Phosphorescent Metal Rotaxane-like Bimetallic Ag/Au Clusters
Zheng, Ji; Wang, Jia-Nan; Wang, Ting; Wu, Kun; Wei, Rong-Jia; Lu, Weigang; Li, Dan; The Journal of Physical Chemistry C  (2021) –; doi:10.1021/acs.jpcc.1c00621

data_1562223
_publ_section_title
;
 Phosphorescent Metal Rotaxane-like Bimetallic Ag/Au Clusters
;
_journal_name_full               'The Journal of Physical Chemistry C'
_journal_paper_doi               10.1021/acs.jpcc.1c00621
_journal_year                    2021
_chemical_formula_moiety         'C94 H46 Ag12 Au F36 N12, 2(C3 N0.5)'
_chemical_formula_sum            'C100 H46 Ag12 Au F36 N13'
_chemical_formula_weight         3604.90
_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     iterative
_audit_creation_date             2020-08-31
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                61.591(4)
_cell_angle_beta                 67.904(3)
_cell_angle_gamma                61.997(4)
_cell_formula_units_Z            1
_cell_length_a                   15.4163(5)
_cell_length_b                   15.5079(7)
_cell_length_c                   15.5847(5)
_cell_measurement_reflns_used    35617
_cell_measurement_temperature    99.98(14)
_cell_measurement_theta_max      77.6430
_cell_measurement_theta_min      3.0150
_cell_volume                     2837.0(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.98(14)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w    -39.00  28.00   0.50    0.50    --   -2.20 -82.00 -30.00  134
  2  \w    -27.00   5.00   0.50    0.50    --   -2.20  82.00-150.00   64
  3  \w     24.00  80.00   0.50    0.50    --   -2.20  19.00 -60.00  112
  4  \w    -36.00  36.00   0.50    0.50    --   -2.20  82.00 -90.00  144
  5  \w    -33.00  -1.00   0.50    0.50    --   -2.20  19.00 -60.00   64
  6  \w    -31.00  25.00   0.50    0.50    --    2.20  82.00 150.00  112
  7  \w    -35.00  37.00   0.50    0.50    --    2.20 -82.00-150.00  144
  8  \w    -31.00  -4.00   0.50    0.50    --    2.20  82.00   0.00   54
  9  \w     17.00 133.00   0.50    1.10    --  106.30 -57.00 120.00  232
 10  \w     91.00 129.00   0.50    1.10    --  106.30 -82.00-150.00   76
 11  \w     17.00  88.00   0.50    1.10    --  106.30 -38.00 -60.00  142
 12  \w     17.00 123.00   0.50    1.10    --  106.30 -19.00 -30.00  212
 13  \w     96.00 122.00   0.50    1.10    --  106.30 -82.00 -90.00   52
 14  \w     23.00 141.00   0.50    1.10    --  106.30 -82.00 120.00  236
 15  \w     18.00  44.00   0.50    1.10    --  106.30 -82.00-150.00   52
 16  \w     65.00 110.00   0.50    1.10    --  106.30 -82.00  60.00   90
 17  \w     78.00 113.00   0.50    1.10    --  106.30 -82.00 150.00   70
 18  \w     76.00 141.00   0.50    1.10    --  106.30 -82.00 -30.00  130
 19  \w     25.00 139.00   0.50    1.10    --  106.30 -19.00-150.00  228
 20  \w    164.00 194.00   0.50    1.10    --  106.30   0.00 150.00   60
 21  \w     59.00 131.00   0.50    1.10    --  106.30 -82.00-120.00  144
 22  \w     21.00 138.00   0.50    1.10    --  106.30 -82.00 -60.00  234
 23  \w     18.00 146.00   0.50    1.10    --  106.30   0.00 150.00  256
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0335046000
_diffrn_orient_matrix_UB_12      -0.0016398000
_diffrn_orient_matrix_UB_13      -0.0486070000
_diffrn_orient_matrix_UB_21      -0.0795648000
_diffrn_orient_matrix_UB_22      -0.0284895000
_diffrn_orient_matrix_UB_23      0.0300722000
_diffrn_orient_matrix_UB_31      -0.0734928000
_diffrn_orient_matrix_UB_32      0.1010432000
_diffrn_orient_matrix_UB_33      0.0109386000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0358
_diffrn_reflns_av_unetI/netI     0.0330
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.955
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            33538
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.416
_diffrn_reflns_theta_min         5.590
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    19.545
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.26716
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.33c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.110
_exptl_crystal_description       block
_exptl_crystal_F_000             1704
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.566
_refine_diff_density_min         -1.766
_refine_diff_density_rms         0.170
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     781
_refine_ls_number_reflns         11652
_refine_ls_number_restraints     74
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0504
_refine_ls_R_factor_gt           0.0459
_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^)+(0.0784P)^2^+10.1846P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1279
_refine_ls_wR_factor_ref         0.1314
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10381
_reflns_number_total             11652
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jp1c00621_si_002.cif
_cod_data_source_block           AgAu_H
_cod_database_code               1562223
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C H O N F Ag Cu '
_shelx_estimated_absorpt_t_max   0.442
_shelx_estimated_absorpt_t_min   0.245
_reflns_odcompleteness_completeness 99.54
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 N7-C48
 1.4 with sigma of 0.02
 N7-C50
 1.4 with sigma of 0.02
 C48-C49
 1.4 with sigma of 0.02
 C50-C51
 1.4 with sigma of 0.02
 C52-C53
 1.4 with sigma of 0.02
 N7-C52
 1.4 with sigma of 0.02
 N7-C54
 1.4 with sigma of 0.02
 C54-C55
 1.4 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C48) \\sim Ueq, Uanis(C53) \\sim Ueq, Uanis(C52) \\sim Ueq, Uanis(N7)
\\sim Ueq, Uanis(C54) \\sim Ueq, Uanis(C50) \\sim Ueq, Uanis(C49) \\sim Ueq,
Uanis(C55) \\sim Ueq, Uanis(C51) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(C53) \\sim Ueq, Uanis(C52) \\sim Ueq, Uanis(N7) \\sim Ueq, Uanis(C48)
\\sim Ueq, Uanis(C54) \\sim Ueq, Uanis(C50) \\sim Ueq, Uanis(C56) \\sim Ueq,
Uanis(C49) \\sim Ueq, Uanis(C55) \\sim Ueq, Uanis(C51) \\sim Ueq, Uanis(C57)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C42') = Uanis(C47) = Uanis(C46') = Uanis(C45') = Uanis(C44') = Uanis(C43')
Uanis(C42) = Uanis(C47') = Uanis(C46) = Uanis(C45) = Uanis(C44) = Uanis(C43)
4. Others
 Fixed Sof: C42(0.5) C43(0.5) H43(0.5) C44(0.5) H44(0.5) C45(0.5) H45(0.5)
 C46(0.5) H46(0.5) C47(0.5) H47(0.5) C42'(0.5) C43'(0.5) H43'(0.5) C44'(0.5)
 H44'(0.5) C45'(0.5) H45'(0.5) C46'(0.5) H46'(0.5) C47'(0.5) H47'(0.5) C53(0.3)
 N7(0.5) C48(0.3) C51(0.3) C54(0.3) C52(0.3) C49(0.3) C50(0.3) C55(0.3)
 C56(0.3) C57(0.3)
5.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C8(H8), C13(H13), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23),
 C27(H27), C28(H28), C29(H29), C30(H30), C31(H31), C35(H35), C36(H36), C37(H37),
  C38(H38), C39(H39), C43(H43), C44(H44), C45(H45), C46(H46), C47(H47),
 C43'(H43'), C44'(H44'), C45'(H45'), C46'(H46'), C47'(H47')
5.b Fitted hexagon refined as free rotating group:
 C42'(C43',C44',C45',C46',C47')
;
_shelx_res_checksum              21275
_shelx_hkl_checksum              99756
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 4.486
_oxdiff_exptl_absorpt_empirical_full_min 0.544