#------------------------------------------------------------------------------ #$Date: 2021-12-03 22:05:18 +0200 (Fri, 03 Dec 2021) $ #$Revision: 271011 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/51/91/4519127.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_4519127 loop_ _publ_author_name 'Seal, Nilanjan' 'Neogi, Subhadip' _publ_section_title ; Intrinsic-Unsaturation-Enriched Biporous and Chemorobust Cu(II) Framework for Efficient Catalytic CO2 Fixation and Pore-Fitting Actuated Size-Exclusive Hantzsch Condensation with Mechanistic Validation. ; _journal_issue 46 _journal_name_full 'ACS applied materials & interfaces' _journal_page_first 55123 _journal_page_last 55135 _journal_paper_doi 10.1021/acsami.1c16984 _journal_volume 13 _journal_year 2021 _chemical_formula_moiety 'C20 H25 N O4' _chemical_formula_sum 'C20 H25 N O4' _chemical_formula_weight 343.41 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_date 2021-05-20 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _cell_angle_alpha 90.00 _cell_angle_beta 97.88(6) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 10.116(13) _cell_length_b 7.483(9) _cell_length_c 24.57(4) _cell_measurement_reflns_used 39617 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 34.32 _cell_measurement_theta_min 2.09 _cell_volume 1842(4) _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 150.15 _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.993 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1124 _diffrn_reflns_av_unetI/netI 0.2263 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_number 39617 _diffrn_reflns_theta_full 34.32 _diffrn_reflns_theta_max 34.32 _diffrn_reflns_theta_min 2.09 _diffrn_source 'fine-focus sealed tube' _exptl_absorpt_coefficient_mu 0.086 _exptl_absorpt_correction_T_max 0.9982 _exptl_absorpt_correction_T_min 0.9705 _exptl_crystal_colour 'pale yellow' _exptl_crystal_density_diffrn 1.238 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 736 _exptl_crystal_size_max 0.351 _exptl_crystal_size_mid 0.056 _exptl_crystal_size_min 0.021 _refine_diff_density_max 0.571 _refine_diff_density_min -0.358 _refine_diff_density_rms 0.086 _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 0.930 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 236 _refine_ls_number_reflns 7625 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.930 _refine_ls_R_factor_all 0.3129 _refine_ls_R_factor_gt 0.1033 _refine_ls_shift/su_max 0.0002 _refine_ls_shift/su_mean 0.0001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1640P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2417 _refine_ls_wR_factor_ref 0.3863 _reflns_number_gt 2029 _reflns_number_total 7625 _reflns_threshold_expression >2sigma(I) _iucr_refine_instructions_details ; REM Old TITL Integration of ORGANIC REM SHELXT solution in P2(1)/n REM R1 0.230, Rweak 0.013, Alpha 0.028, Orientation as input REM Formula found by SHELXT: C20 N O4 REM ##### REM NS6109_0m_a.res in P2(1)/n REM R1 = 0.1030 for 2029 Fo > 4sig(Fo) and 0.3126 for all 7625 data REM 235 parameters refined using 0 restraints REM Highest difference peak 0.570, deepest hole -0.357, 1-sigma level 0.085 TITL NS6109_0m_a.res in P2(1)/n CELL 0.71073 10.1164 7.4827 24.5695 90.000 97.881 90.000 ZERR 4.0000 0.0126 0.0085 0.0351 0.000 0.064 0.000 LATT 1 SYMM 0.5-X, 0.5+Y, 0.5-Z SFAC C H N O UNIT 80 100 4 16 MERG 2 FMAP 2 GRID PLAN 20 TEMP -123 SIZE 0.021 0.056 0.351 BOND $H L.S. 4 ACTA WGHT 0.164000 EXTI 0.000000 FVAR 0.41340 O001 4 0.772519 0.071690 0.496166 11.00000 0.04398 0.03113 = 0.05463 -0.00175 0.00162 -0.00052 H1 2 0.702292 0.794290 0.486018 11.00000 0.01863 O002 4 0.923242 0.257906 0.542181 11.00000 0.04330 0.03775 = 0.04831 0.00577 -0.00567 -0.00185 O003 4 0.422514 0.285154 0.361447 11.00000 0.03809 0.05397 = 0.04930 -0.00959 -0.00249 -0.00605 O004 4 0.345790 0.569726 0.357124 11.00000 0.04351 0.05999 = 0.05488 0.00518 -0.00707 0.00662 N005 3 0.687960 0.690101 0.474783 11.00000 0.04342 0.03023 = 0.04637 -0.00346 0.00068 -0.00296 C006 1 0.746548 0.383817 0.480277 11.00000 0.03169 0.03280 = 0.03872 0.00180 0.00680 -0.00175 C007 1 0.732998 0.317455 0.378715 11.00000 0.03331 0.03741 = 0.03446 0.00090 -0.00398 0.00100 C008 1 0.652767 0.347501 0.427697 11.00000 0.03327 0.03162 = 0.03953 -0.00013 0.00043 -0.00458 AFIX 13 H008 2 0.602643 0.235106 0.433046 11.00000 -1.20000 AFIX 0 C009 1 0.765149 0.553297 0.500389 11.00000 0.03892 0.03263 = 0.03637 0.00147 0.00466 -0.00148 C00A 1 0.812083 0.224841 0.506424 11.00000 0.03652 0.03395 = 0.03399 -0.00266 0.00381 0.00005 C00B 1 0.551480 0.497352 0.414890 11.00000 0.03444 0.04137 = 0.03576 0.00324 0.00241 0.00076 C00C 1 0.576676 0.663313 0.436494 11.00000 0.03742 0.03656 = 0.04149 0.00638 0.00909 0.00175 C00D 1 0.429822 0.461571 0.375324 11.00000 0.03614 0.04826 = 0.04246 0.00398 0.00684 -0.00212 C00E 1 0.858852 0.613361 0.550298 11.00000 0.04602 0.03528 = 0.04094 -0.00392 0.00048 -0.00165 AFIX 137 H00A 2 0.950956 0.609486 0.542142 11.00000 -1.50000 H00B 2 0.849785 0.533714 0.581233 11.00000 -1.50000 H00C 2 0.836556 0.735818 0.559874 11.00000 -1.50000 AFIX 0 C00F 1 0.875582 0.269300 0.287172 11.00000 0.03954 0.06453 = 0.04033 -0.00283 0.00225 0.01226 C00G 1 0.819731 0.448236 0.364039 11.00000 0.05347 0.04192 = 0.04591 -0.00345 0.01358 -0.00713 AFIX 43 H00G 2 0.831079 0.555712 0.384735 11.00000 -1.20000 AFIX 0 C00H 1 0.491442 0.827848 0.424555 11.00000 0.04293 0.04181 = 0.05638 0.00181 0.00577 0.00457 AFIX 137 H00D 2 0.473088 0.846180 0.384740 11.00000 -1.50000 H00E 2 0.538756 0.932081 0.441747 11.00000 -1.50000 H00F 2 0.407115 0.812163 0.439421 11.00000 -1.50000 AFIX 0 C00I 1 0.983246 0.108862 0.574200 11.00000 0.04122 0.04045 = 0.05298 0.00506 -0.00409 0.00320 AFIX 23 H00H 2 1.078484 0.134783 0.586820 11.00000 -1.20000 H00I 2 0.978248 0.000088 0.551070 11.00000 -1.20000 AFIX 0 C00J 1 0.721213 0.161058 0.347815 11.00000 0.04406 0.04499 = 0.05820 -0.01165 0.00599 -0.00533 AFIX 43 H00J 2 0.665104 0.067868 0.357526 11.00000 -1.20000 AFIX 0 C00K 1 0.889634 0.424649 0.319926 11.00000 0.04918 0.05591 = 0.05053 0.00256 0.00947 -0.00353 AFIX 43 H00K 2 0.948864 0.515891 0.311467 11.00000 -1.20000 AFIX 0 C00L 1 0.790243 0.138255 0.302777 11.00000 0.04923 0.05040 = 0.05404 -0.01633 0.01064 0.00304 AFIX 43 H00L 2 0.778711 0.030503 0.282226 11.00000 -1.20000 AFIX 0 C00M 1 0.948736 0.245632 0.237495 11.00000 0.05743 0.07840 = 0.04999 0.00000 0.00950 0.01089 AFIX 137 H00M 2 0.883722 0.238368 0.204110 11.00000 -1.50000 H00N 2 1.001534 0.135452 0.241605 11.00000 -1.50000 H00O 2 1.008056 0.347837 0.234783 11.00000 -1.50000 AFIX 0 C00N 1 0.317860 0.232297 0.318172 11.00000 0.04377 0.07463 = 0.05349 0.00020 -0.00881 -0.01245 AFIX 23 H00P 2 0.235667 0.300209 0.322018 11.00000 -1.20000 H00Q 2 0.298266 0.103708 0.322170 11.00000 -1.20000 AFIX 0 C00O 1 0.355681 0.264674 0.262285 11.00000 0.05955 0.08978 = 0.04827 -0.01054 0.00071 -0.01132 AFIX 137 H00R 2 0.289711 0.208638 0.234565 11.00000 -1.50000 H00S 2 0.443878 0.213040 0.260214 11.00000 -1.50000 H00T 2 0.358249 0.393569 0.255438 11.00000 -1.50000 AFIX 0 C00P 1 0.911407 0.077222 0.623087 11.00000 0.07749 0.06618 = 0.06155 0.01365 0.00665 0.01644 AFIX 137 H00U 2 0.817142 0.051878 0.610470 11.00000 -1.50000 H00V 2 0.918560 0.183981 0.646410 11.00000 -1.50000 H00W 2 0.951755 -0.024789 0.644205 11.00000 -1.50000 HKLF 4 REM NS6109_0m_a.res in P2(1)/n REM R1 = 0.1033 for 2029 Fo > 4sig(Fo) and 0.3129 for all 7625 data REM 236 parameters refined using 0 restraints END WGHT 0.1626 0.0000 REM Highest difference peak 0.571, deepest hole -0.358, 1-sigma level 0.086 Q1 1 0.3511 0.1255 0.2833 11.00000 0.05 0.46 Q2 1 0.7792 0.4400 0.4847 11.00000 0.05 0.42 Q3 1 0.7025 0.3383 0.4081 11.00000 0.05 0.33 Q4 1 0.8853 0.1196 0.2116 11.00000 0.05 0.30 Q5 1 0.7997 -0.1808 0.3340 11.00000 0.05 0.28 Q6 1 0.9549 0.4235 0.5631 11.00000 0.05 0.28 Q7 1 0.2789 0.7981 0.4400 11.00000 0.05 0.28 Q8 1 0.5377 0.9597 0.3663 11.00000 0.05 0.27 Q9 1 0.2995 0.2227 0.2010 11.00000 0.05 0.27 Q10 1 0.7950 0.0057 0.3668 11.00000 0.05 0.26 Q11 1 0.8198 0.2750 0.1940 11.00000 0.05 0.25 Q12 1 0.1534 0.1115 0.2947 11.00000 0.05 0.25 Q13 1 1.0799 0.1789 0.6264 11.00000 0.05 0.25 Q14 1 0.2394 0.4034 0.2950 11.00000 0.05 0.25 Q15 1 0.9163 0.5267 0.3972 11.00000 0.05 0.25 Q16 1 0.8548 0.2314 0.5938 11.00000 0.05 0.25 Q17 1 1.0074 0.4438 0.3414 11.00000 0.05 0.25 Q18 1 0.9321 0.3521 0.2176 11.00000 0.05 0.24 Q19 1 1.0566 0.2025 0.2427 11.00000 0.05 0.24 Q20 1 0.8679 -0.1160 0.5008 11.00000 0.05 0.23 ; _cod_data_source_file am1c16984_si_007.cif _cod_data_source_block 7b _cod_database_code 4519127 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2.a Ternary CH refined with riding coordinates: C008(H008) 2.b Secondary CH2 refined with riding coordinates: C00I(H00H,H00I), C00N(H00P,H00Q) 2.c Aromatic/amide H refined with riding coordinates: C00G(H00G), C00J(H00J), C00K(H00K), C00L(H00L) 2.d Idealised Me refined as rotating group: C00E(H00A,H00B,H00C), C00H(H00D,H00E,H00F), C00M(H00M,H00N,H00O), C00O(H00R, H00S,H00T), C00P(H00U,H00V,H00W) ; _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x+1/2, y+1/2, -z+1/2' 3 '-x, -y, -z' 4 'x-1/2, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_refinement_flags_posn O001 O 0.7725(2) 0.0717(3) 0.49617(12) 0.0437(7) Uani 1 d . . . H1 H 0.702(3) 0.794(4) 0.4860(13) 0.019(8) Uiso 1 d . . . O002 O 0.9232(3) 0.2579(3) 0.54218(12) 0.0442(7) Uani 1 d . . . O003 O 0.4225(2) 0.2852(4) 0.36145(12) 0.0479(7) Uani 1 d . . . O004 O 0.3458(3) 0.5697(4) 0.35712(12) 0.0541(8) Uani 1 d . . . N005 N 0.6880(3) 0.6901(4) 0.47478(14) 0.0405(8) Uani 1 d . . . C006 C 0.7465(3) 0.3838(4) 0.48028(15) 0.0342(8) Uani 1 d . . . C007 C 0.7330(3) 0.3175(5) 0.37871(15) 0.0359(8) Uani 1 d . . . C008 C 0.6528(3) 0.3475(4) 0.42770(15) 0.0352(8) Uani 1 d . . . H008 H 0.6026 0.2351 0.4330 0.042 Uiso 1 calc . . R C009 C 0.7651(3) 0.5533(5) 0.50039(16) 0.0360(8) Uani 1 d . . . C00A C 0.8121(4) 0.2248(5) 0.50642(16) 0.0349(8) Uani 1 d . . . C00B C 0.5515(3) 0.4974(5) 0.41489(16) 0.0374(9) Uani 1 d . . . C00C C 0.5767(4) 0.6633(5) 0.43649(16) 0.0382(9) Uani 1 d . . . C00D C 0.4298(4) 0.4616(5) 0.37532(17) 0.0422(9) Uani 1 d . . . C00E C 0.8589(4) 0.6134(5) 0.55030(16) 0.0413(9) Uani 1 d . . . H00A H 0.9510 0.6095 0.5421 0.062 Uiso 1 calc . . GR H00B H 0.8498 0.5337 0.5812 0.062 Uiso 1 calc . . GR H00C H 0.8366 0.7358 0.5599 0.062 Uiso 1 calc . . GR C00F C 0.8756(4) 0.2693(6) 0.28717(17) 0.0484(11) Uani 1 d . . . C00G C 0.8197(4) 0.4482(5) 0.36404(17) 0.0465(10) Uani 1 d . . . H00G H 0.8311 0.5557 0.3847 0.056 Uiso 1 calc . . R C00H C 0.4914(4) 0.8278(5) 0.42455(19) 0.0471(10) Uani 1 d . . . H00D H 0.4731 0.8462 0.3847 0.071 Uiso 1 calc . . GR H00E H 0.5388 0.9321 0.4417 0.071 Uiso 1 calc . . GR H00F H 0.4071 0.8122 0.4394 0.071 Uiso 1 calc . . GR C00I C 0.9832(4) 0.1089(5) 0.57420(18) 0.0459(10) Uani 1 d . . . H00H H 1.0785 0.1348 0.5868 0.055 Uiso 1 calc . . R H00I H 0.9782 0.0001 0.5511 0.055 Uiso 1 calc . . R C00J C 0.7212(4) 0.1611(5) 0.34782(18) 0.0492(10) Uani 1 d . . . H00J H 0.6651 0.0679 0.3575 0.059 Uiso 1 calc . . R C00K C 0.8896(4) 0.4246(6) 0.31993(18) 0.0516(11) Uani 1 d . . . H00K H 0.9489 0.5159 0.3115 0.062 Uiso 1 calc . . R C00L C 0.7902(4) 0.1383(6) 0.30278(18) 0.0509(11) Uani 1 d . . . H00L H 0.7787 0.0305 0.2822 0.061 Uiso 1 calc . . R C00M C 0.9487(5) 0.2456(6) 0.23749(19) 0.0617(13) Uani 1 d . . . H00M H 0.8837 0.2384 0.2041 0.093 Uiso 1 calc . . GR H00N H 1.0015 0.1355 0.2416 0.093 Uiso 1 calc . . GR H00O H 1.0081 0.3478 0.2348 0.093 Uiso 1 calc . . GR C00N C 0.3179(4) 0.2323(6) 0.31817(19) 0.0587(12) Uani 1 d . . . H00P H 0.2357 0.3002 0.3220 0.070 Uiso 1 calc . . R H00Q H 0.2983 0.1037 0.3222 0.070 Uiso 1 calc . . R C00O C 0.3557(5) 0.2647(7) 0.2623(2) 0.0665(14) Uani 1 d . . . H00R H 0.2897 0.2086 0.2346 0.100 Uiso 1 calc . . GR H00S H 0.4439 0.2130 0.2602 0.100 Uiso 1 calc . . GR H00T H 0.3582 0.3936 0.2554 0.100 Uiso 1 calc . . GR C00P C 0.9114(5) 0.0772(6) 0.6231(2) 0.0687(14) Uani 1 d . . . H00U H 0.8171 0.0519 0.6105 0.103 Uiso 1 calc . . GR H00V H 0.9186 0.1840 0.6464 0.103 Uiso 1 calc . . GR H00W H 0.9518 -0.0248 0.6442 0.103 Uiso 1 calc . . GR 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 O001 0.0440(14) 0.0311(13) 0.0546(18) -0.0018(12) 0.0016(13) -0.0005(11) O002 0.0433(15) 0.0377(14) 0.0483(18) 0.0058(12) -0.0057(13) -0.0018(11) O003 0.0381(14) 0.0540(17) 0.0493(18) -0.0096(14) -0.0025(13) -0.0061(12) O004 0.0435(15) 0.0600(18) 0.055(2) 0.0052(15) -0.0071(14) 0.0066(14) N005 0.0434(18) 0.0302(16) 0.046(2) -0.0035(15) 0.0007(15) -0.0030(14) C006 0.0317(18) 0.0328(18) 0.039(2) 0.0018(16) 0.0068(15) -0.0017(14) C007 0.0333(18) 0.0374(18) 0.034(2) 0.0009(16) -0.0040(15) 0.0010(15) C008 0.0333(18) 0.0316(17) 0.040(2) -0.0001(16) 0.0004(15) -0.0046(14) C009 0.0389(19) 0.0326(18) 0.036(2) 0.0015(16) 0.0047(16) -0.0015(15) C00A 0.0365(19) 0.0340(19) 0.034(2) -0.0027(15) 0.0038(16) 0.0001(15) C00B 0.0344(19) 0.041(2) 0.036(2) 0.0032(17) 0.0024(16) 0.0008(16) C00C 0.0374(19) 0.0366(19) 0.041(2) 0.0064(17) 0.0091(17) 0.0017(16) C00D 0.036(2) 0.048(2) 0.042(2) 0.0040(19) 0.0068(18) -0.0021(17) C00E 0.046(2) 0.0353(19) 0.041(2) -0.0039(17) 0.0005(17) -0.0017(16) C00F 0.040(2) 0.065(3) 0.040(2) -0.003(2) 0.0022(18) 0.0123(19) C00G 0.053(2) 0.042(2) 0.046(3) -0.0034(19) 0.014(2) -0.0071(18) C00H 0.043(2) 0.042(2) 0.056(3) 0.002(2) 0.0058(19) 0.0046(17) C00I 0.041(2) 0.040(2) 0.053(3) 0.0051(19) -0.0041(19) 0.0032(17) C00J 0.044(2) 0.045(2) 0.058(3) -0.012(2) 0.006(2) -0.0053(18) C00K 0.049(2) 0.056(3) 0.051(3) 0.003(2) 0.009(2) -0.004(2) C00L 0.049(2) 0.050(2) 0.054(3) -0.016(2) 0.011(2) 0.0030(19) C00M 0.057(3) 0.078(3) 0.050(3) 0.000(2) 0.010(2) 0.011(2) C00N 0.044(2) 0.075(3) 0.053(3) 0.000(2) -0.009(2) -0.012(2) C00O 0.060(3) 0.090(4) 0.048(3) -0.011(3) 0.001(2) -0.011(3) C00P 0.077(3) 0.066(3) 0.062(3) 0.014(3) 0.007(3) 0.016(3) 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' 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 C00A O002 C00I 117.5(3) . . ? C00D O003 C00N 117.2(3) . . ? C009 N005 H1 119(2) . . ? C00C N005 H1 117(2) . . ? C00C N005 C009 124.0(3) . . ? C009 C006 C008 120.9(3) . . ? C009 C006 C00A 124.3(4) . . ? C00A C006 C008 114.8(3) . . ? C00G C007 C008 120.8(3) . . ? C00J C007 C008 121.9(3) . . ? C00J C007 C00G 117.3(4) . . ? C006 C008 C007 110.6(3) . . ? C006 C008 H008 107.9 . . ? C006 C008 C00B 111.6(3) . . ? C007 C008 H008 107.9 . . ? C00B C008 C007 110.7(3) . . ? C00B C008 H008 107.9 . . ? N005 C009 C00E 113.6(3) . . ? C006 C009 N005 118.8(4) . . ? C006 C009 C00E 127.6(3) . . ? O001 C00A O002 121.5(3) . . ? O001 C00A C006 123.5(3) . . ? O002 C00A C006 115.0(3) . . ? C00C C00B C008 120.4(3) . . ? C00C C00B C00D 120.9(3) . . ? C00D C00B C008 118.5(3) . . ? N005 C00C C00H 113.9(3) . . ? C00B C00C N005 119.4(3) . . ? C00B C00C C00H 126.7(4) . . ? O003 C00D C00B 110.5(3) . . ? O004 C00D O003 122.8(4) . . ? O004 C00D C00B 126.7(4) . . ? C009 C00E H00A 109.5 . . ? C009 C00E H00B 109.5 . . ? C009 C00E H00C 109.5 . . ? H00A C00E H00B 109.5 . . ? H00A C00E H00C 109.5 . . ? H00B C00E H00C 109.5 . . ? C00K C00F C00M 122.1(4) . . ? C00L C00F C00K 116.1(4) . . ? C00L C00F C00M 121.7(4) . . ? C007 C00G H00G 119.3 . . ? C00K C00G C007 121.3(4) . . ? C00K C00G H00G 119.3 . . ? C00C C00H H00D 109.5 . . ? C00C C00H H00E 109.5 . . ? C00C C00H H00F 109.5 . . ? H00D C00H H00E 109.5 . . ? H00D C00H H00F 109.5 . . ? H00E C00H H00F 109.5 . . ? O002 C00I H00H 109.7 . . ? O002 C00I H00I 109.7 . . ? O002 C00I C00P 110.0(3) . . ? H00H C00I H00I 108.2 . . ? C00P C00I H00H 109.7 . . ? C00P C00I H00I 109.7 . . ? C007 C00J H00J 119.3 . . ? C007 C00J C00L 121.3(4) . . ? C00L C00J H00J 119.3 . . ? C00F C00K H00K 119.0 . . ? C00G C00K C00F 122.0(4) . . ? C00G C00K H00K 119.0 . . ? C00F C00L C00J 121.8(4) . . ? C00F C00L H00L 119.1 . . ? C00J C00L H00L 119.1 . . ? C00F C00M H00M 109.5 . . ? C00F C00M H00N 109.5 . . ? C00F C00M H00O 109.5 . . ? H00M C00M H00N 109.5 . . ? H00M C00M H00O 109.5 . . ? H00N C00M H00O 109.5 . . ? O003 C00N H00P 109.2 . . ? O003 C00N H00Q 109.2 . . ? O003 C00N C00O 112.1(4) . . ? H00P C00N H00Q 107.9 . . ? C00O C00N H00P 109.2 . . ? C00O C00N H00Q 109.2 . . ? C00N C00O H00R 109.5 . . ? C00N C00O H00S 109.5 . . ? C00N C00O H00T 109.5 . . ? H00R C00O H00S 109.5 . . ? H00R C00O H00T 109.5 . . ? H00S C00O H00T 109.5 . . ? C00I C00P H00U 109.5 . . ? C00I C00P H00V 109.5 . . ? C00I C00P H00W 109.5 . . ? H00U C00P H00V 109.5 . . ? H00U C00P H00W 109.5 . . ? H00V C00P H00W 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 O001 C00A 1.229(4) . ? O002 C00A 1.352(5) . ? O002 C00I 1.449(4) . ? O003 C00D 1.363(5) . ? O003 C00N 1.449(5) . ? O004 C00D 1.214(4) . ? N005 H1 0.83(3) . ? N005 C009 1.385(5) . ? N005 C00C 1.379(5) . ? C006 C008 1.519(5) . ? C006 C009 1.365(5) . ? C006 C00A 1.466(5) . ? C007 C008 1.557(5) . ? C007 C00G 1.394(5) . ? C007 C00J 1.391(5) . ? C008 H008 1.0000 . ? C008 C00B 1.522(5) . ? C009 C00E 1.512(5) . ? C00B C00C 1.361(5) . ? C00B C00D 1.484(5) . ? C00C C00H 1.509(5) . ? C00E H00A 0.9800 . ? C00E H00B 0.9800 . ? C00E H00C 0.9800 . ? C00F C00K 1.410(6) . ? C00F C00L 1.394(6) . ? C00F C00M 1.522(6) . ? C00G H00G 0.9500 . ? C00G C00K 1.384(6) . ? C00H H00D 0.9800 . ? C00H H00E 0.9800 . ? C00H H00F 0.9800 . ? C00I H00H 0.9900 . ? C00I H00I 0.9900 . ? C00I C00P 1.505(6) . ? C00J H00J 0.9500 . ? C00J C00L 1.398(6) . ? C00K H00K 0.9500 . ? C00L H00L 0.9500 . ? C00M H00M 0.9800 . ? C00M H00N 0.9800 . ? C00M H00O 0.9800 . ? C00N H00P 0.9900 . ? C00N H00Q 0.9900 . ? C00N C00O 1.495(6) . ? C00O H00R 0.9800 . ? C00O H00S 0.9800 . ? C00O H00T 0.9800 . ? C00P H00U 0.9800 . ? C00P H00V 0.9800 . ? C00P H00W 0.9800 . ? loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_squared_meas _refln_F_squared_sigma 2 0 0 585.09 13.32 -2 0 0 585.38 18.1 -2 0 0 556.02 16.47 -2 0 0 575.22 15.79 -2 0 0 581.18 21.52 2 0 0 584.42 18.97 2 0 0 581.09 17.43 2 0 0 556.49 27.08 2 0 0 569.79 19.64 -3 0 0 -3.65 1.31 3 0 0 -2.63 1.6 -3 0 0 1.23 1.27 -3 0 0 -0.37 0.85 -3 0 0 -2.36 2.15 3 0 0 2.01 1.34 3 0 0 0.77 1.46 3 0 0 2.37 2.29 3 0 0 -1.79 0.8 -4 0 0 -0.8 1.64 4 0 0 -0.59 1.06 4 0 0 -1.58 2.04 4 0 0 0.09 2.01 -4 0 0 0.74 1.12 -4 0 0 0.43 1.06 -4 0 0 3.67 3.73 4 0 0 2.11 1.49 -5 0 0 1.05 1.72 5 0 0 -1.49 1.46 -5 0 0 0.76 1.12 -5 0 0 1.2 3.35 -5 0 0 -0.49 2.06 5 0 0 1.65 1.24 -6 0 0 64.16 15.79 6 0 0 85.63 14.22 -6 0 0 93.54 11.03 -6 0 0 94.52 11.97 -6 0 0 88.14 8.37 6 0 0 84.88 8.88 -7 0 0 4.04 2.1 -7 0 0 5.05 4.31 7 0 0 3.13 2.24 7 0 0 3.01 3.18 -7 0 0 4.71 5.94 8 0 0 37.32 10.97 -8 0 0 21.09 10.37 -8 0 0 45.85 9.65 -8 0 0 30 5.69 -9 0 0 -2.45 2.85 9 0 0 0.9 4.94 -9 0 0 0.07 2.91 10 0 0 10.64 8.55 -10 0 0 11.42 8.54 -10 0 0 9.29 4.75 11 0 0 0.25 4.53 -11 0 0 -1.94 4.34 -12 0 0 10.63 8.2 12 0 0 26.98 12.18 -12 0 0 18.45 7.25 13 0 0 -0.56 7.49 -13 0 0 0.57 7.21 -13 0 0 -10.1 5.31 -14 0 0 -1.14 11.45 0 -1 0 0.79 0.72 0 -1 0 0.09 1.05 0 -1 0 0.13 0.72 0 -1 0 1.55 1.14 0 -1 0 1.11 0.49 0 1 0 0.85 1.23 0 1 0 2 0.92 0 1 0 -0.73 0.81 0 1 0 -0.55 0.49 1 -1 0 735.13 28.88 -1 -1 0 711.91 21.18 -1 -1 0 693.68 23.43 1 -1 0 733.04 26.16 -1 -1 0 728.74 12.44 1 -1 0 738.6 19.34 -1 -1 0 730.75 20.96 -1 1 0 735.69 29.51 1 1 0 712.54 23.36 -1 1 0 701.22 26.78 -1 1 0 708.76 19.02 1 1 0 709.8 20.62 1 1 0 707.45 20.35 1 1 0 717.05 12.48 -2 -1 0 2667.47 52.77 2 -1 0 2767.37 43.47 -2 -1 0 2711.04 49.14 2 -1 0 2635.54 65.96 -2 -1 0 2754.02 60.49 2 1 0 2836.68 52.35 2 1 0 2889.24 62.13 -2 1 0 2815.34 44.08 -2 1 0 2753.65 60.49 -2 1 0 2825.34 71.21 2 1 0 2835.47 60.28 3 -1 0 4.74 2.11 3 -1 0 1.04 1.76 3 -1 0 3.67 3.39 3 -1 0 2.01 0.96 -3 -1 0 4.42 2.6 -3 -1 0 -2.61 1.78 3 -1 0 2.57 1.24 -3 -1 0 7.56 3.82 -3 1 0 0.49 1.33 3 1 0 3.48 1.85 -3 1 0 2.66 2.65 3 1 0 2.38 2.36 -3 1 0 3.23 2.87 3 1 0 1.09 2.75 -4 -1 0 206.62 18.47 4 -1 0 196.42 13.08 4 -1 0 183.43 17.18 4 -1 0 187.03 11.84 4 -1 0 165.19 12.22 -4 -1 0 183.66 15.74 4 1 0 193.17 6.11 -4 1 0 177.74 20.23 -4 1 0 190.56 10.75 -4 1 0 209.22 14.13 -4 1 0 186.88 23.19 -4 1 0 195.35 7.79 4 1 0 171.58 16.73 -5 -1 0 3.37 2.85 5 -1 0 2.86 2.2 -5 -1 0 -0.83 2.06 -5 1 0 -1.42 1.18 -5 1 0 2.44 2.75 5 1 0 0.97 0.97 -5 1 0 0.8 1.19 -5 1 0 3.36 1.87 5 1 0 -0.73 2.44 6 -1 0 102.64 12.72 -6 -1 0 132.33 15.47 6 1 0 113.64 6.87 -6 1 0 120.29 8.95 -6 1 0 115.52 9.74 -6 1 0 130.33 12.75 6 1 0 83.45 14.33 -6 1 0 71.15 14.73 7 -1 0 55.11 11.29 -7 -1 0 71.05 12.71 -7 -1 0 53.12 13.5 -7 1 0 77.47 7.81 -7 1 0 81.25 9.09 -7 1 0 56.37 9.15 -7 1 0 59.62 15.35 7 1 0 56.17 13.19 -8 -1 0 20.15 10.06 -8 -1 0 40.83 9.76 8 -1 0 30.5 9.02 -8 1 0 31.77 7.99 -8 1 0 25.8 9.54 8 1 0 43.67 12.15 -8 1 0 32.31 6.27 -8 1 0 44.44 6.68 9 -1 0 14.96 6.39 -9 -1 0 6.29 7.34 -9 -1 0 17.71 6.72 -9 1 0 22.78 4.52 -9 1 0 13.86 4.96 -9 1 0 19.08 5.08 -9 1 0 1.28 5.05 9 1 0 18.75 8.07 10 -1 0 66.62 15.66 -10 -1 0 23.58 10.42 -10 -1 0 52.49 11.68 -10 1 0 38.04 13.41 10 1 0 72.37 18.35 -10 1 0 54.53 9.55 -11 -1 0 7.73 5.87 11 -1 0 -7.42 4.7 -11 -1 0 0.95 11.81 -11 1 0 3.68 6.33 11 1 0 6.96 6.61 12 -1 0 18.89 9.04 -12 -1 0 12.78 7.8 -12 -1 0 6.59 8.69 12 1 0 20.3 9.15 -12 1 0 3.55 8.33 -13 -1 0 5.05 8.31 -13 -1 0 13.9 10.48 13 -1 0 10.84 9.42 -13 1 0 15.72 7.52 13 1 0 14.44 11.3 -14 -1 0 -2.7 10.59 -14 -1 0 16.3 9.93 -14 1 0 -1.05 11.72 -15 -1 0 -10.52 10.77 -15 1 0 -16.03 10.71 0 -2 0 872.14 32.47 0 -2 0 903.08 22.21 0 -2 0 891.27 39.22 0 -2 0 883.36 23.37 0 2 0 875.08 32.4 0 2 0 866.55 24.99 0 2 0 847.55 37.19 1 -2 0 309.47 18.44 1 -2 0 305.37 15.97 -1 -2 0 299.53 16.68 1 -2 0 319.95 23.09 1 -2 0 304.8 28.35 -1 -2 0 283.48 16.33 -1 -2 0 311.81 20.46 -1 -2 0 286.76 12.47 1 2 0 273.18 19.06 -1 2 0 323.21 24.89 1 2 0 300.65 12.92 1 2 0 310.94 16.52 -1 2 0 314.69 24.8 -1 2 0 311.89 16.37 2 -2 0 4.53 2.96 -2 -2 0 7.37 2.06 -2 -2 0 4.24 2.88 -2 -2 0 4.08 3.63 2 -2 0 6.39 2.83 2 -2 0 9.48 3.02 -2 -2 0 7.8 3.2 2 2 0 4.83 2.99 2 2 0 7.54 3.28 2 2 0 7.57 1.67 2 2 0 16.33 6.2 -2 2 0 7.3 2.8 -2 2 0 9.33 4.37 -2 2 0 7.04 4.11 -3 -2 0 8.94 4.22 -3 -2 0 11.95 5.21 -3 2 0 7.1 3.25 3 2 0 11.11 4.74 -3 2 0 2.64 3.44 3 2 0 9.81 1.57 -3 2 0 2.76 3.26 4 -2 0 70.73 5.03 4 -2 0 90.25 6.25 -4 -2 0 56.99 10.65 -4 -2 0 58.68 12.66 -4 2 0 59.6 9.54 -4 2 0 45.17 10.92 -4 2 0 52.74 11.32 4 2 0 68.28 12.32 -5 -2 0 206.64 25.21 5 -2 0 227.82 12.83 5 -2 0 257.76 14.78 -5 -2 0 257.45 22.57 -5 2 0 259.29 28.97 -5 2 0 242.46 32.52 5 2 0 252.94 23.87 -5 2 0 260.14 19.81 -6 -2 0 -0.41 2.04 -6 -2 0 -3.26 2.79 -6 2 0 -0.16 2.8 -6 2 0 2.59 3.48 -6 2 0 -4.15 1.83 7 -2 0 2.79 4.24 -7 -2 0 -1.29 4.87 -7 -2 0 2.39 4.8 7 2 0 16.76 6.81 -7 2 0 1.84 4.73 -7 2 0 6.52 3.72 8 -2 0 30.22 8.66 -8 -2 0 20.82 7.97 -8 -2 0 17.48 7.36 -8 2 0 30.36 12.03 -8 2 0 34.47 8.22 8 2 0 8.75 5.83 -9 -2 0 30.49 10 9 -2 0 29.87 7.29 -9 -2 0 22.49 6.87 -9 2 0 19.28 6.78 -9 2 0 24.23 11.62 9 2 0 10.79 9.07 -10 -2 0 4.28 4.19 10 -2 0 14.88 8.1 -10 -2 0 17 8.32 10 2 0 11 8.39 -10 2 0 9.52 4.26 -10 2 0 7.03 5.79 11 -2 0 -4.25 6.45 -11 -2 0 18.48 15.7 -11 -2 0 6.11 6.29 -11 2 0 1.92 3.55 -11 2 0 13.12 5.87 11 2 0 5.31 8.15 12 -2 0 -10.22 5.44 -12 -2 0 2.43 5.4 -12 -2 0 3.67 11.95 -12 2 0 0.05 8.67 -13 -2 0 5.88 15.21 13 -2 0 0.14 6.94 -13 -2 0 2.3 6.9 -13 2 0 2.1 8.37 -14 -2 0 1.58 9.87 -14 -2 0 16.95 10.32 -14 2 0 -6.29 9.4 -15 -2 0 0.53 13.18 -15 -2 0 8.53 9.95 -15 2 0 1.13 11.19 0 -3 0 2.17 1.24 0 -3 0 2.05 4.13 0 -3 0 1.25 1 0 3 0 0.76 1.46 0 3 0 1.82 1.9 1 -3 0 0.78 2.55 -1 -3 0 1.41 2.53 -1 -3 0 0.61 1.69 1 -3 0 0.07 1.86 -1 -3 0 -0.12 1.5 1 -3 0 0.36 1.2 1 3 0 -0.54 1.81 -1 3 0 0.6 1.33 1 3 0 -0.14 1.29 -1 3 0 -0.79 1.09 -1 3 0 -0.67 2.63 2 -3 0 584.99 30.93 -2 -3 0 525.96 28.09 -2 -3 0 548.62 34.77 -2 -3 0 592.55 20.73 -2 3 0 580.62 28.68 -2 3 0 564.51 42.21 2 3 0 579.14 20.96 -2 3 0 666.38 46.19 -3 -3 0 241.64 21.01 -3 -3 0 258.68 24.65 3 3 0 223.22 19.61 -3 3 0 262.51 20.13 3 3 0 253.54 12.04 -3 3 0 252.99 29.02 -4 -3 0 12.68 5.55 -4 -3 0 19.29 7.54 4 3 0 6 3.61 -4 3 0 10.12 6.68 -4 3 0 6.74 4.3 4 3 0 9.34 1.97 -4 3 0 11.71 4.85 5 -3 0 3.59 1.69 5 -3 0 7.15 1.76 -5 -3 0 8.37 4.61 -5 -3 0 -2.54 2.97 5 3 0 1.89 3.99 -5 3 0 3.67 2.84 -5 3 0 -1.36 3.48 -5 3 0 8.28 6.03 -6 -3 0 26.62 8.61 6 -3 0 14.07 3.63 6 -3 0 8.33 3.54 -6 -3 0 21.06 9.25 -6 3 0 8.3 5.92 6 3 0 24.29 8.98 -6 3 0 8.35 6 -6 3 0 25.02 7.41 -7 -3 0 34.16 11.07 7 -3 0 20.32 6.23 -7 -3 0 15.88 7.51 -7 3 0 3.19 5.76 7 3 0 15.13 7.59 -7 3 0 18.57 7.03 -7 3 0 6.31 4.8 8 -3 0 25.68 6.56 -8 -3 0 22.72 9.13 -8 -3 0 25.26 10.98 -8 3 0 23.69 7.31 8 3 0 21.99 8.27 -8 3 0 46.92 15.7 -8 3 0 7.67 7.47 -9 -3 0 -0.92 3.25 -9 -3 0 4.08 6.38 9 -3 0 -0.27 3.82 9 3 0 -2.22 4.5 -9 3 0 1.65 3.61 -10 -3 0 17.59 9.69 -10 -3 0 5.69 16.74 -10 3 0 10.85 6.64 10 3 0 16.26 9.64 -10 3 0 20.46 9.05 -11 -3 0 9.16 6.71 11 -3 0 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