# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 #TrackingRef '- all_cif_dranka.cif' #========================================================= # 1. SUBMISSION DETAILS _publ_contact_author ; Dr. Maciej Dranka, Warsaw University of Technology Faculty of Chemistry Department of Inorganic Chemistry and Solid State Technology Noakowskiego 3, PL-00-664 Warszawa Poland ; _publ_contact_author_fax '048 22 6282741' _publ_contact_author_email mdranka@ch.pw.edu.pl #========================================================= # 2. TITLE AND AUTHOR LIST _publ_section_title ; Supramolecular structure of ammonium polyoxoarsenates(III) ; loop_ _publ_author_name _publ_author_address P.A.Gunka ; Warsaw University of Technology Faculty of Chemistry Department of Inorganic Chemistry and Solid State Technology Noakowskiego 3, PL-00-664 Warszawa Poland e-mail: piogun@ch.pw.edu.pl ; 'Maciej Dranka' ; Warsaw University of Technology Faculty of Chemistry Department of Inorganic Chemistry and Solid State Technology Noakowskiego 3, PL-00-664 Warszawa Poland e-mail: mdranka@ch.pw.edu.pl ; 'Janusz Zachara' ; Warsaw University of Technology Faculty of Chemistry Department of Inorganic Chemistry and Solid State Technology Noakowskiego 3, PL-00-664 Warszawa Poland e-mail: janzac@ch.pw.edu.pl ; _publ_contact_author_name 'Dr. Maciej Dranka' # 3. CRYSTAL DATA #========================================================================= # COMPOUND 1 - LOW-TEMPERATURE DATA data_aa_ump _database_code_depnum_ccdc_archive 'CCDC 810890' #TrackingRef '- all_cif_dranka.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ammonium metaarsenate(III) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'As O2, H4 N' _chemical_formula_sum 'As H4 N O2' _chemical_formula_weight 124.96 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall -P_2ybc _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z+1/2' _cell_length_a 5.24562(17) _cell_length_b 4.73223(13) _cell_length_c 12.3051(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.426(3) _cell_angle_gamma 90.00 _cell_volume 305.446(15) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 18603 _cell_measurement_theta_min 3.3039 _cell_measurement_theta_max 37.7603 _exptl_crystal_description platelet _exptl_crystal_colour colourless _exptl_crystal_size_max 0.69 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.717 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 240 _exptl_absorpt_coefficient_mu 10.879 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.20018 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.54 (release 04-12-2009 CrysAlis171 .NET) (compiled Dec 4 2009,17:18:47) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; The crystals are twinned. The twin matrix is: 1 0 0 0 -1 0 0 0 -1 The twin obliquity equals 0.426(3)deg which causes substantial overlapping of reflections. The diffraction data were not untwinned during the integration process. The twin law was determined during the indexation process and untwinning was carried out during the structure refinement in SHELXL-97. The twin ratio was refined to 0.635 : 0.365. ; _diffrn_ambient_temperature 100(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 '\k-geometry diffractometer' _diffrn_measurement_device_type 'Xcalibur, Atlas, Gemini ultra' _diffrn_measurement_method 'area detector \w scans' _diffrn_detector_area_resol_mean 10.3347 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31209 _diffrn_reflns_av_R_equivalents 0.0756 _diffrn_reflns_av_sigmaI/netI 0.0413 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.31 _diffrn_reflns_theta_max 37.81 _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 37.81 _diffrn_measured_fraction_theta_full 0.985 _reflns_number_total 1610 _reflns_number_gt 1506 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'CrysAlisPro (Oxford Diffraction Ltd. 2009)' _computing_cell_refinement 'CrysAlisPro (Oxford Diffraction Ltd. 2009)' _computing_data_reduction 'CrysAlisPro (Oxford Diffraction Ltd. 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond v3.2 (Brandenburg, 2010)' _computing_publication_material ; SHELXL-97 (Sheldrick, 1997) PLATON, A.L.Spek (2010), Utrecht Univ., Utrecht, The Netherlands ; _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^)+(0.0211P)^2^+1.1134P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1610 _refine_ls_number_parameters 41 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0308 _refine_ls_R_factor_gt 0.0285 _refine_ls_wR_factor_ref 0.0681 _refine_ls_wR_factor_gt 0.0676 _refine_ls_goodness_of_fit_ref 1.188 _refine_ls_restrained_S_all 1.188 _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 As1 As 0.21019(6) 0.22958(4) 0.24468(3) 0.00548(6) Uani 1 1 d . . . O1 O 0.2595(4) 0.2551(4) 0.10741(18) 0.0080(3) Uani 1 1 d . . . O2 O -0.1140(4) 0.3631(3) 0.2493(2) 0.0107(3) Uani 1 1 d . . . N1 N 0.2540(4) 0.7533(6) -0.0074(2) 0.0084(3) Uani 1 1 d G . . H1 H 0.2480 0.5960 0.0350 0.013 Uiso 1 1 d G . . H2 H 0.2524 0.9099 0.0355 0.013 Uiso 1 1 d G . . H3 H 0.1164 0.7561 -0.0528 0.013 Uiso 1 1 d G . . H4 H 0.3994 0.7511 -0.0473 0.013 Uiso 1 1 d G . . 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 0.00869(9) 0.00444(8) 0.00333(9) -0.00006(8) 0.00176(12) -0.00059(7) O1 0.0120(9) 0.0060(7) 0.0061(7) 0.0004(5) 0.0025(6) -0.0005(5) O2 0.0129(8) 0.0060(6) 0.0133(8) -0.0018(8) 0.0070(11) 0.0002(5) N1 0.0109(8) 0.0077(7) 0.0066(8) 0.0003(6) 0.0013(8) -0.0007(11) _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 As1 O1 1.715(2) . ? As1 O2 1.8079(16) 2_545 ? As1 O2 1.8152(19) . ? N1 H1 0.9100 . ? N1 H2 0.9100 . ? N1 H3 0.9100 . ? N1 H4 0.9100 . ? 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 O1 As1 O2 98.77(11) . 2_545 ? O1 As1 O2 98.88(12) . . ? O2 As1 O2 94.06(5) 2_545 . ? As1 O2 As1 126.66(10) 2 . ? H1 N1 H2 109.5 . . ? H1 N1 H3 109.5 . . ? H2 N1 H3 109.5 . . ? H1 N1 H4 109.5 . . ? H2 N1 H4 109.5 . . ? H3 N1 H4 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 _geom_hbond_publ_flag N1 H1 O1 0.9100 1.8400 2.749(3) 173.00 . yes N1 H2 O1 0.9100 1.8600 2.763(3) 173.00 1_565 yes N1 H3 O1 0.9100 2.0800 2.953(3) 161.00 3_565 yes N1 H3 O2 0.9100 2.4800 3.110(3) 126.00 3_565 yes N1 H4 O1 0.9100 1.9400 2.842(3) 170.00 3_665 yes _refine_diff_density_max 1.166 _refine_diff_density_min -1.540 _refine_diff_density_rms 0.187 #========================================================================= # COMPOUND 1 - ROOM-TEMPERATURE DATA data_asmn _database_code_depnum_ccdc_archive 'CCDC 810891' #TrackingRef '- all_cif_dranka.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ammonium metaarsenate(III) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'As O2, H4 N' _chemical_formula_sum 'As H4 N O2' _chemical_formula_weight 124.96 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source N N 0.0061 0.0033 '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' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall -P_2ybc _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z+1/2' _cell_length_a 5.3555(13) _cell_length_b 4.7543(8) _cell_length_c 12.313(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.124(19) _cell_angle_gamma 90.00 _cell_volume 313.52(12) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 3.30 _cell_measurement_theta_max 14.44 _exptl_crystal_description platelet _exptl_crystal_colour colourless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.647 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 240 _exptl_absorpt_coefficient_mu 10.599 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.520 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ; XEMP, Siemens P3 Software (1990) Ellipsoid correction with mean mu*r = 0.0940 based on 12 psi-scanned reflections. ; _exptl_special_details ; The crystals are twinned. The twin matrix is: 1 0 0 0 -1 0 0 0 -1 The twin obliquity equals 0.124(19)deg which causes substantial overlapping of reflections. The diffraction data were not untwinned during the integration process. Untwinning was carried out during the structure refinement in SHELXL-97. The twin ratio was refined to 0.788 : 0.212. ; _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 'four-circle diffractometer' _diffrn_measurement_device_type 'Siemens P3' _diffrn_measurement_method 'profile data from \q/2\q scans' _diffrn_detector 'scintillation counter' _diffrn_standards_number 2 _diffrn_standards_interval_count 70 _diffrn_standards_decay_% 0 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 0 2 -2 2 0 -4 _diffrn_reflns_number 1805 _diffrn_reflns_av_R_equivalents 0.0308 _diffrn_reflns_av_sigmaI/netI 0.0311 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.31 _diffrn_reflns_theta_max 27.56 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.56 _diffrn_measured_fraction_theta_full 1.000 _diffrn_special_details ; 2\q scan width: 2.4\% plus K\a1-K\a2 separation; variable scan speed: 4.2 to 29.3\%(2\q)/min, background/peak time ratio 0.5 ; _reflns_number_total 730 _reflns_number_gt 692 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Siemens P3 software' _computing_cell_refinement 'Siemens P3 software' _computing_data_reduction 'XDISK, Siemens P3 software' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; Diamond v3.2 (Brandenburg, 2010)' Ortep-3 for Windows, L.J.Farrugia (1997) J.Appl.Cryst. 30, 565. ; _computing_publication_material ; SHELXL-97 (Sheldrick, 1997) PLATON, A.L.Spek (2010), Utrecht Univ., Utrecht, The Netherlands ; _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^)+(0.0157P)^2^+2.9954P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.011(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 730 _refine_ls_number_parameters 42 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0437 _refine_ls_R_factor_gt 0.0410 _refine_ls_wR_factor_ref 0.1039 _refine_ls_wR_factor_gt 0.1028 _refine_ls_goodness_of_fit_ref 1.461 _refine_ls_restrained_S_all 1.461 _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 As1 As 0.70643(16) 0.76793(13) 0.25646(9) 0.0174(3) Uani 1 1 d . . . N1 N 0.7566(13) 0.2490(17) 0.5085(7) 0.0221(14) Uani 1 1 d G . . H1 H 0.7535 0.3966 0.4640 0.029 Uiso 1 1 d G . . H2 H 0.7573 0.0913 0.4695 0.029 Uiso 1 1 d G . . H3 H 0.6220 0.2519 0.5507 0.029 Uiso 1 1 d G . . H4 H 0.8934 0.2560 0.5495 0.029 Uiso 1 1 d G . . O1 O 0.7584(12) 0.7450(11) 0.3932(5) 0.0221(13) Uani 1 1 d . . . O2 O 0.3913(11) 0.6302(10) 0.2525(6) 0.0292(13) 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 0.0246(5) 0.0134(4) 0.0141(4) -0.0002(3) -0.0018(3) 0.0008(3) N1 0.029(3) 0.018(3) 0.019(3) -0.001(2) -0.001(4) -0.001(4) O1 0.033(4) 0.018(3) 0.015(2) 0.0022(19) -0.007(2) 0.001(2) O2 0.035(3) 0.016(2) 0.037(3) -0.009(3) -0.019(4) 0.000(2) _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 As1 O1 1.710(6) . ? As1 O2 1.803(5) 2_655 ? As1 O2 1.811(6) . ? N1 H1 0.8900 . ? N1 H2 0.8900 . ? N1 H3 0.8900 . ? N1 H4 0.8900 . ? 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 O1 As1 O2 99.6(3) . 2_655 ? O1 As1 O2 98.8(3) . . ? O2 As1 O2 94.21(16) 2_655 . ? H1 N1 H2 109.5 . . ? H1 N1 H3 109.5 . . ? H2 N1 H3 109.5 . . ? H1 N1 H4 109.5 . . ? H2 N1 H4 109.5 . . ? H3 N1 H4 109.5 . . ? As1 O2 As1 128.1(3) 2_645 . ? 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 _geom_hbond_publ_flag N1 H1 O1 0.8900 1.8700 2.753(10) 170.00 . yes N1 H2 O1 0.8900 1.9000 2.785(10) 177.00 1_545 yes N1 H3 O1 0.8900 2.1500 3.015(10) 163.00 3_666 yes N1 H3 O2 0.8900 2.4900 3.103(11) 127.00 3_666 yes N1 H4 O1 0.8900 1.9900 2.863(10) 166.00 3_766 yes _refine_diff_density_max 1.442 _refine_diff_density_min -1.583 _refine_diff_density_rms 0.174 #========================================================================= # COMPOUND 2 data_eda_aoptsh _database_code_depnum_ccdc_archive 'CCDC 810892' #TrackingRef '- all_cif_dranka.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ethylenediamonnium metaarsenate(III) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C2 H10 N2, 2(As O2)' _chemical_formula_sum 'C2 H10 As2 N2 O4' _chemical_formula_weight 275.96 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' _symmetry_space_group_name_Hall -C_2yc _symmetry_Int_Tables_number 15 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' '-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 17.9898(15) _cell_length_b 4.64836(12) _cell_length_c 12.8789(11) _cell_angle_alpha 90.00 _cell_angle_beta 132.957(14) _cell_angle_gamma 90.00 _cell_volume 788.2(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6725 _cell_measurement_theta_min 4.32 _cell_measurement_theta_max 29.33 _exptl_crystal_description platelet _exptl_crystal_colour colourles _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.326 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 536 _exptl_absorpt_coefficient_mu 8.458 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.204 _exptl_absorpt_correction_T_max 0.681 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 -1 0 0.1040 -1 0 0 0.0370 0 0 1 0.0709 0 0 -1 0.0175 -1 1 -2 0.0957 1 0 0 0.0130 -1 0 1 0.1006 0 1 0 0.1258 _exptl_absorpt_process_details ; CrysAlisPro (Oxford Diffraction Ltd., 2010) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 '\k-geometry diffractometer' _diffrn_measurement_device_type 'Xcalibur, Atlas, Gemini ultra' _diffrn_measurement_method 'area detector \w scans' _diffrn_detector_area_resol_mean 10.3347 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12522 _diffrn_reflns_av_R_equivalents 0.0927 _diffrn_reflns_av_sigmaI/netI 0.0651 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 4.32 _diffrn_reflns_theta_max 29.40 _diffrn_measured_fraction_theta_max 0.955 _diffrn_reflns_theta_full 25.24 _diffrn_measured_fraction_theta_full 0.997 _reflns_number_total 1043 _reflns_number_gt 877 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'CrysAlisPro (Oxford Diffraction Ltd. 2009)' _computing_cell_refinement 'CrysAlisPro (Oxford Diffraction Ltd. 2009)' _computing_data_reduction 'CrysAlisPro (Oxford Diffraction Ltd. 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond v3.2 (Brandenburg, 2010)' _computing_publication_material ; SHELXL-97 (Sheldrick, 1997) PLATON, A.L.Spek (2010), Utrecht Univ., Utrecht, The Netherlands ; _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^)+(0.0446P)^2^+0.0000P] 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 refxyz _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1043 _refine_ls_number_parameters 44 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0359 _refine_ls_R_factor_gt 0.0289 _refine_ls_wR_factor_ref 0.0720 _refine_ls_wR_factor_gt 0.0704 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _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 As1 As 0.33170(2) 0.52049(5) 0.34407(3) 0.01035(13) Uani 1 1 d . . . O1 O 0.33679(18) 0.4988(3) 0.4815(2) 0.0131(4) Uani 1 1 d . . . O2 O 0.20241(14) 0.3977(4) 0.20130(19) 0.0179(4) Uani 1 1 d . . . C1 C 0.4595(2) 0.0019(5) 0.7534(3) 0.0120(6) Uani 1 1 d . . . H1D H 0.4671 -0.1703 0.8051 0.014 Uiso 1 1 calc R . . H1E H 0.4668 0.1749 0.8045 0.014 Uiso 1 1 calc R . . N1 N 0.3588(2) 0.0009(3) 0.6077(2) 0.0098(5) Uani 1 1 d . . . H1A H 0.3097 0.0057 0.6107 0.015 Uiso 1 1 calc R . . H1B H 0.3517 -0.1616 0.5622 0.015 Uiso 1 1 calc R . . H1C H 0.3527 0.1580 0.5602 0.015 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 As1 0.0154(2) 0.00392(16) 0.0151(2) 0.00102(8) 0.01177(17) 0.00091(8) O1 0.0198(11) 0.0068(9) 0.0143(10) 0.0000(5) 0.0123(9) -0.0012(6) O2 0.0222(10) 0.0041(8) 0.0191(10) 0.0015(7) 0.0108(8) -0.0001(8) C1 0.0111(14) 0.0106(12) 0.0131(15) 0.0007(8) 0.0078(13) 0.0003(8) N1 0.0097(11) 0.0068(10) 0.0134(12) 0.0000(7) 0.0080(10) 0.0002(7) _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 As1 O1 1.711(2) . ? As1 O2 1.8131(19) . ? As1 O2 1.8178(18) 4 ? C1 N1 1.473(4) . ? C1 C1 1.518(6) 2_656 ? 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 O1 As1 O2 99.08(10) . . ? O1 As1 O2 99.08(8) . 4 ? O2 As1 O2 93.37(6) . 4 ? As1 O2 As1 123.25(10) . 4_545 ? N1 C1 C1 108.9(3) . 2_656 ? 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 _geom_hbond_publ_flag N1 H1C O1 0.9100 1.8000 2.698(3) 171.00 . yes N1 H1B O1 0.9100 1.8100 2.715(3) 175.00 1_545 yes N1 H1A O1 0.9100 2.0200 2.862(5) 153.00 7_556 yes _refine_diff_density_max 1.015 _refine_diff_density_min -0.844 _refine_diff_density_rms 0.165 #========================================================================= # COMPOUND 3 data_bznsh _database_code_depnum_ccdc_archive 'CCDC 810893' #TrackingRef '- all_cif_dranka.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; benzylammonium metaarsenate(III) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C7 H10 N, As O2' _chemical_formula_sum 'C7 H10 As N O2' _chemical_formula_weight 215.08 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall -P_2ybc _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y+1/2, z+1/2' _cell_length_a 15.4872(9) _cell_length_b 4.63256(13) _cell_length_c 12.4361(6) _cell_angle_alpha 90.00 _cell_angle_beta 112.001(6) _cell_angle_gamma 90.00 _cell_volume 827.26(7) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2647 _cell_measurement_theta_min 3.2711 _cell_measurement_theta_max 29.2952 _exptl_crystal_description platelet _exptl_crystal_colour colourless _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.727 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 432 _exptl_absorpt_coefficient_mu 4.057 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.484 _exptl_absorpt_correction_T_max 0.962 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 0 -1 0.0394 -1 1 2 0.1540 -1 0 0 0.0020 1 0 0 0.0074 1 -1 -2 0.1829 0 0 1 0.0412 0 1 0 0.1868 0 -1 0 0.2220 _exptl_absorpt_process_details ; CrysAlisPro (Oxford Diffraction Ltd., 2010) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 '\k-geometry diffractometer' _diffrn_measurement_device_type 'Xcalibur, Atlas, Gemini ultra' _diffrn_measurement_method 'area detector \w scans' _diffrn_detector_area_resol_mean 10.3347 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7047 _diffrn_reflns_av_R_equivalents 0.0807 _diffrn_reflns_av_sigmaI/netI 0.1440 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.28 _diffrn_reflns_theta_max 24.99 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.998 _reflns_number_total 1463 _reflns_number_gt 981 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'CrysAlisPro (Oxford Diffraction Ltd. 2009)' _computing_cell_refinement 'CrysAlisPro (Oxford Diffraction Ltd. 2009)' _computing_data_reduction 'CrysAlisPro (Oxford Diffraction Ltd. 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond v3.2 (Brandenburg, 2010)' _computing_publication_material ; SHELXL-97 (Sheldrick, 1997) PLATON, A.L.Spek (2010), Utrecht Univ., Utrecht, The Netherlands ; _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^)+(0.0462P)^2^+0.0000P] 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 refxyz _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1463 _refine_ls_number_parameters 101 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0715 _refine_ls_R_factor_gt 0.0410 _refine_ls_wR_factor_ref 0.0878 _refine_ls_wR_factor_gt 0.0822 _refine_ls_goodness_of_fit_ref 0.911 _refine_ls_restrained_S_all 0.911 _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 As1 As 0.42509(4) 0.77377(9) 0.69945(5) 0.01280(19) Uani 1 1 d . . . O1 O 0.4211(2) 0.7370(7) 0.5616(3) 0.0149(8) Uani 1 1 d . . . O2 O 0.5444(2) 0.6543(7) 0.7775(3) 0.0172(9) Uani 1 1 d . . . N1 N 0.3945(3) 0.2430(9) 0.4428(3) 0.0128(9) Uani 1 1 d . . . H1A H 0.4401 0.2404 0.4133 0.019 Uiso 1 1 calc R . . H1B H 0.3982 0.0801 0.4852 0.019 Uiso 1 1 calc R . . H1C H 0.4018 0.4006 0.4890 0.019 Uiso 1 1 calc R . . C7 C 0.3020(3) 0.2555(11) 0.3463(4) 0.0170(11) Uani 1 1 d . . . H7A H 0.3049 0.1496 0.2785 0.020 Uiso 1 1 calc R . . H7B H 0.2862 0.4591 0.3230 0.020 Uiso 1 1 calc R . . C1 C 0.2270(4) 0.1259(10) 0.3807(5) 0.0155(12) Uani 1 1 d . . . C2 C 0.1638(4) -0.0649(11) 0.3060(6) 0.0272(15) Uani 1 1 d . . . H2 H 0.1669 -0.1083 0.2329 0.033 Uiso 1 1 calc R . . C3 C 0.0955(4) -0.1936(12) 0.3385(6) 0.0344(17) Uani 1 1 d . . . H3 H 0.0527 -0.3267 0.2879 0.041 Uiso 1 1 calc R . . C4 C 0.0903(4) -0.1277(13) 0.4428(6) 0.0349(17) Uani 1 1 d . . . H4 H 0.0439 -0.2164 0.4645 0.042 Uiso 1 1 calc R . . C5 C 0.1513(4) 0.0653(12) 0.5171(6) 0.0306(16) Uani 1 1 d . . . H5 H 0.1469 0.1121 0.5892 0.037 Uiso 1 1 calc R . . C6 C 0.2196(4) 0.1906(11) 0.4851(5) 0.0206(13) Uani 1 1 d . . . H6 H 0.2620 0.3237 0.5362 0.025 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 As1 0.0230(3) 0.0037(2) 0.0148(3) -0.0010(3) 0.0106(2) -0.0010(3) O1 0.026(2) 0.0082(16) 0.0133(18) 0.0018(16) 0.0103(16) 0.0019(17) O2 0.027(2) 0.0058(15) 0.017(2) -0.0019(14) 0.0055(17) -0.0048(15) N1 0.021(2) 0.0053(18) 0.017(2) -0.0034(19) 0.0125(19) -0.001(2) C7 0.025(3) 0.011(2) 0.015(3) -0.004(3) 0.007(2) 0.003(3) C1 0.018(3) 0.007(2) 0.022(3) 0.001(2) 0.008(3) 0.005(2) C2 0.030(4) 0.016(3) 0.030(4) 0.004(3) 0.005(3) 0.008(3) C3 0.022(4) 0.013(3) 0.058(5) 0.002(3) 0.003(3) -0.001(3) C4 0.021(4) 0.029(3) 0.059(5) 0.018(3) 0.020(4) 0.008(3) C5 0.027(4) 0.028(3) 0.040(4) 0.004(3) 0.017(3) 0.001(3) C6 0.019(3) 0.017(3) 0.026(3) 0.001(3) 0.008(3) 0.000(2) _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 As1 O1 1.701(3) . ? As1 O2 1.822(4) . ? As1 O2 1.820(3) 2_656 ? N1 C7 1.486(6) . ? C7 C1 1.505(7) . ? C1 C6 1.379(8) . ? C1 C2 1.386(8) . ? C2 C3 1.400(9) . ? C3 C4 1.364(9) . ? C4 C5 1.375(9) . ? C5 C6 1.388(8) . ? 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 O1 As1 O2 98.82(16) . . ? O1 As1 O2 99.50(16) . 2_656 ? O2 As1 O2 93.36(11) 2_656 . ? As1 O2 As1 122.00(18) 2_646 . ? N1 C7 C1 111.6(4) . . ? C6 C1 C2 118.9(5) . . ? C6 C1 C7 121.8(5) . . ? C2 C1 C7 119.3(5) . . ? C1 C2 C3 119.9(6) . . ? C4 C3 C2 120.0(6) . . ? C3 C4 C5 120.9(6) . . ? C4 C5 C6 119.0(6) . . ? C1 C6 C5 121.3(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 _geom_hbond_publ_flag N1 H1C O1 0.9100 1.7700 2.671(5) 171.00 . yes N1 H1B O1 0.9100 1.8200 2.719(5) 170.00 1_545 yes N1 H1A O1 0.9100 2.0600 2.878(6) 150.00 3_666 yes N1 H1A O2 0.9100 2.5200 3.251(5) 138.00 3_666 yes _refine_diff_density_max 1.507 _refine_diff_density_min -0.762 _refine_diff_density_rms 0.153 #========================================================================= # COMPOUND 4 data_ma2optsh _database_code_depnum_ccdc_archive 'CCDC 810894' #TrackingRef '- all_cif_dranka.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; methylammonium metaarsenate(III) hydrate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'As O2, C H6 N, H2 O' _chemical_formula_sum 'C H8 As N O3' _chemical_formula_weight 157.00 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' As As 0.0499 2.0058 '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 monoclinic _symmetry_space_group_name_H-M 'P 21' _symmetry_space_group_name_Hall 'P 2yb' _symmetry_Int_Tables_number 4 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 5.47942(18) _cell_length_b 4.65117(16) _cell_length_c 10.4691(3) _cell_angle_alpha 90.00 _cell_angle_beta 94.937(3) _cell_angle_gamma 90.00 _cell_volume 265.822(15) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3602 _cell_measurement_theta_min 3.72 _cell_measurement_theta_max 29.52 _exptl_crystal_description platelet _exptl_crystal_colour colourless _exptl_crystal_size_max 0.58 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.962 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 156 _exptl_absorpt_coefficient_mu 6.253 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.186 _exptl_absorpt_correction_T_max 0.724 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist -8 -1 2 0.2449 0 0 1 0.0328 0 1 0 0.1623 1 -3 0 0.1111 0 0 -1 0.0190 7 3 -2 0.3059 7 -4 -1 0.2045 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 '\k-geometry diffractometer' _diffrn_measurement_device_type 'Xcalibur, Atlas, Gemini ultra' _diffrn_measurement_method 'area detector \w scans' _diffrn_detector_area_resol_mean 10.3347 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4230 _diffrn_reflns_av_R_equivalents 0.0319 _diffrn_reflns_av_sigmaI/netI 0.0255 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.73 _diffrn_reflns_theta_max 29.58 _diffrn_measured_fraction_theta_max 0.917 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.998 _reflns_number_total 1299 _reflns_number_gt 1224 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.54 (release 04-12-2009 CrysAlis171 .NET) (compiled Dec 4 2009,17:18:47) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.54 (release 04-12-2009 CrysAlis171 .NET) (compiled Dec 4 2009,17:18:47) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.54 (release 04-12-2009 CrysAlis171 .NET) (compiled Dec 4 2009,17:18:47) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond v3.2 (Brandenburg, 2010)' _computing_publication_material ; SHELXL-97 (Sheldrick, 1997) PLATON, A.L.Spek (2010), Utrecht Univ., Utrecht, The Netherlands ; _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^)+(0.0274P)^2^+0.0105P] 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 constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.031(3) _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, 538 Friedel pairs' _refine_ls_abs_structure_Flack 0.410(17) _refine_ls_number_reflns 1299 _refine_ls_number_parameters 62 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0188 _refine_ls_R_factor_gt 0.0172 _refine_ls_wR_factor_ref 0.0426 _refine_ls_wR_factor_gt 0.0423 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _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 As1 As 0.55951(3) 0.3829 0.602567(17) 0.00563(8) Uani 1 1 d . . . O1 O 0.3036(2) 0.3805(11) 0.68409(14) 0.0101(3) Uani 1 1 d . . . O2 O 0.4308(3) 0.5081(4) 0.44704(18) 0.0096(3) Uani 1 1 d . . . C1 C -0.0370(4) 0.8886(14) 0.8338(2) 0.0159(4) Uani 1 1 d . . . H1D H 0.1033 0.8479 0.8956 0.019 Uiso 1 1 calc R . . H1E H -0.1630 0.7412 0.8408 0.019 Uiso 1 1 calc R . . H1F H -0.1046 1.0778 0.8520 0.019 Uiso 1 1 calc R . . N1 N 0.0439(3) 0.8868(12) 0.70158(16) 0.0098(3) Uani 1 1 d . . . H1A H -0.0881 0.8592 0.6440 0.012 Uiso 1 1 calc R . . H1B H 0.1157 1.0580 0.6856 0.012 Uiso 1 1 calc R . . H1C H 0.1536 0.7420 0.6943 0.012 Uiso 1 1 calc R . . O3 O 0.5073(4) 0.4158(9) 0.93437(19) 0.0208(6) Uani 1 1 d G . . H3A H 0.4155 0.3903 0.8650 0.033 Uiso 1 1 d G . . H3B H 0.4886 0.2681 0.9811 0.033 Uiso 1 1 d G . . 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 0.00636(11) 0.00451(11) 0.00590(11) -0.00035(19) -0.00008(6) -0.00020(19) O1 0.0118(6) 0.0076(6) 0.0114(7) -0.0001(18) 0.0045(5) -0.0002(18) O2 0.0161(9) 0.0054(7) 0.0072(8) 0.0016(7) -0.0002(6) -0.0022(7) C1 0.0154(9) 0.0176(11) 0.0154(11) 0.005(3) 0.0048(8) 0.000(3) N1 0.0083(7) 0.0087(8) 0.0125(8) 0.002(2) 0.0009(6) 0.003(2) O3 0.0374(9) 0.014(2) 0.0101(8) 0.0011(11) -0.0032(7) -0.0027(12) _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 As1 O1 1.7030(13) . ? As1 O2 1.8137(19) . ? As1 O2 1.8212(19) 2_646 ? C1 N1 1.490(3) . ? C1 H1D 0.9800 . ? C1 H1E 0.9800 . ? C1 H1F 0.9800 . ? N1 H1A 0.9100 . ? N1 H1B 0.9100 . ? N1 H1C 0.9100 . ? O3 H3A 0.8550 . ? O3 H3B 0.8549 . ? 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 O1 As1 O2 100.30(9) . . ? O1 As1 O2 100.48(18) . 2_646 ? O2 As1 O2 94.01(6) . 2_646 ? As1 O2 As1 123.00(10) . 2_656 ? N1 C1 H1D 109.5 . . ? N1 C1 H1E 109.5 . . ? H1D C1 H1E 109.5 . . ? N1 C1 H1F 109.5 . . ? H1D C1 H1F 109.5 . . ? H1E C1 H1F 109.5 . . ? C1 N1 H1B 109.5 . . ? C1 N1 H1A 109.5 . . ? H1B N1 H1A 109.5 . . ? C1 N1 H1C 109.5 . . ? H1B N1 H1C 109.5 . . ? H1A N1 H1C 109.5 . . ? H3A O3 H3B 106.5 . . ? 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 _geom_hbond_publ_flag N1 H1C O1 0.9100 1.8800 2.766(7) 164.00 . yes N1 H1B O1 0.9100 1.8200 2.716(6) 168.00 1_565 yes N1 H1A O2 0.9100 2.1500 2.968(3) 150.00 2_556 yes O3 H3A O1 0.8600 1.9400 2.763(2) 161.00 . yes O3 H3B O3 0.8500 1.8600 2.7059 169.00 2_647 yes _refine_diff_density_max 0.411 _refine_diff_density_min -0.341 _refine_diff_density_rms 0.079 #========================================================================= # COMPOUND 5 data_etol15m _database_code_depnum_ccdc_archive 'CCDC 810895' #TrackingRef '- all_cif_dranka.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ethanolammonium metaarsenate(III) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'As O2, C2 H8 N O' _chemical_formula_sum 'C2 H8 As N O3' _chemical_formula_weight 169.01 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21' _symmetry_space_group_name_Hall 'P 2yb' _symmetry_Int_Tables_number 4 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 4.7049(4) _cell_length_b 18.8608(16) _cell_length_c 6.1721(5) _cell_angle_alpha 90.00 _cell_angle_beta 91.821(9) _cell_angle_gamma 90.00 _cell_volume 547.42(8) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3389 _cell_measurement_theta_min 3.24 _cell_measurement_theta_max 32.89 _exptl_crystal_description platelet _exptl_crystal_colour colourles _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.055 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 336 _exptl_absorpt_coefficient_mu 6.091 _exptl_absorpt_correction_T_min 0.675 _exptl_absorpt_correction_T_max 0.906 _exptl_absorpt_correction_type analytical loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 0 -1 0.0216 0 0 1 0.0212 1 0 1 0.0323 -1 0 1 0.0572 1 0 -1 0.0225 -1 0 -1 0.0457 0 1 0 0.0094 0 -1 0 0.0069 _exptl_absorpt_process_details ; CrysAlisPro (Oxford Diffraction Ltd., 2010) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; The crystals are twinned. The twin matrix is: -1 0 0 0 -1 0 0 0 1 The twin law was determined during the indexation process. Data reduction was carried out for both components and the profiles of partially overlapping reflections were deconvoluted. Overlap threshold was set to 0.800. The twin ratio was refined to 0.640 : 0.360. ; _diffrn_ambient_temperature 100(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 '\k-geometry diffractometer' _diffrn_measurement_device_type 'Xcalibur, Atlas, Gemini ultra' _diffrn_measurement_method 'area detector \w scans' _diffrn_detector_area_resol_mean 10.3347 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2439 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0569 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 3.47 _diffrn_reflns_theta_max 32.89 _diffrn_measured_fraction_theta_max 0.964 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _reflns_number_total 2439 _reflns_number_gt 2097 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'CrysAlisPro (Oxford Diffraction Ltd. 2009)' _computing_cell_refinement 'CrysAlisPro (Oxford Diffraction Ltd. 2009)' _computing_data_reduction 'CrysAlisPro (Oxford Diffraction Ltd. 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond v3.2 (Brandenburg, 2010)' _computing_publication_material ; SHELXL-97 (Sheldrick, 1997) PLATON, A.L.Spek (2010), Utrecht Univ., Utrecht, The Netherlands ; _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. The hklf5 file was merged using the MERGEHKLF5 program (M. Lutz, M. M. Schreurs; Laboratory for Crystal and Structural Chemistry, Bijvoet Center for Biomolecular Research, Padualaan 8, NL-3584 CH Utrecht, The Netherlands). The refinement of ADPs of O2 and O6 atoms was restrained (s.u. of 0.005). ; _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^)+(0.0383P)^2^+0.4043P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881, 1146 Friedel pairs' _refine_ls_abs_structure_Flack 0.00(3) _refine_ls_number_reflns 2439 _refine_ls_number_parameters 132 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.0505 _refine_ls_R_factor_gt 0.0396 _refine_ls_wR_factor_ref 0.0799 _refine_ls_wR_factor_gt 0.0765 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _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 As1 As 0.49747(17) 0.49899(2) 0.28234(10) 0.0090(2) Uani 1 1 d . . . As2 As -0.00060(17) 0.61361(3) 0.24250(9) 0.0096(2) Uani 1 1 d . . . O1 O 0.4984(10) 0.5077(2) 0.5590(6) 0.0095(9) Uani 1 1 d . . . O2 O 0.6341(11) 0.5865(3) 0.2147(8) 0.0147(13) Uani 1 1 d U . . O3 O 0.0246(10) 0.6457(2) -0.0147(8) 0.0127(10) Uani 1 1 d . . . O4 O 0.1341(10) 0.5244(3) 0.2042(7) 0.0094(12) Uani 1 1 d . . . N1 N 0.5165(14) 0.6405(5) -0.2450(8) 0.011(2) Uani 1 1 d . . . H1A H 0.6663 0.6361 -0.1491 0.017 Uiso 1 1 calc R . . H1B H 0.5243 0.6055 -0.3462 0.017 Uiso 1 1 calc R . . H1C H 0.3511 0.6369 -0.1733 0.017 Uiso 1 1 calc R . . C1 C 0.5292(18) 0.7112(4) -0.3543(11) 0.0107(17) Uani 1 1 d . . . H1D H 0.7225 0.7190 -0.4084 0.013 Uiso 1 1 calc R . . H1E H 0.3931 0.7122 -0.4799 0.013 Uiso 1 1 calc R . . C2 C 0.4581(16) 0.7684(4) -0.1995(10) 0.0155(17) Uani 1 1 d . . . H2D H 0.5646 0.7601 -0.0609 0.019 Uiso 1 1 calc R . . H2E H 0.5218 0.8143 -0.2583 0.019 Uiso 1 1 calc R . . O5 O 0.1652(9) 0.7727(3) -0.1583(8) 0.0130(11) Uani 1 1 d . . . H5 H 0.1091 0.7338 -0.1092 0.020 Uiso 1 1 calc R . . N2 N 1.0105(14) 0.4744(5) 0.7687(8) 0.0092(19) Uani 1 1 d . . . H2A H 1.1558 0.4823 0.6779 0.014 Uiso 1 1 calc R . . H2B H 1.0311 0.5030 0.8868 0.014 Uiso 1 1 calc R . . H2C H 0.8420 0.4840 0.6983 0.014 Uiso 1 1 calc R . . C3 C 1.015(2) 0.3992(5) 0.8388(12) 0.0192(19) Uani 1 1 d . . . H3A H 0.8947 0.3938 0.9668 0.023 Uiso 1 1 calc R . . H3B H 1.2115 0.3858 0.8828 0.023 Uiso 1 1 calc R . . C4 C 0.9063(17) 0.3492(4) 0.6600(12) 0.0166(18) Uani 1 1 d . . . H4A H 0.9207 0.2994 0.7095 0.020 Uiso 1 1 calc R . . H4B H 0.7046 0.3596 0.6219 0.020 Uiso 1 1 calc R . . O6 O 1.0770(11) 0.3600(3) 0.4775(8) 0.0206(12) Uani 1 1 d U . . H6 H 1.0342 0.3298 0.3817 0.031 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 As1 0.0075(5) 0.0113(5) 0.0083(3) -0.0011(4) 0.0002(3) 0.0017(4) As2 0.0080(5) 0.0123(5) 0.0085(3) -0.0007(3) 0.0001(3) 0.0004(4) O1 0.013(2) 0.008(2) 0.0078(17) 0.0023(17) 0.0026(18) 0.000(2) O2 0.007(2) 0.018(3) 0.019(2) 0.008(2) 0.0010(18) -0.002(2) O3 0.007(3) 0.014(2) 0.017(2) 0.010(2) 0.003(2) 0.002(3) O4 0.011(3) 0.011(3) 0.007(2) -0.006(2) 0.0009(18) -0.002(2) N1 0.010(5) 0.011(5) 0.012(3) -0.001(2) -0.004(3) -0.001(3) C1 0.009(4) 0.008(4) 0.015(3) 0.002(3) -0.003(3) -0.006(4) C2 0.010(4) 0.027(5) 0.010(3) 0.002(3) 0.006(3) 0.000(4) O5 0.010(3) 0.008(3) 0.022(3) 0.002(2) 0.005(2) 0.001(2) N2 0.011(5) 0.010(5) 0.006(2) -0.002(2) 0.003(3) -0.001(3) C3 0.022(5) 0.022(5) 0.014(3) 0.006(3) 0.004(4) -0.001(4) C4 0.025(5) 0.007(4) 0.018(4) -0.006(3) 0.003(4) -0.002(4) O6 0.020(3) 0.023(3) 0.019(3) -0.014(2) 0.006(2) -0.002(2) _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 As1 O1 1.715(4) . ? As1 O2 1.825(6) . ? As1 O4 1.826(5) . ? As2 O3 1.707(5) . ? As2 O2 1.796(5) 1_455 ? As2 O4 1.816(5) . ? N1 C1 1.495(11) . ? C1 C2 1.486(11) . ? C2 O5 1.412(8) . ? N2 C3 1.483(12) . ? C3 C4 1.526(11) . ? C4 O6 1.419(9) . ? 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 O1 As1 O2 98.7(2) . . ? O1 As1 O4 102.2(2) . . ? O2 As1 O4 92.0(3) . . ? O3 As2 O2 96.1(2) . 1_455 ? O3 As2 O4 99.9(2) . . ? O2 As2 O4 93.5(3) 1_455 . ? As2 O2 As1 125.3(3) 1_655 . ? As2 O4 As1 122.5(3) . . ? C2 C1 N1 110.1(6) . . ? O5 C2 C1 113.5(6) . . ? N2 C3 C4 112.2(6) . . ? O6 C4 C3 107.6(7) . . ? 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 _geom_hbond_publ_flag N1 H1C O3 0.9100 1.8600 2.756(8) 170.00 . yes N1 H1A O3 0.9100 1.8600 2.744(8) 162.00 1_655 yes N1 H1A O2 0.9100 2.4400 3.049(8) 124.00 . yes N1 H1B O1 0.9100 1.9400 2.782(10) 153.00 1_554 yes N2 H2C O1 0.9100 1.8600 2.771(8) 177.00 . yes N2 H2A O1 0.9100 1.8600 2.744(8) 165.00 1_655 yes N2 H2B O4 0.9100 2.0400 2.890(7) 154.00 1_656 yes O5 H5 O3 0.8400 1.8100 2.645(7) 174.00 . yes O6 H6 O5 0.8400 1.9600 2.784(7) 164.00 2_645 yes _refine_diff_density_max 0.491 _refine_diff_density_min -0.743 _refine_diff_density_rms 0.119