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_4085998
_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         'C72 H84 N8 S10 Sn6, C H2 Cl2'
_chemical_formula_sum            'C73 H86 Cl2 N8 S10 Sn6'
_chemical_formula_weight         2179.13
_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                114.43(3)
_cell_angle_beta                 105.70(3)
_cell_angle_gamma                93.95(3)
_cell_formula_units_Z            1
_cell_length_a                   10.859(2)
_cell_length_b                   14.864(3)
_cell_length_c                   16.490(3)
_cell_measurement_temperature    100
_cell_volume                     2282.7(11)
_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
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  IPDS-2T
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0539
_diffrn_reflns_av_unetI/netI     0.0457
_diffrn_reflns_laue_measured_fraction_full 0.999
_diffrn_reflns_laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            21393
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.742
_diffrn_reflns_theta_min         1.436
_exptl_absorpt_coefficient_mu    1.944
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.585
_exptl_crystal_description       plate
_exptl_crystal_F_000             1074
_exptl_crystal_preparation       DCM
_exptl_crystal_recrystallization_method 'layering with toluene'
_exptl_crystal_size_max          0.314
_exptl_crystal_size_mid          0.097
_exptl_crystal_size_min          0.07
_refine_diff_density_max         2.555
_refine_diff_density_min         -1.590
_refine_diff_density_rms         0.157
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     495
_refine_ls_number_reflns         9648
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0491
_refine_ls_R_factor_gt           0.0376
_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^)+(0.0725P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1036
_refine_ls_wR_factor_ref         0.1090
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7837
_reflns_number_total             9648
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00295_si_004.cif
_cod_data_source_block           Compound8
_cod_depositor_comments
'Adding full bibliography for 4085995--4085998.cif.'
_cod_original_cell_volume        2282.7(10)
_cod_database_code               4085998
_shelxl_version_number           2013-3
_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
 Cl4-C38 = Cl3-C38 = Cl1-C37 = Cl2-C37
 1.74 with sigma of 0.02
3. Others
 Fixed Sof: Cl3(0.25) Cl4(0.25) C38(0.25) H38A(0.25) H38B(0.25) Cl1(0.25)
 C37(0.25) H37A(0.25) H37B(0.25) Cl2(0.25)
4.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C22(H22A,H22B), C38(H38A,H38B), C37(H37A,H37B)
4.b Aromatic/amide H refined with riding coordinates:
 C36(H36), C14(H14), C28(H28), C10(H10), C11(H11), C32(H32), C35(H35),
 C29(H29), C34(H34), C18(H18), C33(H33), C16(H16), C15(H15), C17(H17)
4.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C26(H26A,H26B,H26C), C2(H2A,H2B,H2C), C21(H21A,H21B,H21C),
 C6(H6A,H6B,H6C), C20(H20A,H20B,H20C), C24(H24A,H24B,H24C), C3(H3A,H3B,H3C)
;
_shelx_res_checksum              43807
_shelx_hkl_checksum              7181
_olex2_submission_original_sample_id FSD2Acetonaphthon
_olex2_submission_special_instructions 'No special instructions were received'