Total structural determination of alloyed Au<sub>15.37</sub>Cu<sub>16.63</sub>(S-Adm)<sub>20</sub> nanoclusters with double superatomic chains.
Tang, Li; Deng, Shiyao; Wang, Shuxin; Pei, Yong; Zhu, Manzhou; Chemical communications (Cambridge, England) 57 (2021) 2017–2020; doi:10.1039/d0cc07482a

data_7127871
_publ_section_title
;
 Total structural determination of alloyed
 Au<sub>15.37</sub>Cu<sub>16.63</sub>(S-Adm)<sub>20</sub> nanoclusters
 with double superatomic chains.
;
_journal_issue                   16
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              2017
_journal_page_last               2020
_journal_paper_doi               10.1039/d0cc07482a
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety
'C200 H300 Au15.373 Cu16.627 S20, 1[CH2Cl2], 3[C4H10O]'
_chemical_formula_sum            'C213 H332 Au15.37 Cl2 Cu16.63 O3 S20'
_chemical_formula_weight         7736.91
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2019-04-15
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-12-23 deposited with the CCDC.	2021-01-15 downloaded from the CCDC.
;
_cell_angle_alpha                103.748(4)
_cell_angle_beta                 110.733(4)
_cell_angle_gamma                93.756(4)
_cell_formula_units_Z            1
_cell_length_a                   17.4596(9)
_cell_length_b                   18.8819(10)
_cell_length_c                   19.6255(10)
_cell_measurement_reflns_used    37934
_cell_measurement_temperature    120
_cell_measurement_theta_max      71.70
_cell_measurement_theta_min      2.97
_cell_volume                     5797.3(6)
_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_temperature      120
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_R_equivalents  0.0985
_diffrn_reflns_av_unetI/netI     0.1702
_diffrn_reflns_Laue_measured_fraction_full 0.960
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            49313
_diffrn_reflns_point_group_measured_fraction_full 0.960
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        67.500
_diffrn_reflns_theta_max         67.500
_diffrn_reflns_theta_min         2.972
_exptl_absorpt_coefficient_mu    21.334
_exptl_absorpt_correction_T_max  0.9811
_exptl_absorpt_correction_T_min  0.3484
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE LANA, absorption correction by scaling of reflection intensities.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(\m~2~-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
Afterwards a spherical absorption correction was performed within STOE LANA.
;
_exptl_crystal_colour            'dark black'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    2.128
_exptl_crystal_description       block
_exptl_crystal_F_000             3516
_exptl_crystal_preparation       Luminescent
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.01
_refine_diff_density_max         5.965
_refine_diff_density_min         -5.120
_refine_diff_density_rms         0.433
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1137
_refine_ls_number_reflns         20077
_refine_ls_number_restraints     2710
_refine_ls_restrained_S_all      0.934
_refine_ls_R_factor_all          0.1261
_refine_ls_R_factor_gt           0.0856
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2071
_refine_ls_wR_factor_ref         0.2247
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10512
_reflns_number_total             20077
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc07482a2.cif
_cod_data_source_block           1
_cod_depositor_comments          'Adding full bibliography for 7127871.cif.'
_cod_original_cell_volume        5797.3(5)
_cod_database_code               7127871
_shelx_shelxl_version_number     2016/4
_shelx_estimated_absorpt_t_max   0.815
_shelx_estimated_absorpt_t_min   0.224
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Shared sites
{Cu9, Au9}
{Cu8, Au8}
3. Restrained distances
 H01F_$1-H01F_$2
 2.1 with sigma of 0.01
 C2-C10
 1.46 with sigma of 0.01
 C025-C012
 1.45 with sigma of 0.01
 C038-C02Y
 1.45 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
C00R \\sim C00S \\sim C00T \\sim C00U \\sim C00V \\sim C00W \\sim C00X \\sim
C00Y \\sim C00Z \\sim C010 \\sim C011 \\sim C012 \\sim C013 \\sim C014 \\sim
C015 \\sim C016 \\sim C017 \\sim C018 \\sim C019 \\sim C01A \\sim C01B \\sim
C01C \\sim C01D \\sim C01E \\sim C01F \\sim C01G \\sim C01H \\sim C01I \\sim
C01J \\sim C01K \\sim C01L \\sim C01M \\sim C01N \\sim C01O \\sim C01P \\sim
C01Q \\sim C01R \\sim C01S \\sim C01T \\sim C01U \\sim C01V \\sim C01W \\sim
C01X \\sim C01Y \\sim C020 \\sim C021 \\sim C022 \\sim C023 \\sim C024 \\sim
C025 \\sim C026 \\sim C027 \\sim C028 \\sim C029 \\sim C02A \\sim C02B \\sim
C02C \\sim C02D \\sim C02E \\sim C02F \\sim C02G \\sim C02H \\sim C02I \\sim
C02J \\sim C02K \\sim C02L \\sim C02M \\sim C02N \\sim C02O \\sim C02Q \\sim
C02R \\sim C02S \\sim C02T \\sim C02U \\sim C02V \\sim C02W \\sim C02X \\sim
C02Y \\sim C02Z \\sim C031 \\sim C033 \\sim C034 \\sim C036 \\sim C038 \\sim
C03A \\sim C03B \\sim C03C \\sim C03E \\sim C03F \\sim C03G \\sim C2 \\sim C4
\\sim C6 \\sim C8 \\sim C5 \\sim C0AA \\sim C9 \\sim C10 \\sim C7 \\sim C1AA:
within 3.8A with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Cu9) = Uanis(Au9)
Uanis(Cu8) = Uanis(Au8)
5. Others
 Sof(Au9)=1-FVAR(1)
 Sof(Cu9)=FVAR(1)
 Sof(Au8)=1-FVAR(2)
 Sof(Cu8)=FVAR(2)
6.a Ternary CH refined with riding coordinates:
 C012(H012), C01B(H01Q), C01D(H01T), C01F(H01W), C01G(H01X), C01L(H1AA),
 C01M(H2AA), C01T(H8AA), C01V(H0BA), C01W(H1BA), C01X(H2BA), C022(H022),
 C023(H023), C029(H029), C02B(H02Q), C02F(H02X), C02I(H02Z), C02K(H4BA),
 C02O(H8BA), C02R(H0CA), C02T(H2CA), C02W(H5CA), C02Z(H8CA), C031(H031),
 C036(H036), C038(H038), C03G(H03O), C4(H4), C0AA(H0AB), C7(H7)
6.b Secondary CH2 refined with riding coordinates:
 C00R(H00A,H00B), C00W(H00C,H00D), C00Y(H00E,H00F), C00Z(H00G,H00H), C010(H01A,
 H01B), C011(H01C,H01D), C013(H01E,H01F), C014(H01G,H01H), C015(H01I,H01J),
 C016(H01K,H01L), C017(H01M,H01N), C01A(H01O,H01P), C01C(H01R,H01S), C01E(H01U,
 H01V), C01H(H01Y,H), C01I(H01Z,HA), C01J(H01,HB), C01K(H0AA,HC), C01N(H3AA,HD),
  C01P(H4AA,HE), C01Q(H5AA,HF), C01R(H6AA,HG), C01S(H7AA,HH), C01U(H9AA,HI),
 C01Y(H3BA,HJ), C020(H02A,H02B), C021(H02C,H02D), C024(H02E,H02F), C025(H02G,
 H02H), C026(H02I,H02J), C027(H02K,H02L), C028(H02M,H02N), C02A(H02O,H02P),
 C02C(H02R,H02S), C02D(H02T,H02U), C02E(H02V,H02W), C02H(H02Y,HK), C02J(H02,HL),
  C02L(H5BA,HM), C02M(H6BA,HN), C02N(H7BA,HO), C02Q(H9BA,HP), C02S(H1CA,HQ),
 C02U(H3CA,HR), C02V(H4CA,HS), C02X(H6CA,HT), C02Y(H7CA,HU), C033(H03A,H03B),
 C034(H03C,H03D), C03A(H03E,H03F), C03B(H03G,H03H), C03C(H03I,H03J), C03E(H03K,
 H03L), C03F(H03M,H03N), C6(H6A,H6B), C8(H8A,H8B), C5(H5A,H5B), C9(H9A,H9B),
 C10(H10A,H10B), C1AA(H1AB,H1AC)
;
_shelx_res_checksum              16446
_shelx_fab_checksum              89029
_olex2_submission_special_instructions 'No special instructions were received'