#------------------------------------------------------------------------------ #$Date: 2019-08-17 05:17:46 +0300 (Sat, 17 Aug 2019) $ #$Revision: 217570 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/05/87/7058762.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_7058762 loop_ _publ_author_name 'Trubenstein, Henry Jared' 'Moaven, Shiva' 'Vega, Maythe' 'Unruh, Daniel K.' 'Cozzolino, Anthony Frank' _publ_section_title ; Pnictogen Bonding with Alkoxide Cages: Which Pnictogen is Best? ; _journal_name_full 'New Journal of Chemistry' _journal_paper_doi 10.1039/C9NJ03648B _journal_year 2019 _chemical_formula_sum 'C5 H9 As O3' _chemical_formula_weight 192.04 _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _symmetry_cell_setting monoclinic _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _atom_sites_solution_secondary difmap _audit_creation_date 2018-01-18T09:38:46-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_update_record ; 2019-08-13 deposited with the CCDC. 2019-08-13 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 100.379(4) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 5.9923(18) _cell_length_b 10.546(3) _cell_length_c 10.779(3) _cell_measurement_reflns_used 1481 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 25.16 _cell_measurement_theta_min 2.72 _cell_volume 670.0(3) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'DIAMOND 4.5' _computing_publication_material 'Microsoft Word 2017' _computing_structure_refinement 'SHELXL-2016/6 (Sheldrick, 2016)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 1 _diffrn_measured_fraction_theta_max 0.992 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\w scans' _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 0.0499 _diffrn_reflns_av_unetI/netI 0.0477 _diffrn_reflns_Laue_measured_fraction_full 1 _diffrn_reflns_Laue_measured_fraction_max 0.992 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 5947 _diffrn_reflns_point_group_measured_fraction_full 1 _diffrn_reflns_point_group_measured_fraction_max 0.992 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.538 _diffrn_reflns_theta_min 2.724 _exptl_absorpt_coefficient_mu 5.003 _exptl_absorpt_correction_T_max 0.7454 _exptl_absorpt_correction_T_min 0.5890 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.904 _exptl_crystal_description blade _exptl_crystal_F_000 384 _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.01 _refine_diff_density_max 0.411 _refine_diff_density_min -0.507 _refine_diff_density_rms 0.104 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 83 _refine_ls_number_reflns 1387 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.037 _refine_ls_R_factor_all 0.0455 _refine_ls_R_factor_gt 0.0293 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0123P)^2^+0.7991P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0546 _refine_ls_wR_factor_ref 0.0588 _reflns_number_gt 1086 _reflns_number_total 1387 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9nj03648b3.cif _cod_data_source_block 2-As _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 7058762 _shelx_estimated_absorpt_t_min 0.406 _shelx_estimated_absorpt_t_max 0.952 _shelx_res_file ; TITL coz18_06_a.res in P2(1)/n coz18_06_a.res created by SHELXL-2016/6 at 08:39:28 on 18-Jan-2018 REM Old TITL coz18_06 in P2(1)/n REM SHELXT solution in P2(1)/n REM R1 0.069, Rweak 0.003, Alpha 0.027, Orientation as input REM Formula found by SHELXT: C5 As O3 CELL 0.71073 5.9923 10.5456 10.7787 90.000 100.379 90.000 ZERR 4.000 0.0018 0.0031 0.0032 0.000 0.004 0.000 LATT 1 SYMM 1/2-X, 1/2+Y, 1/2-Z SFAC C H AS O UNIT 20 36 4 12 TEMP -173 SIZE 0.22 0.05 0.01 L.S. 10 BOND $H HTAB FMAP 2 PLAN 20 ACTA LIST 4 WGHT 0.012300 0.799100 FVAR 0.71213 AS1 3 0.269124 0.410656 0.069446 11.00000 0.01656 0.02041 = 0.01468 0.00138 0.00314 0.00238 O1 4 0.098265 0.522355 0.133058 11.00000 0.02560 0.01553 = 0.01267 0.00266 0.00393 0.00397 O2 4 0.115618 0.272757 0.095377 11.00000 0.02735 0.01841 = 0.01667 -0.00403 0.00460 -0.00230 O3 4 0.482459 0.397882 0.206772 11.00000 0.01566 0.03874 = 0.02151 0.00495 0.00556 0.00050 C1 1 0.061215 0.497887 0.260452 11.00000 0.01872 0.01374 = 0.01458 -0.00086 0.00291 0.00206 AFIX 23 H1A 2 -0.103049 0.504264 0.262118 11.00000 -1.20000 H1B 2 0.140149 0.563682 0.317643 11.00000 -1.20000 AFIX 0 C2 1 0.037505 0.266367 0.214866 11.00000 0.01547 0.01421 = 0.02138 0.00032 0.00230 0.00048 AFIX 23 H2A 2 0.072627 0.181383 0.252351 11.00000 -1.20000 H2B 2 -0.129319 0.277159 0.199674 11.00000 -1.20000 AFIX 0 C3 1 0.405748 0.362494 0.320817 11.00000 0.01592 0.02147 = 0.01638 0.00169 -0.00019 -0.00020 AFIX 23 H3A 2 0.475154 0.420129 0.389540 11.00000 -1.20000 H3B 2 0.458631 0.275393 0.344495 11.00000 -1.20000 AFIX 0 C4 1 0.146215 0.367372 0.308801 11.00000 0.01358 0.01316 = 0.01335 -0.00068 0.00413 -0.00108 C5 1 0.085345 0.341772 0.436677 11.00000 0.02038 0.02402 = 0.01836 0.00380 0.00489 0.00096 AFIX 137 H5A 2 -0.080082 0.339816 0.429013 11.00000 -1.50000 H5B 2 0.147959 0.409049 0.495499 11.00000 -1.50000 H5C 2 0.148712 0.259862 0.468389 11.00000 -1.50000 AFIX 0 HKLF 4 REM coz18_06_a.res in P2(1)/n REM R1 = 0.0293 for 1086 Fo > 4sig(Fo) and 0.0455 for all 1387 data REM 83 parameters refined using 0 restraints END WGHT 0.0123 0.7991 REM No hydrogen bonds found for HTAB generation REM Highest difference peak 0.411, deepest hole -0.507, 1-sigma level 0.104 Q1 1 0.1935 0.4184 -0.0268 11.00000 0.05 0.41 Q2 1 0.2103 0.5411 0.0918 11.00000 0.05 0.40 Q3 1 0.3838 0.4208 0.1646 11.00000 0.05 0.40 Q4 1 0.1124 0.3852 0.3758 11.00000 0.05 0.38 Q5 1 0.1163 0.4359 0.2847 11.00000 0.05 0.37 Q6 1 0.0619 0.5021 0.2009 11.00000 0.05 0.37 Q7 1 0.0997 0.3279 0.2594 11.00000 0.05 0.35 Q8 1 0.2459 0.3601 0.4157 11.00000 0.05 0.34 Q9 1 0.5643 0.4151 0.1777 11.00000 0.05 0.34 Q10 1 0.2721 0.3814 0.2897 11.00000 0.05 0.34 Q11 1 0.5741 0.4168 0.4563 11.00000 0.05 0.33 Q12 1 0.2814 0.2736 0.0726 11.00000 0.05 0.32 Q13 1 0.3999 0.4141 -0.0118 11.00000 0.05 0.32 Q14 1 0.6198 0.1794 0.3162 11.00000 0.05 0.32 Q15 1 -0.1008 0.4167 0.3251 11.00000 0.05 0.31 Q16 1 0.3226 0.5192 0.1654 11.00000 0.05 0.31 Q17 1 0.4373 0.4170 0.4965 11.00000 0.05 0.31 Q18 1 -0.2614 0.3473 0.4372 11.00000 0.05 0.31 Q19 1 0.0374 0.3809 0.0458 11.00000 0.05 0.30 Q20 1 0.3789 0.2356 0.1837 11.00000 0.05 0.30 ; _shelx_res_checksum 12070 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' 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_calc_flag As1 As 0.26912(6) 0.41066(4) 0.06945(3) 0.01718(12) Uani 1 d O1 O 0.0983(4) 0.5224(2) 0.1331(2) 0.0179(5) Uani 1 d O2 O 0.1156(4) 0.2728(2) 0.0954(2) 0.0207(6) Uani 1 d O3 O 0.4825(4) 0.3979(3) 0.2068(2) 0.0250(6) Uani 1 d C1 C 0.0612(6) 0.4979(3) 0.2605(3) 0.0157(7) Uani 1 d H1A H -0.103049 0.504264 0.262118 0.019 Uiso 1 calc H1B H 0.140149 0.563682 0.317643 0.019 Uiso 1 calc C2 C 0.0375(5) 0.2664(3) 0.2149(3) 0.0171(7) Uani 1 d H2A H 0.072627 0.181383 0.252351 0.021 Uiso 1 calc H2B H -0.129319 0.277159 0.199674 0.021 Uiso 1 calc C3 C 0.4057(5) 0.3625(3) 0.3208(3) 0.0183(8) Uani 1 d H3A H 0.475154 0.420129 0.38954 0.022 Uiso 1 calc H3B H 0.458631 0.275393 0.344495 0.022 Uiso 1 calc C4 C 0.1462(5) 0.3674(3) 0.3088(3) 0.0132(7) Uani 1 d C5 C 0.0853(6) 0.3418(4) 0.4367(3) 0.0207(8) Uani 1 d H5A H -0.080082 0.339816 0.429013 0.031 Uiso 1 calc H5B H 0.147959 0.409049 0.495499 0.031 Uiso 1 calc H5C H 0.148712 0.259862 0.468389 0.031 Uiso 1 calc 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 0.01656(17) 0.0204(2) 0.01468(18) 0.00138(18) 0.00314(12) 0.00238(18) O1 0.0256(13) 0.0155(13) 0.0127(12) 0.0027(10) 0.0039(10) 0.0040(11) O2 0.0273(13) 0.0184(14) 0.0167(12) -0.0040(11) 0.0046(10) -0.0023(11) O3 0.0157(12) 0.0387(17) 0.0215(13) 0.0050(12) 0.0056(10) 0.0005(12) C1 0.0187(18) 0.0137(19) 0.0146(17) -0.0009(14) 0.0029(14) 0.0021(14) C2 0.0155(17) 0.0142(19) 0.0214(18) 0.0003(15) 0.0023(14) 0.0005(14) C3 0.0159(17) 0.021(2) 0.0164(18) 0.0017(15) -0.0002(14) -0.0002(15) C4 0.0136(16) 0.0132(18) 0.0134(17) -0.0007(13) 0.0041(13) -0.0011(13) C5 0.0204(18) 0.024(2) 0.0184(18) 0.0038(16) 0.0049(15) 0.0010(15) 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 0 '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 0.006 '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 O2 As1 O1 97.57(11) O2 As1 O3 97.03(11) O1 As1 O3 96.13(11) C1 O1 As1 116.33(19) C2 O2 As1 116.0(2) C3 O3 As1 116.04(19) O1 C1 C4 112.6(3) O1 C1 H1A 109.1 C4 C1 H1A 109.1 O1 C1 H1B 109.1 C4 C1 H1B 109.1 H1A C1 H1B 107.8 O2 C2 C4 112.8(3) O2 C2 H2A 109 C4 C2 H2A 109 O2 C2 H2B 109 C4 C2 H2B 109 H2A C2 H2B 107.8 O3 C3 C4 113.2(3) O3 C3 H3A 108.9 C4 C3 H3A 108.9 O3 C3 H3B 108.9 C4 C3 H3B 108.9 H3A C3 H3B 107.8 C5 C4 C1 110.6(3) C5 C4 C2 109.6(3) C1 C4 C2 109.0(3) C5 C4 C3 108.9(3) C1 C4 C3 109.2(3) C2 C4 C3 109.6(3) C4 C5 H5A 109.5 C4 C5 H5B 109.5 H5A C5 H5B 109.5 C4 C5 H5C 109.5 H5A C5 H5C 109.5 H5B C5 H5C 109.5 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance As1 O2 1.770(2) As1 O1 1.777(2) As1 O3 1.778(2) O1 C1 1.453(4) O2 C2 1.449(4) O3 C3 1.437(4) C1 C4 1.526(5) C1 H1A 0.99 C1 H1B 0.99 C2 C4 1.532(4) C2 H2A 0.99 C2 H2B 0.99 C3 C4 1.538(4) C3 H3A 0.99 C3 H3B 0.99 C4 C5 1.512(5) C5 H5A 0.98 C5 H5B 0.98 C5 H5C 0.98