Selective and Benign Alkylation of Sulfido-Oxo Stannate Clusters with Propyl, Pentyl, or Hexyl Substituents
Stuhrmann, Gina; Schneider, Jannik; Schmidt, Kilian; Dehnen, Stefanie Susanne; Chemical Communications  (2023) –; doi:10.1039/D3CC03525E

data_7132202
_publ_section_title
;
 Selective and Benign Alkylation of Sulfido-Oxo Stannate Clusters with
 Propyl, Pentyl, or Hexyl Substituents
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D3CC03525E
_journal_year                    2023
_chemical_formula_moiety         'C12 H28 O4 S20 Sn10, 4(C9 H16 N2), 4[C5H12]'
_chemical_formula_sum            'C48 H88 N8 O4 S20 Sn10'
_chemical_formula_weight         2669.36
_space_group_crystal_system      tetragonal
_space_group_IT_number           122
_space_group_name_Hall           'I -4 2bw'
_space_group_name_H-M_alt        'I -4 2 d'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-08-29
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2023-10-05 deposited with the CCDC.	2023-10-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.9274(11)
_cell_length_b                   19.9274(11)
_cell_length_c                   26.2914(18)
_cell_measurement_reflns_used    13280
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.03
_cell_measurement_theta_min      2.76
_cell_volume                     10440.3(11)
_computing_cell_refinement       'X-Area Recipe 1.33.0.0 (STOE, 2015)'
_computing_data_collection       'X-Area Pilatus3_SV 1.31.139.0 (STOE, 2018)'
_computing_data_reduction
;
X-Area Integrate 1.77.0.0 (STOE, 2019)
X-Area LANA 1.77.1.0 (STOE, 2019)
;
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.00
_diffrn_detector                 Pilatus300K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'DECTRIS PILATUS 300K'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details      '4391 frames, detector distance = 60 mm'
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_R_equivalents  0.0673
_diffrn_reflns_av_unetI/netI     0.0353
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            102797
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         76.248
_diffrn_reflns_theta_min         2.782
_diffrn_source                   'GeniX 3D HF Cu'
_diffrn_source_target            Mo
_exptl_absorpt_coefficient_mu    22.696
_exptl_absorpt_correction_T_max  0.9903
_exptl_absorpt_correction_T_min  0.4254
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE LANA, absorption correction by scaling of reflection intensities.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(\m~2~-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
Afterwards a spherical absorption correction was performed within STOE LANA.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.698
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plates
_exptl_crystal_F_000             5136
_exptl_crystal_size_max          0.092
_exptl_crystal_size_mid          0.067
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.510
_refine_diff_density_min         -0.949
_refine_diff_density_rms         0.116
_refine_ls_abs_structure_details
;
 Flack x determined using 1820 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.031(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.936
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     210
_refine_ls_number_reflns         5441
_refine_ls_number_restraints     49
_refine_ls_restrained_S_all      0.944
_refine_ls_R_factor_all          0.0442
_refine_ls_R_factor_gt           0.0371
_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^)+(0.0608P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0922
_refine_ls_wR_factor_ref         0.0944
_reflns_Friedel_coverage         0.844
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.990
_reflns_number_gt                4501
_reflns_number_total             5441
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc03525e2.cif
_cod_data_source_block           gs133i50b
_cod_original_cell_volume        10440.3(14)
_cod_database_code               7132202
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.660
_shelx_estimated_absorpt_t_min   0.229
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, H4 of C4, H5 of C5
 At 1.5 times of:
  All C(H,H,H) groups, H12 of C12
2. Restrained distances
 C12-H12 \\sim C11-H11A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C5) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C4) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C8) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C9) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C12) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C2) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(N2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C3) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
4.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C8(H8A,H8B), C9(H9A,H9B), C11(H11A,H11B)
4.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5)
4.c Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C7(H7A,H7B,H7C), C10(H10A,H10B,H10C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 692 electrons were 
found in a volume of 2324\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
1 [pentane] per Asymmetric Unit 
which account for 640 electrons 
per unit cell.
;
_shelx_res_checksum              87431
_shelx_hkl_checksum              63616
_shelx_fab_checksum              76874
_olex2_submission_special_instructions 'No special instructions were received'