof(H19)=FVAR(1)
 Sof(Se4A)=Sof(C27A)=Sof(H27A)=Sof(C28A)=Sof(H28A)=Sof(C29A)=Sof(H29A)=1-FVAR(2)
 Sof(Se4)=Sof(C27)=Sof(H27)=Sof(C28)=Sof(H28)=Sof(C29)=Sof(H29)=FVAR(2)
 Sof(Se2A)=Sof(C11A)=Sof(H11A)=Sof(C12A)=Sof(H12A)=Sof(C13A)=Sof(H13A)=1-FVAR(3)
 Sof(Se2)=Sof(C11)=Sof(H11)=Sof(C12)=Sof(H12)=Sof(C13)=Sof(H13)=FVAR(3)
6.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C6(H6), C8(H8), C14(H14), C15(H15), C16(H16),
 C22(H22), C24(H24), C11(H11), C12(H12), C13(H13), C17(H17), C18(H18), C19(H19),
  C27(H27), C28(H28), C29(H29), C11A(H11A), C12A(H12A), C13A(H13A), C17A(H17A),
 C18A(H18A), C19A(H19A), C27A(H27A), C28A(H28A), C29A(H29A)
6.b Idealised Me refined as rotating group:
 C31(H31a,H31b,H31c), C33(H33a,H33b,H33c), C35(H35a,H35b,H35c)
;
_olex2_submission_special_instructions 'No special instructions were received'