[Hyp-Au-Sn9(Hyp)3-Au-Sn9(Hyp)3-Au-Hyp]-: The longest intermetalloid chain compound of tin TBC - Phil Power's 65th birthday
Binder, Mareike; Schrenk, Claudio; Poettgen, Rainer; Block, Theresa; Schnepf, Andreas; Chem. Commun.  (2017) –; doi:10.1039/C7CC07029B

data_7120703
_publ_section_title
;
 [Hyp-Au-Sn9(Hyp)3-Au-Sn9(Hyp)3-Au-Hyp]-: The longest intermetalloid chain
 compound of tin TBC - Phil Power's 65th birthday
;
_journal_name_full               'Chem. Commun.'
_journal_paper_doi               10.1039/C7CC07029B
_journal_year                    2017
_chemical_formula_moiety         'C72 H216 Au3 Si32 Sn18'
_chemical_formula_sum            'C72 H216 Au3 Si32 Sn18'
_chemical_formula_weight         4708.63
_chemical_properties_physical
', Air-sensitive,Moisture-sensitive,Oxygen-sensitive,Pyrophoric'
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2017-05-16
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2017-05-19 deposited with the CCDC.
2017-09-25 downloaded from the CCDC.
;
_cell_angle_alpha                81.862(2)
_cell_angle_beta                 87.078(2)
_cell_angle_gamma                63.232(2)
_cell_formula_units_Z            1
_cell_length_a                   14.9081(6)
_cell_length_b                   16.3138(7)
_cell_length_c                   24.6890(10)
_cell_measurement_reflns_used    9907
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      25.550
_cell_measurement_theta_min      2.279
_cell_volume                     5306.6(4)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 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_temperature      180.0
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0986
_diffrn_reflns_av_unetI/netI     0.1007
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            109833
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.487
_diffrn_reflns_theta_min         1.411
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    4.341
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5555
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1141 before and 0.0738 after correction. The Ratio of minimum to maximum transmission is 0.7452. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.473
_exptl_crystal_description       block
_exptl_crystal_F_000             2233
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: thf, toluene'
_exptl_crystal_size_max          0.279
_exptl_crystal_size_mid          0.079
_exptl_crystal_size_min          0.067
_refine_diff_density_max         2.696
_refine_diff_density_min         -1.577
_refine_diff_density_rms         0.221
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     586
_refine_ls_number_reflns         21803
_refine_ls_number_restraints     344
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.1268
_refine_ls_R_factor_gt           0.0708
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1128P)^2^+6.4580P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1898
_refine_ls_wR_factor_ref         0.2171
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12378
_reflns_number_total             21803
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc07029b2.cif
_cod_data_source_block           7
_cod_database_code               7120703
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
2. Restrained distances
 Si32-C306 = Si32-C305 = Si32-C304
 1.88 with sigma of 0.02
 C110-C106
 2.95 with sigma of 0.05
 Si16-C115 = Si11-C116
 1.88 with sigma of 0.02
 Si15-C113 = Si16-C113
 1.88 with sigma of 0.02
 Si11-C101 = Si11-C103
 1.88 with sigma of 0.02
 Si13-Si1 \\sim Si14-Si1 \\sim Si15-Si1 \\sim Si16-Si1 \\sim Si11-Si1 \\sim
Si12-Si1
 with sigma of 0.02
 Si15-C112 \\sim Si15-C111 \\sim Si15-C113 \\sim Si16-C113 \\sim Si16-C114
\\sim Si12-C104 \\sim Si12-
 C102 \\sim Si14-C110 \\sim Si14-C108 \\sim Si14-C106 \\sim Si11-C103
 with sigma of 0.02
 C101-C103 \\sim C113-C114 \\sim C102-C104 \\sim C113-C112 \\sim C112-C111
\\sim C111-C113
 with sigma of 0.02
 Si1-C101 \\sim Si1-C103 \\sim Si1-C110 \\sim Si1-C106 \\sim Si1-C108 \\sim
Si1-C114 \\sim Si1-C113
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Si15 \\sim Si16: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
Si13 \\sim Si14: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
Si11 \\sim Si12: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.04
C109 \\sim C110: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
C116 \\sim C115: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
C113 \\sim C103 \\sim C105 \\sim C107 \\sim C109 \\sim C111 \\sim C112 \\sim
C102 \\sim C104 \\sim C106 \\sim C108 \\sim C110 \\sim C114: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
C113 \\sim Si15 \\sim Si16: within 3A with sigma of 0.04 and sigma for terminal
atoms of 0.08
C101 \\sim C102 \\sim C104: within 3A with sigma of 0.02 and sigma for terminal
atoms of 0.04
C101: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02
C101 \\sim Si11 \\sim Si12: within 3A with sigma of 0.04 and sigma for terminal
atoms of 0.08
Si21 \\sim C201 \\sim C202 \\sim C203: within 3A with sigma of 0.04 and sigma
for terminal atoms of 0.08
Si41 \\sim C401 \\sim C402 \\sim C403: within 3A with sigma of 0.04 and sigma
for terminal atoms of 0.08
Si42 \\sim C404 \\sim C405 \\sim C406: within 3A with sigma of 0.04 and sigma
for terminal atoms of 0.08
Si43 \\sim C407 \\sim C408 \\sim C409: within 3A with sigma of 0.04 and sigma
for terminal atoms of 0.08
Uanis(C402) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.05
Uanis(C305) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.05
Uanis(C201) \\sim Ueq, Uanis(C306) \\sim Ueq: with sigma of 0.03 and sigma for
terminal atoms of 0.06
Uanis(Si11) \\sim Ueq, Uanis(Si12) \\sim Ueq: with sigma of 0.02 and sigma for
terminal atoms of 0.05
Uanis(Si16) \\sim Ueq, Uanis(Si14) \\sim Ueq, Uanis(Si12) \\sim Ueq, : with
sigma of 0.05 and sigma for terminal atoms of 0.1
Uanis(C203) \\sim Ueq: with sigma of 0.03 and sigma for terminal atoms of 0.06
Uanis(C113) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C201) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C101) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
4. Others
 Sof(H10D)=Sof(H10E)=Sof(H10F)=Sof(H11D)=Sof(H11E)=Sof(H11F)=Sof(Si12)=
 Sof(Si14)=Sof(Si16)=Sof(C102)=Sof(H10S)=Sof(H10T)=Sof(H10U)=Sof(C104)=
 Sof(H10V)=Sof(H10W)=Sof(H10X)=Sof(C106)=Sof(H10Z)=Sof(HF)=Sof(HG)=Sof(C108)=
 Sof(H10Y)=Sof(HD)=Sof(HE)=Sof(C110)=Sof(H11P)=Sof(H11Q)=Sof(H11R)=Sof(C114)=
 Sof(H11M)=Sof(H11N)=Sof(H11O)=Sof(C115)=Sof(H11S)=Sof(H11T)=Sof(H11U)=1-FVAR(1)
 Sof(H10A)=Sof(H10B)=Sof(H10C)=Sof(H11A)=Sof(H11B)=Sof(H11C)=Sof(Si11)=
 Sof(Si13)=Sof(Si15)=Sof(C103)=Sof(H10P)=Sof(H10Q)=Sof(H10R)=Sof(C105)=
 Sof(H10M)=Sof(H10N)=Sof(H10O)=Sof(C107)=Sof(H10G)=Sof(H10H)=Sof(H10I)=
 Sof(C109)=Sof(H10J)=Sof(H10K)=Sof(H10L)=Sof(C111)=Sof(H11J)=Sof(H11K)=
 Sof(H11L)=Sof(C112)=Sof(H11G)=Sof(H11H)=Sof(H11I)=Sof(C116)=Sof(H11V)=
 Sof(H11W)=Sof(H11X)=FVAR(1)
5.a Me refined with riding coordinates:
 C101(H10A,H10B,H10C), C101(H10D,H10E,H10F), C113(H11A,H11B,H11C), C113(H11D,
 H11E,H11F), C201(H20A,H20B,H20C), C202(H20S,H20T,H20U), C203(H20G,H20H,H20I),
 C204(H20D,H20E,H20F), C205(H20Y,HB,HC), C206(H20P,H20Q,H20R), C207(H20J,H20K,
 H20L), C208(H20M,H20N,H20O), C209(H20V,H20W,H20X), C301(H30V,H30W,H30X),
 C302(H30D,H30E,H30F), C303(H30G,H30H,H30I), C304(H30P,H30Q,H30R), C305(H30Y,HH,
 HI), C306(H30M,H30N,H30O), C307(H30A,H30B,H30C), C308(H30S,H30T,H30U),
 C309(H30J,H30K,H30L), C401(H40S,H40T,H40U), C402(H40A,H40B,H40C), C403(H40P,
 H40Q,H40R), C404(H40V,H40W,H40X), C405(H40M,H40N,H40O), C406(H40J,H40K,H40L),
 C407(H40Y,H,HA), C408(H40D,H40E,H40F), C409(H40G,H40H,H40I), C103(H10P,H10Q,
 H10R), C105(H10M,H10N,H10O), C107(H10G,H10H,H10I), C109(H10J,H10K,H10L),
 C111(H11J,H11K,H11L), C112(H11G,H11H,H11I), C116(H11V,H11W,H11X), C102(H10S,
 H10T,H10U), C104(H10V,H10W,H10X), C106(H10Z,HF,HG), C108(H10Y,HD,HE),
 C110(H11P,H11Q,H11R), C114(H11M,H11N,H11O), C115(H11S,H11T,H11U)
;
_shelx_res_checksum              6695
_shelx_fab_checksum              16728
_olex2_submission_special_instructions 'No special instructions were received'