#------------------------------------------------------------------------------ #$Date: 2017-08-02 05:23:24 +0300 (Wed, 02 Aug 2017) $ #$Revision: 199448 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/22/88/7228824.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_7228824 loop_ _publ_author_name 'Bhat, Gulzar A.' 'Kalita, Alok Ch' 'Murugavel, Ramaswamy' _publ_section_title ; Intriguing Structural Chemistry of Neutral and Anionic Layered Monoalkylphosphates: Single-Source Precursors for High-Yield Ceramic Phosphates ; _journal_name_full CrystEngComm _journal_paper_doi 10.1039/C7CE01066D _journal_year 2017 _chemical_formula_sum 'C13 H37 N2 O7 P' _chemical_formula_weight 364.41 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2017-03-06 deposited with the CCDC. 2017-08-01 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 98.918(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 12.6511(5) _cell_length_b 6.4515(2) _cell_length_c 24.2892(7) _cell_measurement_reflns_used 3447 _cell_measurement_temperature 298(2) _cell_measurement_theta_max 28.8810 _cell_measurement_theta_min 2.3480 _cell_volume 1958.48(11) _computing_cell_refinement 'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)' _computing_data_collection 'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)' _computing_molecular_graphics ' Diamond' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution Sir92 _diffrn_ambient_temperature 298(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Rigaku Saturn724' _diffrn_measurement_method \w _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0353 _diffrn_reflns_av_unetI/netI 0.0307 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_number 14283 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 24.997 _diffrn_reflns_theta_max 24.997 _diffrn_reflns_theta_min 2.529 _exptl_absorpt_coefficient_mu 0.173 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.83359 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'NUMABS (Rigaku, 1999)' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.236 _exptl_crystal_description needles _exptl_crystal_F_000 800 _exptl_crystal_size_max 0.230 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.060 _refine_diff_density_max 1.629 _refine_diff_density_min -0.416 _refine_diff_density_rms 0.080 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 220 _refine_ls_number_reflns 3446 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.043 _refine_ls_R_factor_all 0.0927 _refine_ls_R_factor_gt 0.0794 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1345P)^2^+3.0445P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2217 _refine_ls_wR_factor_ref 0.2375 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2816 _reflns_number_total 3446 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c7ce01066d2.cif _cod_data_source_block 1 _cod_database_code 7228824 _shelx_shelxl_version_number 2014/7 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_min 0.961 _shelx_estimated_absorpt_t_max 0.990 _shelx_res_file ; shelx.res created by SHELXL-2014/7 TITL gb-701-a_a.res in P2(1)/c CELL 0.71073 12.6511 6.4515 24.2892 90.000 98.918 90.000 ZERR 4.00 0.0005 0.0002 0.0007 0.000 0.003 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O P UNIT 52 148 8 28 4 MERG 2 OMIT -3.00 50.00 OMIT 0 0 2 OMIT -1 0 2 EQIV $1 1-X,2-Y,1-Z EQIV $2 1-X,1-Y,1-Z EQIV $3 +X,-1+Y,+Z EQIV $4 1-X,-0.5+Y,1.5-Z HTAB O6 O3_$1 HTAB O6 O2_$2 HTAB N2 O2 HTAB N2 O3_$3 HTAB N2 O3_$4 HTAB N1 O6 HTAB N1 O5_$2 HTAB N1 O4 HTAB O5 O4 HTAB O5 O4_$1 HTAB O7 O4_$3 HTAB O7 O1_$3 HTAB O7 O2 HTAB C1 O7 HTAB C8 O1 MORE -1 FMAP 2 PLAN 20 SIZE 0.060 0.150 0.230 ACTA BOND $H CONF LIST 6 L.S. 30 TEMP 25.00 WGHT 0.134500 3.044500 FVAR 0.42380 P1 5 0.414074 0.845486 0.630476 11.00000 0.04112 0.02270 = 0.02808 0.00233 0.00263 -0.00082 O2 4 0.427418 0.615560 0.640429 11.00000 0.06236 0.02537 = 0.05518 0.00659 0.00988 0.00212 O3 4 0.484620 0.978719 0.671082 11.00000 0.07956 0.04060 = 0.04822 -0.01022 -0.01757 0.00739 AFIX 6 O6 4 0.416867 0.678720 0.382133 11.00000 0.05888 0.04640 = 0.06701 0.00344 0.02249 -0.00294 H6C 2 0.444016 0.792811 0.373768 11.00000 -1.50000 H6D 2 0.460629 0.580682 0.379414 11.00000 -1.50000 AFIX 0 N2 3 0.412209 0.337381 0.725484 11.00000 0.04860 0.02706 = 0.03022 -0.00042 0.00222 0.00036 AFIX 137 H2A 2 0.423465 0.437202 0.701774 11.00000 -1.20000 H2B 2 0.430513 0.215637 0.712531 11.00000 -1.20000 H2C 2 0.451571 0.361538 0.758516 11.00000 -1.20000 AFIX 0 O4 4 0.410976 0.901026 0.570443 11.00000 0.09193 0.05207 = 0.03788 0.00727 0.00829 -0.00433 N1 3 0.336817 0.618510 0.482747 11.00000 0.04913 0.03796 = 0.03916 0.00048 0.00040 -0.00024 AFIX 137 H1A 2 0.363978 0.658469 0.452774 11.00000 -1.20000 H1B 2 0.356548 0.488556 0.491275 11.00000 -1.20000 H1C 2 0.360989 0.701191 0.511263 11.00000 -1.20000 AFIX 6 O5 4 0.586872 0.795889 0.513887 11.00000 0.07424 0.06244 = 0.08450 0.02138 0.02376 0.02173 H5C 2 0.559596 0.851330 0.540176 11.00000 -1.50000 H5D 2 0.566968 0.862107 0.483817 11.00000 -1.50000 AFIX 0 O1 4 0.297955 0.915451 0.647833 11.00000 0.05541 0.05857 = 0.08017 -0.01141 0.00846 0.00412 AFIX 6 O7 4 0.277440 0.338485 0.580406 11.00000 0.09440 0.05075 = 0.07301 0.00928 -0.00891 -0.00008 H7A 2 0.297691 0.213018 0.584257 11.00000 -1.50000 H7B 2 0.322419 0.415940 0.600364 11.00000 -1.50000 AFIX 0 C7 1 0.296305 0.333626 0.731591 11.00000 0.04482 0.02510 = 0.02863 0.00111 0.00176 0.00185 AFIX 13 H7 2 0.254431 0.312298 0.694572 11.00000 -1.20000 AFIX 0 C1 1 0.217653 0.630776 0.470890 11.00000 0.04351 0.03418 = 0.03671 0.00162 0.00478 -0.00047 AFIX 13 H1 2 0.189485 0.600233 0.505385 11.00000 -1.20000 AFIX 0 C8 1 0.264088 0.540120 0.753542 11.00000 0.06493 0.02466 = 0.04952 0.00105 0.01756 0.00064 AFIX 23 H8A 2 0.278858 0.650147 0.728600 11.00000 -1.20000 H8B 2 0.305721 0.566246 0.789885 11.00000 -1.20000 AFIX 0 C6 1 0.174877 0.470328 0.427892 11.00000 0.04965 0.03551 = 0.05942 -0.00851 0.00173 0.00041 AFIX 23 H6A 2 0.195508 0.333038 0.441902 11.00000 -1.20000 H6B 2 0.205503 0.492666 0.394153 11.00000 -1.20000 AFIX 0 C12 1 0.272262 0.156290 0.768711 11.00000 0.06489 0.02454 = 0.03985 0.00306 0.01006 -0.00099 AFIX 23 H12A 2 0.313934 0.172101 0.805504 11.00000 -1.20000 H12B 2 0.291895 0.025741 0.753255 11.00000 -1.20000 AFIX 0 C2 1 0.183578 0.846944 0.452471 11.00000 0.05591 0.03222 = 0.05622 0.00265 -0.00115 -0.00310 AFIX 23 H2D 2 0.214623 0.883462 0.419685 11.00000 -1.20000 H2E 2 0.209564 0.944708 0.481804 11.00000 -1.20000 AFIX 0 C4 1 0.015874 0.700315 0.396525 11.00000 0.04397 0.06118 = 0.05986 -0.00128 0.00268 0.00443 AFIX 23 H4A 2 0.037775 0.731796 0.360904 11.00000 -1.20000 H4B 2 -0.061625 0.706021 0.391788 11.00000 -1.20000 AFIX 0 C9 1 0.144476 0.539562 0.758220 11.00000 0.06608 0.04332 = 0.06656 0.00262 0.01867 0.01313 AFIX 23 H9A 2 0.125512 0.670105 0.773933 11.00000 -1.20000 H9B 2 0.102736 0.525746 0.721382 11.00000 -1.20000 AFIX 0 C11 1 0.153899 0.155356 0.773030 11.00000 0.06899 0.04377 = 0.05105 -0.00069 0.01507 -0.01647 AFIX 23 H11A 2 0.139321 0.044010 0.797619 11.00000 -1.20000 H11B 2 0.113026 0.128949 0.736513 11.00000 -1.20000 AFIX 0 C3 1 0.062276 0.860479 0.439143 11.00000 0.06176 0.03972 = 0.07668 0.00113 0.00429 0.01276 AFIX 23 H3A 2 0.032106 0.840432 0.473114 11.00000 -1.20000 H3B 2 0.042170 0.997827 0.424992 11.00000 -1.20000 AFIX 0 C5 1 0.053136 0.484163 0.414636 11.00000 0.05005 0.04693 = 0.06151 -0.00849 0.00211 -0.00713 AFIX 23 H5A 2 0.027449 0.386633 0.385193 11.00000 -1.20000 H5B 2 0.022576 0.445489 0.447411 11.00000 -1.20000 AFIX 0 C10 1 0.117898 0.360436 0.795208 11.00000 0.06163 0.05228 = 0.06052 -0.00118 0.02501 -0.00233 AFIX 23 H10A 2 0.153739 0.381693 0.833071 11.00000 -1.20000 H10B 2 0.041411 0.356701 0.795733 11.00000 -1.20000 AFIX 0 C13 1 0.202170 0.835908 0.620189 11.00000 0.04437 0.06524 = 0.06177 -0.00480 -0.00040 -0.00019 AFIX 137 H13A 2 0.191324 0.882371 0.582183 11.00000 -1.50000 H13B 2 0.144190 0.883176 0.638188 11.00000 -1.50000 H13C 2 0.204813 0.687216 0.621095 11.00000 -1.50000 AFIX 0 HKLF 4 REM gb-701-a_a.res in P2(1)/c REM R1 = 0.0794 for 2816 Fo > 4sig(Fo) and 0.0927 for all 3446 data REM 220 parameters refined using 0 restraints END WGHT 0.1346 3.0437 REM Highest difference peak 1.629, deepest hole -0.416, 1-sigma level 0.080 Q1 1 0.3041 0.8849 0.5957 11.00000 0.05 1.63 Q2 1 0.4982 0.9355 0.5904 11.00000 0.05 1.45 Q3 1 0.4225 0.9236 0.6866 11.00000 0.05 1.24 Q4 1 0.4824 0.6371 0.6561 11.00000 0.05 0.27 Q5 1 0.4250 0.7408 0.6357 11.00000 0.05 0.27 Q6 1 0.3352 0.3471 0.7327 11.00000 0.05 0.26 Q7 1 0.1379 0.8530 0.4570 11.00000 0.05 0.26 Q8 1 0.2793 0.2356 0.7470 11.00000 0.05 0.25 Q9 1 0.1375 0.4307 0.7722 11.00000 0.05 0.25 Q10 1 0.3412 0.3199 0.5476 11.00000 0.05 0.25 Q11 1 0.2765 0.4336 0.7428 11.00000 0.05 0.24 Q12 1 0.1364 0.2628 0.7852 11.00000 0.05 0.23 Q13 1 0.1847 0.8560 0.4237 11.00000 0.05 0.23 Q14 1 0.0353 0.5920 0.4055 11.00000 0.05 0.23 Q15 1 0.1225 0.4831 0.4183 11.00000 0.05 0.23 Q16 1 0.6171 0.8129 0.5403 11.00000 0.05 0.23 Q17 1 0.1893 0.5663 0.7800 11.00000 0.05 0.21 Q18 1 0.4651 0.6854 0.4068 11.00000 0.05 0.21 Q19 1 0.2069 0.9100 0.4476 11.00000 0.05 0.20 Q20 1 0.4251 0.6367 0.6671 11.00000 0.05 0.20 ; _shelx_res_checksum 72839 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp P1 P 0.41407(7) 0.84549(13) 0.63048(3) 0.0309(3) Uani 1 1 d . . O2 O 0.4274(2) 0.6156(4) 0.64043(12) 0.0476(7) Uani 1 1 d . . O3 O 0.4846(3) 0.9787(5) 0.67108(12) 0.0590(9) Uani 1 1 d . . O6 O 0.4169(3) 0.6787(5) 0.38213(14) 0.0561(8) Uani 1 1 d G . H6C H 0.4440 0.7928 0.3738 0.084 Uiso 1 1 d G U H6D H 0.4606 0.5807 0.3794 0.084 Uiso 1 1 d G U N2 N 0.4122(2) 0.3374(4) 0.72548(12) 0.0357(7) Uani 1 1 d . . H2A H 0.4235 0.4372 0.7018 0.043 Uiso 1 1 calc R U H2B H 0.4305 0.2156 0.7125 0.043 Uiso 1 1 calc R U H2C H 0.4516 0.3615 0.7585 0.043 Uiso 1 1 calc R U O4 O 0.4110(3) 0.9010(5) 0.57044(11) 0.0608(9) Uani 1 1 d . . N1 N 0.3368(3) 0.6185(5) 0.48275(13) 0.0428(8) Uani 1 1 d . . H1A H 0.3640 0.6585 0.4528 0.051 Uiso 1 1 calc R U H1B H 0.3565 0.4886 0.4913 0.051 Uiso 1 1 calc R U H1C H 0.3610 0.7012 0.5113 0.051 Uiso 1 1 calc R U O5 O 0.5869(3) 0.7959(6) 0.51389(17) 0.0725(10) Uani 1 1 d G . H5C H 0.5596 0.8513 0.5402 0.109 Uiso 1 1 d G U H5D H 0.5670 0.8621 0.4838 0.109 Uiso 1 1 d G U O1 O 0.2980(3) 0.9155(5) 0.64783(15) 0.0649(9) Uani 1 1 d . . O7 O 0.2774(3) 0.3385(5) 0.58041(17) 0.0750(11) Uani 1 1 d G . H7A H 0.2977 0.2130 0.5843 0.113 Uiso 1 1 d G U H7B H 0.3224 0.4159 0.6004 0.113 Uiso 1 1 d G U C7 C 0.2963(3) 0.3336(5) 0.73159(14) 0.0333(8) Uani 1 1 d . . H7 H 0.2544 0.3123 0.6946 0.040 Uiso 1 1 calc R U C1 C 0.2177(3) 0.6308(6) 0.47089(16) 0.0383(8) Uani 1 1 d . . H1 H 0.1895 0.6002 0.5054 0.046 Uiso 1 1 calc R U C8 C 0.2641(3) 0.5401(6) 0.75354(17) 0.0455(10) Uani 1 1 d . . H8A H 0.2789 0.6501 0.7286 0.055 Uiso 1 1 calc R U H8B H 0.3057 0.5662 0.7899 0.055 Uiso 1 1 calc R U C6 C 0.1749(3) 0.4703(6) 0.42789(18) 0.0489(10) Uani 1 1 d . . H6A H 0.1955 0.3330 0.4419 0.059 Uiso 1 1 calc R U H6B H 0.2055 0.4927 0.3942 0.059 Uiso 1 1 calc R U C12 C 0.2723(3) 0.1563(5) 0.76871(16) 0.0429(9) Uani 1 1 d . . H12A H 0.3139 0.1721 0.8055 0.051 Uiso 1 1 calc R U H12B H 0.2919 0.0257 0.7533 0.051 Uiso 1 1 calc R U C2 C 0.1836(3) 0.8469(6) 0.45247(19) 0.0492(10) Uani 1 1 d . . H2D H 0.2146 0.8835 0.4197 0.059 Uiso 1 1 calc R U H2E H 0.2096 0.9447 0.4818 0.059 Uiso 1 1 calc R U C4 C 0.0159(4) 0.7003(7) 0.3965(2) 0.0556(11) Uani 1 1 d . . H4A H 0.0378 0.7318 0.3609 0.067 Uiso 1 1 calc R U H4B H -0.0616 0.7060 0.3918 0.067 Uiso 1 1 calc R U C9 C 0.1445(4) 0.5396(7) 0.7582(2) 0.0578(11) Uani 1 1 d . . H9A H 0.1255 0.6701 0.7739 0.069 Uiso 1 1 calc R U H9B H 0.1027 0.5257 0.7214 0.069 Uiso 1 1 calc R U C11 C 0.1539(4) 0.1554(7) 0.77303(19) 0.0540(11) Uani 1 1 d . . H11A H 0.1393 0.0440 0.7976 0.065 Uiso 1 1 calc R U H11B H 0.1130 0.1289 0.7365 0.065 Uiso 1 1 calc R U C3 C 0.0623(4) 0.8605(7) 0.4391(2) 0.0601(12) Uani 1 1 d . . H3A H 0.0321 0.8404 0.4731 0.072 Uiso 1 1 calc R U H3B H 0.0422 0.9978 0.4250 0.072 Uiso 1 1 calc R U C5 C 0.0531(3) 0.4842(7) 0.4146(2) 0.0535(11) Uani 1 1 d . . H5A H 0.0274 0.3866 0.3852 0.064 Uiso 1 1 calc R U H5B H 0.0226 0.4455 0.4474 0.064 Uiso 1 1 calc R U C10 C 0.1179(4) 0.3604(7) 0.7952(2) 0.0565(12) Uani 1 1 d . . H10A H 0.1537 0.3817 0.8331 0.068 Uiso 1 1 calc R U H10B H 0.0414 0.3567 0.7957 0.068 Uiso 1 1 calc R U C13 C 0.2022(4) 0.8359(8) 0.6202(2) 0.0580(12) Uani 1 1 d . . H13A H 0.1913 0.8824 0.5822 0.087 Uiso 1 1 calc R U H13B H 0.1442 0.8832 0.6382 0.087 Uiso 1 1 calc R U H13C H 0.2048 0.6872 0.6211 0.087 Uiso 1 1 calc R U 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 P1 0.0411(6) 0.0227(5) 0.0281(5) 0.0023(3) 0.0026(4) -0.0008(3) O2 0.0624(18) 0.0254(14) 0.0552(16) 0.0066(12) 0.0099(14) 0.0021(12) O3 0.080(2) 0.0406(16) 0.0482(16) -0.0102(13) -0.0176(15) 0.0074(15) O6 0.0589(19) 0.0464(17) 0.067(2) 0.0034(15) 0.0225(16) -0.0029(14) N2 0.0486(18) 0.0271(15) 0.0302(15) -0.0004(12) 0.0022(13) 0.0004(12) O4 0.092(2) 0.0521(18) 0.0379(16) 0.0073(13) 0.0083(15) -0.0043(17) N1 0.0491(19) 0.0380(18) 0.0392(17) 0.0005(14) 0.0004(14) -0.0002(14) O5 0.074(2) 0.062(2) 0.085(2) 0.021(2) 0.024(2) 0.0217(18) O1 0.0554(19) 0.059(2) 0.080(2) -0.0114(18) 0.0085(16) 0.0041(15) O7 0.094(3) 0.051(2) 0.073(2) 0.0093(18) -0.009(2) -0.0001(19) C7 0.045(2) 0.0251(17) 0.0286(17) 0.0011(13) 0.0018(14) 0.0019(14) C1 0.044(2) 0.034(2) 0.0367(18) 0.0016(15) 0.0048(15) -0.0005(15) C8 0.065(3) 0.0247(19) 0.050(2) 0.0010(16) 0.0176(19) 0.0006(17) C6 0.050(2) 0.036(2) 0.059(2) -0.0085(19) 0.0017(19) 0.0004(17) C12 0.065(3) 0.0245(18) 0.040(2) 0.0031(15) 0.0101(18) -0.0010(16) C2 0.056(3) 0.032(2) 0.056(2) 0.0026(18) -0.001(2) -0.0031(17) C4 0.044(2) 0.061(3) 0.060(3) -0.001(2) 0.0027(19) 0.004(2) C9 0.066(3) 0.043(2) 0.067(3) 0.003(2) 0.019(2) 0.013(2) C11 0.069(3) 0.044(2) 0.051(2) -0.0007(19) 0.015(2) -0.016(2) C3 0.062(3) 0.040(2) 0.077(3) 0.001(2) 0.004(2) 0.013(2) C5 0.050(2) 0.047(2) 0.062(3) -0.008(2) 0.0021(19) -0.0071(19) C10 0.062(3) 0.052(3) 0.061(3) -0.001(2) 0.025(2) -0.002(2) C13 0.044(2) 0.065(3) 0.062(3) -0.005(2) 0.000(2) 0.000(2) 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' P P 0.1023 0.0942 '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 O3 P1 O4 115.34(19) O3 P1 O2 114.78(17) O4 P1 O2 112.16(18) O3 P1 O1 97.93(18) O4 P1 O1 107.05(19) O2 P1 O1 108.03(17) H6C O6 H6D 109.5 C7 N2 H2A 109.5 C7 N2 H2B 109.5 H2A N2 H2B 109.5 C7 N2 H2C 109.5 H2A N2 H2C 109.5 H2B N2 H2C 109.5 C1 N1 H1A 109.5 C1 N1 H1B 109.5 H1A N1 H1B 109.5 C1 N1 H1C 109.5 H1A N1 H1C 109.5 H1B N1 H1C 109.5 H5C O5 H5D 109.5 C13 O1 P1 121.3(3) H7A O7 H7B 109.5 N2 C7 C8 110.0(3) N2 C7 C12 111.2(3) C8 C7 C12 111.4(3) N2 C7 H7 108.1 C8 C7 H7 108.1 C12 C7 H7 108.1 N1 C1 C2 109.9(3) N1 C1 C6 109.9(3) C2 C1 C6 111.9(3) N1 C1 H1 108.3 C2 C1 H1 108.3 C6 C1 H1 108.3 C7 C8 C9 110.3(3) C7 C8 H8A 109.6 C9 C8 H8A 109.6 C7 C8 H8B 109.6 C9 C8 H8B 109.6 H8A C8 H8B 108.1 C1 C6 C5 110.3(3) C1 C6 H6A 109.6 C5 C6 H6A 109.6 C1 C6 H6B 109.6 C5 C6 H6B 109.6 H6A C6 H6B 108.1 C7 C12 C11 109.6(3) C7 C12 H12A 109.8 C11 C12 H12A 109.8 C7 C12 H12B 109.8 C11 C12 H12B 109.8 H12A C12 H12B 108.2 C1 C2 C3 110.4(3) C1 C2 H2D 109.6 C3 C2 H2D 109.6 C1 C2 H2E 109.6 C3 C2 H2E 109.6 H2D C2 H2E 108.1 C3 C4 C5 111.0(4) C3 C4 H4A 109.4 C5 C4 H4A 109.4 C3 C4 H4B 109.4 C5 C4 H4B 109.4 H4A C4 H4B 108.0 C10 C9 C8 110.7(4) C10 C9 H9A 109.5 C8 C9 H9A 109.5 C10 C9 H9B 109.5 C8 C9 H9B 109.5 H9A C9 H9B 108.1 C12 C11 C10 111.9(4) C12 C11 H11A 109.2 C10 C11 H11A 109.2 C12 C11 H11B 109.2 C10 C11 H11B 109.2 H11A C11 H11B 107.9 C4 C3 C2 112.2(4) C4 C3 H3A 109.2 C2 C3 H3A 109.2 C4 C3 H3B 109.2 C2 C3 H3B 109.2 H3A C3 H3B 107.9 C4 C5 C6 111.9(4) C4 C5 H5A 109.2 C6 C5 H5A 109.2 C4 C5 H5B 109.2 C6 C5 H5B 109.2 H5A C5 H5B 107.9 C11 C10 C9 110.0(4) C11 C10 H10A 109.7 C9 C10 H10A 109.7 C11 C10 H10B 109.7 C9 C10 H10B 109.7 H10A C10 H10B 108.2 O1 C13 H13A 109.5 O1 C13 H13B 109.5 H13A C13 H13B 109.5 O1 C13 H13C 109.5 H13A C13 H13C 109.5 H13B C13 H13C 109.5 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance P1 O3 1.495(3) P1 O4 1.496(3) P1 O2 1.508(3) P1 O1 1.653(3) O6 H6C 0.8501 O6 H6D 0.8499 N2 C7 1.497(5) N2 H2A 0.8900 N2 H2B 0.8900 N2 H2C 0.8900 N1 C1 1.492(5) N1 H1A 0.8900 N1 H1B 0.8900 N1 H1C 0.8900 O5 H5C 0.8503 O5 H5D 0.8499 O1 C13 1.389(5) O7 H7A 0.8498 O7 H7B 0.8503 C7 C8 1.514(5) C7 C12 1.516(5) C7 H7 0.9800 C1 C2 1.507(5) C1 C6 1.510(5) C1 H1 0.9800 C8 C9 1.535(6) C8 H8A 0.9700 C8 H8B 0.9700 C6 C5 1.526(6) C6 H6A 0.9700 C6 H6B 0.9700 C12 C11 1.517(6) C12 H12A 0.9700 C12 H12B 0.9700 C2 C3 1.521(6) C2 H2D 0.9700 C2 H2E 0.9700 C4 C3 1.515(7) C4 C5 1.515(6) C4 H4A 0.9700 C4 H4B 0.9700 C9 C10 1.533(6) C9 H9A 0.9700 C9 H9B 0.9700 C11 C10 1.525(6) C11 H11A 0.9700 C11 H11B 0.9700 C3 H3A 0.9700 C3 H3B 0.9700 C5 H5A 0.9700 C5 H5B 0.9700 C10 H10A 0.9700 C10 H10B 0.9700 C13 H13A 0.9600 C13 H13B 0.9600 C13 H13C 0.9600 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 O6 H6C O3 0.85 2.12 2.934(4) 161.2 3_676 O6 H6D O2 0.85 2.01 2.850(4) 167.9 3_666 N2 H2A O2 0.89 1.89 2.766(4) 167.8 . N2 H2B O3 0.89 2.01 2.884(4) 167.6 1_545 N2 H2C O3 0.89 1.93 2.798(4) 165.2 2_646 N1 H1A O6 0.89 1.94 2.814(4) 166.6 . N1 H1B O5 0.89 1.98 2.839(5) 161.6 3_666 N1 H1C O4 0.89 1.96 2.850(4) 175.7 . O5 H5C O4 0.85 2.15 2.872(5) 143.0 . O5 H5D O4 0.85 2.06 2.835(5) 150.4 3_676 O7 H7A O4 0.85 2.52 3.317(5) 155.9 1_545 O7 H7A O1 0.85 2.46 3.173(5) 141.5 1_545 O7 H7B O2 0.85 1.99 2.840(5) 174.3 . C1 H1 O7 0.98 2.60 3.253(5) 123.8 . C8 H8A O1 0.97 2.64 3.603(5) 170.5 . loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion O3 P1 O1 C13 178.4(4) O4 P1 O1 C13 58.8(4) O2 P1 O1 C13 -62.2(4) N2 C7 C8 C9 178.3(3) C12 C7 C8 C9 -58.0(4) N1 C1 C6 C5 -178.9(3) C2 C1 C6 C5 -56.5(5) N2 C7 C12 C11 -179.0(3) C8 C7 C12 C11 57.9(4) N1 C1 C2 C3 178.9(3) C6 C1 C2 C3 56.5(5) C7 C8 C9 C10 56.5(5) C7 C12 C11 C10 -57.4(5) C5 C4 C3 C2 54.0(5) C1 C2 C3 C4 -55.0(5) C3 C4 C5 C6 -53.9(5) C1 C6 C5 C4 55.1(5) C12 C11 C10 C9 56.6(5) C8 C9 C10 C11 -55.6(5)