Homoleptic alkynyl-protected gold nanoclusters with unusual compositions and structures.
Guan, Zong-Jie; Hu, Feng; Li, Jiao-Jiao; Liu, Zi-Rui; Wang, Quan-Ming; Nanoscale 12 (2020) 13346–13350; doi:10.1039/d0nr02986f

data_1558280
_publ_section_title
;
 Homoleptic alkynyl-protected gold nanoclusters with unusual compositions
 and structures.
;
_journal_issue                   25
_journal_name_full               Nanoscale
_journal_page_first              13346
_journal_page_last               13350
_journal_paper_doi               10.1039/d0nr02986f
_journal_volume                  12
_journal_year                    2020
_chemical_formula_moiety         'C208 H104 Au50 F26'
_chemical_formula_sum            'C208 H104 Au50 F26'
_chemical_formula_weight         12945.23
_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
_audit_creation_date             2020-04-14
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2020-05-24 deposited with the CCDC.	2020-06-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.332(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.5491(3)
_cell_length_b                   38.7530(8)
_cell_length_c                   32.9349(10)
_cell_measurement_reflns_used    18750
_cell_measurement_temperature    99.99(13)
_cell_measurement_theta_max      59.9710
_cell_measurement_theta_min      3.7920
_cell_volume                     22392.3(9)
_computing_cell_refinement       'CrysAlisPro 1.171.39.7e (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.7e (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.7e (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.99(13)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2137
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.958
_diffrn_measured_fraction_theta_max 0.958
_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    -65.00  -6.00   1.00    6.00    --  -40.81  38.00-120.00   59
  2  \w      8.00  33.00   1.00    6.00    --  -40.81  38.00-120.00   25
  3  \w    -63.00  33.00   1.00    6.00    --  -40.81  38.00 -30.00   96
  4  \w     36.00 113.00   1.00   25.00    --   89.35-125.00-150.00   77
  5  \w     28.00 115.00   1.00   25.00    --   89.35-125.00   0.00   87
  6  \w     62.00 101.00   1.00   25.00    --   89.35  30.00 120.00   39
  7  \w     69.00 162.00   1.00   25.00    --   89.35  45.00 -90.00   93
  8  \w    130.00 155.00   1.00   25.00    --   89.35  30.00 120.00   25
  9  \w     16.00  69.00   1.00   25.00    --   89.35 -45.00   0.00   53
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0007169000
_diffrn_orient_matrix_UB_12      -0.0220767000
_diffrn_orient_matrix_UB_13      -0.0388066000
_diffrn_orient_matrix_UB_21      -0.0157799000
_diffrn_orient_matrix_UB_22      -0.0324541000
_diffrn_orient_matrix_UB_23      0.0255591000
_diffrn_orient_matrix_UB_31      -0.0864491000
_diffrn_orient_matrix_UB_32      0.0061168000
_diffrn_orient_matrix_UB_33      -0.0054354000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0553
_diffrn_reflns_av_unetI/netI     0.0717
_diffrn_reflns_Laue_measured_fraction_full 0.958
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            65239
_diffrn_reflns_point_group_measured_fraction_full 0.958
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        60.109
_diffrn_reflns_theta_max         60.109
_diffrn_reflns_theta_min         3.523
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    60.319
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.42465
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.7e (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark black'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    3.840
_exptl_crystal_description       block
_exptl_crystal_F_000             22144
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_platon_squeeze_details
;
;
_refine_diff_density_max         4.170
_refine_diff_density_min         -4.615
_refine_diff_density_rms         0.487
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2245
_refine_ls_number_reflns         31955
_refine_ls_number_restraints     1588
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.1148
_refine_ls_R_factor_gt           0.0984
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1409P)^2^+1749.9249P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2644
_refine_ls_wR_factor_ref         0.2777
_reflns_Friedel_coverage         0.000
_reflns_number_gt                24759
_reflns_number_total             31955
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nr02986f2.cif
_cod_data_source_block           au50
_cod_depositor_comments
'Adding full bibliography for 1558279--1558280.cif.'
_cod_database_code               1558280
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C11 H10 N O'
_shelx_estimated_absorpt_t_max   0.265
_shelx_estimated_absorpt_t_min   0.074
_reflns_odcompleteness_completeness 83.61
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     64.99
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 F6-C67
 1.35 with sigma of 0.02
 Au48-C211
 1.89 with sigma of 0.02
 C212-C211
 1.2 with sigma of 0.02
 Au48-C212
 3.1 with sigma of 0.02
 C44-F4
 2.36 with sigma of 0.02
 C46-F4
 2.36 with sigma of 0.02
 F4-C45
 1.36 with sigma of 0.02
 F26-C267
 1.36 with sigma of 0.02
 C268-F26
 2.36 with sigma of 0.02
 F26-C266
 2.36 with sigma of 0.02
 Au39-C51
 1.89 with sigma of 0.02
 C52-C51
 1.2 with sigma of 0.02
 Au39-C52
 3.1 with sigma of 0.02
 C53-C52
 1.54 with sigma of 0.02
 C51-C53
 2.74 with sigma of 0.02
 C261-C263
 2.74 with sigma of 0.02
 C262-C263
 1.54 with sigma of 0.02
 C262-Au38
 3.1 with sigma of 0.02
 C262-C261
 1.2 with sigma of 0.02
 Au38-C261
 1.89 with sigma of 0.02
 Au45-C201
 1.89 with sigma of 0.02
 C201-C202
 1.2 with sigma of 0.02
 Au45-C202
 3.1 with sigma of 0.02
 C203-C202
 1.54 with sigma of 0.02
 C201-C203
 2.74 with sigma of 0.02
 C212-C213
 1.54 with sigma of 0.02
 C211-C213
 2.74 with sigma of 0.02
 C212-C218
 2.54 with sigma of 0.02
 C212-C214
 2.54 with sigma of 0.02
 Au48-C213
 4.66 with sigma of 0.02
 F21-C217
 1.36 with sigma of 0.02
 C218-F21
 2.36 with sigma of 0.02
 C216-F21
 2.36 with sigma of 0.02
 C22-C23
 1.46 with sigma of 0.02
 C22-Au46
 3.1 with sigma of 0.02
 C24-C22
 2.51 with sigma of 0.02
 C22-C28
 2.51 with sigma of 0.02
 Au46-C21
 1.89 with sigma of 0.02
 C22-C21
 1.2 with sigma of 0.02
 C21-C23
 2.7 with sigma of 0.02
 Au23-C21
 2.317 with sigma of 0.02
 C73-C72
 1.46 with sigma of 0.02
 Au40-C72
 3.1 with sigma of 0.02
 Au40-C71
 1.89 with sigma of 0.02
 C72-C71
 1.2 with sigma of 0.02
 C73-C71
 2.76 with sigma of 0.02
 Au17-C71
 2.32 with sigma of 0.02
3. Restrained planarity
 F6, C61, C62, C63, C64, C65, C66, C67, C68
 with sigma of 0.1
 F26, C261, C262, C263, C264, C265, C266, C267, C268
 with sigma of 0.1
 F19, C191, C192, C193, C194, C195, C196, C197, C198
 with sigma of 0.1
 F22, C221, C222, C223, C224, C225, C226, C227, C228
 with sigma of 0.1
 F21, C211, C212, C213, C214, C215, C216, C217, C218
 with sigma of 0.1
 F2, C21, C22, C23, C24, C26, C27, C28
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
F20 \\sim C207 \\sim C205 \\sim C206 \\sim C204 \\sim C203 \\sim C208 \\sim
C202 \\sim C201 \\sim Au45 \\sim Au19: within 2A with sigma of 0.001 and sigma
for terminal atoms of 0.002 within 2A
F22 \\sim C225 \\sim C226 \\sim C227 \\sim C224 \\sim C228 \\sim C223 \\sim
C222 \\sim C221 \\sim Au48 \\sim Au49: within 2A with sigma of 0.001 and sigma
for terminal atoms of 0.002 within 2A
F6 \\sim C63 \\sim C68 \\sim C67 \\sim C66 \\sim C65 \\sim C64 \\sim C62 \\sim
C61 \\sim Au39 \\sim Au31: within 2A with sigma of 0.001 and sigma for terminal
atoms of 0.002 within 2A
F26 \\sim C263 \\sim C264 \\sim C265 \\sim C266 \\sim C267 \\sim C268 \\sim
C262 \\sim C261 \\sim Au14 \\sim Au38: within 2A with sigma of 0.001 and sigma
for terminal atoms of 0.002 within 2A
F16 \\sim C162 \\sim C163 \\sim C168 \\sim C167 \\sim C166 \\sim C165 \\sim
C164 \\sim C161 \\sim Au43 \\sim Au21: within 2A with sigma of 0.001 and sigma
for terminal atoms of 0.002 within 2A
F25 \\sim C253 \\sim C254 \\sim C255 \\sim C256 \\sim C257 \\sim C258 \\sim
C252 \\sim C251 \\sim Au29 \\sim Au42: within 2A with sigma of 0.001 and sigma
for terminal atoms of 0.002 within 2A
F3 \\sim C33 \\sim C38 \\sim C37 \\sim C36 \\sim C35 \\sim C34 \\sim C32 \\sim
C31 \\sim Au47 \\sim Au50: within 2A with sigma of 0.001 and sigma for terminal
atoms of 0.002 within 2A
C41 \\sim Au47 \\sim Au30 \\sim C42 \\sim C43 \\sim C48 \\sim C47 \\sim C46
\\sim C45 \\sim C44 \\sim F4: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.002 within 2A
F5 \\sim C53 \\sim C54 \\sim C55 \\sim C56 \\sim C57 \\sim C58 \\sim C52 \\sim
C51 \\sim Au39 \\sim Au13: within 2A with sigma of 0.001 and sigma for terminal
atoms of 0.002 within 2A
F12 \\sim C128 \\sim C127 \\sim C126 \\sim C125 \\sim C124 \\sim C122 \\sim
C123 \\sim C121 \\sim Au35 \\sim Au36: within 2A with sigma of 0.001 and sigma
for terminal atoms of 0.002 within 2A
F19 \\sim C193 \\sim C198 \\sim C197 \\sim C196 \\sim C195 \\sim C194 \\sim
C192 \\sim C191 \\sim Au45 \\sim Au25: within 2A with sigma of 0.001 and sigma
for terminal atoms of 0.002 within 2A
F24 \\sim C243 \\sim C244 \\sim C245 \\sim C246 \\sim C247 \\sim C248 \\sim
C242 \\sim C241 \\sim Au28 \\sim Au42: within 2A with sigma of 0.001 and sigma
for terminal atoms of 0.002 within 2A
F21 \\sim C218 \\sim C217 \\sim C216 \\sim C215 \\sim C214 \\sim C213 \\sim
C212 \\sim C211 \\sim Au18 \\sim Au48: within 2A with sigma of 0.001 and sigma
for terminal atoms of 0.002 within 2A
Au40 \\sim C81 \\sim C82 \\sim Au15 \\sim C83 \\sim C84 \\sim C85 \\sim C86
\\sim C87 \\sim C88 \\sim F8: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.002 within 2A
Au37 \\sim C141 \\sim C142 \\sim Au26 \\sim C143 \\sim C144 \\sim C145 \\sim
C146 \\sim C147 \\sim C148 \\sim F14: within 2A with sigma of 0.001 and sigma
for terminal atoms of 0.002 within 2A
F8 \\sim C85 \\sim C86 \\sim C87 \\sim C88 \\sim C83 \\sim C84 \\sim C82 \\sim
C81 \\sim Au40 \\sim Au15: within 2A with sigma of 0.001 and sigma for terminal
atoms of 0.002 within 2A
Au49 \\sim C231 \\sim C232 \\sim Au33 \\sim F23 \\sim C233 \\sim C238 \\sim
C237 \\sim C236 \\sim C235 \\sim C234: within 2A with sigma of 0.001 and sigma
for terminal atoms of 0.002 within 2A
F11 \\sim C115 \\sim C116 \\sim C117 \\sim C113 \\sim C118 \\sim C114 \\sim
C112 \\sim C111 \\sim Au36 \\sim Au34: within 2A with sigma of 0.001 and sigma
for terminal atoms of 0.002 within 2A
F10 \\sim C103 \\sim C108 \\sim C107 \\sim C106 \\sim C105 \\sim C104 \\sim
C102 \\sim C101 \\sim Au41 \\sim Au32: within 2A with sigma of 0.001 and sigma
for terminal atoms of 0.002 within 2A
F9 \\sim C92 \\sim C93 \\sim C98 \\sim C97 \\sim C96 \\sim C95 \\sim C94 \\sim
C91 \\sim Au16 \\sim Au41: within 2A with sigma of 0.001 and sigma for terminal
atoms of 0.002 within 2A
F15 \\sim C153 \\sim C154 \\sim C155 \\sim C156 \\sim C157 \\sim C158 \\sim
C152 \\sim C151 \\sim Au43 \\sim Au27: within 2A with sigma of 0.001 and sigma
for terminal atoms of 0.002 within 2A
F1 \\sim C12 \\sim C13 \\sim C18 \\sim C17 \\sim C16 \\sim C15 \\sim C14 \\sim
C11 \\sim Au46 \\sim Au24: within 2A with sigma of 0.001 and sigma for terminal
atoms of 0.002 within 2A
F13 \\sim C138 \\sim C137 \\sim C136 \\sim C135 \\sim C134 \\sim C133 \\sim
C132 \\sim C131 \\sim Au37 \\sim Au38: within 2A with sigma of 0.001 and sigma
for terminal atoms of 0.002 within 2A
F17 \\sim C176 \\sim C177 \\sim C178 \\sim C173 \\sim C174 \\sim C175 \\sim
C172 \\sim Au22 \\sim Au44 \\sim C171: within 2A with sigma of 0.001 and sigma
for terminal atoms of 0.002 within 2A
F18 \\sim C183 \\sim C184 \\sim C185 \\sim C186 \\sim C187 \\sim C188 \\sim
C182 \\sim C181 \\sim Au20 \\sim Au44: within 2A with sigma of 0.001 and sigma
for terminal atoms of 0.002 within 2A
F2 \\sim C27 \\sim C26 \\sim C25 \\sim C24 \\sim C23 \\sim C28 \\sim C22 \\sim
C21 \\sim Au46 \\sim Au23: within 2A with sigma of 0.001 and sigma for terminal
atoms of 0.002 within 2A
Au40 \\sim C71 \\sim C72 \\sim Au17 \\sim C73 \\sim C74 \\sim C75 \\sim C76
\\sim C77 \\sim C78 \\sim F7: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.002 within 2A
5.a Aromatic/amide H refined with riding coordinates:
 C18(H18), C16(H16), C15(H15), C14(H14), C28(H28), C26(H26), C25(H25),
 C24(H24), C38(H38), C36(H36), C35(H35), C34(H34), C48(H48), C47(H47), C46(H46),
  C44(H44), C54(H54), C56(H56), C57(H57), C58(H58), C68(H68), C66(H66),
 C65(H65), C64(H64), C74(H74), C75(H75), C76(H76), C78(H78), C84(H84), C85(H85),
  C86(H86), C88(H88), C98(H98), C96(H96), C95(H95), C94(H94), C108(H108),
 C106(H106), C105(H105), C104(H104), C114(H114), C115(H115), C116(H116),
 C118(H118), C128(H128), C126(H126), C125(H125), C124(H124), C138(H138),
 C136(H136), C135(H135), C134(H134), C148(H148), C146(H146), C145(H145),
 C144(H144), C154(H154), C155(H155), C156(H156), C158(H158), C168(H168),
 C166(H166), C165(H165), C164(H164), C174(H174), C175(H175), C176(H176),
 C178(H178), C184(H184), C185(H185), C186(H186), C188(H188), C198(H198),
 C196(H196), C195(H195), C194(H194), C208(H208), C206(H206), C205(H205),
 C204(H204), C218(H218), C216(H216), C215(H215), C214(H214), C224(H224),
 C225(H225), C226(H226), C228(H228), C238(H238), C236(H236), C235(H235),
 C234(H234), C244(H244), C245(H245), C246(H246), C248(H248), C254(H254),
 C255(H255), C256(H256), C258(H258), C264(H264), C265(H265), C266(H266),
 C268(H268)
5.b Fitted hexagon refined as free rotating group:
 C13(C18,C17,C16,C15,C14), C23(C28,C27,C26,C25,C24), C33(C38,C37,C36,C35,C34),
 C43(C48,C47,C46,C45,C44), C53(C54,C55,C56,C57,C58), C63(C68,C67,C66,C65,C64),
 C73(C74,C75,C76,C77,C78), C83(C84,C85,C86,C87,C88), C93(C98,C97,C96,C95,C94),
 C103(C108,C107,C106,C105,C104), C113(C114,C115,C116,C117,C118), C123(C128,C127,
 C126,C125,C124), C133(C138,C137,C136,C135,C134), C143(C148,C147,C146,C145,
 C144), C153(C154,C155,C156,C157,C158), C163(C168,C167,C166,C165,C164),
 C173(C174,C175,C176,C177,C178), C183(C184,C185,C186,C187,C188), C193(C198,C197,
 C196,C195,C194), C203(C208,C207,C206,C205,C204), C213(C218,C217,C216,C215,
 C214), C223(C224,C225,C226,C227,C228), C233(C238,C237,C236,C235,C234),
 C243(C244,C245,C246,C247,C248), C253(C254,C255,C256,C257,C258), C263(C264,C265,
 C266,C267,C268)
;
_shelx_res_checksum              5160
_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 2.607
_oxdiff_exptl_absorpt_empirical_full_min 0.665