#------------------------------------------------------------------------------
#$Date: 2016-03-23 02:46:51 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179204 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/38/4313815.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_4313815
loop_
_publ_author_name
'Ashrafomolouk Asadi'
'Colin Eaborn'
'Peter B. Hitchcock'
'Margaret M. Meehan'
'J. David Smith'
_publ_section_title
;
 The Structure of Tri(cyclohexyl)tin Chloride between 108 and 298 K: A
 Compound in Which Molecular Dimensions Vary with Temperature
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4141
_journal_page_last               4146
_journal_paper_doi               10.1021/ic026272f
_journal_volume                  42
_journal_year                    2003
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C18 H33 Cl1 Sn1'
_chemical_formula_sum            'C18 H33 Cl Sn'
_chemical_formula_weight         403.58
_chemical_name_common            '[cy3SnCl] at 248K'
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      11
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.2
_audit_creation_date             2002-09-09T16:46:55-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 108.487(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.6230(4)
_cell_length_b                   17.0754(6)
_cell_length_c                   5.6281(2)
_cell_measurement_reflns_used    15154
_cell_measurement_temperature    248(2)
_cell_measurement_theta_max      28
_cell_measurement_theta_min      4
_cell_measurement_wavelength     0.71073
_cell_volume                     968.21(6)
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      248(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0504
_diffrn_reflns_av_unetI/netI     0.0483
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            8913
_diffrn_reflns_theta_full        27.89
_diffrn_reflns_theta_max         27.89
_diffrn_reflns_theta_min         3.71
_exptl_absorpt_coefficient_mu    1.449
_exptl_absorpt_correction_T_max  0.8937
_exptl_absorpt_correction_T_min  0.8205
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.384
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             416
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.686
_refine_diff_density_min         -0.716
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     97
_refine_ls_number_reflns         2382
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0772
_refine_ls_R_factor_gt           0.0513
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0659P)²+1.5049P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1232
_refine_ls_wR_factor_ref         0.1367
_reflns_number_gt                1788
_reflns_number_total             2382
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic026272fsi20021216_045625_6.cif
_cod_data_source_block           cy3sncl248
_cod_database_code               4313815
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, z'
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
Sn Sn 0.03152(4) 0.25 0.25440(8) 0.0484(2) Uani 1 2 d S . .
Cl Cl 0.0304(3) 0.25 0.6847(5) 0.1143(12) Uani 1 2 d S . .
C1 C 0.1335(6) 0.3587(4) 0.2502(12) 0.0679(15) Uani 1 1 d . . .
H1 H 0.0978 0.3783 0.0762 0.082 Uiso 1 1 calc R . .
C2 C 0.2700(9) 0.3548(6) 0.301(3) 0.180(7) Uani 1 1 d . . .
H2A H 0.2896 0.3185 0.182 0.216 Uiso 1 1 calc R . .
H2B H 0.3105 0.3336 0.4696 0.216 Uiso 1 1 calc R . .
C3 C 0.3333(11) 0.4354(6) 0.283(4) 0.195(7) Uani 1 1 d . . .
H3A H 0.4299 0.4295 0.333 0.234 Uiso 1 1 calc R . .
H3B H 0.3027 0.453 0.1077 0.234 Uiso 1 1 calc R . .
C4 C 0.3007(12) 0.4949(7) 0.4380(19) 0.135(4) Uani 1 1 d . . .
H4A H 0.337 0.4806 0.6154 0.163 Uiso 1 1 calc R . .
H4B H 0.3381 0.5456 0.4133 0.163 Uiso 1 1 calc R . .
C5 C 0.1660(15) 0.4993(7) 0.368(4) 0.277(13) Uani 1 1 d . . .
H5A H 0.1313 0.515 0.1918 0.332 Uiso 1 1 calc R . .
H5B H 0.1402 0.5393 0.4687 0.332 Uiso 1 1 calc R . .
C6 C 0.1031(17) 0.4182(8) 0.404(5) 0.283(13) Uani 1 1 d . . .
H6A H 0.1374 0.4025 0.5799 0.339 Uiso 1 1 calc R . .
H6B H 0.0066 0.4239 0.359 0.339 Uiso 1 1 calc R . .
C7 C -0.1813(8) 0.25 0.0678(17) 0.073(2) Uani 1 2 d S . .
H7 H -0.192 0.25 -0.1135 0.087 Uiso 1 2 calc SR . .
C8 C -0.2467(9) 0.3186(6) 0.107(3) 0.206(9) Uani 1 1 d . . .
H8A H -0.2072 0.364 0.0515 0.248 Uiso 1 1 calc R . .
H8B H -0.2319 0.3246 0.2874 0.248 Uiso 1 1 calc R . .
C9 C -0.3976(9) 0.3180(7) -0.031(4) 0.219(9) Uani 1 1 d . . .
H9A H -0.4379 0.3641 0.0188 0.262 Uiso 1 1 calc R . .
H9B H -0.4127 0.3216 -0.2122 0.262 Uiso 1 1 calc R . .
C10 C -0.4604(10) 0.25 0.019(3) 0.119(5) Uani 1 2 d S . .
H10A H -0.457 0.25 0.1946 0.143 Uiso 1 2 calc SR . .
H10B H -0.5538 0.25 -0.0856 0.143 Uiso 1 2 calc SR . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Sn 0.0400(3) 0.0649(4) 0.0418(3) 0 0.0151(2) 0
Cl 0.104(2) 0.202(4) 0.0438(11) 0 0.0345(13) 0
C1 0.062(4) 0.070(4) 0.071(4) -0.011(3) 0.020(3) -0.010(3)
C2 0.071(6) 0.080(6) 0.38(2) 0.018(9) 0.066(9) -0.011(5)
C3 0.105(8) 0.096(7) 0.41(2) -0.034(11) 0.126(11) -0.038(6)
C4 0.136(9) 0.144(9) 0.126(8) -0.057(7) 0.042(7) -0.085(8)
C5 0.170(14) 0.111(9) 0.61(4) -0.147(17) 0.205(19) -0.060(9)
C6 0.230(15) 0.142(10) 0.60(3) -0.202(16) 0.31(2) -0.125(11)
C7 0.038(4) 0.118(8) 0.065(5) 0 0.020(4) 0
C8 0.048(4) 0.095(7) 0.43(3) 0.002(10) 0.006(8) 0.005(5)
C9 0.046(5) 0.134(9) 0.43(3) 0.058(12) 0.016(9) 0.013(6)
C10 0.043(5) 0.178(13) 0.141(11) 0 0.034(6) 0
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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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 Sn C1 119.1(3) . 4_565 ?
C1 Sn C7 116.45(18) . . ?
C1 Sn C7 116.45(18) 4_565 . ?
C1 Sn Cl 99.95(17) . . ?
C1 Sn Cl 99.95(17) 4_565 . ?
C7 Sn Cl 98.6(2) . . ?
C1 Sn Cl 80.28(17) . 1_554 ?
C1 Sn Cl 80.28(17) 4_565 1_554 ?
C7 Sn Cl 81.0(2) . 1_554 ?
Cl Sn Cl 179.52(13) . 1_554 ?
Sn Cl Sn 179.52(13) . 1_556 ?
C2 C1 C6 109.3(10) . . ?
C2 C1 Sn 116.9(5) . . ?
C6 C1 Sn 113.2(6) . . ?
C1 C2 C3 113.0(8) . . ?
C4 C3 C2 113.0(11) . . ?
C5 C4 C3 107.1(9) . . ?
C4 C5 C6 111.4(14) . . ?
C1 C6 C5 111.1(10) . . ?
C8 C7 C8 111.8(11) 4_565 . ?
C8 C7 Sn 114.3(5) 4_565 . ?
C8 C7 Sn 114.3(5) . . ?
C7 C8 C9 113.4(10) . . ?
C10 C9 C8 112.6(10) . . ?
C9 C10 C9 110.8(14) 4_565 . ?
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
Sn C1 2.153(6) . ?
Sn C1 2.153(6) 4_565 ?
Sn C7 2.170(8) . ?
Sn Cl 2.426(2) . ?
Sn Cl 3.202(2) 1_554 ?
Cl Sn 3.202(2) 1_556 ?
C1 C2 1.388(11) . ?
C1 C6 1.435(12) . ?
C2 C3 1.550(12) . ?
C3 C4 1.452(14) . ?
C4 C5 1.360(17) . ?
C5 C6 1.577(16) . ?
C7 C8 1.415(11) 4_565 ?
C7 C8 1.415(11) . ?
C8 C9 1.545(13) . ?
C9 C10 1.411(13) . ?
C10 C9 1.411(13) 4_565 ?
