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_1562225
_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
'2(C102 H62 Ag12.2 Au0.8 F36 N12 O8), 2(C6 H6)'
_chemical_formula_sum            'C228 H170 Ag24.4 Au1.6 F72 N26 O17'
_chemical_formula_weight         7861.06
_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             2021-01-05
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_cell_angle_alpha                86.2278(7)
_cell_angle_beta                 87.0958(7)
_cell_angle_gamma                64.9064(12)
_cell_formula_units_Z            1
_cell_length_a                   15.21283(19)
_cell_length_b                   16.46205(18)
_cell_length_c                   27.06694(16)
_cell_measurement_reflns_used    41986
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      66.8760
_cell_measurement_theta_min      3.3190
_cell_volume                     6123.47(12)
_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    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_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    -21.00   9.00   0.50    0.50    --    0.00  45.00-125.00   60
  2  \w     58.00  84.00   0.50    0.50    --    0.00  45.00-125.00   52
  3  \w     10.00  50.00   0.50    0.50    --    0.00  45.00-125.00   80
  4  \w     75.00 172.00   0.50    1.28    --   82.70  45.00-125.00  194
  5  \w    -39.00  32.00   0.50    0.50    --    0.00 -82.00-180.00  142
  6  \w      3.00  33.00   0.50    0.50    --    0.00  82.00 120.00   60
  7  \w    -39.00  33.00   0.50    0.50    --    0.00 -82.00-120.00  144
  8  \w    -36.00  32.00   0.50    0.50    --    0.00 -82.00  90.00  136
  9  \w    -54.00 -29.00   0.50    0.50    --    0.00 -45.00  84.00   50
 10  \w    -20.00   5.00   0.50    0.50    --    0.00  82.00-150.00   50
 11  \w      7.00  32.00   0.50    0.50    --    0.00  38.00  30.00   50
 12  \w     48.00 116.00   0.50    1.28    --   82.70 -82.00 120.00  136
 13  \w     -3.00  40.00   0.50    1.28    --   82.70 -82.00 120.00   86
 14  \w     -7.00 113.00   0.50    1.28    --   82.70 -77.00 -30.00  240
 15  \w     64.00 116.00   0.50    1.28    --   82.70 -82.00-120.00  104
 16  \w     56.00 172.00   0.50    1.28    --   82.70  57.00-150.00  232
 17  \w     46.00 116.00   0.50    1.28    --   82.70 -82.00   0.00  140
 18  \w     34.00 102.00   0.50    1.28    --   82.70 -57.00-150.00  136
 19  \w     63.00 172.00   0.50    1.28    --   82.70  57.00 -90.00  218
 20  \w     -3.00 117.00   0.50    1.28    --   82.70 -82.00  30.00  240
 21  \w     91.00 117.00   0.50    1.28    --   82.70 -82.00-180.00   52
 22  \w     -6.00  71.00   0.50    1.28    --   82.70 -82.00-180.00  154
 23  \w     58.00  95.00   0.50    1.28    --   82.70  57.00-180.00   74
 24  \w    113.00 143.00   0.50    1.28    --   82.70  57.00-180.00   60
 25  \w     92.00 117.00   0.50    1.28    --   82.70  82.00-120.00   50
 26  \w    113.00 170.00   0.50    1.28    --   82.70  82.00 120.00  114
 27  \w     51.00  76.00   0.50    1.28    --   82.70 -82.00-150.00   50
 28  \w     77.00 102.00   0.50    1.28    --   82.70 -82.00 -60.00   50
 29  \w     18.00  61.00   0.50    1.28    --   82.70 -45.00  84.00   86
;
_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      -0.0045764000
_diffrn_orient_matrix_UB_12      0.0845144000
_diffrn_orient_matrix_UB_13      -0.0299628000
_diffrn_orient_matrix_UB_21      0.1070243000
_diffrn_orient_matrix_UB_22      -0.0258605000
_diffrn_orient_matrix_UB_23      0.0114165000
_diffrn_orient_matrix_UB_31      0.0322000000
_diffrn_orient_matrix_UB_32      -0.0537824000
_diffrn_orient_matrix_UB_33      -0.0471970000
_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  0.0690
_diffrn_reflns_av_unetI/netI     0.0543
_diffrn_reflns_Laue_measured_fraction_full 0.966
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            72946
_diffrn_reflns_point_group_measured_fraction_full 0.966
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        67.133
_diffrn_reflns_theta_max         67.133
_diffrn_reflns_theta_min         2.968
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    18.049
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.29599
_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    2.132
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3777
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         4.349
_refine_diff_density_min         -2.834
_refine_diff_density_rms         0.222
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1599
_refine_ls_number_reflns         21138
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0781
_refine_ls_R_factor_gt           0.0688
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0933P)^2^+95.3950P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1906
_refine_ls_wR_factor_ref         0.1947
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18523
_reflns_number_total             21138
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jp1c00621_si_002.cif
_cod_data_source_block           AgAu_OMe
_cod_original_formula_sum        'C228 H170 Ag24.40 Au1.60 F72 N26 O17'
_cod_database_code               1562225
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N Au Ag O F'
_shelx_estimated_absorpt_t_max   0.466
_shelx_estimated_absorpt_t_min   0.265
_reflns_odcompleteness_completeness 99.72
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     61.08
_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
 C41-C40
 1.35 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(Au1) \\sim Ueq, Uanis(Ag14) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(Au2) \\sim Ueq, Uanis(Ag13) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(Au2) = Uanis(Ag13)
Uanis(Au1) = Uanis(Ag14)
Uanis(O7) = Uanis(C104)
4. Others
 Fixed Sof: Au1(0.4) Au2(0.4) Ag13(0.1) Ag14(0.1)
5.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C7(H7), C12(H12), C34(H34), C35(H35), C36(H36), C38(H38), C43(H43),
 C44(H44), C45(H45), C47(H47), C52(H52), C53(H53), C54(H54), C56(H56), C61(H61),
  C62(H62), C63(H63), C65(H65), C17(H17), C22(H22), C27(H27), C70(H70),
 C71(H71), C72(H72), C73(H73), C79(H79), C80(H80), C81(H81), C83(H83), C88(H88),
  C90(H90), C91(H91), C92(H92), C96(H96), C98(H98), C99(H99), C100(H100),
 C101(H101), C102(H102), C103(H103), C105(H105), C106(H106), C114(H114)
5.b Idealised Me refined as rotating group:
 C39(H39A,H39B,H39C), C48(H48A,H48B,H48C), C57(H57A,H57B,H57C), C66(H66A,H66B,
 H66C), C75(H75A,H75B,H75C), C84(H84A,H84B,H84C), C104(H10A,H10B,H10C),
 C107(H10D,H10E,H10F)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              73232
_shelx_hkl_checksum              82552
_shelx_fab_checksum              98659
_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 3.943
_oxdiff_exptl_absorpt_empirical_full_min 0.322