Higher stability within metalloid tin clusters via Cation-Anion interaction.
Schnepf, Andreas; Schrenk, Claudio; Kimmich, Roman; Dalton Transactions  (2021) –; doi:10.1039/D1DT02591K

data_7708428
_publ_section_title
;
 Higher stability within metalloid tin clusters via Cation-Anion
 interaction.
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT02591K
_journal_year                    2021
_chemical_formula_moiety         'C67 H164 K2 O6 Si16 Sn10, C7 H8'
_chemical_formula_sum            'C74 H172 K2 O6 Si16 Sn10'
_chemical_formula_weight         2872.65
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-12-07
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-07-27 deposited with the CCDC.	2021-09-24 downloaded from the CCDC.
;
_cell_angle_alpha                90.518(3)
_cell_angle_beta                 101.709(3)
_cell_angle_gamma                102.171(3)
_cell_formula_units_Z            2
_cell_length_a                   17.545(3)
_cell_length_b                   19.004(4)
_cell_length_c                   20.559(4)
_cell_measurement_reflns_used    9954
_cell_measurement_temperature    150
_cell_measurement_theta_max      24.980
_cell_measurement_theta_min      2.196
_cell_volume                     6552(2)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2016)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2016)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.0
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0759
_diffrn_reflns_av_unetI/netI     0.0677
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            98404
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.750
_diffrn_reflns_theta_max         24.750
_diffrn_reflns_theta_min         1.877
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    2.116
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5627
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1432 before and 0.0615 after correction. The Ratio of minimum to maximum transmission is 0.7549. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.456
_exptl_crystal_description       plate
_exptl_crystal_F_000             2852
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: toluene'
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.057
_exptl_crystal_size_min          0.018
_refine_diff_density_max         1.860
_refine_diff_density_min         -0.793
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1149
_refine_ls_number_reflns         22437
_refine_ls_number_restraints     433
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0847
_refine_ls_R_factor_gt           0.0470
_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^)+(0.0482P)^2^+24.0225P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1057
_refine_ls_wR_factor_ref         0.1332
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15024
_reflns_number_total             22437
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02591k2.cif
_cod_data_source_block           2_sq
_cod_database_code               7708428
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.963
_shelx_estimated_absorpt_t_min   0.560
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C320-C321 \\sim C321-C322 \\sim C322-C323 \\sim C323-C324 \\sim C324-C325
\\sim C325-C320
 with sigma of 0.02
 C320-C324 \\sim C320-C322 \\sim C325-C323 \\sim C321-C325 \\sim C322-C324
\\sim C321-C323
 with sigma of 0.04
 C319-C325 \\sim C319-C321
 with sigma of 0.04
 C327-C332 \\sim C332-C331 \\sim C331-C330 \\sim C330-C329 \\sim C329-C328
\\sim C328-C327
 with sigma of 0.02
 C327-C329 \\sim C327-C331 \\sim C328-C330 \\sim C332-C328 \\sim C331-C329
\\sim C332-C330
 with sigma of 0.04
 C326-C328 \\sim C326-C332
 with sigma of 0.04
 Si91-C916 \\sim Si91-C914 \\sim Si91-C913 \\sim Si91-C912 \\sim Si91-C915
\\sim Si91-C911
 with sigma of 0.02
3. Restrained planarity
 C319, C320, C321, C322, C323, C324, C325
 with sigma of 0.1
 C326, C327, C328, C329, C330, C331, C332
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C319 \\sim C320 \\sim C321 \\sim C322 \\sim C323 \\sim C324 \\sim C325: within
2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C326 \\sim C327 \\sim C328 \\sim C329 \\sim C330 \\sim C331 \\sim C332: within
2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C433 \\sim C439: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
C623 \\sim C646: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
C632 \\sim C651: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
C436 \\sim C440: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
Uanis(C914) \\sim Ueq, Uanis(C911) \\sim Ueq, Uanis(C915) \\sim Ueq,
Uanis(C912) \\sim Ueq, Uanis(C916) \\sim Ueq, Uanis(C913) \\sim Ueq: with sigma
of 0.015 and sigma for terminal atoms of 0.03
Uanis(C646) \\sim Ueq, Uanis(C623) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C425) \\sim Ueq, Uanis(C423) \\sim Ueq, Uanis(C424) \\sim Ueq,
Uanis(C422) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C214) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C432) \\sim Ueq, Uanis(C437) \\sim Ueq, Uanis(C431) \\sim Ueq,
Uanis(C438) \\sim Ueq, Uanis(C440) \\sim Ueq, Uanis(C436) \\sim Ueq,
Uanis(C439) \\sim Ueq, Uanis(C433) \\sim Ueq, Uanis(C441) \\sim Ueq,
Uanis(C435) \\sim Ueq, Uanis(C442) \\sim Ueq, Uanis(C434) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 C319, C320, C321, C322, C323, C324, C325
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C326, C327, C328, C329, C330, C331, C332
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(C914)=Sof(H91J)=Sof(H91K)=Sof(H91L)=Sof(C915)=Sof(H91M)=Sof(H91N)=
 Sof(H91O)=Sof(C916)=Sof(H91P)=Sof(H91Q)=Sof(H91R)=1-FVAR(1)
 Sof(C911)=Sof(H91A)=Sof(H91B)=Sof(H91C)=Sof(C912)=Sof(H91D)=Sof(H91E)=
 Sof(H91F)=Sof(C913)=Sof(H91G)=Sof(H91H)=Sof(H91I)=FVAR(1)
 Sof(C437)=Sof(H43P)=Sof(H43Q)=Sof(H43R)=Sof(C438)=Sof(H43S)=Sof(H43T)=
 Sof(H43U)=Sof(C439)=Sof(C440)=Sof(H44A)=Sof(H44B)=Sof(H44C)=Sof(C441)=
 Sof(H44D)=Sof(H44E)=Sof(H44F)=Sof(C442)=Sof(H44G)=Sof(H44H)=Sof(H44I)=1-FVAR(2)
 Sof(C431)=Sof(H43A)=Sof(H43B)=Sof(H43C)=Sof(C432)=Sof(H43D)=Sof(H43E)=
 Sof(H43F)=Sof(C433)=Sof(C434)=Sof(H43G)=Sof(H43H)=Sof(H43I)=Sof(C435)=
 Sof(H43J)=Sof(H43K)=Sof(H43L)=Sof(C436)=Sof(H43M)=Sof(H43N)=Sof(H43O)=FVAR(2)
 Sof(Si64)=Sof(Si65)=Sof(C641)=Sof(H64A)=Sof(H64B)=Sof(H64C)=Sof(C642)=
 Sof(H64D)=Sof(H64E)=Sof(H64F)=Sof(C643)=Sof(C644)=Sof(H64G)=Sof(H64H)=
 Sof(H64I)=Sof(C645)=Sof(H64J)=Sof(H64K)=Sof(H64L)=Sof(C646)=Sof(H64M)=
 Sof(H64N)=Sof(H64O)=Sof(C651)=Sof(H65A)=Sof(H65B)=Sof(H65C)=Sof(C652)=
 Sof(H65D)=Sof(H65E)=Sof(H65F)=Sof(C653)=Sof(H65G)=Sof(H65H)=Sof(H65I)=1-FVAR(3)
 Sof(Si62)=Sof(Si63)=Sof(C621)=Sof(H62A)=Sof(H62B)=Sof(H62C)=Sof(C622)=
 Sof(H62D)=Sof(H62E)=Sof(H62F)=Sof(C623)=Sof(H62G)=Sof(H62H)=Sof(H62I)=
 Sof(C631)=Sof(H63A)=Sof(H63B)=Sof(H63C)=Sof(C632)=Sof(H63D)=Sof(H63E)=
 Sof(H63F)=Sof(C633)=Sof(C634)=Sof(H63G)=Sof(H63H)=Sof(H63I)=Sof(C635)=
 Sof(H63J)=Sof(H63K)=Sof(H63L)=Sof(C636)=Sof(H63M)=Sof(H63N)=Sof(H63O)=FVAR(3)
 Sof(C424)=Sof(H42J)=Sof(H42K)=Sof(H42L)=Sof(C425)=Sof(H42M)=Sof(H42N)=
 Sof(H42O)=1-FVAR(4)
 Sof(C422)=Sof(H42D)=Sof(H42E)=Sof(H42F)=Sof(C423)=Sof(H42G)=Sof(H42H)=
 Sof(H42I)=FVAR(4)
7.a Free rotating group:
 C319(C320,C321,C322,C323,C324,C325), C326(C327,C328,C329,C330,C331,C332)
7.b Secondary CH2 refined with riding coordinates:
 C302(H30A,H30B), C303(H30C,H30D), C305(H30E,H30F), C306(H30G,H30H), C308(H30I,
 H30J), C309(H30K,H30L), C311(H31A,H31B), C312(H31C,H31D), C314(H31E,H31F),
 C315(H31G,H31H), C317(H31I,H31J), C318(H31K,H31L)
7.c Me refined with riding coordinates:
 C211(H21A,H21B,H21C), C212(H21D,H21E,H21F), C214(H21G,H21H,H21I), C215(H21J,
 H21K,H21L), C216(H21M,H21N,H21O), C221(H22A,H22B,H22C), C222(H22D,H22E,H22F),
 C223(H22G,H22H,H22I), C231(H23A,H23B,H23C), C232(H23D,H23E,H23F), C233(H23G,
 H23H,H23I), C319(H31M,H31N,H31O), C411(H41A,H41B,H41C), C412(H41D,H41E,H41F),
 C413(H41G,H41H,H41I), C421(H42A,H42B,H42C), C422(H42D,H42E,H42F), C423(H42G,
 H42H,H42I), C424(H42J,H42K,H42L), C425(H42M,H42N,H42O), C431(H43A,H43B,H43C),
 C432(H43D,H43E,H43F), C434(H43G,H43H,H43I), C435(H43J,H43K,H43L), C436(H43M,
 H43N,H43O), C437(H43P,H43Q,H43R), C438(H43S,H43T,H43U), C440(H44A,H44B,H44C),
 C441(H44D,H44E,H44F), C442(H44G,H44H,H44I), C611(H61A,H61B,H61C), C612(H61D,
 H61E,H61F), C613(H61G,H61H,H61I), C621(H62A,H62B,H62C), C622(H62D,H62E,H62F),
 C623(H62G,H62H,H62I), C631(H63A,H63B,H63C), C632(H63D,H63E,H63F), C634(H63G,
 H63H,H63I), C635(H63J,H63K,H63L), C636(H63M,H63N,H63O), C641(H64A,H64B,H64C),
 C642(H64D,H64E,H64F), C644(H64G,H64H,H64I), C645(H64J,H64K,H64L), C646(H64M,
 H64N,H64O), C651(H65A,H65B,H65C), C652(H65D,H65E,H65F), C653(H65G,H65H,H65I),
 C911(H91A,H91B,H91C), C912(H91D,H91E,H91F), C913(H91G,H91H,H91I), C914(H91J,
 H91K,H91L), C915(H91M,H91N,H91O), C916(H91P,H91Q,H91R), C921(H92A,H92B,H92C),
 C922(H92D,H92E,H92F), C924(H92G,H92H,H92I), C925(H92J,H92K,H92L), C926(H92M,
 H92N,H92O), C931(H93A,H93B,H93C), C932(H93D,H93E,H93F), C933(H93G,H93H,H93I)
7.d Aromatic/amide H refined with riding coordinates:
 C321(H321), C322(H322), C323(H323), C324(H324), C325(H325), C328(H328),
 C329(H329), C330(H330), C331(H331), C332(H332)
7.e Idealised Me refined as rotating group:
 C326(H32A,H32B,H32C)
;
_shelx_res_checksum              96459
_shelx_fab_checksum              21567
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'