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_7128142
_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_formula_moiety         'C238 H277 Au29 Cd2 Fe2 P4 S17'
_chemical_formula_sum            'C238 H277 Au29 Cd2 Fe2 P4 S17'
_chemical_formula_weight         9855.01
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2020-10-15
_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            4
_cell_length_a                   27.2386(12)
_cell_length_b                   44.9120(15)
_cell_length_c                   25.7433(13)
_cell_measurement_reflns_used    97378
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      70.17
_cell_measurement_theta_min      5.96
_cell_volume                     31493(2)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_R_equivalents  0.0604
_diffrn_reflns_av_unetI/netI     0.0529
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       51
_diffrn_reflns_limit_k_min       -54
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            170838
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         69.788
_diffrn_reflns_theta_min         5.954
_exptl_absorpt_coefficient_mu    27.952
_exptl_crystal_density_diffrn    2.079
_exptl_crystal_description       block
_exptl_crystal_F_000             17904
_refine_diff_density_max         3.988
_refine_diff_density_min         -3.792
_refine_diff_density_rms         0.295
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1369
_refine_ls_number_reflns         28819
_refine_ls_number_restraints     828
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0746
_refine_ls_R_factor_gt           0.0582
_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^)+(0.0694P)^2^+714.1132P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1431
_refine_ls_wR_factor_ref         0.1500
_reflns_Friedel_coverage         0.000
_reflns_number_gt                22567
_reflns_number_total             28819
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc00577d2.cif
_cod_data_source_block           1_sq
_cod_depositor_comments
'Adding full bibliography for 7128141--7128142.cif.'
_cod_database_code               7128142
_shelx_shelxl_version_number     2016/4
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C1IA-C9IA
 1.5 with sigma of 0.01
 C49-C29
 1.5 with sigma of 0.01
 C2GA-C0IA
 1.5 with sigma of 0.01
 C54-C29 = C29-C16 = C31-C29
 1.55 with sigma of 0.01
 C16-C31
 2.5 with sigma of 0.01
 C54-C16
 2.5 with sigma of 0.01
 C54-C31
 2.5 with sigma of 0.01
 C5-C1IA
 1.55 with sigma of 0.01
 H5B-H2JB_$1
 2 with sigma of 0.01
 H5A-H2JB_$1
 2 with sigma of 0.01
 H16C-H64
 2 with sigma of 0.01
 H5B-H2JA_$1
 2 with sigma of 0.01
 H5B_$1-H5B
 2 with sigma of 0.01
 H4IA-H4IA_$1
 2 with sigma of 0.01
 C5-C1IA \\sim C4-C1IA \\sim C2JA-C1IA
 with sigma of 0.02
 C2JA-C4 \\sim C2JA-C5 \\sim C4-C5
 with sigma of 0.02
 C9IA-C2JA \\sim C9IA-C4 \\sim C9IA-C5
 with sigma of 0.02
 C1IA-C5IA \\sim C1IA-C5GA
 with sigma of 0.02
 C29-C16 \\sim C54-C29 \\sim C31-C29
 with sigma of 0.02
 C3-C0IA \\sim C2-C0IA \\sim C1-C0IA
 with sigma of 0.02
 C1-C2 \\sim C1-C3 \\sim C2-C3
 with sigma of 0.02
 C2GA-C1 \\sim C2GA-C2 \\sim C2GA-C3
 with sigma of 0.02
 C9EA-C17 \\sim C9EA-C17A
 with sigma of 0.02
 C9EA-C2IA \\sim C9EA-C2IB
 with sigma of 0.02
 C9EA-C3IA \\sim C9EA-C3IB
 with sigma of 0.02
 S29-C42 \\sim S29-C6FA
 with sigma of 0.02
3. Restrained planarity
 S10, C4AA, C5IA, C5GA
 with sigma of 0.1
 C1IA, C9IA, C4IA, C3EA
 with sigma of 0.1
 S29, C47, C6IA, C64, C29
 with sigma of 0.1
 C0IA, C2GA, S9, C4BA
 with sigma of 0.1
 C3JA, C15, C104, C13
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C4IA \\sim C3EA \\sim C5GA \\sim C9IA \\sim C5IA \\sim C4 \\sim C1IA \\sim C5
\\sim C2JA \\sim C4AA: within 1.7A with sigma of 0.004 and sigma for terminal
atoms of 0.008
C47 \\sim C6FA \\sim C6IA \\sim C49 \\sim C64 \\sim C42 \\sim C29 \\sim C16
\\sim C54 \\sim C31: within 1.7A with sigma of 0.004 and sigma for terminal
atoms of 0.008
C4BA \\sim C6CA \\sim C5EA \\sim C4HA \\sim C2GA \\sim C0JA \\sim C2 \\sim C0IA
\\sim C1 \\sim C3: within 1.7A with sigma of 0.004 and sigma for terminal atoms
of 0.008
C0AA \\sim C1BA \\sim C9BA \\sim C6AA \\sim C9AA \\sim C2BA \\sim C9EA \\sim
C2IA \\sim C3IA \\sim C17A \\sim C2IB \\sim C3IB \\sim C17: within 1.7A with
sigma of 0.004 and sigma for terminal atoms of 0.008
Uanis(C29) \\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(C54)
\\sim Ueq, Uanis(C64) \\sim Ueq, Uanis(C42) \\sim Ueq, Uanis(C47) \\sim Ueq,
Uanis(C49) \\sim Ueq, Uanis(C6IA) \\sim Ueq, Uanis(C6FA) \\sim Ueq, Uanis(C4IA)
\\sim Ueq, Uanis(C4AA) \\sim Ueq, Uanis(C3EA) \\sim Ueq, Uanis(C5GA) \\sim Ueq,
Uanis(C9IA) \\sim Ueq, Uanis(C5IA) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C1IA)
\\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C2JA) \\sim Ueq, Uanis(C2) \\sim Ueq,
Uanis(C0IA) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C9EA)
\\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C2IA) \\sim Ueq, Uanis(C3IA) \\sim Ueq,
Uanis(C9GA) \\sim Ueq, Uanis(C0HA) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C14)
\\sim Ueq, Uanis(C3JA) \\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(C87) \\sim Ueq,
Uanis(C100) \\sim Ueq, Uanis(C3BA) \\sim Ueq, Uanis(C8BA) \\sim Ueq,
Uanis(C7AA) \\sim Ueq, Uanis(C8AA) \\sim Ueq, Uanis(C4DA) \\sim Ueq,
Uanis(C5DA) \\sim Ueq, Uanis(C1EA) \\sim Ueq, Uanis(C5HA) \\sim Ueq,
Uanis(C1GA) \\sim Ueq, Uanis(C0FA) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C11)
\\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C24) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C17A) \\sim Ueq, Uanis(C2IB) \\sim Ueq, Uanis(C3IB) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C6) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C6HA) \\sim Ueq, Uanis(C4EA)
\\sim Ueq, Uanis(C9HA) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C7IA) \\sim Ueq,
Uanis(C8IA) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C8GA) \\sim Ueq, Uanis(C15)
\\sim Ueq, Uanis(C104) \\sim Ueq, Uanis(C3JA) \\sim Ueq, Uanis(C33) \\sim Ueq,
Uanis(C87) \\sim Ueq, Uanis(C100) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C3FA) \\sim Ueq, Uanis(C2EA) \\sim Ueq, Uanis(C3GA) \\sim Ueq,
Uanis(C3HA) \\sim Ueq, Uanis(C7HA) \\sim Ueq, Uanis(C7FA) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C5BA) \\sim Ueq, Uanis(C3DA) \\sim Ueq, Uanis(C8DA) \\sim Ueq,
Uanis(C2CA) \\sim Ueq, Uanis(C4FA) \\sim Ueq, Uanis(C6EA) \\sim Ueq,
Uanis(C7EA) \\sim Ueq, Uanis(C2FA) \\sim Ueq, Uanis(C6GA) \\sim Ueq,
Uanis(C1JA) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Sof(C17A)=Sof(H17D)=Sof(H17E)=Sof(H17F)=Sof(C2IB)=Sof(H2ID)=Sof(H2IE)=
 Sof(H2IF)=Sof(C3IB)=Sof(H3ID)=Sof(H3IE)=Sof(H3IF)=1-FVAR(1)
 Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(H17C)=Sof(C2IA)=Sof(H2IA)=Sof(H2IB)=
 Sof(H2IC)=Sof(C3IA)=Sof(H3IA)=Sof(H3IB)=Sof(H3IC)=FVAR(1)
 Fixed Sof: C7IA(0.5) C13(0.5) H13(0.5) C8GA(0.5) H8GA(0.5) C15(0.5) C8IA(0.5)
 H8IA(0.5) C104(0.5) H104(0.5) C3JA(0.5) C33(0.5) H33A(0.5) H33B(0.5) H33C(0.5)
 C87(0.5) H87A(0.5) H87B(0.5) H87C(0.5) C100(0.5) H10A(0.5) H10B(0.5) H10C(0.5)
6.a Riding coordinates:
 C4(H4A,H4B,H4C), C33(H33A,H33B,H33C)
6.b Aromatic/amide H refined with riding coordinates:
 C1BA(H1BA), C3BA(H3BA), C7BA(H7BA), C8BA(H8BA), C9BA(H9BA), C1AA(H1AA),
 C2AA(H2AA), C3AA(H3AA), C5AA(H5AA), C6AA(H6AA), C9AA(H9AA), C1DA(H1DA),
 C3DA(H3DA), C4DA(H4DA), C5DA(H5DA), C7DA(H7DA), C8DA(H8DA), C9DA(H9DA),
 C1CA(H1CA), C2CA(H2CA), C4CA(H4CA), C5CA(H5CA), C6CA(H6CA), C7CA(H7CA),
 C8CA(H8CA), C9CA(H9CA), C0DA(H0DA), C2DA(H2DA), C0EA(H0EA), C4FA(H4FA),
 C5FA(H5FA), C7FA(H7FA), C8FA(H8FA), C9FA(H9FA), C2EA(H2EA), C5EA(H5EA),
 C0GA(H0GA), C1HA(H1HA), C3HA(H3HA), C4HA(H4HA), C7HA(H7HA), C3GA(H3GA),
 C4GA(H4GA), C7GA(H7GA), C2HA(H2HA), C0JA(H0JA), C6(H6), C7(H7), C9HA(H9HA),
 C6HA(H6HA), C19(H19), C10(H10), C13(H13), C8GA(H8GA), C8IA(H8IA), C104(H104),
 C4IA(H4IA), C3EA(H3EA), C5GA(H5GA), C5IA(H5IA), C42(H42), C64(H64), C6IA(H6IA),
  C6FA(H6FA)
6.c Fitted hexagon refined as free rotating group:
 C6(C7,C9HA,C4EA,C6HA,C19), C7IA(C13,C8GA,C15,C8IA,C104), C4IA(C4AA,C3EA,C5GA,
 C9IA,C5IA), C47(C42,C64,C49,C6IA,C6FA)
6.d Idealised Me refined as rotating group:
 C6EA(H6EA,H6EB,H6EC), C0FA(H0FA,H0FB,H0FC), C5HA(H5HA,H5HB,H5HC), C1GA(H1GA,
 H1GB,H1GC), C6GA(H6GA,H6GB,H6GC), C9GA(H9GA,H9GB,H9GC), C0HA(H0HA,H0HB,H0HC),
 C1JA(H1JA,H1JB,H1JC), C11(H11A,H11B,H11C), C14(H14A,H14B,H14C), C17(H17A,H17B,
 H17C), C20(H20A,H20B,H20C), C2IA(H2IA,H2IB,H2IC), C3IA(H3IA,H3IB,H3IC),
 C24(H24A,H24B,H24C), C5(H5A,H5B,H5C), C2JA(H2JA,H2JB,H2JC), C16(H16A,H16B,
 H16C), C31(H31A,H31B,H31C), C54(H54A,H54B,H54C), C2(H2A,H2B,H2C), C1(H1A,H1B,
 H1C), C3(H3A,H3B,H3C), C87(H87A,H87B,H87C), C100(H10A,H10B,H10C), C17A(H17D,
 H17E,H17F), C2IB(H2ID,H2IE,H2IF), C3IB(H3ID,H3IE,H3IF)
;
_shelx_res_checksum              22930
_shelx_hkl_checksum              97903
_shelx_fab_checksum              28510
_olex2_submission_special_instructions 'No special instructions were received'