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_7202278
_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, 3(C4 H8 O)'
_chemical_formula_sum            'C10 H19 N3 O3 S Sn'
_chemical_formula_weight         380.06
_chemical_name_common
'Dimethyl(pyruvic-thiosemicarbazonate)tin(IV) THF solvate'
_space_group_IT_number           176
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-P 6c'
_symmetry_space_group_name_H-M   'P 63/m'
_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                120.00
_cell_formula_units_Z            6
_cell_length_a                   18.2141(5)
_cell_length_b                   18.2141(5)
_cell_length_c                   7.6303(3)
_cell_measurement_reflns_used    11200
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.60
_cell_measurement_theta_min      3.25
_cell_volume                     2192.24(12)
_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 0.985
_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  0.0390
_diffrn_reflns_av_sigmaI/netI    0.0244
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            37222
_diffrn_reflns_theta_full        36.60
_diffrn_reflns_theta_max         36.60
_diffrn_reflns_theta_min         3.42
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.895
_exptl_absorpt_correction_T_max  0.8045
_exptl_absorpt_correction_T_min  0.7513
_exptl_absorpt_correction_type   'numeric 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    1.727
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1140
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.445
_refine_diff_density_min         -0.675
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     126
_refine_ls_number_reflns         3772
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0378
_refine_ls_R_factor_gt           0.0259
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0297P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0529
_refine_ls_wR_factor_ref         0.0550
_reflns_number_gt                3183
_reflns_number_total             3772
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b809216h.txt
_cod_data_source_block           a1abs
_cod_original_sg_symbol_H-M      P63/m
_cod_database_code               7202278