#------------------------------------------------------------------------------ #$Date: 2019-11-08 03:00:33 +0200 (Fri, 08 Nov 2019) $ #$Revision: 224940 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/05/87/7058763.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_7058763 loop_ _publ_author_name 'Trubenstein, Henry J.' 'Moaven, Shiva' 'Vega, Maythe' 'Unruh, Daniel K.' 'Cozzolino, Anthony F.' _publ_section_title ; Pnictogen bonding with alkoxide cages: which pnictogen is best? ; _journal_issue 36 _journal_name_full 'New Journal of Chemistry' _journal_page_first 14305 _journal_paper_doi 10.1039/C9NJ03648B _journal_volume 43 _journal_year 2019 _chemical_formula_sum 'C6 H11 As O3' _chemical_formula_weight 206.07 _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 2018-01-18T15:47:20-00:00 _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 92.280(6) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 6.018(2) _cell_length_b 11.627(5) _cell_length_c 10.644(4) _cell_measurement_reflns_used 5042 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 27.17 _cell_measurement_theta_min 2.60 _cell_volume 744.2(5) _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 0.999 _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 0.0189 _diffrn_reflns_av_unetI/netI 0.0139 _diffrn_reflns_Laue_measured_fraction_full 1 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 8373 _diffrn_reflns_point_group_measured_fraction_full 1 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.117 _diffrn_reflns_theta_min 2.595 _exptl_absorpt_coefficient_mu 4.512 _exptl_absorpt_correction_T_max 0.7455 _exptl_absorpt_correction_T_min 0.5899 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.839 _exptl_crystal_description block _exptl_crystal_F_000 416 _exptl_crystal_size_max 0.475 _exptl_crystal_size_mid 0.425 _exptl_crystal_size_min 0.4 _refine_diff_density_max 0.409 _refine_diff_density_min -0.237 _refine_diff_density_rms 0.055 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 92 _refine_ls_number_reflns 1643 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.076 _refine_ls_R_factor_all 0.0177 _refine_ls_R_factor_gt 0.0158 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0150P)^2^+0.5645P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.038 _refine_ls_wR_factor_ref 0.0385 _reflns_number_gt 1550 _reflns_number_total 1643 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9nj03648b3.cif _cod_data_source_block 3-As _cod_depositor_comments 'Adding full bibliography for 7058762--7058763.cif.' _cod_original_cell_volume 744.1(5) _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 7058763 _shelx_estimated_absorpt_t_min 0.223 _shelx_estimated_absorpt_t_max 0.266 _shelx_res_file ; coz18_07_0m_a.res created by SHELXL-2014/7 TITL coz18_07_0m_a.res in P2(1)/n REM Old TITL Integration of coz18_07 REM SHELXT solution in P2(1)/n REM R1 0.047, Rweak 0.004, Alpha 0.030, Orientation as input REM Formula found by SHELXT: C6 As O3 CELL 0.71073 6.0177 11.6274 10.6436 90.000 92.280 90.000 ZERR 4.000 0.0023 0.0047 0.0043 0.000 0.006 0.000 LATT 1 SYMM 1/2-X, 1/2+Y, 1/2-Z SFAC C H AS O UNIT 24 44 4 12 TEMP -173 SIZE 0.400 0.425 0.475 L.S. 10 BOND $H HTAB FMAP 2 PLAN 20 ACTA LIST 4 WGHT 0.015000 0.564500 FVAR 0.64678 AS1 3 0.725908 0.440424 0.393681 11.00000 0.01247 0.01274 = 0.01325 0.00075 0.00024 -0.00258 O1 4 0.766020 0.318731 0.493631 11.00000 0.01277 0.01509 = 0.01368 0.00061 -0.00347 -0.00106 O2 4 0.428653 0.440893 0.389533 11.00000 0.01344 0.01112 = 0.02128 -0.00123 -0.00164 0.00060 O3 4 0.752691 0.364488 0.248970 11.00000 0.01887 0.01939 = 0.01262 0.00024 0.00447 -0.00712 C1 1 0.600263 0.228721 0.476838 11.00000 0.01331 0.01276 = 0.01042 0.00123 0.00048 0.00015 AFIX 23 H1A 2 0.489000 0.236463 0.542373 11.00000 -1.20000 H1B 2 0.673226 0.152875 0.487822 11.00000 -1.20000 AFIX 0 C2 1 0.323047 0.337038 0.341563 11.00000 0.01153 0.01327 = 0.01653 0.00099 -0.00152 -0.00012 AFIX 23 H2A 2 0.269932 0.349961 0.253467 11.00000 -1.20000 H2B 2 0.192013 0.319673 0.391643 11.00000 -1.20000 AFIX 0 C3 1 0.655493 0.250113 0.246004 11.00000 0.01663 0.01773 = 0.01087 -0.00194 0.00418 -0.00276 AFIX 23 H3A 2 0.775138 0.192457 0.259461 11.00000 -1.20000 H3B 2 0.584522 0.236311 0.161844 11.00000 -1.20000 AFIX 0 C4 1 0.481115 0.233610 0.346494 11.00000 0.01106 0.01212 = 0.00926 0.00003 0.00132 0.00029 C5 1 0.354733 0.121069 0.318228 11.00000 0.01725 0.01442 = 0.01330 -0.00259 0.00223 -0.00281 AFIX 23 H5A 2 0.272401 0.129372 0.236339 11.00000 -1.20000 H5B 2 0.464784 0.058611 0.309268 11.00000 -1.20000 AFIX 0 C6 1 0.189751 0.084412 0.417054 11.00000 0.01831 0.01430 = 0.01728 -0.00068 0.00359 -0.00316 AFIX 137 H6A 2 0.082610 0.146495 0.429286 11.00000 -1.50000 H6B 2 0.270804 0.068282 0.496790 11.00000 -1.50000 H6C 2 0.110522 0.015060 0.388172 11.00000 -1.50000 AFIX 0 HKLF 4 REM coz18_07_0m_a.res in P2(1)/n REM R1 = 0.0158 for 1550 Fo > 4sig(Fo) and 0.0177 for all 1643 data REM 92 parameters refined using 0 restraints END WGHT 0.0150 0.5645 REM Instructions for potential hydrogen bonds EQIV $1 x-1/2, -y+1/2, z-1/2 HTAB C3 O1_$1 REM Highest difference peak 0.409, deepest hole -0.237, 1-sigma level 0.055 Q1 1 0.5600 0.2424 0.3009 11.00000 0.05 0.41 Q2 1 0.5346 0.2366 0.4066 11.00000 0.05 0.38 Q3 1 0.4025 0.2794 0.3394 11.00000 0.05 0.37 Q4 1 0.4231 0.1784 0.3309 11.00000 0.05 0.31 Q5 1 0.7423 0.3805 0.4559 11.00000 0.05 0.30 Q6 1 0.7289 0.4003 0.3018 11.00000 0.05 0.30 Q7 1 0.5565 0.4455 0.3643 11.00000 0.05 0.28 Q8 1 0.7912 0.5191 0.3915 11.00000 0.05 0.27 Q9 1 0.2629 0.1166 0.3655 11.00000 0.05 0.26 Q10 1 0.5437 0.4325 0.4326 11.00000 0.05 0.25 Q11 1 0.7082 0.3216 0.2470 11.00000 0.05 0.23 Q12 1 0.3918 0.3943 0.3603 11.00000 0.05 0.22 Q13 1 0.7497 0.5009 0.4563 11.00000 0.05 0.20 Q14 1 0.7053 0.1741 0.4565 11.00000 0.05 0.19 Q15 1 0.8177 0.3794 0.1994 11.00000 0.05 0.18 Q16 1 0.6948 0.2764 0.4837 11.00000 0.05 0.18 Q17 1 0.4535 0.4809 0.3285 11.00000 0.05 0.16 Q18 1 0.3666 0.4863 0.4011 11.00000 0.05 0.16 Q19 1 0.3998 0.4402 0.4461 11.00000 0.05 0.15 Q20 1 0.3235 0.1299 0.2758 11.00000 0.05 0.15 ; _shelx_res_checksum 40122 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 0.72591(3) 0.44042(2) 0.39368(2) 0.01283(6) Uani 1 d O1 O 0.76602(17) 0.31873(10) 0.49363(10) 0.0140(2) Uani 1 d O2 O 0.42865(19) 0.44089(9) 0.38953(11) 0.0153(2) Uani 1 d O3 O 0.75269(19) 0.36449(10) 0.24897(10) 0.0169(2) Uani 1 d C1 C 0.6003(3) 0.22872(13) 0.47684(14) 0.0122(3) Uani 1 d H1A H 0.489 0.2365 0.5424 0.015 Uiso 1 calc H1B H 0.6732 0.1529 0.4878 0.015 Uiso 1 calc C2 C 0.3230(3) 0.33704(13) 0.34156(15) 0.0138(3) Uani 1 d H2A H 0.2699 0.35 0.2535 0.017 Uiso 1 calc H2B H 0.192 0.3197 0.3916 0.017 Uiso 1 calc C3 C 0.6555(3) 0.25011(14) 0.24600(15) 0.0150(3) Uani 1 d H3A H 0.7751 0.1925 0.2595 0.018 Uiso 1 calc H3B H 0.5845 0.2363 0.1618 0.018 Uiso 1 calc C4 C 0.4811(2) 0.23361(13) 0.34649(14) 0.0108(3) Uani 1 d C5 C 0.3547(3) 0.12107(14) 0.31823(15) 0.0149(3) Uani 1 d H5A H 0.2724 0.1294 0.2363 0.018 Uiso 1 calc H5B H 0.4648 0.0586 0.3093 0.018 Uiso 1 calc C6 C 0.1898(3) 0.08441(14) 0.41705(15) 0.0166(3) Uani 1 d H6A H 0.0826 0.1465 0.4293 0.025 Uiso 1 calc H6B H 0.2708 0.0683 0.4968 0.025 Uiso 1 calc H6C H 0.1105 0.0151 0.3882 0.025 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 0.01247(9) 0.01274(9) 0.01325(9) 0.00075(6) 0.00024(6) -0.00258(6) O1 0.0128(5) 0.0151(6) 0.0137(5) 0.0006(4) -0.0035(4) -0.0011(4) O2 0.0134(5) 0.0111(5) 0.0213(6) -0.0012(4) -0.0016(4) 0.0006(4) O3 0.0189(6) 0.0194(6) 0.0126(5) 0.0002(4) 0.0045(4) -0.0071(5) C1 0.0133(7) 0.0128(7) 0.0104(7) 0.0012(6) 0.0005(6) 0.0001(6) C2 0.0115(7) 0.0133(8) 0.0165(8) 0.0010(6) -0.0015(6) -0.0001(6) C3 0.0166(8) 0.0177(8) 0.0109(7) -0.0019(6) 0.0042(6) -0.0028(6) C4 0.0111(7) 0.0121(7) 0.0093(7) 0.0000(6) 0.0013(5) 0.0003(6) C5 0.0173(8) 0.0144(8) 0.0133(8) -0.0026(6) 0.0022(6) -0.0028(6) C6 0.0183(8) 0.0143(8) 0.0173(8) -0.0007(6) 0.0036(6) -0.0032(6) 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 O1 As1 O2 97.41(5) O1 As1 O3 96.17(6) O2 As1 O3 96.01(5) C1 O1 As1 115.03(9) C2 O2 As1 115.52(9) C3 O3 As1 114.88(9) O1 C1 C4 112.21(12) O1 C1 H1A 109.2 C4 C1 H1A 109.2 O1 C1 H1B 109.2 C4 C1 H1B 109.2 H1A C1 H1B 107.9 O2 C2 C4 112.28(12) O2 C2 H2A 109.1 C4 C2 H2A 109.1 O2 C2 H2B 109.1 C4 C2 H2B 109.1 H2A C2 H2B 107.9 O3 C3 C4 112.58(13) O3 C3 H3A 109.1 C4 C3 H3A 109.1 O3 C3 H3B 109.1 C4 C3 H3B 109.1 H3A C3 H3B 107.8 C2 C4 C1 109.05(12) C2 C4 C5 111.08(13) C1 C4 C5 110.76(12) C2 C4 C3 108.51(13) C1 C4 C3 108.98(12) C5 C4 C3 108.40(12) C6 C5 C4 115.51(13) C6 C5 H5A 108.4 C4 C5 H5A 108.4 C6 C5 H5B 108.4 C4 C5 H5B 108.4 H5A C5 H5B 107.5 C5 C6 H6A 109.5 C5 C6 H6B 109.5 H6A C6 H6B 109.5 C5 C6 H6C 109.5 H6A C6 H6C 109.5 H6B C6 H6C 109.5 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance As1 O1 1.7809(12) As1 O2 1.7876(13) As1 O3 1.7882(13) O1 C1 1.4519(18) O2 C2 1.4481(19) O3 C3 1.453(2) C1 C4 1.537(2) C1 H1A 0.99 C1 H1B 0.99 C2 C4 1.533(2) C2 H2A 0.99 C2 H2B 0.99 C3 C4 1.540(2) C3 H3A 0.99 C3 H3B 0.99 C4 C5 1.537(2) C5 C6 1.535(2) C5 H5A 0.99 C5 H5B 0.99 C6 H6A 0.98 C6 H6B 0.98 C6 H6C 0.98