Ultrastable hydrido gold nanoclusters with the protection of phosphines.
Yuan, Shang-Fu; Li, Jiao-Jiao; Guan, Zong-Jie; Lei, Zhen; Wang, Quan-Ming; Chemical communications (Cambridge, England) 56 (2020) 7037–7040; doi:10.1039/d0cc02339f

data_7126563
_publ_section_title
;
 Ultrastable hydrido gold nanoclusters with the protection of phosphines.
;
_journal_issue                   51
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              7037
_journal_page_last               7040
_journal_paper_doi               10.1039/d0cc02339f
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety
'2(C223 H185 Au20 O2 P12 S), 5(F6 P), 2(O), 10(C O)'
_chemical_formula_sum            'C456 H418 Au40 F36 O16 P30 S2'
_chemical_formula_weight         15709.76
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2017-05-15
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2018-09-13 deposited with the CCDC.	2020-05-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.8269(13)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   21.5346(4)
_cell_length_b                   43.3916(6)
_cell_length_c                   27.3200(4)
_cell_measurement_reflns_used    27489
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      65.8520
_cell_measurement_theta_min      3.9810
_cell_volume                     25525.7(7)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4273
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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     90.00 154.00   1.00   20.00    --   89.35  45.00 -60.00   64
  2  \w     73.00 154.00   1.00   20.00    --   89.35  30.00-150.00   81
  3  \w     62.00 130.00   1.00   20.00    --   89.35  61.00 -30.00   68
  4  \w     52.00 109.00   1.00   20.00    --   89.35 -45.00-180.00   57
  5  \w     13.00 119.00   1.00   20.00    --   89.35 -77.00  60.00  106
  6  \w    -50.00  30.00   1.00    6.00    --  -40.81  38.00 120.00   80
  7  \w   -106.00  -6.00   1.00    6.00    --  -40.81 -19.00 -60.00  100
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0452937000
_diffrn_orient_matrix_UB_12      -0.0179622000
_diffrn_orient_matrix_UB_13      -0.0335763000
_diffrn_orient_matrix_UB_21      0.0266609000
_diffrn_orient_matrix_UB_22      0.0165682000
_diffrn_orient_matrix_UB_23      -0.0449706000
_diffrn_orient_matrix_UB_31      0.0485429000
_diffrn_orient_matrix_UB_32      -0.0257660000
_diffrn_orient_matrix_UB_33      -0.0054354000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0461
_diffrn_reflns_av_unetI/netI     0.0595
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       49
_diffrn_reflns_limit_k_min       -47
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            85836
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        60.998
_diffrn_reflns_theta_max         60.998
_diffrn_reflns_theta_min         3.681
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    22.459
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66287
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown-black
_exptl_crystal_density_diffrn    2.044
_exptl_crystal_description       sheet
_exptl_crystal_F_000             14496
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.02
_platon_squeeze_details
;
;
_refine_diff_density_max         2.462
_refine_diff_density_min         -1.793
_refine_diff_density_rms         0.219
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2440
_refine_ls_number_reflns         39014
_refine_ls_number_restraints     58
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0612
_refine_ls_R_factor_gt           0.0470
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0605P)^2^+87.3576P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1165
_refine_ls_wR_factor_ref         0.1240
_reflns_Friedel_coverage         0.000
_reflns_number_gt                30978
_reflns_number_total             39014
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc02339f2.cif
_cod_data_source_block           ljj35cb
_cod_depositor_comments
'Adding full bibliography for 7126562--7126563.cif.'
_cod_database_code               7126563
_shelx_shelxl_version_number     2014/7
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     61.08
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups
2. Restrained distances
 O6S-C6S
 1.45 with sigma of 0.02
 C2S-O2G
 1.45 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O2G \\sim O32 \\sim C2S: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
O1 \\sim O2 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim
C17: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: O2G(0.5) O32(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C1A(H1A), C1C(H1C), C1D(H1D), C1E(H1E), C1F(H1F), C1G(H1G), C1I(H1I),
 C1J(H1J), C1K(H1K), C1L(H1L), C1M(H1M), C1N(H1N), C1Q(H1Q), C1R(H1R), C1S(H1S),
  C1T(H1T), C1U(H1U), C1W(H1W), C1X(H1X), C1Y(H1Y), C1Z(H1Z), C2(H2A),
 C2A(H2AA), C2B(H2B), C2C(H2C), C2D(H2D), C2E(H2E), C2F(H2F), C3(H3), C4(H4),
 C5(H5), C6(H6), C7(H7), C9(H9), C10(H10), C12(H12), C13(H13), C14(H14),
 C15(H15), C18(H18), C19(H19), C20(H20), C22(H22), C23(H23), C24(H24), C25(H25),
  C26(H26), C29(H29), C112(H112), C113(H113), C114(H114), C115(H115),
 C116(H116), C122(H122), C123(H123), C124(H124), C125(H125), C126(H126),
 C132(H132), C133(H133), C134(H134), C135(H135), C136(H136), C212(H212),
 C213(H213), C214(H214), C215(H215), C216(H216), C222(H222), C223(H223),
 C224(H224), C225(H225), C226(H226), C232(H232), C233(H233), C234(H234),
 C235(H235), C236(H236), C312(H312), C313(H313), C314(H314), C315(H315),
 C316(H316), C322(H322), C323(H323), C324(H324), C325(H325), C326(H326),
 C332(H332), C333(H333), C334(H334), C335(H335), C336(H336), C412(H412),
 C413(H413), C414(H414), C415(H415), C416(H416), C422(H422), C423(H423),
 C424(H424), C425(H425), C426(H426), C432(H432), C433(H433), C434(H434),
 C435(H435), C436(H436), C512(H512), C513(H513), C514(H514), C515(H515),
 C516(H516), C522(H522), C523(H523), C524(H524), C525(H525), C526(H526),
 C532(H532), C533(H533), C534(H534), C535(H535), C536(H536), C612(H612),
 C613(H613), C614(H614), C615(H615), C616(H616), C622(H622), C623(H623),
 C624(H624), C625(H625), C626(H626), C632(H632), C633(H633), C634(H634),
 C635(H635), C636(H636), C712(H712), C713(H713), C714(H714), C715(H715),
 C716(H716), C722(H722), C723(H723), C724(H724), C725(H725), C726(H726),
 C732(H732), C733(H733), C734(H734), C735(H735), C736(H736), C812(H812),
 C813(H813), C814(H814), C815(H815), C816(H816), C822(H822), C823(H823),
 C824(H824), C825(H825), C826(H826), C832(H832), C833(H833), C834(H834),
 C835(H835), C836(H836), C912(H912), C913(H913), C914(H914), C915(H915),
 C916(H916), C922(H922), C923(H923), C924(H924), C925(H925), C926(H926),
 C932(H932), C933(H933), C934(H934), C935(H935), C936(H936)
5.b Tetrahedral OH refined with riding coordinates:
 O2(H2)
;
_olex2_date_sample_data_collection 2017-04-01
_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 1.768
_oxdiff_exptl_absorpt_empirical_full_min 0.716