Functionalization of Sn/S Clusters with Hetero- and Polyaromatics
Leusmann, Eliza; Schneck, Felix; Dehnen, Stefanie; Organometallics 34 (2015) 3264–; doi:10.1021/acs.organomet.5b00295

data_4085995
_publ_section_title
;
 Functionalization of Sn/S Clusters with Hetero- and Polyaromatics
;
_journal_issue                   13
_journal_name_full               Organometallics
_journal_page_first              3264
_journal_paper_doi               10.1021/acs.organomet.5b00295
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C52 H68 N8 S10 Sn6'
_chemical_formula_sum            'C52 H68 N8 S10 Sn6'
_chemical_formula_weight         1837.88
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-01-08
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.06 svn.r3119 for OlexSys, GUI svn.r4979)
;
_cell_angle_alpha                100.816(2)
_cell_angle_beta                 110.245(2)
_cell_angle_gamma                91.817(2)
_cell_formula_units_Z            1
_cell_length_a                   10.7206(5)
_cell_length_b                   12.9145(6)
_cell_length_c                   13.9280(7)
_cell_measurement_temperature    100
_cell_volume                     1767.28(15)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.01
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker D8Quest'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0718
_diffrn_reflns_av_unetI/netI     0.0863
_diffrn_reflns_laue_measured_fraction_full 0.999
_diffrn_reflns_laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            25120
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.319
_diffrn_reflns_theta_min         2.015
_exptl_absorpt_coefficient_mu    2.421
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   none
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.727
_exptl_crystal_description       bar
_exptl_crystal_F_000             896
_exptl_crystal_preparation       'in DCM'
_exptl_crystal_recrystallization_method 'layering with n-hexane'
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.044
_exptl_crystal_size_min          0.032
_refine_diff_density_max         3.077
_refine_diff_density_min         -1.015
_refine_diff_density_rms         0.332
_refine_ls_extinction_coef       0.0045(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     314
_refine_ls_number_reflns         8717
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.1038
_refine_ls_R_factor_gt           0.0573
_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^)+(0.0743P)^2^+5.1867P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1368
_refine_ls_wR_factor_ref         0.1570
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5919
_reflns_number_total             8717
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00295_si_002.cif
_cod_data_source_block           Compound6
_cod_depositor_comments
'Adding full bibliography for 4085995--4085998.cif.'
_cod_database_code               4085995
_shelxl_version_number           2013-3
_shelx_estimated_absorpt_t_max   0.927
_shelx_estimated_absorpt_t_min   0.698
_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
 C22B-C21B = C23B-C24B = C25B-C26B
 1.4 with sigma of 0.02
 C26B-C21B
 1.4 with sigma of 0.02
 C22A-C23A
 1.4 with sigma of 0.02
3. Others
 Fixed Sof: N3A(0.5) C17A(0.5) H17A(0.5) H17B(0.5) C18A(0.5) C14A(0.5)
 C19A(0.5) H19A(0.5) H19B(0.5) H19C(0.5) N4A(0.5) C16A(0.5) H16A(0.5) H16B(0.5)
 H16C(0.5) C16B(0.5) H16D(0.5) H16E(0.5) H16F(0.5) C22B(0.5) H22B(0.5)
 C21B(0.5) C26B(0.5) H26B(0.5) C25B(0.5) H25B(0.5) C24B(0.5) H24B(0.5)
 C23B(0.5) H23B(0.5) C18B(0.5) C14B(0.5) N4B(0.5) C15B(0.5) H15A(0.5) H15B(0.5)
 H15C(0.5) C19B(0.5) H19D(0.5) H19E(0.5) H19F(0.5) N3B(0.5) C15A(0.5) H15D(0.5)
 H15E(0.5) H15F(0.5) C20A(0.5) H20A(0.5) C23A(0.5) H23A(0.5) C22A(0.5)
 H22A(0.5) C21A(0.5) C26A(0.5) H26A(0.5) C25A(0.5) H25A(0.5) C24A(0.5)
 H24A(0.5) C20B(0.5) H20B(0.5) C17B(0.5) H17C(0.5) H17D(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C17A(H17A,H17B), C4(H4A,H4B), C17B(H17C,H17D)
4.b Aromatic/amide H refined with riding coordinates:
 C13(H13), C12(H12), C7(H7), C11(H11), C9(H9), C10(H10), C22B(H22B),
 C26B(H26B), C25B(H25B), C24B(H24B), C23B(H23B), C20A(H20A), C23A(H23A),
 C22A(H22A), C26A(H26A), C25A(H25A), C24A(H24A), C20B(H20B)
4.c Fitted hexagon refined as free rotating group:
 C22B(C21B,C26B,C25B,C24B,C23B), C23A(C22A,C21A,C26A,C25A,C24A)
4.d Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C6(H6A,H6B,H6C), C19A(H19A,H19B,H19C),
 C16A(H16A,H16B,H16C), C16B(H16D,H16E,H16F), C15B(H15A,H15B,H15C), C19B(H19D,
 H19E,H19F), C15A(H15D,H15E,H15F)
;
_shelx_res_checksum              53508
_shelx_hkl_checksum              76734
_olex2_submission_original_sample_id Compound6-Benzaldehyde
_olex2_submission_special_instructions 'No special instructions were received'