#------------------------------------------------------------------------------
#$Date: 2017-07-11 14:26:40 +0300 (Tue, 11 Jul 2017) $
#$Revision: 198632 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/07/69/4076972.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_4076972
loop_
_publ_author_name
'Jambor, Roman'
'Dostál, Libor'
'R°užička, Aleš'
'Císařová, Ivana'
'Brus, Jiří'
'Holčapek, Michal'
'Holeček, Jaroslav'
_publ_section_title
;
 Organotin(IV) Derivatives of Some O,C,O-Chelating Ligands
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              3996
_journal_paper_doi               10.1021/om020361i
_journal_volume                  21
_journal_year                    2002
_chemical_formula_sum            'C16 H18 Cl2 O2 Sn'
_chemical_formula_weight         431.89
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           145
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'P 32'
_symmetry_space_group_name_H-M   'P 32'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   12.5240(2)
_cell_length_b                   12.5240(2)
_cell_length_c                   9.2900(2)
_cell_measurement_reflns_used    10767
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.1
_cell_measurement_theta_min      1
_cell_volume                     1261.92(4)
_computing_cell_refinement       'COLLECT and DENZO'
_computing_data_collection
'COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997)'
_computing_data_reduction        'COLLECT and DENZO'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Nonius KappaCCD area detector'
_diffrn_measurement_method       'φ and ω scans to fill the Ewald sphere'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0305
_diffrn_reflns_av_sigmaI/netI    0.0254
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            16486
_diffrn_reflns_theta_full        29.13
_diffrn_reflns_theta_max         29.13
_diffrn_reflns_theta_min         3.76
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.837
_exptl_absorpt_correction_T_max  0.583
_exptl_absorpt_correction_T_min  0.508
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SORTAV; Blessing 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.705
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             642
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.306
_refine_diff_density_min         -0.504
_refine_diff_density_rms         0.052
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.012(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     192
_refine_ls_number_reflns         4497
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.0153
_refine_ls_R_factor_gt           0.0150
_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)+(0.0076P)²+0.2685P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0340
_refine_ls_wR_factor_ref         0.0341
_reflns_number_gt                4452
_reflns_number_total             4497
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            om020361i.cif
_cod_data_source_block           snphoco-sort
_cod_depositor_comments
;
The following automatic conversions were performed:

'_geom_bond_publ_flag' value 'Y' changed to 'y' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (6
times).

'_geom_angle_publ_flag' value 'Y' changed to 'y' according
to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary
named 'cif_core.dic' version 2.4.1 from 2010-06-29 (15 times).

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'multi-scans' was replaced
with the value 'multi-scan' as specified in the replacement file
'src/cod-tools/trunk/data/replacement-values/replacement_values.lst'.

Automatic conversion script
Id: cif_fix_values 5376 2017-05-30 11:51:03Z andrius 
;
_cod_database_code               4076972
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z+2/3'
'-x+y, -x, z+1/3'
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 -0.031048(9) 0.657622(9) 0.203670(8) 0.01429(3) Uani 1 1 d .
Cl1 Cl -0.02577(4) 0.83768(4) 0.29957(5) 0.02348(9) Uani 1 1 d .
Cl2 Cl -0.24048(4) 0.53727(4) 0.28377(5) 0.02387(9) Uani 1 1 d .
C11 C 0.07082(15) 0.60302(15) 0.33604(16) 0.0149(3) Uani 1 1 d .
C12 C 0.02798(16) 0.47798(16) 0.35838(17) 0.0179(3) Uani 1 1 d .
C13 C 0.09152(18) 0.44237(18) 0.4526(2) 0.0244(4) Uani 1 1 d .
H13 H 0.0631 0.3591 0.4683 0.029 Uiso 1 1 calc R
C14 C 0.19638(19) 0.5301(2) 0.5226(2) 0.0261(4) Uani 1 1 d .
H14 H 0.2352 0.5059 0.5897 0.031 Uiso 1 1 calc R
C15 C 0.24366(16) 0.65433(18) 0.49273(18) 0.0218(4) Uani 1 1 d .
H15 H 0.3167 0.7129 0.5359 0.026 Uiso 1 1 calc R
C16 C 0.18194(15) 0.69159(16) 0.39811(17) 0.0167(3) Uani 1 1 d .
C17 C -0.08353(17) 0.38167(16) 0.2795(2) 0.0224(4) Uani 1 1 d .
H17A H -0.0782 0.3076 0.2673 0.027 Uiso 1 1 calc R
H17B H -0.1577 0.3607 0.3337 0.027 Uiso 1 1 calc R
C18 C -0.19461(19) 0.34524(18) 0.0612(2) 0.0286(4) Uani 1 1 d .
H18A H -0.1933 0.2698 0.0485 0.043 Uiso 1 1 calc R
H18B H -0.1943 0.3796 -0.0313 0.043 Uiso 1 1 calc R
H18C H -0.2677 0.3288 0.1128 0.043 Uiso 1 1 calc R
C19 C 0.23825(16) 0.82464(16) 0.35656(18) 0.0204(3) Uani 1 1 d .
H19A H 0.2056 0.8653 0.4161 0.024 Uiso 1 1 calc R
H19B H 0.3271 0.8667 0.3685 0.024 Uiso 1 1 calc R
C20 C 0.25985(18) 0.94992(17) 0.1543(2) 0.0263(4) Uani 1 1 d .
H20A H 0.2408 0.9980 0.2187 0.039 Uiso 1 1 calc R
H20B H 0.2265 0.9485 0.0608 0.039 Uiso 1 1 calc R
H20C H 0.3477 0.9859 0.1473 0.039 Uiso 1 1 calc R
C21 C -0.02444(15) 0.68951(16) -0.02128(17) 0.0163(3) Uani 1 1 d .
C22 C -0.03656(18) 0.78783(17) -0.07149(19) 0.0238(4) Uani 1 1 d .
H22 H -0.0495 0.8371 -0.0071 0.029 Uiso 1 1 calc R
C23 C -0.02916(19) 0.8119(2) -0.2194(2) 0.0319(5) Uani 1 1 d .
H23 H -0.0372 0.8773 -0.2534 0.038 Uiso 1 1 calc R
C24 C -0.0100(2) 0.7390(2) -0.3146(2) 0.0329(5) Uani 1 1 d .
H24 H -0.0062 0.7550 -0.4128 0.039 Uiso 1 1 calc R
C25 C 0.00380(18) 0.6421(2) -0.2659(2) 0.0300(5) Uani 1 1 d .
H25 H 0.0173 0.5935 -0.3308 0.036 Uiso 1 1 calc R
C26 C -0.00269(16) 0.61815(19) -0.1192(2) 0.0226(4) Uani 1 1 d .
H26 H 0.0076 0.5538 -0.0860 0.027 Uiso 1 1 calc R
O1 O -0.08753(12) 0.43142(11) 0.14139(13) 0.0198(2) Uani 1 1 d .
O2 O 0.20690(11) 0.82636(11) 0.20823(13) 0.0189(2) Uani 1 1 d .
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'
O O 0.0106 0.0060 '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_publ_flag
C11 Sn1 C21 131.30(6) y
C11 Sn1 Cl1 110.54(5) y
C21 Sn1 Cl1 102.07(5) y
C11 Sn1 Cl2 105.26(4) y
C21 Sn1 Cl2 110.58(4) y
Cl1 Sn1 Cl2 89.025(16) y
C11 Sn1 O1 70.08(5) y
C21 Sn1 O1 87.13(6) y
Cl1 Sn1 O1 165.09(3) y
Cl2 Sn1 O1 76.68(3) y
C11 Sn1 O2 68.28(5) y
C21 Sn1 O2 86.75(5) y
Cl1 Sn1 O2 75.70(3) y
Cl2 Sn1 O2 159.19(3) y
O1 Sn1 O2 116.95(4) y
C12 C11 C16 120.07(15) ?
C12 C11 Sn1 119.59(12) ?
C16 C11 Sn1 120.32(12) ?
C11 C12 C13 119.41(16) ?
C11 C12 C17 120.69(15) ?
C13 C12 C17 119.88(16) ?
C14 C13 C12 120.47(17) ?
C14 C13 H13 119.8 ?
C12 C13 H13 119.8 ?
C13 C14 C15 120.02(17) ?
C13 C14 H14 120.0 ?
C15 C14 H14 120.0 ?
C14 C15 C16 120.21(17) ?
C14 C15 H15 119.9 ?
C16 C15 H15 119.9 ?
C15 C16 C11 119.49(16) ?
C15 C16 C19 120.15(15) ?
C11 C16 C19 120.26(14) ?
O1 C17 C12 107.88(13) ?
O1 C17 H17A 110.1 ?
C12 C17 H17A 110.1 ?
O1 C17 H17B 110.1 ?
C12 C17 H17B 110.1 ?
H17A C17 H17B 108.4 ?
O1 C18 H18A 109.5 ?
O1 C18 H18B 109.5 ?
H18A C18 H18B 109.5 ?
O1 C18 H18C 109.5 ?
H18A C18 H18C 109.5 ?
H18B C18 H18C 109.5 ?
O2 C19 C16 106.47(13) ?
O2 C19 H19A 110.4 ?
C16 C19 H19A 110.4 ?
O2 C19 H19B 110.4 ?
C16 C19 H19B 110.4 ?
H19A C19 H19B 108.6 ?
O2 C20 H20A 109.5 ?
O2 C20 H20B 109.5 ?
H20A C20 H20B 109.5 ?
O2 C20 H20C 109.5 ?
H20A C20 H20C 109.5 ?
H20B C20 H20C 109.5 ?
C22 C21 C26 119.35(16) ?
C22 C21 Sn1 118.98(13) ?
C26 C21 Sn1 121.60(13) ?
C21 C22 C23 119.58(18) ?
C21 C22 H22 120.2 ?
C23 C22 H22 120.2 ?
C24 C23 C22 120.23(19) ?
C24 C23 H23 119.9 ?
C22 C23 H23 119.9 ?
C23 C24 C25 120.70(19) ?
C23 C24 H24 119.6 ?
C25 C24 H24 119.6 ?
C24 C25 C26 119.4(2) ?
C24 C25 H25 120.3 ?
C26 C25 H25 120.3 ?
C25 C26 C21 120.72(18) ?
C25 C26 H26 119.6 ?
C21 C26 H26 119.6 ?
C17 O1 C18 110.99(14) ?
C17 O1 Sn1 102.85(9) ?
C18 O1 Sn1 124.90(11) ?
C20 O2 C19 111.64(14) ?
C20 O2 Sn1 125.61(11) ?
C19 O2 Sn1 102.11(9) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Sn1 C11 2.1166(15) y
Sn1 C21 2.1214(16) y
Sn1 Cl1 2.3947(4) y
Sn1 Cl2 2.3983(4) y
Sn1 O1 2.6185(12) y
Sn1 O2 2.6554(13) y
C11 C12 1.394(2) ?
C11 C16 1.399(2) ?
C12 C13 1.398(2) ?
C12 C17 1.502(2) ?
C13 C14 1.383(3) ?
C13 H13 0.9300 ?
C14 C15 1.388(3) ?
C14 H14 0.9300 ?
C15 C16 1.396(2) ?
C15 H15 0.9300 ?
C16 C19 1.499(2) ?
C17 O1 1.438(2) ?
C17 H17A 0.9700 ?
C17 H17B 0.9700 ?
C18 O1 1.439(2) ?
C18 H18A 0.9600 ?
C18 H18B 0.9600 ?
C18 H18C 0.9600 ?
C19 O2 1.436(2) ?
C19 H19A 0.9700 ?
C19 H19B 0.9700 ?
C20 O2 1.435(2) ?
C20 H20A 0.9600 ?
C20 H20B 0.9600 ?
C20 H20C 0.9600 ?
C21 C22 1.394(2) ?
C21 C26 1.394(3) ?
C22 C23 1.399(3) ?
C22 H22 0.9300 ?
C23 C24 1.376(3) ?
C23 H23 0.9300 ?
C24 C25 1.384(3) ?
C24 H24 0.9300 ?
C25 C26 1.388(3) ?
C25 H25 0.9300 ?
C26 H26 0.9300 ?
