Molecular cage-bridged plasmonic structures with well-defined nanogaps as well as the capability of reversible and selective guest trapping.
Wang, Chen; Tian, Li; Zhu, Wei; Wang, Shiqiang; Gao, Ning; Zhou, Kang; Yin, Xianpeng; Zhang, Wanlin; Zhao, Liang; Li, Guangtao; Chemical science 9 (2018) 889–895; doi:10.1039/c7sc03536e

data_1548134
_publ_section_title
;
 Molecular cage-bridged plasmonic structures with well-defined nanogaps as
 well as the capability of reversible and selective guest trapping.
;
_journal_issue                   4
_journal_name_full               'Chemical science'
_journal_page_first              889
_journal_page_last               895
_journal_paper_doi               10.1039/c7sc03536e
_journal_volume                  9
_journal_year                    2018
_chemical_formula_moiety         'C84 H60 N12 Pd2 S4, 4(C F3 O3 S)'
_chemical_formula_sum            'C88 H60 F12 N12 O12 Pd2 S8'
_chemical_formula_weight         2174.76
_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
_audit_creation_date             2016-05-23
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-07-11 deposited with the CCDC.
2017-11-20 downloaded from the CCDC.
;
_cell_angle_alpha                100.641(4)
_cell_angle_beta                 102.198(5)
_cell_angle_gamma                98.202(6)
_cell_formula_units_Z            1
_cell_length_a                   12.284(4)
_cell_length_b                   15.243(5)
_cell_length_c                   17.550(7)
_cell_measurement_reflns_used    8848
_cell_measurement_temperature    173.1500
_cell_measurement_theta_max      27.4302
_cell_measurement_theta_min      1.2174
_cell_volume                     3099.8(19)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_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
;
????
;
_diffrn_ambient_temperature      173.1500
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
scan:
    Number of images: 360
               Slice: -110.0000 - 70.0000
         Image width: 0.5000
            Exp time: 6.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 0.0000
                 XTD: 45.1853
              2theta: -20.0129
scan:
    Number of images: 360
               Slice: -110.0000 - 70.0000
         Image width: 0.5000
            Exp time: 6.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 90.0000
                 XTD: 45.1853
              2theta: -20.0129
scan:
    Number of images: 284
               Slice: -79.0000 - 63.0000
         Image width: 0.5000
            Exp time: 6.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 270.0000
                 XTD: 45.1853
              2theta: -20.0129
scan:
    Number of images: 272
               Slice: -83.7500 - 52.2500
         Image width: 0.5000
            Exp time: 6.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 180.0000
                 XTD: 45.1853
              2theta: -20.0129
;
_diffrn_measurement_device
;
Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_device_details
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       dtprofit.ref
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      0.0832
_diffrn_orient_matrix_UB_12      -0.0055
_diffrn_orient_matrix_UB_13      -0.0154
_diffrn_orient_matrix_UB_21      0.0128
_diffrn_orient_matrix_UB_22      0.0623
_diffrn_orient_matrix_UB_23      -0.0240
_diffrn_orient_matrix_UB_31      0.0254
_diffrn_orient_matrix_UB_32      0.0273
_diffrn_orient_matrix_UB_33      0.0467
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0567
_diffrn_reflns_av_unetI/netI     0.0558
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            44945
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.389
_diffrn_reflns_theta_min         1.217
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0000
_diffrn_source_power             1.2000
_diffrn_source_voltage           50.0000
_exptl_absorpt_coefficient_mu    0.493
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72687
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.165
_exptl_crystal_description       block
_exptl_crystal_F_000             1096
_exptl_crystal_size_max          0.256
_exptl_crystal_size_mid          0.243
_exptl_crystal_size_min          0.134
_refine_diff_density_max         2.657
_refine_diff_density_min         -0.921
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.138
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     663
_refine_ls_number_reflns         14030
_refine_ls_number_restraints     173
_refine_ls_restrained_S_all      1.147
_refine_ls_R_factor_all          0.1099
_refine_ls_R_factor_gt           0.0984
_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^)+(0.1532P)^2^+3.8968P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2755
_refine_ls_wR_factor_ref         0.2873
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11854
_reflns_number_total             14030
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7sc03536e2.cif
_cod_data_source_block           mx4847a_sq
_cod_depositor_comments          'Adding full bibliography for 1548134.cif.'
_cod_original_cell_volume        3099.8(18)
_cod_database_code               1548134
_diffrn_number_total             14034
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 S2-C41 = S2-C42
 1.82 with sigma of 0.01
 S3A-C01Q = S3-C01Q
 1.82 with sigma of 0.01
 S3A-O3A = S3-O3 = S3A-O1A = S3A-O2A = S3-O1
 1.4 with sigma of 0.01
 S2A-C42A = S2A-C41
 1.82 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
S3 \\sim O1 \\sim O3A \\sim O3 \\sim S3A \\sim O1A \\sim O2 \\sim O2A: within
1.7A with sigma of 0.02 and sigma for terminal atoms of 0.04
S2A \\sim C41 \\sim S2 \\sim C42 \\sim C42A: within 1.7A with sigma of 0.02 and
sigma for terminal atoms of 0.04
Uanis(S3) \\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(O3A) \\sim Ueq, Uanis(O3) \\sim
Ueq, Uanis(S3A) \\sim Ueq, Uanis(O1A) \\sim Ueq, Uanis(O2) \\sim Ueq,
Uanis(O2A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C42A) \\sim Ueq, Uanis(S2A) \\sim Ueq, Uanis(C41) \\sim Ueq, Uanis(S2)
\\sim Ueq, Uanis(C42) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
4. Others
 Sof(S2A)=Sof(H41C)=Sof(H41D)=Sof(C42A)=Sof(H42D)=Sof(H42E)=Sof(H42F)=1-FVAR(1)
 Sof(S2)=Sof(H41A)=Sof(H41B)=Sof(C42)=Sof(H42A)=Sof(H42B)=Sof(H42C)=FVAR(1)
 Sof(O3A)=Sof(S3A)=Sof(O1A)=Sof(O2A)=1-FVAR(2)
 Sof(S3)=Sof(O1)=Sof(O3)=Sof(O2)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C41(H41A,H41B), C41(H41C,H41D)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C5(H5), C9(H9), C11(H11), C16(H16), C17(H17),
 C18(H18), C19(H19), C22(H22), C23(H23), C24(H24), C26(H26), C30(H30), C32(H32),
  C37(H37), C38(H38), C39(H39), C40(H40)
5.c Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C42(H42A,H42B,H42C), C42A(H42D,H42E,H42F)
;
_shelx_res_checksum              41778
_shelx_fab_checksum              21043
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'