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_1562224
_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 H38 Ag12.4 Au0.6 F44 N12'
_chemical_formula_sum            'C94 H38 Ag12.4 Au0.6 F44 N13'
_chemical_formula_weight         3641.14
_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
_audit_creation_date             2021-01-05
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_cell_angle_alpha                62.885(6)
_cell_angle_beta                 67.963(6)
_cell_angle_gamma                61.886(6)
_cell_formula_units_Z            1
_cell_length_a                   15.3601(9)
_cell_length_b                   15.6093(9)
_cell_length_c                   15.6475(11)
_cell_measurement_reflns_used    8564
_cell_measurement_temperature    100.00(13)
_cell_measurement_theta_max      76.6600
_cell_measurement_theta_min      3.2120
_cell_volume                     2883.2(4)
_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 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(13)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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    -36.00  28.00   0.50    0.60    --   -2.20  82.00   0.00  128
  2  \w     27.00  92.00   0.50    0.60    --    2.20  38.00 150.00  130
  3  \w    -20.00  14.00   0.50    0.60    --    2.20  38.00 150.00   68
  4  \w    -10.00  92.00   0.50    0.60    --    2.20  38.00 -90.00  204
  5  \w    -20.00   5.00   0.50    0.60    --    2.20  82.00 -60.00   50
  6  \w      8.00  39.00   0.50    0.60    --    2.20  82.00 -60.00   62
  7  \w    -14.00  40.00   0.50    0.60    --    2.20  82.00-180.00  108
  8  \w     97.00 134.00   0.50    2.39    --  106.30 -82.00   0.00   74
  9  \w     18.00 126.00   0.50    2.39    --  106.30 -19.00-180.00  216
 10  \w     54.00 139.00   0.50    2.39    --  106.30 -77.00 150.00  170
 11  \w     24.00 137.00   0.50    2.39    --  106.30 -19.00  60.00  226
 12  \w     80.00 105.00   0.50    2.39    --  106.30 -82.00 -90.00   50
 13  \w     17.00 129.00   0.50    2.39    --  106.30 -57.00 -30.00  224
 14  \w     62.00 140.00   0.50    2.39    --  106.30 -82.00-180.00  156
 15  \w     58.00 139.00   0.50    2.39    --  106.30 -82.00  90.00  162
 16  \w     35.00 106.00   0.50    2.39    --  106.30 -38.00 120.00  142
 17  \w     18.00 138.00   0.50    2.39    --  106.30 -82.00 -30.00  240
 18  \w     31.00  57.00   0.50    2.39    --  106.30 -82.00 -60.00   52
 19  \w     83.00 108.00   0.50    2.39    --  106.30 -82.00 -60.00   50
 20  \w     40.00 193.00   0.50    2.39    --  106.30   0.00 -60.00  306
;
_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      0.0055965000
_diffrn_orient_matrix_UB_12      -0.0376026000
_diffrn_orient_matrix_UB_13      -0.0781109000
_diffrn_orient_matrix_UB_21      0.0054556000
_diffrn_orient_matrix_UB_22      -0.1068641000
_diffrn_orient_matrix_UB_23      0.0783261000
_diffrn_orient_matrix_UB_31      -0.1159014000
_diffrn_orient_matrix_UB_32      0.0365684000
_diffrn_orient_matrix_UB_33      0.0230586000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0626
_diffrn_reflns_av_unetI/netI     0.0636
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            24607
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        65.000
_diffrn_reflns_theta_max         65.000
_diffrn_reflns_theta_min         3.241
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    18.953
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.12997
_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 black'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    2.097
_exptl_crystal_description       block
_exptl_crystal_F_000             1719
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         4.043
_refine_diff_density_min         -2.422
_refine_diff_density_rms         0.291
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     601
_refine_ls_number_reflns         9783
_refine_ls_number_restraints     138
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.1120
_refine_ls_R_factor_gt           0.1060
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1645P)^2^+58.0532P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2975
_refine_ls_wR_factor_ref         0.3028
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8647
_reflns_number_total             9783
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jp1c00621_si_002.cif
_cod_data_source_block           AgAu_F
_cod_original_formula_sum        'C94 H38 Ag12.40 Au0.60 F44 N13'
_cod_database_code               1562224
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N Au Ag F '
_shelx_estimated_absorpt_t_max   0.451
_shelx_estimated_absorpt_t_min   0.253
_reflns_odcompleteness_completeness 99.52
_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. Uiso/Uaniso restraints and constraints
Uanis(C34) \\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(C36) \\sim Ueq, Uanis(C37)
\\sim Ueq, Uanis(C38') \\sim Ueq, Uanis(C39') \\sim Ueq, Uanis(F21) \\sim Ueq:
with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C34') \\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(C38) \\sim Ueq, Uanis(C37')
\\sim Ueq, Uanis(C36') \\sim Ueq, Uanis(C35') \\sim Ueq, Uanis(F21') \\sim Ueq:
with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C26) \\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C30)
\\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(F20) \\sim Ueq,
Uanis(C27) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C25) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C34') = Uanis(C39) = Uanis(C38) = Uanis(C37') = Uanis(C36') = Uanis(C35')
= Uanis(F21')
Uanis(C19) = Uanis(C18) = Uanis(C23) = Uanis(C22) = Uanis(C21) = Uanis(C20)
Uanis(C34) = Uanis(C35) = Uanis(C36) = Uanis(C37) = Uanis(C38') = Uanis(C39') =
Uanis(F21)
Uanis(C26) = Uanis(C31) = Uanis(C30) = Uanis(C29) = Uanis(C28) = Uanis(F20) =
Uanis(C27)
Uanis(Au1) = Uanis(Ag7)
3. Others
 Fixed Sof: Au1(0.3) F21(0.5) F21'(0.5) C34(0.5) C39'(0.5) H39'(0.5) C38'(0.5)
 H38'(0.5) C37(0.5) H37(0.5) C36(0.5) C35(0.5) H35(0.5) C36'(0.5) C35'(0.5)
 H35'(0.5) C34'(0.5) C39(0.5) H39(0.5) C38(0.5) H38(0.5) C37'(0.5) H37'(0.5)
 Ag7(0.2)
4.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C8(H8), C13(H13), C19(H19), C23(H23), C22(H22), C21(H21), C31(H31),
 C30(H30), C29(H29), C27(H27), C39'(H39'), C38'(H38'), C37(H37), C35(H35),
 C35'(H35'), C39(H39), C38(H38), C37'(H37'), C43(H43), C44(H44), C45(H45),
 C47(H47)
4.b Fitted hexagon refined as free rotating group:
 C19(C18,C23,C22,C21,C20), C26(C31,C30,C29,C28,C27), C34(C39',C38',C37,C36,
 C35), C36'(C35',C34',C39,C38,C37'), C43(C44,C45,C46,C47,C42)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              81877
_shelx_hkl_checksum              99753
_shelx_fab_checksum              9884
_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 5.268
_oxdiff_exptl_absorpt_empirical_full_min 0.451