First Example of a Hydrogen-Bonded Three-DimensionalPillaredStructure Involving an Organotin Motif: Synthesis and X-ray Crystal Structures of {[nBu2Sn(H2O)3(L)Sn(H2O)3nBu2]2+[L]2-}·2MeOH·2H2O and {[Ph3Sn(L)Sn(H2O)Ph3]n}·THF (L = 1,5-Naphthalenedisulfonate)
Chandrasekhar, Vadapalli; Boomishankar, Ramamoorthy; Steiner, Alexander; Bickley, Jamie F.; Organometallics 22 (2003) 3342–; doi:10.1021/om030423k

data_4076620
_publ_section_title
;
 First Example of a Hydrogen-Bonded Three-DimensionalPillaredStructure
 Involving an Organotin Motif:&#x00A0; Synthesis and X-ray Crystal
 Structures of
 {[nBu2Sn(H2O)3(L)Sn(H2O)3nBu2]2+[L]2-}&#x00B7;2MeOH&#x00B7;2H2O and
 {[Ph3Sn(L)Sn(H2O)Ph3]n}&#x00B7;THF (L = 1,5-Naphthalenedisulfonate)
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              3342
_journal_paper_doi               10.1021/om030423k
_journal_volume                  22
_journal_year                    2003
_chemical_formula_sum            'C50 H46 O8 S2 Sn2'
_chemical_formula_weight         1076.37
_chemical_name_systematic
;

 ?

;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 107.4430(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.3593(6)
_cell_length_b                   15.9365(7)
_cell_length_c                   20.5615(9)
_cell_measurement_temperature    100(2)
_cell_volume                     4488.9(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.920
_diffrn_measured_fraction_theta_max 0.920
_diffrn_measurement_device_type  'Bruker-AXS Smart Apex'
_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  0.0220
_diffrn_reflns_av_sigmaI/netI    0.0263
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            27492
_diffrn_reflns_theta_full        28.30
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         1.49
_exptl_absorpt_coefficient_mu    1.261
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.822
_exptl_absorpt_correction_type   semi-empirical
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.593
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'square blocks'
_exptl_crystal_F_000             2168
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.449
_refine_diff_density_min         -0.465
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     743
_refine_ls_number_reflns         10292
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0280
_refine_ls_R_factor_gt           0.0246
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0314P)^2^+3.4314P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0623
_refine_ls_wR_factor_ref         0.0640
_reflns_number_gt                9259
_reflns_number_total             10292
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om030423k.cif
_cod_data_source_block           compd_5
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4076620