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_4085996
_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, 6(C H2 Cl2)'
_chemical_formula_sum            'C78 H96 Cl12 N8 S10 Sn6'
_chemical_formula_weight         2603.76
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-01-07
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.06 svn.r3119 for OlexSys, GUI svn.r4979)
;
_cell_angle_alpha                90
_cell_angle_beta                 121.84
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   32.9747(15)
_cell_length_b                   11.4272(5)
_cell_length_c                   31.2524(13)
_cell_measurement_temperature    100
_cell_volume                     10004.1(8)
_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      100.0
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Bruker D8Quest'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0910
_diffrn_reflns_av_unetI/netI     0.0988
_diffrn_reflns_laue_measured_fraction_full 0.978
_diffrn_reflns_laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            47461
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.209
_exptl_absorpt_coefficient_mu    2.048
_exptl_absorpt_correction_T_max  0.78
_exptl_absorpt_correction_T_min  0.70
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   multi-scan
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.729
_exptl_crystal_description       needle
_exptl_crystal_F_000             5136
_exptl_crystal_preparation       'in DCM'
_exptl_crystal_recrystallization_method 'layering with Et2O'
_exptl_crystal_size_max          0.179
_exptl_crystal_size_mid          0.095
_exptl_crystal_size_min          0.078
_refine_diff_density_max         2.159
_refine_diff_density_min         -1.527
_refine_diff_density_rms         0.200
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     522
_refine_ls_number_reflns         9976
_refine_ls_number_restraints     157
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.1181
_refine_ls_R_factor_gt           0.0616
_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^)+(0.0623P)^2^+153.5827P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1287
_refine_ls_wR_factor_ref         0.1530
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6529
_reflns_number_total             9976
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00295_si_003.cif
_cod_data_source_block           Compound7
_cod_depositor_comments
'Adding full bibliography for 4085995--4085998.cif.'
_cod_database_code               4085996
_shelxl_version_number           2013-3
_shelx_estimated_absorpt_t_max   0.857
_shelx_estimated_absorpt_t_min   0.711
_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. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C22(H22A,H22B), C37(H37A,H37B), C39(H39A,H39B), C38(H38A,H38B)
3.b Aromatic/amide H refined with riding coordinates:
 C32(H32), C17(H17), C30(H30), C33(H33), C29(H29), C28(H28), C12(H12),
 C34(H34), C11(H11), C10(H10), C35(H35), C16(H16), C15(H15), C14(H14)
3.c Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C6(H6A,H6B,H6C), C21(H21A,H21B,H21C), C24(H24A,H24B,
 H24C), C8(H8A,H8B,H8C), C3(H3A,H3B,H3C), C2(H2A,H2B,H2C), C26(H26A,H26B,H26C)
;
_shelx_res_checksum              82657
_shelx_hkl_checksum              59377
_olex2_submission_original_sample_id FSD1-Acetonaphthon
_olex2_submission_special_instructions 'No special instructions were received'