Surface engineering of linearly fused Au<sub>13</sub> units using diphosphine and Cd doping.
Li, Tianrong; Li, Qinzhen; Yang, Sha; Xu, Liyun; Chai, Jinsong; Li, Peng; Zhu, Manzhou; Chemical communications (Cambridge, England) 57 (2021) 4682–4685; doi:10.1039/d1cc00577d

data_7128141
_publ_section_title
;
 Surface engineering of linearly fused Au<sub>13</sub> units using
 diphosphine and Cd doping.
;
_journal_issue                   38
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              4682
_journal_page_last               4685
_journal_paper_doi               10.1039/d1cc00577d
_journal_volume                  57
_journal_year                    2021
_chemical_absolute_configuration rmad
_chemical_formula_moiety         'C126 H178 Au17 Cd2 P4 S12, C24 H20 B'
_chemical_formula_sum            'C150 H204 Au17 B Cd2 P4 S12'
_chemical_formula_weight         6099.76
_space_group_crystal_system      orthorhombic
_space_group_IT_number           17
_space_group_name_Hall           'P 2c 2'
_space_group_name_H-M_alt        'P 2 2 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-07-25
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-01-18 deposited with the CCDC.	2021-04-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   19.544(4)
_cell_length_b                   18.626(4)
_cell_length_c                   26.122(5)
_cell_measurement_reflns_used    60337
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      68.11
_cell_measurement_theta_min      4.06
_cell_volume                     9509(3)
_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      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0634
_diffrn_reflns_av_unetI/netI     0.0492
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            71306
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.288
_diffrn_reflns_theta_min         1.875
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    13.476
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_correction_T_min  0.5
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    2.130
_exptl_crystal_description       block
_exptl_crystal_F_000             5600
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         6.759
_refine_diff_density_min         -4.632
_refine_diff_density_rms         0.434
_refine_ls_abs_structure_details
;
 Flack x determined using 4325 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.501(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.968
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     856
_refine_ls_number_reflns         17007
_refine_ls_number_restraints     1198
_refine_ls_restrained_S_all      0.960
_refine_ls_R_factor_all          0.0948
_refine_ls_R_factor_gt           0.0734
_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^)+(0.1615P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1965
_refine_ls_wR_factor_ref         0.2182
_reflns_Friedel_coverage         0.817
_reflns_Friedel_fraction_full    0.973
_reflns_Friedel_fraction_max     0.968
_reflns_number_gt                11321
_reflns_number_total             17007
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc00577d2.cif
_cod_data_source_block           test
_cod_depositor_comments
'Adding full bibliography for 7128141--7128142.cif.'
_cod_database_code               7128141
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.552
_shelx_estimated_absorpt_t_min   0.134
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C25-C26 = C27-C26 = C28-C27 = C28-C29 = C30-C29 = C30-C25
 1.53 with sigma of 0.02
 C36-C31 = C32-C31 = C32-C33 = C34-C33 = C34-C35 = C36-C35
 1.53 with sigma of 0.02
 C20-C19 = C20-C21 = C22-C21 = C22-C23 = C24-C23 = C24-C19
 1.53 with sigma of 0.02
 C76-B1 = C82-B1 = C70-B1 = C64-B1
 1.6 with sigma of 0.02
 C13-C14 = C18-C13 = C18-C17 = C15-C16 = C17-C16 = C15-C14
 1.53 with sigma of 0.02
 C50-C49 = C50-C51
 1.53 with sigma of 0.02
 C49-C43
 2.4 with sigma of 0.02
 P1-C49
 1.6 with sigma of 0.02
 C8-C7 = C9-C8 = C9-C10 = C11-C10 = C11-C12 = C12-C7
 1.53 with sigma of 0.02
 C11_$1-C5
 2.8 with sigma of 0.02
 C6-C5
 1.53 with sigma of 0.02
 C1-C6 = C6-C5 = C5-C4 = C3-C4 = C3-C2 = C1-C2
 1.53 with sigma of 0.02
 C3-C5
 2.48 with sigma of 0.02
 C1-C5
 2.48 with sigma of 0.02
 C12-C1_$1
 2.8 with sigma of 0.02
 H12B-H1_$1
 2 with sigma of 0.02
 H11B-H4A_$1
 2 with sigma of 0.02
 S6_$1-C1_$1
 1.64 with sigma of 0.02
 C18-C18_$2
 2.8 with sigma of 0.02
 H1_$1-H11A
 2 with sigma of 0.02
 H25-H32A_$1
 2 with sigma of 0.02
 C18-C13 = C14-C13 = C15-C14 = C16-C15 = C17-C16 = C18-C17
 1.5 with sigma of 0.02
 C64-C82 \\sim C82-C70
 with sigma of 0.02
 C82-C70 \\sim C70-C64
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C4) \\sim
Ueq, Uanis(C5) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C8)
\\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C11) \\sim Ueq,
Uanis(C12) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C15)
\\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C18) \\sim Ueq,
Uanis(C19) \\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C22)
\\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C25) \\sim Ueq,
Uanis(C26) \\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C29)
\\sim Ueq, Uanis(C30) \\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(C32) \\sim Ueq,
Uanis(C33) \\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(C36)
\\sim Ueq, Uanis(C37) \\sim Ueq, Uanis(C42) \\sim Ueq, Uanis(C41) \\sim Ueq,
Uanis(C40) \\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(C38) \\sim Ueq, Uanis(C43)
\\sim Ueq, Uanis(C48) \\sim Ueq, Uanis(C47) \\sim Ueq, Uanis(C46) \\sim Ueq,
Uanis(C45) \\sim Ueq, Uanis(C44) \\sim Ueq, Uanis(C49) \\sim Ueq, Uanis(C50)
\\sim Ueq, Uanis(C51) \\sim Ueq, Uanis(C52) \\sim Ueq, Uanis(C53) \\sim Ueq,
Uanis(C54) \\sim Ueq, Uanis(C55) \\sim Ueq, Uanis(C56) \\sim Ueq, Uanis(C57)
\\sim Ueq, Uanis(C58) \\sim Ueq, Uanis(C63) \\sim Ueq, Uanis(C62) \\sim Ueq,
Uanis(C61) \\sim Ueq, Uanis(C60) \\sim Ueq, Uanis(C59) \\sim Ueq, Uanis(C64)
\\sim Ueq, Uanis(C65) \\sim Ueq, Uanis(C66) \\sim Ueq, Uanis(C67) \\sim Ueq,
Uanis(C68) \\sim Ueq, Uanis(C69) \\sim Ueq, Uanis(C70) \\sim Ueq, Uanis(C71)
\\sim Ueq, Uanis(C72) \\sim Ueq, Uanis(C73) \\sim Ueq, Uanis(C74) \\sim Ueq,
Uanis(C75) \\sim Ueq, Uanis(C76) \\sim Ueq, Uanis(C77) \\sim Ueq, Uanis(C78)
\\sim Ueq, Uanis(C79) \\sim Ueq, Uanis(C80) \\sim Ueq, Uanis(C81) \\sim Ueq,
Uanis(C82) \\sim Ueq, Uanis(C83) \\sim Ueq, Uanis(C84) \\sim Ueq, Uanis(C85)
\\sim Ueq, Uanis(C86) \\sim Ueq, Uanis(C87) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: H5A(0.5) H5B(0.5) H18A(0.5) H18B(0.5) H20A(0.5) H20B(0.5) C64(0.5)
 C65(0.5) H65(0.5) C66(0.5) H66(0.5) C67(0.5) H67(0.5) C68(0.5) H68(0.5)
 C69(0.5) H69(0.5) C70(0.5) C71(0.5) H71(0.5) C72(0.5) H72(0.5) C73(0.5)
 H73(0.5) C74(0.5) H74(0.5) C75(0.5) H75(0.5) C76(0.5) C77(0.5) H77(0.5)
 C78(0.5) H78(0.5) C79(0.5) H79(0.5) C80(0.5) H80(0.5) C81(0.5) H81(0.5)
 C82(0.5) C83(0.5) H83(0.5) C84(0.5) H84(0.5) C85(0.5) H85(0.5) C86(0.5)
 H86(0.5) C87(0.5) H87(0.5) B1(0.5)
5.a Ternary CH refined with riding coordinates:
 C1(H1), C7(H7), C13(H13), C19(H19), C25(H25), C31(H31)
5.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C8(H8A,H8B),
 C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C14(H14A,H14B),
 C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B), C20(H20A,H20B),
  C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C26(H26A,
 H26B), C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B),
 C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B),
  C49(H49A,H49B), C50(H50A,H50B), C51(H51A,H51B)
5.c Aromatic/amide H refined with riding coordinates:
 C42(H42), C41(H41), C40(H40), C39(H39), C38(H38), C48(H48), C47(H47),
 C46(H46), C45(H45), C44(H44), C53(H53), C54(H54), C55(H55), C56(H56), C57(H57),
  C63(H63), C62(H62), C61(H61), C60(H60), C59(H59), C65(H65), C66(H66),
 C67(H67), C68(H68), C69(H69), C71(H71), C72(H72), C73(H73), C74(H74), C75(H75),
  C77(H77), C78(H78), C79(H79), C80(H80), C81(H81), C83(H83), C84(H84),
 C85(H85), C86(H86), C87(H87)
5.d Fitted hexagon refined as free rotating group:
 C37(C42,C41,C40,C39,C38), C43(C48,C47,C46,C45,C44), C52(C53,C54,C55,C56,C57),
 C58(C63,C62,C61,C60,C59), C64(C65,C66,C67,C68,C69), C70(C71,C72,C73,C74,C75),
 C76(C77,C78,C79,C80,C81), C82(C83,C84,C85,C86,C87)
;
_shelx_res_checksum              30273
_shelx_hkl_checksum              47706
_shelx_fab_checksum              59812
_olex2_submission_special_instructions 'No special instructions were received'