#------------------------------------------------------------------------------
#$Date: 2016-03-23 02:46:51 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179204 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/38/4313814.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_4313814
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 223K'
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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             2002-09-05T16:58:56-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 108.945(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.6523(3)
_cell_length_b                   17.0131(4)
_cell_length_c                   11.1760(3)
_cell_measurement_reflns_used    18609
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      27.878
_cell_measurement_theta_min      3.705
_cell_measurement_wavelength     0.71073
_cell_volume                     1915.70(9)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_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      223(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0594
_diffrn_reflns_av_unetI/netI     0.0561
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            17329
_diffrn_reflns_theta_full        27.89
_diffrn_reflns_theta_max         27.89
_diffrn_reflns_theta_min         3.73
_exptl_absorpt_coefficient_mu    1.465
_exptl_absorpt_correction_T_max  0.8936
_exptl_absorpt_correction_T_min  0.8221
_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    1.399
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             832
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.617
_refine_diff_density_min         -0.626
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         4547
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0735
_refine_ls_R_factor_gt           0.0409
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0314P)²+2.0172P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0811
_refine_ls_wR_factor_ref         0.0914
_reflns_number_gt                3131
_reflns_number_total             4547
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic026272fsi20021216_045625_5.cif
_cod_data_source_block           cy3sncl223
_cod_database_code               4313814
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
Sn Sn 0.02881(2) 0.244216(13) 0.87120(2) 0.03221(10) Uani 1 1 d . . .
Cl Cl 0.02769(13) 0.23019(7) 1.08824(10) 0.0575(3) Uani 1 1 d . . .
C1 C 0.1271(4) 0.3566(2) 0.8817(4) 0.0390(9) Uani 1 1 d . . .
H1 H 0.0716 0.3867 0.8075 0.047 Uiso 1 1 calc R . .
C2 C 0.2628(4) 0.3538(2) 0.8682(4) 0.0522(11) Uani 1 1 d . . .
H2A H 0.2583 0.3254 0.7906 0.063 Uiso 1 1 calc R . .
H2B H 0.3232 0.3251 0.94 0.063 Uiso 1 1 calc R . .
C3 C 0.3173(5) 0.4364(3) 0.8632(5) 0.0653(13) Uani 1 1 d . . .
H3A H 0.4079 0.4326 0.86 0.078 Uiso 1 1 calc R . .
H3B H 0.2627 0.4628 0.7857 0.078 Uiso 1 1 calc R . .
C4 C 0.3181(5) 0.4848(3) 0.9756(5) 0.0687(14) Uani 1 1 d . . .
H4A H 0.3823 0.4626 1.052 0.082 Uiso 1 1 calc R . .
H4B H 0.3461 0.5385 0.9652 0.082 Uiso 1 1 calc R . .
C5 C 0.1836(6) 0.4869(3) 0.9910(5) 0.0734(15) Uani 1 1 d . . .
H5A H 0.1225 0.516 0.9202 0.088 Uiso 1 1 calc R . .
H5B H 0.1894 0.5148 1.0693 0.088 Uiso 1 1 calc R . .
C6 C 0.1284(5) 0.4048(3) 0.9955(5) 0.0616(13) Uani 1 1 d . . .
H6A H 0.1827 0.3781 1.0727 0.074 Uiso 1 1 calc R . .
H6B H 0.0378 0.409 0.9988 0.074 Uiso 1 1 calc R . .
C7 C -0.1850(4) 0.2461(3) 0.7765(4) 0.0508(11) Uani 1 1 d . . .
H7 H -0.1973 0.2571 0.6865 0.061 Uiso 1 1 calc R . .
C8 C -0.2495(5) 0.3089(4) 0.8179(9) 0.143(4) Uani 1 1 d . . .
H8A H -0.2113 0.3588 0.8029 0.172 Uiso 1 1 calc R . .
H8B H -0.2319 0.3039 0.9092 0.172 Uiso 1 1 calc R . .
C9 C -0.4012(6) 0.3112(4) 0.7510(10) 0.165(4) Uani 1 1 d . . .
H9A H -0.44 0.3507 0.7922 0.198 Uiso 1 1 calc R . .
H9B H -0.419 0.3275 0.6629 0.198 Uiso 1 1 calc R . .
C10 C -0.4644(5) 0.2377(4) 0.7526(7) 0.0877(19) Uani 1 1 d . . .
H10A H -0.4633 0.2265 0.839 0.105 Uiso 1 1 calc R . .
H10B H -0.5573 0.241 0.6984 0.105 Uiso 1 1 calc R . .
C11 C -0.4019(6) 0.1752(4) 0.7103(10) 0.177(5) Uani 1 1 d . . .
H11A H -0.4191 0.1808 0.6191 0.212 Uiso 1 1 calc R . .
H11B H -0.4412 0.1254 0.7243 0.212 Uiso 1 1 calc R . .
C12 C -0.2509(5) 0.1720(4) 0.7776(10) 0.158(4) Uani 1 1 d . . .
H12A H -0.234 0.1557 0.8656 0.19 Uiso 1 1 calc R . .
H12B H -0.2126 0.1321 0.7366 0.19 Uiso 1 1 calc R . .
C13 C 0.1344(4) 0.1371(2) 0.8610(4) 0.0433(10) Uani 1 1 d . . .
H13 H 0.1327 0.132 0.7722 0.052 Uiso 1 1 calc R . .
C14 C 0.2748(5) 0.1395(3) 0.9398(9) 0.133(3) Uani 1 1 d . . .
H14A H 0.2807 0.1489 1.028 0.16 Uiso 1 1 calc R . .
H14B H 0.3185 0.1835 0.9126 0.16 Uiso 1 1 calc R . .
C15 C 0.3479(6) 0.0630(3) 0.9319(10) 0.172(5) Uani 1 1 d . . .
H15A H 0.3537 0.0578 0.8466 0.207 Uiso 1 1 calc R . .
H15B H 0.4386 0.0658 0.9915 0.207 Uiso 1 1 calc R . .
C16 C 0.2820(5) -0.0072(3) 0.9608(5) 0.0767(16) Uani 1 1 d . . .
H16A H 0.328 -0.0545 0.9473 0.092 Uiso 1 1 calc R . .
H16B H 0.2868 -0.0059 1.0499 0.092 Uiso 1 1 calc R . .
C17 C 0.1429(5) -0.0102(3) 0.8803(6) 0.0787(17) Uani 1 1 d . . .
H17A H 0.0993 -0.055 0.9055 0.094 Uiso 1 1 calc R . .
H17B H 0.1385 -0.0181 0.7922 0.094 Uiso 1 1 calc R . .
C18 C 0.0695(5) 0.0649(3) 0.8902(6) 0.0777(17) Uani 1 1 d . . .
H18A H -0.0215 0.0618 0.8315 0.093 Uiso 1 1 calc R . .
H18B H 0.0648 0.0693 0.9761 0.093 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 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
C13 Sn C1 119.75(16) . . ?
C13 Sn C7 117.78(16) . . ?
C1 Sn C7 115.12(15) . . ?
C13 Sn Cl 98.08(11) . . ?
C1 Sn Cl 101.01(10) . . ?
C7 Sn Cl 98.18(12) . . ?
C13 Sn Cl 84.10(10) . 4_565 ?
C1 Sn Cl 77.23(10) . 4_565 ?
C7 Sn Cl 81.36(12) . 4_565 ?
Cl Sn Cl 177.712(17) . 4_565 ?
Sn Cl Sn 166.53(5) . 4_566 ?
C2 C1 C6 110.9(3) . . ?
C2 C1 Sn 115.5(3) . . ?
C6 C1 Sn 113.4(3) . . ?
C1 C2 C3 111.3(4) . . ?
C4 C3 C2 111.9(4) . . ?
C5 C4 C3 111.3(4) . . ?
C4 C5 C6 112.1(4) . . ?
C1 C6 C5 111.6(4) . . ?
C8 C7 C12 111.3(5) . . ?
C8 C7 Sn 113.1(3) . . ?
C12 C7 Sn 114.7(3) . . ?
C7 C8 C9 113.6(5) . . ?
C10 C9 C8 113.4(6) . . ?
C11 C10 C9 112.3(6) . . ?
C10 C11 C12 113.2(6) . . ?
C7 C12 C11 113.5(6) . . ?
C14 C13 C18 110.1(4) . . ?
C14 C13 Sn 113.0(3) . . ?
C18 C13 Sn 113.3(3) . . ?
C13 C14 C15 112.2(5) . . ?
C16 C15 C14 112.8(6) . . ?
C17 C16 C15 110.7(5) . . ?
C16 C17 C18 111.6(4) . . ?
C13 C18 C17 112.9(4) . . ?
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 C13 2.163(4) . ?
Sn C1 2.165(4) . ?
Sn C7 2.178(4) . ?
Sn Cl 2.4412(11) . ?
Sn Cl 3.1884(11) 4_565 ?
Cl Sn 3.1884(11) 4_566 ?
C1 C2 1.502(5) . ?
C1 C6 1.510(5) . ?
C2 C3 1.529(6) . ?
C3 C4 1.499(7) . ?
C4 C5 1.498(7) . ?
C5 C6 1.522(6) . ?
C7 C8 1.426(7) . ?
C7 C12 1.444(7) . ?
C8 C9 1.545(8) . ?
C9 C10 1.423(8) . ?
C10 C11 1.414(8) . ?
C11 C12 1.540(8) . ?
C13 C14 1.470(7) . ?
C13 C18 1.497(6) . ?
C14 C15 1.535(7) . ?
C15 C16 1.473(8) . ?
C16 C17 1.463(7) . ?
C17 C18 1.520(6) . ?
