#------------------------------------------------------------------------------
#$Date: 2016-03-23 20:08:37 +0100 (Wed 23 de Mar de 2016) $
#$Revision: 179441 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/38/4333802.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_4333802
loop_
_publ_author_name
'Xiang-Ying Qian'
'Jun-Ling Song'
'Jiang-Gao Mao'
_publ_section_title
;
 Silver Pyroarsonates Obtained from Ag(I)-Mediated in Situ Condensation of
 Aryl Arsonate Ligands under Solvothermal Conditions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1843
_journal_page_last               1853
_journal_paper_doi               10.1021/ic301935g
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C12 H10 As2 N2 O9'
_chemical_formula_weight         476.06
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.436(5)
_cell_length_b                   7.843(5)
_cell_length_c                   23.140(14)
_cell_measurement_reflns_used    4244
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.4835
_cell_measurement_theta_min      2.4142
_cell_volume                     1531.0(16)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 13.6612
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Mercury2 (1x1 bin mode)'
_diffrn_measurement_method       CCD_Profile_fitting
_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  0.0843
_diffrn_reflns_av_sigmaI/netI    0.0573
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            11066
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         2.99
_exptl_absorpt_coefficient_mu    4.419
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.2853
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.065
_exptl_crystal_description       Prism
_exptl_crystal_F_000             936
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.488
_refine_diff_density_min         -0.677
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     114
_refine_ls_number_reflns         1751
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0410
_refine_ls_R_factor_gt           0.0349
_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)+(0.0332P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0835
_refine_ls_wR_factor_ref         0.0870
_reflns_number_gt                1504
_reflns_number_total             1751
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic301935g_si_001_1.cif
_cod_data_source_block           C12H10As2N2O9
_cod_original_cell_volume        1531.1(15)
_cod_database_code               4333802
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'-x, y, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'x, -y, 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
As1 As 0.05638(3) 0.03554(4) 0.686620(12) 0.02672(13) Uani 1 1 d .
N1 N -0.0108(4) -0.1195(3) 0.56155(11) 0.0397(6) Uani 1 1 d .
C1 C -0.1419(3) 0.0085(3) 0.64693(12) 0.0277(6) Uani 1 1 d .
C2 C -0.1546(3) -0.0636(3) 0.59200(13) 0.0308(6) Uani 1 1 d .
C3 C -0.2976(4) -0.0869(4) 0.56461(13) 0.0408(7) Uani 1 1 d .
H3A H -0.3021 -0.1343 0.5278 0.049 Uiso 1 1 calc R
C4 C -0.4351(4) -0.0381(4) 0.5930(2) 0.0472(9) Uani 1 1 d .
H4A H -0.5332 -0.0548 0.5756 0.057 Uiso 1 1 calc R
C5 C -0.4263(4) 0.0347(4) 0.64678(19) 0.0437(9) Uani 1 1 d .
H5A H -0.5189 0.0677 0.6655 0.052 Uiso 1 1 calc R
C6 C -0.2798(4) 0.0601(3) 0.67382(14) 0.0333(6) Uani 1 1 d .
H6A H -0.2754 0.1117 0.7100 0.040 Uiso 1 1 calc R
O1 O 0.1523(2) -0.1334(3) 0.70890(9) 0.0409(5) Uani 1 1 d .
O2 O 0.1612(2) 0.1859(3) 0.65204(9) 0.0479(6) Uani 1 1 d .
H2A H 0.2178 0.2362 0.6752 0.072 Uiso 1 1 calc R
O3 O 0.0000 0.1434(3) 0.7500 0.0316(6) Uani 1 2 d S
O4 O 0.1159(3) -0.1001(3) 0.58605(10) 0.0499(6) Uani 1 1 d .
O5 O -0.0251(3) -0.1851(4) 0.51399(11) 0.0596(7) 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
As1 0.0228(2) 0.0314(2) 0.0259(2) 0.00194(10) -0.00055(9) 0.00096(10)
N1 0.0500(17) 0.0380(14) 0.0313(15) -0.0007(12) 0.0028(12) 0.0073(11)
C1 0.0283(15) 0.0248(11) 0.0299(15) 0.0016(11) -0.0042(11) -0.0007(10)
C2 0.0342(15) 0.0284(12) 0.0299(15) 0.0015(11) -0.0007(12) 0.0017(11)
C3 0.047(2) 0.0387(15) 0.0367(17) -0.0019(14) -0.0103(14) -0.0053(13)
C4 0.037(2) 0.048(2) 0.057(3) 0.0055(17) -0.0154(15) -0.0090(13)
C5 0.0246(17) 0.0459(19) 0.060(3) 0.0039(16) -0.0012(14) 0.0025(12)
C6 0.0283(15) 0.0367(15) 0.0348(15) 0.0008(12) 0.0006(13) -0.0002(11)
O1 0.0417(13) 0.0452(12) 0.0357(11) 0.0030(10) -0.0024(10) 0.0193(9)
O2 0.0465(14) 0.0616(14) 0.0357(12) 0.0097(11) -0.0030(10) -0.0237(11)
O3 0.0360(15) 0.0267(13) 0.0320(15) 0.000 0.0001(13) 0.000
O4 0.0370(14) 0.0728(16) 0.0398(13) -0.0016(12) 0.0026(11) 0.0134(12)
O5 0.0787(18) 0.0655(15) 0.0346(13) -0.0181(13) 0.0040(12) 0.0069(14)
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'
As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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_3
O1 As1 O2 117.34(12) .
O1 As1 O3 105.11(10) .
O2 As1 O3 101.66(11) .
O1 As1 C1 119.49(11) .
O2 As1 C1 107.97(11) .
O3 As1 C1 102.50(9) .
O4 N1 O5 123.9(3) .
O4 N1 C2 117.6(3) .
O5 N1 C2 118.5(3) .
C6 C1 C2 117.7(3) .
C6 C1 As1 119.1(2) .
C2 C1 As1 123.2(2) .
C3 C2 C1 122.8(3) .
C3 C2 N1 117.6(3) .
C1 C2 N1 119.6(3) .
C2 C3 C4 118.6(3) .
C2 C3 H3A 120.7 .
C4 C3 H3A 120.7 .
C5 C4 C3 120.0(3) .
C5 C4 H4A 120.0 .
C3 C4 H4A 120.0 .
C4 C5 C6 120.8(3) .
C4 C5 H5A 119.6 .
C6 C5 H5A 119.6 .
C1 C6 C5 120.1(3) .
C1 C6 H6A 120.0 .
C5 C6 H6A 120.0 .
As1 O2 H2A 109.5 .
As1 O3 As1 122.48(15) 3_556
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
As1 O1 1.636(2) .
As1 O2 1.677(2) .
As1 O3 1.7588(14) .
As1 C1 1.920(3) .
N1 O4 1.220(4) .
N1 O5 1.221(3) .
N1 C2 1.470(4) .
C1 C6 1.380(4) .
C1 C2 1.396(4) .
C2 C3 1.375(4) .
C3 C4 1.387(5) .
C3 H3A 0.9300 .
C4 C5 1.371(6) .
C4 H4A 0.9300 .
C5 C6 1.399(4) .
C5 H5A 0.9300 .
C6 H6A 0.9300 .
O2 H2A 0.8200 .
O3 As1 1.7588(14) 3_556
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
O2 H2A O1 0.82 1.69 2.494(3) 166.3 8_665
