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#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/14/4111488.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_4111488
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         'C54 H96 N3 O19.50 Sn3'
_chemical_formula_sum            'C54 H96 N3 O19.5 Sn3'
_chemical_formula_weight         1455.41
_chemical_melting_point          573
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           197
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  'I 2 2 3'
_symmetry_space_group_name_H-M   'I 2 3'
_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                90.00
_cell_formula_units_Z            8
_cell_length_a                   25.1483(10)
_cell_length_b                   25.1483(10)
_cell_length_c                   25.1483(10)
_cell_measurement_reflns_used    8923
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      55.0
_cell_measurement_theta_min      4.6
_cell_volume                     15904.7(11)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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      100(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  0.0712
_diffrn_reflns_av_sigmaI/netI    0.0444
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            40446
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         1.15
_exptl_absorpt_coefficient_mu    0.991
_exptl_absorpt_correction_T_max  0.853
_exptl_absorpt_correction_T_min  0.563
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.216
_exptl_crystal_description       cube
_exptl_crystal_F_000             5976
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.692
_refine_diff_density_min         -1.189
_refine_diff_density_rms         0.268
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.06(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.280
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     215
_refine_ls_number_reflns         4960
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.279
_refine_ls_R_factor_all          0.0930
_refine_ls_R_factor_gt           0.0916
_refine_ls_shift/su_max          1.080
_refine_ls_shift/su_mean         0.016
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1119P)²+254.8190P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2275
_refine_ls_wR_factor_ref         0.2285
_reflns_number_gt                4859
_reflns_number_total             4960
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0437095si20041202_030437_4.cif
_cod_data_source_block           zgarsixm
_cod_original_formula_sum        'C54 H96 N3 O19.50 Sn3'
_cod_database_code               4111488
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-x, y, -z'
'x, -y, -z'
'z, x, y'
'z, -x, -y'
'-z, -x, y'
'-z, x, -y'
'y, z, x'
'-y, z, -x'
'y, -z, -x'
'-y, -z, x'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'z+1/2, x+1/2, y+1/2'
'z+1/2, -x+1/2, -y+1/2'
'-z+1/2, -x+1/2, y+1/2'
'-z+1/2, x+1/2, -y+1/2'
'y+1/2, z+1/2, x+1/2'
'-y+1/2, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x+1/2'
'-y+1/2, -z+1/2, x+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 0.62849(3) 0.72251(3) 0.89638(3) 0.0201(2) Uani 1 1 d .
N1 N 0.7017(4) 0.6642(4) 0.8842(4) 0.026(2) Uani 1 1 d .
O1 O 0.6289(4) 0.6623(3) 0.9611(3) 0.0291(15) Uani 1 1 d .
O2 O 0.6651(3) 0.5893(3) 0.9971(3) 0.0165(16) Uani 1 1 d .
O3 O 0.5926(3) 0.7924(3) 0.8508(3) 0.0291(15) Uani 1 1 d .
O4 O 0.6684(5) 0.7640(4) 0.8166(5) 0.051(3) Uani 1 1 d .
O5 O 0.5565(3) 0.7469(3) 0.9467(3) 0.0177(16) Uani 1 1 d .
C1 C 0.7381(6) 0.6655(5) 0.8441(6) 0.036(3) Uani 1 1 d .
H1 H 0.7376 0.6944 0.8198 0.043 Uiso 1 1 calc R
C2 C 0.7768(5) 0.6252(6) 0.8375(5) 0.034(3) Uani 1 1 d .
C3 C 0.7774(5) 0.5843(5) 0.8746(4) 0.0241(18) Uani 1 1 d .
H3 H 0.8035 0.5571 0.8722 0.029 Uiso 1 1 calc R
C4 C 0.7407(5) 0.5829(5) 0.9144(5) 0.0241(18) Uani 1 1 d .
H4 H 0.7410 0.5546 0.9394 0.029 Uiso 1 1 calc R
C5 C 0.7030(5) 0.6229(5) 0.9184(5) 0.024(3) Uani 1 1 d .
C6 C 0.6628(4) 0.6256(5) 0.9633(4) 0.021(2) Uani 1 1 d .
C7 C 0.6286(6) 0.7962(5) 0.8167(6) 0.035(3) Uani 1 1 d .
C8 C 0.6762(5) 0.7767(7) 0.9412(9) 0.079(8) Uani 1 1 d D
H8A H 0.6892 0.8034 0.9154 0.095 Uiso 1 1 calc R
H8B H 0.6513 0.7957 0.9650 0.095 Uiso 1 1 calc R
C9 C 0.7245(8) 0.7621(6) 0.9758(9) 0.103(7) Uani 1 1 d D
H9A H 0.7132 0.7402 1.0066 0.124 Uiso 1 1 calc R
H9B H 0.7507 0.7415 0.9548 0.124 Uiso 1 1 calc R
C10 C 0.7494(8) 0.8146(8) 0.9951(7) 0.113(8) Uani 1 1 d D
H10A H 0.7875 0.8161 0.9853 0.136 Uiso 1 1 calc R
H10B H 0.7310 0.8452 0.9786 0.136 Uiso 1 1 calc R
C11 C 0.7432(13) 0.8164(13) 1.0560(8) 0.125(9) Uani 1 1 d D
H11A H 0.7262 0.7836 1.0684 0.188 Uiso 1 1 calc R
H11B H 0.7211 0.8470 1.0659 0.188 Uiso 1 1 calc R
H11C H 0.7783 0.8199 1.0726 0.188 Uiso 1 1 calc R
C12 C 0.5844(6) 0.6695(5) 0.8464(5) 0.028(3) Uani 1 1 d .
H12A H 0.5997 0.6718 0.8102 0.034 Uiso 1 1 calc R
H12B H 0.5906 0.6329 0.8594 0.034 Uiso 1 1 calc R
C13 C 0.5268(10) 0.6771(12) 0.8417(12) 0.103(7) Uani 1 1 d .
H13A H 0.5200 0.7141 0.8300 0.124 Uiso 1 1 calc R
H13B H 0.5107 0.6728 0.8773 0.124 Uiso 1 1 calc R
C14 C 0.4987(13) 0.6397(11) 0.8036(12) 0.113(8) Uani 1 1 d .
H14A H 0.5144 0.6444 0.7678 0.136 Uiso 1 1 calc R
H14B H 0.5061 0.6027 0.8149 0.136 Uiso 1 1 calc R
C15 C 0.4393(12) 0.6466(14) 0.7992(13) 0.125(9) Uani 1 1 d .
H15A H 0.4305 0.6845 0.8016 0.188 Uiso 1 1 calc R
H15B H 0.4219 0.6273 0.8283 0.188 Uiso 1 1 calc R
H15C H 0.4271 0.6324 0.7651 0.188 Uiso 1 1 calc R
O11 O 0.5000 0.6723(4) 0.0000 0.021(2) Uani 1 2 d S
O21 O 0.4316(4) 0.6051(4) 0.9493(4) 0.039(2) Uani 1 1 d D
H21 H 0.4056 0.6017 0.9700 0.059 Uiso 1 1 calc R
C21 C 0.4488(6) 0.5528(5) 0.9310(9) 0.078(7) Uani 1 1 d D
H21A H 0.4615 0.5311 0.9613 0.094 Uiso 1 1 calc R
H21B H 0.4780 0.5562 0.9049 0.094 Uiso 1 1 calc R
C22 C 0.3998(9) 0.5267(10) 0.9051(12) 0.117(11) Uani 1 1 d D
H22A H 0.3825 0.5525 0.8809 0.140 Uiso 1 1 calc R
H22B H 0.3739 0.5168 0.9330 0.140 Uiso 1 1 calc R
C23 C 0.4159(12) 0.4767(9) 0.8736(15) 0.18(2) Uani 1 1 d D
H23A H 0.4397 0.4869 0.8444 0.269 Uiso 1 1 calc R
H23B H 0.3841 0.4597 0.8590 0.269 Uiso 1 1 calc R
H23C H 0.4343 0.4518 0.8972 0.269 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 0.0000 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'
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_3
C8 Sn1 C12 175.7(7) .
C8 Sn1 O1 92.6(6) .
C12 Sn1 O1 90.5(4) .
C8 Sn1 O3 89.7(6) .
C12 Sn1 O3 88.8(4) .
O1 Sn1 O3 153.3(3) .
C8 Sn1 O5 88.9(5) .
C12 Sn1 O5 94.7(4) .
O1 Sn1 O5 77.4(3) .
O3 Sn1 O5 76.1(3) .
C8 Sn1 N1 91.5(5) .
C12 Sn1 N1 86.7(5) .
O1 Sn1 N1 70.8(3) .
O3 Sn1 N1 135.8(3) .
O5 Sn1 N1 148.1(3) .
C8 Sn1 O4 86.0(7) .
C12 Sn1 O4 89.8(5) .
O1 Sn1 O4 151.6(3) .
O3 Sn1 O4 55.2(3) .
O5 Sn1 O4 130.9(3) .
N1 Sn1 O4 80.8(3) .
C5 N1 C1 118.3(10) .
C5 N1 Sn1 114.3(8) .
C1 N1 Sn1 127.1(8) .
C6 O1 Sn1 122.4(7) .
C7 O3 Sn1 96.7(8) .
C7 O4 Sn1 87.0(7) .
N1 C1 C2 122.2(11) .
C3 C2 C1 117.4(11) .
C3 C2 C7 121.3(12) 5
C1 C2 C7 121.2(12) 5
C4 C3 C2 120.3(11) .
C3 C4 C5 120.0(10) .
N1 C5 C4 121.8(11) .
N1 C5 C6 115.1(11) .
C4 C5 C6 122.9(10) .
O2 C6 O1 126.9(10) .
O2 C6 C5 116.2(10) .
O1 C6 C5 116.8(10) .
O3 C7 O4 121.1(11) .
O3 C7 C2 119.2(12) 9
O4 C7 C2 119.8(12) 9
C9 C8 Sn1 126.0(11) .
C10 C9 C8 107.0(6) .
C11 C10 C9 107.3(6) .
C13 C12 Sn1 118.6(12) .
C12 C13 C14 115(2) .
C15 C14 C13 116(2) .
O21 C21 C22 106.3(11) .
C21 C22 C23 111(2) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Sn1 C8 2.138(15) .
Sn1 C12 2.141(12) .
Sn1 O1 2.222(8) .
Sn1 O3 2.284(8) .
Sn1 O5 2.291(8) .
Sn1 N1 2.373(10) .
Sn1 O4 2.475(9) .
N1 C5 1.351(14) .
N1 C1 1.363(15) .
O1 C6 1.259(14) .
O2 C6 1.249(14) .
O3 C7 1.251(15) .
O4 C7 1.287(17) .
C1 C2 1.415(18) .
C2 C3 1.389(16) .
C2 C7 1.447(17) 5
C3 C4 1.362(16) .
C4 C5 1.387(17) .
C5 C6 1.517(15) .
C7 C2 1.447(17) 9
C8 C9 1.5399(10) .
C9 C10 1.5402(10) .
C10 C11 1.5400(10) .
C12 C13 1.47(3) .
C13 C14 1.52(3) .
C14 C15 1.51(4) .
O21 C21 1.4599(10) .
C21 C22 1.5399(10) .
C22 C23 1.5400(10) .
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
_geom_torsion_site_symmetry_4
C8 Sn1 N1 C5 98.2(11) . .
C12 Sn1 N1 C5 -85.8(10) . .
O1 Sn1 N1 C5 6.0(9) . .
O3 Sn1 N1 C5 -170.6(8) . .
O5 Sn1 N1 C5 7.8(14) . .
O4 Sn1 N1 C5 -176.1(10) . .
C8 Sn1 N1 C1 -88.7(14) . .
C12 Sn1 N1 C1 87.4(13) . .
O1 Sn1 N1 C1 179.1(13) . .
O3 Sn1 N1 C1 2.5(15) . .
O5 Sn1 N1 C1 -179.1(11) . .
O4 Sn1 N1 C1 -3.0(12) . .
C8 Sn1 O1 C6 -92.8(11) . .
C12 Sn1 O1 C6 84.2(10) . .
O3 Sn1 O1 C6 172.6(9) . .
O5 Sn1 O1 C6 178.9(11) . .
N1 Sn1 O1 C6 -2.1(10) . .
O4 Sn1 O1 C6 -6.3(16) . .
C8 Sn1 O3 C7 84.6(11) . .
C12 Sn1 O3 C7 -91.3(10) . .
O1 Sn1 O3 C7 179.9(9) . .
O5 Sn1 O3 C7 173.6(10) . .
N1 Sn1 O3 C7 -7.3(11) . .
O4 Sn1 O3 C7 -0.8(9) . .
C8 Sn1 O4 C7 -91.7(10) . .
C12 Sn1 O4 C7 89.5(10) . .
O1 Sn1 O4 C7 -179.9(9) . .
O3 Sn1 O4 C7 0.7(9) . .
O5 Sn1 O4 C7 -6.6(12) . .
N1 Sn1 O4 C7 176.1(10) . .
C5 N1 C1 C2 0(2) . .
Sn1 N1 C1 C2 -172.9(11) . .
N1 C1 C2 C3 -2(2) . .
N1 C1 C2 C7 -177.0(15) . 5
C1 C2 C3 C4 2(2) . .
C7 C2 C3 C4 177.4(14) 5 .
C2 C3 C4 C5 -1(2) . .
C1 N1 C5 C4 1(2) . .
Sn1 N1 C5 C4 175.1(9) . .
C1 N1 C5 C6 177.4(12) . .
Sn1 N1 C5 C6 -8.8(13) . .
C3 C4 C5 N1 -1(2) . .
C3 C4 C5 C6 -176.7(12) . .
Sn1 O1 C6 O2 -177.7(9) . .
Sn1 O1 C6 C5 -1.8(15) . .
N1 C5 C6 O2 -176.3(11) . .
C4 C5 C6 O2 -0.2(18) . .
N1 C5 C6 O1 7.4(17) . .
C4 C5 C6 O1 -176.6(12) . .
Sn1 O3 C7 O4 1.4(17) . .
Sn1 O3 C7 C2 -178.8(13) . 9
Sn1 O4 C7 O3 -1.3(15) . .
Sn1 O4 C7 C2 178.9(14) . 9
O1 Sn1 C8 C9 41.2(19) . .
O3 Sn1 C8 C9 -165.4(19) . .
O5 Sn1 C8 C9 118.5(19) . .
N1 Sn1 C8 C9 -29.6(19) . .
O4 Sn1 C8 C9 -110.3(19) . .
Sn1 C8 C9 C10 174.0(14) . .
C8 C9 C10 C11 115(2) . .
O1 Sn1 C12 C13 99.7(18) . .
O3 Sn1 C12 C13 -53.6(18) . .
O5 Sn1 C12 C13 22.3(18) . .
N1 Sn1 C12 C13 170.4(18) . .
O4 Sn1 C12 C13 -108.8(18) . .
Sn1 C12 C13 C14 177(2) . .
C12 C13 C14 C15 179(3) . .
O21 C21 C22 C23 168(2) . .
