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

data_7708429
_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         'C48 H132 K2 Si16 Sn10'
_chemical_formula_sum            'C48 H132 K2 Si16 Sn10'
_chemical_formula_weight         2424.07
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-05-12
_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
_cell_angle_beta                 116.477(6)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   35.991(4)
_cell_length_b                   18.5716(18)
_cell_length_c                   34.997(4)
_cell_measurement_reflns_used    9860
_cell_measurement_temperature    100
_cell_measurement_theta_max      23.981
_cell_measurement_theta_min      2.192
_cell_volume                     20939(4)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 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      100
_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  0.1100
_diffrn_reflns_av_unetI/netI     0.0536
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            144454
_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         1.546
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    2.628
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5265
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1208 before and 0.0712 after correction. The Ratio of minimum to maximum transmission is 0.7063. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.538
_exptl_crystal_description       irregular
_exptl_crystal_F_000             9456
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: toluene'
_exptl_crystal_size_max          0.339
_exptl_crystal_size_mid          0.228
_exptl_crystal_size_min          0.024
_refine_diff_density_max         1.744
_refine_diff_density_min         -0.956
_refine_diff_density_rms         0.201
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.158
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     825
_refine_ls_number_reflns         17913
_refine_ls_number_restraints     378
_refine_ls_restrained_S_all      1.153
_refine_ls_R_factor_all          0.1059
_refine_ls_R_factor_gt           0.0630
_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^)+(0.0509P)^2^+799.7802P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1397
_refine_ls_wR_factor_ref         0.1838
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12190
_reflns_number_total             17913
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02591k2.cif
_cod_data_source_block           6_sq
_cod_database_code               7708429
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
2. Restrained distances
 C125-C126
 1.54 with sigma of 0.02
 C127-C128 = C130-C129
 1.54 with sigma of 0.02
 C333-C334 = C335-C334
 1.54 with sigma of 0.02
 C734-C735 = C737-C736
 1.54 with sigma of 0.02
 C732-C731 = C733-C731
 1.54 with sigma of 0.02
 C740-C738 = C739-C738
 1.54 with sigma of 0.02
 C332-C331
 1.54 with sigma of 0.02
 Si31-C316 \\sim Si31-C312 \\sim Si31-C311 \\sim Si31-C315 \\sim Si31-C314
\\sim Si31-C313
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C123 \\sim C125: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
C734 \\sim C735: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
C322 \\sim C325: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
C127 \\sim C129: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
C128 \\sim C130: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
C124 \\sim C126: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
C312 \\sim C316: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
C313 \\sim C314: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
C321 \\sim C324: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
C333 \\sim C335: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
C532 \\sim C533: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
C732 \\sim C733: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
C311 \\sim C315: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
C534 \\sim C535: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
C336 \\sim C337: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
C333 \\sim C334: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
Uanis(C128) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C331) \\sim Ueq, Uanis(C332) \\sim Ueq, Uanis(C337) \\sim Ueq,
Uanis(C336) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C321) \\sim Ueq, Uanis(C324) \\sim Ueq, Uanis(C322) \\sim Ueq,
Uanis(C325) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C314) \\sim Ueq, Uanis(C313) \\sim Ueq, Uanis(C315) \\sim Ueq,
Uanis(C311) \\sim Ueq, Uanis(C312) \\sim Ueq, Uanis(C316) \\sim Ueq: with sigma
of 0.02 and sigma for terminal atoms of 0.04
Uanis(C735) \\sim Ueq, Uanis(C734) \\sim Ueq, Uanis(C736) \\sim Ueq,
Uanis(C737) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C123) \\sim Ueq, Uanis(C125) \\sim Ueq: with sigma of 0.02 and sigma for
terminal atoms of 0.04
Uanis(C334) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C324) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C333) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C535) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C122) \\sim Ueq, Uanis(C121) \\sim Ueq: with sigma of 0.02 and sigma for
terminal atoms of 0.04
4. Rigid body (RIGU) restrains
 Si73, C731, C732, C733, C734, C735, C736, C737, C738, C739, C740
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Si31, C311, C312, C313, C314, C315, C316
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C121, C122
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C125)=Sof(H12K)=Sof(H12L)=Sof(H12M)=Sof(C126)=Sof(H12N)=Sof(H12O)=
 Sof(C129)=Sof(H12U)=Sof(H12V)=Sof(H12W)=Sof(C130)=Sof(H13A)=Sof(H13B)=1-FVAR(1)
 Sof(C123)=Sof(H12F)=Sof(H12G)=Sof(H12H)=Sof(C124)=Sof(H12I)=Sof(H12J)=
 Sof(C127)=Sof(H12P)=Sof(H12Q)=Sof(H12R)=Sof(C128)=Sof(H12S)=Sof(H12T)=FVAR(1)
 Sof(C311)=Sof(H31A)=Sof(H31B)=Sof(H31C)=Sof(C312)=Sof(H31D)=Sof(H31E)=
 Sof(H31F)=Sof(C313)=Sof(H31G)=Sof(H31H)=Sof(H31I)=Sof(C321)=Sof(H32A)=
 Sof(H32B)=Sof(H32C)=Sof(C322)=Sof(H32D)=Sof(H32E)=Sof(H32F)=Sof(H33I)=
 Sof(H33J)=Sof(C335)=Sof(H33M)=Sof(H33N)=Sof(H33O)=Sof(H53C)=Sof(H53D)=
 Sof(C533)=Sof(H53H)=Sof(H53I)=Sof(H53J)=Sof(H73D)=Sof(H73E)=Sof(H73F)=
 Sof(C732)=Sof(H73G)=Sof(H73H)=Sof(C734)=Sof(H73K)=Sof(H73L)=Sof(H73M)=
 Sof(C735)=Sof(H73N)=Sof(H73O)=Sof(H73X)=Sof(H73Y)=Sof(H)=Sof(C739)=Sof(H73Z)=
 Sof(HA)=1-FVAR(2)
 Sof(C314)=Sof(H31J)=Sof(H31K)=Sof(H31L)=Sof(C315)=Sof(H31M)=Sof(H31N)=
 Sof(H31O)=Sof(C316)=Sof(H31P)=Sof(H31Q)=Sof(H31R)=Sof(C324)=Sof(H32J)=
 Sof(H32K)=Sof(H32L)=Sof(C325)=Sof(H32M)=Sof(H32N)=Sof(H32O)=Sof(C333)=
 Sof(H33F)=Sof(H33G)=Sof(H33H)=Sof(H33K)=Sof(H33L)=Sof(H53A)=Sof(H53B)=
 Sof(C532)=Sof(H53E)=Sof(H53F)=Sof(H53G)=Sof(H73A)=Sof(H73B)=Sof(H73C)=
 Sof(C733)=Sof(H73I)=Sof(H73J)=Sof(C736)=Sof(H73P)=Sof(H73Q)=Sof(H73R)=
 Sof(C737)=Sof(H73S)=Sof(H73T)=Sof(H73U)=Sof(H73V)=Sof(H73W)=Sof(C740)=
 Sof(H74A)=Sof(H74B)=FVAR(2)
6.a Secondary CH2 refined with riding coordinates:
 C122(H12D,H12E), C124(H12I,H12J), C126(H12N,H12O), C128(H12S,H12T), C130(H13A,
 H13B), C332(H33D,H33E), C334(H33K,H33L), C334(H33I,H33J), C337(H33S,H33T),
 C531(H53C,H53D), C531(H53A,H53B), C534(H53K,H53L), C536(H53P,H53Q), C732(H73G,
 H73H), C733(H73I,H73J), C735(H73N,H73O), C737(H73S,H73T), C739(H73Z,HA),
 C740(H74A,H74B)
6.b Me refined with riding coordinates:
 C111(H11A,H11B,H11C), C113(H11G,H11H,H11I), C121(H12A,H12B,H12C), C123(H12F,
 H12G,H12H), C125(H12K,H12L,H12M), C127(H12P,H12Q,H12R), C129(H12U,H12V,H12W),
 C131(H13C,H13D,H13E), C132(H13F,H13G,H13H), C133(H13I,H13J,H13K), C311(H31A,
 H31B,H31C), C312(H31D,H31E,H31F), C313(H31G,H31H,H31I), C314(H31J,H31K,H31L),
 C315(H31M,H31N,H31O), C316(H31P,H31Q,H31R), C321(H32A,H32B,H32C), C322(H32D,
 H32E,H32F), C323(H32G,H32H,H32I), C324(H32J,H32K,H32L), C325(H32M,H32N,H32O),
 C331(H33A,H33B,H33C), C333(H33F,H33G,H33H), C335(H33M,H33N,H33O), C336(H33P,
 H33Q,H33R), C511(H51A,H51B,H51C), C512(H51D,H51E,H51F), C513(H51G,H51H,H51I),
 C521(H52A,H52B,H52C), C522(H52D,H52E,H52F), C523(H52G,H52H,H52I), C532(H53E,
 H53F,H53G), C533(H53H,H53I,H53J), C535(H53M,H53N,H53O), C537(H53R,H53S,H53T),
 C711(H71A,H71B,H71C), C712(H71D,H71E,H71F), C713(H71G,H71H,H71I), C721(H72A,
 H72B,H72C), C722(H72D,H72E,H72F), C723(H72G,H72H,H72I), C731(H73D,H73E,H73F),
 C731(H73A,H73B,H73C), C734(H73K,H73L,H73M), C736(H73P,H73Q,H73R), C738(H73U,
 H73V,H73W), C738(H73X,H73Y,H)
6.c Idealised Me refined as rotating group:
 C112(H11D,H11E,H11F)
;
_shelx_res_checksum              15869
_shelx_fab_checksum              77017
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'