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_1550197
_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         'C154 H154 Ag30 F24 N4 O28 S20'
_chemical_formula_sum            'C154 H154 Ag30 F24 N4 O28 S20'
_chemical_formula_weight         6842.10
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_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                 94.9090(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   19.8067(2)
_cell_length_b                   21.3657(2)
_cell_length_c                   24.6098(3)
_cell_measurement_reflns_used    19502
_cell_measurement_temperature    200.00(10)
_cell_measurement_theta_max      73.9350
_cell_measurement_theta_min      3.6380
_cell_volume                     10376.27(19)
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      200.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.959
_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    -89.00 -40.00   0.50    0.50    --    0.00 -38.00-180.00   98
  2  \w    -38.00  19.00   0.50    0.50    --    0.00 -38.00-180.00  114
  3  \w      6.00 115.00   0.50    0.80    --   95.20 -15.00-150.00  218
  4  \w      7.00 126.00   0.50    0.80    --   95.20 -82.00 -90.00  238
  5  \w     20.00 117.00   0.50    0.80    --   95.20 -61.00 -90.00  194
  6  \w    106.00 185.00   0.50    0.80    --   95.20  30.00-180.00  158
  7  \w     68.00 167.00   0.50    0.80    --   95.20  15.00 120.00  198
;
_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      -0.0357828000
_diffrn_orient_matrix_UB_12      -0.0060425000
_diffrn_orient_matrix_UB_13      -0.0578473000
_diffrn_orient_matrix_UB_21      -0.0629188000
_diffrn_orient_matrix_UB_22      -0.0274414000
_diffrn_orient_matrix_UB_23      0.0240398000
_diffrn_orient_matrix_UB_31      -0.0292804000
_diffrn_orient_matrix_UB_32      0.0664030000
_diffrn_orient_matrix_UB_33      0.0046972000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0575
_diffrn_reflns_av_unetI/netI     0.0717
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            48870
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.292
_diffrn_reflns_theta_min         2.743
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    24.681
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.29148
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.190
_exptl_crystal_description       block
_exptl_crystal_F_000             6552
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.895
_refine_diff_density_min         -2.606
_refine_diff_density_rms         0.179
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1228
_refine_ls_number_reflns         20293
_refine_ls_number_restraints     1716
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0790
_refine_ls_R_factor_gt           0.0584
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0734P)^2^+31.3488P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1537
_refine_ls_wR_factor_ref         0.1616
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15166
_reflns_number_total             20293
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8nr07714b2.cif
_cod_data_source_block           ag30
_cod_database_code               1550197
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_usercomment     'C H Ag F N O S'
_shelx_estimated_absorpt_t_max   0.130
_shelx_estimated_absorpt_t_min   0.095
_reflns_odcompleteness_completeness 99.10
_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
 H13_$1-H33
 2.45 with sigma of 0.005
 F7A-C67 \\sim F8B-C67 \\sim F8A-C67 \\sim F9B-C67 \\sim F9A-C67 \\sim F7B-C67
 with sigma of 0.01
 F4A-C71 \\sim F4B-C71 \\sim F5A-C71 \\sim F5B-C71 \\sim F6A-C71
 with sigma of 0.01
 N1-C76 \\sim N1-C77 \\sim N2-C73 \\sim N2-C74
 with sigma of 0.01
 F2A-C65 \\sim F3B-C65 \\sim F3A-C65 \\sim F1B-C65 \\sim F1A-C65 \\sim F2B-C65
 with sigma of 0.01
 C14-C9 \\sim C10-C9 \\sim C11-C10 \\sim C11-C12 \\sim C13-C12 \\sim C13-C14
\\sim C44-C45 \\sim C46-C45 ~
 C47-C46 \\sim C47-C48 \\sim C48-C49 \\sim C49-C44 \\sim C28-C27 \\sim C26-C27
\\sim C26-C25 \\sim C25-C24
 \\sim C24-C23 \\sim C28-C23 \\sim C4-C5 \\sim C5-C6 \\sim C6-C7 \\sim C7-C2
\\sim C3-C2 \\sim C4-C3 \\sim C20-C21
 \\sim C21-C16 \\sim C18-C17 \\sim C17-C16 \\sim C18-C19 \\sim C19-C20 \\sim
C31-C30 \\sim C35-C30 \\sim C34-
 C35 \\sim C33-C34 \\sim C33-C32 \\sim C32-C31 \\sim C63-C58 \\sim C62-C63
\\sim C61-C62 \\sim C61-C60 ~
 C60-C59 \\sim C59-C58 \\sim C42-C37 \\sim C41-C42 \\sim C41-C40 \\sim C39-C40
\\sim C39-C38 \\sim C38-C37
 \\sim C56-C55 \\sim C54-C55 \\sim C53-C54 \\sim C53-C52 \\sim C52-C51 \\sim
C56-C51
 with sigma of 0.01
3. Rigid bond restraints
 S6, O5, O6, O7, O8
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
F7B \\sim F9A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
S6 \\sim O5 \\sim O6 \\sim O7 \\sim O8: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
Uanis(F6B) \\sim Ueq, Uanis(F10) \\sim Ueq, Uanis(F2A) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.01
Uanis(O8) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C26)
\\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(F3B) \\sim Ueq,
Uanis(F2B) \\sim Ueq, Uanis(F1A) \\sim Ueq, Uanis(C41) \\sim Ueq, Uanis(C40)
\\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(F7A) \\sim Ueq, Uanis(F8B) \\sim Ueq,
Uanis(F8A) \\sim Ueq, Uanis(F9B) \\sim Ueq, Uanis(F7B) \\sim Ueq, Uanis(F9A)
\\sim Ueq, Uanis(C46) \\sim Ueq, Uanis(C47) \\sim Ueq, Uanis(C48) \\sim Ueq,
Uanis(C49) \\sim Ueq, Uanis(F6B) \\sim Ueq, Uanis(F6A) \\sim Ueq, Uanis(F5B)
\\sim Ueq, Uanis(F5A) \\sim Ueq, Uanis(F4B) \\sim Ueq, Uanis(F4A) \\sim Ueq,
Uanis(C27) \\sim Ueq, Uanis(F1B) \\sim Ueq, Uanis(C42) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(F3A) = Uanis(F3B)
Uanis(O6) = Uanis(O7)
Uanis(C16) = Uanis(C19) = Uanis(C18) = Uanis(C20)
5. Others
 Sof(F4B)=Sof(F5B)=Sof(F6B)=1-FVAR(1)
 Sof(F4A)=Sof(F5A)=Sof(F6A)=FVAR(1)
 Sof(F1B)=Sof(F2B)=Sof(F3B)=1-FVAR(2)
 Sof(F1A)=Sof(F2A)=Sof(F3A)=FVAR(2)
 Fixed Sof: F7A(0.4) F7B(0.6) F8A(0.4) F8B(0.6) F9A(0.6) F9B(0.4)
6.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C8(H8A,H8B), C15(H15A,H15B), C22(H22A,H22B), C29(H29A,H29B),
 C36(H36A,H36B), C43(H43A,H43B), C50(H50A,H50B), C57(H57A,H57B)
6.b 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), C17(H17), C18(H18), C19(H19), C20(H20), C21(H21), C24(H24),
  C25(H25), C26(H26), C27(H27), C28(H28), C31(H31), C32(H32), C33(H33),
 C34(H34), C35(H35), C38(H38), C39(H39), C40(H40), C41(H41), C42(H42), C45(H45),
  C46(H46), C47(H47), C48(H48), C49(H49), C52(H52), C53(H53), C54(H54),
 C55(H55), C56(H56), C59(H59), C60(H60), C61(H61), C62(H62), C63(H63), C72(H72),
  C75(H75)
6.c Idealised Me refined as rotating group:
 C73(H73A,H73B,H73C), C74(H74A,H74B,H74C), C76(H76A,H76B,H76C), C77(H77A,H77B,
 H77C)
;
_shelx_res_checksum              95909
_shelx_hkl_checksum              80773
_shelx_fab_checksum              67840
_platon_squeeze_void_probe_radius 1.20
_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 2.845
_oxdiff_exptl_absorpt_empirical_full_min 0.548