#------------------------------------------------------------------------------
#$Date: 2016-02-16 21:30:59 +0100 (mar 16 de feb de 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/00/02/4000257.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4000257
_journal_name_full               'Chemistry of Materials'
_journal_paper_doi               10.1021/cm020650x
_journal_year                    2003
_chemical_formula_sum            'C H10 N2 O6 P2 Sn'
_chemical_formula_weight         326.76
_space_group_IT_number           61
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            9
_cell_length_a                   10.3417(10)
_cell_length_b                   10.0475(10)
_cell_length_c                   16.9927(17)
_cell_measurement_temperature    293(2)
_cell_volume                     1765.7(3)
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_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  0.0752
_diffrn_reflns_av_sigmaI/netI    0.0377
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            7246
_diffrn_reflns_theta_max         23.30
_diffrn_reflns_theta_min         2.40
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_exptl_absorpt_coefficient_mu    3.252
_exptl_crystal_density_diffrn    2.398
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1200
_refine_ls_extinction_coef       0.0022(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     92
_refine_ls_number_reflns         1270
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0310
_refine_ls_R_factor_gt           0.0268
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0395P)²+3.1764P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0714
_refine_ls_wR_factor_ref         0.0734
_reflns_number_gt                1119
_reflns_number_total             1270
_reflns_threshold_expression     >2sigma(I)
_cod_original_sg_symbol_H-M      'P ?'
_cod_original_formula_sum        'C1 H10 N2 O6 P2 Sn1'
_cod_database_code               4000257
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Sn1 Sn 0.89186(3) 0.00990(3) 0.402671(19) 0.0228(2) Uani 1 1 d . . .
P1 P 0.87694(11) 0.34435(11) 0.34227(7) 0.0195(3) Uani 1 1 d . . .
P2 P 0.78732(12) 0.27021(11) 0.50358(7) 0.0219(3) Uani 1 1 d . . .
O1 O 0.7784(3) 0.1220(3) 0.48156(18) 0.0293(8) Uani 1 1 d . . .
O2 O 0.9912(3) 0.3956(3) 0.29472(19) 0.0311(8) Uani 1 1 d . . .
C1 C 0.91589(13) 0.34531(14) 0.44601(8) 0.0228(10) Uani 1 1 d . . .
H1 H 0.9292 0.4363 0.4633 0.027 Uiso 1 1 calc R . .
H2 H 0.9956 0.2966 0.4545 0.027 Uiso 1 1 calc R . .
O3 O 0.83630(13) 0.20421(14) 0.31994(8) 0.0270(7) Uani 1 1 d R . .
O4 O 0.83789(13) -0.16007(14) 0.48005(8) 0.0314(8) Uani 1 1 d R . .
N1 N 0.76102(13) 0.53136(14) 0.66090(8) 0.0357(11) Uani 1 1 d R . .
O5 O 0.73593(13) -0.05575(14) 0.33263(8) 0.0265(7) Uani 1 1 d R . .
N2 N 0.94970(13) 0.68551(14) 0.31529(8) 0.0348(10) Uani 1 1 d R . .
O6 O 0.81960(13) 0.28471(14) 0.58942(8) 0.0379(9) Uani 1 1 d R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Sn1 0.0200(3) 0.0178(3) 0.0306(3) -0.00297(12) -0.00147(13) -0.00019(12)
P1 0.0199(6) 0.0157(6) 0.0230(7) 0.0000(5) 0.0026(5) 0.0000(5)
P2 0.0282(7) 0.0163(6) 0.0213(6) 0.0000(5) 0.0018(5) 0.0003(5)
O1 0.039(2) 0.0181(16) 0.0307(18) -0.0005(13) 0.0087(15) -0.0015(14)
O2 0.0291(19) 0.0297(18) 0.0346(19) -0.0004(15) 0.0110(15) -0.0059(15)
C1 0.021(2) 0.022(2) 0.026(3) 0.0003(19) -0.001(2) -0.0028(19)
O3 0.0342(19) 0.0170(16) 0.0299(17) -0.0031(13) 0.0005(15) -0.0041(14)
O4 0.0273(19) 0.0231(17) 0.044(2) 0.0103(15) -0.0091(16) -0.0025(14)
N1 0.038(3) 0.036(2) 0.033(2) 0.0000(19) 0.002(2) -0.002(2)
O5 0.0291(18) 0.0242(18) 0.0262(17) 0.0024(14) -0.0044(15) -0.0096(14)
N2 0.038(3) 0.025(2) 0.042(2) 0.0014(19) 0.008(2) -0.0015(19)
O6 0.054(2) 0.035(2) 0.0257(18) -0.0018(14) -0.0035(17) -0.0034(18)
