#------------------------------------------------------------------------------ #$Date: 2023-05-05 04:45:21 +0300 (Fri, 05 May 2023) $ #$Revision: 283244 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/71/21/7712166.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_7712166 loop_ _publ_author_name 'Matharoo, Navneet' 'Walawalkar, Mrinalini G.' 'Murugavel, Ramaswamy' _publ_section_title ; A rigid calcium 2-ethylhexylphosphate one-dimensional polymer: synthesis, structure, thermal behaviour and decomposition chemistry. ; _journal_issue 8 _journal_name_full 'Dalton transactions (Cambridge, England : 2003)' _journal_page_first 2412 _journal_page_last 2423 _journal_paper_doi 10.1039/d2dt03529d _journal_volume 52 _journal_year 2023 _chemical_formula_moiety 'C28 H44 Ca N2 O8 P2' _chemical_formula_sum 'C28 H44 Ca N2 O8 P2' _chemical_formula_weight 638.67 _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-I 2ya' _space_group_name_H-M_alt 'I 1 2/a 1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary iterative _audit_creation_date 2023-01-08 _audit_creation_method ; Olex2 1.5 (compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498) ; _audit_update_record ; 2023-01-11 deposited with the CCDC. 2023-01-19 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 96.050(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 9.4853(3) _cell_length_b 11.0551(3) _cell_length_c 30.9403(12) _cell_measurement_reflns_used 3853 _cell_measurement_temperature 233.15 _cell_measurement_theta_max 21.8870 _cell_measurement_theta_min 1.9510 _cell_volume 3226.36(18) _computing_cell_refinement 'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)' _computing_data_collection 'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)' _computing_data_reduction 'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'olex2.solve 1.5 (Bourhis et al., 2015)' _diffrn_ambient_temperature 233.15 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'Saxi-CrysAlisPro-abstract goniometer imported SAXI images' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0972 _diffrn_reflns_av_unetI/netI 0.0480 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_number 31460 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_theta_full 25.000 _diffrn_reflns_theta_max 25.000 _diffrn_reflns_theta_min 1.957 _exptl_absorpt_coefficient_mu 0.342 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.45171 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10 ; _exptl_crystal_colour 'clear whiteish colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier whiteish _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.315 _exptl_crystal_description plate _exptl_crystal_F_000 1360 _exptl_crystal_size_max 0.441 _exptl_crystal_size_mid 0.277 _exptl_crystal_size_min 0.011 _refine_diff_density_max 0.355 _refine_diff_density_min -0.340 _refine_diff_density_rms 0.055 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 253 _refine_ls_number_reflns 2842 _refine_ls_number_restraints 133 _refine_ls_restrained_S_all 1.018 _refine_ls_R_factor_all 0.0783 _refine_ls_R_factor_gt 0.0513 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0699P)^2^+2.0291P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1252 _refine_ls_wR_factor_ref 0.1417 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2028 _reflns_number_total 2842 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; TITL rm_nm_ca_ehp_233k_a.res in I2/a nm_ehp_233k.res created by SHELXL-2018/3 at 22:55:13 on 08-Jan-2023 REM Old TITL rm_nm_ca_ehp_233k_a.res in I2/a REM SHELXT solution in I2/a: R1 0.205, Rweak 0.011, Alpha 0.060 REM 0.418 for 180 systematic absences, Orientation as input REM Formula found by SHELXT: C24 Ca N4 O10 P2 CELL 0.71073 9.4853 11.0551 30.9403 90 96.05 90 ZERR 4 0.0003 0.0003 0.0012 0 0.003 0 LATT 2 SYMM 0.5-X,+Y,-Z SFAC C H Ca N O P UNIT 112 176 4 8 32 8 SADI C14A C15A C14B C15B SADI C14A C19A C14B C19B SADI C19A C20A C19B C20B SADI 0.04 C15A C19A C15B C19B SADI C15A C16A C15B C16B SADI C16A C17A C16B C17B RIGU C13A C17A C19A C14A C18A C15A C20A C16A SADI C17A C18A C17B C18B RIGU C17B C19B C14B C18B C15B C20B C16B SIMU 0.01 0.02 2 C19A C19B SADI 0.04 O4 C14A O4 C14B SADI 0.04 C14A C16A C14B C16B SADI 0.04 C14A C20A C14B C20B SADI 0.04 C15A C17A C15B C17B SADI 0.04 C16A C18A C16B C18B SADI 0.0001 C16B C15B C17B C16B C18B C17B C15B C14B C15A C14A C16A C15A = C17A C16A C18A C17A SIMU 0.001 0.002 2 C17B C17A SIMU 0.001 0.002 2 C20B C20A L.S. 25 PLAN 6 0 0 SIZE 0.441 0.277 0.011 TEMP -40 CONF CONN 6 $Ca BOND list 4 MORE -1 BOND $H fmap 2 acta OMIT -3 50 REM REM REM > REM REM > REM > REM REM WGHT 0.069900 2.029100 FVAR 0.22122 0.45120 CA1 3 0.250000 0.148854 0.500000 10.50000 0.03420 0.01929 = 0.06590 0.00000 0.00883 0.00000 P1 6 0.495390 0.037018 0.432712 11.00000 0.03237 0.02586 = 0.06245 0.00065 0.00654 0.00079 O1 5 0.437934 0.132529 0.459683 11.00000 0.03737 0.02705 = 0.08094 -0.00740 0.01542 -0.00309 O2 5 0.638070 -0.015468 0.447447 11.00000 0.03343 0.03747 = 0.06787 0.00373 0.00677 0.00381 O3 5 0.386783 -0.071040 0.425732 11.00000 0.03754 0.02856 = 0.09147 -0.01278 0.01312 -0.00336 AFIX 147 H3 2 0.307463 -0.048119 0.431404 11.00000 -1.50000 AFIX 0 O4 5 0.502363 0.095821 0.386129 11.00000 0.05769 0.05128 = 0.06702 0.01318 0.00897 0.00162 N1 4 0.360149 0.341583 0.532259 11.00000 0.04201 0.02546 = 0.06251 0.00124 0.01047 0.00099 C1 1 0.469662 0.343754 0.562735 11.00000 0.05030 0.03181 = 0.06466 0.00042 0.00692 -0.00111 AFIX 43 H1 2 0.505802 0.269480 0.573768 11.00000 -1.20000 AFIX 0 C2 1 0.534673 0.450322 0.579457 11.00000 0.05407 0.04198 = 0.06783 -0.00554 0.00293 -0.00408 AFIX 43 H2 2 0.613240 0.446823 0.600643 11.00000 -1.20000 AFIX 0 C3 1 0.482426 0.558336 0.564586 11.00000 0.04815 0.03518 = 0.07840 -0.01280 0.01368 -0.00752 AFIX 43 H3A 2 0.523657 0.630702 0.575739 11.00000 -1.20000 AFIX 0 C4 1 0.366114 0.561693 0.532357 11.00000 0.03798 0.02595 = 0.07498 -0.00668 0.01613 -0.00402 C5 1 0.308558 0.450427 0.516836 11.00000 0.03648 0.02074 = 0.06523 -0.00201 0.01612 0.00017 C6 1 0.304766 0.672723 0.515009 11.00000 0.04453 0.02095 = 0.10934 -0.00460 0.01507 -0.00179 AFIX 43 H6 2 0.343564 0.746864 0.525282 11.00000 -1.20000 AFIX 0 C13A 1 0.562649 0.029552 0.352739 11.00000 0.13876 0.06859 = 0.06022 -0.00440 0.01725 -0.01443 PART 1 AFIX 23 H13A 2 0.530527 -0.054742 0.351239 21.00000 -1.20000 H13B 2 0.666498 0.032096 0.356401 21.00000 -1.20000 AFIX 23 PART 2 H13C 2 0.505708 -0.043435 0.346230 -21.00000 -1.20000 H13D 2 0.658163 0.003464 0.364100 -21.00000 -1.20000 AFIX 0 PART 1 C14A 1 0.495956 0.108365 0.310333 21.00000 0.05667 0.08993 = 0.06748 0.01233 0.01171 -0.01486 AFIX 13 H14A 2 0.391658 0.115359 0.309528 21.00000 -1.20000 AFIX 0 C15A 1 0.536785 0.032244 0.273185 21.00000 0.09845 0.13370 = 0.08156 -0.01270 0.03841 -0.00601 AFIX 23 H15A 2 0.498356 -0.049157 0.276421 21.00000 -1.20000 H15B 2 0.640334 0.025036 0.276270 21.00000 -1.20000 AFIX 0 C16A 1 0.490496 0.074662 0.227580 21.00000 0.13837 0.10351 = 0.09642 -0.00318 0.03152 -0.02223 AFIX 23 H16A 2 0.550199 0.143621 0.221455 21.00000 -1.20000 H16B 2 0.510475 0.009603 0.207592 21.00000 -1.20000 AFIX 0 C17A 1 0.337925 0.111881 0.216806 21.00000 0.14301 0.11737 = 0.08906 -0.03695 -0.01150 -0.03176 AFIX 23 H17A 2 0.274715 0.045237 0.222818 21.00000 -1.20000 H17B 2 0.316179 0.181666 0.234476 21.00000 -1.20000 AFIX 0 C18A 1 0.317417 0.144216 0.169219 21.00000 0.15096 0.24633 = 0.07745 -0.02935 0.03096 -0.01210 AFIX 3 H18A 2 0.227887 0.186476 0.163199 21.00000 -1.50000 H18B 2 0.394587 0.198056 0.164029 21.00000 -1.50000 H18C 2 0.318507 0.074236 0.150349 21.00000 -1.50000 AFIX 0 C19A 1 0.567567 0.234730 0.313582 21.00000 0.07111 0.09288 = 0.07516 0.02108 0.00108 -0.00370 AFIX 23 H19A 2 0.537883 0.279348 0.286793 21.00000 -1.20000 H19B 2 0.531712 0.278936 0.337608 21.00000 -1.20000 AFIX 0 C20A 1 0.720298 0.235269 0.320235 21.00000 0.07695 0.14400 = 0.17777 0.05322 -0.04572 -0.04244 AFIX 137 H20A 2 0.750961 0.240342 0.351095 21.00000 -1.50000 H20B 2 0.756189 0.304425 0.305502 21.00000 -1.50000 H20C 2 0.756510 0.161401 0.308583 21.00000 -1.50000 AFIX 0 PART 2 C14B 1 0.572444 0.096979 0.311144 -21.00000 0.07335 0.08360 = 0.05538 0.00007 0.00849 -0.01527 AFIX 13 H14B 2 0.646628 0.056291 0.296192 -21.00000 -1.20000 AFIX 0 C15B 1 0.434705 0.080386 0.282692 -21.00000 0.07681 0.08054 = 0.07421 -0.00415 -0.00915 -0.00318 AFIX 23 H15C 2 0.413546 -0.006364 0.281075 -21.00000 -1.20000 H15D 2 0.359416 0.119193 0.297116 -21.00000 -1.20000 AFIX 0 C16B 1 0.427345 0.128602 0.236929 -21.00000 0.08449 0.09324 = 0.06274 -0.01477 0.00721 -0.00072 AFIX 23 H16C 2 0.511002 0.100217 0.223823 -21.00000 -1.20000 H16D 2 0.432246 0.217089 0.238264 -21.00000 -1.20000 AFIX 0 C17B 1 0.296934 0.093310 0.207520 -21.00000 0.14279 0.11731 = 0.08908 -0.03697 -0.01178 -0.03188 AFIX 23 H17C 2 0.291630 0.004867 0.205943 -21.00000 -1.20000 H17D 2 0.212873 0.122050 0.220329 -21.00000 -1.20000 AFIX 0 C18B 1 0.294022 0.143198 0.162083 -21.00000 0.10950 0.12644 = 0.08414 -0.02323 -0.02578 0.03804 AFIX 3 H18D 2 0.200192 0.129988 0.147123 -21.00000 -1.50000 H18E 2 0.315922 0.228918 0.162113 -21.00000 -1.50000 H18F 2 0.363382 0.099318 0.147293 -21.00000 -1.50000 AFIX 0 C19B 1 0.620165 0.231983 0.318025 -21.00000 0.07604 0.10294 = 0.09199 0.03901 -0.00926 -0.02664 AFIX 23 H19C 2 0.606977 0.272584 0.289731 -21.00000 -1.20000 H19D 2 0.555830 0.270711 0.336612 -21.00000 -1.20000 AFIX 0 C20B 1 0.760062 0.253968 0.336355 -21.00000 0.07789 0.14308 = 0.17705 0.05255 -0.04595 -0.04297 AFIX 137 H20D 2 0.779480 0.206753 0.362736 -21.00000 -1.50000 H20E 2 0.771368 0.339286 0.343176 -21.00000 -1.50000 H20F 2 0.825705 0.231008 0.315781 -21.00000 -1.50000 AFIX 0 HKLF 4 REM rm_nm_ca_ehp_233k_a.res in I2/a REM wR2 = 0.1417, GooF = S = 1.030, Restrained GooF = 1.018 for all data REM R1 = 0.0513 for 2028 Fo > 4sig(Fo) and 0.0783 for all 2842 data REM 253 parameters refined using 133 restraints END WGHT 0.0699 2.0291 REM Highest difference peak 0.355, deepest hole -0.340, 1-sigma level 0.055 Q1 1 0.4065 0.0717 0.1882 11.00000 0.05 0.36 Q2 1 0.7500 0.0670 0.5000 10.50000 0.05 0.32 Q3 1 0.2500 0.7753 0.5000 10.50000 0.05 0.27 Q4 1 0.6899 0.1545 0.3147 11.00000 0.05 0.25 Q5 1 0.3509 0.1575 0.4678 11.00000 0.05 0.20 Q6 1 0.6239 -0.0723 0.4498 11.00000 0.05 0.20 REM The information below was added by Olex2. REM REM R1 = 0.0513 for 2028 Fo > 4sig(Fo) and 0.0783 for all 46513 data REM 253 parameters refined using n/a restraints REM Highest difference peak 0.36, deepest hole -0.34 REM Mean Shift 0, Max Shift 0.001. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0783 REM R1_gt = 0.0513 REM wR_ref = 0.1417 REM GOOF = 1.030 REM Shift_max = 0.001 REM Shift_mean = 0 REM Reflections_all = 46513 REM Reflections_gt = 2028 REM Parameters = 253 REM Hole = -0.34 REM Peak = 0.36 REM Flack = n/a ; _cod_data_source_file d2dt03529d2.cif _cod_data_source_block nm_ehp_233k _cod_depositor_comments 'Adding full bibliography for 7712164--7712167.cif.' _cod_database_code 7712166 _shelx_shelxl_version_number 2018/3 _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_max 0.996 _shelx_estimated_absorpt_t_min 0.864 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups At 1.5 times of: All C(H,H,H) groups, All O(H) groups 2. Restrained distances C14A-C15A \\sim C14B-C15B with sigma of 0.02 C14A-C19A \\sim C14B-C19B with sigma of 0.02 C19A-C20A \\sim C19B-C20B with sigma of 0.02 C15A-C19A \\sim C15B-C19B with sigma of 0.04 C15A-C16A \\sim C15B-C16B with sigma of 0.02 C16A-C17A \\sim C16B-C17B with sigma of 0.02 C17A-C18A \\sim C17B-C18B with sigma of 0.02 O4-C14A \\sim O4-C14B with sigma of 0.04 C14A-C16A \\sim C14B-C16B with sigma of 0.04 C14A-C20A \\sim C14B-C20B with sigma of 0.04 C15A-C17A \\sim C15B-C17B with sigma of 0.04 C16A-C18A \\sim C16B-C18B with sigma of 0.04 C16B-C15B \\sim C17B-C16B \\sim C18B-C17B \\sim C15B-C14B \\sim C15A-C14A \\sim C16A-C15A \\sim C17A- C16A \\sim C18A-C17A with sigma of 0.0001 3. Uiso/Uaniso restraints and constraints C19A \\sim C19B: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A C17B \\sim C17A: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002 within 2A C20B \\sim C20A: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002 within 2A 4. Rigid body (RIGU) restrains C13A, C17A, C19A, C14A, C18A, C15A, C20A, C16A with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 C17B, C19B, C14B, C18B, C15B, C20B, C16B with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 5. Others Sof(H13C)=Sof(H13D)=Sof(C14B)=Sof(H14B)=Sof(C15B)=Sof(H15C)=Sof(H15D)= Sof(C16B)=Sof(H16C)=Sof(H16D)=Sof(C17B)=Sof(H17C)=Sof(H17D)=Sof(C18B)= Sof(H18D)=Sof(H18E)=Sof(H18F)=Sof(C19B)=Sof(H19C)=Sof(H19D)=Sof(C20B)= Sof(H20D)=Sof(H20E)=Sof(H20F)=1-FVAR(1) Sof(H13A)=Sof(H13B)=Sof(C14A)=Sof(H14A)=Sof(C15A)=Sof(H15A)=Sof(H15B)= Sof(C16A)=Sof(H16A)=Sof(H16B)=Sof(C17A)=Sof(H17A)=Sof(H17B)=Sof(C18A)= Sof(H18A)=Sof(H18B)=Sof(H18C)=Sof(C19A)=Sof(H19A)=Sof(H19B)=Sof(C20A)= Sof(H20A)=Sof(H20B)=Sof(H20C)=FVAR(1) 6.a Riding coordinates: C18A(H18A,H18B,H18C), C18B(H18D,H18E,H18F) 6.b Ternary CH refined with riding coordinates: C14A(H14A), C14B(H14B) 6.c Secondary CH2 refined with riding coordinates: C13A(H13A,H13B), C13A(H13C,H13D), C15A(H15A,H15B), C16A(H16A,H16B), C17A(H17A, H17B), C19A(H19A,H19B), C15B(H15C,H15D), C16B(H16C,H16D), C17B(H17C,H17D), C19B(H19C,H19D) 6.d Aromatic/amide H refined with riding coordinates: C1(H1), C2(H2), C3(H3A), C6(H6) 6.e Idealised Me refined as rotating group: C20A(H20A,H20B,H20C), C20B(H20D,H20E,H20F) 6.f Idealised tetrahedral OH refined as rotating group: O3(H3) ; _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z' '-x+1/2, -y+1/2, -z+1/2' '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 _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ca1 Ca 0.250000 0.14885(7) 0.500000 0.0395(3) Uani 1 2 d S T P . . P1 P 0.49539(8) 0.03702(7) 0.43271(3) 0.0401(3) Uani 1 1 d . . . . . O1 O 0.4379(2) 0.13253(17) 0.45968(7) 0.0478(6) Uani 1 1 d . . . . . O2 O 0.6381(2) -0.01547(18) 0.44745(7) 0.0462(6) Uani 1 1 d . . . . . O3 O 0.3868(2) -0.07104(18) 0.42573(8) 0.0521(6) Uani 1 1 d . . . . . H3 H 0.307463 -0.048119 0.431404 0.078 Uiso 1 1 calc R U . . . O4 O 0.5024(2) 0.0958(2) 0.38613(8) 0.0585(6) Uani 1 1 d D . . . . N1 N 0.3601(3) 0.3416(2) 0.53226(9) 0.0430(6) Uani 1 1 d . . . . . C1 C 0.4697(3) 0.3438(3) 0.56273(11) 0.0489(8) Uani 1 1 d . . . . . H1 H 0.505802 0.269480 0.573768 0.059 Uiso 1 1 calc R U . . . C2 C 0.5347(4) 0.4503(3) 0.57946(12) 0.0549(9) Uani 1 1 d . . . . . H2 H 0.613240 0.446823 0.600643 0.066 Uiso 1 1 calc R U . . . C3 C 0.4824(3) 0.5583(3) 0.56459(12) 0.0534(9) Uani 1 1 d . . . . . H3A H 0.523657 0.630702 0.575739 0.064 Uiso 1 1 calc R U . . . C4 C 0.3661(3) 0.5617(3) 0.53236(11) 0.0456(8) Uani 1 1 d . . . . . C5 C 0.3086(3) 0.4504(2) 0.51684(10) 0.0401(7) Uani 1 1 d . . . . . C6 C 0.3048(3) 0.6727(3) 0.51501(13) 0.0578(10) Uani 1 1 d . . . . . H6 H 0.343564 0.746864 0.525282 0.069 Uiso 1 1 calc R U . . . C13A C 0.5626(6) 0.0296(4) 0.35274(13) 0.0887(14) Uani 1 1 d . . . . . H13A H 0.530527 -0.054742 0.351239 0.106 Uiso 0.451(6) 1 calc R U P A 1 H13B H 0.666498 0.032096 0.356401 0.106 Uiso 0.451(6) 1 calc R U P A 1 H13C H 0.505708 -0.043435 0.346230 0.106 Uiso 0.549(6) 1 calc R U P A 2 H13D H 0.658163 0.003464 0.364100 0.106 Uiso 0.549(6) 1 calc R U P A 2 C14A C 0.4960(6) 0.1084(4) 0.31033(10) 0.071(3) Uani 0.451(6) 1 d D . P A 1 H14A H 0.391658 0.115359 0.309528 0.085 Uiso 0.451(6) 1 calc R U P A 1 C15A C 0.5368(7) 0.0322(4) 0.27318(6) 0.103(4) Uani 0.451(6) 1 d D . P A 1 H15A H 0.498356 -0.049157 0.276421 0.123 Uiso 0.451(6) 1 calc R U P A 1 H15B H 0.640334 0.025036 0.276270 0.123 Uiso 0.451(6) 1 calc R U P A 1 C16A C 0.4905(3) 0.0747(5) 0.22758(8) 0.111(4) Uani 0.451(6) 1 d D . P A 1 H16A H 0.550199 0.143621 0.221455 0.134 Uiso 0.451(6) 1 calc R U P A 1 H16B H 0.510475 0.009603 0.207592 0.134 Uiso 0.451(6) 1 calc R U P A 1 C17A C 0.3379(3) 0.1119(6) 0.21681(8) 0.118(2) Uani 0.451(6) 1 d D U P A 1 H17A H 0.274715 0.045237 0.222818 0.142 Uiso 0.451(6) 1 calc R U P A 1 H17B H 0.316179 0.181666 0.234476 0.142 Uiso 0.451(6) 1 calc R U P A 1 C18A C 0.317(2) 0.1442(9) 0.16922(8) 0.157(11) Uani 0.451(6) 1 d D . P A 1 H18A H 0.227887 0.186476 0.163199 0.235 Uiso 0.451(6) 1 d R U P A 1 H18B H 0.394587 0.198056 0.164029 0.235 Uiso 0.451(6) 1 d R U P A 1 H18C H 0.318507 0.074236 0.150349 0.235 Uiso 0.451(6) 1 d R U P A 1 C19A C 0.5676(18) 0.2347(13) 0.3136(9) 0.080(4) Uani 0.451(6) 1 d D U P A 1 H19A H 0.537883 0.279348 0.286793 0.096 Uiso 0.451(6) 1 calc R U P A 1 H19B H 0.531712 0.278936 0.337608 0.096 Uiso 0.451(6) 1 calc R U P A 1 C20A C 0.720(2) 0.235(2) 0.3202(9) 0.137(5) Uani 0.451(6) 1 d D U P A 1 H20A H 0.750961 0.240342 0.351095 0.206 Uiso 0.451(6) 1 calc R U P A 1 H20B H 0.756189 0.304425 0.305502 0.206 Uiso 0.451(6) 1 calc R U P A 1 H20C H 0.756510 0.161401 0.308583 0.206 Uiso 0.451(6) 1 calc R U P A 1 C14B C 0.5724(3) 0.0970(8) 0.31114(14) 0.071(3) Uani 0.549(6) 1 d D . P A 2 H14B H 0.646628 0.056291 0.296192 0.085 Uiso 0.549(6) 1 calc R U P A 2 C15B C 0.4347(3) 0.0804(5) 0.28269(7) 0.078(2) Uani 0.549(6) 1 d D . P A 2 H15C H 0.413546 -0.006364 0.281075 0.094 Uiso 0.549(6) 1 calc R U P A 2 H15D H 0.359416 0.119193 0.297116 0.094 Uiso 0.549(6) 1 calc R U P A 2 C16B C 0.4273(3) 0.1286(5) 0.23693(7) 0.080(3) Uani 0.549(6) 1 d D . P A 2 H16C H 0.511002 0.100217 0.223823 0.096 Uiso 0.549(6) 1 calc R U P A 2 H16D H 0.432246 0.217089 0.238264 0.096 Uiso 0.549(6) 1 calc R U P A 2 C17B C 0.2969(3) 0.0933(5) 0.20752(7) 0.118(2) Uani 0.549(6) 1 d D U P A 2 H17C H 0.291630 0.004867 0.205943 0.142 Uiso 0.549(6) 1 calc R U P A 2 H17D H 0.212873 0.122050 0.220329 0.142 Uiso 0.549(6) 1 calc R U P A 2 C18B C 0.2940(17) 0.1432(5) 0.16208(9) 0.109(5) Uani 0.549(6) 1 d D . P A 2 H18D H 0.200192 0.129988 0.147123 0.164 Uiso 0.549(6) 1 d R U P A 2 H18E H 0.315922 0.228918 0.162113 0.164 Uiso 0.549(6) 1 d R U P A 2 H18F H 0.363382 0.099318 0.147293 0.164 Uiso 0.549(6) 1 d R U P A 2 C19B C 0.6202(14) 0.2320(11) 0.3180(7) 0.092(4) Uani 0.549(6) 1 d D U P A 2 H19C H 0.606977 0.272584 0.289731 0.110 Uiso 0.549(6) 1 calc R U P A 2 H19D H 0.555830 0.270711 0.336612 0.110 Uiso 0.549(6) 1 calc R U P A 2 C20B C 0.7601(17) 0.2540(19) 0.3364(7) 0.137(5) Uani 0.549(6) 1 d D U P A 2 H20D H 0.779480 0.206753 0.362736 0.205 Uiso 0.549(6) 1 calc R U P A 2 H20E H 0.771368 0.339286 0.343176 0.205 Uiso 0.549(6) 1 calc R U P A 2 H20F H 0.825705 0.231008 0.315781 0.205 Uiso 0.549(6) 1 calc R U P A 2 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 Ca1 0.0342(5) 0.0193(4) 0.0659(6) 0.000 0.0088(4) 0.000 P1 0.0324(4) 0.0259(4) 0.0624(6) 0.0006(4) 0.0065(4) 0.0008(3) O1 0.0374(11) 0.0270(11) 0.0809(16) -0.0074(10) 0.0154(11) -0.0031(9) O2 0.0334(11) 0.0375(12) 0.0679(15) 0.0037(11) 0.0068(10) 0.0038(9) O3 0.0375(12) 0.0286(11) 0.0915(18) -0.0128(11) 0.0131(12) -0.0034(9) O4 0.0577(15) 0.0513(15) 0.0670(16) 0.0132(12) 0.0090(12) 0.0016(12) N1 0.0420(14) 0.0255(13) 0.0625(18) 0.0012(12) 0.0105(13) 0.0010(11) C1 0.0503(19) 0.0318(18) 0.065(2) 0.0004(16) 0.0069(16) -0.0011(14) C2 0.054(2) 0.042(2) 0.068(2) -0.0055(17) 0.0029(17) -0.0041(16) C3 0.0481(19) 0.0352(18) 0.078(3) -0.0128(17) 0.0137(18) -0.0075(15) C4 0.0380(17) 0.0259(16) 0.075(2) -0.0067(15) 0.0161(16) -0.0040(13) C5 0.0365(16) 0.0207(15) 0.065(2) -0.0020(13) 0.0161(13) 0.0002(12) C6 0.0445(19) 0.0209(15) 0.109(3) -0.0046(17) 0.0151(18) -0.0018(13) C13A 0.139(4) 0.069(3) 0.060(3) -0.004(2) 0.017(3) -0.014(3) C14A 0.057(7) 0.090(6) 0.067(6) 0.012(5) 0.012(5) -0.015(5) C15A 0.098(8) 0.134(10) 0.082(6) -0.013(6) 0.038(6) -0.006(7) C16A 0.138(8) 0.104(10) 0.096(7) -0.003(7) 0.032(7) -0.022(8) C17A 0.143(6) 0.117(5) 0.089(4) -0.037(4) -0.012(4) -0.032(5) C18A 0.151(19) 0.25(3) 0.077(8) -0.029(11) 0.031(10) -0.012(16) C19A 0.071(10) 0.093(5) 0.075(7) 0.021(5) 0.001(8) -0.004(6) C20A 0.077(9) 0.144(8) 0.178(16) 0.053(9) -0.046(7) -0.042(6) C14B 0.073(6) 0.084(5) 0.055(5) 0.000(4) 0.008(4) -0.015(5) C15B 0.077(5) 0.081(6) 0.074(5) -0.004(4) -0.009(4) -0.003(4) C16B 0.084(6) 0.093(7) 0.063(4) -0.015(4) 0.007(4) -0.001(5) C17B 0.143(6) 0.117(5) 0.089(4) -0.037(4) -0.012(4) -0.032(5) C18B 0.109(11) 0.126(13) 0.084(6) -0.023(7) -0.026(7) 0.038(9) C19B 0.076(11) 0.103(5) 0.092(7) 0.039(5) -0.009(8) -0.027(6) C20B 0.078(9) 0.143(8) 0.177(16) 0.053(9) -0.046(7) -0.043(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 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ca Ca 0.2262 0.3064 '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_ _diffrn_refln_index_h _diffrn_refln_index_k _diffrn_refln_index_l _diffrn_refln_intensity_net _diffrn_refln_intensity_u 0 0 4 1271.54 22.67 0 0 4 1209.03 24.96 0 0 -4 1256.62 25.4 0 0 4 1236.27 21.97 0 0 -4 1238.52 22.11 0 0 -4 1195.98 21 0 0 -4 1239.88 25.72 0 0 -4 1267.23 22.19 0 0 4 1224.27 25.31 0 0 6 4.16 2.14 0 0 -6 5.14 1.94 0 0 -6 5.45 2.39 0 0 6 3 1.86 0 0 6 2.77 1.46 0 0 -6 5.84 2.28 0 0 6 3.82 2.03 0 0 -6 7.15 2.42 0 0 6 4.01 2.17 0 0 -6 6.87 2.98 0 0 8 2366.42 44.72 0 0 8 2274.61 48.94 0 0 -8 2213.24 49.54 0 0 -8 2400.46 43.7 0 0 8 2412.13 44.23 0 0 8 2360.41 41.21 0 0 -8 2400.56 40.62 0 0 -8 2320.15 49.63 0 0 -8 2380.97 43.76 0 0 8 2410.31 51.3 0 0 10 250.26 16.51 0 0 -10 264.1 18.85 0 0 10 235.34 18.81 0 0 -10 256.65 16.73 0 0 10 259.07 16.97 0 0 -10 250.9 15.2 0 0 10 224.2 15.2 0 0 -10 254.28 18.89 0 0 10 258.3 19.39 0 0 -10 253.18 15.92 0 0 12 42.89 7.69 0 0 -12 47.32 7.65 0 0 -12 49.07 9.23 0 0 12 42.78 8.55 0 0 -12 44.48 7.68 0 0 12 46.93 7.42 0 0 -12 40.51 7.03 0 0 12 48.21 8.43 0 0 12 32.18 7.84 0 0 -12 47.35 9.73 0 0 14 499.69 28.14 0 0 14 501.7 31.45 0 0 -14 447.99 30.51 0 0 14 491.96 25.21 0 0 14 504.23 27.67 0 0 -14 506.1 27.21 0 0 -14 512.89 26.78 0 0 -14 488.46 30.88 0 0 14 495.16 30.79 0 0 16 227.47 20.62 0 0 -16 229.01 22.94 0 0 16 228.52 23.97 0 0 16 258.75 21.47 0 0 16 233.69 19.69 0 0 -16 241.32 18.8 0 0 -16 239.49 20.53 0 0 16 240.37 23.75 0 0 -16 259.49 20.14 0 0 -16 239.62 23.8 0 0 18 138.21 17.12 0 0 18 141.25 19.62 0 0 -18 134.85 19.17 0 0 18 125.25 18.31 0 0 -18 139.86 17.21 0 0 18 124.69 15.94 0 0 -18 132.36 15.63 0 0 18 109.12 18.15 0 0 -18 122.65 15.53 0 0 20 41.84 10.57 0 0 -20 57.98 11.24 0 0 -20 47.7 12.65 0 0 20 63.76 14.69 0 0 20 55.99 12.86 0 0 -20 58.56 11.64 0 0 20 63.68 12.58 0 0 -20 46.68 9.9 0 0 20 51.63 11.15 0 0 -20 70.25 14.26 0 0 20 50.17 12.46 0 0 22 58.26 13.37 0 0 22 46.18 13.71 0 0 22 53.2 13.51 0 0 -22 54.47 11.03 0 0 -22 60.91 13.56 0 0 22 76.5 14.69 0 0 -22 80.7 16.5 0 0 22 60.37 14.09 0 0 -24 39.66 10.3 0 0 -24 57.24 15.31 0 0 24 44.63 11.88 0 0 24 50.34 13.55 0 0 -24 30.78 10.03 0 0 24 50.1 13.07 0 0 24 30.3 9.28 0 0 -24 42.17 12.64 0 0 26 74.11 18.46 0 0 26 57.8 15.5 0 0 26 87.24 16.58 0 0 26 102.41 18.97 0 0 -26 78.54 19.24 0 0 28 74.97 19.73 0 0 28 105.62 20.11 0 0 28 82.36 17.57 0 0 -28 103.89 22.25 0 0 30 17.69 9.98 0 0 30 17.94 8.68 0 0 30 26.55 11.82 0 0 -30 12.59 8.54 0 0 32 30.09 12.51 0 0 32 26.72 13.64 0 0 -32 14.19 8.64 0 0 34 -4.64 7.2 0 0 34 3.04 7.57 0 0 34 -15.28 9.92 0 0 -34 7.98 10.37 0 0 36 -7.24 10.68 0 0 36 0.11 6.5 0 0 36 6.19 7.3 0 0 -36 -17.48 15.59 0 0 38 -0.72 6.6 0 0 38 -1.72 8.58 0 0 38 -6.03 6.27 0 0 -38 -14 13.1 0 0 40 -11.53 12.74 0 0 40 -7.89 9.29 0 0 42 14.57 14.58 0 0 42 -1.98 7.59 0 0 42 25.52 17.31 0 0 -42 7.7 15.08 0 0 44 -3.57 9.07 0 1 -1 693.26 17.83 0 1 1 761.64 20.06 0 -1 1 698.89 18.04 0 1 -1 702.3 21.15 0 -1 -1 699.08 20.9 0 1 1 696.25 18.85 0 1 -1 716.61 18.44 0 1 -1 700.4 18.08 0 -1 1 679.81 17.71 0 -1 -1 690.58 17.06 0 -1 -1 708.23 18.14 0 1 1 683.46 16.99 0 -1 -3 153.24 9.89 0 1 -3 137.78 8.51 0 1 3 143.14 9.81 0 1 -3 139.88 9.91 0 -1 3 143.07 10.13 0 -1 -3 145.17 10.08 0 1 3 141.98 9.66 0 1 3 149.62 8.42 0 -1 3 141.42 8.8 0 -1 3 144.2 8.88 0 -1 -3 144.34 8.78 0 1 -3 134.32 8.22 0 1 -3 154.24 8.89 0 -1 -3 146.32 8.82 0 1 3 140.49 8.66 0 1 3 145.52 8.31 0 -1 -3 139.54 8.38 0 1 5 464.17 20.14 0 -1 -5 456.29 19.6 0 -1 5 444.87 19.98 0 -1 -5 444.91 19.37 0 1 5 453.93 19.15 0 1 -5 439.35 19.33 0 -1 5 435.84 17.57 0 1 -5 438.91 16.51 0 -1 -5 454.59 17.25 0 -1 5 457.21 17.63 0 1 5 460.92 16.7 0 1 -5 445.99 16.3 0 -1 5 466.16 18.82 0 1 5 460.02 17.01 0 1 -5 431.65 18.59 0 1 5 461.48 18.85 0 -1 -5 447.67 17.06 0 -1 -5 434.95 17.99 0 1 7 200.14 14.97 0 -1 -7 202.41 14.88 0 1 -7 206.3 11.85 0 -1 7 210.33 15.59 0 1 -7 197.63 15.21 0 -1 -7 201.98 14.89 0 1 7 204.81 14.49 0 -1 -7 205.25 13.1 0 -1 7 209.37 13.14 0 1 -7 205.26 12.15 0 1 7 202.57 12.48 0 1 -7 205.33 12.77 0 -1 7 199.38 13.2 0 -1 -7 197.66 13.12 0 1 7 207 14.39 0 1 7 211.65 13.28 0 -1 7 203.88 14.41 0 -1 -7 212.68 14.45 0 1 -7 197.27 14.47 0 1 9 181.86 16.11 0 1 -9 191.33 12.86 0 -1 -9 183.64 15.88 0 -1 9 172.19 15.71 0 1 9 182.2 15.06 0 1 -9 168.13 15.34 0 1 -9 181.42 12.71 0 1 9 170.69 13.32 0 -1 9 179.19 13.57 0 -1 -9 179.84 13.91 0 -1 9 190.64 14.58 0 1 9 170.59 11.81 0 1 -9 176.16 13.2 0 1 -9 185.46 15.76 0 -1 9 181.43 15.3 0 1 9 182.07 15.41 0 1 9 186.64 13.79 0 -1 -9 179.28 13.83 0 -1 -9 153.99 14.57 0 -1 -11 21.67 5.34 0 1 -11 21.55 4.75 0 1 11 16.5 4.47 0 -1 11 23.56 7.06 0 1 11 17.28 5.68 0 1 11 18.89 6.09 0 1 -11 21.79 4.97 0 -1 11 16.08 4.52 0 1 11 15.14 4.56 0 1 11 16.37 4.33 0 1 -11 21.45 5.54 0 -1 11 15.97 5.02 0 -1 -11 15.57 5.39 0 -1 11 15.09 5.69 0 1 -11 18.7 5.81 0 1 11 21.45 6.07 0 1 -13 6.69 3.28 0 -1 -13 7.01 3.85 0 1 13 2.76 2.32 0 1 -13 3.31 3.68 0 -1 -13 6.6 4.01 0 1 13 7.33 4.26 0 1 13 7.02 4.2 0 -1 13 5.35 3.63 0 1 -13 6.53 3.76 0 -1 13 4.03 3.35 0 -1 -13 4.67 2.72 0 1 -13 1.49 1.48 0 1 13 7.11 3.41 0 -1 13 7.14 3.52 0 1 13 4.32 2.55 0 1 -13 8.14 3.66 0 -1 13 5.3 3 0 -1 -13 6.16 3.93 0 1 13 6.16 3.58 0 1 15 571.2 31.83 0 1 15 526.28 34.21 0 1 15 542.61 34.05 0 -1 -15 561.65 35.2 0 1 -15 559.94 35.29 0 -1 15 546.08 36.05 0 -1 15 594.3 32.97 0 -1 -15 584.57 31.79 0 1 -15 614.3 29.26 0 1 15 585.39 28.19 0 -1 15 593.83 31.25 0 1 15 583.25 30.62 0 1 -15 593.06 30.66 0 -1 15 576.27 35.14 0 1 -15 582.35 35.85 0 1 15 584.18 35.89 0 -1 -15 609.71 35.73 0 -1 -15 568.88 30.22 0 1 -15 591.9 29.04 0 1 17 296.52 27.45 0 1 17 308.14 25.06 0 -1 17 283.53 27.93 0 1 -17 283.29 27.79 0 -1 -17 297.72 27.17 0 1 17 303.16 27.12 0 1 -17 313.05 24.2 0 -1 17 321.94 26.23 0 1 17 299.76 21.96 0 1 17 324.69 24.58 0 1 -17 322.82 23.22 0 -1 17 296.44 24.22 0 -1 -17 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8.06 13 0 -9 -13.48 8.5 13 0 -9 6.92 12.03 13 0 -9 -12.65 15.3 13 0 -7 0.14 12.2 13 0 -7 -27.93 11.95 13 0 -7 18.02 11.25 13 0 -7 -14.05 18.63 13 0 -5 7.79 14.89 13 0 -5 19.45 15.71 13 0 -5 -18.5 10.47 13 0 -5 -4.44 6.67 13 0 -5 29.8 21.43 13 0 -3 -13.92 11.74 13 0 -3 -12.65 10.57 13 0 -3 3.03 11.98 13 0 -1 -2.78 11.65 13 0 -1 -13.41 12.23 13 0 -1 -7.05 6.94 13 0 -1 9.62 15.01 13 0 1 15.75 15.92 13 0 1 -4.15 8.81 13 0 1 12.28 9.6 13 0 1 -4.88 5.54 13 0 1 1.38 13.67 13 0 3 -9.92 15.37 13 0 3 3.46 7.51 13 0 3 -0.68 5.36 13 0 3 -3.36 8.7 13 0 3 -18 17.28 13 0 5 -0.16 9.07 13 0 5 9.21 7.07 13 0 5 -4.08 7.45 13 0 5 2.24 12.64 13 0 7 -16.73 10.46 13 0 7 -2.96 10.36 13 0 9 4.89 13.4 13 0 9 12.31 10.25 13 0 9 5.96 8.72 13 0 9 20.27 16.32 13 0 11 23.64 18.98 13 0 11 14.17 10.27 13 0 11 -0.96 8.64 13 0 13 -20.71 15.35 13 0 15 14.87 9.92 13 0 15 11.93 12.46 13 -1 -24 -17.27 15.5 13 -1 -22 -13.22 19.9 13 1 -22 -12 10.18 13 1 -20 8.46 17.82 13 1 -20 -6.95 8.13 13 -1 -20 -35.9 26.35 13 -1 -18 25.19 22.55 13 1 -18 -0.18 14.62 13 -1 -18 7.04 15.39 13 1 -18 13.96 14.25 13 1 -16 6.9 10.35 13 -1 -16 15.68 17.49 13 -1 -16 16.64 15.26 13 1 -16 -5.27 10.2 13 1 -14 23.95 15.77 13 1 -14 14.15 17.52 13 -1 -14 28.46 14.06 13 -1 -14 19.69 20.24 13 1 -14 17.64 14.02 13 -1 -12 31.5 16.13 13 1 -12 20.94 13.24 13 -1 -12 -1.93 14.86 13 -1 -12 -2.28 14.12 13 1 -12 31.22 16.12 13 1 -12 9.98 15.16 13 1 -10 34.32 15.73 13 -1 -10 24.41 17.94 13 -1 -10 -8.51 12.08 13 1 -10 22.44 14.42 13 1 -10 7.12 11.6 13 1 -8 9.41 8.08 13 -1 -8 6.58 16.11 13 1 -8 2.03 10.66 13 -1 -8 -5.46 11.29 13 1 -8 10.71 5.88 13 1 -8 30.45 13.19 13 -1 -8 12.26 17 13 1 -8 23.33 17.14 13 1 -6 1.03 8.86 13 -1 -6 11.58 13.64 13 1 -6 10.37 12.06 13 -1 -6 0.06 6.01 13 1 -6 -2.52 4.58 13 1 -6 -11.83 9.83 13 -1 -6 -9.37 7.56 13 -1 -6 9.6 11.75 13 1 -6 2.88 10.29 13 1 -4 -4.35 10.25 13 -1 -4 -0.87 8.97 13 -1 -4 1.38 10.03 13 1 -4 1.85 12.05 13 1 -4 -1.04 6.23 13 1 -4 7.38 13.01 13 -1 -4 14 9.82 13 -1 -4 -9.13 7.62 13 -1 -4 -14.33 20 13 1 -4 31 20.08 13 1 -2 -17.66 16.6 13 -1 -2 -15.64 17.13 13 1 -2 9.37 11.75 13 -1 -2 -11.45 12.07 13 1 -2 -6.28 7.81 13 -1 -2 0.67 6.93 13 1 -2 -10.06 6.98 13 -1 -2 -3.82 5.2 13 -1 -2 28.3 22.19 13 1 -2 -1.69 10.77 13 1 0 41.54 20.03 13 -1 0 9.9 15.45 13 1 0 -16.92 14.61 13 -1 0 -5.4 8.55 13 1 0 -1.06 6.75 13 -1 0 -5.41 9.76 13 1 0 7.38 10.12 13 -1 0 26.31 11.76 13 -1 0 14.4 22.29 13 1 0 -1.44 10.78 13 1 2 -22.43 16.33 13 -1 2 23.69 20.16 13 1 2 14.51 13.37 13 -1 2 -5.25 6.79 13 1 2 -7.52 7.1 13 -1 2 -4.21 8.35 13 1 2 1.71 6.46 13 -1 2 -23.85 16.74 13 1 2 11.01 13.73 13 -1 4 -0.34 12.89 13 1 4 -14.49 13.13 13 1 4 2.66 6.55 13 -1 4 14.81 10.58 13 1 4 22.67 11.07 13 -1 4 3.46 16.09 13 1 4 -19.85 17.88 13 1 6 4.27 10.52 13 -1 6 4.46 8.19 13 1 6 1.73 7.97 13 -1 6 4.6 8.04 13 1 6 22.62 12.1 13 -1 6 37.43 18.84 13 1 6 -6.26 10.1 13 -1 8 2.31 9.81 13 -1 8 4.2 9.47 13 1 8 2.21 6.74 13 1 8 -14.17 11.2 13 1 8 0.25 12.44 13 1 10 -12.25 15.31 13 -1 10 -12.4 14.12 13 1 10 11.55 9.51 13 -1 10 8.12 8.79 13 1 10 2.73 7.26 13 -1 10 10.08 12.61 13 -1 10 -2.06 10.08 13 1 10 20.4 17.38 13 -1 12 18.82 9.2 13 -1 12 -5.15 11.89 13 1 12 -16.23 16.24 13 1 14 32.31 17.23 13 -1 14 -18.74 13.86 13 -1 16 -11.12 13.08 13 1 16 13.19 13.45 13 2 -21 45.5 24.61 13 -2 -21 -12.84 22 13 -2 -21 0.99 15.95 13 2 -19 12.47 11.38 13 -2 -19 -6.83 13.08 13 2 -17 14.34 11.32 13 2 -17 -4.57 17.08 13 2 -15 10.11 12.78 13 -2 -15 10.79 15.57 13 2 -15 28.1 20.57 13 2 -13 36.86 17.72 13 -2 -13 20.01 14.31 13 -2 -13 -12.91 14.58 13 -2 -11 29.66 16.96 13 2 -11 38.38 18.49 13 -2 -11 -7.48 13.58 13 -2 -11 -17.17 13.01 13 2 -11 -0.25 12.34 13 2 -11 36.85 21.94 13 -2 -9 -1.47 9.78 13 2 -9 17.14 7.9 13 2 -9 17.7 11.58 13 -2 -9 7.74 12.29 13 -2 -9 22.66 14.08 13 2 -9 1.83 8.57 13 2 -7 13.51 11.1 13 -2 -7 25.46 18.78 13 2 -7 12.03 18.48 13 -2 -7 -7.58 12.79 13 2 -7 1.23 7.53 13 2 -7 -3.3 5.94 13 -2 -7 1.65 16.37 13 2 -7 -14.33 11.77 13 2 -5 -19.49 12.96 13 -2 -5 -5.45 12.33 13 -2 -5 -1.88 10.06 13 2 -5 -31.31 21.89 13 -2 -5 -8.77 7.34 13 2 -5 18.02 11.33 13 2 -5 11.45 7.17 13 -2 -5 -4.35 15.98 13 2 -5 -11.19 13.55 13 -2 -3 -36.87 21.61 13 2 -3 6.32 14.26 13 2 -3 -20.76 12.11 13 2 -3 6.86 7.32 13 -2 -3 37.35 22.97 13 2 -3 6.7 11.68 13 2 -1 12.58 14.9 13 -2 -1 2.49 11.52 13 2 -1 -2.82 9.82 13 -2 -1 3.65 8.6 13 2 -1 10.65 12.66 13 2 -1 -2.03 7.28 13 -2 -1 5.07 16.57 13 -2 1 -4.84 11.93 13 2 1 9.09 14.36 13 2 1 4.87 11.79 13 -2 1 26.85 11.87 13 2 1 0.38 7.66 13 2 1 5.51 6.88 13 -2 1 -16.32 12.19 13 -2 3 16.36 17.11 13 2 3 -10.44 13.04 13 2 3 12.28 12.4 13 2 3 20.61 11.71 13 2 3 8.98 7.85 13 -2 3 6.64 6.36 13 -2 3 -2.28 15.53 13 2 3 48.53 28.38 13 -2 5 32.73 23.97 13 2 5 10.18 12.28 13 2 5 36.16 18.18 13 -2 5 25.93 17.31 13 2 5 -1.32 9.48 13 2 5 3.58 5.7 13 2 5 9.97 11.05 13 -2 7 -3.55 14.31 13 2 7 13.78 12.95 13 2 7 3.58 8.64 13 -2 7 28.23 15.13 13 2 7 13.1 9.1 13 2 7 23.51 16.43 13 -2 7 3.38 11.68 13 2 7 -9.65 14.94 13 -2 9 16.6 17.38 13 2 9 -3.65 8.65 13 -2 9 18.15 12.38 13 2 9 11 10.06 13 -2 9 -4.03 10.16 13 2 9 -11.75 13.83 13 2 11 3.58 12.09 13 -2 11 21.42 11.6 13 2 11 -14.52 13.21 13 -2 11 4.42 13.27 13 2 11 -3.63 11.35 13 2 13 10.33 11.41 13 2 13 -20.89 17.45 13 3 -24 -5.2 15.08 13 3 -20 50.85 23.74 13 3 -18 -9.54 12.77 13 -3 -18 -7.8 17.59 13 -3 -18 -35.49 25.53 13 3 -16 6.79 11.49 13 -3 -16 32.04 22.57 13 -3 -16 -6.47 14.31 13 3 -16 28.4 21.87 13 -3 -14 -15.21 16.42 13 3 -14 -32.37 21.91 13 -3 -14 27.76 18.97 13 3 -14 -17.61 19.36 13 -3 -14 -8.16 20.26 13 -3 -12 20.4 15.06 13 3 -12 -0.39 10.03 13 -3 -12 -15.24 17.88 13 -3 -12 -23.46 18.77 13 3 -12 36.46 24.45 13 -3 -10 15.14 14.3 13 3 -10 10.99 10.97 13 3 -8 15.15 15.68 13 -3 -8 -5.7 11.25 13 3 -8 -0.25 10.64 13 3 -6 -2.59 12.43 13 -3 -6 -1.43 11.3 13 3 -6 3.24 5.57 13 3 -6 2.99 9.08 13 3 -4 -9.31 11.57 13 -3 -4 -8.64 15.81 13 3 -4 17.42 19.62 13 -3 -4 -12.29 10.61 13 3 -4 8.85 8.05 13 3 -4 12.23 10.93 13 3 -2 9.4 11.78 13 -3 -2 -3.45 16.9 13 3 -2 26.31 16.44 13 3 -2 17.03 9.58 13 3 -2 26.2 14.1 13 -3 -2 -22.63 14.11 13 3 0 -10.72 13.25 13 3 0 -7.03 10.41 13 -3 0 8.32 8.25 13 3 0 6.08 6.41 13 3 0 -5.89 10.41 13 3 2 39.65 18.53 13 3 2 27.31 17.19 13 -3 2 24.24 14.06 13 3 2 9.52 7.81 13 3 2 14.45 9.97 13 -3 2 18.85 14.21 13 -3 4 1.71 14.13 13 3 4 -2.52 12.69 13 3 4 17.62 15.25 13 -3 4 25.67 14.02 13 3 4 28.75 14.13 13 -3 4 -11.91 17.65 13 -3 6 8.58 16.32 13 3 6 -3.4 9.15 13 3 6 4.83 9.18 13 -3 6 4.57 11.46 13 3 6 -3.34 6.44 13 3 8 -9.64 8.88 13 -3 8 -7.1 14.28 13 3 8 -5.88 9.14 13 3 8 -18.1 12.78 13 -3 8 6.08 10.78 13 3 10 -12.83 13.45 13 3 10 42.33 18.58 13 -3 10 7.89 10.14 13 3 10 29.86 15.6 13 4 -23 -3.01 16.89 13 4 -21 34.08 29.56 13 4 -19 23.41 22.11 13 -4 -17 -42.55 26.21 13 -4 -15 20.5 16.57 13 -4 -15 4.81 13.15 13 -4 -13 27.36 18.99 13 4 -13 -1.56 20.22 13 4 -13 -14.42 19.31 13 -4 -13 -27.01 22.69 13 4 -11 -23.01 22.29 13 -4 -11 -26.39 20.19 13 4 -11 28.98 22.22 13 -4 -11 14.02 12.72 13 4 -9 27.67 19.99 13 -4 -9 -16.54 16.93 13 4 -9 17.19 9.24 13 4 -9 0.15 11.53 13 -4 -9 -24.38 16.75 13 4 -7 6.87 7.62 13 4 -7 -14.89 15.21 13 -4 -7 -14.79 14.63 13 -4 -5 20.29 17.92 13 4 -5 24.95 10.78 13 4 -5 35.74 18.63 13 -4 -5 13.24 16.17 13 -4 -3 29.37 19.68 13 4 -3 34.2 23.38 13 4 -3 33.16 14.07 13 4 -3 62.17 24.28 13 -4 -3 27.69 24.3 13 4 -1 20.24 11.8 13 4 -1 14.5 10.71 13 4 -1 23.9 13.29 13 -4 -1 18.78 12.14 13 -4 -1 19.55 22.3 13 -4 1 -53.07 29.63 13 4 1 -23.55 19.37 13 4 1 16.72 14.31 13 -4 1 -23.64 15.37 13 4 1 10.74 7.02 13 -4 1 -42.82 20.13 13 -4 3 -10.63 17.63 13 4 3 -32.09 21.38 13 4 3 4.38 7.83 13 -4 3 -21.75 13.47 13 4 3 -12.29 12.31 13 -4 3 8.37 11.48 13 -4 5 -14.79 18.26 13 4 5 -19.73 17.45 13 4 5 12.92 13.62 13 4 5 7.08 9.78 13 4 5 -10.83 8.67 13 -4 5 -12.07 10.26 13 4 7 -16.04 13.46 13 4 7 9.14 15.63 13 4 7 12.42 10.7 13 4 7 36.32 18.59 13 4 9 14.48 12.42 13 4 9 51.45 18.31 13 -4 9 14.14 13.49 13 4 11 21.05 15.53 13 4 11 20.29 14.68 13 -5 -16 21.51 17.26 13 5 -16 44.72 27.59 13 -5 -14 37.24 24.21 13 5 -14 35.15 28.92 13 -5 -12 23.11 21.32 13 5 -12 -29.82 22.59 13 -5 -10 -13.17 17 13 5 -10 11.33 10.04 13 5 -10 4.71 13.61 13 5 -8 7.36 15.53 13 5 -8 10.65 9.33 13 5 -8 -3.41 11.13 13 5 -6 12.94 10.38 13 5 -6 12.72 16.44 13 5 -4 16.16 21.45 13 -5 -4 46.84 23.85 13 5 -4 18.27 11.24 13 5 -4 19.75 20.4 13 -5 -2 16.56 20.75 13 5 -2 43.2 24.02 13 5 -2 16.9 10.97 13 5 -2 17.99 16.4 13 -5 0 -8.94 14.38 13 5 0 -13.1 20.15 13 5 0 -29.62 19.05 13 -5 0 -30.61 16.5 13 5 2 21.58 19.82 13 5 2 8.81 10.1 13 -5 2 -4.78 10.44 13 5 2 15.55 10.03 13 5 2 14.66 12.87 13 5 4 27.09 23.15 13 5 4 13.19 11.12 13 -5 4 1.65 11.59 13 5 4 16.74 12.29 13 5 6 28.29 16.28 13 5 6 1.79 11.2 13 5 8 24.58 15.03 13 5 8 48.69 24.21 13 -5 8 12.18 14.42 13 5 10 24.78 16.5 13 5 10 -22.04 19.43 13 5 12 14.87 17.02 13 -6 -17 -22.17 19.23 13 -6 -15 -6.83 17.95 13 -6 -13 -5 15.56 13 -6 -11 21.29 21.24 13 -6 -9 -31.6 25.32 13 6 -9 -10.77 8.14 13 -6 -7 -14.45 16.15 13 6 -7 -0.37 5.76 13 -6 -5 44.69 23.71 13 6 -5 21.04 11.29 13 6 -1 -7.6 9.43 13 6 1 10.79 8.73 13 -6 1 21.21 16.91 13 -6 3 -0.74 10.97 13 -6 7 1.95 17.93 13 6 9 19.85 14.25 13 7 -6 -0.33 7.34 13 7 -4 -4.34 6.74 13 7 -2 -7.05 7.44 13 -7 6 27.91 22.07 14 0 -16 19.5 18.28 14 0 -14 -11.15 20.05 14 0 -14 -11.68 16.2 14 0 -12 9.21 16.29 14 0 -12 4.26 17.09 14 0 -10 -39.81 24.23 14 0 -10 6.05 15.32 14 0 -8 42.06 26.66 14 0 -8 20.76 21.95 14 0 -6 -9.21 18.3 14 0 -4 -38.76 20.56 14 0 -4 -40.71 25.09 14 0 -2 -28.71 19.33 14 0 -2 -46.87 27.24 14 0 0 29.96 22.95 14 0 0 27 13.95 14 0 0 11.81 20 14 0 2 6.12 12.06 14 0 2 39.36 27.38 14 0 4 -1.88 13.11 14 0 4 -12.76 9.63 14 0 6 1.22 9.11 14 0 6 7.14 14.77 14 0 8 -31.47 19.8 14 -1 -19 -5.33 14.34 14 -1 -17 12.24 19.13 14 -1 -17 26.93 18.08 14 1 -15 -7.41 18.85 14 -1 -15 -46.5 25.13 14 -1 -13 2.58 15.85 14 -1 -13 36.27 25.99 14 1 -13 14.41 17.98 14 1 -9 91.41 32.61 14 1 -7 -4.31 18.04 14 -1 -5 32.07 23.77 14 1 -5 15.46 15.9 14 -1 -3 -4.27 11.66 14 1 -1 23.82 19.37 14 1 -1 14.52 11.83 14 1 1 18.12 18.52 14 -1 1 -9.98 15.77 14 1 1 6.08 8.51 14 -1 1 56.74 20.89 14 1 1 17.23 14.36 14 -1 1 30.55 27.19 14 -1 3 16.44 16.2 14 1 3 18.88 13.11 14 1 3 15.71 12.63 14 -1 3 -13.43 16.76 14 1 5 -30.48 19.63 14 1 5 29.33 15.13 14 -1 5 14.38 16.06 14 -1 5 -18.16 20.56 14 1 7 4.6 10.56 14 1 9 7.68 14.07 14 -2 -14 13.45 20.45 14 2 -12 -21.85 22.16 14 -2 -12 -19.78 24.48 14 2 -10 48.19 27.57 14 -2 -10 -43.13 27.94 14 2 -8 35.04 15.33 14 -2 -8 -7.37 16.68 14 -2 -6 5.17 13.56 14 2 -6 5.07 9.66 14 -2 -4 -0.33 11.99 14 2 -4 26.57 20.32 14 2 -4 50.43 18.87 14 -2 -4 -18.66 16.64 14 2 -2 -2.2 12.34 14 2 -2 10.19 10.17 14 2 -2 -4.19 10.54 14 -2 -2 7.15 18.56 14 2 0 -1.48 8.94 14 2 0 31.17 15.99 14 -2 0 51.56 33.27 14 2 2 -26.84 19.12 14 -2 2 8.53 16.46 14 2 2 -6.02 8.58 14 -2 2 -1.43 9.18 14 2 4 -21.59 18.35 14 2 4 -10.63 7.04 14 2 6 -15.61 18.09 14 -2 6 -31.81 16.53 14 2 6 19.97 16.17 14 3 -9 33.26 25.38 14 3 -7 -28.41 25.23 14 -3 -7 8.36 14.72 14 3 -5 -19.19 14.3 14 -3 -3 -28.5 21.36 14 3 -3 29.04 23.48 14 3 -3 -1.29 10.3 14 -3 -1 29.06 20.53 14 3 -1 26.72 14.46 14 3 1 39.68 16.35 14 3 1 6.39 7.04 14 3 3 -23.74 12.49 14 3 3 -4.98 9.48 14 3 5 26.51 18.73 14 -3 5 -28.08 15.87 14 4 -14 -20.65 22.17 14 4 -12 11.2 13.75 14 4 -10 -5.69 19.42 14 -4 -8 -9.35 17.46 14 4 -8 30.36 19.46 14 -4 -6 28.24 23.15 14 4 -6 11.61 14.65 14 -4 -4 -17.02 18.26 14 4 -4 -10.74 15.97 14 4 -2 -42.84 23 14 4 0 34.64 23.76 14 4 0 3.16 7.93 14 4 2 8.04 14.48 14 5 -3 43.96 16.12 14 5 -1 31.35 16.2 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 Ca1 O1 170.95(10) . 2_556 y O1 Ca1 O2 90.38(8) 2_556 6 y O1 Ca1 O2 83.97(7) 2_556 5_656 y O1 Ca1 O2 83.97(7) . 6 y O1 Ca1 O2 90.38(7) . 5_656 y O1 Ca1 N1 99.46(8) 2_556 . y O1 Ca1 N1 88.19(8) 2_556 2_556 y O1 Ca1 N1 99.46(8) . 2_556 y O1 Ca1 N1 88.19(8) . . y O2 Ca1 O2 102.76(11) 6 5_656 y O2 Ca1 N1 96.72(8) 5_656 . y O2 Ca1 N1 159.00(8) 5_656 2_556 y O2 Ca1 N1 96.73(8) 6 2_556 y O2 Ca1 N1 159.00(8) 6 . y N1 Ca1 N1 65.36(12) . 2_556 y O1 P1 Ca1 27.10(8) . . ? O1 P1 O2 118.53(13) . . ? O1 P1 O3 110.03(12) . . ? O1 P1 O4 105.77(13) . . ? O2 P1 Ca1 126.18(9) . . ? O2 P1 O3 107.71(12) . . ? O2 P1 O4 108.17(12) . . ? O3 P1 Ca1 83.31(8) . . ? O3 P1 O4 105.94(14) . . ? O4 P1 Ca1 119.20(9) . . ? P1 O1 Ca1 135.71(12) . . ? P1 O2 Ca1 140.98(12) . 5_656 ? P1 O3 H3 109.5 . . ? C13A O4 P1 120.2(2) . . ? C1 N1 Ca1 123.70(19) . . ? C1 N1 C5 117.2(3) . . ? C5 N1 Ca1 119.1(2) . . ? N1 C1 H1 118.1 . . ? N1 C1 C2 123.9(3) . . ? C2 C1 H1 118.1 . . ? C1 C2 H2 120.5 . . ? C3 C2 C1 119.0(3) . . ? C3 C2 H2 120.5 . . ? C2 C3 H3A 120.2 . . ? C2 C3 C4 119.7(3) . . ? C4 C3 H3A 120.2 . . ? C3 C4 C5 117.7(3) . . ? C3 C4 C6 122.9(3) . . ? C5 C4 C6 119.4(3) . . ? N1 C5 C4 122.6(3) . . ? N1 C5 C5 118.24(17) . 2_556 ? C4 C5 C5 119.20(18) . 2_556 ? C4 C6 H6 119.3 . . ? C6 C6 C4 121.38(18) 2_556 . ? C6 C6 H6 119.3 2_556 . ? O4 C13A H13A 112.0 . . ? O4 C13A H13B 112.0 . . ? O4 C13A H13C 108.4 . . ? O4 C13A H13D 108.4 . . ? O4 C13A C14A 98.9(3) . . ? O4 C13A C14B 115.5(4) . . ? H13A C13A H13B 109.7 . . ? H13C C13A H13D 107.5 . . ? C14A C13A H13A 112.0 . . ? C14A C13A H13B 112.0 . . ? C14B C13A H13C 108.4 . . ? C14B C13A H13D 108.4 . . ? C13A C14A H14A 111.1 . . ? C15A C14A C13A 101.8(3) . . ? C15A C14A H14A 111.1 . . ? C15A C14A C19A 114.0(10) . . ? C19A C14A C13A 107.2(9) . . ? C19A C14A H14A 111.1 . . ? C14A C15A H15A 107.8 . . ? C14A C15A H15B 107.8 . . ? C14A C15A C16A 117.8(3) . . ? H15A C15A H15B 107.2 . . ? C16A C15A H15A 107.8 . . ? C16A C15A H15B 107.8 . . ? C15A C16A H16A 107.8 . . ? C15A C16A H16B 107.8 . . ? H16A C16A H16B 107.1 . . ? C17A C16A C15A 118.0(3) . . ? C17A C16A H16A 107.8 . . ? C17A C16A H16B 107.8 . . ? C16A C17A H17A 110.2 . . ? C16A C17A H17B 110.2 . . ? H17A C17A H17B 108.5 . . ? C18A C17A C16A 107.6(9) . . ? C18A C17A H17A 110.2 . . ? C18A C17A H17B 110.2 . . ? C17A C18A H18A 108.8 . . ? C17A C18A H18B 106.6 . . ? C17A C18A H18C 113.0 . . ? H18A C18A H18B 109.5 . . ? H18A C18A H18C 109.5 . . ? H18B C18A H18C 109.5 . . ? C14A C19A H19A 108.3 . . ? C14A C19A H19B 108.3 . . ? H19A C19A H19B 107.4 . . ? C20A C19A C14A 116.1(13) . . ? C20A C19A H19A 108.3 . . ? C20A C19A H19B 108.3 . . ? C19A C20A H20A 109.5 . . ? C19A C20A H20B 109.5 . . ? C19A C20A H20C 109.5 . . ? H20A C20A H20B 109.5 . . ? H20A C20A H20C 109.5 . . ? H20B C20A H20C 109.5 . . ? C13A C14B H14B 106.7 . . ? C13A C14B C15B 108.2(4) . . ? C13A C14B C19B 113.6(9) . . ? C15B C14B H14B 106.7 . . ? C15B C14B C19B 114.5(7) . . ? C19B C14B H14B 106.7 . . ? C14B C15B H15C 108.0 . . ? C14B C15B H15D 108.0 . . ? H15C C15B H15D 107.2 . . ? C16B C15B C14B 117.2(3) . . ? C16B C15B H15C 108.0 . . ? C16B C15B H15D 108.0 . . ? C15B C16B H16C 108.4 . . ? C15B C16B H16D 108.4 . . ? C15B C16B C17B 115.4(3) . . ? H16C C16B H16D 107.5 . . ? C17B C16B H16C 108.4 . . ? C17B C16B H16D 108.4 . . ? C16B C17B H17C 108.8 . . ? C16B C17B H17D 108.8 . . ? H17C C17B H17D 107.7 . . ? C18B C17B C16B 113.7(6) . . ? C18B C17B H17C 108.8 . . ? C18B C17B H17D 108.8 . . ? C17B C18B H18D 108.4 . . ? C17B C18B H18E 111.9 . . ? C17B C18B H18F 108.1 . . ? H18D C18B H18E 109.5 . . ? H18D C18B H18F 109.5 . . ? H18E C18B H18F 109.5 . . ? C14B C19B H19C 107.9 . . ? C14B C19B H19D 107.9 . . ? H19C C19B H19D 107.2 . . ? C20B C19B C14B 117.7(11) . . ? C20B C19B H19C 107.9 . . ? C20B C19B H19D 107.9 . . ? C19B C20B H20D 109.5 . . ? C19B C20B H20E 109.5 . . ? C19B C20B H20F 109.5 . . ? H20D C20B H20E 109.5 . . ? H20D C20B H20F 109.5 . . ? H20E C20B H20F 109.5 . . ? 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 Ca1 O1 2.288(2) . y Ca1 O1 2.288(2) 2_556 y Ca1 O2 2.363(2) 6 y Ca1 O2 2.363(2) 5_656 y Ca1 N1 2.531(3) . y Ca1 N1 2.531(3) 2_556 y P1 O1 1.485(2) . ? P1 O2 1.499(2) . ? P1 O3 1.577(2) . ? P1 O4 1.589(2) . ? O3 H3 0.8300 . ? O4 C13A 1.434(5) . ? N1 C1 1.327(4) . ? N1 C5 1.366(4) . ? C1 H1 0.9400 . ? C1 C2 1.403(4) . ? C2 H2 0.9400 . ? C2 C3 1.355(5) . ? C3 H3A 0.9400 . ? C3 C4 1.407(5) . ? C4 C5 1.409(4) . ? C4 C6 1.438(4) . ? C5 C5 1.441(6) 2_556 ? C6 C6 1.318(7) 2_556 ? C6 H6 0.9400 . ? C13A H13A 0.9800 . ? C13A H13B 0.9800 . ? C13A H13C 0.9800 . ? C13A H13D 0.9800 . ? C13A C14A 1.645(6) . ? C13A C14B 1.499(7) . ? C14A H14A 0.9900 . ? C14A C15A 1.5077(16) . ? C14A C19A 1.552(13) . ? C15A H15A 0.9800 . ? C15A H15B 0.9800 . ? C15A C16A 1.5077(16) . ? C16A H16A 0.9800 . ? C16A H16B 0.9800 . ? C16A C17A 1.5077(16) . ? C17A H17A 0.9800 . ? C17A H17B 0.9800 . ? C17A C18A 1.5077(16) . ? C18A H18A 0.9699 . ? C18A H18B 0.9699 . ? C18A H18C 0.9699 . ? C19A H19A 0.9800 . ? C19A H19B 0.9800 . ? C19A C20A 1.442(14) . ? C20A H20A 0.9700 . ? C20A H20B 0.9700 . ? C20A H20C 0.9700 . ? C14B H14B 0.9900 . ? C14B C15B 1.5077(16) . ? C14B C19B 1.568(11) . ? C15B H15C 0.9800 . ? C15B H15D 0.9800 . ? C15B C16B 1.5077(16) . ? C16B H16C 0.9800 . ? C16B H16D 0.9800 . ? C16B C17B 1.5077(16) . ? C17B H17C 0.9800 . ? C17B H17D 0.9800 . ? C17B C18B 1.5077(16) . ? C18B H18D 0.9700 . ? C18B H18E 0.9701 . ? C18B H18F 0.9701 . ? C19B H19C 0.9800 . ? C19B H19D 0.9800 . ? C19B C20B 1.408(11) . ? C20B H20D 0.9700 . ? C20B H20E 0.9700 . ? C20B H20F 0.9700 . ? 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Ca1 P1 O2 Ca1 43.4(2) . . . 5_656 ? Ca1 P1 O4 C13A -158.6(3) . . . . ? Ca1 N1 C1 C2 177.3(2) . . . . ? Ca1 N1 C5 C4 -178.5(2) . . . . ? Ca1 N1 C5 C5 1.0(4) . . . 2_556 ? P1 O4 C13A C14A 162.2(3) . . . . ? P1 O4 C13A C14B -176.1(3) . . . . ? O1 P1 O2 Ca1 74.4(2) . . . 5_656 ? O1 P1 O4 C13A 175.8(3) . . . . ? O2 P1 O1 Ca1 -114.39(19) . . . . ? O2 P1 O4 C13A 47.9(3) . . . . ? O3 P1 O1 Ca1 10.1(2) . . . . ? O3 P1 O2 Ca1 -51.3(2) . . . 5_656 ? O3 P1 O4 C13A -67.4(3) . . . . ? O4 P1 O1 Ca1 124.13(18) . . . . ? O4 P1 O2 Ca1 -165.37(18) . . . 5_656 ? O4 C13A C14A C15A -171.7(4) . . . . ? O4 C13A C14A C19A 68.4(9) . . . . ? O4 C13A C14B C15B -87.4(6) . . . . ? O4 C13A C14B C19B 40.9(8) . . . . ? N1 C1 C2 C3 1.3(5) . . . . ? C1 N1 C5 C4 -0.7(4) . . . . ? C1 N1 C5 C5 178.9(3) . . . 2_556 ? C1 C2 C3 C4 -1.0(5) . . . . ? C2 C3 C4 C5 0.0(5) . . . . ? C2 C3 C4 C6 179.9(3) . . . . ? C3 C4 C5 N1 0.9(5) . . . . ? C3 C4 C5 C5 -178.6(3) . . . 2_556 ? C3 C4 C6 C6 -179.6(4) . . . 2_556 ? C5 N1 C1 C2 -0.4(5) . . . . ? C5 C4 C6 C6 0.3(6) . . . 2_556 ? C6 C4 C5 N1 -179.1(3) . . . . ? C6 C4 C5 C5 1.4(5) . . . 2_556 ? C13A C14A C15A C16A 178.8(5) . . . . ? C13A C14A C19A C20A 51(2) . . . . ? C13A C14B C15B C16B -173.0(4) . . . . ? C13A C14B C19B C20B 67.9(19) . . . . ? C14A C15A C16A C17A -48.1(7) . . . . ? C15A C14A C19A C20A -61(2) . . . . ? C15A C16A C17A C18A -177.3(6) . . . . ? C19A C14A C15A C16A -66.2(10) . . . . ? C14B C15B C16B C17B 170.8(5) . . . . ? C15B C14B C19B C20B -167.1(16) . . . . ? C15B C16B C17B C18B -179.9(5) . . . . ? C19B C14B C15B C16B 59.2(11) . . . . ?