Tuning the properties of atomically precise gold nanoclusters for biolabeling and drug delivery.
Xu, Man-Man; Jia, Tong-Tong; Li, Bingjie; Ma, Wang; Chen, Xiaoyuan; Zhao, Xueli; Zang, Shuang-Quan; Chemical communications (Cambridge, England) 56 (2020) 8766–8769; doi:10.1039/d0cc03498c

data_7127185
_publ_section_title
;
 Tuning the properties of atomically precise gold nanoclusters for
 biolabeling and drug delivery.
;
_journal_issue                   62
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              8766
_journal_page_last               8769
_journal_paper_doi               10.1039/d0cc03498c
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C210 H270 Au10 O20, 2(C2 H6 O S)'
_chemical_formula_sum            'C214 H282 Au10 O22 S2'
_chemical_formula_weight         5240.16
_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_Hall           'P 2 2ab'
_space_group_name_H-M_alt        'P 21 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-07-17
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-04-09 deposited with the CCDC.	2020-07-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   19.6562(4)
_cell_length_b                   28.6975(5)
_cell_length_c                   21.2232(4)
_cell_measurement_reflns_used    55797
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      25.4900
_cell_measurement_theta_min      2.1610
_cell_volume                     11971.7(4)
_computing_cell_refinement       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_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_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -23.00  85.00   0.50    8.50    --    7.20  57.00-150.00  216
  2  \w    -23.00  83.00   0.50    8.50    --    7.20  57.00  30.00  212
  3  \w     49.00  75.00   0.50    8.50    --   -7.40  82.00 -30.00   52
  4  \w    -50.00  29.00   0.50    8.50    --   -7.40  82.00 -30.00  158
  5  \w    -48.00  79.00   0.50    8.50    --   -7.40  82.00  90.00  254
  6  \w    -39.00  81.00   0.50    8.50    --   -7.40  77.00-120.00  240
  7  \w    -47.00  80.00   0.50    8.50    --   -7.40  82.00  60.00  254
  8  \w    -50.00  28.00   0.50    8.50    --   -7.40  82.00 150.00  156
  9  \w     52.00  79.00   0.50    8.50    --   -7.40  82.00 150.00   54
 10  \w    -50.00  80.00   0.50    8.50    --   -7.40  82.00 -90.00  260
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0064176000
_diffrn_orient_matrix_UB_12      0.0026422000
_diffrn_orient_matrix_UB_13      -0.0326983000
_diffrn_orient_matrix_UB_21      0.0287369000
_diffrn_orient_matrix_UB_22      0.0140636000
_diffrn_orient_matrix_UB_23      0.0069037000
_diffrn_orient_matrix_UB_31      0.0208698000
_diffrn_orient_matrix_UB_32      -0.0201467000
_diffrn_orient_matrix_UB_33      0.0005447000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1049
_diffrn_reflns_av_unetI/netI     0.0761
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            319546
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.091
_diffrn_reflns_theta_min         1.919
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.172
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72324
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.27b (Rigaku Oxford Diffraction, 2015)
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    1.454
_exptl_crystal_description       plate
_exptl_crystal_F_000             5128
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.971
_refine_diff_density_min         -0.987
_refine_diff_density_rms         0.149
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.156(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1130
_refine_ls_number_reflns         30031
_refine_ls_number_restraints     187
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0760
_refine_ls_R_factor_gt           0.0460
_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^)+(0.0606P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1064
_refine_ls_wR_factor_ref         0.1138
_reflns_Friedel_coverage         0.868
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.959
_reflns_number_gt                22104
_reflns_number_total             30031
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc03498c2.cif
_cod_data_source_block           hy
_cod_database_code               7127185
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         'C H O N S Au'
_chemical_oxdiff_usercomment     'C H O'
_shelx_estimated_absorpt_t_max   0.748
_shelx_estimated_absorpt_t_min   0.259
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.844(8)
 0.156(8)
2. 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, All O(H) groups
3. Restrained distances
 O11-C107
 1.3 with sigma of 0.01
 H98C_$1-H98C_$2
 2.2 with sigma of 0.01
 H13B-H77C
 2 with sigma of 0.01
 C99-C96
 1.53 with sigma of 0.01
 O2_$3-C25_$3 = O5-C70
 1.46 with sigma of 0.01
 C106-C105
 2.55 with sigma of 0.01
 C102-C103 \\sim C106-C103 \\sim C107-C106 \\sim C107-C105 \\sim C105-C104
 with sigma of 0.01
 C106-O11 \\sim O11-C105
 with sigma of 0.01
4. Rigid bond restraints
 O11, C107
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
C50 \\sim C59 \\sim C81 \\sim C93 \\sim C102 \\sim C103 \\sim C104 \\sim C105
\\sim C106 \\sim C107: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
C100 \\sim C101: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
O4 \\sim O7 \\sim O8 \\sim O10 \\sim O11: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(O11) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O9) \\sim Ueq, Uanis(O10) \\sim Ueq, Uanis(C89) \\sim Ueq, Uanis(C92)
\\sim Ueq, Uanis(C95) \\sim Ueq, Uanis(C101) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(O9) \\sim Ueq, Uanis(C101) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(C104) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C60) \\sim Ueq, Uanis(C84) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O7) \\sim Ueq, Uanis(C101) \\sim Ueq, Uanis(C75) \\sim Ueq, Uanis(C100)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O7) \\sim Ueq, Uanis(O5) \\sim Ueq, Uanis(O7) \\sim Ueq, Uanis(O8) \\sim
Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O7) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C99) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C84) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
6.a Ternary CH refined with riding coordinates:
 C5(H5A), C14(H14), C15(H15), C16(H16), C17(H17), C20(H20), C24(H24), C31(H31),
  C37(H37), C42(H42), C45(H45), C59(H59), C62(H62), C64(H64), C65(H65),
 C69(H69), C72(H72), C74(H74), C81(H81), C102(H102)
6.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C13(H13A,H13B), C18(H18A,H18B), C21(H21A,H21B), C23(H23A,
 H23B), C26(H26A,H26B), C29(H29A,H29B), C30(H30A,H30B), C33(H33A,H33B),
 C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B), C39(H39A,H39B), C41(H41A,H41B),
  C43(H43A,H43B), C44(H44A,H44B), C46(H46A,H46B), C47(H47A,H47B), C48(H48A,
 H48B), C50(H50A,H50B), C52(H52A,H52B), C53(H53A,H53B), C54(H54A,H54B),
 C55(H55A,H55B), C56(H56A,H56B), C58(H58A,H58B), C61(H61A,H61B), C66(H66A,H66B),
  C67(H67A,H67B), C71(H71A,H71B), C73(H73A,H73B), C75(H75A,H75B), C76(H76A,
 H76B), C82(H82A,H82B), C83(H83A,H83B), C87(H87A,H87B), C88(H88A,H88B),
 C91(H91A,H91B), C93(H93A,H93B), C95(H95A,H95B), C97(H97A,H97B), C99(H99A,H99B),
  C100(H10C,H10D), C104(H10H,H10I), C105(H10J,H10K)
6.c Aromatic/amide H refined with riding coordinates:
 C49(H49), C68(H68), C86(H86), C94(H94), C106(H106)
6.d Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C63(H63A,H63B,H63C), C77(H77A,H77B,H77C), C89(H89A,H89B,
 H89C), C101(H10E,H10F,H10G), C92(H92A,H92B,H92C), C98(H98A,H98B,H98C)
6.e Idealised tetrahedral OH refined as rotating group:
 O1(H1), O2(H2), O3(H3), O5(H5), O7(H7)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              9981
_shelx_fab_checksum              45053
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.342
_oxdiff_exptl_absorpt_empirical_full_min 0.743