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

data_7708430
_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         'C54 H148 K N2 Si16 Sn10, C18 H48 K N6'
_chemical_formula_sum            'C72 H196 K2 N8 Si16 Sn10'
_chemical_formula_weight         2888.90
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-01-27
_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                 92.523(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.108(3)
_cell_length_b                   30.136(4)
_cell_length_c                   23.877(3)
_cell_measurement_reflns_used    9283
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.395
_cell_measurement_theta_min      2.193
_cell_volume                     13017(3)
_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      100.0
_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 0.999
_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  0.0898
_diffrn_reflns_av_unetI/netI     0.0359
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            346768
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         2.114
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    2.128
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5505
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1406 before and 0.0735 after correction. The Ratio of minimum to maximum transmission is 0.7378. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.474
_exptl_crystal_description       plank
_exptl_crystal_F_000             5784
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: pentane'
_exptl_crystal_size_max          0.483
_exptl_crystal_size_mid          0.088
_exptl_crystal_size_min          0.052
_refine_diff_density_max         1.682
_refine_diff_density_min         -0.853
_refine_diff_density_rms         0.149
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.176
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1219
_refine_ls_number_reflns         25575
_refine_ls_number_restraints     408
_refine_ls_restrained_S_all      1.173
_refine_ls_R_factor_all          0.0733
_refine_ls_R_factor_gt           0.0477
_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^)+(0.0331P)^2^+100.9207P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1048
_refine_ls_wR_factor_ref         0.1291
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19611
_reflns_number_total             25575
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02591k2.cif
_cod_data_source_block           4_sq
_cod_original_cell_volume        13018(3)
_cod_database_code               7708430
_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
 Si74-C741 = Si74-C742 = Si74-C746
 1.98 with sigma of 0.02
 Si74-C743 = Si74-C744 = Si74-C745
 2.84 with sigma of 0.02
 C742-C743 = C742-C744 = C742-C745
 1.54 with sigma of 0.02
 C734-C733 \\sim C733-C735 \\sim C736-C733
 with sigma of 0.02
 C644-C643 \\sim C645-C643 \\sim C633-C636 \\sim C633-C635 \\sim C634-C633
 with sigma of 0.02
 N806-C809 \\sim N806-C805
 with sigma of 0.02
 N802-C801 \\sim N802-C811
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C634 \\sim C635 \\sim C636 \\sim C644 \\sim C645 \\sim C646: within 5A with
sigma of 0.01 and sigma for terminal atoms of 0.02
Si73 \\sim Si75: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
Si72 \\sim Si74: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
C722 \\sim C741: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
C732 \\sim C752: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
Si63 \\sim Si64: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
C912 \\sim C917: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
C913 \\sim C918: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
C916 \\sim C919: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
C915 \\sim C920: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
C804 \\sim C805 \\sim C809 \\sim C810: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
C801 \\sim C811: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
C925 \\sim C928: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
Uanis(C114) \\sim Ueq, Uanis(C116) \\sim Ueq, Uanis(C115) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C643) \\sim Ueq, Uanis(C633) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C632) \\sim Ueq, Uanis(C642) \\sim Ueq, Uanis(C631) \\sim Ueq,
Uanis(C641) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C721) \\sim Ueq, Uanis(C743) \\sim Ueq, Uanis(C742) \\sim Ueq,
Uanis(C744) \\sim Ueq, Uanis(C745) \\sim Ueq, Uanis(C732) \\sim Ueq,
Uanis(C752) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C746) \\sim Ueq, Uanis(C723) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C732) \\sim Ueq, Uanis(C751) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(Si64) \\sim Ueq, Uanis(Si63) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C927) \\sim Ueq, Uanis(C930) \\sim Ueq, Uanis(C926) \\sim Ueq,
Uanis(C929) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C912) \\sim Ueq, Uanis(C917) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C913) \\sim Ueq, Uanis(C918) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C928) \\sim Ueq, Uanis(C925) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(N931) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(Si64)=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(C809)=Sof(H80Q)=Sof(H80R)=Sof(C810)=Sof(H81A)=Sof(H81B)=
 Sof(C811)=Sof(H81E)=Sof(H81C)=Sof(H81D)=1-FVAR(1)
 Sof(Si63)=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)=Sof(C801)=Sof(H80A)=Sof(H80B)=Sof(H80C)=Sof(C804)=Sof(H80G)=
 Sof(H80H)=Sof(C805)=Sof(H80I)=Sof(H80J)=FVAR(1)
 Sof(Si74)=Sof(Si75)=Sof(H73D)=Sof(H73E)=Sof(H73F)=Sof(C741)=Sof(H74D)=
 Sof(H74E)=Sof(H74F)=Sof(C742)=Sof(C743)=Sof(H74G)=Sof(H74H)=Sof(H74I)=
 Sof(C744)=Sof(H74J)=Sof(H74K)=Sof(H74L)=Sof(C745)=Sof(H74M)=Sof(H74N)=
 Sof(H74O)=Sof(C746)=Sof(H74A)=Sof(H74B)=Sof(H74C)=Sof(C751)=Sof(H75A)=
 Sof(H75B)=Sof(H75C)=Sof(C752)=Sof(H75D)=Sof(H75E)=Sof(H75F)=1-FVAR(2)
 Sof(Si72)=Sof(Si73)=Sof(C721)=Sof(H72A)=Sof(H72B)=Sof(H72C)=Sof(C722)=
 Sof(H72D)=Sof(H72E)=Sof(H72F)=Sof(C723)=Sof(H72G)=Sof(H72H)=Sof(H72I)=
 Sof(H73A)=Sof(H73B)=Sof(H73C)=Sof(C732)=Sof(H73G)=Sof(H73H)=Sof(H73I)=
 Sof(C733)=Sof(C734)=Sof(H73J)=Sof(H73K)=Sof(H73L)=Sof(C735)=Sof(H73M)=
 Sof(H73N)=Sof(H73O)=Sof(C736)=Sof(H73P)=Sof(H73Q)=Sof(H73R)=FVAR(2)
 Sof(C917)=Sof(H91N)=Sof(H91O)=Sof(C918)=Sof(H91P)=Sof(H91Q)=Sof(C919)=
 Sof(H91R)=Sof(H91S)=Sof(H91T)=Sof(C920)=Sof(H92A)=Sof(H92B)=Sof(H92C)=
 Sof(H92J)=Sof(H92K)=Sof(C925)=Sof(H92N)=Sof(H92O)=Sof(C926)=Sof(H92P)=
 Sof(H92Q)=Sof(H92R)=Sof(C927)=Sof(H92S)=Sof(H92T)=Sof(H92U)=1-FVAR(3)
 Sof(C912)=Sof(H91D)=Sof(H91E)=Sof(C913)=Sof(H91F)=Sof(H91G)=Sof(C915)=
 Sof(H91H)=Sof(H91I)=Sof(H91J)=Sof(C916)=Sof(H91K)=Sof(H91L)=Sof(H91M)=
 Sof(H92L)=Sof(H92M)=Sof(C928)=Sof(H92V)=Sof(H92W)=Sof(C929)=Sof(H)=Sof(H92X)=
 Sof(H92Y)=Sof(C930)=Sof(H93A)=Sof(H93B)=Sof(H93C)=FVAR(3)
5.a Secondary CH2 refined with riding coordinates:
 C804(H80G,H80H), C805(H80I,H80J), C809(H80Q,H80R), C810(H81A,H81B), C904(H90G,
 H90H), C905(H90I,H90J), C912(H91D,H91E), C913(H91F,H91G), C917(H91N,H91O),
 C918(H91P,H91Q), C924(H92J,H92K), C924(H92L,H92M), C925(H92N,H92O), C928(H92V,
 H92W)
5.b Me refined with riding coordinates:
 C111(H11A,H11B,H11C), C112(H11D,H11E,H11F), C114(H11G,H11H,H11I), C115(H11J,
 H11K,H11L), C116(H11M,H11N,H11O), C121(H12C,H12A,H12B), C122(H12D,H12E,H12F),
 C123(H12G,H12H,H12I), C131(H13A,H13B,H13C), C132(H13D,H13E,H13F), C133(H13G,
 H13H,H13I), C511(H51A,H51B,H51C), C512(H51D,H51E,H51F), C513(H51G,H51H,H51I),
 C521(H52A,H52B,H52C), C522(H52D,H52E,H52F), C523(H52G,H52H,H52I), C531(H53A,
 H53B,H53C), C532(H53D,H53E,H53F), C534(H53G,H53H,H53I), C535(H53J,H53K,H53L),
 C536(H53M,H53N,H53O), 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), 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(H73A,H73B,H73C), C731(H73D,
 H73E,H73F), C732(H73G,H73H,H73I), C734(H73J,H73K,H73L), C735(H73M,H73N,H73O),
 C736(H73P,H73Q,H73R), C741(H74D,H74E,H74F), C743(H74G,H74H,H74I), C744(H74J,
 H74K,H74L), C745(H74M,H74N,H74O), C746(H74A,H74B,H74C), C751(H75A,H75B,H75C),
 C752(H75D,H75E,H75F), C801(H80A,H80B,H80C), C803(H80D,H80E,H80F), C807(H80K,
 H80L,H80M), C808(H80N,H80O,H80P), C811(H81E,H81C,H81D), C901(H90A,H90B,H90C),
 C902(H90D,H90E,H90F), C907(H90K,H90L,H90M), C908(H90N,H90O,H90P), C909(H90Q,
 H90R,H90S), C910(H91A,H91B,H91C), C915(H91H,H91I,H91J), C916(H91K,H91L,H91M),
 C919(H91R,H91S,H91T), C920(H92A,H92B,H92C), C921(H92D,H92E,H92F), C922(H92G,
 H92H,H92I), C926(H92P,H92Q,H92R), C927(H92S,H92T,H92U), C929(H,H92X,H92Y),
 C930(H93A,H93B,H93C)
;
_shelx_res_checksum              65760
_shelx_fab_checksum              19814
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'