#------------------------------------------------------------------------------
#$Date: 2016-03-21 14:53:35 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178728 $
#$URL: svn://www.crystallography.net/cod/cif/4/08/39/4083970.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4083970
loop_
_publ_author_name
'Henning, Jens'
'Eichele, Klaus'
'Fink, Reinhold F.'
'Wesemann, Lars'
_publ_section_title
;
 Structural and Spectroscopic Characterization of Tin--Tin Double Bonds in
 Cyclic Distannenes
;
_journal_issue                   14
_journal_name_full               Organometallics
_journal_page_first              3904
_journal_paper_doi               10.1021/om500645b
_journal_volume                  33
_journal_year                    2014
_chemical_formula_sum            'C58 H56 Sn2'
_chemical_formula_weight         990.41
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.366(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.4863(5)
_cell_length_b                   29.3901(10)
_cell_length_c                   11.3016(4)
_cell_measurement_reflns_used    389
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      31.0895
_cell_measurement_theta_min      12.6738
_cell_volume                     4797.7(3)
_computing_cell_refinement       'APEX2 v2011.8--0 (Bruker AXS)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT V7.68A (Bruker AXS, 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD Duo'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  'Bruker Triump'
_diffrn_radiation_source         microsource
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0326
_diffrn_reflns_av_sigmaI/netI    0.0073
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            180922
_diffrn_reflns_theta_full        27.55
_diffrn_reflns_theta_max         27.55
_diffrn_reflns_theta_min         1.57
_exptl_absorpt_coefficient_mu    1.077
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.93
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.371
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2016
_exptl_crystal_size_max          0.225
_exptl_crystal_size_mid          0.146
_exptl_crystal_size_min          0.036
_refine_diff_density_max         0.534
_refine_diff_density_min         -0.392
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.159
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     278
_refine_ls_number_reflns         5555
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.159
_refine_ls_R_factor_all          0.0243
_refine_ls_R_factor_gt           0.0217
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0216P)²+8.7538P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0546
_refine_ls_wR_factor_ref         0.0574
_reflns_number_gt                5217
_reflns_number_total             5555
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om500645b_si_002.cif
_cod_data_source_block           distannene3
_cod_depositor_comments
'Adding full bibliography for 4083969--4083976.cif.'
_cod_database_code               4083970
#BEGIN Tags that were not found in dictionaries:
_computing_bruker_data_scaling   'SADABS V2008/1 (Bruker AXS)'
#END Tags that were not found in dictionaries
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Sn1 Sn 0.093024(8) 0.142103(4) 0.780313(10) 0.02220(5) Uani 1 1 d .
C1 C 0.08166(11) 0.21586(6) 0.79873(14) 0.0202(3) Uani 1 1 d .
C2 C 0.15671(12) 0.24120(6) 0.84301(16) 0.0252(4) Uani 1 1 d .
H2 H 0.2106 0.2258 0.8749 0.030 Uiso 1 1 calc R
C3 C 0.15633(13) 0.28924(7) 0.84267(18) 0.0297(4) Uani 1 1 d .
H3 H 0.2091 0.3057 0.8741 0.036 Uiso 1 1 calc R
C4 C 0.07954(13) 0.31189(6) 0.79676(17) 0.0282(4) Uani 1 1 d .
H4 H 0.0793 0.3442 0.7961 0.034 Uiso 1 1 calc R
C5 C 0.0000 0.28784(8) 0.7500 0.0231(5) Uani 1 2 d S
C6 C 0.0000 0.23915(8) 0.7500 0.0187(4) Uani 1 2 d S
C7 C 0.15579(11) 0.11958(5) 0.95153(15) 0.0196(3) Uani 1 1 d .
C8 C 0.11137(12) 0.12475(5) 1.05712(15) 0.0205(3) Uani 1 1 d .
C9 C 0.15816(13) 0.11289(6) 1.16559(16) 0.0252(4) Uani 1 1 d .
H9 H 0.1288 0.1167 1.2373 0.030 Uiso 1 1 calc R
C10 C 0.24758(14) 0.09554(6) 1.16874(17) 0.0288(4) Uani 1 1 d .
H10 H 0.2800 0.0887 1.2429 0.035 Uiso 1 1 calc R
C11 C 0.28975(13) 0.08812(6) 1.06452(18) 0.0268(4) Uani 1 1 d .
H11 H 0.3500 0.0753 1.0675 0.032 Uiso 1 1 calc R
C12 C 0.24402(12) 0.09947(6) 0.95469(16) 0.0223(3) Uani 1 1 d .
C13 C 0.01244(12) 0.14001(6) 1.05383(15) 0.0206(3) Uani 1 1 d .
C14 C -0.01058(13) 0.18560(6) 1.07358(15) 0.0237(3) Uani 1 1 d .
C15 C -0.10346(14) 0.19844(6) 1.06398(17) 0.0281(4) Uani 1 1 d .
H15 H -0.1188 0.2294 1.0764 0.034 Uiso 1 1 calc R
C16 C -0.17430(13) 0.16747(7) 1.03689(16) 0.0276(4) Uani 1 1 d .
C17 C -0.15036(13) 0.12203(6) 1.02029(16) 0.0260(4) Uani 1 1 d .
H17 H -0.1980 0.1003 1.0028 0.031 Uiso 1 1 calc R
C18 C -0.05848(13) 0.10782(6) 1.02879(15) 0.0233(3) Uani 1 1 d .
C19 C 0.06281(14) 0.22072(6) 1.10710(18) 0.0301(4) Uani 1 1 d .
H19A H 0.1184 0.2140 1.0660 0.045 Uiso 1 1 calc R
H19B H 0.0781 0.2199 1.1931 0.045 Uiso 1 1 calc R
H19C H 0.0396 0.2510 1.0840 0.045 Uiso 1 1 calc R
C20 C -0.27420(15) 0.18253(8) 1.0252(2) 0.0400(5) Uani 1 1 d .
H20A H -0.2916 0.1910 0.9426 0.060 Uiso 1 1 calc R
H20B H -0.2821 0.2088 1.0768 0.060 Uiso 1 1 calc R
H20C H -0.3138 0.1575 1.0485 0.060 Uiso 1 1 calc R
C21 C -0.03630(14) 0.05851(6) 1.00702(19) 0.0303(4) Uani 1 1 d .
H21A H -0.0940 0.0415 0.9902 0.045 Uiso 1 1 calc R
H21B H -0.0022 0.0458 1.0776 0.045 Uiso 1 1 calc R
H21C H 0.0017 0.0562 0.9391 0.045 Uiso 1 1 calc R
C22 C 0.28624(12) 0.08778(6) 0.84179(17) 0.0232(3) Uani 1 1 d .
C23 C 0.35110(12) 0.11647(6) 0.79316(18) 0.0277(4) Uani 1 1 d .
C24 C 0.38859(13) 0.10396(7) 0.68818(19) 0.0302(4) Uani 1 1 d .
H24 H 0.4320 0.1236 0.6555 0.036 Uiso 1 1 calc R
C25 C 0.36457(13) 0.06365(7) 0.62968(19) 0.0307(4) Uani 1 1 d .
C26 C 0.29989(13) 0.03570(6) 0.67821(19) 0.0302(4) Uani 1 1 d .
H26 H 0.2823 0.0081 0.6391 0.036 Uiso 1 1 calc R
C27 C 0.26008(13) 0.04710(6) 0.78272(18) 0.0267(4) Uani 1 1 d .
C28 C 0.38076(14) 0.16058(7) 0.8536(2) 0.0369(5) Uani 1 1 d .
H28A H 0.4172 0.1785 0.8008 0.055 Uiso 1 1 calc R
H28B H 0.4185 0.1539 0.9273 0.055 Uiso 1 1 calc R
H28C H 0.3258 0.1779 0.8720 0.055 Uiso 1 1 calc R
C29 C 0.40749(17) 0.05102(9) 0.5165(2) 0.0445(5) Uani 1 1 d .
H29A H 0.3800 0.0226 0.4851 0.067 Uiso 1 1 calc R
H29B H 0.4744 0.0469 0.5330 0.067 Uiso 1 1 calc R
H29C H 0.3960 0.0753 0.4578 0.067 Uiso 1 1 calc R
C30 C 0.18886(15) 0.01591(6) 0.8307(2) 0.0345(4) Uani 1 1 d .
H30A H 0.1279 0.0305 0.8222 0.052 Uiso 1 1 calc R
H30B H 0.2058 0.0097 0.9147 0.052 Uiso 1 1 calc R
H30C H 0.1867 -0.0127 0.7862 0.052 Uiso 1 1 calc R
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
C7 Sn1 C1 104.26(6) . .
C7 Sn1 Sn1 124.09(4) . 2_556
C1 Sn1 Sn1 86.78(4) . 2_556
C2 C1 C6 118.92(16) . .
C2 C1 Sn1 120.47(13) . .
C6 C1 Sn1 120.07(13) . .
C1 C2 C3 122.41(17) . .
C4 C3 C2 119.45(17) . .
C3 C4 C5 120.93(18) . .
C4 C5 C4 120.3(2) . 2_556
C4 C5 C6 119.87(12) . .
C4 C5 C6 119.87(12) 2_556 .
C5 C6 C1 118.40(11) . 2_556
C5 C6 C1 118.40(11) . .
C1 C6 C1 123.2(2) 2_556 .
C12 C7 C8 119.84(15) . .
C12 C7 Sn1 117.88(12) . .
C8 C7 Sn1 122.28(12) . .
C9 C8 C7 119.61(16) . .
C9 C8 C13 119.65(16) . .
C7 C8 C13 120.62(15) . .
C10 C9 C8 120.15(17) . .
C11 C10 C9 120.44(17) . .
C10 C11 C12 120.41(17) . .
C11 C12 C7 119.33(17) . .
C11 C12 C22 120.26(16) . .
C7 C12 C22 120.31(15) . .
C14 C13 C18 119.65(16) . .
C14 C13 C8 121.34(15) . .
C18 C13 C8 119.01(15) . .
C15 C14 C13 119.08(17) . .
C15 C14 C19 119.47(16) . .
C13 C14 C19 121.45(17) . .
C16 C15 C14 122.19(17) . .
C15 C16 C17 118.02(17) . .
C15 C16 C20 120.99(18) . .
C17 C16 C20 121.00(18) . .
C18 C17 C16 121.60(17) . .
C17 C18 C13 119.42(16) . .
C17 C18 C21 119.45(16) . .
C13 C18 C21 121.10(16) . .
C23 C22 C27 119.22(17) . .
C23 C22 C12 121.64(16) . .
C27 C22 C12 119.13(16) . .
C24 C23 C22 119.41(17) . .
C24 C23 C28 119.72(17) . .
C22 C23 C28 120.86(18) . .
C25 C24 C23 122.11(18) . .
C24 C25 C26 117.95(18) . .
C24 C25 C29 120.58(19) . .
C26 C25 C29 121.48(19) . .
C25 C26 C27 121.80(18) . .
C26 C27 C22 119.49(17) . .
C26 C27 C30 119.72(17) . .
C22 C27 C30 120.78(17) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Sn1 C7 2.1775(16) .
Sn1 C1 2.1850(17) .
Sn1 Sn1 2.7299(3) 2_556
C1 C2 1.380(2) .
C1 C6 1.4396(19) .
C2 C3 1.412(3) .
C3 C4 1.364(3) .
C4 C5 1.419(2) .
C5 C4 1.419(2) 2_556
C5 C6 1.431(3) .
C6 C1 1.4396(19) 2_556
C7 C12 1.406(2) .
C7 C8 1.406(2) .
C8 C9 1.399(2) .
C8 C13 1.499(2) .
C9 C10 1.390(3) .
C10 C11 1.385(3) .
C11 C12 1.402(2) .
C12 C22 1.496(3) .
C13 C14 1.403(2) .
C13 C18 1.409(2) .
C14 C15 1.394(3) .
C14 C19 1.509(3) .
C15 C16 1.388(3) .
C16 C17 1.396(3) .
C16 C20 1.509(3) .
C17 C18 1.391(3) .
C18 C21 1.509(2) .
C22 C23 1.405(3) .
C22 C27 1.407(2) .
C23 C24 1.391(3) .
C23 C28 1.513(3) .
C24 C25 1.388(3) .
C25 C26 1.390(3) .
C25 C29 1.511(3) .
C26 C27 1.394(3) .
C27 C30 1.511(3) .
