#------------------------------------------------------------------------------
#$Date: 2012-02-28 14:14:52 +0200 (Tue, 28 Feb 2012) $
#$Revision: 35911 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/08/1100805.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_1100805
_chemical_formula_sum    'C13 H20 N O5 P Si2 W'
_chemical_formula_weight          541.30
loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'   0.0033   0.0016
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H'  'H'   0.0000   0.0000
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N'  'N'   0.0061   0.0033
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O'  'O'   0.0106   0.0060
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Si'  'Si'   0.0817   0.0704
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'P'  'P'   0.1023   0.0942
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'W'  'W'  -0.8490   6.8722
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting            triclinic
_symmetry_space_group_name_H-M    'P -1'
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x, -y, -z'
_cell_length_a                    6.9618(4)
_cell_length_b                    9.6073(8)
_cell_length_c                    16.1541(9)
_cell_angle_alpha                 73.219(3)
_cell_angle_beta                  89.975(3)
_cell_angle_gamma                 81.823(3)
_cell_volume                      1022.98(12)
_cell_formula_units_Z             2
_cell_measurement_temperature     133(2)
_cell_measurement_reflns_used     7126
_cell_measurement_theta_min       2.242
_cell_measurement_theta_max       30.539
_exptl_crystal_description        prism
_exptl_crystal_colour             colourless
_exptl_crystal_size_max           0.16
_exptl_crystal_size_mid           0.15
_exptl_crystal_size_min           0.08
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.757
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              524
_exptl_absorpt_coefficient_mu     5.860
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.7289
_exptl_absorpt_correction_T_max   0.9281
_exptl_absorpt_process_details    sadabs
_diffrn_ambient_temperature       133(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_radiation_source          'fine-focus sealed tube'
_diffrn_radiation_monochromator   graphite
_diffrn_measurement_device_type   'Bruker AXS Smart 1000CCD'
_diffrn_measurement_method        '\w- & \f-scan'
_diffrn_detector_area_resol_mean  8.192
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             19997
_diffrn_reflns_av_R_equivalents   0.0234
_diffrn_reflns_av_sigmaI/netI     0.0240
_diffrn_reflns_limit_h_min        -9
_diffrn_reflns_limit_h_max        9
_diffrn_reflns_limit_k_min        -13
_diffrn_reflns_limit_k_max        13
_diffrn_reflns_limit_l_min        -22
_diffrn_reflns_limit_l_max        22
_diffrn_reflns_theta_min          1.32
_diffrn_reflns_theta_max          30.03
_reflns_number_total              5954
_reflns_number_gt                 5515
_reflns_threshold_expression      >2sigma(I)
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
 'calc w=1/[\s^2^(Fo^2^)+(0.0177P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary      heavy-atom
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     'PH free, rigid methyls, others riding'
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        ?
_refine_ls_number_reflns          5954
_refine_ls_number_parameters      218
_refine_ls_number_restraints      21
_refine_ls_R_factor_all           0.0185
_refine_ls_R_factor_gt            0.0159
_refine_ls_wR_factor_ref          0.0346
_refine_ls_wR_factor_gt           0.0341
_refine_ls_goodness_of_fit_ref    0.998
_refine_ls_restrained_S_all       0.997
_refine_ls_shift/su_max           0.001
_refine_ls_shift/su_mean          0.000
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
W W 0.261181(10) 0.716083(8) 0.116808(5) 0.01703(2) Uani 1 1 d . . .
N N -0.1900(3) 0.4336(2) 0.24210(13) 0.0367(4) Uani 1 1 d . . .
P P 0.21119(6) 0.46014(5) 0.18983(3) 0.01652(9) Uani 1 1 d . . .
H0 H 0.208(3) 0.382(2) 0.1354(14) 0.025(6) Uiso 1 1 d . . .
Si1 Si 0.27506(8) 0.35607(6) 0.39420(3) 0.02167(10) Uani 1 1 d U . .
Si2 Si 0.41973(8) 0.14789(6) 0.27166(3) 0.02091(10) Uani 1 1 d U . .
O1 O 0.0283(2) 0.70023(19) -0.04908(10) 0.0380(4) Uani 1 1 d . . .
O2 O -0.1250(2) 0.83559(19) 0.19606(12) 0.0451(4) Uani 1 1 d . . .
O3 O 0.2884(2) 1.04673(17) 0.01445(12) 0.0412(4) Uani 1 1 d . . .
O4 O 0.6480(2) 0.59289(17) 0.03919(10) 0.0328(3) Uani 1 1 d . . .
O5 O 0.5215(2) 0.72042(18) 0.27815(10) 0.0349(3) Uani 1 1 d . . .
C1 C 0.1083(3) 0.7053(2) 0.01169(13) 0.0244(4) Uani 1 1 d . . .
C2 C 0.0128(3) 0.7923(2) 0.16746(14) 0.0271(4) Uani 1 1 d . . .
C3 C 0.2853(3) 0.9260(2) 0.05228(14) 0.0273(4) Uani 1 1 d . . .
C4 C 0.5099(3) 0.6370(2) 0.06706(12) 0.0221(4) Uani 1 1 d . . .
C5 C 0.4272(3) 0.7202(2) 0.21995(13) 0.0236(4) Uani 1 1 d . . .
C6 C 0.3553(2) 0.34070(19) 0.28357(11) 0.0174(3) Uani 1 1 d U . .
H6 H 0.4825 0.3789 0.2774 0.021 Uiso 1 1 calc R . .
C7 C 0.1395(3) 0.5418(2) 0.38876(14) 0.0310(4) Uani 1 1 d U . .
H7A H 0.0142 0.5562 0.3575 0.037 Uiso 1 1 calc R . .
H7B H 0.2157 0.6179 0.3584 0.037 Uiso 1 1 calc R . .
H7C H 0.1175 0.5483 0.4475 0.037 Uiso 1 1 calc R . .
C8 C 0.5040(3) 0.3274(3) 0.46181(14) 0.0328(5) Uani 1 1 d U . .
H8A H 0.4714 0.3325 0.5200 0.039 Uiso 1 1 calc R . .
H8B H 0.5828 0.4040 0.4351 0.039 Uiso 1 1 calc R . .
H8C H 0.5775 0.2307 0.4657 0.039 Uiso 1 1 calc R . .
C9 C 0.1132(3) 0.2172(2) 0.44494(14) 0.0307(4) Uani 1 1 d U . .
H9A H 0.1818 0.1181 0.4512 0.037 Uiso 1 1 calc R . .
H9B H -0.0047 0.2345 0.4081 0.037 Uiso 1 1 calc R . .
H9C H 0.0778 0.2265 0.5020 0.037 Uiso 1 1 calc R . .
C10 C 0.5860(3) 0.0301(2) 0.36344(14) 0.0320(5) Uani 1 1 d U . .
H10A H 0.6244 -0.0668 0.3549 0.038 Uiso 1 1 calc R . .
H10B H 0.5190 0.0190 0.4178 0.038 Uiso 1 1 calc R . .
H10C H 0.7018 0.0763 0.3658 0.038 Uiso 1 1 calc R . .
C11 C 0.1942(3) 0.0656(2) 0.26610(15) 0.0321(5) Uani 1 1 d U . .
H11A H 0.1051 0.1326 0.2201 0.039 Uiso 1 1 calc R . .
H11B H 0.1312 0.0498 0.3217 0.039 Uiso 1 1 calc R . .
H11C H 0.2279 -0.0286 0.2536 0.039 Uiso 1 1 calc R . .
C12 C 0.5538(3) 0.1627(3) 0.17020(14) 0.0342(5) Uani 1 1 d U . .
H12A H 0.6622 0.2175 0.1704 0.041 Uiso 1 1 calc R . .
H12B H 0.4656 0.2144 0.1201 0.041 Uiso 1 1 calc R . .
H12C H 0.6041 0.0640 0.1668 0.041 Uiso 1 1 calc R . .
C13 C -0.0360(3) 0.4402(2) 0.22160(13) 0.0235(4) Uani 1 1 d . . .
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
W 0.01575(4) 0.01504(4) 0.01936(4) -0.00395(3) 0.00147(2) -0.00150(2)
N 0.0265(10) 0.0383(11) 0.0426(12) -0.0068(9) -0.0004(8) -0.0061(8)
P 0.0159(2) 0.0161(2) 0.0177(2) -0.00515(17) 0.00028(15) -0.00250(17)
Si1 0.0244(3) 0.0239(3) 0.0178(3) -0.0074(2) 0.00223(18) -0.0045(2)
Si2 0.0241(3) 0.0172(2) 0.0201(3) -0.00514(19) -0.00080(18) 0.0010(2)
O1 0.0322(8) 0.0521(10) 0.0302(9) -0.0128(7) -0.0067(6) -0.0063(7)
O2 0.0320(9) 0.0371(10) 0.0631(12) -0.0138(9) 0.0178(8) 0.0038(7)
O3 0.0368(9) 0.0211(8) 0.0566(11) 0.0025(7) 0.0051(7) -0.0038(7)
O4 0.0272(8) 0.0378(9) 0.0299(8) -0.0083(7) 0.0064(6) 0.0036(6)
O5 0.0323(8) 0.0460(10) 0.0323(9) -0.0185(7) -0.0017(6) -0.0096(7)
C1 0.0202(9) 0.0243(10) 0.0268(10) -0.0049(8) 0.0033(7) -0.0026(7)
C2 0.0250(10) 0.0196(10) 0.0349(12) -0.0056(8) 0.0033(8) -0.0024(8)
C3 0.0216(9) 0.0256(11) 0.0331(11) -0.0069(8) 0.0015(7) -0.0009(8)
C4 0.0237(9) 0.0211(9) 0.0190(9) -0.0021(7) 0.0000(7) -0.0029(7)
C5 0.0237(9) 0.0220(10) 0.0274(10) -0.0105(8) 0.0069(7) -0.0042(7)
C6 0.0163(8) 0.0184(9) 0.0168(9) -0.0040(6) 0.0000(6) -0.0024(6)
C7 0.0384(12) 0.0295(11) 0.0285(11) -0.0142(9) 0.0097(8) -0.0042(9)
C8 0.0379(12) 0.0372(12) 0.0264(11) -0.0129(9) -0.0059(8) -0.0074(9)
C9 0.0336(11) 0.0331(12) 0.0245(11) -0.0059(9) 0.0069(8) -0.0074(9)
C10 0.0368(12) 0.0248(11) 0.0296(11) -0.0051(8) -0.0078(8) 0.0050(9)
C11 0.0366(12) 0.0234(11) 0.0397(13) -0.0141(9) -0.0020(9) -0.0051(9)
C12 0.0405(12) 0.0335(12) 0.0267(11) -0.0110(9) 0.0070(9) 0.0053(10)
C13 0.0227(9) 0.0196(9) 0.0264(10) -0.0034(7) -0.0038(7) -0.0042(7)
_cod_database_code 1100805