Multi-Ligand-Directed Synthesis of Chiral Silver Nanoclusters
Zou, Xuejuan; Jin, Shan; Du, Wenjun; Li, Yangfeng; Wang, Shuxin; li, peng; Zhu, Manzhou; Nanoscale  (2017) –; doi:10.1039/C7NR06338E

data_1547468
_publ_section_title
;
 Multi-Ligand-Directed Synthesis of Chiral Silver Nanoclusters
;
_journal_name_full               Nanoscale
_journal_paper_doi               10.1039/C7NR06338E
_journal_year                    2017
_chemical_formula_moiety         'C164 H232 Ag51 Br6 P8 S16, 3(F6 Sb)'
_chemical_formula_sum            'C164 H232 Ag51 Br6 F18 P8 S16 Sb3'
_chemical_formula_weight         9652.28
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-07-24
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_cell_angle_alpha                90
_cell_angle_beta                 95.223(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   34.3699(8)
_cell_length_b                   36.2763(9)
_cell_length_c                   26.3392(6)
_cell_measurement_reflns_used    9466
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.46
_cell_measurement_theta_min      2.53
_cell_volume                     32703.7(13)
_computing_cell_refinement       'SAINT V8.35A (?, 2016)'
_computing_data_reduction        'SAINT V8.35A (?, 2016)'
_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_temperature      150
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0761
_diffrn_reflns_av_unetI/netI     0.0657
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       47
_diffrn_reflns_limit_k_min       -47
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            190096
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.512
_diffrn_reflns_theta_min         0.818
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.126
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6052
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1011 before and 0.0625 after correction.
The Ratio of minimum to maximum transmission is 0.8116.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.960
_exptl_crystal_description       block
_exptl_crystal_F_000             18056
_refine_diff_density_max         4.077
_refine_diff_density_min         -4.904
_refine_diff_density_rms         0.446
_refine_ls_extinction_coef       0.000060(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/4 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1172
_refine_ls_number_reflns         37525
_refine_ls_number_restraints     1524
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0996
_refine_ls_R_factor_gt           0.0657
_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^)+(0.1281P)^2^+490.4971P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1951
_refine_ls_wR_factor_ref         0.2216
_reflns_Friedel_coverage         0.000
_reflns_number_gt                25086
_reflns_number_total             37525
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7nr06338e3.cif
_cod_data_source_block           20161103b_0m_sq
_cod_depositor_comments
;
 Removing the "&#x00EF;&#x00BF;&#x00BD;&#x00EF;&#x00BF;&#x00BD;" string
 from the beginning and end of some data values.

 Antanas Vaitkus,
 2018-08-09
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_cod_database_code               1547468
_shelx_shelxl_version_number     2016/4
_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. Uiso/Uaniso restraints and constraints
F019 \\sim F01B \\sim F01C \\sim F01E \\sim F01H \\sim F01J \\sim F03G \\sim
F03H \\sim F03M \\sim F03N \\sim F28 \\sim F37: within 3.8A with sigma of 0.01
and sigma for terminal atoms of 0.02
C01D \\sim C01N \\sim C02O \\sim C023 \\sim C02I \\sim C02K \\sim C01F \\sim
C01G \\sim C01K \\sim C01T \\sim C02A \\sim C01W \\sim C01L \\sim C01I \\sim
C01P \\sim C020 \\sim C02Q \\sim C02F \\sim C01S \\sim C01M \\sim C01O \\sim
C01Q \\sim C02H \\sim C02S \\sim C022 \\sim C02L \\sim C029 \\sim C01R \\sim
C01U \\sim C01V \\sim C01Y \\sim C01Z \\sim C021 \\sim C024 \\sim C025 \\sim
C026 \\sim C027 \\sim C028 \\sim C039 \\sim C03R \\sim C33 \\sim C03L \\sim
C03F \\sim C02B \\sim C02C \\sim C02D \\sim C02E \\sim C02P \\sim C034 \\sim
C033 \\sim C03D \\sim C02W \\sim C02G \\sim C02J \\sim C02M \\sim C02N \\sim
C02R \\sim C035 \\sim C38 \\sim C03O \\sim C03I \\sim C02Z \\sim C02T \\sim
C02U \\sim C02V \\sim C02X \\sim C02Y \\sim C030 \\sim C031 \\sim C032 \\sim
C036 \\sim C037 \\sim C038 \\sim C03A \\sim C03B \\sim C03C \\sim C03E \\sim
C03J \\sim C03K \\sim C03P \\sim C03S \\sim C30: within 3.8A with sigma of 0.01
and sigma for terminal atoms of 0.02
3. Others
 Fixed Sof: Sb0W(0.5) F03G(0.5) F03H(0.5) F03M(0.5) F03N(0.5) F28(0.5) F37(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C01F(H01A,H01B), C01M(H01C,H01D)
4.b Aromatic/amide H refined with riding coordinates:
 C01N(H01N), C02O(H02O), C023(H023), C02I(H02I), C02K(H02K), C01K(H01K),
 C01T(H01T), C02A(H02A), C01W(H01W), C01L(H01L), C01P(H01P), C020(H020),
 C02Q(H02Q), C02F(H02F), C01S(H01S), C02H(H02H), C02S(H02S), C022(H022),
 C02L(H02L), C029(H029), C024(H024), C039(H039), C03R(H03R), C33(H33),
 C03L(H03L), C03F(H03F), C02B(H02M), C02P(H02P), C034(H034), C033(H033),
 C03D(H03D), C02W(H02W), C035(H035), C38(H38), C03O(H03O), C03I(H03I),
 C02Z(H02), C02X(H3AA), C030(H030), C038(H038)
4.c Fitted hexagon refined as free rotating group:
 C01D(C01N,C02O,C023,C02I,C02K), C01G(C01K,C01T,C02A,C01W,C01L), C01I(C01P,
 C020,C02Q,C02F,C01S), C01Q(C02H,C02S,C022,C02L,C029), C028(C039,C03R,C33,C03L,
 C03F), C02E(C02P,C034,C033,C03D,C02W), C02R(C035,C38,C03O,C03I,C02Z)
4.d Idealised Me refined as rotating group:
 C01O(H01E,H01F,H01G), C01R(H01H,H01I,H01J), C025(H02B,H02C,H02D), C027(H02E,
 H02G,H02J), C02G(H02N,H02R,H02T), C02J(H02U,H02V,H02X), C02M(H02Y,H,HA),
 C02N(H02Z,HB,HC), C02T(H0AA,HD,HE), C02U(H1AA,HF,HG), C02V(H2AA,HH,HI),
 C02Y(H4AA,HJ,HK), C031(H03A,H03B,H03C), C032(H03E,H03G,H03H), C036(H03J,H03K,
 H03M), C03A(H03N,H03P,H03Q), C03B(H03S,H03T,H03U), C03C(H03V,H03W,H03X),
 C03E(H03Y,HL,HM), C03J(H03Z,HN,HO), C03K(H03,HP,HQ), C03P(H5AA,HR,HS),
 C03S(H6AA,HT,HU), C30(H30A,H30B,H30C)
;
_shelx_res_checksum              71913
_shelx_hkl_checksum              87448
_shelx_fab_checksum              63162
_olex2_submission_special_instructions 'No special instructions were received'