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_1550198
_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 Ag34 F27 N6 O24 S20'
_chemical_formula_sum            'C162 H168 Ag34 F27 N6 O24 S20'
_chemical_formula_weight         7404.79
_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
_atom_sites_solution_primary     dual
_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                   30.3700(4)
_cell_length_b                   30.3700(4)
_cell_length_c                   39.4849(6)
_cell_measurement_reflns_used    10467
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      72.6240
_cell_measurement_theta_min      2.8210
_cell_volume                     31539.2(8)
_computing_cell_refinement       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.27b (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)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.983
_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    -28.00  27.00   0.50    3.00    --    0.00  57.00 -90.00  110
  2  \w     86.00 185.00   0.50   10.00    --   97.60  33.00  67.00  198
  3  \w     13.00  45.00   0.50   10.00    --   97.60 -82.00  30.00   64
  4  \w     54.00 135.00   0.50   10.00    --   97.60 -82.00  30.00  162
  5  \w     65.00 187.00   0.50   10.00    --   97.60  30.00 120.00  244
;
_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      -0.0240694000
_diffrn_orient_matrix_UB_12      -0.0175006000
_diffrn_orient_matrix_UB_13      -0.0353231000
_diffrn_orient_matrix_UB_21      0.0051160000
_diffrn_orient_matrix_UB_22      0.0524705000
_diffrn_orient_matrix_UB_23      -0.0060968000
_diffrn_orient_matrix_UB_31      0.0531107000
_diffrn_orient_matrix_UB_32      0.0191983000
_diffrn_orient_matrix_UB_33      -0.0154354000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0363
_diffrn_reflns_av_unetI/netI     0.0308
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_number            26916
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.261
_diffrn_reflns_theta_min         2.799
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    27.293
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.29929
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.27b (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    2.339
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             21210
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.988
_refine_diff_density_min         -1.165
_refine_diff_density_rms         0.183
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     469
_refine_ls_number_reflns         6929
_refine_ls_number_restraints     281
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0797
_refine_ls_R_factor_gt           0.0600
_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^)+(0.1128P)^2^+512.6708P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1731
_refine_ls_wR_factor_ref         0.1941
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5138
_reflns_number_total             6929
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8nr07714b2.cif
_cod_data_source_block           ag34
_cod_original_cell_volume        31539.2(10)
_cod_database_code               1550198
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C H O N Cu'
_chemical_oxdiff_usercomment     'C H O'
_shelx_estimated_absorpt_t_max   0.115
_shelx_estimated_absorpt_t_min   0.097
_reflns_odcompleteness_completeness 99.64
_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, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N1-C25
 1.45 with sigma of 0.01
 C7A-C2A
 1.4 with sigma of 0.01
 H12_$1-H26B
 2 with sigma of 0.01
 H26A-H25B
 1.9 with sigma of 0.01
 O1-H24
 1.65 with sigma of 0.01
 H5B-H20_$2
 2.43 with sigma of 0.01
 C7B-C3B \\sim C6B-C4B
 with sigma of 0.01
 C7A-C3A \\sim C6A-C4A
 with sigma of 0.01
 C9-C10 \\sim C10-C11 \\sim C12-C11 \\sim C13-C12 \\sim C13-C14 \\sim C9-C14
 with sigma of 0.01
 C17-C16 \\sim C18-C17 \\sim C19-C18 \\sim C20-C19 \\sim C20-C21 \\sim C21-C16
 with sigma of 0.01
 C16-C19 \\sim C17-C20 \\sim C18-C21
 with sigma of 0.01
 F6-C28 \\sim F5-C28 \\sim F4-C28
 with sigma of 0.01
 F5-F6 \\sim F6-F4
 with sigma of 0.01
 N1-C25 \\sim N1-C26
 with sigma of 0.01
 C5A-C6A \\sim C5A-C4A \\sim C3A-C4A \\sim C3A-C2A \\sim C7A-C2A \\sim C6A-C7A
 with sigma of 0.01
 C2A-C5A \\sim C3A-C6A \\sim C4A-C7A
 with sigma of 0.01
 C5A-C3A \\sim C6A-C2A
 with sigma of 0.01
 C7A-C5A \\sim C2A-C4A
 with sigma of 0.01
 C3B-C2B \\sim C3B-C4B \\sim C4B-C5B \\sim C6B-C5B \\sim C7B-C6B \\sim C7B-C2B
 with sigma of 0.01
 C2B-C5B \\sim C3B-C6B \\sim C4B-C7B
 with sigma of 0.01
 C5B-C3B \\sim C6B-C2B
 with sigma of 0.01
 F1-C23 \\sim F2-C23 \\sim F3-C23
 with sigma of 0.01
 F1-F2 \\sim F2-F3
 with sigma of 0.01
3. Restrained planarity
 C2A, C3A, C4A, C5A, C6A, C7A
 with sigma of 0.1
 C2B, C3B, C4B, C5B, C6B, C7B
 with sigma of 0.1
4. Rigid bond restraints
 C6A, C6B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N1, C24, C25, C26
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
C3A \\sim C3B \\sim C4A \\sim C4B: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
N1 \\sim C25 \\sim C26: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
O1 \\sim N1 \\sim C24: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C26) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F6) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F5) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C19) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F4) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C3A) \\sim Ueq, Uanis(C4A) \\sim Ueq, Uanis(C5B) \\sim Ueq, Uanis(C3B)
\\sim Ueq, Uanis(C5A) \\sim Ueq, Uanis(C7A) \\sim Ueq, Uanis(C2A) \\sim Ueq,
Uanis(C7B) \\sim Ueq, Uanis(C6A) \\sim Ueq, Uanis(C4B) \\sim Ueq, Uanis(C6B)
\\sim Ueq, Uanis(C2B) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C24) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F3) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C2A) = Uanis(C2B)
Uanis(C6B) = Uanis(C5B)
Uanis(C4B) = Uanis(C5A)
6. Others
 Fixed Sof: S4(0.33333) F4(0.5) F5(0.5) F6(0.5) H1AA(0.5) H1AB(0.5) H1BC(0.5)
 H1BD(0.5) C2A(0.5) C2B(0.5) C3A(0.5) H3A(0.5) C3B(0.5) H3B(0.5) C4A(0.5)
 H4A(0.5) C4B(0.5) H4B(0.5) C5A(0.5) H5A(0.5) C5B(0.5) H5B(0.5) C6A(0.5)
 H6A(0.5) C6B(0.5) H6B(0.5) C7A(0.5) H7A(0.5) C7B(0.5) H7B(0.5)
7.a Riding coordinates:
 C25(H25A,H25B,H25C)
7.b Secondary CH2 refined with riding coordinates:
 C1(H1AA,H1AB), C1(H1BC,H1BD), C8(H8A,H8B), C15(H15A,H15B)
7.c Aromatic/amide H refined with riding coordinates:
 C3A(H3A), C3B(H3B), C4A(H4A), C4B(H4B), C5A(H5A), C5B(H5B), C6A(H6A),
 C6B(H6B), C7A(H7A), C7B(H7B), C10(H10), C11(H11), C12(H12), C13(H13), C14(H14),
  C17(H17), C18(H18), C19(H19), C20(H20), C21(H21), C24(H24)
7.d Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C)
;
_shelx_res_checksum              96979
_shelx_hkl_checksum              330
_shelx_fab_checksum              66185
_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 3.209
_oxdiff_exptl_absorpt_empirical_full_min 0.498