data_sfax68
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C8 H28 As3 N O12'
_chemical_formula_weight          555.07
 
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'
 'As'  'As'   0.0499   2.0058
 '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'
 
_symmetry_cell_setting            ?
_symmetry_space_group_name_H-M    ?
 
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 'x, -y, z+1/2'
 'x+1/2, y+1/2, z'
 'x+1/2, -y+1/2, z+1/2'
 
_cell_length_a                    20.105
_cell_length_b                    7.342
_cell_length_c                    15.292
_cell_angle_alpha                 90.00
_cell_angle_beta                  115.00
_cell_angle_gamma                 90.00
_cell_volume                      2045.8
_cell_formula_units_Z             4
_cell_measurement_temperature     293(2)
_cell_measurement_reflns_used     ?
_cell_measurement_theta_min       ?
_cell_measurement_theta_max       ?
 
_exptl_crystal_description        ?
_exptl_crystal_colour             ?
_exptl_crystal_size_max           0.40
_exptl_crystal_size_mid           0.20
_exptl_crystal_size_min           0.10
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     3.604
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              2224
_exptl_absorpt_coefficient_mu     9.846
_exptl_absorpt_correction_type    ?
_exptl_absorpt_correction_T_min   0.2604
_exptl_absorpt_correction_T_max   0.5745
_exptl_absorpt_process_details    ?
 
_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature       293(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   ?
_diffrn_measurement_method        ?
_diffrn_detector_area_resol_mean  ?
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             5066
_diffrn_reflns_av_R_equivalents   0.0290
_diffrn_reflns_av_sigmaI/netI     0.0395
_diffrn_reflns_limit_h_min        -25
_diffrn_reflns_limit_h_max        25
_diffrn_reflns_limit_k_min        -9
_diffrn_reflns_limit_k_max        1
_diffrn_reflns_limit_l_min        -19
_diffrn_reflns_limit_l_max        19
_diffrn_reflns_theta_min          2.84
_diffrn_reflns_theta_max          27.08
_reflns_number_total              4383
_reflns_number_gt                 3366
_reflns_threshold_expression      >2sigma(I)
 
_computing_data_collection        ?
_computing_cell_refinement        ?
_computing_data_reduction         ?
_computing_structure_solution     ?
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics     ?
_computing_publication_material   ?
 
_refine_special_details
;
 Refinement of F^2^ against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F^2^, conventional R-factors R are based
 on F, with F set to zero for negative F^2^. The threshold expression of
 F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F^2^ are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
 
_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^)+(0.1687P)^2^+1.7854P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     mixed
_refine_ls_extinction_method      SHELXL
_refine_ls_extinction_coef        0.0001(5)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^'
_refine_ls_abs_structure_details
 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack    0.00
_refine_ls_number_reflns          4383
_refine_ls_number_parameters      197
_refine_ls_number_restraints      6
_refine_ls_R_factor_all           0.0926
_refine_ls_R_factor_gt            0.0717
_refine_ls_wR_factor_ref          0.2200
_refine_ls_wR_factor_gt           0.1960
_refine_ls_goodness_of_fit_ref    1.038
_refine_ls_restrained_S_all       1.048
_refine_ls_shift/su_max           0.000
_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
O8 O 0.3340(7) -0.2459(17) 0.3250(10) 0.065(4) Uani 1 1 d . . .
C1 C -0.0094(7) 0.1379(19) 0.2730(11) 0.056(3) Uani 1 1 d . . .
H1A H -0.0056 0.1317 0.2119 0.067 Uiso 1 1 calc R . .
H1B H -0.0110 0.0159 0.2963 0.067 Uiso 1 1 calc R . .
C2 C 0.1092(7) 0.296(2) 0.3038(11) 0.069(4) Uani 1 1 d D . .
H2A H 0.1360 0.1852 0.3058 0.083 Uiso 1 1 calc R . .
H2B H 0.1446 0.3869 0.3422 0.083 Uiso 1 1 calc R . .
C3 C 0.0229(7) 0.4288(16) 0.3659(10) 0.055(3) Uani 1 1 d D . .
H3A H -0.0137 0.4028 0.3899 0.067 Uiso 1 1 calc R . .
H3B H -0.0006 0.4942 0.3054 0.067 Uiso 1 1 calc R . .
C5 C 0.0856(6) 0.5467(13) 0.4405(8) 0.042(2) Uani 1 1 d D . .
H5A H 0.0657 0.6597 0.4502 0.063 Uiso 1 1 calc R . .
H5B H 0.1218 0.5707 0.4166 0.063 Uiso 1 1 calc R . .
H5C H 0.1079 0.4823 0.5006 0.063 Uiso 1 1 calc R . .
C8 C 0.0702(8) 0.366(2) 0.1938(9) 0.069(4) Uani 1 1 d D . .
H8A H 0.1066 0.3846 0.1695 0.058 Uiso 1 1 calc R . .
H8B H 0.0454 0.4794 0.1914 0.088 Uiso 1 1 calc R . .
H8C H 0.0353 0.2772 0.1550 0.088 Uiso 1 1 calc R . .
As1 As 0.36285(4) 0.2190(2) 0.42953(4) 0.0324(4) Uani 1 1 d . . .
As2 As 0.25063(4) -0.2164(2) 0.26201(5) 0.0339(4) Uani 1 1 d . . .
As3 As 0.30657(14) 0.25920(11) 0.09615(16) 0.0360(3) Uani 1 1 d . . .
N N 0.0546(8) 0.258(2) 0.3507(12) 0.0357(18) Uani 1 1 d D . .
O1 O 0.3873(6) 0.0054(18) 0.4669(8) 0.057(3) Uani 1 1 d . . .
H11 H 0.3758 -0.0620 0.4200 0.086 Uiso 1 1 calc R . .
O2 O 0.4040(6) 0.2751(19) 0.3591(12) 0.071(4) Uani 1 1 d . . .
O3 O 0.3849(6) 0.352(2) 0.5224(9) 0.065(4) Uani 1 1 d . . .
H13 H 0.3731 0.4567 0.5041 0.098 Uiso 1 1 calc R . .
O4 O 0.2665(4) 0.2446(14) 0.3545(7) 0.035(2) Uani 1 1 d . . .
H14 H 0.2545 0.1761 0.3079 0.053 Uiso 1 1 calc R . .
O5 O 0.1999(5) -0.2871(14) 0.3233(6) 0.039(2) Uani 1 1 d . . .
H22 H 0.2081 -0.3951 0.3374 0.059 Uiso 1 1 calc R . .
O6 O 0.2320(7) -0.3652(17) 0.1660(8) 0.062(4) Uani 1 1 d . . .
H23 H 0.2418 -0.4696 0.1864 0.093 Uiso 1 1 calc R . .
O7 O 0.2276(5) -0.0063(12) 0.2207(7) 0.038(2) Uani 1 1 d . . .
O12 O 0.2870(6) 0.3837(16) -0.0054(8) 0.050(3) Uani 1 1 d . . .
H31 H 0.3217 0.4504 0.0025 0.074 Uiso 1 1 calc R . .
O9 O 0.3177(6) 0.3816(16) 0.1906(6) 0.043(3) Uani 1 1 d . . .
O10 O 0.2300(5) 0.1249(12) 0.0655(7) 0.053(3) Uani 1 1 d . . .
H33 H 0.2355 0.0569 0.1106 0.079 Uiso 1 1 calc R . .
O11 O 0.3817(4) 0.1219(11) 0.1308(4) 0.077(5) Uani 1 1 d . . .
H34 H 0.3703 0.0175 0.1378 0.116 Uiso 1 1 calc R . .
C4 C 0.1015(4) 0.1585(11) 0.4379(4) 0.058(3) Uani 1 1 d R . .
H4A H 0.1387 0.2404 0.4811 0.070 Uiso 1 1 calc R . .
H4B H 0.1262 0.0610 0.4206 0.070 Uiso 1 1 calc R . .
C6 C 0.0601(4) 0.0803(11) 0.4890(4) 0.055 Uani 1 1 d R . .
H6A H 0.0931 0.0154 0.5451 0.069 Uiso 1 1 calc R . .
H6B H 0.0234 -0.0019 0.4468 0.069 Uiso 1 1 calc R . .
H6C H 0.0368 0.1765 0.5084 0.069 Uiso 1 1 calc R . .
C7 C -0.0767(4) 0.2575(11) 0.2663(4) 0.060 Uani 1 1 d R . .
H7A H -0.1216 0.2023 0.2218 0.090 Uiso 1 1 calc R . .
H7B H -0.0726 0.3776 0.2443 0.090 Uiso 1 1 calc R . .
H7C H -0.0770 0.2653 0.3288 0.090 Uiso 1 1 calc 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
O8 0.085(9) 0.061(8) 0.067(8) -0.034(6) 0.049(8) -0.015(6)
C1 0.054(6) 0.054(7) 0.067(8) -0.015(6) 0.033(6) -0.016(6)
C2 0.068(8) 0.070(9) 0.100(12) -0.016(8) 0.066(9) -0.016(7)
C3 0.064(7) 0.056(7) 0.064(8) 0.012(6) 0.044(6) 0.009(6)
C5 0.069(7) 0.023(4) 0.040(5) -0.016(4) 0.030(5) -0.020(4)
C8 0.112(11) 0.060(8) 0.070(9) 0.019(7) 0.073(9) 0.022(8)
As1 0.0384(7) 0.0352(9) 0.0237(8) -0.0003(9) 0.0133(6) 0.0003(9)
As2 0.0469(8) 0.0320(8) 0.0252(8) -0.0027(9) 0.0175(7) 0.0007(9)
As3 0.0597(5) 0.0312(4) 0.0209(4) -0.0015(10) 0.0208(4) -0.0010(12)
N 0.032(3) 0.041(4) 0.039(4) -0.002(3) 0.020(3) -0.004(3)
O1 0.079(8) 0.057(8) 0.035(6) 0.009(6) 0.022(6) 0.000(7)
O2 0.039(5) 0.083(9) 0.099(11) -0.022(7) 0.037(6) -0.021(5)
O3 0.077(7) 0.078(9) 0.038(6) 0.006(6) 0.022(6) 0.051(7)
O4 0.007(3) 0.064(6) 0.022(4) -0.004(4) -0.006(3) 0.011(3)
O5 0.043(5) 0.052(5) 0.016(4) 0.019(4) 0.004(3) -0.012(4)
O6 0.092(8) 0.040(6) 0.027(5) -0.027(5) -0.001(5) 0.002(6)
O7 0.067(6) 0.019(5) 0.034(5) -0.003(4) 0.026(5) -0.005(5)
O12 0.071(7) 0.037(7) 0.046(6) 0.015(5) 0.031(5) 0.000(5)
O9 0.072(6) 0.045(7) 0.015(4) 0.006(4) 0.022(4) 0.009(5)
O10 0.080(8) 0.036(6) 0.042(6) 0.008(5) 0.026(6) -0.028(5)
O11 0.097(10) 0.096(13) 0.032(6) 0.013(7) 0.021(7) 0.040(9)
C4 0.054(6) 0.058(8) 0.050(7) 0.007(6) 0.009(6) -0.003(6)
C6 0.056 0.054 0.044 0.006 0.011 -0.001
C7 0.060 0.057 0.048 0.015 0.009 -0.006
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_atom_site_label_2
 _geom_bond_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
O8 As2 1.556(14) . ?
C1 C7 1.580(15) . ?
C1 N 1.60(2) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 N 1.571(14) . ?
C2 C8 1.611(14) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 N 1.470(14) . ?
C3 C5 1.556(13) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
As1 O3 1.622(13) . ?
As1 O2 1.663(14) . ?
As1 O1 1.671(12) . ?
As1 O4 1.796(7) . ?
As2 O7 1.657(9) 1 ?
As2 O7 1.657(9) . ?
As2 O5 1.731(9) . ?
As2 O6 1.739(10) . ?
As3 O9 1.634(10) . ?
As3 O12 1.698(11) . ?
As3 O11 1.704(7) . ?
As3 O10 1.718(8) . ?
N C4 1.462(17) . ?
O1 H11 0.8200 . ?
O3 H13 0.8200 . ?
O4 H14 0.8200 . ?
O5 H22 0.8200 . ?
O6 H23 0.8200 . ?
O7 O7 0.000(18) 1 ?
O12 H31 0.8200 . ?
O10 H33 0.8200 . ?
O11 H34 0.8200 . ?
C4 C6 1.4777 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
 
loop_
 _geom_angle_atom_site_label_1
 _geom_angle_atom_site_label_2
 _geom_angle_atom_site_label_3
 _geom_angle
 _geom_angle_site_symmetry_1
 _geom_angle_site_symmetry_3
 _geom_angle_publ_flag
C7 C1 N 98.1(9) . . ?
C7 C1 H1A 112.1 . . ?
N C1 H1A 112.1 . . ?
C7 C1 H1B 112.1 . . ?
N C1 H1B 112.1 . . ?
H1A C1 H1B 109.8 . . ?
N C2 C8 114.1(12) . . ?
N C2 H2A 108.7 . . ?
C8 C2 H2A 108.7 . . ?
N C2 H2B 108.7 . . ?
C8 C2 H2B 108.7 . . ?
H2A C2 H2B 107.6 . . ?
N C3 C5 108.7(10) . . ?
N C3 H3A 110.0 . . ?
C5 C3 H3A 110.0 . . ?
N C3 H3B 110.0 . . ?
C5 C3 H3B 110.0 . . ?
H3A C3 H3B 108.3 . . ?
C3 C5 H5A 109.5 . . ?
C3 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C3 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C2 C8 H8A 109.5 . . ?
C2 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C2 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
O3 As1 O2 113.0(6) . . ?
O3 As1 O1 109.4(6) . . ?
O2 As1 O1 107.4(7) . . ?
O3 As1 O4 108.6(5) . . ?
O2 As1 O4 104.9(6) . . ?
O1 As1 O4 113.5(6) . . ?
O8 As2 O7 114.8(6) . 1 ?
O8 As2 O7 114.8(6) . . ?
O7 As2 O7 0.0(12) 1 . ?
O8 As2 O5 110.5(6) . . ?
O7 As2 O5 110.6(5) 1 . ?
O7 As2 O5 110.6(5) . . ?
O8 As2 O6 103.1(6) . . ?
O7 As2 O6 109.7(5) 1 . ?
O7 As2 O6 109.7(5) . . ?
O5 As2 O6 107.6(6) . . ?
O9 As3 O12 113.8(3) . . ?
O9 As3 O11 106.2(5) . . ?
O12 As3 O11 115.8(5) . . ?
O9 As3 O10 109.2(5) . . ?
O12 As3 O10 103.0(5) . . ?
O11 As3 O10 108.6(4) . . ?
C4 N C3 115.9(12) . . ?
C4 N C2 101.6(10) . . ?
C3 N C2 110.7(12) . . ?
C4 N C1 114.2(12) . . ?
C3 N C1 108.8(12) . . ?
C2 N C1 104.9(11) . . ?
As1 O1 H11 109.5 . . ?
As1 O3 H13 109.5 . . ?
As1 O4 H14 109.5 . . ?
As2 O5 H22 109.5 . . ?
As2 O6 H23 109.5 . . ?
O7 O7 As2 0(10) 1 . ?
As3 O12 H31 109.5 . . ?
As3 O10 H33 109.5 . . ?
As3 O11 H34 109.5 . . ?
N C4 C6 112.7(6) . . ?
N C4 H4A 109.1 . . ?
C6 C4 H4A 109.1 . . ?
N C4 H4B 109.1 . . ?
C6 C4 H4B 109.1 . . ?
H4A C4 H4B 107.8 . . ?
C4 C6 H6A 109.5 . . ?
C4 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C4 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C1 C7 H7A 109.5 . . ?
C1 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C1 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
 
loop_
 _geom_hbond_atom_site_label_D
 _geom_hbond_atom_site_label_H
 _geom_hbond_atom_site_label_A
 _geom_hbond_distance_DH
 _geom_hbond_distance_HA
 _geom_hbond_distance_DA
 _geom_hbond_angle_DHA
 _geom_hbond_site_symmetry_A

 
_diffrn_measured_fraction_theta_max    0.977
_diffrn_reflns_theta_full              27.08
_diffrn_measured_fraction_theta_full   0.977
_refine_diff_density_max    1.735
_refine_diff_density_min   -2.448
_refine_diff_density_rms    0.224