#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:15:55 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179319 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/16/4321605.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_4321605
loop_
_publ_author_name
'Barrett E. Eichler'
'Philip P. Power'
_publ_section_title
;
 Characterization of the Sterically Encumbered Terphenyl-Substituted
 Species 2,6-Trip2H3C6S̈n-Sn(Me)2C6H3-2,6-Trip2, an Unsymmetric, Group 14
 Element, Methylmethylene, Valence Isomer of an Alkene, Its Related
 Lithium Derivative 2,6-Trip2H3C6(Me)2Sn-Sn(Li)(Me)C6H3-2,6-Trip2, and the
 Monomer Sn(t-Bu)C6H3-2,6-Trip2 (Trip = C6H2-2,4,6-i-Pr3)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5444
_journal_page_last               5449
_journal_paper_doi               10.1021/ic0005137
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C40 H58 Sn'
_chemical_formula_weight         657.55
_chemical_melting_point          113
_chemical_name_common            Bert*Sn(t-Bu)
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_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                 106.9000(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   32.1821(13)
_cell_length_b                   9.5744(4)
_cell_length_c                   24.7577(10)
_cell_measurement_reflns_used    9542
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.67
_cell_measurement_theta_min      2.23
_cell_volume                     7299.0(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL v. 5.10'
_computing_molecular_graphics    'XP, Bruker SHELXTL v. 5.10'
_computing_publication_material  'XCIF, Bruker SHELXTL v. 5.10'
_computing_structure_refinement  'XL, Bruker SHELXTL v. 5.10'
_computing_structure_solution    'XS, Bruker SHELXTL v. 5.10'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'Bruker SMART 1000'
_diffrn_measurement_method       /w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0601
_diffrn_reflns_av_sigmaI/netI    0.0616
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            81158
_diffrn_reflns_theta_full        31.52
_diffrn_reflns_theta_max         31.52
_diffrn_reflns_theta_min         1.32
_diffrn_standards_decay_%        <0.01
_diffrn_standards_number         '50 frames remeasured'
_exptl_absorpt_coefficient_mu    0.724
_exptl_absorpt_correction_T_max  0.8868
_exptl_absorpt_correction_T_min  0.8807
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;SADABS: an empirical absorption program by G. M. Sheldrick
 using the method described by Blessing, R. H.; Acta Cryst.
 A51, 1995, 33.  
;
_exptl_crystal_colour            purple-red
_exptl_crystal_density_diffrn    1.197
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       shard
_exptl_crystal_F_000             2784
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.163
_refine_diff_density_min         -0.553
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.908
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     398
_refine_ls_number_reflns         11794
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.908
_refine_ls_R_factor_all          0.0695
_refine_ls_R_factor_gt           0.0385
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0416P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0774
_refine_ls_wR_factor_ref         0.0856
_reflns_number_gt                8029
_reflns_number_total             11794
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0005137_1.cif
_cod_data_source_block           be23
_cod_database_code               4321605
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Sn1 Sn 0.656162(5) 0.284040(18) 0.964166(6) 0.02808(5) Uani 1 1 d . A .
C1 C 0.60084(5) 0.14841(19) 0.92105(7) 0.0148(3) Uani 1 1 d . . .
C2 C 0.59633(6) 0.01461(19) 0.94159(7) 0.0149(3) Uani 1 1 d . . .
C3 C 0.56490(6) -0.0763(2) 0.90974(8) 0.0175(4) Uani 1 1 d . . .
H3A H 0.5617 -0.1647 0.9236 0.021 Uiso 1 1 calc R . .
C4 C 0.53816(6) -0.0352(2) 0.85707(8) 0.0183(4) Uani 1 1 d . . .
H4A H 0.5171 -0.0961 0.8361 0.022 Uiso 1 1 calc R . .
C5 C 0.54285(6) 0.0958(2) 0.83586(8) 0.0175(4) Uani 1 1 d . . .
H5A H 0.5251 0.1224 0.8005 0.021 Uiso 1 1 calc R . .
C6 C 0.57417(6) 0.18816(18) 0.86748(8) 0.0147(4) Uani 1 1 d . . .
C7 C 0.58176(6) 0.32780(19) 0.84454(8) 0.0152(3) Uani 1 1 d . . .
C8 C 0.61486(6) 0.3427(2) 0.81820(8) 0.0185(4) Uani 1 1 d . . .
C9 C 0.62266(6) 0.4742(2) 0.79831(8) 0.0200(4) Uani 1 1 d . . .
H9A H 0.6446 0.4835 0.7811 0.024 Uiso 1 1 calc R . .
C10 C 0.59864(6) 0.59085(19) 0.80350(8) 0.0179(4) Uani 1 1 d . . .
C11 C 0.56608(6) 0.57385(19) 0.82983(8) 0.0173(4) Uani 1 1 d . . .
H11A H 0.5499 0.6515 0.8341 0.021 Uiso 1 1 calc R . .
C12 C 0.55676(6) 0.44543(19) 0.85001(7) 0.0151(4) Uani 1 1 d . . .
C13 C 0.62828(6) -0.02939(19) 0.99636(8) 0.0154(4) Uani 1 1 d . . .
C14 C 0.67205(6) -0.0529(2) 0.99722(8) 0.0192(4) Uani 1 1 d . . .
C15 C 0.70286(6) -0.0794(2) 1.04855(8) 0.0220(4) Uani 1 1 d . . .
H15A H 0.7318 -0.0902 1.0493 0.026 Uiso 1 1 calc R . .
C16 C 0.69204(6) -0.0904(2) 1.09850(8) 0.0216(4) Uani 1 1 d . . .
C17 C 0.64851(6) -0.0757(2) 1.09637(8) 0.0215(4) Uani 1 1 d . . .
H17A H 0.6406 -0.0871 1.1294 0.026 Uiso 1 1 calc R . .
C18 C 0.61630(6) -0.0445(2) 1.04641(8) 0.0183(4) Uani 1 1 d . . .
C19 C 0.56915(6) -0.0316(2) 1.04688(9) 0.0237(4) Uani 1 1 d . . .
H19A H 0.5534 0.0220 1.0135 0.028 Uiso 1 1 calc R . .
C20 C 0.56437(8) 0.0446(3) 1.09917(10) 0.0380(6) Uani 1 1 d . . .
H20A H 0.5816 0.1280 1.1053 0.057 Uiso 1 1 calc R . .
H20B H 0.5740 -0.0152 1.1315 0.057 Uiso 1 1 calc R . .
H20C H 0.5344 0.0687 1.0935 0.057 Uiso 1 1 calc R . .
C21 C 0.54769(8) -0.1754(3) 1.04330(11) 0.0369(6) Uani 1 1 d . . .
H21A H 0.5475 -0.2197 1.0085 0.055 Uiso 1 1 calc R . .
H21B H 0.5184 -0.1647 1.0448 0.055 Uiso 1 1 calc R . .
H21C H 0.5637 -0.2320 1.0744 0.055 Uiso 1 1 calc R . .
C22 C 0.72692(7) -0.1223(2) 1.15348(8) 0.0270(5) Uani 1 1 d . . .
H22A H 0.7550 -0.1173 1.1457 0.032 Uiso 1 1 calc R . .
C23 C 0.72760(7) -0.0148(3) 1.19907(9) 0.0331(5) Uani 1 1 d . . .
H23A H 0.7314 0.0768 1.1854 0.050 Uiso 1 1 calc R . .
H23B H 0.7512 -0.0349 1.2321 0.050 Uiso 1 1 calc R . .
H23C H 0.7007 -0.0186 1.2084 0.050 Uiso 1 1 calc R . .
C24 C 0.72220(8) -0.2694(2) 1.17362(10) 0.0325(5) Uani 1 1 d . . .
H24A H 0.7228 -0.3348 1.1445 0.049 Uiso 1 1 calc R . .
H24B H 0.6951 -0.2775 1.1823 0.049 Uiso 1 1 calc R . .
H24C H 0.7457 -0.2889 1.2068 0.049 Uiso 1 1 calc R . .
C25 C 0.68434(7) -0.0691(2) 0.94264(8) 0.0265(5) Uani 1 1 d . . .
H25A H 0.6644 -0.0117 0.9137 0.032 Uiso 1 1 calc R . .
C26 C 0.67715(8) -0.2221(3) 0.92395(10) 0.0389(6) Uani 1 1 d . . .
H26A H 0.6472 -0.2464 0.9182 0.058 Uiso 1 1 calc R . .
H26B H 0.6952 -0.2811 0.9526 0.058 Uiso 1 1 calc R . .
H26C H 0.6845 -0.2345 0.8893 0.058 Uiso 1 1 calc R . .
C27 C 0.73074(7) -0.0235(3) 0.94660(10) 0.0402(6) Uani 1 1 d . . .
H27A H 0.7364 0.0660 0.9648 0.060 Uiso 1 1 calc R . .
H27B H 0.7340 -0.0170 0.9093 0.060 Uiso 1 1 calc R . .
H27C H 0.7509 -0.0909 0.9682 0.060 Uiso 1 1 calc R . .
C28 C 0.63992(6) 0.2166(2) 0.80688(9) 0.0230(4) Uani 1 1 d . . .
H28A H 0.6367 0.1415 0.8323 0.028 Uiso 1 1 calc R . .
C29 C 0.68845(7) 0.2430(2) 0.81750(10) 0.0294(5) Uani 1 1 d . . .
H29A H 0.7006 0.2789 0.8550 0.044 Uiso 1 1 calc R . .
H29B H 0.6926 0.3098 0.7906 0.044 Uiso 1 1 calc R . .
H29C H 0.7026 0.1571 0.8135 0.044 Uiso 1 1 calc R . .
C30 C 0.61921(7) 0.1667(2) 0.74611(9) 0.0283(5) Uani 1 1 d . . .
H30A H 0.5892 0.1445 0.7409 0.042 Uiso 1 1 calc R . .
H30B H 0.6342 0.0850 0.7391 0.042 Uiso 1 1 calc R . .
H30C H 0.6213 0.2393 0.7203 0.042 Uiso 1 1 calc R . .
C31 C 0.60583(6) 0.7342(2) 0.78094(9) 0.0209(4) Uani 1 1 d . . .
H31A H 0.6098 0.8011 0.8120 0.025 Uiso 1 1 calc R . .
C32 C 0.64589(7) 0.7431(2) 0.76003(11) 0.0318(5) Uani 1 1 d . . .
H32A H 0.6710 0.7135 0.7895 0.048 Uiso 1 1 calc R . .
H32B H 0.6498 0.8377 0.7497 0.048 Uiso 1 1 calc R . .
H32C H 0.6421 0.6835 0.7278 0.048 Uiso 1 1 calc R . .
C33 C 0.56566(7) 0.7804(2) 0.73367(9) 0.0275(4) Uani 1 1 d . . .
H33A H 0.5403 0.7717 0.7463 0.041 Uiso 1 1 calc R . .
H33B H 0.5625 0.7225 0.7011 0.041 Uiso 1 1 calc R . .
H33C H 0.5690 0.8760 0.7240 0.041 Uiso 1 1 calc R . .
C34 C 0.51880(6) 0.4303(2) 0.87459(8) 0.0190(4) Uani 1 1 d . . .
H34A H 0.5246 0.3489 0.8997 0.023 Uiso 1 1 calc R . .
C35 C 0.51241(7) 0.5563(2) 0.90924(9) 0.0269(5) Uani 1 1 d . . .
H35A H 0.5393 0.5781 0.9370 0.040 Uiso 1 1 calc R . .
H35B H 0.4908 0.5349 0.9277 0.040 Uiso 1 1 calc R . .
H35C H 0.5031 0.6351 0.8847 0.040 Uiso 1 1 calc R . .
C36 C 0.47689(6) 0.4012(2) 0.82718(10) 0.0279(5) Uani 1 1 d . . .
H36A H 0.4800 0.3157 0.8084 0.042 Uiso 1 1 calc R . .
H36B H 0.4715 0.4767 0.8005 0.042 Uiso 1 1 calc R . .
H36C H 0.4530 0.3929 0.8429 0.042 Uiso 1 1 calc R . .
C37 C 0.63198(8) 0.3829(2) 1.03069(10) 0.0339(5) Uani 1 1 d . . .
C38 C 0.58702(8) 0.3537(3) 1.02948(12) 0.0316(7) Uani 0.827(4) 1 d P A 1
H38A H 0.5810 0.3971 1.0614 0.047 Uiso 0.827(4) 1 calc PR A 1
H38B H 0.5829 0.2546 1.0310 0.047 Uiso 0.827(4) 1 calc PR A 1
H38C H 0.5676 0.3903 0.9953 0.047 Uiso 0.827(4) 1 calc PR A 1
C39 C 0.66457(10) 0.3300(4) 1.08723(14) 0.0383(8) Uani 0.827(4) 1 d P A 1
H39A H 0.6576 0.3724 1.1186 0.057 Uiso 0.827(4) 1 calc PR A 1
H39B H 0.6936 0.3549 1.0881 0.057 Uiso 0.827(4) 1 calc PR A 1
H39C H 0.6624 0.2303 1.0896 0.057 Uiso 0.827(4) 1 calc PR A 1
C40 C 0.64029(10) 0.5430(3) 1.02852(15) 0.0428(8) Uani 0.827(4) 1 d P A 1
H40A H 0.6335 0.5881 1.0596 0.064 Uiso 0.827(4) 1 calc PR A 1
H40B H 0.6222 0.5805 0.9936 0.064 Uiso 0.827(4) 1 calc PR A 1
H40C H 0.6702 0.5590 1.0311 0.064 Uiso 0.827(4) 1 calc PR A 1
C41 C 0.6494(4) 0.4318(15) 1.0755(6) 0.031(2) Uiso 0.173(4) 1 d P A 2
H41A H 0.6670 0.5082 1.0674 0.037 Uiso 0.173(4) 1 calc PR A 2
C42 C 0.6228(4) 0.4994(14) 1.1097(5) 0.031(2) Uiso 0.173(4) 1 d P A 2
H42A H 0.6025 0.5637 1.0863 0.046 Uiso 0.173(4) 1 calc PR A 2
H42B H 0.6418 0.5488 1.1410 0.046 Uiso 0.173(4) 1 calc PR A 2
H42C H 0.6074 0.4287 1.1235 0.046 Uiso 0.173(4) 1 calc PR A 2
C43 C 0.6821(5) 0.3322(16) 1.1119(7) 0.031(2) Uiso 0.173(4) 1 d P A 2
H43A H 0.7010 0.2984 1.0910 0.046 Uiso 0.173(4) 1 calc PR A 2
H43B H 0.6672 0.2549 1.1225 0.046 Uiso 0.173(4) 1 calc PR A 2
H43C H 0.6990 0.3799 1.1451 0.046 Uiso 0.173(4) 1 calc PR A 2
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
_geom_angle_publ_flag
C1 Sn1 C37 101.61(8) . . ?
C2 C1 C6 119.36(16) . . ?
C2 C1 Sn1 121.03(13) . . ?
C6 C1 Sn1 118.76(13) . . ?
C3 C2 C1 120.05(16) . . ?
C3 C2 C13 121.95(16) . . ?
C1 C2 C13 117.87(16) . . ?
C2 C3 C4 120.18(17) . . ?
C5 C4 C3 120.30(18) . . ?
C4 C5 C6 120.07(17) . . ?
C5 C6 C1 120.02(17) . . ?
C5 C6 C7 121.47(16) . . ?
C1 C6 C7 118.44(16) . . ?
C8 C7 C12 119.46(17) . . ?
C8 C7 C6 119.58(16) . . ?
C12 C7 C6 120.94(16) . . ?
C9 C8 C7 119.37(17) . . ?
C9 C8 C28 119.31(17) . . ?
C7 C8 C28 121.16(17) . . ?
C10 C9 C8 122.02(18) . . ?
C9 C10 C11 117.68(17) . . ?
C9 C10 C31 122.93(18) . . ?
C11 C10 C31 119.38(17) . . ?
C12 C11 C10 122.69(17) . . ?
C11 C12 C7 118.78(17) . . ?
C11 C12 C34 120.62(16) . . ?
C7 C12 C34 120.52(16) . . ?
C18 C13 C14 119.64(17) . . ?
C18 C13 C2 122.13(16) . . ?
C14 C13 C2 118.22(16) . . ?
C15 C14 C13 118.93(17) . . ?
C15 C14 C25 119.52(17) . . ?
C13 C14 C25 121.01(17) . . ?
C16 C15 C14 122.25(18) . . ?
C15 C16 C17 118.06(18) . . ?
C15 C16 C22 120.20(18) . . ?
C17 C16 C22 121.71(18) . . ?
C16 C17 C18 122.30(18) . . ?
C17 C18 C13 118.63(17) . . ?
C17 C18 C19 119.64(17) . . ?
C13 C18 C19 121.71(17) . . ?
C18 C19 C21 111.07(18) . . ?
C18 C19 C20 112.91(18) . . ?
C21 C19 C20 108.82(19) . . ?
C24 C22 C16 111.24(18) . . ?
C24 C22 C23 111.42(18) . . ?
C16 C22 C23 112.03(18) . . ?
C14 C25 C27 114.47(18) . . ?
C14 C25 C26 108.08(18) . . ?
C27 C25 C26 110.53(19) . . ?
C8 C28 C29 114.02(18) . . ?
C8 C28 C30 108.98(16) . . ?
C29 C28 C30 110.56(16) . . ?
C32 C31 C10 114.05(17) . . ?
C32 C31 C33 109.44(17) . . ?
C10 C31 C33 110.79(16) . . ?
C12 C34 C35 113.81(16) . . ?
C12 C34 C36 109.91(16) . . ?
C35 C34 C36 109.95(16) . . ?
C41 C37 C38 106.9(7) . . ?
C41 C37 C40 66.7(7) . . ?
C38 C37 C40 111.4(2) . . ?
C41 C37 C39 44.0(7) . . ?
C38 C37 C39 110.9(2) . . ?
C40 C37 C39 105.7(2) . . ?
C41 C37 Sn1 133.5(7) . . ?
C38 C37 Sn1 117.33(18) . . ?
C40 C37 Sn1 106.98(18) . . ?
C39 C37 Sn1 103.66(17) . . ?
C37 C41 C43 111.5(12) . . ?
C37 C41 C42 120.2(11) . . ?
C43 C41 C42 110.3(11) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sn1 C1 2.2114(18) . ?
Sn1 C37 2.227(2) . ?
C1 C2 1.401(3) . ?
C1 C6 1.407(2) . ?
C2 C3 1.392(3) . ?
C2 C13 1.504(2) . ?
C3 C4 1.394(3) . ?
C4 C5 1.385(3) . ?
C5 C6 1.397(3) . ?
C6 C7 1.500(2) . ?
C7 C8 1.409(3) . ?
C7 C12 1.413(2) . ?
C8 C9 1.401(3) . ?
C8 C28 1.522(3) . ?
C9 C10 1.385(3) . ?
C10 C11 1.395(3) . ?
C10 C31 1.525(3) . ?
C11 C12 1.392(3) . ?
C12 C34 1.522(2) . ?
C13 C18 1.408(3) . ?
C13 C14 1.420(3) . ?
C14 C15 1.389(3) . ?
C14 C25 1.522(3) . ?
C15 C16 1.383(3) . ?
C16 C17 1.394(3) . ?
C16 C22 1.523(3) . ?
C17 C18 1.396(3) . ?
C18 C19 1.526(3) . ?
C19 C21 1.531(3) . ?
C19 C20 1.532(3) . ?
C22 C24 1.516(3) . ?
C22 C23 1.523(3) . ?
C25 C27 1.531(3) . ?
C25 C26 1.533(3) . ?
C28 C29 1.527(3) . ?
C28 C30 1.534(3) . ?
C31 C32 1.525(3) . ?
C31 C33 1.535(3) . ?
C34 C35 1.529(3) . ?
C34 C36 1.534(3) . ?
C37 C41 1.184(14) . ?
C37 C38 1.466(3) . ?
C37 C40 1.560(4) . ?
C37 C39 1.569(4) . ?
C41 C43 1.51(2) . ?
C41 C42 1.513(18) . ?
