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_7120643
_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         'C138 H108 Au11 N6 P8, 5(B F4)'
_chemical_formula_sum            'C138 H108 Au11 B5 F20 N6 P8'
_chemical_formula_weight         4698.74
_space_group_crystal_system      trigonal
_space_group_IT_number           155
_space_group_name_Hall           'R 3 2"'
_space_group_name_H-M_alt        'R 3 2'
_symmetry_space_group_name_Hall  'R 3 2"'
_symmetry_space_group_name_H-M   'R 3 2 :H'
_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                120
_cell_formula_units_Z            3
_cell_length_a                   26.6485(13)
_cell_length_b                   26.6485(13)
_cell_length_c                   22.8335(19)
_cell_measurement_reflns_used    3401
_cell_measurement_temperature    173.00(14)
_cell_measurement_theta_max      26.1800
_cell_measurement_theta_min      3.0680
_cell_volume                     14042.6(15)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0357
_diffrn_reflns_av_unetI/netI     0.0523
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            11116
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.939
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    8.708
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.47791
_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            red
_exptl_crystal_density_diffrn    1.667
_exptl_crystal_description       block
_exptl_crystal_F_000             6516
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_platon_squeeze_details
;
;
_refine_diff_density_max         2.239
_refine_diff_density_min         -2.834
_refine_diff_density_rms         0.205
_refine_ls_abs_structure_details
;
 Flack x determined using 1786 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.504(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     228
_refine_ls_number_reflns         5519
_refine_ls_number_restraints     189
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0693
_refine_ls_R_factor_gt           0.0560
_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^)+(0.1103P)^2^+28.0450P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1593
_refine_ls_wR_factor_ref         0.1704
_reflns_Friedel_coverage         0.870
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                4537
_reflns_number_total             5519
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc06944h2.cif
_cod_data_source_block           2
_cod_original_cell_volume        14042.6(18)
_cod_database_code               7120643
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 B2-F3 = B2-F4 = B2-F5 = B2-F6
 1.35 with sigma of 0.02
 F3-F4 = F3-F5 = F3-F6 = F4-F5 = F4-F6 = F5-F6
 2.25 with sigma of 0.02
3. Restrained planarity
 Au1, P1, N1, C13, C14, C15, C16, C17
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
F1 \\sim F2 \\sim B1: within 2A with sigma of 0.001 and sigma for terminal
atoms of 0.002
Au1 \\sim P1 \\sim N1 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17: within
2A with sigma of 0.001 and sigma for terminal atoms of 0.002
P1 \\sim C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6: within 2A with sigma
of 0.001 and sigma for terminal atoms of 0.002
P1 \\sim C7 \\sim C8 \\sim C9 \\sim C10 \\sim C11 \\sim C12: within 2A with
sigma of 0.001 and sigma for terminal atoms of 0.002
P2 \\sim C18 \\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim C23: within 2A with
sigma of 0.001 and sigma for terminal atoms of 0.002
F3 \\sim F4 \\sim F5 \\sim F6 \\sim B2: within 2A with sigma of 0.001 and sigma
for terminal atoms of 0.002
5. Others
 Fixed Sof: F3(0.33333) F4(0.33333) F5(0.33333) F6(0.33333) B2(0.33333)
6.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C12(H12), C11(H11), C10(H10), C9(H9),
 C8(H8), C14(H14), C15(H15), C16(H16), C23(H23), C22(H22), C21(H21), C20(H20),
 C19(H19)
6.b Fitted hexagon refined as free rotating group:
 C1(C2,C3,C4,C5,C6), C7(C12,C11,C10,C9,C8), C17(N1,C13,C14,C15,C16), C18(C23,
 C22,C21,C20,C19)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'