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#$Date: 2016-03-22 11:06:59 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178885 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/14/4111487.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_4111487
loop_
_publ_author_name
'Reyes García-Zarracino'
'Herbert Höpfl'
_publ_contact_author_address
;
     Centro de Inverstigaciones Químicas
     Universidad Autónoma del Estado de Morelos
     Av. Universidad 1001, C.P. 62210 Cuernavaca
     México
;
_publ_contact_author_email       hhopfl@buzon.uaem.mx
_publ_contact_author_fax         '+52 777-329-7997'
_publ_contact_author_name        'Herbert Höpfl'
_publ_contact_author_phone       '+52 777-329-7997'
_publ_section_title
;
 Self-Assembly of Diorganotin(IV) Oxides (R = Me,nBu, Ph) and
 2,5-Pyridinedicarboxylic Acid to Polymeric and Trinuclear Macrocyclic
 Hybrids with Porous Solid-State Structures: Influence of Substituents and
 Solvent on the Supramolecular Structure
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3120
_journal_page_last               3130
_journal_paper_doi               10.1021/ja0437095
_journal_volume                  127
_journal_year                    2005
_chemical_formula_moiety         'C51 H81 N3 O15 S3 Sn3, 3(C2 H6 O S)'
_chemical_formula_sum            'C57 H99 N3 O18 S6 Sn3'
_chemical_formula_weight         1662.82
_chemical_melting_point          579(1)
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           176
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-P 6c'
_symmetry_space_group_name_H-M   'P 63/m'
_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            2
_cell_length_a                   16.214(14)
_cell_length_b                   16.214(14)
_cell_length_c                   17.23(2)
_cell_measurement_reflns_used    6698
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      50.8
_cell_measurement_theta_min      4.7
_cell_volume                     3923(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0995
_diffrn_reflns_av_sigmaI/netI    0.0488
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            40873
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.45
_exptl_absorpt_coefficient_mu    1.167
_exptl_absorpt_correction_T_max  0.880
_exptl_absorpt_correction_T_min  0.695
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.408
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             1704
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.510
_refine_diff_density_min         -0.906
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         2658
_refine_ls_number_restraints     152
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0944
_refine_ls_R_factor_gt           0.0611
_refine_ls_shift/su_max          0.759
_refine_ls_shift/su_mean         0.061
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0998P)²+8.0198P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1782
_refine_ls_wR_factor_ref         0.2012
_reflns_number_gt                1762
_reflns_number_total             2658
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0437095si20041202_030437_3.cif
_cod_data_source_block           reyevzwm
_cod_database_code               4111487
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z-1/2'
'-y, x-y, -z-1/2'
'-x+y, -x, -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
Sn1 Sn 0.25940(4) -0.07497(4) 0.7500 0.0604(3) Uani 1 2 d S
S1 S 0.3930(2) -0.1965(2) 0.7500 0.131(2) Uani 1 2 d SU
N1 N 0.2920(5) 0.0862(5) 0.7500 0.056(2) Uani 1 2 d SU
O1 O 0.4137(4) 0.0179(4) 0.7500 0.066(2) Uani 1 2 d SU
O2 O 0.5386(5) 0.1623(5) 0.7500 0.099(3) Uani 1 2 d SU
O4 O 0.1011(5) 0.1881(5) 0.7500 0.077(2) Uani 1 2 d SU
O3 O 0.2206(5) 0.3361(4) 0.7500 0.084(3) Uani 1 2 d SU
O5 O 0.3048(5) -0.1845(5) 0.7500 0.144(5) Uani 1 2 d SU
C1 C 0.2312(6) 0.1180(6) 0.7500 0.056(3) Uani 1 2 d SU
H1 H 0.1662 0.0743 0.7500 0.068 Uiso 1 2 calc SR
C2 C 0.2608(6) 0.2141(6) 0.7500 0.055(2) Uani 1 2 d SU
C3 C 0.3569(7) 0.2788(6) 0.7500 0.064(3) Uani 1 2 d SU
H3 H 0.3782 0.3437 0.7500 0.077 Uiso 1 2 calc SR
C4 C 0.4221(7) 0.2468(6) 0.7500 0.064(3) Uani 1 2 d SU
H4 H 0.4872 0.2900 0.7500 0.076 Uiso 1 2 calc SR
C5 C 0.3895(6) 0.1517(6) 0.7500 0.057(3) Uani 1 2 d SU
C6 C 0.4560(6) 0.1117(7) 0.7500 0.062(3) Uani 1 2 d SU
C7 C 0.1880(7) 0.2462(6) 0.7500 0.065(3) Uani 1 2 d SU
C8 C 0.2462(8) -0.0815(8) 0.6270(7) 0.114(4) Uani 1 1 d DU
H8A H 0.2442 -0.1396 0.6104 0.137 Uiso 1 1 calc R
H8B H 0.1847 -0.0884 0.6147 0.137 Uiso 1 1 calc R
C9 C 0.3188(11) -0.0022(10) 0.5776(9) 0.189(7) Uani 1 1 d DU
H9A H 0.3816 0.0071 0.5884 0.227 Uiso 1 1 calc R
H9B H 0.3194 0.0565 0.5897 0.227 Uiso 1 1 calc R
C10 C 0.2951(18) -0.026(2) 0.4913(9) 0.236(9) Uani 1 1 d DU
H10A H 0.2366 -0.0868 0.4860 0.283 Uiso 1 1 calc R
H10B H 0.2864 0.0225 0.4664 0.283 Uiso 1 1 calc R
C11 C 0.376(2) -0.032(3) 0.4536(18) 0.48(3) Uani 1 1 d DU
H11A H 0.4123 0.0237 0.4219 0.713 Uiso 1 1 calc R
H11B H 0.3512 -0.0877 0.4219 0.713 Uiso 1 1 calc R
H11C H 0.4167 -0.0343 0.4930 0.713 Uiso 1 1 calc R
C12 C 0.4657(7) -0.1300(8) 0.8271(7) 0.116(4) Uani 1 1 d .
H12A H 0.4866 -0.0638 0.8190 0.174 Uiso 1 1 calc R
H12B H 0.5200 -0.1387 0.8299 0.174 Uiso 1 1 calc R
H12C H 0.4304 -0.1509 0.8747 0.174 Uiso 1 1 calc R
S100 S 0.4109(15) 0.7326(19) 0.0512(14) 0.42(2) Uani 0.33 1 d PDU
O100 O 0.405(5) 0.8225(14) 0.052(2) 0.52(4) Uani 0.33 1 d PDU
C100 C 0.3333 0.6667 -0.0262(16) 0.37(3) Uani 1 3 d SD
C101 C 0.3333 0.6667 0.1287(15) 0.37(3) Uani 1 3 d SD
S200 S 0.089(4) 0.000(6) 0.470(3) 0.33(3) Uani 0.17 1 d PDU
O200 O 0.065(9) 0.023(16) 0.549(3) 0.32(4) Uani 0.17 1 d PDU
C200 C 0.0000 0.0000 0.408(4) 0.52(6) Uani 1 3 d SDU
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'
N N 0.0061 0.0033 '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'
S S 0.1246 0.1234 '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
C8 Sn1 C8 170.0(6) . 10_557
C8 Sn1 O1 94.9(3) . .
C8 Sn1 O1 94.9(3) 10_557 .
C8 Sn1 O5 91.5(3) . .
C8 Sn1 O5 91.5(3) 10_557 .
O1 Sn1 O5 80.1(2) . .
C8 Sn1 O3 85.7(3) . 3
C8 Sn1 O3 85.7(3) 10_557 3
O1 Sn1 O3 156.1(2) . 3
O5 Sn1 O3 76.0(3) . 3
C8 Sn1 N1 90.9(3) . .
C8 Sn1 N1 90.9(3) 10_557 .
O1 Sn1 N1 72.3(2) . .
O5 Sn1 N1 152.4(3) . .
O3 Sn1 N1 131.6(2) 3 .
O5 S1 C12 107.8(4) . .
O5 S1 C12 107.8(4) . 10_557
C12 S1 C12 99.1(7) . 10_557
C1 N1 C5 119.0(7) . .
C1 N1 Sn1 128.7(6) . .
C5 N1 Sn1 112.2(5) . .
C6 O1 Sn1 123.4(5) . .
C7 O3 Sn1 98.5(5) . 2
S1 O5 Sn1 142.8(5) . .
N1 C1 C2 122.2(8) . .
C3 C2 C1 118.8(8) . .
C3 C2 C7 121.3(8) . .
C1 C2 C7 119.8(8) . .
C2 C3 C4 119.9(8) . .
C5 C4 C3 119.1(9) . .
C4 C5 N1 120.9(8) . .
C4 C5 C6 122.1(8) . .
N1 C5 C6 117.0(7) . .
O2 C6 O1 124.1(8) . .
O2 C6 C5 120.8(9) . .
O1 C6 C5 115.1(7) . .
O4 C7 O3 122.0(8) . .
O4 C7 C2 121.6(8) . .
O3 C7 C2 116.4(8) . .
C9 C8 Sn1 120.5(9) . .
C8 C9 C10 110.1(12) . .
C11 C10 C9 108.5(13) . .
O100 S100 C100 102.7(13) . .
O100 S100 C101 101.9(13) . .
C100 S100 C101 97.3(11) . .
O200 S200 C200 103.5(13) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Sn1 C8 2.127(13) .
Sn1 C8 2.127(13) 10_557
Sn1 O1 2.182(6) .
Sn1 O5 2.237(7) .
Sn1 O3 2.347(7) 3
Sn1 N1 2.393(7) .
S1 O5 1.537(8) .
S1 C12 1.745(13) .
S1 C12 1.745(13) 10_557
N1 C1 1.322(11) .
N1 C5 1.396(11) .
O1 C6 1.320(11) .
O2 C6 1.170(11) .
O4 C7 1.243(11) .
O3 C7 1.278(11) .
O3 Sn1 2.347(7) 2
C1 C2 1.382(12) .
C2 C3 1.375(13) .
C2 C7 1.509(12) .
C3 C4 1.391(13) .
C4 C5 1.357(12) .
C5 C6 1.510(12) .
C8 C9 1.500(9) .
C9 C10 1.535(10) .
C10 C11 1.508(10) .
S100 O100 1.509(10) .
S100 C100 1.777(10) .
S100 C101 1.779(10) .
S100 S100 2.03(3) 3_565
S100 S100 2.03(3) 2_665
C100 S100 1.777(10) 2_665
C100 S100 1.777(10) 3_565
C101 S100 1.779(10) 2_665
C101 S100 1.779(10) 3_565
S200 O200 1.0(2) 8_556
S200 O200 1.501(11) .
S200 O200 1.6(2) 9_556
S200 S200 1.76(8) 8_556
S200 S200 1.76(8) 9_556
S200 C200 1.794(10) .
S200 S200 2.49(7) 3
S200 S200 2.49(7) 2
O200 S200 1.0(2) 9_556
O200 C200 1.19(10) 7_556
O200 O200 1.60(19) 3
O200 O200 1.60(19) 2
O200 S200 1.6(2) 8_556
C200 O200 1.19(10) 8_556
C200 O200 1.19(10) 9_556
C200 O200 1.19(10) 7_556
C200 S200 1.794(10) 3
C200 S200 1.794(10) 2
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
C8 Sn1 N1 C1 85.1(3) .
C8 Sn1 N1 C1 -85.1(3) 10_557
O1 Sn1 N1 C1 180.0 .
O5 Sn1 N1 C1 180.0 .
O3 Sn1 N1 C1 0.0 3
C8 Sn1 N1 C5 -94.9(3) .
C8 Sn1 N1 C5 94.9(3) 10_557
O1 Sn1 N1 C5 0.0 .
O5 Sn1 N1 C5 0.0 .
O3 Sn1 N1 C5 180.0 3
C8 Sn1 O1 C6 89.4(3) .
C8 Sn1 O1 C6 -89.4(3) 10_557
O5 Sn1 O1 C6 180.0 .
O3 Sn1 O1 C6 180.0 3
N1 Sn1 O1 C6 0.0 .
C12 S1 O5 Sn1 53.1(4) .
C12 S1 O5 Sn1 -53.1(4) 10_557
C8 Sn1 O5 S1 94.8(3) .
C8 Sn1 O5 S1 -94.8(3) 10_557
O1 Sn1 O5 S1 0.0 .
O3 Sn1 O5 S1 180.0 3
N1 Sn1 O5 S1 0.0 .
C5 N1 C1 C2 0.0 .
Sn1 N1 C1 C2 180.0 .
N1 C1 C2 C3 0.0 .
N1 C1 C2 C7 180.0 .
C1 C2 C3 C4 0.0 .
C7 C2 C3 C4 180.0 .
C2 C3 C4 C5 0.0 .
C3 C4 C5 N1 0.0 .
C3 C4 C5 C6 180.0 .
C1 N1 C5 C4 0.0 .
Sn1 N1 C5 C4 180.0 .
C1 N1 C5 C6 180.0 .
Sn1 N1 C5 C6 0.0 .
Sn1 O1 C6 O2 180.0 .
Sn1 O1 C6 C5 0.0 .
C4 C5 C6 O2 0.0 .
N1 C5 C6 O2 180.0 .
C4 C5 C6 O1 180.0 .
N1 C5 C6 O1 0.0 .
Sn1 O3 C7 O4 0.0 2
Sn1 O3 C7 C2 180.0 2
C3 C2 C7 O4 180.0 .
C1 C2 C7 O4 0.0 .
C3 C2 C7 O3 0.0 .
C1 C2 C7 O3 180.0 .
C8 Sn1 C8 C9 147(3) 10_557
O1 Sn1 C8 C9 -25.9(11) .
O5 Sn1 C8 C9 -106.1(11) .
O3 Sn1 C8 C9 178.1(11) 3
N1 Sn1 C8 C9 46.4(11) .
Sn1 C8 C9 C10 177.7(11) .
C8 C9 C10 C11 -118(3) .
