Unexpected structural transformation into noria-like Ag<sub>13</sub> metal clusters and a copper-doping induced boost in photoluminescence.
Peng, Su-Kao; Lu, Zhou; Xie, Mo; Huang, Yong-Liang; Luo, Dong; Wang, Jia-Nan; Zhu, Xiao-Wei; Li, Xue; Zhou, Xiao-Ping; Li, Dan; Chemical communications (Cambridge, England) 56 (2020) 4789–4792; doi:10.1039/c9cc09818f

data_7126066
_publ_section_title
;
 Unexpected structural transformation into noria-like Ag<sub>13</sub>
 metal clusters and a copper-doping induced boost in photoluminescence.
;
_journal_issue                   35
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              4789
_journal_page_last               4792
_journal_paper_doi               10.1039/c9cc09818f
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C94 H46 Ag12.05 Cu0.9 F36 N12'
_chemical_formula_sum            'C94 H46 Ag11.96 Cu F36 N12'
_chemical_formula_weight         3381.09
_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
_audit_creation_date             2019-01-23
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-02-26 deposited with the CCDC.	2020-02-26 downloaded from the CCDC.
;
_cell_angle_alpha                60.608(3)
_cell_angle_beta                 65.701(3)
_cell_angle_gamma                61.289(3)
_cell_formula_units_Z            1
_cell_length_a                   15.5019(4)
_cell_length_b                   15.7093(4)
_cell_length_c                   15.9495(6)
_cell_measurement_reflns_used    10969
_cell_measurement_temperature    100(10)
_cell_measurement_theta_max      75.7240
_cell_measurement_theta_min      5.1270
_cell_volume                     2888.52(18)
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(10)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0332
_diffrn_reflns_av_unetI/netI     0.0393
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.951
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            30961
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.239
_diffrn_reflns_theta_min         5.558
_exptl_absorpt_coefficient_mu    16.992
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65632
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.944
_exptl_crystal_description       lump
_exptl_crystal_F_000             1609
_refine_diff_density_max         3.833
_refine_diff_density_min         -1.735
_refine_diff_density_rms         0.194
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     771
_refine_ls_number_reflns         11777
_refine_ls_number_restraints     359
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0955
_refine_ls_R_factor_gt           0.0876
_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^)+(0.1496P)^2^+16.6741P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2459
_refine_ls_wR_factor_ref         0.2533
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9790
_reflns_number_total             11777
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc09818f2.cif
_cod_data_source_block           Ag118Cu12
_cod_depositor_comments
'Adding full bibliography for 7126064--7126066.cif.'
_cod_original_cell_volume        2888.55(19)
_cod_database_code               7126066
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Shared sites
{Ag07, Cu0A}
{Ag05, Cu1A}
{Cu12, Ag06}
3. Restrained distances
 C2-C1 = C1-C2A
 1.2 with sigma of 0.02
 C17-C2A
 1.5 with sigma of 0.02
 C1-C17
 2.7 with sigma of 0.02
4. Rigid bond restraints
 C01P, C69, C66, C19, C020, C2AA
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C59, C53, C35, C29, C28, C49
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C12, C64, C65, C75, C17, C24
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C33, C54, C48, C56, C39, C61
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C1, C2A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
C01P \\sim C69 \\sim C66 \\sim C19 \\sim C020 \\sim C2AA: within 1.7A with
sigma of 0.04 and sigma for terminal atoms of 0.08
C59 \\sim C53 \\sim C35 \\sim C29 \\sim C28 \\sim C49: within 1.7A with sigma
of 0.04 and sigma for terminal atoms of 0.08
C12 \\sim C64 \\sim C65 \\sim C75 \\sim C17 \\sim C24: within 1.7A with sigma
of 0.04 and sigma for terminal atoms of 0.08
C33 \\sim C54 \\sim C48 \\sim C56 \\sim C39 \\sim C61: within 1.7A with sigma
of 0.04 and sigma for terminal atoms of 0.08
C1 \\sim C2A: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
Uanis(C01P) \\sim Ueq, Uanis(C69) \\sim Ueq, Uanis(C66) \\sim Ueq, Uanis(C19)
\\sim Ueq, Uanis(C020) \\sim Ueq, Uanis(C2AA) \\sim Ueq: with sigma of 0.1 and
sigma for terminal atoms of 0.2
Uanis(C59) \\sim Ueq, Uanis(C53) \\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(C29)
\\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C49) \\sim Ueq: with sigma of 0.1 and
sigma for terminal atoms of 0.2
Uanis(C12) \\sim Ueq, Uanis(C64) \\sim Ueq, Uanis(C65) \\sim Ueq, Uanis(C75)
\\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C24) \\sim Ueq: with sigma of 0.1 and
sigma for terminal atoms of 0.2
Uanis(C33) \\sim Ueq, Uanis(C54) \\sim Ueq, Uanis(C48) \\sim Ueq, Uanis(C56)
\\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(C61) \\sim Ueq: with sigma of 0.1 and
sigma for terminal atoms of 0.2
Uanis(C1) \\sim Ueq, Uanis(C2A) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
Uanis(Ag07) = Uanis(Cu0A)
Uanis(Ag05) = Uanis(Cu1A)
Uanis(Ag06) = Uanis(Cu12)
Uanis(Cu12) = Uanis(Ag06)
6. Others
 Sof(Ag06)=1-FVAR(1)
 Sof(Cu12)=FVAR(1)
 Fixed Sof: Ag05(0.9) Ag07(0.25) C01P(0.5) H01P(0.5) C69(0.5) H69(0.5)
 C66(0.5) H66(0.5) C19(0.5) H19(0.5) C020(0.5) H020(0.5) C2AA(0.5) C12(0.5)
 H12(0.5) C64(0.5) H64(0.5) C65(0.5) H65(0.5) C75(0.5) H75(0.5) C17(0.5)
 C24(0.5) H24(0.5) C33(0.5) H33(0.5) C54(0.5) H54(0.5) C48(0.5) C56(0.5)
 H56(0.5) C39(0.5) H39(0.5) C61(0.5) H61(0.5) C59(0.5) H59(0.5) C53(0.5)
 C35(0.5) H35(0.5) C29(0.5) H29(0.5) C28(0.5) H28(0.5) C49(0.5) H49(0.5)
 Cu0A(0.25) Cu1A(0.1) C2(0.5) C2A(0.5)
7.a Aromatic/amide H refined with riding coordinates:
 C00W(H00W), C011(H011), C016(H016), C01D(H01D), C01F(H01F), C01J(H01J),
 C01M(H01M), C01N(H01N), C01P(H01P), C69(H69), C66(H66), C19(H19), C020(H020),
 C01R(H01R), C01S(H01S), C01T(H01T), C01V(H01V), C01X(H01X), C12(H12), C64(H64),
  C65(H65), C75(H75), C24(H24), C33(H33), C54(H54), C56(H56), C39(H39),
 C61(H61), C59(H59), C35(H35), C29(H29), C28(H28), C49(H49)
7.b Fitted hexagon refined as free rotating group:
 C01P(C69,C66,C19,C020,C2AA), C12(C64,C65,C75,C17,C24), C33(C54,C48,C56,C39,
 C61), C59(C53,C35,C29,C28,C49)
;
_shelx_res_checksum              88494
_shelx_fab_checksum              94409
_olex2_submission_special_instructions 'No special instructions were received'