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_4085997
_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         'C64 H72 N12 S10 Sn6, 2(C H2 Cl2)'
_chemical_formula_sum            'C66 H76 Cl4 N12 S10 Sn6'
_chemical_formula_weight         2211.92
_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
_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                83.918(2)
_cell_angle_beta                 86.837(2)
_cell_angle_gamma                83.666(2)
_cell_formula_units_Z            1
_cell_length_a                   10.7352(6)
_cell_length_b                   10.8246(6)
_cell_length_c                   17.6041(10)
_cell_measurement_temperature    100(2)
_cell_volume                     2019.8(2)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0831
_diffrn_reflns_av_unetI/netI     0.0719
_diffrn_reflns_laue_measured_fraction_full 0.998
_diffrn_reflns_laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            36863
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.191
_diffrn_reflns_theta_min         2.128
_exptl_absorpt_coefficient_mu    2.264
_exptl_absorpt_correction_T_max  0.97
_exptl_absorpt_correction_T_min  0.84
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_crystal_density_diffrn    1.819
_exptl_crystal_F_000             1084
_exptl_crystal_size_max          0.196
_exptl_crystal_size_mid          0.128
_exptl_crystal_size_min          0.015
_refine_diff_density_max         1.292
_refine_diff_density_min         -0.840
_refine_diff_density_rms         0.168
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     448
_refine_ls_number_reflns         8950
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0734
_refine_ls_R_factor_gt           0.0361
_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^)+(0.0088P)^2^+7.6271P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0559
_refine_ls_wR_factor_ref         0.0702
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6409
_reflns_number_total             8950
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00295_si_005.cif
_cod_data_source_block           compound10
_cod_depositor_comments
'Adding full bibliography for 4085995--4085998.cif.'
_cod_database_code               4085997
_shelxl_version_number           2013-3
_shelx_estimated_absorpt_t_max   0.967
_shelx_estimated_absorpt_t_min   0.665
_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.a Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C4(H4A,H4B), C33(H33A,H33B)
2.b Aromatic/amide H refined with riding coordinates:
 C23(H23), C32(H32), C31(H31), C25(H25), C27(H27), C28(H28), C29(H29), C7(H7),
 C9(H9), C11(H11), C15(H15), C16(H16), C12(H12), C13(H13)
2.c Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C22(H22A,H22B,H22C), C19(H19A,H19B,H19C), C2(H2A,H2B,
 H2C), C3(H3A,H3B,H3C), C6(H6A,H6B,H6C)
;
_shelx_res_checksum              72496
_shelx_hkl_checksum              56301
_olex2_submission_special_instructions 'No special instructions were received'