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_4313757
_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         C32H44O8Sn2
_chemical_formula_sum            'C32 H44 O8 Sn2'
_chemical_formula_weight         794.05
_chemical_melting_point          499
_chemical_name_common            'Di-n-butyltin(IV) phtalate'
_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                 94.2430(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.7166(6)
_cell_length_b                   9.8931(5)
_cell_length_c                   29.4262(16)
_cell_measurement_temperature    100(2)
_cell_volume                     3401.5(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0243
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5984
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.39
_exptl_absorpt_coefficient_mu    1.514
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.551
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1600
_refine_diff_density_max         2.080
_refine_diff_density_min         -0.502
_refine_diff_density_rms         0.095
_refine_ls_extinction_coef       0.00000(6)
_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   1.188
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     384
_refine_ls_number_reflns         5984
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.188
_refine_ls_R_factor_all          0.0394
_refine_ls_R_factor_gt           0.0375
_refine_ls_shift/su_max          10.441
_refine_ls_shift/su_mean         0.027
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0246P)^2^+9.2743P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0779
_refine_ls_wR_factor_ref         0.0789
_reflns_number_gt                5726
_reflns_number_total             5984
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic026270vsi20021214_073513_2.cif
_cod_data_source_block           trixie
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4313757