Self-Assembly of Dialkyltin(IV) Moieties and Aromatic Dicarboxylates to Complexes with a Polymeric or a Discrete Trinuclear Macrocyclic Structure in the Solid State and a Mixture of Fast Interchanging Cyclooligomeric Structures in Solution
Reyes García-Zarracino; Jesús Ramos-Quiñones; Herbert Höpfl; Inorganic Chemistry 42 (2003) 3835–3845; doi:10.1021/ic026270v

data_4313758
_publ_section_title
;
 Self-Assembly of Dialkyltin(IV) Moieties and Aromatic Dicarboxylates to
 Complexes with a Polymeric or a Discrete Trinuclear Macrocyclic Structure
 in the Solid State and a Mixture of Fast Interchanging Cyclooligomeric
 Structures in Solution
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3835
_journal_page_last               3845
_journal_paper_doi               10.1021/ic026270v
_journal_volume                  42
_journal_year                    2003
_chemical_formula_moiety         C48H66O12Sn3
_chemical_formula_sum            'C60 H78 O12 Sn3'
_chemical_formula_weight         1347.29
_chemical_melting_point          327.0(10)
_chemical_name_common            Tris(di-n-butyltin-1,3-benzenedicarboxylate)
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 103.078(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.5232(16)
_cell_length_b                   26.670(3)
_cell_length_c                   17.996(2)
_cell_measurement_temperature    293(2)
_cell_volume                     6322.2(12)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.1133
_diffrn_reflns_av_sigmaI/netI    0.1194
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            45917
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.39
_exptl_absorpt_coefficient_mu    1.231
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.416
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2736
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.41
_exptl_crystal_size_min          0.48
_refine_diff_density_max         1.252
_refine_diff_density_min         -0.405
_refine_diff_density_rms         0.118
_refine_ls_extinction_coef       0.00000(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.799
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     653
_refine_ls_number_reflns         11130
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      0.812
_refine_ls_R_factor_all          0.1594
_refine_ls_R_factor_gt           0.0580
_refine_ls_shift/su_max          15.000
_refine_ls_shift/su_mean         0.063
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0657P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1276
_refine_ls_wR_factor_ref         0.1548
_reflns_number_gt                4009
_reflns_number_total             11130
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic026270vsi20021214_073513_3.cif
_cod_data_source_block           reyezeim
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/adriana/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1555 2011-01-17 13:19:09Z saulius 

The following automatic conversions were performed:

'_chemical_melting_point' value '326-328' was changed to '327.0(10)'
- the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1569 2011-02-09 13:29:24Z adriana 
;
_cod_original_cell_volume        6322.1(13)
_cod_database_code               4313758