Dibutylammonium bis(hydrogen methylphosphonato-κ<i>O</i>)triphenylstannate(IV)
Diop, Tidiane; Diop, Libasse; Fall, Djibril; van der Lee, Arie; Acta Crystallographica Section E 68 (2012) m1284–m1285; doi:10.1107/S1600536812038445

data_2236695
_publ_section_title
;
 Dibutylammonium bis(hydrogen
 methylphosphonato-\k<i>O</i>)triphenylstannate(IV)
;
_journal_coeditor_code           WM2676
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1284
_journal_page_last               m1285
_journal_paper_doi               10.1107/S1600536812038445
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '(C8 H20 N) [Sn (C6 H5)3 (C H4 O3 P)2]'
_chemical_formula_moiety         'C20 H23 O6 P2 Sn, C8 H20 N'
_chemical_formula_sum            'C28 H43 N O6 P2 Sn'
_chemical_formula_weight         670.28
_chemical_name_systematic
;
Dibutylammonium bis(hydrogen methylphosphonato-\k<i>O</i>)triphenylstannate(IV)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     charge-flipping
_cell_angle_alpha                90
_cell_angle_beta                 93.220(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.1963(8)
_cell_length_b                   18.9088(8)
_cell_length_c                   21.1989(11)
_cell_measurement_reflns_used    7455
_cell_measurement_temperature    175
_cell_measurement_theta_max      29.1449
_cell_measurement_theta_min      1.4383
_cell_volume                     6482.0(5)
_computing_cell_refinement       '<i>CrysAlis PRO</i>  (Agilent, 2010)'
_computing_data_collection       '<i>CrysAlis PRO</i> (Agilent, 2010)'
_computing_data_reduction        '<i>CrysAlis PRO</i>  (Agilent, 2010)'
_computing_molecular_graphics
'<i>OLEX2</i> (Dolomanov <i>et al.</i>, 2009)'
_computing_publication_material
;
<i>CRYSTALS</i> (Betteridge <i>et al.</i>, 2003) and <i>publCIF</i>
(Westrip, 2010)
;
_computing_structure_refinement
'<i>CRYSTALS</i> (Betteridge <i>et al.</i>, 2003)'
_computing_structure_solution
'<i>Superflip</i> (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      175
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.902
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction Gemini'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.085
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            64843
_diffrn_reflns_theta_full        25.174
_diffrn_reflns_theta_max         29.145
_diffrn_reflns_theta_min         1.438
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.925
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.96051
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>CrysAlis PRO</i>; Agilent, 2010)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.374
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2768
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.28
_refine_diff_density_min         -1.66
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9916
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     686
_refine_ls_number_reflns         17225
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.1015
_refine_ls_R_factor_gt           0.0672
_refine_ls_shift/su_max          0.0025
_refine_ls_shift/su_mean         0.00002
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994; Prince, 1982)
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
 Method = Robust Weighting (Prince, 1982)
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
 A~i~ are:
 15.1 4.23 12.3 3.23
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0791
_refine_ls_wR_factor_gt          0.0674
_refine_ls_wR_factor_ref         0.0674
_reflns_number_gt                17225
_reflns_number_total             26060
_reflns_threshold_expression     I>2.0\s(I)
_cod_data_source_file            wm2676.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2236695
_cod_database_fobs_code          2236695