New stable isomorphous Ag34 and Ag33Au nanoclusters with open shell electronic structure
Zang, Shuang-Quan; Xi, Xiao-Juan; Yang, Jin-Sen; Wang, Jia-Yin; Dong, Xi-Yan; Nanoscale  (2018) –; doi:10.1039/C8NR07714B

data_1550199
_publ_section_title
;
 New stable isomorphous Ag34 and Ag33Au nanoclusters with open shell
 electronic structure
;
_journal_name_full               Nanoscale
_journal_paper_doi               10.1039/C8NR07714B
_journal_year                    2018
_chemical_formula_moiety         'C162 H168 Ag33 Au1 F27 N6 O24 S20'
_chemical_formula_sum            'C162 H168 Ag33 Au F27 N6 O24 S20'
_chemical_formula_weight         7493.89
_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_Hall           '-R 3 2"c'
_space_group_name_H-M_alt        'R -3 c'
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2018-09-13
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-09-17 deposited with the CCDC.
2018-11-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   30.3706(5)
_cell_length_b                   30.3706(5)
_cell_length_c                   39.4126(8)
_cell_measurement_reflns_used    7332
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      71.7110
_cell_measurement_theta_min      2.8050
_cell_volume                     31482.7(10)
_computing_cell_refinement       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.986
_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    -29.00  -1.00   0.50    2.50    --    0.00  38.00   0.00   56
  2  \w     33.00  84.00   0.50    2.50    --    0.00  38.00   0.00  102
  3  \w     16.00  45.00   0.50   11.00    --   97.60 -61.00 -60.00   58
  4  \w     87.00 180.00   0.50   11.00    --   97.60  45.00   0.00  186
  5  \w     95.00 184.00   0.50   11.00    --   97.60  45.00 -30.00  178
  6  \w     66.00  95.00   0.50   11.00    --   97.60 -61.00 -60.00   58
  7  \w      9.00 127.00   0.50   11.00    --   97.60 -61.00  30.00  236
;
_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      -0.0542727000
_diffrn_orient_matrix_UB_12      -0.0219695000
_diffrn_orient_matrix_UB_13      0.0141107000
_diffrn_orient_matrix_UB_21      0.0068740000
_diffrn_orient_matrix_UB_22      -0.0388844000
_diffrn_orient_matrix_UB_23      0.0209750000
_diffrn_orient_matrix_UB_31      0.0209100000
_diffrn_orient_matrix_UB_32      0.0379324000
_diffrn_orient_matrix_UB_33      0.0298200000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0439
_diffrn_reflns_av_unetI/netI     0.0370
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            31150
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.291
_diffrn_reflns_theta_min         2.802
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    27.889
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.43439
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.28b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    2.372
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             21402
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.14
_refine_diff_density_max         2.066
_refine_diff_density_min         -1.328
_refine_diff_density_rms         0.155
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     519
_refine_ls_number_reflns         6945
_refine_ls_number_restraints     312
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0796
_refine_ls_R_factor_gt           0.0536
_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^)+(0.0902P)^2^+417.4030P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1472
_refine_ls_wR_factor_ref         0.1718
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4817
_reflns_number_total             6945
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8nr07714b2.cif
_cod_data_source_block           ag33au
_cod_original_cell_volume        31482.8(12)
_cod_database_code               1550199
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C H Ag Au F N O S'
_chemical_oxdiff_usercomment     'C H Ag Au F N O S'
_shelx_estimated_absorpt_t_max   0.112
_shelx_estimated_absorpt_t_min   0.095
_reflns_odcompleteness_completeness 99.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O3-C22A \\sim O3-C22B
 with sigma of 0.01
 F5-C28 \\sim F6-C28 \\sim F4-C28
 with sigma of 0.01
 F4-F6 \\sim F6-F5
 with sigma of 0.01
 C21B-C16B \\sim C21B-C20B \\sim C19B-C20B \\sim C19B-C18B \\sim C17B-C18B
\\sim C16A-C17A \\sim C17A-
 C18A \\sim C19A-C18A \\sim C20A-C19A \\sim C20A-C21A \\sim C16A-C21A
 with sigma of 0.01
 C16B-C19B \\sim C17B-C20B \\sim C18B-C21B \\sim C16A-C19A \\sim C21A-C18A
\\sim C20A-C17A
 with sigma of 0.01
 C16A-C17B \\sim C19A-C18B \\sim C20B-C21B
 with sigma of 0.01
 S1-C15A \\sim S1-C15B
 with sigma of 0.01
 C6-C5 \\sim C7-C6 \\sim C7-C2 \\sim C3-C2 \\sim C4-C3 \\sim C5-C4
 with sigma of 0.01
3. Restrained planarity
 C16B, C21B, C20B, C19B, C18B, C17B
 with sigma of 0.1
 C16A, C17A, C18A, C19A, C20A, C21A
 with sigma of 0.1
4. Rigid bond restraints
 C17B, C18B, C19B, C20B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
N1 \\sim C24A \\sim N1 \\sim C24B: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
C17B \\sim C18B \\sim C19B \\sim C20B: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
S1 \\sim C15A \\sim S1 \\sim C15B: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
N1 \\sim C23A \\sim N1 \\sim C23B: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C28) \\sim Ueq, Uanis(C22B) \\sim Ueq, Uanis(C22A) \\sim Ueq, Uanis(F5)
\\sim Ueq, Uanis(F6) \\sim Ueq, Uanis(F4) \\sim Ueq, Uanis(C21B) \\sim Ueq,
Uanis(F2) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C17A) \\sim Ueq, Uanis(C16B)
\\sim Ueq, Uanis(C19A) \\sim Ueq, Uanis(C21A) \\sim Ueq, Uanis(C17B) \\sim Ueq,
Uanis(C18B) \\sim Ueq, Uanis(C20A) \\sim Ueq, Uanis(C18A) \\sim Ueq,
Uanis(C19B) \\sim Ueq, Uanis(C16A) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(O3)
\\sim Ueq, Uanis(Ag3) \\sim Ueq, Uanis(Ag5) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C19A) = Uanis(C17A)
6. Others
 Fixed Sof: C15A(0.5) H15A(0.5) H15B(0.5) C16A(0.5) C17A(0.5) H17A(0.5)
 C18A(0.5) H18A(0.5) C19A(0.5) H19A(0.5) C20A(0.5) H20A(0.5) C21A(0.5)
 H21A(0.5) C15B(0.5) H15C(0.5) H15D(0.5) C16B(0.5) C17B(0.5) H17B(0.5)
 C18B(0.5) H18B(0.5) C19B(0.5) H19B(0.5) C20B(0.5) H20B(0.5) C21B(0.5)
 H21B(0.5) C22A(0.5) H22A(0.5) C22B(0.5) H22B(0.5) C23A(0.5) H23A(0.5)
 H23B(0.5) H23C(0.5) C24A(0.5) H24A(0.5) H24B(0.5) H24C(0.5) C23B(0.5)
 H23D(0.5) H23E(0.5) H23F(0.5) C24B(0.5) H24D(0.5) H24E(0.5) H24F(0.5) F4(0.5)
 F5(0.5) F6(0.5) S4(0.33333)
7.a Riding coordinates:
 C23B(H23D,H23E,H23F)
7.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C8(H8A,H8B), C15A(H15A,H15B), C15B(H15C,H15D)
7.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C10(H10), C11(H11), C12(H12),
 C13(H13), C14(H14), C17A(H17A), C18A(H18A), C19A(H19A), C20A(H20A), C21A(H21A),
  C17B(H17B), C18B(H18B), C19B(H19B), C20B(H20B), C21B(H21B), C22A(H22A),
 C22B(H22B)
7.d Idealised Me refined as rotating group:
 C23A(H23A,H23B,H23C), C24A(H24A,H24B,H24C), C24B(H24D,H24E,H24F)
;
_shelx_res_checksum              68879
_shelx_hkl_checksum              90720
_shelx_fab_checksum              53954
_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 2.346
_oxdiff_exptl_absorpt_empirical_full_min 0.627