Diphosphine-protected ultrasmall gold nanoclusters: opened icosahedral Au<sub>13</sub> and heart-shaped Au<sub>8</sub> clusters.
Zhang, Shan-Shan; Feng, Lei; Senanayake, Ravithree D.; Aikens, Christine M.; Wang, Xing-Po; Zhao, Quan-Qin; Tung, Chen-Ho; Sun, Di; Chemical science 9 (2018) 1251–1258; doi:10.1039/c7sc03566g

data_1553981
_publ_section_title
;
 Diphosphine-protected ultrasmall gold nanoclusters: opened icosahedral
 Au<sub>13</sub> and heart-shaped Au<sub>8</sub> clusters.
;
_journal_issue                   5
_journal_name_full               'Chemical science'
_journal_page_first              1251
_journal_page_last               1258
_journal_paper_doi               10.1039/c7sc03566g
_journal_volume                  9
_journal_year                    2018
_chemical_formula_moiety         'C100 H88 Au8 P8 S2, 2(Cl), 4(C H2 Cl2)'
_chemical_formula_sum            'C104 H96 Au8 Cl10 P8 S2'
_chemical_formula_weight         3587.91
_space_group_crystal_system      orthorhombic
_space_group_IT_number           68
_space_group_name_Hall           '-C 2a 2ac'
_space_group_name_H-M_alt        'C c c a :2'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-10-03
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2017-10-03 deposited with the CCDC.
2017-12-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   29.8513(7)
_cell_length_b                   27.0724(7)
_cell_length_c                   28.9960(6)
_cell_measurement_reflns_used    20164
_cell_measurement_temperature    93.0(3)
_cell_measurement_theta_max      30.7940
_cell_measurement_theta_min      3.4660
_cell_volume                     23433.0(10)
_computing_cell_refinement       'CrysAlisPro 1.171.39.30d (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.30d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.30d (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      93.0(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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    -52.00   3.00   1.00   30.00    --    5.65 -47.00 152.00   55
  2  \w    -24.00  29.00   1.00   30.00    --   -4.48 -99.00 -60.00   53
  3  \w    -26.00  29.00   1.00   30.00    --   -4.48 -99.00-180.00   55
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0154977000
_diffrn_orient_matrix_UB_12      0.0101074000
_diffrn_orient_matrix_UB_13      -0.0159561000
_diffrn_orient_matrix_UB_21      -0.0178785000
_diffrn_orient_matrix_UB_22      0.0113346000
_diffrn_orient_matrix_UB_23      -0.0121667000
_diffrn_orient_matrix_UB_31      0.0021384000
_diffrn_orient_matrix_UB_32      0.0213438000
_diffrn_orient_matrix_UB_33      0.0140039000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0699
_diffrn_reflns_av_unetI/netI     0.0492
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            57061
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.379
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    10.391
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.43338
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.30d (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    2.034
_exptl_crystal_description       block
_exptl_crystal_F_000             13392
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         5.089
_refine_diff_density_min         -2.474
_refine_diff_density_rms         0.250
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     595
_refine_ls_number_reflns         11919
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0552
_refine_ls_R_factor_gt           0.0418
_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^)+(0.0323P)^2^+989.1260P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0968
_refine_ls_wR_factor_ref         0.1033
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9961
_reflns_number_total             11919
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7sc03566g3.cif
_cod_data_source_block           SD_Au2_93K
_cod_original_sg_symbol_Hall     '-C 2b 2bc'
_cod_original_sg_symbol_H-M      'C c c e'
_cod_database_code               1553981
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         AuPSCH
_shelx_estimated_absorpt_t_max   0.490
_shelx_estimated_absorpt_t_min   0.423
_diffrn_oxdiff_ac3_digest_frames
;
01f4b1244a10e56f383d4703d603a0751d0002544d0
;
_diffrn_oxdiff_ac3_digest_hkl
;
01777e48061fbfac3f3083925f2289ac7ea2d6
;
_reflns_odcompleteness_completeness 80.72
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.55
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C38(H38A,H38B), C51(H51A,H51B), C52(H52A,H52B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C21(H21), C22(H22),
  C23(H23), C24(H24), C25(H25), C27(H27), C28(H28), C29(H29), C30(H30),
 C31(H31), C33(H33), C34(H34), C35(H35), C36(H36), C37(H37), C40(H40), C41(H41),
  C42(H42), C43(H43), C44(H44), C46(H46), C47(H47), C48(H48), C49(H49), C50(H50)
;
_shelx_res_checksum              84137
_shelx_fab_checksum              96579
_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 1.974
_oxdiff_exptl_absorpt_empirical_full_min 0.773