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
Reyes García-Zarracino; Herbert Höpfl; Journal of the American Chemical Society 127 (2005) 3120–3130; doi:10.1021/ja0437095

data_4111489
_publ_contact_author_address
;
     Centro de Inverstigaciones Qu\'imicas
     Universidad Aut\'onoma del Estado de Morelos
     Av. Universidad 1001, C.P. 62210 Cuernavaca
     M\'exico
;
_publ_contact_author_email       hhopfl@buzon.uaem.mx
_publ_contact_author_fax         '+52 777-329-7997'
_publ_contact_author_name        'Herbert H\"opfl'
_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         'C63 H57 N3 O15 S3 Sn3, 5(C2 H6 O S)'
_chemical_formula_sum            'C73 H87 N3 O20 S8 Sn3'
_chemical_formula_weight         1939.01
_chemical_melting_point          573
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                102.151(3)
_cell_angle_beta                 104.815(4)
_cell_angle_gamma                119.645(3)
_cell_formula_units_Z            2
_cell_length_a                   17.878(3)
_cell_length_b                   17.958(3)
_cell_length_c                   18.053(3)
_cell_measurement_reflns_used    2645
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      35.2
_cell_measurement_theta_min      4.5
_cell_volume                     4461.1(13)
_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      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.1170
_diffrn_reflns_av_sigmaI/netI    0.1893
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            46940
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.27
_exptl_absorpt_coefficient_mu    1.084
_exptl_absorpt_correction_T_max  0.878
_exptl_absorpt_correction_T_min  0.764
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.444
_exptl_crystal_description       rectangular
_exptl_crystal_F_000             1968
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.118
_refine_diff_density_min         -0.747
_refine_diff_density_rms         0.154
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.963
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     862
_refine_ls_number_reflns         17452
_refine_ls_number_restraints     199
_refine_ls_restrained_S_all      0.960
_refine_ls_R_factor_all          0.2035
_refine_ls_R_factor_gt           0.0904
_refine_ls_shift/su_max          3.401
_refine_ls_shift/su_mean         0.047
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1207P)^2^+25.0244P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2316
_refine_ls_wR_factor_ref         0.2912
_reflns_number_gt                7604
_reflns_number_total             17452
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0437095si20041202_030437_5.cif
_cod_data_source_block           reyefivx
_cod_original_cell_volume        4460.9(14)
_cod_database_code               4111489