#------------------------------------------------------------------------------ #$Date: 2008-01-13 22:15:36 +0000 (Sun, 13 Jan 2008) $ #$Revision: 14 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003483.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_2003483 _journal_name_full 'Acta Crystallographica' _journal_year 1995 _journal_volume C51 _journal_page_first 997 _journal_page_last 1001 _publ_section_title ; Tripotassium Phosphoglycolate Dihydrate and Tris(cyclohexylammonium) Phosphoglycolate Trihydrate ; _chemical_formula_moiety '3C6 H14 N 1+ , (C2 H2 O6 P) 3- , 3H2 O' _chemical_formula_sum 'C20 H50 N3 O9 P' _chemical_formula_weight 507.60 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' _symmetry_space_group_name_H-M 'P n a 21' _cell_length_a 22.512(9) _cell_length_b 19.613(9) _cell_length_c 6.201(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2737.9(21) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.231(2) _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71069 _cell_measurement_reflns_used '40 [25]' _cell_measurement_theta_min '10 [9]' _cell_measurement_theta_max '15 [15]' _exptl_absorpt_coefficient_mu 0.149 _cell_measurement_temperature '85(2) [299(1)]' _exptl_crystal_description 'needle like' _exptl_crystal_size_max 0.8 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_colour 'colourless' _diffrn_measurement_device 'Kuma KM-4' _diffrn_measurement_method \w/2\q _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _diffrn_reflns_number 2941 _reflns_number_total 2941 _reflns_number_observed 2157 _reflns_observed_criterion >2sigma(I) _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_theta_max 26 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 7 _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_decay_% 2 _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_obs 0.0431 _refine_ls_wR_factor_obs 0.1157 _refine_ls_goodness_of_fit_obs 1.096 _refine_ls_number_reflns 2157 _refine_ls_number_parameters 342 _refine_ls_hydrogen_treatment ? _refine_ls_weighting_scheme ; calc w = 1/[\s^2^(F~o~^2^) + (0.0648P)^2^ + 2.69P] where P = (F~o~^2^ + 2F~c~^2^)/3 ; _refine_ls_shift/esd_max 0.078 _refine_diff_density_max 0.28 _refine_diff_density_min -0.25 _refine_ls_extinction_method none loop_ _atom_type_symbol _atom_type_description _atom_type_scat_source _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag 'C' 'C' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0033 0.001 'H' 'H' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0000 0.000 'N' 'N' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0061 0.003 'O' 'O' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0106 0.006 'P' 'P' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.1023 0.094 _refine_ls_abs_structure_details 'Flack, H. D. (1983). Acta Cryst. A39, 876- _refine_ls_abs_structure_Flack -0.04(22) loop_ _atom_site_label _atom_site_occupancy _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv P 1 0.62657(5) 0.04293(6) 0.5 0.0103(2) O1 1 0.6450(2) 0.1043(2) 0.3698(6) 0.0147(8) O2 1 0.6851(2) -0.0053(2) 0.4762(7) 0.0148(7) O3 1 0.5746(2) 0.0040(2) 0.4090(6) 0.0139(7) O4 1 0.6181(2) 0.0556(2) 0.7411(6) 0.0152(8) O5 1 0.7129(2) -0.1038(2) 0.1809(6) 0.0188(8) O6 1 0.7143(2) -0.1834(2) 0.4412(6) 0.0174(8) O7 1 0.6045(2) 0.1700(2) -0.0023(7) 0.0172(7) O8 1 0.7115(2) -0.2189(2) -0.1196(7) 0.0229(9) O9 1 0.6743(2) 0.2368(2) 0.4303(7) 0.0250(9) N1 1 0.4550(2) 0.0301(2) 0.4954(9) 0.0121(8) N2 1 0.7082(2) 0.0337(2) 0.0369(7) 0.0132(9) N3 1 0.8313(2) -0.2192(2) 0.3479(8) 0.0198(10) C1 1 0.7053(2) -0.1238(3) 0.3719(9) 0.0148(11) C2 1 0.6824(2) -0.0748(3) 0.5419(9) 0.0156(11) C11 1 0.4413(2) 0.1033(3) 0.4511(8) 0.0120(10) C12 1 0.4588(2) 0.1478(3) 0.6409(9) 0.0161(10) C13 1 0.4451(3) 0.2223(3) 0.5914(10) 0.0200(12) C14 1 0.4774(3) 0.2459(3) 0.3843(9) 0.0193(12) C15 1 0.4609(3) 0.2008(3) 0.1954(9) 0.0162(11) C16 1 0.4739(3) 0.1259(3) 0.2448(9) 0.0152(11) C21 1 0.7694(2) 0.0554(3) -0.0239(9) 0.0150(10) C22 1 0.8078(3) 0.0578(3) 0.1803(9) 0.0199(12) C23 1 0.8705(3) 0.0827(3) 0.1259(11) 0.0224(12) C24 1 0.8692(3) 0.1516(3) 0.0113(13) 0.0245(12) C25 1 0.8306(3) 0.1488(3) -0.1887(11) 0.0265(13) C26 1 0.7673(3) 0.1244(3) -0.1331(11) 0.0227(12) C31 1 0.8641(3) -0.1528(3) 0.3707(10) 0.0178(12) C32 1 0.9261(3) -0.1607(3) 0.2766(11) 0.0227(12) C33 1 0.9614(3) -0.0946(3) 0.3036(13) 0.0325(18) C34 1 0.9633(3) -0.0718(3) 0.5388(13) 0.0378(18) C35 1 0.9016(3) -0.0651(3) 0.6319(12) 0.0317(15) C36 1 0.8657(3) -0.1314(3) 0.6031(11) 0.0242(13) H7 1 0.6105(26) 0.1292(16) -0.088(8) 0.021 H71 1 0.6117(26) 0.1468(23) 0.133(5) 0.021 H8 1 0.7089(27) -0.1817(19) -0.017(7) 0.028 H81 1 0.7132(29) -0.1946(24) -0.256(5) 0.028 H9 1 0.7134(13) 0.2465(27) 0.372(11) 0.030 H91 1 0.6642(24) 0.1888(8) 0.421(12) 0.030 H1N1 1 0.4312(20) -0.0011(22) 0.402(8) 0.014 H2N1 1 0.4309(21) 0.0190(25) 0.626(6) 0.014 H3N1 1 0.4972(8) 0.0201(24) 0.456(9) 0.014 H1N2 1 0.7114(24) -0.0138(11) 0.094(10) 0.016 H2N2 1 0.6781(19) 0.0364(26) -0.081(7) 0.016 H3N2 1 0.6927(23) 0.0668(22) 0.146(7) 0.016 H1N3 1 0.8263(26) -0.2330(30) 0.194(4) 0.024 H2N3 1 0.7909(12) -0.2096(28) 0.407(10) 0.024 H3N3 1 0.8561(22) -0.2545(22) 0.422(10) 0.024 H2 1 0.6408 -0.0866 0.5765 0.019 H20 1 0.7062 -0.0805 0.6750 0.019 H11 1 0.3976 0.1080 0.4269 0.014 H12 1 0.5018 0.1425 0.6703 0.019 H121 1 0.4367 0.1334 0.7710 0.019 H13 1 0.4578 0.2511 0.7142 0.024 H131 1 0.4017 0.2281 0.5728 0.024 H14 1 0.4663 0.2937 0.3519 0.023 H141 1 0.5209 0.2442 0.4074 0.023 H15 1 0.4837 0.2150 0.0665 0.019 H151 1 0.4181 0.2063 0.1629 0.019 H16 1 0.5173 0.1195 0.2639 0.018 H161 1 0.4610 0.0972 0.1221 0.018 H21 1 0.7866 0.0213 -0.1263 0.018 H22 1 0.7894 0.0888 0.2870 0.024 H221 1 0.8100 0.0117 0.2450 0.024 H23 1 0.8939 0.0868 0.2605 0.027 H231 1 0.8904 0.0488 0.0323 0.027 H24 1 0.8536 0.1868 0.1109 0.029 H241 1 0.9101 0.1648 -0.0299 0.029 H25 1 0.8485 0.1172 -0.2949 0.032 H251 1 0.8286 0.1946 -0.2551 0.032 H26 1 0.7480 0.1579 -0.0361 0.027 H261 1 0.7434 0.1213 -0.2666 0.027 H31 1 0.8425 -0.1171 0.2863 0.021 H32 1 0.9232 -0.1723 0.1216 0.027 H321 1 0.9471 -0.1984 0.3507 0.027 H33 1 1.0025 -0.1016 0.2509 0.039 H331 1 0.9430 -0.0583 0.2152 0.039 H34 1 0.9861 -0.1055 0.6242 0.045 H341 1 0.9839 -0.0274 0.5490 0.045 H35 1 0.8806 -0.0271 0.5595 0.038 H351 1 0.9045 -0.0541 0.7874 0.038 H36 1 0.8839 -0.1681 0.6906 0.029 H361 1 0.8246 -0.1243 0.6555 0.029 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_22 _atom_site_aniso_U_23 _atom_site_aniso_U_33 P 0.0129(5) 0.0006(5) 0.0003(6) 0.0094(5) -0.0002(5) 0.0087(5) O1 0.019(2) -0.0012(14) 0.002(2) 0.013(2) 0.001(2) 0.012(2) O2 0.015(2) 0.0040(13) 0.001(2) 0.016(2) 0.002(2) 0.014(2) O3 0.016(2) -0.0005(14) -0.001(2) 0.015(2) 0.001(2) 0.011(2) O4 0.022(2) 0.0019(15) 0.001(2) 0.014(2) -0.000(2) 0.009(2) O5 0.025(2) 0.001(2) 0.003(2) 0.018(2) 0.001(2) 0.013(2) O6 0.020(2) 0.0030(14) 0.002(2) 0.014(2) -0.002(2) 0.017(2) O7 0.025(2) 0.0003(13) -0.001(2) 0.013(2) -0.001(2) 0.013(2) O8 0.036(2) 0.003(2) 0.001(2) 0.018(2) 0.003(2) 0.014(2) O9 0.030(2) -0.003(2) -0.001(2) 0.016(2) -0.002(2) 0.029(2) N1 0.014(2) -0.0032(15) 0.000(2) 0.013(2) -0.001(2) 0.009(2) N2 0.015(2) -0.001(2) -0.002(2) 0.013(2) -0.001(2) 0.012(2) N3 0.022(2) -0.001(2) 0.002(2) 0.014(2) -0.002(2) 0.024(3) C1 0.005(2) -0.001(2) -0.001(2) 0.021(3) 0.001(2) 0.018(3) C2 0.015(2) 0.004(2) -0.001(2) 0.014(2) 0.004(2) 0.018(3) C11 0.010(2) 0.002(2) 0.001(2) 0.015(2) 0.002(2) 0.011(3) C12 0.017(2) 0.000(2) -0.001(2) 0.019(2) -0.001(2) 0.012(2) C13 0.024(3) 0.000(2) 0.004(2) 0.016(3) -0.004(2) 0.020(3) C14 0.031(3) 0.001(2) -0.004(2) 0.013(2) 0.002(2) 0.014(3) C15 0.021(3) -0.002(2) 0.002(2) 0.015(2) 0.001(2) 0.013(2) C16 0.018(3) 0.000(2) 0.003(2) 0.014(2) 0.000(2) 0.013(3) C21 0.015(2) 0.001(2) 0.004(2) 0.014(2) 0.001(2) 0.015(3) C22 0.018(3) 0.000(2) -0.003(2) 0.025(3) 0.006(2) 0.017(3) C23 0.016(3) -0.001(2) -0.002(3) 0.026(3) 0.002(3) 0.025(3) C24 0.021(2) -0.002(2) 0.008(3) 0.016(2) -0.002(3) 0.036(3) C25 0.020(3) -0.006(2) 0.002(3) 0.024(3) 0.009(3) 0.035(4) C26 0.017(3) 0.000(2) -0.002(3) 0.020(3) 0.012(3) 0.031(3) C31 0.023(3) -0.002(2) -0.002(2) 0.013(2) -0.001(2) 0.017(3) C32 0.020(3) 0.002(2) 0.005(3) 0.020(3) -0.001(3) 0.028(3) C33 0.019(3) -0.004(2) 0.001(3) 0.027(3) 0.007(3) 0.052(5) C34 0.029(3) -0.007(2) -0.020(4) 0.024(3) 0.004(3) 0.059(5) C35 0.037(3) 0.000(3) -0.014(3) 0.026(3) -0.009(3) 0.032(3) C36 0.026(3) 0.000(2) -0.003(3) 0.023(3) -0.003(3) 0.024(3)