#------------------------------------------------------------------------------
#$Date: 2018-08-11 17:03:44 +0300 (Sat, 11 Aug 2018) $
#$Revision: 209571 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/03/05/7030547.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_7030547
loop_
_publ_author_name
'Hitchcock, Peter B.'
'Lappert, Michael F.'
'Protchenko, Andrey V.'
'Uiterweerd, Patrick G. H.'
_publ_section_title
;
 Synthesis and structures of halides and pseudohalides of
 bis[2,6-bis(dimethylamino)phenyl]tin(IV)
;
_journal_coden_ASTM              DTARAF
_journal_issue                   2
_journal_name_full               'Dalton Transactions'
_journal_page_first              353
_journal_page_last               361
_journal_paper_doi               10.1039/b813353k
_journal_year                    2009
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C20 H30 Cl2 N4 Sn'
_chemical_formula_sum            'C20 H30 Cl2 N4 Sn'
_chemical_formula_weight         516.07
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      33
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location
ftp://ftp.iucr.org/cifdics/cif_core_2.1beta5.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.1beta5
_audit_creation_date             2000-03-17T15:08:49-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.2558(4)
_cell_length_b                   17.2642(4)
_cell_length_c                   7.9120(2)
_cell_measurement_reflns_used    10750
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      30.034
_cell_measurement_theta_min      4.529
_cell_measurement_wavelength     0.71073
_cell_volume                     2220.45(9)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_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      173(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       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  0.0412
_diffrn_reflns_av_sigmaI/netI    0.037
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            18152
_diffrn_reflns_theta_full        30.04
_diffrn_reflns_theta_max         30.04
_diffrn_reflns_theta_min         4.56
_exptl_absorpt_coefficient_mu    1.404
_exptl_absorpt_correction_T_max  0.798
_exptl_absorpt_correction_T_min  0.711
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.544
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1048
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.444
_refine_diff_density_min         -0.616
_refine_diff_density_rms         0.069
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.06(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         5153
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0347
_refine_ls_R_factor_gt           0.0285
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0300P)²+1.4495P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.067
_refine_ls_wR_factor_ref         0.0702
_reflns_number_gt                4572
_reflns_number_total             5153
_reflns_threshold_expression     >2sigma(I)
_cod_duplicate_entry             7000261
_cod_data_source_file            b813353k.txt
_cod_data_source_block           (4)-mar2900
_cod_original_sg_symbol_H-M      Pna21
_cod_database_code               7030547
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x+1/2, y+1/2, z+1/2'
'x+1/2, -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
Sn Sn 0.250947(10) 0.411603(9) 0.26433(7) 0.01861(5) Uani 1 1 d .
Cl1 Cl 0.23272(5) 0.53126(5) 0.11161(10) 0.02945(15) Uani 1 1 d .
Cl2 Cl 0.21403(5) 0.33840(5) 0.01957(10) 0.03200(16) Uani 1 1 d .
N1 N 0.25198(14) 0.28323(16) 0.4306(4) 0.0261(6) Uani 1 1 d .
N2 N 0.04995(16) 0.48919(18) 0.4137(4) 0.0328(6) Uani 1 1 d .
N3 N 0.31644(13) 0.50928(13) 0.5053(3) 0.0218(5) Uani 1 1 d .
N4 N 0.43194(15) 0.31300(14) 0.1381(3) 0.0249(5) Uani 1 1 d .
C1 C 0.15155(17) 0.38362(18) 0.4302(4) 0.0232(6) Uani 1 1 d .
C2 C 0.17250(19) 0.31091(18) 0.4895(4) 0.0262(6) Uani 1 1 d .
C3 C 0.1206(2) 0.2678(2) 0.5934(4) 0.0385(8) Uani 1 1 d .
H3 H 0.1376 0.2195 0.6392 0.046 Uiso 1 1 calc R
C4 C 0.0436(2) 0.2975(2) 0.6275(5) 0.0426(9) Uani 1 1 d .
H4 H 0.0061 0.2683 0.6937 0.051 Uiso 1 1 calc R
C5 C 0.0205(2) 0.3690(2) 0.5672(4) 0.0379(8) Uani 1 1 d .
H5 H -0.0333 0.3875 0.5914 0.045 Uiso 1 1 calc R
C6 C 0.07346(19) 0.41531(18) 0.4716(4) 0.0272(7) Uani 1 1 d .
C7 C 0.2459(2) 0.2098(2) 0.3346(6) 0.0368(8) Uani 1 1 d .
H7A H 0.3009 0.1936 0.2985 0.055 Uiso 1 1 calc R
H7B H 0.211 0.2176 0.2351 0.055 Uiso 1 1 calc R
H7C H 0.2218 0.1697 0.4068 0.055 Uiso 1 1 calc R
C8 C 0.3117(2) 0.2739(2) 0.5681(5) 0.0399(9) Uani 1 1 d .
H8A H 0.3639 0.255 0.522 0.06 Uiso 1 1 calc R
H8B H 0.2905 0.2365 0.6505 0.06 Uiso 1 1 calc R
H8C H 0.3205 0.3239 0.6238 0.06 Uiso 1 1 calc R
C9 C 0.1047(2) 0.5526(2) 0.4560(5) 0.0344(7) Uani 1 1 d .
H9A H 0.0824 0.601 0.4106 0.052 Uiso 1 1 calc R
H9B H 0.159 0.5429 0.407 0.052 Uiso 1 1 calc R
H9C H 0.1095 0.5566 0.5792 0.052 Uiso 1 1 calc R
C10 C -0.0358(2) 0.5115(3) 0.4416(5) 0.0517(12) Uani 1 1 d .
H10A H -0.045 0.5638 0.3974 0.078 Uiso 1 1 calc R
H10B H -0.0478 0.5106 0.563 0.078 Uiso 1 1 calc R
H10C H -0.0721 0.4749 0.3831 0.078 Uiso 1 1 calc R
C11 C 0.37873(16) 0.41444(15) 0.3240(4) 0.0183(5) Uani 1 1 d .
C12 C 0.38877(16) 0.46397(16) 0.4611(4) 0.0200(5) Uani 1 1 d .
C13 C 0.46230(17) 0.46734(17) 0.5513(4) 0.0252(6) Uani 1 1 d .
H13 H 0.4687 0.5018 0.644 0.03 Uiso 1 1 calc R
C14 C 0.52547(18) 0.41917(17) 0.5020(4) 0.0270(6) Uani 1 1 d .
H14 H 0.5761 0.4206 0.562 0.032 Uiso 1 1 calc R
C15 C 0.51679(17) 0.36852(17) 0.3663(4) 0.0220(6) Uani 1 1 d .
H15 H 0.5612 0.3356 0.3357 0.026 Uiso 1 1 calc R
C16 C 0.44366(15) 0.36563(15) 0.2749(4) 0.0203(5) Uani 1 1 d .
C17 C 0.2921(2) 0.5003(2) 0.6842(4) 0.0310(7) Uani 1 1 d .
H17A H 0.2431 0.5317 0.7066 0.046 Uiso 1 1 calc R
H17B H 0.3371 0.5175 0.7573 0.046 Uiso 1 1 calc R
H17C H 0.2798 0.4457 0.7072 0.046 Uiso 1 1 calc R
C18 C 0.3304(2) 0.59189(16) 0.4671(5) 0.0289(7) Uani 1 1 d .
H18A H 0.2813 0.6218 0.4973 0.043 Uiso 1 1 calc R
H18B H 0.3416 0.598 0.3461 0.043 Uiso 1 1 calc R
H18C H 0.3775 0.6108 0.5324 0.043 Uiso 1 1 calc R
C19 C 0.4897(2) 0.24780(17) 0.1305(6) 0.0368(8) Uani 1 1 d .
H19A H 0.4763 0.215 0.0331 0.055 Uiso 1 1 calc R
H19B H 0.4854 0.2172 0.2345 0.055 Uiso 1 1 calc R
H19C H 0.5459 0.2676 0.1187 0.055 Uiso 1 1 calc R
C20 C 0.4212(2) 0.3484(2) -0.0264(4) 0.0323(7) Uani 1 1 d .
H20A H 0.4133 0.3079 -0.1117 0.048 Uiso 1 1 calc R
H20B H 0.4701 0.379 -0.0546 0.048 Uiso 1 1 calc R
H20C H 0.3729 0.3823 -0.0243 0.048 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'
N N 0.0061 0.0033 '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
C11 Sn C1 127.31(11)
C11 Sn Cl2 115.89(8)
C1 Sn Cl2 100.85(8)
C11 Sn Cl1 102.19(7)
C1 Sn Cl1 114.11(9)
Cl2 Sn Cl1 90.93(3)
C11 Sn N1 84.28(9)
C1 Sn N1 59.81(10)
Cl2 Sn N1 87.73(7)
Cl1 Sn N1 173.30(5)
C2 N1 C8 112.7(3)
C2 N1 C7 112.7(2)
C8 N1 C7 109.3(3)
C2 N1 Sn 82.84(17)
C8 N1 Sn 118.5(2)
C7 N1 Sn 118.3(3)
C6 N2 C9 116.2(3)
C6 N2 C10 116.6(3)
C9 N2 C10 110.6(3)
C12 N3 C18 110.3(2)
C12 N3 C17 113.0(2)
C18 N3 C17 109.8(2)
C16 N4 C20 115.4(2)
C16 N4 C19 115.8(2)
C20 N4 C19 111.3(3)
C2 C1 C6 119.4(3)
C2 C1 Sn 103.1(2)
C6 C1 Sn 136.9(2)
C1 C2 C3 122.4(3)
C1 C2 N1 114.1(3)
C3 C2 N1 123.5(3)
C4 C3 C2 117.7(3)
C5 C4 C3 121.0(3)
C4 C5 C6 122.1(3)
C5 C6 N2 121.8(3)
C5 C6 C1 117.1(3)
N2 C6 C1 121.1(3)
C12 C11 C16 119.7(3)
C12 C11 Sn 107.54(19)
C16 C11 Sn 131.1(2)
C11 C12 C13 121.7(3)
C11 C12 N3 115.0(2)
C13 C12 N3 123.2(3)
C14 C13 C12 118.0(3)
C13 C14 C15 121.5(3)
C16 C15 C14 120.6(3)
C15 C16 C11 118.5(3)
C15 C16 N4 122.1(2)
C11 C16 N4 119.4(2)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Sn C11 2.131(3)
Sn C1 2.137(3)
Sn Cl2 2.3890(9)
Sn Cl1 2.4115(8)
Sn N1 2.577(3)
N1 C2 1.454(4)
N1 C8 1.467(4)
N1 C7 1.480(5)
N2 C6 1.408(4)
N2 C9 1.449(5)
N2 C10 1.463(4)
N3 C12 1.455(3)
N3 C18 1.475(4)
N3 C17 1.478(4)
N4 C16 1.426(4)
N4 C20 1.449(4)
N4 C19 1.467(4)
C1 C2 1.383(4)
C1 C6 1.421(4)
C2 C3 1.394(4)
C3 C4 1.379(6)
C4 C5 1.376(6)
C5 C6 1.397(4)
C11 C12 1.391(4)
C11 C16 1.405(4)
C12 C13 1.393(4)
C13 C14 1.378(4)
C14 C15 1.392(4)
C15 C16 1.392(4)
