#------------------------------------------------------------------------------ #$Date: 2017-04-21 05:21:56 +0300 (Fri, 21 Apr 2017) $ #$Revision: 195642 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/04/27/7042731.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_7042731 loop_ _publ_author_name 'Schmitt, Wolfgang' 'Marzec, Bartosz' 'Zhang, Lei' 'Zhu, Nian Yong' _publ_section_title ; Bio-inspired synthetic approaches: From hierarchical, hybrid supramolecular assemblies to CaCO3-based microspheres ; _journal_name_full 'Dalton Trans.' _journal_paper_doi 10.1039/C7DT00914C _journal_year 2017 _chemical_formula_moiety 'C13 H21 Ca N O8, H2 O' _chemical_formula_sum 'C13 H23 Ca N O9' _chemical_formula_weight 377.40 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2016/6 _audit_update_record ; 2017-04-12 deposited with the CCDC. 2017-04-20 downloaded from the CCDC. ; _cell_angle_alpha 96.66(2) _cell_angle_beta 94.77(2) _cell_angle_gamma 92.07(2) _cell_formula_units_Z 4 _cell_length_a 6.2649(10) _cell_length_b 8.2062(10) _cell_length_c 33.649(6) _cell_measurement_reflns_used 6602 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 25.86 _cell_measurement_theta_min 2.45 _cell_volume 1710.5(5) _computing_cell_refinement 'Bruker Smart' _computing_data_collection 'Bruker Smart' _computing_data_reduction 'Bruker Saint' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL-2016/6 (Sheldrick, 2016)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 150(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device_type 'Bruker Smart Apex' _diffrn_measurement_method 'omega and phi scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0402 _diffrn_reflns_av_unetI/netI 0.0805 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_number 6606 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.997 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.865 _diffrn_reflns_theta_min 0.612 _exptl_absorpt_coefficient_mu 0.413 _exptl_crystal_colour Colourless _exptl_crystal_density_diffrn 1.466 _exptl_crystal_density_method 'not measured' _exptl_crystal_description Needle _exptl_crystal_F_000 800 _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: H2O/MeOH 1:1 (v/v)' _exptl_crystal_size_max 0.600 _exptl_crystal_size_mid 0.050 _exptl_crystal_size_min 0.050 _refine_diff_density_max 0.433 _refine_diff_density_min -0.548 _refine_diff_density_rms 0.119 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 493 _refine_ls_number_reflns 6606 _refine_ls_number_restraints 13 _refine_ls_restrained_S_all 1.043 _refine_ls_R_factor_all 0.0677 _refine_ls_R_factor_gt 0.0514 _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^)+(0.0665P)^2^+0.0282P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1191 _refine_ls_wR_factor_ref 0.1316 _reflns_Friedel_coverage 0.000 _reflns_number_gt 5135 _reflns_number_total 6606 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c7dt00914c2.cif _cod_data_source_block shelx _cod_database_code 7042731 _shelx_shelxl_version_number 2016/6 _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 0.790 _shelx_estimated_absorpt_t_max 0.980 _shelx_res_file ; TITL CAME2HDA OLEX2: imported from CIF shelx.res created by SHELXL-2016/6 at 20:24:22 on 06-Apr-2017 CELL 0.71073 6.2649 8.2062 33.6491 96.657 94.771 92.072 ZERR 4.00 0.0010 0.0010 0.0060 0.020 0.020 0.020 LATT 1 SFAC C H CA N O UNIT 52 92 4 4 36 MERG 2 EQIV $1 2-X,2-Y,1-Z EQIV $2 1+X,+Y,+Z EQIV $3 -1+X,-1+Y,+Z EQIV $4 -X,2-Y,1-Z EQIV $5 +X,1+Y,+Z EQIV $6 -X,1-Y,1-Z EQIV $7 1-X,2-Y,1-Z EQIV $8 +X,-1+Y,+Z EQIV $9 1-X,2-Y,2-Z EQIV $10 2-X,3-Y,2-Z EQIV $11 x-1,y,z DFIX 0.900 0.020 O1 H1 O2 H2 DFIX 0.920 0.020 O17 H17A O17 H17B O17 H17C DANG 1.40 0.04 H17A H17B H17A H17C DFIX 0.920 0.020 O0AA H0AA O0AA H0AB DANG 1.50 0.08 H0AA H0AB H0AA H1AB DFIX 0.920 0.020 O1AA H0AA O1AA H1AB HTAB FMAP 2 PLAN 40 SIZE 0.050 0.050 0.600 ACTA L.S. 8 TEMP -123.00 WGHT 0.066500 0.028200 FVAR 0.99927 0.49947 CA1 3 0.103544 0.758783 0.565895 11.00000 0.01505 0.01531 = 0.01719 0.00267 0.00062 0.00033 O1 5 0.179041 0.987592 0.630406 11.00000 0.03277 0.02915 = 0.03618 0.01576 -0.00965 -0.00314 O3 5 -0.241167 0.843733 0.584300 11.00000 0.02161 0.03226 = 0.02660 0.00220 0.00185 0.00502 O4 5 0.099323 0.463563 0.561802 11.00000 0.03484 0.02083 = 0.01712 0.00279 0.00126 0.00370 O5 5 0.203546 0.254122 0.592958 11.00000 0.10787 0.01736 = 0.02632 0.00401 0.00005 0.01511 O6 5 -0.558344 0.731205 0.594413 11.00000 0.01465 0.07067 = 0.03219 -0.00145 -0.00221 -0.00037 O7 5 0.304727 0.684863 0.504240 11.00000 0.04428 0.02174 = 0.02723 0.00205 0.00717 0.00123 O8 5 0.147503 1.004403 0.534494 11.00000 0.03546 0.01815 = 0.02519 0.00163 0.00235 0.00152 AFIX 137 H8C 2 0.026964 1.010746 0.514300 10.50000 0.05639 H8B 2 0.281871 1.002426 0.521507 10.50000 0.11157 H8A 2 0.151629 1.100357 0.554850 11.00000 0.07597 AFIX 0 O9 5 -0.186330 0.663732 0.511445 11.00000 0.03389 0.02892 = 0.01998 -0.00186 -0.00209 0.00601 N1 4 -0.022342 0.636295 0.628406 11.00000 0.02065 0.01961 = 0.01794 0.00044 -0.00020 -0.00173 C1 1 0.295771 0.945735 0.663851 11.00000 0.02755 0.01751 = 0.02897 0.00212 -0.00742 0.00459 C2 1 0.206507 0.818087 0.681657 11.00000 0.03084 0.01687 = 0.01742 -0.00244 -0.00363 0.00430 C3 1 0.321014 0.766638 0.714770 11.00000 0.04539 0.02256 = 0.02017 0.00013 -0.00091 0.00590 AFIX 43 H3 2 0.261888 0.678760 0.727029 11.00000 -1.20000 AFIX 0 C4 1 0.518057 0.838531 0.730598 11.00000 0.04130 0.03300 = 0.02280 -0.00810 -0.01224 0.01309 C5 1 0.596632 0.967599 0.712584 11.00000 0.02459 0.02951 = 0.04323 -0.01418 -0.01519 0.00769 AFIX 43 H5 2 0.729350 1.020692 0.723531 11.00000 -1.20000 AFIX 0 C6 1 0.491734 1.024290 0.679181 11.00000 0.02596 0.02020 = 0.04707 -0.00120 -0.00446 0.00131 C7 1 0.588674 1.162938 0.660496 11.00000 0.03964 0.03510 = 0.09083 0.01585 -0.00970 -0.00922 AFIX 137 H7C 2 0.488085 1.251546 0.659979 11.00000 -1.50000 H7D 2 0.619195 1.123966 0.632995 11.00000 -1.50000 H7E 2 0.722246 1.204127 0.676274 11.00000 -1.50000 AFIX 0 C8 1 0.640708 0.779514 0.766134 11.00000 0.06086 0.07155 = 0.03480 -0.00247 -0.02014 0.02539 AFIX 137 H8F 2 0.572586 0.676666 0.772018 11.00000 -1.50000 H8D 2 0.640745 0.862638 0.789527 11.00000 -1.50000 H8E 2 0.788692 0.760792 0.760006 11.00000 -1.50000 AFIX 0 C9 1 -0.012173 0.745448 0.666841 11.00000 0.03276 0.02245 = 0.01719 0.00219 0.00431 -0.00108 AFIX 23 H9D 2 -0.065721 0.682209 0.687597 11.00000 -1.20000 H9F 2 -0.109842 0.836019 0.663517 11.00000 -1.20000 AFIX 0 C19 1 -0.250576 0.597050 0.615333 11.00000 0.02120 0.03150 = 0.02919 -0.00039 0.00396 -0.01015 AFIX 23 H19A 2 -0.326162 0.571889 0.638743 11.00000 -1.20000 H19B 2 -0.262964 0.497653 0.595427 11.00000 -1.20000 AFIX 0 C20 1 -0.359015 0.736488 0.596780 11.00000 0.02277 0.04001 = 0.01279 -0.00723 0.00048 -0.00226 C21 1 0.092416 0.486571 0.632687 11.00000 0.03009 0.02187 = 0.01722 0.00539 -0.00028 -0.00205 AFIX 23 H21A 2 0.007750 0.413965 0.647629 11.00000 -1.20000 H21B 2 0.231370 0.515596 0.648632 11.00000 -1.20000 AFIX 0 C22 1 0.133013 0.394392 0.592667 11.00000 0.03408 0.01650 = 0.01958 0.00253 -0.00232 -0.00420 CA2 3 0.783466 1.311136 0.935544 11.00000 0.01521 0.01562 = 0.01716 0.00341 0.00338 0.00124 O2 5 0.811329 1.093294 0.873655 11.00000 0.03282 0.02218 = 0.02825 0.00895 0.01247 0.00603 O10 5 0.900793 1.828693 0.911495 11.00000 0.02933 0.01688 = 0.02678 0.00376 0.00101 -0.00331 O11 5 0.804080 1.614884 0.941808 11.00000 0.03259 0.01975 = 0.01714 0.00269 0.00053 -0.00265 O12 5 0.688066 1.404758 1.002725 11.00000 0.04061 0.02592 = 0.02794 0.00118 0.01236 0.00618 AFIX 137 H12A 2 0.696286 1.313802 1.019184 10.50000 -1.50000 H12B 2 0.541669 1.443229 1.001141 10.50000 -1.50000 H12F 2 0.787795 1.494975 1.014925 11.00000 -1.50000 AFIX 0 O13 5 1.092615 1.239284 0.979298 11.00000 0.02236 0.05626 = 0.02372 0.00487 -0.00004 -0.00374 AFIX 137 H13A 2 1.109374 1.316941 1.003891 10.50000 -1.50000 H13B 2 1.222833 1.244599 0.965164 11.00000 -1.50000 H13F 2 1.068548 1.127745 0.986234 10.50000 -1.50000 AFIX 0 O14 5 0.685132 1.047010 0.958554 11.00000 0.02412 0.02114 = 0.02656 0.00209 0.00303 -0.00138 AFIX 137 H14F 2 0.536984 1.013616 0.948401 10.50000 0.01193 H14A 2 0.697759 1.058743 0.987982 10.50000 0.07372 H14B 2 0.781470 0.963425 0.948447 11.00000 0.08207 AFIX 0 O15 5 0.092911 1.383687 0.905318 11.00000 0.01503 0.04488 = 0.02980 0.01165 0.00452 0.00300 O16 5 0.400581 1.279368 0.925118 11.00000 0.01913 0.03378 = 0.03600 0.01731 0.00874 0.00563 N2 4 0.619758 1.445215 0.873532 11.00000 0.01393 0.01669 = 0.01909 0.00073 0.00133 -0.00006 C10 1 1.049356 1.243563 0.771181 11.00000 0.03100 0.02851 = 0.01997 -0.00292 0.00476 -0.00789 C11 1 1.135137 1.300646 0.734294 11.00000 0.05286 0.05058 = 0.02767 0.00827 0.01410 -0.00029 AFIX 137 H11A 2 1.117859 1.210963 0.712192 11.00000 -1.50000 H11B 2 1.287516 1.333499 0.740113 11.00000 -1.50000 H11C 2 1.055755 1.394554 0.726619 11.00000 -1.50000 AFIX 0 C12 1 1.190426 0.935156 0.844065 11.00000 0.04480 0.03980 = 0.05689 0.01741 0.02518 0.01923 AFIX 137 H12C 2 1.095549 0.836824 0.842945 11.00000 -1.50000 H12D 2 1.234234 0.976569 0.872164 11.00000 -1.50000 H12E 2 1.317693 0.907438 0.830057 11.00000 -1.50000 AFIX 0 C13 1 1.072769 1.065844 0.824035 11.00000 0.03064 0.01918 = 0.03075 -0.00023 0.00706 0.00192 C14 1 1.144681 1.118913 0.789759 11.00000 0.02931 0.02308 = 0.02793 -0.00624 0.01225 -0.00192 AFIX 43 H14 2 1.263522 1.068241 0.778539 11.00000 -1.20000 AFIX 0 C15 1 0.872992 1.311666 0.787416 11.00000 0.03179 0.02370 = 0.01775 0.00052 0.00033 -0.00418 AFIX 43 H15 2 0.805195 1.396796 0.775003 11.00000 -1.20000 AFIX 0 C16 1 0.790945 1.260210 0.821278 11.00000 0.02409 0.02131 = 0.01617 -0.00306 0.00083 -0.00284 C17 1 0.894557 1.137305 0.839564 11.00000 0.02691 0.01652 = 0.02021 -0.00088 0.00601 -0.00378 C18 1 0.591445 1.330981 0.836060 11.00000 0.02319 0.02492 = 0.01546 0.00093 -0.00341 -0.00261 AFIX 23 H18A 2 0.521591 1.389437 0.814719 11.00000 -1.20000 H18B 2 0.492026 1.239142 0.840197 11.00000 -1.20000 AFIX 0 C23 1 0.754614 1.589990 0.869952 11.00000 0.01696 0.01656 = 0.02041 0.00457 0.00169 -0.00100 AFIX 23 H23A 2 0.674355 1.663126 0.853296 11.00000 -1.20000 H23B 2 0.882858 1.556290 0.856328 11.00000 -1.20000 AFIX 0 C24 1 0.824957 1.683471 0.911216 11.00000 0.01494 0.01570 = 0.02189 0.00249 0.00215 0.00252 C25 1 0.405615 1.494673 0.883725 11.00000 0.01592 0.02260 = 0.02750 0.00518 0.00420 0.00402 AFIX 23 H25A 2 0.317157 1.508011 0.858630 11.00000 -1.20000 H25B 2 0.420314 1.602832 0.900366 11.00000 -1.20000 AFIX 0 C26 1 0.290461 1.375004 0.905959 11.00000 0.01713 0.02408 = 0.01847 0.00102 0.00356 0.00298 O17 5 0.294099 0.871611 0.957623 11.00000 0.02531 0.03787 = 0.03141 0.00913 0.00020 -0.00309 PART 2 O0AA 5 0.642386 1.157137 0.560623 21.00000 0.05776 0.04405 = 0.04927 0.02639 0.02295 0.02110 PART 1 O1AA 5 0.614695 1.034757 0.531089 -21.00000 0.02534 0.03775 = 0.03346 0.01541 0.00412 0.00239 PART 0 H0AA 2 0.661656 1.043176 0.558180 11.00000 0.11638 H17A 2 0.172078 0.867287 0.941233 11.00000 0.07244 H9B 2 9.699612 10.742620 10.511992 11.00000 0.15763 H9A 2 9.873590 10.656950 10.485286 11.00000 0.08867 H7A 2 10.276197 10.764462 10.485065 11.00000 0.07437 H7B 2 10.256559 10.574533 10.491568 11.00000 0.08076 H1 2 0.210662 1.090197 0.625877 11.00000 0.05869 H2 2 0.851243 0.994348 0.878400 11.00000 0.05580 PART 2 H17B 2 0.243909 0.894965 0.982312 10.50000 0.07381 H0AB 2 0.512914 1.169904 0.571631 21.00000 0.04653 PART 1 H17C 2 0.394130 0.926315 0.944969 10.50000 0.13238 H1AB 2 0.483021 0.983545 0.524888 -21.00000 0.07966 HKLF 4 REM CAME2HDA OLEX2: imported from CIF REM R1 = 0.0514 for 5135 Fo > 4sig(Fo) and 0.0677 for all 6606 data REM 493 parameters refined using 13 restraints END WGHT 0.0665 0.0282 REM Instructions for potential hydrogen bonds HTAB O8 O8_$4 HTAB O8 O1AA HTAB O8 O1AA_$7 HTAB O8 O5_$5 HTAB O12 O17_$9 EQIV $12 -x+1, -y+3, -z+2 HTAB O12 O12_$12 HTAB O12 O13_$10 HTAB O13 O11_$10 HTAB O13 O12_$10 HTAB O13 O16_$2 HTAB O14 O17 HTAB O14 O17_$9 HTAB O14 O10_$8 HTAB O0AA O3_$2 HTAB O1AA O3_$2 HTAB O17 O10_$3 HTAB O9 O7_$11 HTAB O9 O1AA_$11 HTAB O9 O4_$6 HTAB O7 O0AA_$7 HTAB O7 O1AA_$7 HTAB O7 O9_$6 HTAB O1 O5_$5 HTAB O2 O10_$8 HTAB O17 O14_$9 HTAB O0AA O5_$5 HTAB O17 O14 HTAB O1AA O7 HTAB O1AA O8 HTAB O1AA O1AA_$7 REM Highest difference peak 0.433, deepest hole -0.548, 1-sigma level 0.119 Q1 1 0.0747 0.2432 0.5982 11.00000 0.05 0.43 Q2 1 1.1306 1.2890 0.7565 11.00000 0.05 0.40 Q3 1 1.0112 1.2580 0.7490 11.00000 0.05 0.40 Q4 1 1.0268 1.3204 0.7870 11.00000 0.05 0.37 Q5 1 0.5328 0.8036 0.7430 11.00000 0.05 0.37 Q6 1 1.0666 1.1710 0.7711 11.00000 0.05 0.37 Q7 1 0.7242 0.6751 0.7587 11.00000 0.05 0.37 Q8 1 0.0846 0.8709 0.5656 11.00000 0.05 0.37 Q9 1 0.8422 1.2897 0.8026 11.00000 0.05 0.36 Q10 1 0.6319 1.2988 0.9411 11.00000 0.05 0.36 Q11 1 1.2017 1.4303 0.7431 11.00000 0.05 0.35 Q12 1 1.1382 1.2132 0.7811 11.00000 0.05 0.35 Q13 1 0.2696 0.7594 0.6908 11.00000 0.05 0.35 Q14 1 1.2839 1.2355 0.7281 11.00000 0.05 0.34 Q15 1 0.5084 0.7580 0.7864 11.00000 0.05 0.34 Q16 1 0.4052 0.9835 0.6718 11.00000 0.05 0.33 Q17 1 0.5254 0.9762 0.6901 11.00000 0.05 0.33 Q18 1 0.9253 1.0602 0.8221 11.00000 0.05 0.32 Q19 1 0.9121 1.2566 0.9313 11.00000 0.05 0.32 Q20 1 1.0569 1.0731 0.7978 11.00000 0.05 0.32 Q21 1 1.1546 1.2569 1.0033 11.00000 0.05 0.32 Q22 1 0.3965 0.8614 0.7289 11.00000 0.05 0.32 Q23 1 0.4388 0.8187 0.7295 11.00000 0.05 0.31 Q24 1 0.9175 1.2472 0.7739 11.00000 0.05 0.31 Q25 1 0.2381 0.9770 0.6522 11.00000 0.05 0.30 Q26 1 0.2279 0.8171 0.7014 11.00000 0.05 0.30 Q27 1 0.2459 0.2156 0.5909 11.00000 0.05 0.30 Q28 1 0.5143 1.0304 0.7006 11.00000 0.05 0.30 Q29 1 0.1822 0.6993 0.7258 11.00000 0.05 0.30 Q30 1 0.1030 0.7672 0.7576 11.00000 0.05 0.30 Q31 1 1.0904 0.9746 0.8235 11.00000 0.05 0.29 Q32 1 1.1460 1.1214 0.8093 11.00000 0.05 0.29 Q33 1 0.1592 0.7968 0.7671 11.00000 0.05 0.29 Q34 1 0.0823 0.4235 0.6461 11.00000 0.05 0.29 Q35 1 0.7155 1.3021 0.8305 11.00000 0.05 0.29 Q36 1 0.6944 1.1244 0.6498 11.00000 0.05 0.29 Q37 1 0.4442 1.1059 0.6844 11.00000 0.05 0.29 Q38 1 0.6187 1.3662 0.8584 11.00000 0.05 0.29 Q39 1 1.0124 1.1343 0.8331 11.00000 0.05 0.29 Q40 1 -0.0329 0.8510 0.7187 11.00000 0.05 0.28 ; _shelx_res_checksum 68984 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' 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 0.10354(8) 0.75878(6) 0.56589(2) 0.01585(15) Uani 1 1 d . . . . . O1 O 0.1790(3) 0.9876(3) 0.63041(7) 0.0326(5) Uani 1 1 d D . . . . O3 O -0.2412(3) 0.8437(2) 0.58430(6) 0.0269(5) Uani 1 1 d . . . . . O4 O 0.0993(3) 0.4636(2) 0.56180(6) 0.0242(4) Uani 1 1 d . . . . . O5 O 0.2035(5) 0.2541(3) 0.59296(7) 0.0504(7) Uani 1 1 d . . . . . O6 O -0.5583(3) 0.7312(3) 0.59441(7) 0.0401(6) Uani 1 1 d . . . . . O7 O 0.3047(3) 0.6849(2) 0.50424(6) 0.0309(5) Uani 1 1 d . . . . . O8 O 0.1475(3) 1.0044(2) 0.53449(6) 0.0264(5) Uani 1 1 d . . . . . H8C H 0.026964 1.010746 0.514300 0.06(2) Uiso 0.5 1 calc R . P . . H8B H 0.281871 1.002426 0.521507 0.11(4) Uiso 0.5 1 calc R . P . . H8A H 0.151629 1.100357 0.554850 0.076(14) Uiso 1 1 calc R . . . . O9 O -0.1863(3) 0.6637(2) 0.51144(6) 0.0281(5) Uani 1 1 d . . . . . N1 N -0.0223(3) 0.6363(3) 0.62841(7) 0.0197(5) Uani 1 1 d . . . . . C1 C 0.2958(5) 0.9457(3) 0.66385(9) 0.0252(7) Uani 1 1 d . . . . . C2 C 0.2065(5) 0.8181(3) 0.68166(8) 0.0223(6) Uani 1 1 d . . . . . C3 C 0.3210(5) 0.7666(4) 0.71477(9) 0.0297(7) Uani 1 1 d . . . . . H3 H 0.261888 0.678760 0.727029 0.036 Uiso 1 1 calc R U . . . C4 C 0.5181(5) 0.8385(4) 0.73060(9) 0.0338(8) Uani 1 1 d . . . . . C5 C 0.5966(5) 0.9676(4) 0.71258(10) 0.0348(8) Uani 1 1 d . . . . . H5 H 0.729350 1.020692 0.723531 0.042 Uiso 1 1 calc R U . . . C6 C 0.4917(5) 1.0243(4) 0.67918(10) 0.0319(7) Uani 1 1 d . . . . . C7 C 0.5887(6) 1.1629(4) 0.66050(14) 0.0557(11) Uani 1 1 d . . . . . H7C H 0.488085 1.251546 0.659979 0.084 Uiso 1 1 calc R U . . . H7D H 0.619195 1.123966 0.632995 0.084 Uiso 1 1 calc R U . . . H7E H 0.722246 1.204127 0.676274 0.084 Uiso 1 1 calc R U . . . C8 C 0.6407(7) 0.7795(5) 0.76613(11) 0.0573(11) Uani 1 1 d . . . . . H8F H 0.572586 0.676666 0.772018 0.086 Uiso 1 1 calc R U . . . H8D H 0.640745 0.862638 0.789527 0.086 Uiso 1 1 calc R U . . . H8E H 0.788692 0.760792 0.760006 0.086 Uiso 1 1 calc R U . . . C9 C -0.0122(5) 0.7454(4) 0.66684(8) 0.0241(6) Uani 1 1 d . . . . . H9D H -0.065721 0.682209 0.687597 0.029 Uiso 1 1 calc R U . . . H9F H -0.109842 0.836019 0.663517 0.029 Uiso 1 1 calc R U . . . C19 C -0.2506(4) 0.5971(4) 0.61533(9) 0.0278(7) Uani 1 1 d . . . . . H19A H -0.326162 0.571889 0.638743 0.033 Uiso 1 1 calc R U . . . H19B H -0.262964 0.497653 0.595427 0.033 Uiso 1 1 calc R U . . . C20 C -0.3590(5) 0.7365(4) 0.59678(8) 0.0262(7) Uani 1 1 d . . . . . C21 C 0.0924(5) 0.4866(3) 0.63269(8) 0.0230(6) Uani 1 1 d . . . . . H21A H 0.007750 0.413965 0.647629 0.028 Uiso 1 1 calc R U . . . H21B H 0.231370 0.515596 0.648632 0.028 Uiso 1 1 calc R U . . . C22 C 0.1330(5) 0.3944(3) 0.59267(8) 0.0238(6) Uani 1 1 d . . . . . Ca2 Ca 0.78347(8) 1.31114(6) 0.93554(2) 0.01576(15) Uani 1 1 d . . . . . O2 O 0.8113(3) 1.0933(2) 0.87366(6) 0.0266(5) Uani 1 1 d D . . . . O10 O 0.9008(3) 1.8287(2) 0.91149(6) 0.0244(4) Uani 1 1 d . . . . . O11 O 0.8041(3) 1.6149(2) 0.94181(5) 0.0233(4) Uani 1 1 d . . . . . O12 O 0.6881(3) 1.4048(3) 1.00273(6) 0.0310(5) Uani 1 1 d . . . . . H12A H 0.696286 1.313802 1.019184 0.047 Uiso 0.5 1 calc R U P . . H12B H 0.541669 1.443229 1.001141 0.047 Uiso 0.5 1 calc R U P . . H12F H 0.787795 1.494975 1.014925 0.047 Uiso 1 1 calc R U . . . O13 O 1.0926(3) 1.2393(3) 0.97930(6) 0.0344(5) Uani 1 1 d . . . . . H13A H 1.109374 1.316941 1.003891 0.052 Uiso 0.5 1 calc R U P . . H13B H 1.222833 1.244599 0.965164 0.052 Uiso 1 1 calc R U . . . H13F H 1.068548 1.127745 0.986234 0.052 Uiso 0.5 1 calc R U P . . O14 O 0.6851(3) 1.0470(2) 0.95855(6) 0.0240(5) Uani 1 1 d . . . . . H14F H 0.536984 1.013616 0.948401 0.012(13) Uiso 0.5 1 calc R . P . . H14A H 0.697759 1.058743 0.987982 0.07(3) Uiso 0.5 1 calc R . P . . H14B H 0.781470 0.963425 0.948447 0.082(15) Uiso 1 1 calc R . . . . O15 O 0.0929(3) 1.3837(3) 0.90532(6) 0.0292(5) Uani 1 1 d . . . . . O16 O 0.4006(3) 1.2794(3) 0.92512(6) 0.0281(5) Uani 1 1 d . . . . . N2 N 0.6198(3) 1.4452(3) 0.87353(6) 0.0167(5) Uani 1 1 d . . . . . C10 C 1.0494(5) 1.2436(4) 0.77118(9) 0.0270(7) Uani 1 1 d . . . . . C11 C 1.1351(6) 1.3006(5) 0.73429(10) 0.0429(9) Uani 1 1 d . . . . . H11A H 1.117859 1.210963 0.712192 0.064 Uiso 1 1 calc R U . . . H11B H 1.287516 1.333499 0.740113 0.064 Uiso 1 1 calc R U . . . H11C H 1.055755 1.394554 0.726619 0.064 Uiso 1 1 calc R U . . . C12 C 1.1904(6) 0.9352(4) 0.84406(12) 0.0447(9) Uani 1 1 d . . . . . H12C H 1.095549 0.836824 0.842945 0.067 Uiso 1 1 calc R U . . . H12D H 1.234234 0.976569 0.872164 0.067 Uiso 1 1 calc R U . . . H12E H 1.317693 0.907438 0.830057 0.067 Uiso 1 1 calc R U . . . C13 C 1.0728(5) 1.0658(3) 0.82404(9) 0.0268(7) Uani 1 1 d . . . . . C14 C 1.1447(5) 1.1189(4) 0.78976(9) 0.0270(7) Uani 1 1 d . . . . . H14 H 1.263522 1.068241 0.778539 0.032 Uiso 1 1 calc R U . . . C15 C 0.8730(5) 1.3117(4) 0.78742(8) 0.0248(6) Uani 1 1 d . . . . . H15 H 0.805195 1.396796 0.775003 0.030 Uiso 1 1 calc R U . . . C16 C 0.7909(4) 1.2602(3) 0.82128(8) 0.0211(6) Uani 1 1 d . . . . . C17 C 0.8946(4) 1.1373(3) 0.83956(8) 0.0214(6) Uani 1 1 d . . . . . C18 C 0.5914(4) 1.3310(3) 0.83606(8) 0.0217(6) Uani 1 1 d . . . . . H18A H 0.521591 1.389437 0.814719 0.026 Uiso 1 1 calc R U . . . H18B H 0.492026 1.239142 0.840197 0.026 Uiso 1 1 calc R U . . . C23 C 0.7546(4) 1.5900(3) 0.86995(8) 0.0178(6) Uani 1 1 d . . . . . H23A H 0.674355 1.663126 0.853296 0.021 Uiso 1 1 calc R U . . . H23B H 0.882858 1.556290 0.856328 0.021 Uiso 1 1 calc R U . . . C24 C 0.8250(4) 1.6835(3) 0.91122(8) 0.0174(6) Uani 1 1 d . . . . . C25 C 0.4056(4) 1.4947(3) 0.88373(9) 0.0216(6) Uani 1 1 d . . . . . H25A H 0.317157 1.508011 0.858630 0.026 Uiso 1 1 calc R U . . . H25B H 0.420314 1.602832 0.900366 0.026 Uiso 1 1 calc R U . . . C26 C 0.2905(4) 1.3750(3) 0.90596(8) 0.0199(6) Uani 1 1 d . . . . . O17 O 0.2941(3) 0.8716(3) 0.95762(7) 0.0314(5) Uani 1 1 d D . . . . O0AA O 0.6424(9) 1.1571(7) 0.56062(16) 0.0472(19) Uani 0.499(7) 1 d D . P A 2 O1AA O 0.6147(7) 1.0348(6) 0.53109(14) 0.0312(15) Uani 0.501(7) 1 d D . P A 1 H0AA H 0.662(8) 1.043(3) 0.5582(7) 0.12(2) Uiso 1 1 d D . . . . H17A H 0.172(4) 0.867(5) 0.9412(10) 0.072(14) Uiso 1 1 d D . . . . H9B H -0.300388 0.742620 0.511992 0.16(3) Uiso 1 1 d . . . . . H9A H -0.126410 0.656950 0.485286 0.089(16) Uiso 1 1 d . . . . . H7A H 0.276197 0.764462 0.485065 0.074(14) Uiso 1 1 d . . . . . H7B H 0.256559 0.574533 0.491568 0.081(14) Uiso 1 1 d . . . . . H1 H 0.211(6) 1.090(3) 0.6259(11) 0.059(12) Uiso 1 1 d D . . . . H2 H 0.851(6) 0.994(3) 0.8784(11) 0.056(12) Uiso 1 1 d D . . . . H17B H 0.244(10) 0.895(10) 0.9823(9) 0.07(3) Uiso 0.5 1 d D . P B 2 H0AB H 0.513(6) 1.170(8) 0.572(2) 0.05(2) Uiso 0.499(7) 1 d D . P A 2 H17C H 0.394(9) 0.926(13) 0.945(2) 0.13(5) Uiso 0.5 1 d D . P C 1 H1AB H 0.483(7) 0.984(10) 0.525(2) 0.08(3) Uiso 0.501(7) 1 d D . P A 1 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 0.0151(3) 0.0153(3) 0.0172(3) 0.0027(2) 0.0006(2) 0.0003(2) O1 0.0328(12) 0.0291(12) 0.0362(13) 0.0158(10) -0.0096(10) -0.0031(10) O3 0.0216(10) 0.0323(12) 0.0266(11) 0.0022(9) 0.0018(9) 0.0050(9) O4 0.0348(11) 0.0208(10) 0.0171(10) 0.0028(8) 0.0013(9) 0.0037(9) O5 0.108(2) 0.0174(12) 0.0263(13) 0.0040(10) 0.0001(13) 0.0151(13) O6 0.0147(11) 0.0707(17) 0.0322(13) -0.0015(12) -0.0022(9) -0.0004(11) O7 0.0443(13) 0.0217(11) 0.0272(12) 0.0020(9) 0.0072(10) 0.0012(10) O8 0.0355(12) 0.0181(10) 0.0252(11) 0.0016(9) 0.0024(9) 0.0015(9) O9 0.0339(12) 0.0289(11) 0.0200(11) -0.0019(9) -0.0021(9) 0.0060(10) N1 0.0207(12) 0.0196(12) 0.0179(12) 0.0004(10) -0.0002(9) -0.0017(10) C1 0.0275(16) 0.0175(15) 0.0290(17) 0.0021(12) -0.0074(13) 0.0046(12) C2 0.0308(16) 0.0169(14) 0.0174(15) -0.0024(11) -0.0036(12) 0.0043(12) C3 0.0454(19) 0.0226(16) 0.0202(16) 0.0001(12) -0.0009(14) 0.0059(14) C4 0.0413(19) 0.0330(18) 0.0228(16) -0.0081(14) -0.0122(14) 0.0131(15) C5 0.0246(16) 0.0295(17) 0.043(2) -0.0142(15) -0.0152(14) 0.0077(14) C6 0.0260(16) 0.0202(15) 0.047(2) -0.0012(14) -0.0045(14) 0.0013(13) C7 0.040(2) 0.035(2) 0.091(3) 0.016(2) -0.010(2) -0.0092(17) C8 0.061(3) 0.072(3) 0.035(2) -0.0025(19) -0.0201(19) 0.025(2) C9 0.0328(16) 0.0225(15) 0.0172(15) 0.0022(12) 0.0043(12) -0.0011(13) C19 0.0212(15) 0.0315(17) 0.0292(17) -0.0004(13) 0.0040(13) -0.0101(13) C20 0.0228(16) 0.0400(18) 0.0128(14) -0.0072(13) 0.0005(12) -0.0023(13) C21 0.0301(16) 0.0219(15) 0.0172(14) 0.0054(12) -0.0003(12) -0.0020(12) C22 0.0341(17) 0.0165(15) 0.0196(15) 0.0025(12) -0.0023(12) -0.0042(12) Ca2 0.0152(3) 0.0156(3) 0.0172(3) 0.0034(2) 0.0034(2) 0.0012(2) O2 0.0328(12) 0.0222(11) 0.0283(12) 0.0089(9) 0.0125(9) 0.0060(9) O10 0.0293(11) 0.0169(10) 0.0268(11) 0.0038(8) 0.0010(9) -0.0033(8) O11 0.0326(11) 0.0197(10) 0.0171(10) 0.0027(8) 0.0005(8) -0.0026(9) O12 0.0406(13) 0.0259(11) 0.0279(12) 0.0012(9) 0.0124(10) 0.0062(10) O13 0.0224(11) 0.0563(15) 0.0237(11) 0.0049(10) 0.0000(9) -0.0037(10) O14 0.0241(11) 0.0211(10) 0.0266(12) 0.0021(8) 0.0030(9) -0.0014(9) O15 0.0150(10) 0.0449(13) 0.0298(12) 0.0117(10) 0.0045(8) 0.0030(9) O16 0.0191(10) 0.0338(12) 0.0360(12) 0.0173(10) 0.0087(9) 0.0056(9) N2 0.0139(11) 0.0167(11) 0.0191(12) 0.0007(9) 0.0013(9) -0.0001(9) C10 0.0310(16) 0.0285(16) 0.0200(15) -0.0029(13) 0.0048(13) -0.0079(13) C11 0.053(2) 0.051(2) 0.0277(19) 0.0083(16) 0.0141(16) -0.0003(18) C12 0.045(2) 0.040(2) 0.057(2) 0.0174(18) 0.0252(18) 0.0192(17) C13 0.0306(16) 0.0192(15) 0.0307(17) -0.0002(13) 0.0071(13) 0.0019(12) C14 0.0293(16) 0.0231(16) 0.0279(17) -0.0062(13) 0.0122(13) -0.0019(13) C15 0.0318(16) 0.0237(15) 0.0177(15) 0.0005(12) 0.0003(12) -0.0042(13) C16 0.0241(15) 0.0213(15) 0.0162(14) -0.0031(11) 0.0008(11) -0.0028(12) C17 0.0269(15) 0.0165(14) 0.0202(15) -0.0009(12) 0.0060(12) -0.0038(12) C18 0.0232(15) 0.0249(15) 0.0155(14) 0.0009(12) -0.0034(11) -0.0026(12) C23 0.0170(13) 0.0166(14) 0.0204(14) 0.0046(11) 0.0017(11) -0.0010(11) C24 0.0149(13) 0.0157(14) 0.0219(15) 0.0025(11) 0.0021(11) 0.0025(11) C25 0.0159(14) 0.0226(15) 0.0275(16) 0.0052(12) 0.0042(12) 0.0040(11) C26 0.0171(14) 0.0241(15) 0.0185(14) 0.0010(12) 0.0036(11) 0.0030(11) O17 0.0253(12) 0.0379(13) 0.0314(13) 0.0091(11) 0.0002(10) -0.0031(10) O0AA 0.058(4) 0.044(4) 0.049(4) 0.026(3) 0.023(3) 0.021(3) O1AA 0.025(3) 0.038(3) 0.033(3) 0.015(2) 0.004(2) 0.002(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' 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' 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 O6 Ca1 O8 101.88(8) 1_655 . O6 Ca1 O3 140.17(8) 1_655 . O8 Ca1 O3 89.57(7) . . O6 Ca1 O4 81.24(8) 1_655 . O8 Ca1 O4 149.52(7) . . O3 Ca1 O4 107.54(7) . . O6 Ca1 O9 148.57(8) 1_655 . O8 Ca1 O9 87.92(7) . . O3 Ca1 O9 68.58(7) . . O4 Ca1 O9 75.82(7) . . O6 Ca1 O7 78.55(8) 1_655 . O8 Ca1 O7 72.84(7) . . O3 Ca1 O7 140.90(7) . . O4 Ca1 O7 78.23(7) . . O9 Ca1 O7 75.97(7) . . O6 Ca1 N1 85.12(8) 1_655 . O8 Ca1 N1 145.29(7) . . O3 Ca1 N1 65.73(7) . . O4 Ca1 N1 64.82(7) . . O9 Ca1 N1 103.78(7) . . O7 Ca1 N1 141.45(7) . . O6 Ca1 O1 71.56(8) 1_655 . O8 Ca1 O1 78.57(7) . . O3 Ca1 O1 73.67(7) . . O4 Ca1 O1 129.86(7) . . O9 Ca1 O1 139.88(7) . . O7 Ca1 O1 132.84(7) . . N1 Ca1 O1 71.47(7) . . O6 Ca1 C20 133.97(8) 1_655 . O8 Ca1 C20 109.99(8) . . O3 Ca1 C20 20.92(8) . . O4 Ca1 C20 87.14(8) . . O9 Ca1 C20 66.37(7) . . O7 Ca1 C20 141.93(7) . . N1 Ca1 C20 50.06(7) . . O1 Ca1 C20 82.98(7) . . O6 Ca1 C19 111.10(8) 1_655 . O8 Ca1 C19 137.05(8) . . O3 Ca1 C19 47.49(8) . . O4 Ca1 C19 65.04(8) . . O9 Ca1 C19 78.21(7) . . O7 Ca1 C19 139.16(8) . . N1 Ca1 C19 26.72(7) . . O1 Ca1 C19 86.37(8) . . C20 Ca1 C19 27.54(8) . . O6 Ca1 C22 71.43(9) 1_655 . O8 Ca1 C22 165.30(8) . . O3 Ca1 C22 103.95(8) . . O4 Ca1 C22 19.40(7) . . O9 Ca1 C22 91.66(7) . . O7 Ca1 C22 92.80(7) . . N1 Ca1 C22 48.75(7) . . O1 Ca1 C22 110.46(7) . . C20 Ca1 C22 83.16(8) . . C19 Ca1 C22 56.86(8) . . C1 O1 Ca1 118.41(17) . . C20 O3 Ca1 116.17(18) . . C22 O4 Ca1 120.66(17) . . C20 O6 Ca1 156.5(2) . 1_455 C21 N1 C19 110.8(2) . . C21 N1 C9 111.6(2) . . C19 N1 C9 107.4(2) . . C21 N1 Ca1 107.81(16) . . C19 N1 Ca1 100.73(16) . . C9 N1 Ca1 117.92(16) . . O1 C1 C2 115.5(2) . . O1 C1 C6 123.0(3) . . C2 C1 C6 121.5(3) . . C1 C2 C3 118.1(3) . . C1 C2 C9 120.5(2) . . C3 C2 C9 121.4(3) . . C4 C3 C2 122.6(3) . . C5 C4 C3 117.1(3) . . C5 C4 C8 121.2(3) . . C3 C4 C8 121.7(3) . . C4 C5 C6 123.3(3) . . C5 C6 C1 117.4(3) . . C5 C6 C7 120.6(3) . . C1 C6 C7 122.0(3) . . N1 C9 C2 114.8(2) . . N1 C19 C20 112.7(2) . . N1 C19 Ca1 52.55(13) . . C20 C19 Ca1 74.25(15) . . O6 C20 O3 125.9(3) . . O6 C20 C19 116.3(3) . . O3 C20 C19 117.8(2) . . O6 C20 Ca1 157.0(2) . . O3 C20 Ca1 42.91(13) . . C19 C20 Ca1 78.21(15) . . N1 C21 C22 112.6(2) . . O4 C22 O5 124.2(3) . . O4 C22 C21 118.5(2) . . O5 C22 C21 117.2(2) . . O4 C22 Ca1 39.94(13) . . O5 C22 Ca1 155.8(2) . . C21 C22 Ca1 81.25(15) . . O15 Ca2 O16 143.54(7) 1_655 . O15 Ca2 O12 128.01(8) 1_655 . O16 Ca2 O12 79.77(8) . . O15 Ca2 O14 128.40(7) 1_655 . O16 Ca2 O14 73.75(7) . . O12 Ca2 O14 79.63(7) . . O15 Ca2 O13 73.35(7) 1_655 . O16 Ca2 O13 142.28(7) . . O12 Ca2 O13 76.65(8) . . O14 Ca2 O13 73.35(7) . . O15 Ca2 O11 74.06(8) 1_655 . O16 Ca2 O11 96.42(7) . . O12 Ca2 O11 73.80(7) . . O14 Ca2 O11 152.97(7) . . O13 Ca2 O11 104.64(8) . . O15 Ca2 O2 72.94(7) 1_655 . O16 Ca2 O2 89.28(8) . . O12 Ca2 O2 154.40(7) . . O14 Ca2 O2 75.09(7) . . O13 Ca2 O2 99.58(7) . . O11 Ca2 O2 130.84(7) . . O15 Ca2 N2 78.23(7) 1_655 . O16 Ca2 N2 66.28(7) . . O12 Ca2 N2 120.33(7) . . O14 Ca2 N2 129.35(7) . . O13 Ca2 N2 151.41(7) . . O11 Ca2 N2 63.71(7) . . O2 Ca2 N2 74.61(7) . . C17 O2 Ca2 120.50(16) . . C24 O11 Ca2 118.78(17) . . C26 O15 Ca2 145.48(19) . 1_455 C26 O16 Ca2 122.02(17) . . C23 N2 C25 109.8(2) . . C23 N2 C18 112.7(2) . . C25 N2 C18 107.6(2) . . C23 N2 Ca2 107.41(15) . . C25 N2 Ca2 105.42(16) . . C18 N2 Ca2 113.61(16) . . C15 C10 C14 117.6(3) . . C15 C10 C11 121.6(3) . . C14 C10 C11 120.8(3) . . C14 C13 C17 118.5(3) . . C14 C13 C12 119.8(3) . . C17 C13 C12 121.8(3) . . C13 C14 C10 122.3(3) . . C10 C15 C16 122.4(3) . . C15 C16 C17 118.1(3) . . C15 C16 C18 120.1(3) . . C17 C16 C18 121.7(2) . . O2 C17 C13 122.8(3) . . O2 C17 C16 116.1(2) . . C13 C17 C16 121.1(3) . . N2 C18 C16 116.2(2) . . N2 C23 C24 111.1(2) . . O11 C24 O10 124.5(3) . . O11 C24 C23 119.3(2) . . O10 C24 C23 116.3(2) . . N2 C25 C26 113.9(2) . . O15 C26 O16 125.1(3) . . O15 C26 C25 116.5(2) . . O16 C26 C25 118.3(2) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Ca1 O6 2.282(2) 1_655 Ca1 O8 2.399(2) . Ca1 O3 2.401(2) . Ca1 O4 2.410(2) . Ca1 O9 2.505(2) . Ca1 O7 2.541(2) . Ca1 N1 2.601(2) . Ca1 O1 2.698(2) . Ca1 C20 3.165(3) . Ca1 C19 3.219(3) . Ca1 C22 3.229(3) . O1 C1 1.375(3) . O3 C20 1.259(4) . O4 C22 1.247(3) . O5 C22 1.249(4) . O6 C20 1.244(3) . N1 C21 1.461(4) . N1 C19 1.473(4) . N1 C9 1.481(4) . C1 C2 1.388(4) . C1 C6 1.396(4) . C2 C3 1.390(4) . C2 C9 1.496(4) . C3 C4 1.386(5) . C4 C5 1.376(5) . C4 C8 1.504(4) . C5 C6 1.390(4) . C6 C7 1.496(5) . C19 C20 1.520(4) . C21 C22 1.512(4) . Ca2 O15 2.352(2) 1_655 Ca2 O16 2.396(2) . Ca2 O12 2.432(2) . Ca2 O14 2.459(2) . Ca2 O13 2.465(2) . Ca2 O11 2.4748(19) . Ca2 O2 2.604(2) . Ca2 N2 2.622(2) . O2 C17 1.378(3) . O10 C24 1.266(3) . O11 C24 1.243(3) . O15 C26 1.241(3) . O16 C26 1.261(3) . N2 C23 1.455(3) . N2 C25 1.472(3) . N2 C18 1.475(3) . C10 C15 1.381(4) . C10 C14 1.387(4) . C10 C11 1.509(4) . C12 C13 1.513(4) . C13 C14 1.383(4) . C13 C17 1.392(4) . C15 C16 1.391(4) . C16 C17 1.394(4) . C16 C18 1.495(4) . C23 C24 1.529(4) . C25 C26 1.501(4) .