Self-assembly of dialkyltin(IV) moieties and a thiosemicarbone to a trinuclear macrocycle and the unprecedented formation of two pseudo-polymorphs with different cavities
Kovala-Demertzi, Dimitra; Wiecek, Joanna; Plakatouras, John C.; Ciunik, Zbigniew; CrystEngComm 10 (2008) 1291–; doi:10.1039/b809216h

data_7202279
_publ_section_title
;
 Self-assembly of dialkyltin(IV) moieties and a thiosemicarbone to a
 trinuclear macrocycle and the unprecedented formation of two
 pseudo-polymorphs with different cavities
;
_journal_issue                   10
_journal_name_full               CrystEngComm
_journal_page_first              1291
_journal_paper_doi               10.1039/b809216h
_journal_volume                  10
_journal_year                    2008
_chemical_formula_moiety         'C18 H33 N9 O6 S3 Sn3, 1.5(C4 H8 O)'
_chemical_formula_sum            'C8 H15 N3 O2.5 S Sn'
_chemical_formula_weight         343.98
_chemical_name_common
'Dimethyl(pyruvic-thiosemicarbazonate)tin(IV) THF solvate'
_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            24
_cell_length_a                   20.1191(5)
_cell_length_b                   20.1191(5)
_cell_length_c                   20.1191(5)
_cell_measurement_reflns_used    12000
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.61
_cell_measurement_theta_min      3.25
_cell_volume                     8143.8(4)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.13 beta (release 14.11.2003 CrysAlis171 VC++)
(compiled Nov 14 2003,14:35:41)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.13 beta (release 14.11.2003 CrysAlis171 VC++)
(compiled Nov 14 2003,14:35:41)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.13 beta (release 14.11.2003 CrysAlis171 VC++)
(compiled Nov 14 2003,14:35:41)
;
_computing_molecular_graphics    'X-Seed (Barbour, 2001)'
_computing_publication_material
'SHELXL-97 (Sheldrick, 1997); Platon (Spek, 1998)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Kuma KM4CCD'
_diffrn_measurement_method       '\w scan'
_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  0.0600
_diffrn_reflns_av_sigmaI/netI    0.0534
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            66056
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         36.61
_diffrn_reflns_theta_min         3.20
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.029
_exptl_absorpt_correction_T_max  0.7928
_exptl_absorpt_correction_T_min  0.7116
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.13 beta (release 14.11.2003 CrysAlis171 VC++)
(compiled Nov 14 2003,14:35:41)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
;
_exptl_crystal_colour            off-white
_exptl_crystal_density_diffrn    1.683
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4080
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.165
_refine_diff_density_min         -0.847
_refine_diff_density_rms         0.112
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.022(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.903
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     144
_refine_ls_number_reflns         6610
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.903
_refine_ls_R_factor_all          0.0399
_refine_ls_R_factor_gt           0.0292
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0375P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0613
_refine_ls_wR_factor_ref         0.0630
_reflns_number_gt                5473
_reflns_number_total             6610
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b809216h.txt
_cod_data_source_block           a2abs
_cod_original_sg_symbol_H-M      I23
_cod_original_formula_sum        'C8 H15 N3 O2.50 S Sn'
_cod_database_code               7202279