Synthesis, Characterization, and Structural Studies of Mixed-Ligand Diorganotin Esters, [R2Sn(OP(O)(OH)Ph)(OS(O)2R1)]n [R =n-Bu, R1= Me (1), n-Pr (2); R = Et, R1= Me (3)] with 1D and 3D Coordination Polymeric Motifs
Ravi Shankar; Atul Pratap Singh; Archana Jain; Mary F. Mahon; Kieran C. Molloy; Inorganic Chemistry 47 (2008) 5930–5935; doi:10.1021/ic8002433

data_4305289
_publ_section_title
;
Synthesis, Characterization, and Structural Studies of Mixed-Ligand
Diorganotin Esters, [R2Sn(OP(O)(OH)Ph)(OS(O)2R1)]n [R =n-Bu, R1= Me (1), n-Pr
(2); R = Et, R1= Me (3)] with 1D and 3D Coordination Polymeric Motifs
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5930
_journal_page_last               5935
_journal_paper_doi               10.1021/ic8002433
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C60 H105 O24 P4 S4 Sn4'
_chemical_formula_weight         1937.32
_chemical_name_systematic
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 ?
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_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                104.981(1)
_cell_angle_beta                 107.287(1)
_cell_angle_gamma                109.017(1)
_cell_formula_units_Z            2
_cell_length_a                   13.0210(1)
_cell_length_b                   18.8670(2)
_cell_length_c                   19.7880(2)
_cell_measurement_reflns_used    43430
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      2.910
_cell_volume                     4034.08(9)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction
'Denzo & Scalepack (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'ORTEX (P.McArdle, 1995)'
_computing_publication_material  'SHELXL-97/2 (Sheldrick,1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  '95mm CCD camera on \k-goniostat'
_diffrn_measurement_method       CCD
_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    0.1033
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            70599
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         3.52
_exptl_absorpt_coefficient_mu    1.475
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.70
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.595
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1962
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.07
_refine_diff_density_max         2.218
_refine_diff_density_min         -1.302
_refine_diff_density_rms         0.177
_refine_ls_extinction_coef       0.00255(14)
_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   1.053
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     866
_refine_ls_number_reflns         70609
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.1147
_refine_ls_R_factor_gt           0.0765
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0579P)^2^+37.4082P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1733
_refine_ls_wR_factor_ref         0.1954
_reflns_number_gt                49698
_reflns_number_total             70609
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic8002433-file007_1.cif
_cod_data_source_block           h07kcm16
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Multi-Scan' changed
to 'multi-scan' 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_enum 1527 2010-12-29 10:47:43Z saulius 
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_cod_original_cell_volume        4034.08(7)
_cod_database_code               4305289