Sn20(SitBu3)10Cl2 ‒ the largest metalloid group 14 cluster shows a raspberry-like arrangement of smaller units
Schnepf, Andreas; Schrenk, Claudio; Binder, Mareike; Chemical Communications  (2019) –; doi:10.1039/C9CC07099K

data_7124214
_publ_section_title
;
 Sn20(SitBu3)10Cl2 -- the largest metalloid group 14 cluster shows a
 raspberry-like arrangement of smaller units
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC07099K
_journal_year                    2019
_chemical_formula_moiety         'C120 H270 Cl2 Si10 Sn20'
_chemical_formula_sum            'C120 H270 Cl2 Si10 Sn20'
_chemical_formula_weight         4438.94
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-08-21
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-04-23 deposited with the CCDC.    2019-09-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.820(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   19.176(4)
_cell_length_b                   23.573(5)
_cell_length_c                   20.419(4)
_cell_measurement_reflns_used    9939
_cell_measurement_temperature    150
_cell_measurement_theta_max      23.014
_cell_measurement_theta_min      2.216
_cell_volume                     9219(3)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 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    'ShelXS (Sheldrick, 2008)'
_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 0.992
_diffrn_measured_fraction_theta_max 0.992
_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_unetI/netI     0.1393
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            37661
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        24.499
_diffrn_reflns_theta_max         24.499
_diffrn_reflns_theta_min         1.494
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    2.781
_exptl_absorpt_correction_T_max  0.745372
_exptl_absorpt_correction_T_min  0.644062
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.

Final HKLF 4 output contains 127261 reflections, Rint = 0.1227
 (28182 with I > 3sig(I), Rint = 0.0615)
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.599
_exptl_crystal_description       block
_exptl_crystal_F_000             4328
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: toluene, pentane'
_exptl_crystal_size_max          0.108
_exptl_crystal_size_mid          0.091
_exptl_crystal_size_min          0.068
_refine_diff_density_max         1.949
_refine_diff_density_min         -1.306
_refine_diff_density_rms         0.264
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     731
_refine_ls_number_reflns         37661
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.1368
_refine_ls_R_factor_gt           0.0708
_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^)+(0.0730P)^2^+132.6946P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1513
_refine_ls_wR_factor_ref         0.1901
_reflns_Friedel_coverage         0.000
_reflns_number_gt                23655
_reflns_number_total             37661
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc07099k2.cif
_cod_data_source_block           Sn20R10Cl2
_cod_database_code               7124214
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.5226(10)
 0.4774(10)
2. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(C307) \\sim Ueq, Uanis(C208) \\sim Ueq, Uanis(C506) \\sim Ueq,
Uanis(C206) \\sim Ueq, Uanis(C205) \\sim Ueq: with sigma of 0.02 and sigma for
terminal atoms of 0.04
4.a Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C102(H10A,H10B,H10C), C103(H10D,H10E,H10F), C104(H10G,
 H10H,H10I), C106(H10J,H10K,H10L), C107(H10M,H10N,H10O), C108(H10P,H10Q,H10R),
 C110(H11A,H11B,H11C), C111(H11D,H11E,H11F), C112(H11G,H11H,H11I), C202(H20A,
 H20B,H20C), C203(H20D,H20E,H20F), C204(H20G,H20H,H20I), C206(H20J,H20K,H20L),
 C207(H20M,H20N,H20O), C208(H20P,H20Q,H20R), C210(H21A,H21B,H21C), C211(H21D,
 H21E,H21F), C212(H21G,H21H,H21I), C302(H30A,H30B,H30C), C303(H30D,H30E,H30F),
 C304(H30G,H30H,H30I), C306(H30J,H30K,H30L), C307(H30M,H30N,H30O), C308(H30P,
 H30Q,H30R), C310(H31A,H31B,H31C), C311(H31D,H31E,H31F), C312(H31G,H31H,H31I),
 C402(H40A,H40B,H40C), C403(H40D,H40E,H40F), C404(H40G,H40H,H40I), C406(H40J,
 H40K,H40L), C407(H40M,H40N,H40O), C408(H40P,H40Q,H40R), C410(H41A,H41B,H41C),
 C411(H41D,H41E,H41F), C412(H41G,H41H,H41I), C502(H50A,H50B,H50C), C503(H50D,
 H50E,H50F), C505(H50G,H50H,H50I), C506(H50J,H50K,H50L), C507(H50M,H50N,H50O),
 C509(H50P,H50Q,H50R), C510(H51A,H51B,H51C), C511(H51D,H51E,H51F)
;
_shelx_res_checksum              3057
_shelx_fab_checksum              85003
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'