#------------------------------------------------------------------------------ #$Date: 2021-11-03 23:19:28 +0200 (Wed, 03 Nov 2021) $ #$Revision: 270259 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/51/91/4519119.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_4519119 loop_ _publ_author_name 'Mondal, Surajit' 'Dey, Swapan' _publ_section_title ; Strategy to Design a Flexible and Macromolecular Sensor to Bind Cd2+ Ions: A Complete Photophysical Analysis and Bio-Imaging Study. ; _journal_issue 42 _journal_name_full 'ACS omega' _journal_page_first 27936 _journal_page_last 27945 _journal_paper_doi 10.1021/acsomega.1c03793 _journal_volume 6 _journal_year 2021 _chemical_formula_moiety 'C27 H31 N5 O4' _chemical_formula_sum 'C27 H31 N5 O4' _chemical_formula_weight 489.57 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2018-09-08 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _cell_angle_alpha 90 _cell_angle_beta 103.29(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 19.517(4) _cell_length_b 14.714(8) _cell_length_c 9.4101(19) _cell_measurement_reflns_used 1378 _cell_measurement_temperature 293.0(2) _cell_measurement_theta_max 27.7420 _cell_measurement_theta_min 2.5510 _cell_volume 2630.0(16) _computing_cell_refinement 'CrysAlisPro 1.171.39.7f (Rigaku OD, 2015)' _computing_data_collection 'CrysAlisPro 1.171.39.7f (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.39.7f (Rigaku OD, 2015)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_temperature 293.0(2) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 8.0303 _diffrn_detector_type EosS2 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames -------------------------------------------------------------------------- 1 \w 17.00 51.00 1.00 250.00 -- 13.76 -99.00 0.00 34 2 \w -20.00 16.00 1.00 250.00 -- 13.76 -99.00 30.00 36 3 \w -30.00 50.00 1.00 250.00 -- -15.95 57.00 -90.00 80 4 \w -82.00 -11.00 1.00 250.00 -- -15.95 -77.00 120.00 71 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Single source at offset/far, EosS2' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0029903000 _diffrn_orient_matrix_UB_12 -0.0293426000 _diffrn_orient_matrix_UB_13 0.0580672000 _diffrn_orient_matrix_UB_21 0.0095910000 _diffrn_orient_matrix_UB_22 0.0362336000 _diffrn_orient_matrix_UB_23 0.0502972000 _diffrn_orient_matrix_UB_31 -0.0359937000 _diffrn_orient_matrix_UB_32 0.0120927000 _diffrn_orient_matrix_UB_33 -0.0098667000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0689 _diffrn_reflns_av_unetI/netI 0.1306 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_number 11335 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 24.998 _diffrn_reflns_theta_max 24.998 _diffrn_reflns_theta_min 2.144 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 0.085 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.34227 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.7f (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'clear dark red' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier dark _exptl_crystal_colour_primary red _exptl_crystal_density_diffrn 1.236 _exptl_crystal_description block _exptl_crystal_F_000 1040 _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.2 _refine_diff_density_max 0.170 _refine_diff_density_min -0.186 _refine_diff_density_rms 0.037 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.944 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 329 _refine_ls_number_reflns 4619 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.944 _refine_ls_R_factor_all 0.1829 _refine_ls_R_factor_gt 0.0610 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0401P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1034 _refine_ls_wR_factor_ref 0.1429 _reflns_Friedel_coverage 0.000 _reflns_number_gt 1905 _reflns_number_total 4619 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; sm_138.res created by SHELXL-2014/7 TITL sm_138_a.res in P2(1)/c REM Old TITL SM_138 in P2(1)/c REM SHELXT solution in P2(1)/c REM R1 0.228, Rweak 0.093, Alpha 0.049, Orientation as input REM Formula found by SHELXT: C29 N3 O4 CELL 0.71073 19.5168 14.7143 9.4101 90 103.294 90 ZERR 4 0.0035 0.0077 0.0019 0 0.02 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H N O UNIT 108 124 20 16 L.S. 10 PLAN 10 SIZE 0.2 0.22 0.26 TEMP 19.9(2) BOND $H list 4 fmap 2 53 acta OMIT -2 50 OMIT -25 7 2 OMIT -5 13 10 OMIT -22 11 5 OMIT -23 10 4 OMIT 3 0 0 OMIT 2 1 0 REM REM REM WGHT 0.040100 FVAR 0.44571 O001 4 0.579467 0.417877 0.744097 11.00000 0.04591 0.08760 = 0.05571 -0.01376 0.00880 -0.01295 O002 4 0.251827 0.454995 1.034882 11.00000 0.05604 0.06141 = 0.07587 0.00154 0.01809 0.01024 O003 4 0.538012 0.412712 0.942577 11.00000 0.05839 0.12364 = 0.05420 -0.02191 0.00689 -0.01302 N004 3 0.403294 0.357826 0.791687 11.00000 0.04593 0.05920 = 0.05676 -0.00939 0.00969 -0.00087 N005 3 0.311519 0.291933 0.830749 11.00000 0.05255 0.07319 = 0.08258 -0.01537 0.02537 -0.00822 N006 3 0.355658 0.291587 0.743153 11.00000 0.05227 0.07648 = 0.07835 -0.02753 0.01741 -0.01536 N007 3 0.059049 0.315052 0.690845 11.00000 0.06020 0.08148 = 0.08170 -0.01507 0.01304 0.00601 C008 1 0.459251 0.374092 0.719111 11.00000 0.04176 0.04764 = 0.05710 -0.00507 0.00891 -0.00391 C009 1 0.182884 0.452444 0.956087 11.00000 0.05205 0.05209 = 0.05586 0.01008 0.02270 0.00789 N00A 3 0.691399 0.408949 0.347168 11.00000 0.05770 0.12208 = 0.06557 0.00097 0.01978 -0.01813 C00B 1 0.451772 0.360891 0.575754 11.00000 0.04542 0.04869 = 0.05907 -0.00505 0.00142 -0.00486 AFIX 43 H00B 2 0.408219 0.343444 0.518994 11.00000 -1.20000 AFIX 0 C00C 1 0.509397 0.373134 0.508918 11.00000 0.04663 0.05270 = 0.04977 -0.00330 0.00554 -0.00671 C00D 1 0.156630 0.384691 0.859515 11.00000 0.05387 0.05757 = 0.06224 0.00234 0.02671 0.00728 AFIX 43 H00D 2 0.186464 0.338845 0.842088 11.00000 -1.20000 AFIX 0 C00E 1 0.330664 0.357089 0.933179 11.00000 0.04525 0.05627 = 0.05683 -0.00027 0.00770 0.00448 C00F 1 0.573155 0.402681 0.596840 11.00000 0.05193 0.05746 = 0.04728 -0.00126 0.00528 -0.00283 C00G 1 0.632007 0.399822 0.398354 11.00000 0.05333 0.07103 = 0.06012 0.00595 0.01428 -0.00413 C00H 1 0.389328 0.399422 0.909870 11.00000 0.05828 0.05617 = 0.05821 -0.01109 0.01231 -0.00162 AFIX 43 H00H 2 0.414303 0.446706 0.963727 11.00000 -1.20000 AFIX 0 C00I 1 0.508896 0.359590 0.361227 11.00000 0.05433 0.07433 = 0.05334 -0.00486 0.00362 -0.00837 AFIX 43 H00I 2 0.467211 0.341481 0.297917 11.00000 -1.20000 AFIX 0 C00J 1 0.140954 0.524914 0.984146 11.00000 0.06259 0.05294 = 0.06794 0.00474 0.02126 0.01235 C00K 1 0.085057 0.383212 0.785930 11.00000 0.05899 0.05840 = 0.06642 0.00347 0.02415 0.00877 C00L 1 0.567231 0.371975 0.306984 11.00000 0.06347 0.07552 = 0.04846 0.00175 0.00860 -0.00923 AFIX 43 H00L 2 0.564453 0.361964 0.208238 11.00000 -1.20000 AFIX 0 C00M 1 0.525471 0.402056 0.811198 11.00000 0.05176 0.05582 = 0.05500 -0.00683 0.00774 -0.00403 O00N 4 0.132299 0.656586 1.121961 11.00000 0.11625 0.11544 = 0.17035 -0.06608 0.02706 0.02899 C00O 1 0.632595 0.417002 0.545299 11.00000 0.04400 0.07437 = 0.06003 -0.00110 0.00573 -0.01237 AFIX 43 H00O 2 0.673440 0.438189 0.608056 11.00000 -1.20000 AFIX 0 C00P 1 0.292783 0.372713 1.052022 11.00000 0.05636 0.06428 = 0.06649 0.00611 0.01640 0.01697 AFIX 23 H00A 2 0.261813 0.321557 1.055125 11.00000 -1.20000 H00C 2 0.326993 0.374921 1.144794 11.00000 -1.20000 AFIX 0 C00Q 1 0.069628 0.521123 0.910030 11.00000 0.07028 0.07165 = 0.09570 -0.00528 0.02262 0.02608 AFIX 43 H00Q 2 0.039777 0.567184 0.926606 11.00000 -1.20000 AFIX 0 C00R 1 0.104769 0.247208 0.646950 11.00000 0.08144 0.08429 = 0.07149 -0.01552 0.02694 0.00728 AFIX 23 H00E 2 0.148877 0.275988 0.642014 11.00000 -1.20000 H00F 2 0.082710 0.225739 0.549733 11.00000 -1.20000 AFIX 0 C00S 1 0.694796 0.387653 0.197687 11.00000 0.07247 0.08930 = 0.07560 0.01082 0.02849 -0.00969 AFIX 23 H00G 2 0.730345 0.425650 0.170517 11.00000 -1.20000 H00J 2 0.649870 0.402204 0.132846 11.00000 -1.20000 AFIX 0 C00T 1 0.042292 0.453973 0.816000 11.00000 0.06044 0.07478 = 0.10149 -0.01701 0.01288 0.01494 AFIX 43 H00T 2 -0.005379 0.454668 0.770732 11.00000 -1.20000 AFIX 0 C00U 1 0.120246 0.167004 0.747897 11.00000 0.12685 0.07742 = 0.09386 -0.00083 0.04325 0.01566 AFIX 137 H00K 2 0.148973 0.124303 0.710732 11.00000 -1.50000 H00M 2 0.076877 0.138368 0.754411 11.00000 -1.50000 H00N 2 0.144784 0.187062 0.843092 11.00000 -1.50000 AFIX 0 C00V 1 -0.016672 0.307145 0.621761 11.00000 0.07575 0.10120 = 0.10834 -0.01302 0.01328 -0.00350 AFIX 23 H00P 2 -0.043764 0.330957 0.687891 11.00000 -1.20000 H00R 2 -0.028655 0.243452 0.605036 11.00000 -1.20000 AFIX 0 C00W 1 0.167290 0.596476 1.087119 11.00000 0.08426 0.08495 = 0.11034 -0.03251 0.02636 0.01754 AFIX 43 H00W 2 0.215210 0.596297 1.130260 11.00000 -1.20000 AFIX 0 C00X 1 0.760249 0.429409 0.446020 11.00000 0.07761 0.19873 = 0.10452 -0.04509 0.03856 -0.05430 AFIX 23 H00S 2 0.762337 0.399606 0.538864 11.00000 -1.20000 H00U 2 0.797093 0.403544 0.404777 11.00000 -1.20000 AFIX 0 C00Y 1 0.711781 0.290158 0.176738 11.00000 0.16765 0.08332 = 0.15186 -0.02137 0.04247 0.00611 AFIX 137 H00V 2 0.710810 0.279464 0.075656 11.00000 -1.50000 H00X 2 0.677619 0.251995 0.206184 11.00000 -1.50000 H00Y 2 0.757816 0.276433 0.234928 11.00000 -1.50000 AFIX 0 C00Z 1 -0.036621 0.357357 0.479324 11.00000 0.10789 0.17551 = 0.13824 0.02001 -0.01052 0.00651 AFIX 137 H00Z 2 -0.009417 0.334722 0.413940 11.00000 -1.50000 H 2 -0.027404 0.421018 0.496066 11.00000 -1.50000 HA 2 -0.085798 0.348439 0.436886 11.00000 -1.50000 AFIX 0 C010 1 0.774183 0.521963 0.471677 11.00000 0.22073 0.20945 = 0.14795 -0.06403 0.06793 -0.15760 AFIX 137 H01A 2 0.771252 0.552588 0.380393 11.00000 -1.50000 H01B 2 0.820605 0.529410 0.532448 11.00000 -1.50000 H01C 2 0.740256 0.547410 0.519798 11.00000 -1.50000 AFIX 0 HKLF 4 REM sm_138_a.res in P2(1)/c REM R1 = 0.0610 for 1905 Fo > 4sig(Fo) and 0.1829 for all 4619 data REM 329 parameters refined using 0 restraints END WGHT 0.0401 0.0000 REM Highest difference peak 0.170, deepest hole -0.186, 1-sigma level 0.037 Q1 1 -0.0548 0.2805 0.6992 11.00000 0.05 0.17 Q2 1 0.8608 0.4390 0.4176 11.00000 0.05 0.13 Q3 1 0.2182 0.1385 0.9055 11.00000 0.05 0.13 Q4 1 0.1259 0.3564 0.5139 11.00000 0.05 0.13 Q5 1 0.3793 0.3746 0.4779 11.00000 0.05 0.12 Q6 1 0.1556 0.6862 1.0256 11.00000 0.05 0.12 Q7 1 0.5585 0.2827 0.1900 11.00000 0.05 0.12 Q8 1 0.1588 0.6809 1.3376 11.00000 0.05 0.12 Q9 1 0.7822 0.3234 0.1574 11.00000 0.05 0.11 Q10 1 0.8611 0.2936 0.2167 11.00000 0.05 0.11 REM The information below was added by Olex2. REM REM R1 = 0.0610 for 1905 Fo > 4sig(Fo) and 0.1829 for all 13908 data REM n/a parameters refined using n/a restraints REM Highest difference peak 0.17, deepest hole -0.19 REM Mean Shift 0, Max Shift 0.000. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.1829 REM R1_gt = 0.0610 REM wR_ref = 0.1429 REM GOOF = 0.944 REM Shift_max = 0.000 REM Shift_mean = 0 REM Reflections_all = 13908 REM Reflections_gt = 1905 REM Parameters = n/a REM Hole = -0.19 REM Peak = 0.17 REM Flack = n/a ; _cod_data_source_file ao1c03793_si_002.cif _cod_data_source_block Com_3 _cod_original_cell_volume 2629.9(16) _cod_database_code 4519119 _shelx_shelxl_version_number 2014/7 _chemical_oxdiff_formula 'C32 H22 N4 O4 ' _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 0.983 _shelx_estimated_absorpt_t_min 0.978 _reflns_odcompleteness_completeness 99.82 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 26.32 _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 Secondary CH2 refined with riding coordinates: C00P(H00A,H00C), C00R(H00E,H00F), C00S(H00G,H00J), C00V(H00P,H00R), C00X(H00S, H00U) 2.b Aromatic/amide H refined with riding coordinates: C00B(H00B), C00D(H00D), C00H(H00H), C00I(H00I), C00L(H00L), C00O(H00O), C00Q(H00Q), C00T(H00T), C00W(H00W) 2.c Idealised Me refined as rotating group: C00U(H00K,H00M,H00N), C00Y(H00V,H00X,H00Y), C00Z(H00Z,H,HA), C010(H01A,H01B, H01C) ; _olex2_date_sample_data_collection 2018-08-13 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 2.221 _oxdiff_exptl_absorpt_empirical_full_min 0.463 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group O001 O 0.57947(9) 0.41788(19) 0.7441(2) 0.0635(8) Uani 1 1 d . . . . . O002 O 0.25183(11) 0.4550(2) 1.0349(2) 0.0640(8) Uani 1 1 d . . . . . O003 O 0.53801(10) 0.4127(2) 0.9426(2) 0.0797(10) Uani 1 1 d . . . . . N004 N 0.40329(12) 0.3578(2) 0.7917(3) 0.0543(9) Uani 1 1 d . . . . . N005 N 0.31152(12) 0.2919(2) 0.8307(3) 0.0678(10) Uani 1 1 d . . . . . N006 N 0.35566(13) 0.2916(3) 0.7432(3) 0.0686(10) Uani 1 1 d . . . . . N007 N 0.05905(14) 0.3151(3) 0.6908(3) 0.0750(11) Uani 1 1 d . . . . . C008 C 0.45925(14) 0.3741(3) 0.7191(3) 0.0492(10) Uani 1 1 d . . . . . C009 C 0.18288(16) 0.4524(3) 0.9561(3) 0.0517(10) Uani 1 1 d . . . . . N00A N 0.69140(13) 0.4089(3) 0.3472(3) 0.0809(13) Uani 1 1 d . . . . . C00B C 0.45177(14) 0.3609(3) 0.5758(3) 0.0528(10) Uani 1 1 d . . . . . H00B H 0.4082 0.3434 0.5190 0.063 Uiso 1 1 calc R . . . . C00C C 0.50940(14) 0.3731(3) 0.5089(3) 0.0506(11) Uani 1 1 d . . . . . C00D C 0.15663(15) 0.3847(3) 0.8595(3) 0.0557(11) Uani 1 1 d . . . . . H00D H 0.1865 0.3388 0.8421 0.067 Uiso 1 1 calc R . . . . C00E C 0.33066(15) 0.3571(3) 0.9332(3) 0.0534(11) Uani 1 1 d . . . . . C00F C 0.57315(15) 0.4027(3) 0.5968(3) 0.0532(11) Uani 1 1 d . . . . . C00G C 0.63201(16) 0.3998(3) 0.3984(3) 0.0613(12) Uani 1 1 d . . . . . C00H C 0.38933(16) 0.3994(3) 0.9099(3) 0.0577(11) Uani 1 1 d . . . . . H00H H 0.4143 0.4467 0.9637 0.069 Uiso 1 1 calc R . . . . C00I C 0.50890(16) 0.3596(3) 0.3612(3) 0.0621(12) Uani 1 1 d . . . . . H00I H 0.4672 0.3415 0.2979 0.075 Uiso 1 1 calc R . . . . C00J C 0.14095(18) 0.5249(3) 0.9841(4) 0.0601(12) Uani 1 1 d . . . . . C00K C 0.08506(17) 0.3832(3) 0.7859(4) 0.0597(12) Uani 1 1 d . . . . . C00L C 0.56723(16) 0.3720(3) 0.3070(3) 0.0632(12) Uani 1 1 d . . . . . H00L H 0.5645 0.3620 0.2082 0.076 Uiso 1 1 calc R . . . . C00M C 0.52547(15) 0.4021(3) 0.8112(3) 0.0549(11) Uani 1 1 d . . . . . O00N O 0.13230(16) 0.6566(3) 1.1220(3) 0.1350(15) Uani 1 1 d . . . . . C00O C 0.63259(14) 0.4170(3) 0.5453(3) 0.0605(12) Uani 1 1 d . . . . . H00O H 0.6734 0.4382 0.6081 0.073 Uiso 1 1 calc R . . . . C00P C 0.29278(16) 0.3727(3) 1.0520(3) 0.0620(12) Uani 1 1 d . . . . . H00A H 0.2618 0.3216 1.0551 0.074 Uiso 1 1 calc R . . . . H00C H 0.3270 0.3749 1.1448 0.074 Uiso 1 1 calc R . . . . C00Q C 0.06963(19) 0.5211(3) 0.9100(4) 0.0786(14) Uani 1 1 d . . . . . H00Q H 0.0398 0.5672 0.9266 0.094 Uiso 1 1 calc R . . . . C00R C 0.10477(18) 0.2472(3) 0.6469(4) 0.0776(14) Uani 1 1 d . . . . . H00E H 0.1489 0.2760 0.6420 0.093 Uiso 1 1 calc R . . . . H00F H 0.0827 0.2257 0.5497 0.093 Uiso 1 1 calc R . . . . C00S C 0.69480(18) 0.3877(4) 0.1977(4) 0.0773(15) Uani 1 1 d . . . . . H00G H 0.7303 0.4257 0.1705 0.093 Uiso 1 1 calc R . . . . H00J H 0.6499 0.4022 0.1328 0.093 Uiso 1 1 calc R . . . . C00T C 0.04229(19) 0.4540(4) 0.8160(4) 0.0798(14) Uani 1 1 d . . . . . H00T H -0.0054 0.4547 0.7707 0.096 Uiso 1 1 calc R . . . . C00U C 0.1202(2) 0.1670(4) 0.7479(4) 0.0965(16) Uani 1 1 d . . . . . H00K H 0.1490 0.1243 0.7107 0.145 Uiso 1 1 calc GR . . . . H00M H 0.0769 0.1384 0.7544 0.145 Uiso 1 1 calc GR . . . . H00N H 0.1448 0.1871 0.8431 0.145 Uiso 1 1 calc GR . . . . C00V C -0.01667(18) 0.3071(4) 0.6218(4) 0.0964(16) Uani 1 1 d . . . . . H00P H -0.0438 0.3310 0.6879 0.116 Uiso 1 1 calc R . . . . H00R H -0.0287 0.2435 0.6050 0.116 Uiso 1 1 calc R . . . . C00W C 0.1673(2) 0.5965(4) 1.0871(4) 0.0925(16) Uani 1 1 d . . . . . H00W H 0.2152 0.5963 1.1303 0.111 Uiso 1 1 calc R . . . . C00X C 0.7602(2) 0.4294(5) 0.4460(5) 0.124(2) Uani 1 1 d . . . . . H00S H 0.7623 0.3996 0.5389 0.149 Uiso 1 1 calc R . . . . H00U H 0.7971 0.4035 0.4048 0.149 Uiso 1 1 calc R . . . . C00Y C 0.7118(3) 0.2902(4) 0.1767(5) 0.133(2) Uani 1 1 d . . . . . H00V H 0.7108 0.2795 0.0757 0.200 Uiso 1 1 calc GR . . . . H00X H 0.6776 0.2520 0.2062 0.200 Uiso 1 1 calc GR . . . . H00Y H 0.7578 0.2764 0.2349 0.200 Uiso 1 1 calc GR . . . . C00Z C -0.0366(2) 0.3574(5) 0.4793(5) 0.147(2) Uani 1 1 d . . . . . H00Z H -0.0094 0.3347 0.4139 0.220 Uiso 1 1 calc GR . . . . H H -0.0274 0.4210 0.4961 0.220 Uiso 1 1 calc GR . . . . HA H -0.0858 0.3484 0.4369 0.220 Uiso 1 1 calc GR . . . . C010 C 0.7742(3) 0.5220(5) 0.4717(6) 0.189(4) Uani 1 1 d . . . . . H01A H 0.7713 0.5526 0.3804 0.283 Uiso 1 1 calc GR . . . . H01B H 0.8206 0.5294 0.5324 0.283 Uiso 1 1 calc GR . . . . H01C H 0.7403 0.5474 0.5198 0.283 Uiso 1 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 0.0459(11) 0.088(3) 0.0557(12) -0.0138(14) 0.0088(10) -0.0129(13) O002 0.0560(13) 0.061(2) 0.0759(14) 0.0015(15) 0.0181(11) 0.0102(15) O003 0.0584(13) 0.124(3) 0.0542(13) -0.0219(16) 0.0069(11) -0.0130(16) N004 0.0459(14) 0.059(3) 0.0568(16) -0.0094(17) 0.0097(13) -0.0009(17) N005 0.0525(15) 0.073(3) 0.0826(19) -0.015(2) 0.0254(16) -0.0082(18) N006 0.0523(15) 0.076(3) 0.0784(18) -0.028(2) 0.0174(15) -0.0154(18) N007 0.0602(18) 0.081(4) 0.082(2) -0.015(2) 0.0130(16) 0.006(2) C008 0.0418(16) 0.048(3) 0.0571(19) -0.0051(19) 0.0089(15) -0.0039(18) C009 0.0520(19) 0.052(3) 0.056(2) 0.010(2) 0.0227(17) 0.008(2) N00A 0.0577(17) 0.122(4) 0.0656(18) 0.001(2) 0.0198(15) -0.018(2) C00B 0.0454(17) 0.049(3) 0.059(2) -0.005(2) 0.0014(16) -0.0049(19) C00C 0.0466(17) 0.053(3) 0.0498(18) -0.0033(19) 0.0055(15) -0.0067(19) C00D 0.054(2) 0.058(4) 0.062(2) 0.002(2) 0.0267(17) 0.007(2) C00E 0.0453(17) 0.056(3) 0.0568(19) 0.000(2) 0.0077(16) 0.004(2) C00F 0.0519(18) 0.057(3) 0.0473(19) -0.001(2) 0.0053(15) -0.0028(19) C00G 0.0533(19) 0.071(4) 0.060(2) 0.006(2) 0.0143(17) -0.004(2) C00H 0.058(2) 0.056(4) 0.058(2) -0.011(2) 0.0123(17) -0.002(2) C00I 0.0543(18) 0.074(4) 0.0533(19) -0.005(2) 0.0036(16) -0.008(2) C00J 0.063(2) 0.053(4) 0.068(2) 0.005(2) 0.0213(19) 0.012(2) C00K 0.059(2) 0.058(4) 0.066(2) 0.003(2) 0.0241(19) 0.009(2) C00L 0.063(2) 0.076(4) 0.0485(19) 0.002(2) 0.0086(17) -0.009(2) C00M 0.0518(18) 0.056(4) 0.055(2) -0.007(2) 0.0077(17) -0.004(2) O00N 0.116(2) 0.115(4) 0.170(3) -0.066(3) 0.027(2) 0.029(2) C00O 0.0440(17) 0.074(4) 0.060(2) -0.001(2) 0.0057(15) -0.0124(19) C00P 0.0564(19) 0.064(4) 0.066(2) 0.006(2) 0.0164(17) 0.017(2) C00Q 0.070(3) 0.072(5) 0.096(3) -0.005(3) 0.023(2) 0.026(3) C00R 0.081(2) 0.084(5) 0.071(2) -0.016(3) 0.027(2) 0.007(3) C00S 0.072(2) 0.089(5) 0.076(2) 0.011(3) 0.028(2) -0.010(3) C00T 0.060(2) 0.075(4) 0.101(3) -0.017(3) 0.013(2) 0.015(3) C00U 0.127(3) 0.077(5) 0.094(3) -0.001(3) 0.043(3) 0.016(3) C00V 0.076(3) 0.101(5) 0.108(3) -0.013(3) 0.013(2) -0.003(3) C00W 0.084(3) 0.085(5) 0.110(3) -0.033(3) 0.026(3) 0.018(3) C00X 0.078(3) 0.199(8) 0.105(3) -0.045(4) 0.039(2) -0.054(4) C00Y 0.168(5) 0.083(6) 0.152(4) -0.021(4) 0.042(3) 0.006(4) C00Z 0.108(3) 0.176(8) 0.138(4) 0.020(5) -0.011(3) 0.007(4) C010 0.221(6) 0.209(10) 0.148(5) -0.064(6) 0.068(4) -0.158(7) 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 C00M O001 C00F 122.4(2) . . ? C009 O002 C00P 119.0(3) . . ? N006 N004 C008 119.9(3) . . ? C00H N004 N006 110.6(3) . . ? C00H N004 C008 129.5(3) . . ? N006 N005 C00E 109.6(3) . . ? N005 N006 N004 106.4(3) . . ? C00K N007 C00R 122.0(3) . . ? C00K N007 C00V 122.1(3) . . ? C00R N007 C00V 115.9(4) . . ? N004 C008 C00M 115.9(2) . . ? C00B C008 N004 122.5(3) . . ? C00B C008 C00M 121.5(3) . . ? O002 C009 C00J 114.6(4) . . ? C00D C009 O002 123.2(3) . . ? C00D C009 C00J 122.2(3) . . ? C00G N00A C00S 123.5(3) . . ? C00G N00A C00X 121.5(3) . . ? C00S N00A C00X 114.5(3) . . ? C008 C00B H00B 119.5 . . ? C008 C00B C00C 120.9(3) . . ? C00C C00B H00B 119.5 . . ? C00F C00C C00B 117.8(3) . . ? C00F C00C C00I 115.7(3) . . ? C00I C00C C00B 126.5(3) . . ? C009 C00D H00D 119.5 . . ? C009 C00D C00K 121.0(4) . . ? C00K C00D H00D 119.5 . . ? N005 C00E C00H 108.3(3) . . ? N005 C00E C00P 122.7(3) . . ? C00H C00E C00P 128.9(4) . . ? O001 C00F C00C 120.5(3) . . ? C00O C00F O001 116.2(3) . . ? C00O C00F C00C 123.3(3) . . ? N00A C00G C00L 121.9(3) . . ? N00A C00G C00O 121.1(3) . . ? C00O C00G C00L 117.0(3) . . ? N004 C00H C00E 105.1(3) . . ? N004 C00H H00H 127.4 . . ? C00E C00H H00H 127.4 . . ? C00C C00I H00I 118.8 . . ? C00L C00I C00C 122.4(3) . . ? C00L C00I H00I 118.8 . . ? C009 C00J C00Q 115.4(4) . . ? C009 C00J C00W 123.1(4) . . ? C00Q C00J C00W 121.4(4) . . ? N007 C00K C00D 120.8(4) . . ? N007 C00K C00T 122.0(3) . . ? C00T C00K C00D 117.2(4) . . ? C00G C00L H00L 119.4 . . ? C00I C00L C00G 121.2(3) . . ? C00I C00L H00L 119.4 . . ? O001 C00M C008 116.8(2) . . ? O003 C00M O001 116.9(3) . . ? O003 C00M C008 126.3(3) . . ? C00F C00O C00G 120.3(3) . . ? C00F C00O H00O 119.9 . . ? C00G C00O H00O 119.9 . . ? O002 C00P C00E 113.8(3) . . ? O002 C00P H00A 108.8 . . ? O002 C00P H00C 108.8 . . ? C00E C00P H00A 108.8 . . ? C00E C00P H00C 108.8 . . ? H00A C00P H00C 107.7 . . ? C00J C00Q H00Q 118.3 . . ? C00T C00Q C00J 123.4(4) . . ? C00T C00Q H00Q 118.3 . . ? N007 C00R H00E 108.8 . . ? N007 C00R H00F 108.8 . . ? N007 C00R C00U 113.9(3) . . ? H00E C00R H00F 107.7 . . ? C00U C00R H00E 108.8 . . ? C00U C00R H00F 108.8 . . ? N00A C00S H00G 108.9 . . ? N00A C00S H00J 108.9 . . ? N00A C00S C00Y 113.2(4) . . ? H00G C00S H00J 107.7 . . ? C00Y C00S H00G 108.9 . . ? C00Y C00S H00J 108.9 . . ? C00K C00T H00T 119.6 . . ? C00Q C00T C00K 120.7(4) . . ? C00Q C00T H00T 119.6 . . ? C00R C00U H00K 109.5 . . ? C00R C00U H00M 109.5 . . ? C00R C00U H00N 109.5 . . ? H00K C00U H00M 109.5 . . ? H00K C00U H00N 109.5 . . ? H00M C00U H00N 109.5 . . ? N007 C00V H00P 109.1 . . ? N007 C00V H00R 109.1 . . ? N007 C00V C00Z 112.5(4) . . ? H00P C00V H00R 107.8 . . ? C00Z C00V H00P 109.1 . . ? C00Z C00V H00R 109.1 . . ? C00J C00W H00W 117.3 . . ? O00N C00W C00J 125.5(4) . . ? O00N C00W H00W 117.3 . . ? N00A C00X H00S 108.6 . . ? N00A C00X H00U 108.6 . . ? H00S C00X H00U 107.5 . . ? C010 C00X N00A 114.8(6) . . ? C010 C00X H00S 108.6 . . ? C010 C00X H00U 108.6 . . ? C00S C00Y H00V 109.5 . . ? C00S C00Y H00X 109.5 . . ? C00S C00Y H00Y 109.5 . . ? H00V C00Y H00X 109.5 . . ? H00V C00Y H00Y 109.5 . . ? H00X C00Y H00Y 109.5 . . ? C00V C00Z H00Z 109.5 . . ? C00V C00Z H 109.5 . . ? C00V C00Z HA 109.5 . . ? H00Z C00Z H 109.5 . . ? H00Z C00Z HA 109.5 . . ? H C00Z HA 109.5 . . ? C00X C010 H01A 109.5 . . ? C00X C010 H01B 109.5 . . ? C00X C010 H01C 109.5 . . ? H01A C010 H01B 109.5 . . ? H01A C010 H01C 109.5 . . ? H01B C010 H01C 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 C00F 1.381(3) . ? O001 C00M 1.367(3) . ? O002 C009 1.379(3) . ? O002 C00P 1.439(4) . ? O003 C00M 1.214(3) . ? N004 N006 1.352(4) . ? N004 C008 1.435(3) . ? N004 C00H 1.351(4) . ? N005 N006 1.322(3) . ? N005 C00E 1.350(4) . ? N007 C00K 1.362(4) . ? N007 C00R 1.460(5) . ? N007 C00V 1.476(4) . ? C008 C00B 1.337(3) . ? C008 C00M 1.441(4) . ? C009 C00D 1.367(5) . ? C009 C00J 1.406(5) . ? N00A C00G 1.360(3) . ? N00A C00S 1.457(4) . ? N00A C00X 1.479(4) . ? C00B H00B 0.9300 . ? C00B C00C 1.421(4) . ? C00C C00F 1.396(4) . ? C00C C00I 1.402(4) . ? C00D H00D 0.9300 . ? C00D C00K 1.409(4) . ? C00E C00H 1.365(4) . ? C00E C00P 1.493(4) . ? C00F C00O 1.373(4) . ? C00G C00L 1.416(4) . ? C00G C00O 1.403(4) . ? C00H H00H 0.9300 . ? C00I H00I 0.9300 . ? C00I C00L 1.363(4) . ? C00J C00Q 1.407(4) . ? C00J C00W 1.443(5) . ? C00K C00T 1.403(5) . ? C00L H00L 0.9300 . ? O00N C00W 1.208(5) . ? C00O H00O 0.9300 . ? C00P H00A 0.9700 . ? C00P H00C 0.9700 . ? C00Q H00Q 0.9300 . ? C00Q C00T 1.352(5) . ? C00R H00E 0.9700 . ? C00R H00F 0.9700 . ? C00R C00U 1.501(5) . ? C00S H00G 0.9700 . ? C00S H00J 0.9700 . ? C00S C00Y 1.496(6) . ? C00T H00T 0.9300 . ? C00U H00K 0.9600 . ? C00U H00M 0.9600 . ? C00U H00N 0.9600 . ? C00V H00P 0.9700 . ? C00V H00R 0.9700 . ? C00V C00Z 1.501(5) . ? C00W H00W 0.9300 . ? C00X H00S 0.9700 . ? C00X H00U 0.9700 . ? C00X C010 1.399(8) . ? C00Y H00V 0.9600 . ? C00Y H00X 0.9600 . ? C00Y H00Y 0.9600 . ? C00Z H00Z 0.9600 . ? C00Z H 0.9600 . ? C00Z HA 0.9600 . ? C010 H01A 0.9600 . ? C010 H01B 0.9600 . ? C010 H01C 0.9600 . ? loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_squared_meas _refln_F_squared_sigma -2 0 0 636.52 9.85 2 0 0 632.92 11.32 -3 0 0 20.94 2.36 3 0 0 11.28 1.9 -3 0 0 21.52 2.8 3 0 0 13.62 2.46 -4 0 0 62.99 4.65 -4 0 0 59.11 4.91 4 0 0 36.16 3.44 4 0 0 21.57 4.63 -5 0 0 719.76 16.57 -5 0 0 699.72 18.35 5 0 0 688.98 17.14 6 0 0 5.64 1.66 -6 0 0 7.72 2.11 -6 0 0 6.7 2.15 7 0 0 297.35 13.29 -7 0 0 302.46 14.58 -7 0 0 307.86 12.96 -8 0 0 176.28 10.54 8 0 0 178.89 11.17 -8 0 0 178.24 11.52 9 0 0 44.08 6.22 -9 0 0 39.55 6.14 -9 0 0 41.57 5.58 -10 0 0 152.33 12.19 10 0 0 150.69 12.08 -10 0 0 141.81 10.55 -11 0 0 100.44 9.27 11 0 0 91.33 10.19 -11 0 0 89.33 10.23 12 0 0 2.83 2.5 -12 0 0 5.37 3.51 -12 0 0 -0.16 1.24 12 0 0 -1.52 1.99 -13 0 0 64.38 7.73 -13 0 0 54.59 8.86 13 0 0 62.26 8.88 -14 0 0 8.93 2.8 -14 0 0 7.97 4.15 14 0 0 8.9 4.21 -15 0 0 40.79 8.74 -15 0 0 45.55 7.64 -16 0 0 38.01 8.68 -16 0 0 36.41 6.73 -17 0 0 21.16 6.4 -17 0 0 22.07 5.78 -18 0 0 73.18 12.67 -18 0 0 61.6 9.46 -19 0 0 7.67 4.29 -19 0 0 11.55 4.92 -20 0 0 1.93 3.05 -20 0 0 5.34 2.43 -21 0 0 1.3 1.53 -2 -1 0 159.81 6.99 2 1 0 166.51 7.61 -2 -1 0 177.31 7.63 -3 -1 0 251.44 9.23 -3 -1 0 244.34 9.53 3 1 0 239.92 9.46 3 -1 0 245.05 9.13 3 -1 0 244.58 8.03 3 1 0 253.92 10.51 4 -1 0 480.71 14.57 -4 -1 0 482 13.69 -4 1 0 481.71 12.32 4 1 0 503.61 16.61 4 -1 0 474.85 12.81 -4 1 0 501.59 14.38 5 -1 0 404.37 13.42 5 1 0 414.75 16.93 -5 1 0 427.51 12.75 5 1 0 401.32 15.46 -5 1 0 441.05 15.2 5 -1 0 411.88 14.66 -5 -1 0 441.95 14.13 6 1 0 21.05 4.56 -6 -1 0 25.47 4.06 -6 1 0 21.02 2.88 6 -1 0 20.92 3.95 -6 1 0 20.79 3.47 6 -1 0 21.51 3.56 6 1 0 20.86 4.16 -7 -1 0 187.97 10.55 7 1 0 194.81 13.53 7 -1 0 192.86 10.6 -7 -1 0 174.95 11.91 7 -1 0 182.22 12.18 -7 1 0 184.2 11.82 7 1 0 178.3 11.83 -7 1 0 193.67 10.18 8 1 0 162.01 13.26 -8 1 0 168.49 11.62 -8 -1 0 164.54 11.45 -8 1 0 166.42 10.02 8 1 0 171.18 11.76 8 -1 0 161.73 11.86 -8 -1 0 170.63 10.06 8 -1 0 161.49 10.36 -9 -1 0 161.08 12.17 -9 1 0 158.3 10.36 9 -1 0 159.82 11.4 9 1 0 163.64 12.84 -9 -1 0 157.45 10.37 9 1 0 175.18 14.63 9 -1 0 131.69 13.14 -9 1 0 147.04 12.15 -10 1 0 59.71 6.76 10 -1 0 65.2 7.38 10 -1 0 60.43 8.36 -10 1 0 61.19 7.83 -10 -1 0 64.4 7.07 10 1 0 54.43 7.44 10 1 0 64.81 9.31 -10 -1 0 61.57 7.57 11 1 0 51.26 8.09 11 1 0 58.99 10.24 -11 1 0 65.86 7.24 -11 -1 0 60.19 7.18 -11 1 0 55.06 7.88 -11 -1 0 58.85 7.73 11 -1 0 59.31 7.57 12 1 0 12.74 5.53 -12 -1 0 7.28 3.03 -12 1 0 11.06 4.46 12 1 0 6.32 3.13 -12 1 0 7.19 3.11 -12 -1 0 9.02 3.31 12 -1 0 5.61 2.62 13 1 0 6.31 3.51 -13 1 0 8.24 3.52 -13 -1 0 4.4 2.92 -13 1 0 4.38 2.54 -13 -1 0 6 2.98 13 -1 0 1.48 2.29 13 1 0 7.63 4.49 -14 1 0 0.76 1.18 -14 -1 0 2.75 2.98 14 1 0 -0.87 4.4 -14 -1 0 0.76 1 -14 1 0 7.54 4.07 14 -1 0 -0.46 2.04 -15 1 0 72.28 11.31 -15 1 0 83.48 9.43 -15 -1 0 70.97 10.97 -15 -1 0 84.35 10 -16 -1 0 55.49 8.29 -16 -1 0 48.47 9.23 -16 1 0 43.23 8.7 -16 1 0 43.89 7.4 -17 1 0 118.22 15.49 -17 -1 0 126.6 13.07 -17 -1 0 118.64 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