Intensely luminescent gold(I) phosphinopyridyl clusters: visualization of unsupported aurophilic interactions in solution
Lei, Zhen; Zhang, Jin-Yuan; Guan, Zong-Jie; Wang, Quan-Ming; Chem. Commun.  (2017) –; doi:10.1039/C7CC06944H

data_7120644
_publ_section_title
;
 Intensely luminescent gold(I) phosphinopyridyl clusters: visualization of
 unsupported aurophilic interactions in solution
;
_journal_name_full               'Chem. Commun.'
_journal_paper_doi               10.1039/C7CC06944H
_journal_year                    2017
_chemical_formula_moiety         'C102 H78 Au9 N6 P6, 3(B F4)'
_chemical_formula_sum            'C102 H78 Au9 B3 F12 N6 P6'
_chemical_formula_weight         3606.65
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-07-28
_audit_creation_method
;
Olex2 1.2
(compiled 2016.08.25 svn.r3337 for OlexSys, GUI svn.r5221)
;
_audit_update_record
;
2017-09-05 deposited with the CCDC.
2017-09-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.8293(3)
_cell_length_b                   19.8167(2)
_cell_length_c                   27.5843(4)
_cell_measurement_reflns_used    14731
_cell_measurement_temperature    173.00(14)
_cell_measurement_theta_max      62.1100
_cell_measurement_theta_min      3.2560
_cell_volume                     13572.4(3)
_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      173.00(14)
_diffrn_detector_area_resol_mean 16.1903
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0425
_diffrn_reflns_av_unetI/netI     0.0550
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            28481
_diffrn_reflns_point_group_measured_fraction_full 0.750
_diffrn_reflns_point_group_measured_fraction_max 0.750
_diffrn_reflns_theta_full        62.082
_diffrn_reflns_theta_max         62.082
_diffrn_reflns_theta_min         3.204
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    18.913
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.38214
_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            green
_exptl_crystal_density_diffrn    1.765
_exptl_crystal_description       block
_exptl_crystal_F_000             6624
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.16
_platon_squeeze_details
;
;
_refine_diff_density_max         3.480
_refine_diff_density_min         -3.223
_refine_diff_density_rms         0.236
_refine_ls_abs_structure_details
;
 Flack x determined using 4357 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.200(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     952
_refine_ls_number_reflns         16067
_refine_ls_number_restraints     763
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0708
_refine_ls_R_factor_gt           0.0688
_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^)+(0.1261P)^2^+42.2146P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1826
_refine_ls_wR_factor_ref         0.1854
_reflns_Friedel_coverage         0.479
_reflns_Friedel_fraction_full    0.498
_reflns_Friedel_fraction_max     0.498
_reflns_number_gt                15205
_reflns_number_total             16067
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc06944h2.cif
_cod_data_source_block           1
_cod_database_code               7120644
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
P6 \\sim C611 \\sim C612 \\sim C613 \\sim C614 \\sim C615 \\sim C616: within 2A
with sigma of 0.001 and sigma for terminal atoms of 0.002
P3 \\sim C311 \\sim C312 \\sim C313 \\sim C314 \\sim C315 \\sim C316: within 2A
with sigma of 0.001 and sigma for terminal atoms of 0.002
P5 \\sim C521 \\sim C522 \\sim C523 \\sim C524 \\sim C525 \\sim C526: within 2A
with sigma of 0.001 and sigma for terminal atoms of 0.002
P1 \\sim C121 \\sim C122 \\sim C123 \\sim C124 \\sim C125 \\sim C126: within 2A
with sigma of 0.001 and sigma for terminal atoms of 0.002
Au4 \\sim Au5 \\sim N236 \\sim C231 \\sim C232 \\sim C233 \\sim C234 \\sim
C235: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002
P2 \\sim C221 \\sim C222 \\sim C223 \\sim C224 \\sim C225 \\sim C226: within 2A
with sigma of 0.001 and sigma for terminal atoms of 0.002
P4 \\sim C411 \\sim C412 \\sim C413 \\sim C414 \\sim C415 \\sim C416: within 2A
with sigma of 0.001 and sigma for terminal atoms of 0.002
P4 \\sim C421 \\sim C422 \\sim C423 \\sim C424 \\sim C425 \\sim C426: within 2A
with sigma of 0.001 and sigma for terminal atoms of 0.002
F1 \\sim F2 \\sim F3 \\sim F4 \\sim B1: within 2A with sigma of 0.001 and sigma
for terminal atoms of 0.002
F5 \\sim F6 \\sim F7 \\sim F8 \\sim B2: within 2A with sigma of 0.001 and sigma
for terminal atoms of 0.002
F9 \\sim F10 \\sim F11 \\sim F12 \\sim B3: within 2A with sigma of 0.001 and
sigma for terminal atoms of 0.002
Au4 \\sim Au6 \\sim P6 \\sim N636 \\sim C631 \\sim C632 \\sim C633 \\sim C634
\\sim C635 \\sim C635: within 2A with sigma of 0.001 and sigma for terminal
atoms of 0.002
Au1 \\sim Au3 \\sim P1 \\sim N136 \\sim C131 \\sim C132 \\sim C133 \\sim C134
\\sim C135: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002
P1 \\sim C111 \\sim C112 \\sim C113 \\sim C114 \\sim C115 \\sim C116: within 2A
with sigma of 0.001 and sigma for terminal atoms of 0.002
Au5 \\sim Au6 \\sim P4 \\sim N436 \\sim C431 \\sim C432 \\sim C433 \\sim C434
\\sim C435: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002
Au2 \\sim Au3 \\sim P5 \\sim N536 \\sim C531 \\sim C532 \\sim C533 \\sim C534
\\sim C535: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002
P5 \\sim C511 \\sim C512 \\sim C513 \\sim C514 \\sim C515 \\sim C516: within 2A
with sigma of 0.001 and sigma for terminal atoms of 0.002
P3 \\sim C321 \\sim C322 \\sim C323 \\sim C324 \\sim C325 \\sim C326: within 2A
with sigma of 0.001 and sigma for terminal atoms of 0.002
P6 \\sim C621 \\sim C622 \\sim C623 \\sim C624 \\sim C625 \\sim C626: within 2A
with sigma of 0.001 and sigma for terminal atoms of 0.002
Au1 \\sim Au2 \\sim P3 \\sim N336 \\sim C331 \\sim C332 \\sim C333 \\sim C334
\\sim C335: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002
C211 \\sim C212 \\sim C213 \\sim C214 \\sim C215 \\sim C216: within 2A with
sigma of 0.001 and sigma for terminal atoms of 0.002
3.a Aromatic/amide H refined with riding coordinates:
 C112(H112), C116(H116), C115(H115), C114(H114), C113(H113), C124(H124),
 C125(H125), C126(H126), C122(H122), C123(H123), C134(H134), C133(H133),
 C132(H132), C216(H216), C215(H215), C214(H214), C213(H213), C212(H212),
 C222(H222), C223(H223), C224(H224), C225(H225), C226(H226), C232(H232),
 C233(H233), C234(H234), C314(H314), C315(H315), C316(H316), C312(H312),
 C313(H313), C322(H322), C323(H323), C324(H324), C325(H325), C326(H326),
 C332(H332), C333(H333), C334(H334), C412(H412), C413(H413), C414(H414),
 C415(H415), C416(H416), C422(H422), C423(H423), C424(H424), C425(H425),
 C426(H426), C434(H434), C433(H433), C432(H432), C512(H512), C516(H516),
 C515(H515), C514(H514), C513(H513), C522(H522), C523(H523), C524(H524),
 C525(H525), C526(H526), C534(H534), C533(H533), C532(H532), C613(H613),
 C614(H614), C615(H615), C616(H616), C612(H612), C622(H622), C623(H623),
 C624(H624), C625(H625), C626(H626), C634(H634), C633(H633), C632(H632)
3.b Fitted hexagon refined as free rotating group:
 C112(C111,C116,C115,C114,C113), C124(C125,C126,C121,C122,C123), C134(C133,
 C132,C131,N136,C135), C211(C216,C215,C214,C213,C212), C222(C223,C224,C225,C226,
 C221), C231(C232,C233,C234,C235,N236), C314(C315,C316,C311,C312,C313),
 C321(C322,C323,C324,C325,C326), C331(C332,C333,C334,C335,N336), C411(C412,C413,
 C414,C415,C416), C421(C422,C423,C424,C425,C426), C431(N436,C435,C434,C433,
 C432), C512(C511,C516,C515,C514,C513), C521(C522,C523,C524,C525,C526),
 C535(C534,C533,C532,C531,N536), C613(C614,C615,C616,C611,C612), C621(C622,C623,
 C624,C625,C626), C631(N636,C635,C634,C633,C632)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'