A highly luminescent octanuclear gold(i) carbide cluster
Feuerstein, Thomas J.; Poß, Marieke; Seifert, Tim P.; Bestgen, Sebastian; Feldmann, Claus; Roesky, Peter W.; Chem. Commun.  (2017) –; doi:10.1039/C7CC04171C

data_7120505
_publ_section_title
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 A highly luminescent octanuclear gold(i) carbide cluster
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_journal_name_full               'Chem. Commun.'
_journal_paper_doi               10.1039/C7CC04171C
_journal_year                    2017
_chemical_formula_moiety         'C60 H86 Au2 N4 Si2'
_chemical_formula_sum            'C60 H86 Au2 N4 Si2'
_chemical_formula_weight         1313.44
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-05-27
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
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2017-05-29 deposited with the CCDC.
2017-07-19 downloaded from the CCDC.
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_cell_angle_alpha                62.81(3)
_cell_angle_beta                 71.94(3)
_cell_angle_gamma                79.18(3)
_cell_formula_units_Z            1
_cell_length_a                   10.483(2)
_cell_length_b                   14.626(3)
_cell_length_c                   14.711(3)
_cell_measurement_reflns_used    12351
_cell_measurement_temperature    200
_cell_measurement_theta_max      28.38
_cell_measurement_theta_min      1.56
_cell_volume                     1904.6(9)
_computing_cell_refinement       'X-Area Recipe 1.33.0.0 (STOE, 2015)'
_computing_data_collection       'X-Area Pilatus3_SV 1.31.127.0 (STOE, 2016)'
_computing_data_reduction
'X-Area Integrate 1.71.0.0 (STOE, 2016) X-Area X-Red32 1.63.2.0 (STOE, 2017)'
_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_temperature      200.0
_diffrn_detector                 Pilatus100K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'DECTRIS PILATUS 100K'
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '0.5 mm diameter, monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0834
_diffrn_reflns_av_unetI/netI     0.0891
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            15651
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.999
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         1.568
_diffrn_source                   'Mo LFF Sealed Tube'
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    3.909
_exptl_absorpt_correction_T_max  0.3996
_exptl_absorpt_correction_T_min  0.1789
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE X-RED & X-SHAPE'
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.145
_exptl_crystal_description       irregular
_exptl_crystal_F_000             660
_exptl_crystal_size_max          0.612
_exptl_crystal_size_mid          0.457
_exptl_crystal_size_min          0.28
_refine_diff_density_max         1.112
_refine_diff_density_min         -1.274
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.819
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     345
_refine_ls_number_reflns         7403
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      0.819
_refine_ls_R_factor_all          0.0429
_refine_ls_R_factor_gt           0.0319
_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^)+(0.0251P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0655
_refine_ls_wR_factor_ref         0.0668
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5658
_reflns_number_total             7403
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc04171c3.cif
_cod_data_source_block           tjf036
_cod_database_code               7120505
_shelxl_version_number           2014-7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 C4A, C4, C6, C6A, C5A, C5
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C6A) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C5A) \\sim Ueq, Uanis(C5)
\\sim Ueq, Uanis(C4A) \\sim Ueq, Uanis(C4) \\sim Ueq: with sigma of 0.02 and
sigma for terminal atoms of 0.04
Uanis(C4A) \\sim Ueq, Uanis(C6A) \\sim Ueq, Uanis(C5A) \\sim Ueq: with sigma of
0.02 and sigma for terminal atoms of 0.04
4. Others
 Fixed Sof: C5(0.5) H5A(0.5) H5B(0.5) H5C(0.5) C6(0.5) H6A(0.5) H6B(0.5)
 H6C(0.5) C4(0.5) H4A(0.5) H4B(0.5) H4C(0.5) C6A(0.5) H6AA(0.5) H6AB(0.5)
 H6AC(0.5) C4A(0.5) H4AA(0.5) H4AB(0.5) H4AC(0.5) C5A(0.5) H5AA(0.5) H5AB(0.5)
 H5AC(0.5)
 Fixed X: C16(0.614361)
 Fixed Y: C16(0.6644)
 Fixed Z: C16(0.41976)
5.a Ternary CH refined with riding coordinates:
 C13(H13), C16(H16), C25(H25), C28(H28)
5.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C10(H10), C11(H11), C21(H21), C22(H22), C23(H23)
5.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C17(H17A,H17B,H17C), C18(H18A,H18B,
 H18C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C29(H29A,H29B,H29C), C30(H30A,
 H30B,H30C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C4(H4A,H4B,H4C), C6A(H6AA,H6AB,
 H6AC), C4A(H4AA,H4AB,H4AC), C5A(H5AA,H5AB,H5AC)
;
_shelx_res_checksum              87009
_shelx_fab_checksum              25905
_olex2_submission_special_instructions 'No special instructions were received'