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_4076619
_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            'C19 H36 O11 S2 Sn'
_chemical_formula_weight         623.29
_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                113.35(4)
_cell_angle_beta                 94.59(4)
_cell_angle_gamma                100.65(4)
_cell_formula_units_Z            2
_cell_length_a                   9.093(3)
_cell_length_b                   11.484(4)
_cell_length_c                   14.058(4)
_cell_measurement_temperature    213(2)
_cell_volume                     1305.3(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.917
_diffrn_measured_fraction_theta_max 0.917
_diffrn_measurement_device_type  'Stoe IPDS'
_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  0.0460
_diffrn_reflns_av_sigmaI/netI    0.0476
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            8257
_diffrn_reflns_theta_full        24.16
_diffrn_reflns_theta_max         24.16
_diffrn_reflns_theta_min         1.96
_exptl_absorpt_coefficient_mu    1.191
_exptl_absorpt_correction_type   'not applied'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.586
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             640
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.307
_refine_diff_density_min         -1.240
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     327
_refine_ls_number_reflns         3847
_refine_ls_number_restraints     34
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0378
_refine_ls_R_factor_gt           0.0335
_refine_ls_shift/su_max          0.144
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0638P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0886
_refine_ls_wR_factor_ref         0.0906
_reflns_number_gt                3403
_reflns_number_total             3847
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om030423k.cif
_cod_data_source_block           Compd_4
_cod_depositor_comments
;

2021-04-11
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C38 H72 O22 S4 Sn2'
_cod_original_formula_weight         1246.58
_cod_original_formula_units_Z            1
_cod_original_cell_volume        1305.3(7)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4076619