Reaction of Butyltin Hydroxide Oxide withp-Toluenesulfonic Acid: Synthesis, X-ray Crystal Analysis, and Multinuclear NMR Characterization of {(BuSn)12O14(OH)6}(4-CH3C6H4SO3)2
Eychenne-Baron, Christophe; Ribot, François; Steunou, Nathalie; Sanchez, Clément; Fayon, Franck; Biesemans, Monique; Martins, José C.; Willem, Rudolph; Organometallics 19 (2000) 1940–; doi:10.1021/om990877a

data_4077692
_publ_contact_author
;
Fran&#x008D;ois RIBOT
Laboratoire de Chimie de la Mati&#x008F;re Condens&#x008E;e, UMR CNRS 7574
Universit&#x008E; Pierre et Marie Curie - tour 54, 5&#x008F;me &#x008E;tage
4, place Jussieu - 75252 PARIS cedex 05 - FRANCE
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_publ_section_title
;
 Reaction of Butyltin Hydroxide Oxide withp-Toluenesulfonic Acid:
 Synthesis, X-ray Crystal Analysis, and Multinuclear NMR Characterization
 of {(BuSn)12O14(OH)6}(4-CH3C6H4SO3)2
;
_journal_issue                   10
_journal_name_full               Organometallics
_journal_page_first              1940
_journal_paper_doi               10.1021/om990877a
_journal_volume                  19
_journal_year                    2000
_chemical_compound_source        ?
_chemical_formula_moiety         'C33 H68 Sn6 O14 S1'
_chemical_formula_sum            'C33 H68 O14 S Sn6'
_chemical_formula_weight         1433.35
_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   Difmap_and_Geometric
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             99-10-06
_audit_creation_method           CRYSTALS
_cell_angle_alpha                114.003
_cell_angle_beta                 96.616
_cell_angle_gamma                104.237
_cell_formula_units_Z            2
_cell_length_a                   12.722
_cell_length_b                   14.070
_cell_length_c                   16.014
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298
_cell_measurement_theta_max      14.3
_cell_measurement_theta_min      13.9
_cell_volume                     2462.034
_computing_cell_refinement       'CAD-4 software (Enraf-Nonius, 1989)'
_computing_data_collection       'CAD-4 software (Enraf-Nonius, 1989)'
_computing_data_reduction
;
RC93 (Watkin, D.J., Prout, C.K., Lilley, P.M.deQ. 1994)
;
_computing_molecular_graphics
;
 CAMERON (Watkin, Prout & Pearce,  1996)
;
_computing_publication_material
;
CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996)
;
_computing_structure_refinement
;
CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996)
;
_computing_structure_solution    'SHELXS86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      298
_diffrn_measurement_device       '  Enraf-nonius CAD4 '
_diffrn_measurement_method       2\q/\w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.02
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            8984
_diffrn_reflns_theta_max         25.0
_diffrn_reflns_theta_min         1.0
_diffrn_standards_decay_%        8.64
_diffrn_standards_interval_time  120
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    3.10
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.78
_exptl_absorpt_correction_type   DIFABS
_exptl_absorpt_process_details   'refined from delta-F'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.93
_exptl_crystal_description       ' box '
_exptl_crystal_F_000             1388
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.70
_refine_diff_density_min         -0.56
_refine_ls_extinction_coef       34.0
_refine_ls_extinction_method
'Larson 1970 Crystallographic Computing eq 22'
_refine_ls_goodness_of_fit_obs   2.1619
_refine_ls_hydrogen_treatment
;refU 
 Some H atoms were placed from Fourier difference map. The other were placed geometrically before the last refinement cycle. Only two isotropic thermal parameters were considered for H atoms : one for the mu2-OH and one for the hydrogen atoms bound to a carbon.
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     490
_refine_ls_number_reflns         5927
_refine_ls_R_factor_obs          0.0326
_refine_ls_shift/esd_max         0.133797
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      unit
_refine_ls_wR_factor_obs         0.0340
_reflns_limit_h_max              14
_reflns_limit_h_min              -15
_reflns_limit_k_max              15
_reflns_limit_k_min              -16
_reflns_limit_l_max              19
_reflns_limit_l_min              0
_reflns_number_observed          5927
_reflns_number_total             8645
_reflns_observed_criterion       >3.00\s(I)
_cod_data_source_file            om990877a.cif
_cod_data_source_block           CRYSTALS_cif
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_secondary' value 'Difmap' changed to 'difmap'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Direct_Methods' was changed to
'direct'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_cell_volume        2462.10
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        ' C33 H68 Sn6 O14 S1 '
_cod_database_code               4077692