Formation of a Double-Bicapped Hexatin Phosphate Cage by a De-arylation Reaction. Synthesis and Structure of [(PhSn)6(μ-OH)2(μ3-O)2(μ-OEt)4{(ArO)PO3}4] (Ar = 2,6-i-Pr2C6H3)
Chandrasekhar, Vadapalli; Sasikumar, Palani; Thilagar, Pakkirisamy; Organometallics 26 (2007) 4386–; doi:10.1021/om700421b

data_4073527
_publ_section_title
;
 Formation of a Double-Bicapped Hexatin Phosphate Cage by a De-arylation
 Reaction. Synthesis and Structure of
 [(PhSn)6(\m-OH)2(\m3-O)2(\m-OEt)4{(ArO)PO3}4] (Ar = 2,6-i-Pr2C6H3)
;
_journal_issue                   18
_journal_name_full               Organometallics
_journal_page_first              4386
_journal_paper_doi               10.1021/om700421b
_journal_volume                  26
_journal_year                    2007
_chemical_formula_moiety         'C92 H120 O24 P4 Sn6'
_chemical_formula_sum            'C46 H60 O12 P2 Sn3'
_chemical_formula_weight         1222.94
_chemical_melting_point          173
_chemical_name_common            organotinphosphate
_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                90.000(5)
_cell_angle_beta                 95.946(5)
_cell_angle_gamma                90.000(5)
_cell_formula_units_Z            4
_cell_length_a                   15.913(5)
_cell_length_b                   16.520(5)
_cell_length_c                   19.837(5)
_cell_measurement_reflns_used    6626
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      25.80
_cell_measurement_theta_min      2.40
_cell_volume                     5187(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    'Bruker SHELXTL'
_diffrn_ambient_temperature      273(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     0.71069
_diffrn_reflns_av_R_equivalents  0.0423
_diffrn_reflns_av_sigmaI/netI    0.0520
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            28785
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.99
_exptl_absorpt_coefficient_mu    1.551
_exptl_absorpt_correction_T_max  0.7468
_exptl_absorpt_correction_T_min  0.7468
_exptl_absorpt_correction_type   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.565
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2444
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.598
_refine_diff_density_min         -0.648
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     342
_refine_ls_number_reflns         10186
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0705
_refine_ls_R_factor_gt           0.0512
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0704P)^2^+6.9504P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1264
_refine_ls_wR_factor_ref         0.1377
_reflns_number_gt                7723
_reflns_number_total             10186
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om700421b-file002.cif
_cod_data_source_block           VCSN6
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4073527