#------------------------------------------------------------------------------ #$Date: 2024-09-17 04:17:44 +0300 (Tue, 17 Sep 2024) $ #$Revision: 294773 $ #$URL: file:///home/coder/svn-repositories/cod/cif/3/00/04/3000476.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_3000476 loop_ _publ_author_name 'Deka, Poonam' 'Jaiswal, Shilpi' 'Sarma, Parishmita' 'Bora, Debajit' 'Nakane, Takanori' 'Kawamoto, Akihiro' 'Kurisu, Genji' 'Mahanta, Sanjeev Pran' 'Patra, Abhijit' 'Ichiyanagi, Kouhei' 'Sasaki, Toshiyuki' 'Thakuria, Ranjit' _publ_section_title ; Analysis of Solid-State Emission of the p-Bis(2,2-dicyanovinyl)benzene Analogue through Combined X-ray, Synchrotron, and Microcrystal Electron Diffraction ; _journal_name_full 'Crystal Growth & Design' _journal_page_first 7222 _journal_page_last 7234 _journal_paper_doi 10.1021/acs.cgd.4c00856 _journal_volume 24 _journal_year 2024 _chemical_formula_moiety '2(O), C20 H10 N4' _chemical_formula_sum 'C20 H10 N4 O2' _chemical_formula_weight 338.32 _space_group_crystal_system monoclinic _space_group_IT_number 4 _space_group_name_Hall 'P 2yb' _space_group_name_H-M_alt 'P 1 21 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2024-01-09 _audit_creation_method ; Olex2 1.5 (compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498) ; _cell_angle_alpha 90 _cell_angle_beta 92.318(5) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 3.7388(2) _cell_length_b 11.9046(5) _cell_length_c 40.4205(19) _cell_measurement_reflns_used 5277 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 33.0770 _cell_measurement_theta_min 2.2590 _cell_volume 1797.60(15) _computing_cell_refinement 'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)' _computing_data_collection 'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)' _computing_data_reduction 'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)' _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 'SHELXT (Sheldrick, 2015)' _diffrn_ambient_temperature 100 _diffrn_detector 'Dectris Eiger X 1M' _diffrn_detector_area_resol_mean 13.3333 _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 -90.00 89.80 0.20 2.50 -- 25.00 45.00 0.00 899 2 \w -90.00 89.80 0.20 2.50 -- 25.00 45.00 90.00 899 3 \w -90.00 89.80 0.20 2.50 -- 25.00 45.00 180.00 899 4 \w -90.00 89.80 0.20 2.50 -- 25.00 45.00 270.00 899 ; _diffrn_measurement_device 'abstract diffractometer' _diffrn_measurement_device_type 'esperanto-CrysAlisPro-abstract goniometer imported esperanto images' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.1314402000 _diffrn_orient_matrix_UB_12 -0.0199465000 _diffrn_orient_matrix_UB_13 0.0153815000 _diffrn_orient_matrix_UB_21 -0.1498829000 _diffrn_orient_matrix_UB_22 0.0186689000 _diffrn_orient_matrix_UB_23 0.0128915000 _diffrn_orient_matrix_UB_31 -0.0865522000 _diffrn_orient_matrix_UB_32 -0.0625306000 _diffrn_orient_matrix_UB_33 -0.0010752000 _diffrn_radiation_monochromator 'Si(111) Channel Cut' _diffrn_radiation_probe x-ray _diffrn_radiation_type Synchrotron _diffrn_radiation_wavelength 0.812 _diffrn_reflns_av_unetI/netI 0.0669 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_h_min -4 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 50 _diffrn_reflns_limit_l_min -50 _diffrn_reflns_number 8407 _diffrn_reflns_point_group_measured_fraction_full 0.968 _diffrn_reflns_point_group_measured_fraction_max 0.961 _diffrn_reflns_theta_full 29.157 _diffrn_reflns_theta_max 30.486 _diffrn_reflns_theta_min 1.728 _diffrn_source 'Synchrotron radiation SPring-8 BL40XU' _exptl_absorpt_coefficient_mu 0.116 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.35037 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.250 _exptl_crystal_description plate _exptl_crystal_F_000 696 _refine_diff_density_max 0.666 _refine_diff_density_min -0.655 _refine_diff_density_rms 0.198 _refine_ls_abs_structure_details ; Flack x determined using 1274 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 10.0(10) _refine_ls_extinction_coef 0.055(15) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL-2018/3 (Sheldrick 2018)' _refine_ls_goodness_of_fit_ref 1.667 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 353 _refine_ls_number_reflns 8407 _refine_ls_number_restraints 485 _refine_ls_restrained_S_all 1.639 _refine_ls_R_factor_all 0.2474 _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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.4468 _reflns_Friedel_coverage 0.833 _reflns_Friedel_fraction_full 0.933 _reflns_Friedel_fraction_max 0.919 _reflns_number_gt 4134 _reflns_number_total 8407 _reflns_threshold_expression 'I > 2\s(I)' _twin_special_details ; Component 2 rotated by -179.9363\% around [0.92 0.00 -0.38] (reciprocal) or [1.00 0.00 0.00] (direct) ; _cod_data_source_file bp-1_twin.cif _cod_data_source_block bp-1_twin _cod_depositor_comments 'Releasing structure 3000476 into public domain as published material.' _cod_database_code 3000476 _shelx_shelxl_version_number 2018/3 _chemical_oxdiff_formula C20H20N8 _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. ; _olex2_refinement_description ; 1. Twinned data refinement Scales: 0.643(6) 0.357(6) 2. Fixed Uiso At 1.2 times of: All C(H) groups 3. Uiso/Uaniso restraints and constraints N007 \\sim C26 \\sim H20 \\sim C27 \\sim C00M \\sim H25 \\sim H00O \\sim C20 \\sim H00Q \\sim C011 \\sim O4 \\sim O3 \\sim C00H \\sim N00X \\sim N005 \\sim O5 \\sim H00U \\sim C00Z \\sim C014 \\sim C00V \\sim C013 \\sim N00I \\sim C00A \\sim O1 \\sim O2 \\sim C001 \\sim H00M \\sim C00S \\sim C21 \\sim C00J \\sim C00T \\sim C22 \\sim C00R \\sim C00O \\sim H23 \\sim H24 \\sim H21 \\sim C00K \\sim C00N \\sim C00W \\sim C012 \\sim C00Q \\sim H010 \\sim O6 \\sim N00P: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.01 within 2A Uanis(C22) \\sim Ueq, Uanis(C00O) \\sim Ueq, Uanis(C001) \\sim Ueq, Uanis(C00S) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C00J) \\sim Ueq, Uanis(C00T) \\sim Ueq, Uanis(C00R) \\sim Ueq, Uanis(C00K) \\sim Ueq, Uanis(C00N) \\sim Ueq, Uanis(C00W) \\sim Ueq, Uanis(C012) \\sim Ueq, Uanis(C00Q) \\sim Ueq, Uanis(N00P) \\sim Ueq, Uanis(C011) \\sim Ueq, Uanis(N007) \\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C00M) \\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C00H) \\sim Ueq, Uanis(N00X) \\sim Ueq, Uanis(N005) \\sim Ueq, Uanis(C00Z) \\sim Ueq, Uanis(C014) \\sim Ueq, Uanis(C00V) \\sim Ueq, Uanis(C013) \\sim Ueq, Uanis(N00I) \\sim Ueq, Uanis(C00A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.005 Uanis(C25) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.005 Uanis(C014) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001 Uanis(C00Y) = Uanis(C018) = Uanis(C003) = Uanis(C001) = Uanis(C00T) = Uanis(C00A) = Uanis(C01C) = Uanis(C014) = Uanis(C01B) = Uanis(C00Z) = Uanis(C00S) = Uanis(C00L) Uanis(C00M) = Uanis(C22) = Uanis(C20) = Uanis(C21) = Uanis(C00W) = Uanis(C00N) Uanis(C25) = Uanis(C00J) = Uanis(C00K) = Uanis(C00U) = Uanis(C015) = Uanis(C00R) = Uanis(C010) = Uanis(C00V) = Uanis(C26) = Uanis(C00Q) = Uanis(C011) = Uanis(C012) 4. Rigid body (RIGU) restrains H00O, N007, C26, H20, C27, C00M, H25, C20, H00Q, C011, O4, O3, C00H, N00X, N005, O5, H00U, C00Z, C014, C00V, C013, N00I, C00A, C012, O1, O2, C001, H00M, C00S, C21, C00J, C00T, C22, C00R, C00O, H23, H24, H21, C00K, C00N, C00W, C00Q, H010, O6, N00P with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005 5. Others 1*[Sof(O2)]+1*[Sof(O4)]+1*[Sof(O6)]+1*[Sof(O9)]+1*[Sof(O11)]+1*[Sof(O13)]+1* [Sof(O14)]=2 with esd of 0.001 1*[Sof(O1)]+1*[Sof(O3)]+1*[Sof(O5)]+1*[Sof(O7)]+1*[Sof(O8)]+1*[Sof(O10)]+1* [Sof(O12)]=2 with esd of 0.001 6.a Aromatic/amide H refined with riding coordinates: C27(H27), C24(H24), C26(H26), C21(H21), C23(H23), C20(H20), C25(H25), C00H(H00H), C00J(H00J), C00M(H00M), C00N(H00N), C00O(H00O), C00Q(H00Q), C00R(H00R), C00U(H00U), C010(H010), C012(H012), C016(H016), C017(H017), C01A(H01A) ; _shelx_res_file ; TITL bp-1_twin_4-2_twin1_hklf4_a.res in P2(1) bp-1_twin_4-2_twin1_hklf4.res created by SHELXL-2018/3 at 19:13:18 on 09-Jan-2024 REM Old TITL BP-1_Twin_4-2_twin1_hklf4 in P2(1) REM SHELXT solution in P2(1): R1 0.394, Rweak 0.034, Alpha 0.087 REM 0.000 for 0 systematic absences, Orientation as input REM Flack x = -9.990 ( 9.990 ) from 1038 Parsons' quotients REM Formula found by SHELXT: C37 N16 CELL 0.812 3.7388 11.9046 40.4205 90 92.318 90 ZERR 4 0.0002 0.0005 0.0019 0 0.005 0 LATT -1 SYMM -X,0.5+Y,-Z SFAC C H N O DISP C 0.0035 0.0022 15.5022 DISP H 0 0 0.6293 DISP N 0.0066 0.0044 27.5558 DISP O 0.0117 0.0081 46.6654 UNIT 80 40 16 8 RIGU 0.005 0.005 H00O N007 C26 H20 C27 C00M H25 C20 H00Q C011 O4 O3 C00H = N00X N005 O5 H00U C00Z C014 C00V C013 N00I C00A C012 O1 O2 C001 H00M C00S = C21 C00J C00T C22 C00R C00O H23 H24 H21 C00K C00N C00W C00Q H010 O6 N00P ISOR 0.01 0.005 C22 C00O O1 O2 C001 H00M C00S C21 C00J C00T C00R H23 H24 = H21 C00K C00N C00W C012 C00Q H010 O6 N00P C011 N007 C26 H20 C27 C00M H25 = H00O C20 H00Q O4 O3 C00H N00X N005 O5 H00U C00Z C014 C00V C013 N00I C00A SIMU 0.01 0.01 2 N007 C26 H20 C27 C00M H25 H00O C20 H00Q C011 O4 O3 C00H = N00X N005 O5 H00U C00Z C014 C00V C013 N00I C00A O1 O2 C001 H00M C00S C21 = C00J C00T C22 C00R C00O H23 H24 H21 C00K C00N C00W C012 C00Q H010 O6 N00P ISOR 0.005 0.005 C25 EADP C00Y C018 C003 C001 C00T C00A C01C C014 C01B C00Z C00S C00L EADP C00M C22 C20 C21 C00W C00N EADP C25 C00J C00K C00U C015 C00R C010 C00V C26 C00Q C011 C012 ISOR 0.001 0.001 C014 SUMP 2 0.001 1 2 1 3 1 4 1 5 1 6 1 7 1 8 SUMP 2 0.001 1 9 1 10 1 11 1 12 1 13 1 14 1 15 L.S. 100 0 0 PLAN 5 CONF list 4 MORE -1 BOND $H fmap 2 53 acta SHEL 99 0.8 REM REM REM WGHT 0.200000 EXTI 0.055240 BASF 0.35662 FVAR 2.27653 0.22283 0.26151 0.20596 0.48990 0.36069 0.26827 FVAR 0.19097 0.25636 0.14700 0.24921 0.43120 0.27747 0.32021 FVAR 0.31864 PART 1 O1 4 0.589891 -0.686909 -0.868897 91.00000 0.06032 PART 2 O2 4 -0.321739 -1.224620 -0.633103 21.00000 0.07851 PART 3 O3 4 -0.181255 -0.693925 -0.841454 101.00000 0.05107 PART 4 O4 4 -0.645480 -1.213495 -0.635844 31.00000 0.06964 PART 5 O5 4 0.067320 -0.710975 -0.864722 111.00000 0.05646 PART 6 O6 4 -0.364674 -1.197217 -0.652053 41.00000 0.07390 PART 0 C001 1 0.795076 -0.157039 -1.013804 11.00000 0.03302 0.02696 = 0.03602 -0.00023 -0.00302 0.00019 C22 1 -1.045419 -0.658169 -0.544143 11.00000 0.02962 0.01658 = 0.03945 -0.00081 -0.00708 -0.00205 C003 1 0.011229 -0.231183 -0.727729 11.00000 0.03302 0.02696 = 0.03602 -0.00023 -0.00302 0.00019 C27 1 0.627542 -0.110470 -0.987313 11.00000 0.03024 0.01716 = 0.03947 0.00132 -0.01057 0.00178 AFIX 43 H27 2 0.561715 -0.035651 -0.990166 11.00000 -1.20000 AFIX 0 N005 3 -1.502394 -0.864792 -0.482217 11.00000 0.03967 0.03291 = 0.04475 0.00132 0.00128 -0.00144 N006 3 1.006635 -0.364229 -1.017923 11.00000 0.06334 0.01226 = 0.05644 0.00143 -0.01155 0.00778 N007 3 -1.466411 -0.538159 -0.435562 11.00000 0.04459 0.03497 = 0.05238 -0.00403 0.00041 -0.00002 C24 1 -0.684091 -0.737339 -0.699134 11.00000 0.04197 0.01137 = 0.03800 0.00900 0.00487 -0.00210 AFIX 43 H24 2 -0.699198 -0.688344 -0.717056 11.00000 0.01369 AFIX 0 N009 3 0.083340 -0.138198 -0.720957 11.00000 0.08310 0.02259 = 0.05009 -0.01511 -0.01237 0.00208 C00A 1 0.914366 -0.272475 -1.016342 11.00000 0.03302 0.02696 = 0.03602 -0.00023 -0.00302 0.00019 C26 1 0.319714 -0.118989 -0.901698 11.00000 0.03308 0.01659 = 0.04003 -0.00061 -0.00652 0.00178 AFIX 43 H26 2 0.235351 -0.067251 -0.886639 11.00000 -1.20000 AFIX 0 C21 1 -0.998138 -0.808507 -0.584428 11.00000 0.02962 0.01658 = 0.03945 -0.00081 -0.00708 -0.00205 AFIX 43 H21 2 -1.026709 -0.883852 -0.590010 11.00000 0.02835 AFIX 0 C23 1 -0.538860 -0.918303 -0.675652 11.00000 0.04098 0.00772 = 0.04997 -0.00939 -0.01886 0.00797 AFIX 43 H23 2 -0.451880 -0.990955 -0.677954 11.00000 0.07380 AFIX 0 C20 1 -1.089319 -0.771219 -0.553137 11.00000 0.02962 0.01658 = 0.03945 -0.00081 -0.00708 -0.00205 AFIX 43 H20 2 -1.180111 -0.821873 -0.538101 11.00000 0.02767 AFIX 0 C25 1 0.138431 -0.384010 -0.854824 11.00000 0.03308 0.01659 = 0.04003 -0.00061 -0.00652 0.00178 AFIX 43 H25 2 0.130664 -0.433909 -0.872542 11.00000 0.01915 AFIX 0 N00G 3 -0.157124 -0.957188 -0.813440 11.00000 0.05636 0.02186 = 0.06406 -0.00561 -0.00698 -0.00749 C00H 1 -1.134462 -0.610614 -0.511971 11.00000 0.03127 0.01822 = 0.04106 -0.00467 -0.01106 -0.00407 AFIX 43 H00H 2 -1.071443 -0.535618 -0.508981 11.00000 -1.20000 AFIX 0 N00I 3 0.963052 -0.038426 -1.064447 11.00000 0.04129 0.03060 = 0.04881 0.00525 0.00077 0.00290 C00J 1 0.282828 -0.201273 -0.831768 11.00000 0.03308 0.01659 = 0.04003 -0.00061 -0.00652 0.00178 AFIX 43 H00J 2 0.364961 -0.128177 -0.834339 11.00000 -1.20000 AFIX 0 C00K 1 0.259356 -0.272574 -0.859219 11.00000 0.03308 0.01659 = 0.04003 -0.00061 -0.00652 0.00178 C00L 1 -1.376197 -0.590058 -0.457849 11.00000 0.03302 0.02696 = 0.03602 -0.00023 -0.00302 0.00019 C00M 1 -0.896637 -0.584514 -0.567530 11.00000 0.02962 0.01658 = 0.03945 -0.00081 -0.00708 -0.00205 AFIX 43 H00M 2 -0.853831 -0.510134 -0.561554 11.00000 0.03144 AFIX 0 C00N 1 -0.813495 -0.619494 -0.598786 11.00000 0.02962 0.01658 = 0.03945 -0.00081 -0.00708 -0.00205 AFIX 43 H00N 2 -0.725301 -0.568870 -0.613968 11.00000 -1.20000 AFIX 0 C00O 1 -0.646527 -0.884292 -0.644922 11.00000 0.03667 0.01051 = 0.03733 0.00698 -0.00544 -0.00082 AFIX 43 H00O 2 -0.641634 -0.934306 -0.627235 11.00000 0.02792 AFIX 0 N00P 3 -0.582277 -0.639068 -0.778958 11.00000 0.04947 0.03803 = 0.04624 0.00321 0.00199 0.00391 C00Q 1 0.405767 -0.084210 -0.932931 11.00000 0.03308 0.01659 = 0.04003 -0.00061 -0.00652 0.00178 AFIX 43 H00Q 2 0.374932 -0.009130 -0.938729 11.00000 0.03226 AFIX 0 C00R 1 0.032829 -0.418054 -0.824342 11.00000 0.03308 0.01659 = 0.04003 -0.00061 -0.00652 0.00178 AFIX 43 H00R 2 -0.056661 -0.490431 -0.822111 11.00000 -1.20000 AFIX 0 C00S 1 -1.292575 -0.658141 -0.486131 11.00000 0.03302 0.02696 = 0.03602 -0.00023 -0.00302 0.00019 C00T 1 0.882472 -0.090823 -1.042189 11.00000 0.03302 0.02696 = 0.03602 -0.00023 -0.00302 0.00019 C00U 1 0.186486 -0.237188 -0.800891 11.00000 0.03308 0.01659 = 0.04003 -0.00061 -0.00652 0.00178 AFIX 43 H00U 2 0.207402 -0.188974 -0.782812 11.00000 0.00586 AFIX 0 C00V 1 0.359483 -0.233601 -0.892441 11.00000 0.03308 0.01659 = 0.04003 -0.00061 -0.00652 0.00178 C00W 1 -0.864440 -0.733504 -0.607381 11.00000 0.02962 0.01658 = 0.03945 -0.00081 -0.00708 -0.00205 N00X 3 -0.341722 -0.455477 -0.686433 11.00000 0.04865 0.04540 = 0.05269 0.00196 0.00108 -0.00012 C00Y 1 -0.084628 -0.343946 -0.735905 11.00000 0.03302 0.02696 = 0.03602 -0.00023 -0.00302 0.00019 C00Z 1 -1.403226 -0.772701 -0.483894 11.00000 0.03302 0.02696 = 0.03602 -0.00023 -0.00302 0.00019 C010 1 0.498943 -0.308388 -0.915890 11.00000 0.03308 0.01659 = 0.04003 -0.00061 -0.00652 0.00178 AFIX 43 H010 2 0.533772 -0.383355 -0.910146 11.00000 0.02551 AFIX 0 C011 1 0.536698 -0.158252 -0.955813 11.00000 0.03308 0.01659 = 0.04003 -0.00061 -0.00652 0.00178 C012 1 0.584410 -0.272735 -0.947053 11.00000 0.03308 0.01659 = 0.04003 -0.00061 -0.00652 0.00178 AFIX 43 H012 2 0.672702 -0.323424 -0.962212 11.00000 -1.20000 AFIX 0 C013 1 -0.554855 -0.848800 -0.703222 11.00000 0.02686 0.01554 = 0.04391 -0.00128 -0.01170 -0.00157 C014 1 -0.498419 -0.732188 -0.772159 11.00000 0.03302 0.02696 = 0.03602 -0.00023 -0.00302 0.00019 C015 1 0.053711 -0.349449 -0.796823 11.00000 0.03308 0.01659 = 0.04003 -0.00061 -0.00652 0.00178 C016 1 -0.786950 -0.702562 -0.668287 11.00000 0.03205 0.01706 = 0.05728 -0.00467 -0.01055 0.01130 AFIX 43 H016 2 -0.874253 -0.630002 -0.665861 11.00000 -1.20000 AFIX 0 C017 1 -0.428201 -0.892167 -0.734368 11.00000 0.02876 0.02135 = 0.04096 0.00051 -0.00322 -0.00367 AFIX 43 H017 2 -0.354797 -0.966770 -0.733335 11.00000 -1.20000 AFIX 0 C018 1 -0.225280 -0.407752 -0.708606 11.00000 0.03302 0.02696 = 0.03602 -0.00023 -0.00302 0.00019 C019 1 -0.763767 -0.772963 -0.640710 11.00000 0.03175 0.01555 = 0.04404 0.00186 -0.01623 -0.00576 C01A 1 -0.070875 -0.392218 -0.765692 11.00000 0.03880 0.01713 = 0.03811 0.00373 -0.00895 -0.00499 AFIX 43 H01A 2 -0.155487 -0.465659 -0.766624 11.00000 -1.20000 AFIX 0 C01B 1 -0.265052 -0.907016 -0.791457 11.00000 0.03302 0.02696 = 0.03602 -0.00023 -0.00302 0.00019 C01C 1 -0.397339 -0.844779 -0.764313 11.00000 0.03302 0.02696 = 0.03602 -0.00023 -0.00302 0.00019 PART 7 O7 4 -0.411170 -0.790154 -0.889668 121.00000 0.08161 PART 8 O8 4 0.200768 -0.809485 -0.904073 131.00000 0.06972 PART 9 O9 4 -0.205420 -1.299397 -0.606980 51.00000 0.12421 PART 10 O10 4 -0.094384 -0.810722 -0.891826 141.00000 0.11280 PART 11 O11 4 0.450762 -1.301906 -0.610098 61.00000 0.05346 PART 12 O12 4 0.319208 -0.717934 -0.863718 151.00000 0.08586 PART 13 O13 4 -1.043007 -1.191249 -0.631481 71.00000 0.03437 PART 14 O14 4 0.165286 -1.308976 -0.587554 81.00000 0.01186 HKLF 5 REM bp-1_twin_4-2_twin1_hklf4_a.res in P2(1) REM wR2 = 0.4731, GooF = S = 1.667, Restrained GooF = 1.639 for all data REM R1 = 0.1959 for 4134 Fo > 4sig(Fo) and 0.2474 for all 8407 data REM 353 parameters refined using 485 restraints END WGHT 0.2000 0.0000 REM Highest difference peak 0.666, deepest hole -0.655, 1-sigma level 0.198 Q1 1 -1.0350 -0.6516 -0.4963 11.00000 0.05 0.67 Q2 1 -0.7728 -0.7190 -0.6616 11.00000 0.05 0.65 Q3 1 -1.0705 -0.7633 -0.6016 11.00000 0.05 0.62 Q4 1 0.2705 -0.2183 -0.8387 11.00000 0.05 0.61 Q5 1 0.3793 -1.3031 -0.6175 11.00000 0.05 0.60 ; _shelx_res_checksum 80096 _shelx_hkl_file ; 0 12 13 17.4893 118.984 -2 0 -12 -13 17.4893 118.984 1 0 12 -18 81.0865 101.763 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11170.0 110.378 1 0 11 13 9.07339 63.2171 -2 0 -11 -13 9.07339 63.2171 1 0 11 14 11717.0 112.275 -2 0 -11 -14 11717.0 112.275 1 0 11 -15 1.08903 65.6034 -2 0 -11 15 1.08903 65.6034 1 0 11 -16 549.309 70.1525 -2 0 -11 16 549.309 70.1525 1 0 11 -17-5.68946 82.8203 -2 0 -11 17-5.68946 82.8203 1 0 11 -18 1383.08 93.3606 -2 0 -11 18 1383.08 93.3606 1 0 11 -19-1.67401 84.9754 -2 0 -11 19-1.67401 84.9754 1 0 11 -20 1224.92 94.0586 -2 0 -11 20 1224.92 94.0586 1 0 11 -21-2.59122 86.2537 -2 0 -11 21-2.59122 86.2537 1 0 11 -22 1088.88 98.1662 -2 0 -11 22 1088.88 98.1662 1 0 11 -23-8.18967 90.2936 -2 0 -11 23-8.18967 90.2936 1 0 11 -24 1058.28 100.316 -2 0 -11 24 1058.28 100.316 1 0 11 -25 3.99896 96.6277 -2 0 -11 25 3.99896 96.6277 1 0 11 -26 1169.42 114.470 -2 0 -11 26 1169.42 114.470 1 0 11 -27 7.33037 105.357 -2 0 -11 27 7.33037 105.357 1 0 11 -28 693.099 118.268 -2 0 -11 28 693.099 118.268 1 0 11 -29-1.09231 114.967 -2 0 -11 29-1.09231 114.967 1 0 11 -30 143.366 119.656 -2 0 -11 30 143.366 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221.451 -2 1 -14 -11 1688.87 221.451 1 1 14 9-5.74914 199.344 -2 1 -14 -10-5.74914 199.344 1 1 14 8 215.945 194.899 -2 1 -14 -9 215.945 194.899 1 1 14 7 70.6944 187.138 -2 1 -14 -8 70.6944 187.138 1 1 13 19 214.721 219.101 -2 1 -13 -20 214.721 219.101 1 1 13 18 220.637 222.099 -2 1 -13 -19 220.637 222.099 1 1 13 17 3.96448 215.276 -2 1 -13 -18 3.96448 215.276 1 1 13 16 543.205 207.234 -2 1 -13 -17 543.205 207.234 1 1 13 15 1070.73 198.387 -2 1 -13 -16 1070.73 198.387 1 1 13 14 243.203 187.434 -2 1 -13 -15 243.203 187.434 1 1 13 13 202.284 185.935 -2 1 -13 -14 202.284 185.935 1 1 13 12 377.832 178.553 -2 1 -13 -13 377.832 178.553 1 1 13 11 23.6799 175.611 -2 1 -13 -12 23.6799 175.611 1 1 13 10 222.613 183.418 -2 1 -13 -11 222.613 183.418 1 1 13 9 140.655 175.254 -2 1 -13 -10 140.655 175.254 1 1 13 8 1691.32 188.014 -2 1 -13 -9 1691.32 188.014 1 1 13 7 117.051 175.013 -2 1 -13 -8 117.051 175.013 1 1 13 6 415.878 180.979 -2 1 -13 -7 415.878 180.979 1 1 13 5 1.86465 170.856 -2 1 -13 -6 1.86465 170.856 1 1 13 4 195.998 168.111 -2 1 -13 -5 195.998 168.111 1 1 13 3 72.4677 162.954 -2 1 -13 -4 72.4677 162.954 1 -1 12 -29 31.1194 125.777 -2 -1 -12 30 31.1194 125.777 1 -1 12 -28 390.662 123.318 -2 -1 -12 29 390.662 123.318 1 -1 12 -27 302.016 125.241 -2 -1 -12 28 302.016 125.241 1 -1 12 -26 94.7532 118.501 -2 -1 -12 27 94.7532 118.501 1 1 12 23 728.940 252.011 -2 1 -12 -24 728.940 252.011 1 1 12 22 1376.55 244.665 -2 1 -12 -23 1376.55 244.665 1 1 12 21 6.32850 222.659 -2 1 -12 -22 6.32850 222.659 1 1 12 20 1806.68 231.688 -2 1 -12 -21 1806.68 231.688 1 1 12 19 82.3504 208.819 -2 1 -12 -20 82.3504 208.819 1 1 12 18 519.664 208.442 -2 1 -12 -19 519.664 208.442 1 1 12 17 674.913 200.112 -2 1 -12 -18 674.913 200.112 1 1 12 16 1207.76 193.097 -2 1 -12 -17 1207.76 193.097 1 1 12 15 29.3931 188.769 -2 1 -12 -16 29.3931 188.769 1 1 12 14 597.150 189.415 -2 1 -12 -15 597.150 189.415 1 1 12 13 45.7017 182.903 -2 1 -12 -14 45.7017 182.903 1 1 12 12 292.396 170.781 -2 1 -12 -13 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25 231.980 27.0624 1 1 3 -27 6.70578 26.5009 -2 1 -3 26 6.70578 26.5009 1 1 3 -28 1478.76 38.0193 -2 1 -3 27 1478.76 38.0193 1 -1 3 29 15.8253 29.0995 -2 -1 -3 -28 15.8253 29.0995 1 -1 3 30 99.2015 30.6689 -2 -1 -3 -29 99.2015 30.6689 1 1 3 -31 381.573 50.8559 -2 1 -3 30 381.573 50.8559 1 -1 3 32 215.202 199.718 -2 -1 -3 -31 215.202 199.718 1 -1 3 33 9377.72 267.902 -2 -1 -3 -32 9377.72 267.902 1 -1 3 34 300.156 211.253 -2 -1 -3 -33 300.156 211.253 1 -1 3 35 554.540 216.760 -2 -1 -3 -34 554.540 216.760 1 -1 3 36 708.016 224.106 -2 -1 -3 -35 708.016 224.106 1 -1 3 37 86.5398 231.878 -2 -1 -3 -36 86.5398 231.878 1 1 3 -38 1995.23 53.0072 -2 1 -3 37 1995.23 53.0072 1 1 3 -39 6.85711 41.8538 -2 1 -3 38 6.85711 41.8538 1 1 3 -40 1897.42 54.4283 -2 1 -3 39 1897.42 54.4283 1 1 3 -41 3.91138 43.7212 -2 1 -3 40 3.91138 43.7212 1 1 3 -42 1062.03 54.0280 -2 1 -3 41 1062.03 54.0280 1 1 3 -43 15.1597 49.1036 -2 1 -3 42 15.1597 49.1036 1 1 3 -44 1215.49 57.1524 -2 1 -3 43 1215.49 57.1524 1 1 3 -45 1.64542 54.5593 -2 1 -3 44 1.64542 54.5593 1 1 3 -46 559.137 57.9754 -2 1 -3 45 559.137 57.9754 1 1 3 -47 2.82629 56.8728 -2 1 -3 46 2.82629 56.8728 1 1 3 -48 42.9184 60.5337 -2 1 -3 47 42.9184 60.5337 1 1 3 -49 12.5100 63.0085 -2 1 -3 48 12.5100 63.0085 1 1 2 52 30.6092 155.529 -2 1 -2 -53 30.6092 155.529 1 1 2 51 42.1400 146.529 -2 1 -2 -52 42.1400 146.529 1 -1 2 -50 11.9999 86.5850 -2 -1 -2 51 11.9999 86.5850 1 -1 2 -49-0.65307 85.9236 -2 -1 -2 50-0.65307 85.9236 1 1 2 48 14.5763 77.8590 -2 1 -2 -49 14.5763 77.8590 1 1 2 47 24.1429 72.2381 -2 1 -2 -48 24.1429 72.2381 1 1 2 46 283.581 71.1596 -2 1 -2 -47 283.581 71.1596 1 1 2 45 3.44952 66.0507 -2 1 -2 -46 3.44952 66.0507 1 1 2 44 26.9913 63.4662 -2 1 -2 -45 26.9913 63.4662 1 1 2 43 3.39367 60.8285 -2 1 -2 -44 3.39367 60.8285 1 -1 2 -42 26.8882 58.3717 -2 -1 -2 43 26.8882 58.3717 1 -1 2 -41 53.4364 54.8872 -2 -1 -2 42 53.4364 54.8872 1 1 2 40 244.126 53.3598 -2 1 -2 -41 244.126 53.3598 1 1 2 39 38.7343 51.2006 -2 1 -2 -40 38.7343 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41 0.93166 46.4205 1 -2 -3 -42 340.225 304.629 1 2 3 -44 1240.78 69.0954 -2 2 -3 42 1240.78 69.0954 1 2 -3 43 4.52530 48.2626 1 2 -2 -47-2.61774 195.736 1 2 -2 -46 56.5123 186.158 1 2 -2 -45-7.97340 186.898 1 2 -2 -44 101.560 182.008 1 2 -2 -43-2.55135 173.548 1 2 -2 -42 14.4123 158.116 1 2 -2 -41-2.35065 149.705 1 2 -2 -40 183.946 144.693 1 2 -2 -39 8.74874 139.552 1 2 -2 -38 42.7540 132.537 1 2 -2 -37 2.08922 122.126 1 2 -2 -36 116.366 122.678 1 2 -2 -35-7.97724 118.841 1 2 -2 -34 105.205 117.073 1 2 -2 -33 1.66653 39.1197 1 2 -2 -32 1180.93 43.8747 1 2 -2 -31 0.59830 32.3801 1 2 -2 -30 1143.61 38.9895 1 2 -2 -29 0.86003 27.3091 1 2 -2 -28 3700.83 46.7537 1 2 -2 -27 4.78108 27.5980 1 2 -2 -26 150.267 91.3307 1 2 2 24 3949.43 55.8752 -2 2 -2 -26 3949.43 55.8752 1 2 -2 -25 1.21134 27.3111 1 2 -2 -24 173.061 88.3434 1 2 2 22 474.069 47.2953 -2 2 -2 -24 474.069 47.2953 1 2 -2 -23 14.5285 84.2834 1 2 2 21-2.21124 44.3353 -2 2 -2 -23-2.21124 44.3353 1 2 2 20 3262.71 52.9089 -2 2 -2 -22 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25.7489 59.1862 1 3 5 -33 120.048 59.1033 1 3 5 -32 42.5760 55.2111 1 3 5 -31 458.200 65.7033 1 3 5 -30 117.887 60.7544 1 3 5 -29 454.044 62.2742 1 3 5 -28 85.7509 58.6426 1 3 5 -27 460.820 58.0960 1 3 5 -26 133.746 58.1630 1 3 5 -25 469.903 55.2941 1 3 5 -24 182.911 51.6625 1 3 5 -23 338.462 52.9405 1 3 5 -22 72.8563 49.8623 1 -3 5 21 1690.25 41.3357 1 3 5 -20 38.9870 33.0657 1 -3 5 19 167.313 33.6870 1 -3 5 18 81.6685 29.2937 1 -3 5 17 369.139 31.1001 1 -3 5 16 2.86875 28.1872 1 -3 5 15 169.692 28.5870 1 -3 5 14 35.2077 28.1490 1 3 5 -13 895.467 30.8805 1 -3 5 12 21.8266 24.6136 1 3 5 -11 437.467 26.8123 1 -3 5 10 19.7252 23.8360 1 3 5 -9 396.887 25.8375 1 -3 5 8 76.2023 24.5198 1 3 5 -7 1668.88 33.5031 1 -3 5 6 5.83804 29.9027 1 -3 5 5 209.060 31.3554 1 3 5 -4 81.1143 32.3205 1 -3 5 3 439.276 37.7169 1 3 5 -2 202.674 33.6407 1 3 5 -1 915.096 32.6519 1 3 5 0 68.3088 27.4388 1 3 5 1 368.548 28.9683 1 3 5 2 46.1721 26.2439 1 3 5 3 33.1785 25.9929 1 3 5 4 2.68000 28.8403 1 3 5 5 663.081 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124.068 1 -3 10 -22 1.56416 125.348 1 3 11 -23-3.23938 149.775 1 3 11 -22 69.4821 143.875 1 3 11 -21 1.53940 136.304 1 3 11 -20 414.821 136.737 1 3 11 -19-4.19325 130.650 1 3 11 -18 38.0765 126.950 1 3 11 -17 1.32241 121.330 1 3 11 -16 14.8416 72.2807 1 -3 11 15 227.780 49.8205 1 -3 11 14-0.18989 47.7272 1 3 11 -13 757.229 51.5040 1 -3 11 12 4.33588 58.6547 1 3 -11 10 5.20429 99.5547 -2 3 11 -12 5.20429 99.5547 1 3 11 -11 167.848 42.2784 1 -3 11 10 0.77088 52.4709 1 3 -11 8-3.16392 90.4566 -2 3 11 -10-3.16392 90.4566 1 3 11 -9 647.316 47.1258 1 -3 11 8-0.87221 46.4433 1 -3 11 7 912.462 58.7554 1 3 -11 5 1577.70 129.323 -2 3 11 -7 1577.70 129.323 1 -3 11 6 3.87240 49.7916 1 3 11 -5 253.845 73.3012 1 -3 -11 -2 293.727 83.8365 -2 -3 11 5 293.727 83.8365 1 3 11 -4-0.25927 49.5023 1 3 11 -3 246.132 50.7369 1 3 11 -2 4.38600 93.9542 1 -3 -11 1 127.061 76.1244 -2 -3 11 2 127.061 76.1244 1 3 11 -1 319.172 52.1749 1 -3 11 0 3.79511 61.4292 1 3 -11 -2 15.8368 128.125 -2 3 11 0 15.8368 128.125 1 3 11 1 294.596 57.7261 1 3 11 2 1.04987 54.4573 1 3 11 3 20.6040 52.0263 1 3 11 4 5.99010 50.6611 1 3 11 5 125.514 52.6599 1 3 11 6 2.30861 51.5621 1 3 11 7 188.113 54.1182 1 3 11 8 2.41454 55.0086 1 3 11 9 78.3210 50.5140 1 -3 11 -10 4.33984 74.8477 1 3 11 11 48.9422 61.9966 1 -3 11 -12-2.61267 112.529 1 3 11 13 23.5510 242.312 1 3 11 14-8.96748 250.091 1 3 11 15-9.10750 248.271 1 3 -12 8 2.01068 129.185 -2 3 12 -10 2.01068 129.185 1 3 12 -9 217.090 103.312 1 3 12 -8 3.54912 105.204 1 3 12 -7 44.8241 110.529 1 3 12 -6 4.50070 102.484 1 3 12 -5 670.619 104.114 1 3 12 -4 3.34344 103.838 1 3 12 -3 249.688 108.574 1 3 12 -2-1.14384 107.746 1 3 12 -1 138.296 110.077 1 3 12 0 11.0806 105.522 1 3 12 1 1387.86 112.213 1 3 12 2 3.12925 102.105 1 3 12 3 461.598 96.8505 1 3 12 4-0.98038 100.917 1 3 12 5 40.9328 245.623 1 3 12 6-2.60363 243.366 1 3 12 7 45.0178 248.386 1 3 12 8 13.4498 251.479 1 3 12 9-2.73655 256.784 1 3 12 10 2.78361 255.425 1 4 -8 -8 72.6024 274.068 1 4 -8 -7-3.42780 251.844 1 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6.56973 143.757 1 4 3 -10 388.949 65.2125 -2 4 -3 7 388.949 65.2125 1 4 -3 8 837.695 53.3990 1 4 -3 9-1.54965 140.617 1 4 3 -12 232.339 66.0471 -2 4 -3 9 232.339 66.0471 1 4 -3 10 11.4338 132.449 1 4 3 -13 1122.20 73.2276 -2 4 -3 10 1122.20 73.2276 1 4 -3 11 4.00444 53.9160 1 4 3 -15 116.787 77.9270 -2 4 -3 12 116.787 77.9270 1 4 3 -16 429.951 69.8874 -2 4 -3 13 429.951 69.8874 1 4 3 -17 929.803 71.3191 -2 4 -3 14 929.803 71.3191 1 4 -3 15 13.3151 56.1644 1 4 -3 16 2390.82 62.3119 1 4 -3 17 87.0568 46.0040 1 4 -3 18 332.582 46.6409 1 4 -3 19 20.7044 41.9496 1 4 -3 20 61.7665 46.6472 1 4 -3 21 2.85672 51.9735 1 4 -3 22 185.528 61.1451 1 4 -2 -28 20.1212 242.129 1 4 -2 -27-12.5265 217.508 1 4 -2 -26 74.2417 218.562 1 4 -2 -25-12.2246 216.513 1 4 -2 -24 145.905 213.081 1 4 -2 -23 16.0611 181.336 1 4 -2 -22 208.913 184.318 1 4 -2 -21-10.2290 175.223 1 4 -2 -20 140.238 171.883 1 4 2 17 65.3334 71.1774 -2 4 -2 -20 65.3334 71.1774 1 4 -2 -19-9.90208 167.404 1 4 2 16 131.501 72.1189 -2 4 -2 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3 159.973 55.4433 -2 4 -2 -6 159.973 55.4433 1 4 -2 -5 2.22794 165.933 1 4 2 2 121.825 53.1991 -2 4 -2 -5 121.825 53.1991 1 4 -2 -4 119.951 170.559 1 4 2 1 86.2690 54.5137 -2 4 -2 -4 86.2690 54.5137 1 4 -2 -3 2.38026 182.335 1 4 2 0 94.4837 55.5449 -2 4 -2 -3 94.4837 55.5449 1 4 -2 -2 53.1675 182.047 1 4 2 -1 114.787 55.9192 -2 4 -2 -2 114.787 55.9192 1 4 -2 -1 19.9273 177.767 1 4 2 -2 60.0761 58.4054 -2 4 -2 -1 60.0761 58.4054 1 4 -2 0 32.1741 170.573 1 4 2 -3 218.234 56.3675 -2 4 -2 0 218.234 56.3675 1 4 -2 1-2.07927 163.498 1 4 2 -4 45.7275 53.2612 -2 4 -2 1 45.7275 53.2612 1 4 -2 2 49.2217 163.736 1 4 2 -5 341.641 52.9059 -2 4 -2 2 341.641 52.9059 1 4 -2 3-1.91458 158.818 1 4 2 -6 95.1956 55.9779 -2 4 -2 3 95.1956 55.9779 1 4 -2 4 22.1409 177.036 1 4 2 -7 372.187 59.8300 -2 4 -2 4 372.187 59.8300 1 4 -2 5 3.80774 163.045 1 4 2 -8 53.4093 64.0561 -2 4 -2 5 53.4093 64.0561 1 4 -2 6 49.2412 155.545 1 4 2 -9 192.281 68.8630 -2 4 -2 6 192.281 68.8630 1 4 -2 7-1.56478 139.730 1 4 2 -10 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82.9249 84.8846 -2 4 -1 -23 82.9249 84.8846 1 4 -1 -22 356.796 195.227 1 4 1 19 1192.54 87.8627 -2 4 -1 -22 1192.54 87.8627 1 4 -1 -21 8.45343 197.327 1 4 1 18 222.449 81.3323 -2 4 -1 -21 222.449 81.3323 1 4 -1 -20 135.780 198.013 1 4 1 17 1475.92 86.2999 -2 4 -1 -20 1475.92 86.2999 1 4 -1 -19 10.7823 193.820 1 4 1 16 89.8576 75.9152 -2 4 -1 -19 89.8576 75.9152 1 4 -1 -18 228.969 173.651 1 4 1 15 1062.82 81.7490 -2 4 -1 -18 1062.82 81.7490 1 4 -1 -17 11.7938 163.964 1 4 1 14 125.031 73.1911 -2 4 -1 -17 125.031 73.1911 1 4 -1 -16 63.8239 154.733 1 4 1 13 92.6279 72.0746 -2 4 -1 -16 92.6279 72.0746 1 4 -1 -15 6.69215 155.047 1 4 1 12 41.8770 65.8195 -2 4 -1 -15 41.8770 65.8195 1 4 -1 -14 150.123 163.075 1 4 1 11 145.108 68.5432 -2 4 -1 -14 145.108 68.5432 1 4 -1 -13-2.26534 160.488 1 4 1 10 90.0801 69.4639 -2 4 -1 -13 90.0801 69.4639 1 4 -1 -12 454.187 166.371 1 4 1 9 110.973 68.4333 -2 4 -1 -12 110.973 68.4333 1 4 -1 -11 2.43364 175.897 1 4 1 8 263.555 69.8706 -2 4 -1 -11 263.555 69.8706 1 4 -1 -10 26.7604 169.283 1 4 1 7 380.105 71.8539 -2 4 -1 -10 380.105 71.8539 1 4 -1 -9 29.9941 170.001 1 4 1 6 9.67411 70.2729 -2 4 -1 -9 9.67411 70.2729 1 4 -1 -8 122.594 190.520 1 4 1 5 540.548 89.9272 -2 4 -1 -8 540.548 89.9272 1 4 -1 -7-2.64823 199.322 1 4 1 4 63.0397 71.0058 -2 4 -1 -7 63.0397 71.0058 1 4 -1 -6 119.243 200.321 1 4 1 3 53.6323 70.7884 -2 4 -1 -6 53.6323 70.7884 1 4 -1 -5-2.25314 178.126 1 4 1 2 93.9121 69.9296 -2 4 -1 -5 93.9121 69.9296 1 4 -1 -4 160.827 160.148 1 4 1 1 89.3202 66.4414 -2 4 -1 -4 89.3202 66.4414 1 4 -1 -3-4.03260 155.960 1 4 1 0 91.8161 55.8726 -2 4 -1 -3 91.8161 55.8726 1 4 -1 -2 33.2780 167.117 1 4 1 -1 38.2442 54.2097 -2 4 -1 -2 38.2442 54.2097 1 4 -1 -1 29.9298 171.721 1 4 1 -2 19.2002 50.6555 -2 4 -1 -1 19.2002 50.6555 1 4 -1 0 28.9260 173.236 1 4 1 -3 245.837 56.1266 -2 4 -1 0 245.837 56.1266 1 4 -1 1 7.96270 172.075 1 4 1 -4 35.1526 53.9975 -2 4 -1 1 35.1526 53.9975 1 4 -1 2 41.1926 161.981 1 4 1 -5 237.581 61.7142 -2 4 -1 2 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82.1497 1 4 -3 -7 16.0615 78.0547 -2 4 3 4 16.0615 78.0547 1 4 -3 -8 57.4899 72.9831 -2 4 3 5 57.4899 72.9831 1 4 -3 -9 276.720 65.2073 -2 4 3 6 276.720 65.2073 1 4 -3 -10 516.612 64.0042 -2 4 3 7 516.612 64.0042 1 4 -3 -11 800.817 55.3901 -2 4 3 8 800.817 55.3901 1 -4 3 -9 8.55896 74.4771 1 -4 -3 13 534.035 94.3590 -2 -4 3 -10 534.035 94.3590 1 -4 3 -11 63.6994 77.2182 1 -4 3 -12 28.9658 76.7564 1 -4 3 -13 565.066 82.0692 1 -4 3 -14 278.745 77.9330 1 4 -3 -17 657.948 73.4194 -2 4 3 14 657.948 73.4194 1 -4 3 -15 146.943 80.7247 1 4 -3 -18 182.734 79.1834 -2 4 3 15 182.734 79.1834 1 -4 3 -16 2478.53 69.7700 1 -4 3 -17 125.236 108.760 1 4 -3 -20 350.021 92.1697 -2 4 3 17 350.021 92.1697 1 -4 3 -18 387.064 60.4567 1 -4 3 -19 3.02969 117.434 1 4 -3 -22 85.5829 78.3726 -2 4 3 19 85.5829 78.3726 1 -4 3 -20 39.8025 56.8771 1 -4 3 -21-8.56493 112.785 1 4 -3 -24 133.697 80.9056 -2 4 3 21 133.697 80.9056 1 -4 3 -22 139.628 58.9018 1 -4 3 -23 9.11527 64.5746 1 -4 3 -24 31.1308 161.040 1 -4 3 -25 15.8624 173.764 1 4 4 -28 72.0323 142.156 1 4 4 -27-22.4196 138.901 1 4 4 -26 55.1342 142.057 1 4 4 -25-30.4325 134.769 1 4 4 -24 89.5879 132.422 1 4 -4 21 109.931 79.7775 -2 4 4 -24 109.931 79.7775 1 4 4 -23-6.52731 130.424 1 4 -4 20 98.7952 85.7151 -2 4 4 -23 98.7952 85.7151 1 4 4 -22 344.102 136.021 1 4 -4 19 667.709 91.3200 -2 4 4 -22 667.709 91.3200 1 4 4 -21-7.84870 129.672 1 4 -4 18 368.639 88.8401 -2 4 4 -21 368.639 88.8401 1 4 4 -20 88.6364 133.265 1 4 -4 17 115.700 89.6938 -2 4 4 -20 115.700 89.6938 1 4 4 -19 14.5198 125.725 1 4 -4 16 95.7326 91.3158 -2 4 4 -19 95.7326 91.3158 1 4 4 -18 20.5656 131.561 1 4 -4 15 499.177 95.3637 -2 4 4 -18 499.177 95.3637 1 4 4 -17 1.47000 122.567 1 4 -4 14 22.6525 86.3599 -2 4 4 -17 22.6525 86.3599 1 4 4 -16 190.517 113.025 1 4 -4 13 170.326 81.9089 -2 4 4 -16 170.326 81.9089 1 4 4 -15 23.9301 117.089 1 4 -4 12 143.869 84.0428 -2 4 4 -15 143.869 84.0428 1 4 4 -14 426.556 113.068 1 4 -4 11 782.657 87.8465 -2 4 4 -14 782.657 87.8465 1 4 4 -13 8.57936 103.142 1 4 -4 10 301.569 85.1657 -2 4 4 -13 301.569 85.1657 1 4 4 -12 134.868 98.7775 1 4 -4 9 38.7177 83.6708 -2 4 4 -12 38.7177 83.6708 1 4 4 -11 35.1782 94.8924 1 4 -4 8 103.997 85.9930 -2 4 4 -11 103.997 85.9930 1 4 4 -10 104.239 97.1485 1 4 -4 7 989.924 93.6366 -2 4 4 -10 989.924 93.6366 1 4 4 -9 6.73337 99.9602 1 4 -4 6 90.5477 87.6944 -2 4 4 -9 90.5477 87.6944 1 4 4 -8 322.364 117.553 1 4 -4 5 520.692 91.3766 -2 4 4 -8 520.692 91.3766 1 4 -4 4 291.659 84.9223 -2 4 4 -7 291.659 84.9223 1 4 -4 3 14.6023 84.5836 -2 4 4 -6 14.6023 84.5836 1 4 -4 2 49.9597 82.2720 -2 4 4 -5 49.9597 82.2720 1 4 -4 1 320.442 78.3933 -2 4 4 -4 320.442 78.3933 1 4 -4 0 120.123 80.7580 -2 4 4 -3 120.123 80.7580 1 4 -4 -1 98.6424 80.0590 -2 4 4 -2 98.6424 80.0590 1 4 -4 -2 48.3540 80.7921 -2 4 4 -1 48.3540 80.7921 1 4 -4 -3 171.232 82.7798 -2 4 4 0 171.232 82.7798 1 4 -4 -4 219.488 87.1719 -2 4 4 1 219.488 87.1719 1 4 -4 -5 166.518 106.197 -2 4 4 2 166.518 106.197 1 -4 -4 7 506.188 97.1040 -2 -4 4 -4 506.188 97.1040 1 -4 -4 8 523.926 105.743 -2 -4 4 -5 523.926 105.743 1 -4 -4 9 312.707 104.903 -2 -4 4 -6 312.707 104.903 1 -4 -4 10 936.394 98.3591 -2 -4 4 -7 936.394 98.3591 1 -4 4 -8 169.930 58.7880 1 4 4 9 38.9375 104.692 1 4 -4 -12 33.9869 48.9852 -2 4 4 9 33.9869 48.9852 1 4 4 10 87.8800 96.2582 1 4 -4 -13 754.793 55.9015 -2 4 4 10 754.793 55.9015 1 -4 4 -11 5.79659 65.4670 1 4 -4 -14 731.782 68.9906 -2 4 4 11 731.782 68.9906 1 4 4 12 41.0975 101.971 1 4 -4 -15 333.793 59.0013 -2 4 4 12 333.793 59.0013 1 -4 4 -13 81.2760 74.1097 1 4 -4 -16 128.516 68.7092 -2 4 4 13 128.516 68.7092 1 -4 4 -14 32.1465 83.9481 1 4 -4 -17 84.6702 70.1139 -2 4 4 14 84.6702 70.1139 1 -4 4 -15 112.551 94.2734 1 4 -4 -18 318.338 77.7758 -2 4 4 15 318.338 77.7758 1 4 4 16 8.46677 147.426 1 4 -4 -19 282.894 77.3996 -2 4 4 16 282.894 77.3996 1 -4 4 -17 9.05700 105.190 1 4 -4 -20 99.5286 98.4013 -2 4 4 17 99.5286 98.4013 1 -4 4 -18 372.972 105.918 1 4 -4 -21 1337.69 104.226 -2 4 4 18 1337.69 104.226 1 -4 4 -19 14.6832 58.2880 1 4 4 20 273.076 59.4592 1 -4 4 -21 6.02194 61.5583 1 4 4 22 326.582 65.2137 1 -4 4 -23 5.70304 204.794 1 4 5 -27-6.54136 139.982 1 4 5 -26 54.5443 135.992 1 4 5 -25-13.9186 127.660 1 4 5 -24 16.6728 128.764 1 4 5 -23-11.8892 124.358 1 4 5 -22 234.586 123.764 1 4 5 -21 9.99197 119.162 1 4 -5 18 156.459 86.6957 -2 4 5 -21 156.459 86.6957 1 4 5 -20 183.096 123.632 1 4 -5 17 740.230 94.3069 -2 4 5 -20 740.230 94.3069 1 4 5 -19-11.4752 123.858 1 4 -5 16 262.022 97.7160 -2 4 5 -19 262.022 97.7160 1 4 5 -18 2.85917 119.727 1 4 -5 15 108.358 95.3588 -2 4 5 -18 108.358 95.3588 1 4 5 -17 54.7296 117.929 1 4 -5 14 23.4174 97.5166 -2 4 5 -17 23.4174 97.5166 1 4 5 -16 336.498 119.901 1 4 -5 13 902.424 102.456 -2 4 5 -16 902.424 102.456 1 4 5 -15-5.52431 118.781 1 4 -5 12 278.086 89.5082 -2 4 5 -15 278.086 89.5082 1 4 5 -14 209.215 124.168 1 4 -5 11 171.883 83.9980 -2 4 5 -14 171.883 83.9980 1 4 5 -13-3.90497 115.254 1 4 -5 10 160.325 88.8841 -2 4 5 -13 160.325 88.8841 1 4 5 -12 719.856 113.719 1 4 -5 9 33.0026 88.6965 -2 4 5 -12 33.0026 88.6965 1 4 -5 8 560.789 92.3090 -2 4 5 -11 560.789 92.3090 1 4 -5 7 706.452 96.0275 -2 4 5 -10 706.452 96.0275 1 4 -5 6 199.925 95.0108 -2 4 5 -9 199.925 95.0108 1 4 -5 5 562.351 96.3981 -2 4 5 -8 562.351 96.3981 1 4 -5 4 160.178 91.3463 -2 4 5 -7 160.178 91.3463 1 4 -5 3 182.674 89.4946 -2 4 5 -6 182.674 89.4946 1 4 -5 2 132.198 89.2361 -2 4 5 -5 132.198 89.2361 1 4 -5 1 29.7272 88.4017 -2 4 5 -4 29.7272 88.4017 1 -4 -5 5 243.656 81.1851 -2 -4 5 -2 243.656 81.1851 1 4 -5 -6 166.785 67.5272 -2 4 5 3 166.785 67.5272 1 4 -5 -7 405.127 63.6592 -2 4 5 4 405.127 63.6592 1 4 -5 -8 320.406 64.3841 -2 4 5 5 320.406 64.3841 1 4 -5 -9 491.939 65.5613 -2 4 5 6 491.939 65.5613 1 4 -5 -10 697.993 66.2149 -2 4 5 7 697.993 66.2149 1 4 -5 -11 1267.85 65.2072 -2 4 5 8 1267.85 65.2072 1 -4 5 -9 30.0551 65.5147 1 4 -5 -12 26.9928 69.3460 -2 4 5 9 26.9928 69.3460 1 4 -5 -13 359.540 55.4026 -2 4 5 10 359.540 55.4026 1 4 5 11 145.845 111.917 1 4 -5 -14 152.815 62.1184 -2 4 5 11 152.815 62.1184 1 4 5 12 86.7785 129.692 1 4 -5 -15 632.249 60.7809 -2 4 5 12 632.249 60.7809 1 4 5 13 564.728 149.489 1 4 -5 -16 586.223 60.2409 -2 4 5 13 586.223 60.2409 1 4 5 14 13.1634 153.713 1 4 -5 -17 36.6555 57.4853 -2 4 5 14 36.6555 57.4853 1 -4 5 -15 10.1440 71.8426 1 4 -5 -18 54.4090 78.1726 -2 4 5 15 54.4090 78.1726 1 -4 5 -16 216.791 82.5724 1 4 -5 -19 608.217 87.8228 -2 4 5 16 608.217 87.8228 1 -4 5 -17 26.4013 93.0354 1 4 -5 -20 490.891 90.6481 -2 4 5 17 490.891 90.6481 1 -4 5 -18 217.884 101.766 1 4 -5 -21 616.301 109.544 -2 4 5 18 616.301 109.544 1 -4 5 -19-6.46632 150.727 1 4 -5 -22 90.6486 103.293 -2 4 5 19 90.6486 103.293 1 -4 5 -20 73.5454 156.836 1 4 -5 -23 178.822 101.736 -2 4 5 20 178.822 101.736 1 -4 5 -21 11.2459 164.574 1 4 -5 -24 104.601 91.7356 -2 4 5 21 104.601 91.7356 1 4 6 -26 16.2070 138.785 1 4 6 -25 4.76562 139.701 1 4 6 -24 248.966 137.909 1 4 6 -23-18.2878 129.332 1 4 6 -22 47.2826 137.670 1 4 6 -21-4.47894 128.907 1 4 6 -20 12.4838 123.863 1 4 6 -19 2.71408 119.750 1 4 6 -18 26.0905 119.917 1 4 6 -17-7.65256 116.567 1 4 -6 14 11.0388 105.029 -2 4 6 -17 11.0388 105.029 1 4 6 -16 68.6020 114.066 1 4 -6 13 79.4596 103.886 -2 4 6 -16 79.4596 103.886 1 4 6 -15 2.55225 120.720 1 4 -6 12 73.2508 94.8154 -2 4 6 -15 73.2508 94.8154 1 4 -6 11 202.056 89.7559 -2 4 6 -14 202.056 89.7559 1 4 -6 10 56.9961 91.8574 -2 4 6 -13 56.9961 91.8574 1 4 -6 9 187.426 95.6711 -2 4 6 -12 187.426 95.6711 1 4 -6 8 79.6174 95.3753 -2 4 6 -11 79.6174 95.3753 1 4 -6 7 32.3949 95.7948 -2 4 6 -10 32.3949 95.7948 1 4 -6 0 246.172 93.5955 -2 4 6 -3 246.172 93.5955 1 4 -6 -1 1305.34 95.7420 -2 4 6 -2 1305.34 95.7420 1 4 -6 -2 728.472 58.6856 -2 4 6 -1 728.472 58.6856 1 4 -6 -3 427.456 61.7298 -2 4 6 0 427.456 61.7298 1 4 -6 -4 254.616 59.4177 -2 4 6 1 254.616 59.4177 1 4 -6 -5 1008.75 63.1808 -2 4 6 2 1008.75 63.1808 1 4 -6 -6 223.908 63.8754 -2 4 6 3 223.908 63.8754 1 4 -6 -7 899.380 65.2958 -2 4 6 4 899.380 65.2958 1 4 -6 -8 388.894 61.3784 -2 4 6 5 388.894 61.3784 1 4 -6 -9 343.804 61.1053 -2 4 6 6 343.804 61.1053 1 4 -6 -10 41.3637 60.0150 -2 4 6 7 41.3637 60.0150 1 4 -6 -11 145.792 56.6011 -2 4 6 8 145.792 56.6011 1 4 6 9 137.831 121.812 1 4 -6 -12 137.337 61.7391 -2 4 6 9 137.337 61.7391 1 -4 6 -10 133.717 93.6523 1 4 -6 -13 122.794 80.3637 -2 4 6 10 122.794 80.3637 1 -4 6 -11 1.30752 94.4678 1 4 -6 -14 89.2219 77.2398 -2 4 6 11 89.2219 77.2398 1 -4 6 -12 155.184 94.5146 1 4 -6 -15 254.094 88.1933 -2 4 6 12 254.094 88.1933 1 -4 6 -13 1.13576 81.6008 1 4 -6 -16 30.8425 80.6643 -2 4 6 13 30.8425 80.6643 1 -4 6 -14 24.1167 69.4293 1 4 -6 -17 53.8043 78.8984 -2 4 6 14 53.8043 78.8984 1 -4 6 -15 1.90645 68.8832 1 4 -6 -18 177.805 78.2837 -2 4 6 15 177.805 78.2837 1 -4 6 -16 15.5201 80.1403 1 4 -6 -19 6.88471 83.1896 -2 4 6 16 6.88471 83.1896 1 -4 6 -17-3.73462 89.8726 1 4 -6 -20 3.69110 102.826 -2 4 6 17 3.69110 102.826 1 -4 6 -18 166.644 108.507 1 4 -6 -21 198.201 104.165 -2 4 6 18 198.201 104.165 1 4 7 -24 6.06450 146.296 1 4 7 -23 2.96842 142.314 1 4 7 -22 30.4976 132.936 1 4 7 -21 1.42067 134.724 1 4 7 -20 52.4903 131.364 1 4 -7 7 119.138 103.734 -2 4 7 -10 119.138 103.734 1 4 -7 6 192.693 108.641 -2 4 7 -9 192.693 108.641 1 4 -7 5 241.617 109.351 -2 4 7 -8 241.617 109.351 1 4 -7 4 58.5322 107.390 -2 4 7 -7 58.5322 107.390 1 4 -7 3 48.5235 106.451 -2 4 7 -6 48.5235 106.451 1 4 -7 2 231.757 107.156 -2 4 7 -5 231.757 107.156 1 4 -7 1 228.189 57.1759 -2 4 7 -4 228.189 57.1759 1 4 -7 0 148.448 54.3057 -2 4 7 -3 148.448 54.3057 1 4 -7 -1 257.598 53.3995 -2 4 7 -2 257.598 53.3995 1 4 -7 -2 170.858 55.6723 -2 4 7 -1 170.858 55.6723 1 4 -7 -3 266.437 57.8001 -2 4 7 0 266.437 57.8001 1 4 -7 -4 163.901 56.8467 -2 4 7 1 163.901 56.8467 1 4 -7 -5 527.489 60.7895 -2 4 7 2 527.489 60.7895 1 4 -7 -6 68.0287 59.9761 -2 4 7 3 68.0287 59.9761 1 4 -7 -7 162.208 69.3086 -2 4 7 4 162.208 69.3086 1 4 -7 -8 201.627 68.4464 -2 4 7 5 201.627 68.4464 1 4 -7 -9 460.789 68.5928 -2 4 7 6 460.789 68.5928 1 4 -7 -10 137.026 65.2995 -2 4 7 7 137.026 65.2995 1 4 -7 -11 65.5438 66.1871 -2 4 7 8 65.5438 66.1871 1 4 7 9 2.12334 156.307 1 4 -7 -12 10.2756 63.0502 -2 4 7 9 10.2756 63.0502 1 4 -7 -13 51.4238 62.0630 -2 4 7 10 51.4238 62.0630 1 4 -7 -14 62.0203 68.5621 -2 4 7 11 62.0203 68.5621 1 4 -7 -15 0.73352 76.0520 -2 4 7 12 0.73352 76.0520 1 4 -7 -16 36.1562 77.0889 -2 4 7 13 36.1562 77.0889 1 4 -7 -17 159.713 72.1652 -2 4 7 14 159.713 72.1652 1 4 -7 -18 39.1664 85.2764 -2 4 7 15 39.1664 85.2764 1 -4 -8 -3 67.5973 66.9855 -2 -4 8 6 67.5973 66.9855 1 -4 -8 -2 35.5297 69.6824 -2 -4 8 5 35.5297 69.6824 1 4 -8 1 647.831 59.0855 -2 4 8 -4 647.831 59.0855 1 4 -8 0 402.821 54.7080 -2 4 8 -3 402.821 54.7080 1 4 -8 -1 85.6387 55.3218 -2 4 8 -2 85.6387 55.3218 1 4 -8 -2 63.9949 57.2914 -2 4 8 -1 63.9949 57.2914 1 4 -8 -3 650.312 60.0778 -2 4 8 0 650.312 60.0778 1 4 -8 -4 545.461 60.5673 -2 4 8 1 545.461 60.5673 1 4 -8 -5 29.6558 61.9931 -2 4 8 2 29.6558 61.9931 1 4 -8 -6 44.0455 65.5332 -2 4 8 3 44.0455 65.5332 1 4 -8 -7 464.474 72.8815 -2 4 8 4 464.474 72.8815 1 4 -8 -8 155.435 71.7531 -2 4 8 5 155.435 71.7531 1 4 -8 -9 95.4454 80.1665 -2 4 8 6 95.4454 80.1665 1 4 -8 -10 80.8854 82.9221 -2 4 8 7 80.8854 82.9221 1 4 -8 -11 335.842 106.119 -2 4 8 8 335.842 106.119 1 4 -9 8 20.2140 180.067 -2 4 9 -11 20.2140 180.067 1 4 -9 7-24.6080 180.615 -2 4 9 -10-24.6080 180.615 1 4 -9 6 53.6084 179.696 -2 4 9 -9 53.6084 179.696 1 4 -9 5-13.6632 160.526 -2 4 9 -8-13.6632 160.526 1 4 -9 4 94.3948 163.563 -2 4 9 -7 94.3948 163.563 1 4 -9 3-7.94943 167.301 -2 4 9 -6-7.94943 167.301 1 ; _shelx_hkl_checksum 21278 _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 4.920 _oxdiff_exptl_absorpt_empirical_full_min 0.241 _oxdiff_twin_integration_method simultaneous _oxdiff_twin_items 2 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -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 O1 O 0.590(17) -0.687(5) -0.8689(16) 0.060(16) Uiso 0.26(3) 1 d . U P A 1 O2 O -0.32(2) -1.225(8) -0.633(2) 0.079(16) Uiso 0.22(4) 1 d . U P B 2 O3 O -0.18(2) -0.694(7) -0.841(2) 0.051(17) Uiso 0.15(2) 1 d . U P C 3 O4 O -0.645(17) -1.213(6) -0.6358(16) 0.070(15) Uiso 0.26(3) 1 d . U P D 4 O5 O 0.067(18) -0.711(5) -0.8647(15) 0.056(14) Uiso 0.25(3) 1 d . U P E 5 O6 O -0.36(2) -1.197(7) -0.652(2) 0.074(16) Uiso 0.21(3) 1 d . U P F 6 C001 C 0.795(4) -0.1570(16) -1.0138(4) 0.0321(9) Uani 1 1 d . U . . . C22 C -1.045(4) -0.6582(14) -0.5441(5) 0.0288(15) Uani 1 1 d . U . . . C003 C 0.011(4) -0.2312(16) -0.7277(5) 0.0321(9) Uani 1 1 d . . . . . C27 C 0.628(4) -0.1105(15) -0.9873(4) 0.029(3) Uani 1 1 d . U . . . H27 H 0.561715 -0.035651 -0.990166 0.035 Uiso 1 1 calc R U . . . N005 N -1.502(4) -0.8648(14) -0.4822(4) 0.039(4) Uani 1 1 d . U . . . N006 N 1.007(4) -0.3642(13) -1.0179(4) 0.044(4) Uani 1 1 d . . . . . N007 N -1.466(4) -0.5382(13) -0.4356(4) 0.044(4) Uani 1 1 d . U . . . C24 C -0.684(4) -0.7373(14) -0.6991(5) 0.030(4) Uani 1 1 d . . . . . H24 H -0.699198 -0.688344 -0.717056 0.01(4) Uiso 1 1 calc R . . . . N009 N 0.083(5) -0.1382(13) -0.7210(4) 0.052(5) Uani 1 1 d . . . . . C00A C 0.914(4) -0.2725(17) -1.0163(4) 0.0321(9) Uani 1 1 d . U . . . C26 C 0.320(4) -0.1190(15) -0.9017(5) 0.0301(13) Uani 1 1 d . U . . . H26 H 0.235351 -0.067251 -0.886639 0.036 Uiso 1 1 calc R U . . . C21 C -0.998(4) -0.8085(15) -0.5844(4) 0.0288(15) Uani 1 1 d . U . . . H21 H -1.026709 -0.883852 -0.590010 0.028(9) Uiso 1 1 calc R U . . . C23 C -0.539(5) -0.9183(14) -0.6757(4) 0.033(4) Uani 1 1 d . . . . . H23 H -0.451880 -0.990955 -0.677954 0.07(7) Uiso 1 1 calc R . . . . C20 C -1.089(4) -0.7712(15) -0.5531(4) 0.0288(15) Uani 1 1 d . U . . . H20 H -1.180111 -0.821873 -0.538101 0.028(9) Uiso 1 1 calc R U . . . C25 C 0.138(4) -0.3840(14) -0.8548(4) 0.0301(13) Uani 1 1 d . U . . . H25 H 0.130664 -0.433909 -0.872542 0.02(4) Uiso 1 1 calc R . . . . N00G N -0.157(4) -0.9572(13) -0.8134(4) 0.048(5) Uani 1 1 d . . . . . C00H C -1.134(4) -0.6106(15) -0.5120(4) 0.031(3) Uani 1 1 d . U . . . H00H H -1.071443 -0.535618 -0.508981 0.037 Uiso 1 1 calc R U . . . N00I N 0.963(4) -0.0384(12) -1.0644(4) 0.040(4) Uani 1 1 d . U . . . C00J C 0.283(4) -0.2013(15) -0.8318(4) 0.0301(13) Uani 1 1 d . U . . . H00J H 0.364961 -0.128177 -0.834339 0.036 Uiso 1 1 calc R U . . . C00K C 0.259(4) -0.2726(15) -0.8592(4) 0.0301(13) Uani 1 1 d . U . . . C00L C -1.376(4) -0.5901(15) -0.4578(5) 0.0321(9) Uani 1 1 d . . . . . C00M C -0.897(4) -0.5845(14) -0.5675(4) 0.0288(15) Uani 1 1 d . U . . . H00M H -0.853831 -0.510134 -0.561554 0.031(9) Uiso 1 1 calc R U . . . C00N C -0.813(4) -0.6195(14) -0.5988(4) 0.0288(15) Uani 1 1 d . U . . . H00N H -0.725301 -0.568870 -0.613968 0.035 Uiso 1 1 calc R U . . . C00O C -0.647(4) -0.8843(13) -0.6449(4) 0.028(3) Uani 1 1 d . U . . . H00O H -0.641634 -0.934306 -0.627235 0.028(9) Uiso 1 1 calc R U . . . N00P N -0.582(4) -0.6391(14) -0.7790(4) 0.045(4) Uani 1 1 d . U . . . C00Q C 0.406(4) -0.0842(14) -0.9329(4) 0.0301(13) Uani 1 1 d . U . . . H00Q H 0.374932 -0.009130 -0.938729 0.032(9) Uiso 1 1 calc R U . . . C00R C 0.033(4) -0.4181(15) -0.8243(4) 0.0301(13) Uani 1 1 d . U . . . H00R H -0.056661 -0.490431 -0.822111 0.036 Uiso 1 1 calc R U . . . C00S C -1.293(4) -0.6581(15) -0.4861(4) 0.0321(9) Uani 1 1 d . U . . . C00T C 0.882(4) -0.0908(16) -1.0422(5) 0.0321(9) Uani 1 1 d . U . . . C00U C 0.186(4) -0.2372(15) -0.8009(5) 0.0301(13) Uani 1 1 d . . . . . H00U H 0.207402 -0.188974 -0.782812 0.01(4) Uiso 1 1 calc R . . . . C00V C 0.359(4) -0.2336(14) -0.8924(4) 0.0301(13) Uani 1 1 d . U . . . C00W C -0.864(4) -0.7335(14) -0.6074(4) 0.0288(15) Uani 1 1 d . U . . . N00X N -0.342(4) -0.4555(15) -0.6864(4) 0.049(5) Uani 1 1 d . U . . . C00Y C -0.085(4) -0.3439(15) -0.7359(4) 0.0321(9) Uani 1 1 d . . . . . C00Z C -1.403(4) -0.7727(17) -0.4839(4) 0.0321(9) Uani 1 1 d . U . . . C010 C 0.499(4) -0.3084(15) -0.9159(4) 0.0301(13) Uani 1 1 d . . . . . H010 H 0.533772 -0.383355 -0.910146 0.03(4) Uiso 1 1 calc R . . . . C011 C 0.537(4) -0.1583(14) -0.9558(5) 0.0301(13) Uani 1 1 d . U . . . C012 C 0.584(4) -0.2727(15) -0.9471(4) 0.0301(13) Uani 1 1 d . U . . . H012 H 0.672702 -0.323424 -0.962212 0.036 Uiso 1 1 calc R U . . . C013 C -0.555(4) -0.8488(15) -0.7032(5) 0.029(3) Uani 1 1 d . U . . . C014 C -0.498(4) -0.7322(17) -0.7722(5) 0.0321(9) Uani 1 1 d . U . . . C015 C 0.054(4) -0.3494(15) -0.7968(5) 0.0301(13) Uani 1 1 d . . . . . C016 C -0.787(4) -0.7026(15) -0.6683(5) 0.036(4) Uani 1 1 d . . . . . H016 H -0.874253 -0.630002 -0.665861 0.043 Uiso 1 1 calc R U . . . C017 C -0.428(4) -0.8922(15) -0.7344(4) 0.030(5) Uani 1 1 d . . . . . H017 H -0.354797 -0.966770 -0.733335 0.037 Uiso 1 1 calc R U . . . C018 C -0.225(4) -0.4078(15) -0.7086(5) 0.0321(9) Uani 1 1 d . . . . . C019 C -0.764(4) -0.7730(15) -0.6407(4) 0.031(4) Uani 1 1 d . . . . . C01A C -0.071(4) -0.3922(14) -0.7657(4) 0.032(5) Uani 1 1 d . . . . . H01A H -0.155487 -0.465659 -0.766624 0.038 Uiso 1 1 calc R U . . . C01B C -0.265(4) -0.9070(16) -0.7915(5) 0.0321(9) Uani 1 1 d . . . . . C01C C -0.397(4) -0.8448(15) -0.7643(4) 0.0321(9) Uani 1 1 d . . . . . O7 O -0.411(12) -0.790(4) -0.8897(10) 0.082(15) Uiso 0.43(4) 1 d . . P G 7 O8 O 0.201(16) -0.809(5) -0.9041(14) 0.07(2) Uiso 0.28(3) 1 d . . P H 8 O9 O -0.205(14) -1.299(4) -0.6070(12) 0.12(2) Uiso 0.49(4) 1 d . . P I 9 O10 O -0.09(2) -0.811(6) -0.8918(16) 0.11(3) Uiso 0.32(4) 1 d . . P J 10 O11 O 0.451(10) -1.302(3) -0.6101(9) 0.053(13) Uiso 0.36(3) 1 d . . P K 11 O12 O 0.319(19) -0.718(5) -0.8637(15) 0.09(2) Uiso 0.32(4) 1 d . . P L 12 O13 O -1.043(11) -1.191(4) -0.6315(11) 0.034(15) Uiso 0.27(3) 1 d . . P M 13 O14 O 0.165(10) -1.309(4) -0.5876(10) 0.012(12) Uiso 0.19(2) 1 d . . P N 14 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 C001 0.0330(13) 0.0270(13) 0.0360(13) -0.0002(14) -0.0030(10) 0.0002(13) C22 0.030(2) 0.017(3) 0.039(3) -0.001(2) -0.007(2) -0.002(2) C003 0.0330(13) 0.0270(13) 0.0360(13) -0.0002(14) -0.0030(10) 0.0002(13) C27 0.030(6) 0.017(6) 0.039(6) 0.001(5) -0.011(5) 0.002(5) N005 0.040(6) 0.033(5) 0.045(6) 0.001(5) 0.001(5) -0.001(5) N006 0.063(10) 0.012(7) 0.056(10) 0.001(7) -0.012(8) 0.008(7) N007 0.045(6) 0.035(7) 0.052(7) -0.004(6) 0.000(6) 0.000(5) C24 0.042(9) 0.011(7) 0.038(8) 0.009(7) 0.005(7) -0.002(7) N009 0.083(12) 0.023(8) 0.050(10) -0.015(8) -0.012(10) 0.002(9) C00A 0.0330(13) 0.0270(13) 0.0360(13) -0.0002(14) -0.0030(10) 0.0002(13) C26 0.033(2) 0.017(2) 0.040(2) -0.001(2) -0.007(2) 0.0018(19) C21 0.030(2) 0.017(3) 0.039(3) -0.001(2) -0.007(2) -0.002(2) C23 0.041(8) 0.008(7) 0.050(10) -0.009(6) -0.019(8) 0.008(6) C20 0.030(2) 0.017(3) 0.039(3) -0.001(2) -0.007(2) -0.002(2) C25 0.033(2) 0.017(2) 0.040(2) -0.001(2) -0.007(2) 0.0018(19) N00G 0.056(10) 0.022(8) 0.064(11) -0.006(8) -0.007(9) -0.007(8) C00H 0.031(6) 0.018(6) 0.041(6) -0.005(5) -0.011(5) -0.004(5) N00I 0.041(6) 0.031(6) 0.049(6) 0.005(5) 0.001(5) 0.003(5) C00J 0.033(2) 0.017(2) 0.040(2) -0.001(2) -0.007(2) 0.0018(19) C00K 0.033(2) 0.017(2) 0.040(2) -0.001(2) -0.007(2) 0.0018(19) C00L 0.0330(13) 0.0270(13) 0.0360(13) -0.0002(14) -0.0030(10) 0.0002(13) C00M 0.030(2) 0.017(3) 0.039(3) -0.001(2) -0.007(2) -0.002(2) C00N 0.030(2) 0.017(3) 0.039(3) -0.001(2) -0.007(2) -0.002(2) C00O 0.037(7) 0.011(6) 0.037(7) 0.007(6) -0.005(6) -0.001(5) N00P 0.049(6) 0.038(6) 0.046(6) 0.003(5) 0.002(5) 0.004(5) C00Q 0.033(2) 0.017(2) 0.040(2) -0.001(2) -0.007(2) 0.0018(19) C00R 0.033(2) 0.017(2) 0.040(2) -0.001(2) -0.007(2) 0.0018(19) C00S 0.0330(13) 0.0270(13) 0.0360(13) -0.0002(14) -0.0030(10) 0.0002(13) C00T 0.0330(13) 0.0270(13) 0.0360(13) -0.0002(14) -0.0030(10) 0.0002(13) C00U 0.033(2) 0.017(2) 0.040(2) -0.001(2) -0.007(2) 0.0018(19) C00V 0.033(2) 0.017(2) 0.040(2) -0.001(2) -0.007(2) 0.0018(19) C00W 0.030(2) 0.017(3) 0.039(3) -0.001(2) -0.007(2) -0.002(2) N00X 0.049(7) 0.045(7) 0.053(7) 0.002(6) 0.001(6) 0.000(6) C00Y 0.0330(13) 0.0270(13) 0.0360(13) -0.0002(14) -0.0030(10) 0.0002(13) C00Z 0.0330(13) 0.0270(13) 0.0360(13) -0.0002(14) -0.0030(10) 0.0002(13) C010 0.033(2) 0.017(2) 0.040(2) -0.001(2) -0.007(2) 0.0018(19) C011 0.033(2) 0.017(2) 0.040(2) -0.001(2) -0.007(2) 0.0018(19) C012 0.033(2) 0.017(2) 0.040(2) -0.001(2) -0.007(2) 0.0018(19) C013 0.027(7) 0.016(7) 0.044(8) -0.001(6) -0.012(6) -0.002(6) C014 0.0330(13) 0.0270(13) 0.0360(13) -0.0002(14) -0.0030(10) 0.0002(13) C015 0.033(2) 0.017(2) 0.040(2) -0.001(2) -0.007(2) 0.0018(19) C016 0.032(8) 0.017(8) 0.057(11) -0.005(8) -0.011(8) 0.011(7) C017 0.029(9) 0.021(12) 0.041(12) 0.001(10) -0.003(9) -0.004(9) C018 0.0330(13) 0.0270(13) 0.0360(13) -0.0002(14) -0.0030(10) 0.0002(13) C019 0.032(8) 0.016(8) 0.044(9) 0.002(7) -0.016(7) -0.006(7) C01A 0.039(10) 0.017(11) 0.038(12) 0.004(10) -0.009(10) -0.005(9) C01B 0.0330(13) 0.0270(13) 0.0360(13) -0.0002(14) -0.0030(10) 0.0002(13) C01C 0.0330(13) 0.0270(13) 0.0360(13) -0.0002(14) -0.0030(10) 0.0002(13) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0035 0.0022 '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 0.0066 0.0044 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0117 0.0081 '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 C27 C001 C00A 125.9(17) . . C27 C001 C00T 121.6(17) . . C00T C001 C00A 112.5(16) . . C20 C22 C00H 124.8(17) . . C20 C22 C00M 117.7(17) . . C00M C22 C00H 117.4(15) . . N009 C003 C00Y 179(2) . . C001 C27 H27 114.5 . . C001 C27 C011 130.9(17) . . C011 C27 H27 114.5 . . C013 C24 H24 120.3 . . C016 C24 H24 120.3 . . C016 C24 C013 119.4(18) . . N006 C00A C001 179(2) . . C00Q C26 H26 119.9 . . C00Q C26 C00V 120.2(18) . . C00V C26 H26 119.9 . . C20 C21 H21 119.8 . . C00W C21 H21 119.8 . . C00W C21 C20 120.4(17) . . C00O C23 H23 118.6 . . C00O C23 C013 122.9(17) . . C013 C23 H23 118.6 . . C22 C20 H20 119.7 . . C21 C20 C22 120.7(18) . . C21 C20 H20 119.7 . . C00K C25 H25 120.2 . . C00R C25 H25 120.2 . . C00R C25 C00K 119.7(18) . . C22 C00H H00H 114.8 . . C00S C00H C22 130.4(17) . . C00S C00H H00H 114.8 . . C00K C00J H00J 119.4 . . C00U C00J H00J 119.4 . . C00U C00J C00K 121.3(17) . . C25 C00K C00V 120.0(15) . . C00J C00K C25 118.7(17) . . C00J C00K C00V 121.3(15) . . N007 C00L C00S 175(2) . . C22 C00M H00M 118.9 . . C00N C00M C22 122.2(17) . . C00N C00M H00M 118.9 . . C00M C00N H00N 120.6 . . C00M C00N C00W 118.9(18) . . C00W C00N H00N 120.6 . . C23 C00O H00O 120.4 . . C23 C00O C019 119.2(17) . . C019 C00O H00O 120.4 . . C26 C00Q H00Q 119.2 . . C26 C00Q C011 121.6(17) . . C011 C00Q H00Q 119.2 . . C25 C00R H00R 118.6 . . C25 C00R C015 122.7(18) . . C015 C00R H00R 118.6 . . C00H C00S C00L 119.6(17) . . C00H C00S C00Z 126.0(17) . . C00Z C00S C00L 114.4(16) . . N00I C00T C001 178(2) . . C00J C00U H00U 120.2 . . C00J C00U C015 119.7(19) . . C015 C00U H00U 120.2 . . C26 C00V C00K 120.7(16) . . C010 C00V C26 117.7(17) . . C010 C00V C00K 121.5(15) . . C21 C00W C00N 120.0(17) . . C21 C00W C019 120.7(15) . . C00N C00W C019 119.3(16) . . C003 C00Y C018 114.3(18) . . C01A C00Y C003 126.5(19) . . C01A C00Y C018 119.1(17) . . N005 C00Z C00S 178(2) . . C00V C010 H010 119.2 . . C012 C010 C00V 121.6(17) . . C012 C010 H010 119.2 . . C00Q C011 C27 116.1(16) . . C00Q C011 C012 119.4(17) . . C012 C011 C27 124.5(17) . . C010 C012 C011 119.5(18) . . C010 C012 H012 120.2 . . C011 C012 H012 120.2 . . C24 C013 C017 123.6(18) . . C23 C013 C24 117.8(18) . . C23 C013 C017 118.5(16) . . N00P C014 C01C 179(2) . . C00R C015 C00U 117.8(19) . . C00R C015 C01A 118.8(16) . . C00U C015 C01A 123.3(17) . . C24 C016 H016 119.0 . . C24 C016 C019 122.0(17) . . C019 C016 H016 119.0 . . C013 C017 H017 113.9 . . C01C C017 C013 132.2(18) . . C01C C017 H017 113.9 . . N00X C018 C00Y 178(2) . . C00O C019 C00W 119.8(15) . . C016 C019 C00O 118.6(18) . . C016 C019 C00W 121.6(16) . . C00Y C01A C015 130.9(18) . . C00Y C01A H01A 114.5 . . C015 C01A H01A 114.5 . . N00G C01B C01C 180(2) . . C014 C01C C01B 114.4(18) . . C017 C01C C014 124.3(19) . . C017 C01C C01B 121.2(17) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 C001 C27 1.38(2) . C001 C00A 1.45(2) . C001 C00T 1.44(2) . C22 C20 1.40(2) . C22 C00H 1.47(2) . C22 C00M 1.42(2) . C003 N009 1.17(2) . C003 C00Y 1.42(2) . C27 H27 0.9300 . C27 C011 1.45(2) . N005 C00Z 1.16(2) . N006 C00A 1.15(2) . N007 C00L 1.15(2) . C24 H24 0.9300 . C24 C013 1.42(2) . C24 C016 1.38(2) . C26 H26 0.9300 . C26 C00Q 1.38(2) . C26 C00V 1.42(2) . C21 H21 0.9300 . C21 C20 1.40(2) . C21 C00W 1.39(2) . C23 H23 0.9300 . C23 C00O 1.38(2) . C23 C013 1.39(2) . C20 H20 0.9300 . C25 H25 0.9300 . C25 C00K 1.42(2) . C25 C00R 1.37(2) . N00G C01B 1.16(2) . C00H H00H 0.9300 . C00H C00S 1.35(2) . N00I C00T 1.15(2) . C00J H00J 0.9300 . C00J C00K 1.40(2) . C00J C00U 1.38(2) . C00K C00V 1.48(2) . C00L C00S 1.45(2) . C00M H00M 0.9300 . C00M C00N 1.38(2) . C00N H00N 0.9300 . C00N C00W 1.41(2) . C00O H00O 0.9300 . C00O C019 1.41(2) . N00P C014 1.18(2) . C00Q H00Q 0.9300 . C00Q C011 1.38(2) . C00R H00R 0.9300 . C00R C015 1.38(2) . C00S C00Z 1.43(2) . C00U H00U 0.9300 . C00U C015 1.44(2) . C00V C010 1.42(2) . C00W C019 1.49(2) . N00X C018 1.16(2) . C00Y C018 1.46(2) . C00Y C01A 1.34(2) . C010 H010 0.9300 . C010 C012 1.38(2) . C011 C012 1.42(2) . C012 H012 0.9300 . C013 C017 1.46(2) . C014 C01C 1.42(2) . C015 C01A 1.45(2) . C016 H016 0.9300 . C016 C019 1.39(2) . C017 H017 0.9300 . C017 C01C 1.34(2) . C01A H01A 0.9300 . C01B C01C 1.43(2) . 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 C001 C27 C011 C00Q 172.6(17) . . . . C001 C27 C011 C012 -5(3) . . . . C22 C00H C00S C00L -175.2(17) . . . . C22 C00H C00S C00Z 2(3) . . . . C22 C00M C00N C00W -3(2) . . . . C003 C00Y C01A C015 3(3) . . . . C27 C011 C012 C010 177.9(15) . . . . C24 C013 C017 C01C 1(3) . . . . C24 C016 C019 C00O -3(3) . . . . C24 C016 C019 C00W 178.0(16) . . . . C00A C001 C27 C011 2(3) . . . . C26 C00Q C011 C27 -178.1(16) . . . . C26 C00Q C011 C012 0(3) . . . . C26 C00V C010 C012 -2(2) . . . . C21 C00W C019 C00O -29(2) . . . . C21 C00W C019 C016 150.4(16) . . . . C23 C00O C019 C00W -177.1(15) . . . . C23 C00O C019 C016 4(2) . . . . C23 C013 C017 C01C -177.1(17) . . . . C20 C22 C00H C00S -5(3) . . . . C20 C22 C00M C00N 3(2) . . . . C20 C21 C00W C00N 1(2) . . . . C20 C21 C00W C019 179.5(14) . . . . C25 C00K C00V C26 150.4(16) . . . . C25 C00K C00V C010 -30(2) . . . . C25 C00R C015 C00U 1(3) . . . . C25 C00R C015 C01A 178.9(15) . . . . C00H C22 C20 C21 179.7(15) . . . . C00H C22 C00M C00N -178.0(15) . . . . C00J C00K C00V C26 -30(3) . . . . C00J C00K C00V C010 149.8(16) . . . . C00J C00U C015 C00R 1(2) . . . . C00J C00U C015 C01A -176.7(16) . . . . C00K C25 C00R C015 -3(3) . . . . C00K C00J C00U C015 -1(3) . . . . C00K C00V C010 C012 178.5(15) . . . . C00M C22 C20 C21 -2(2) . . . . C00M C22 C00H C00S 176.2(17) . . . . C00M C00N C00W C21 0(2) . . . . C00M C00N C00W C019 -177.9(15) . . . . C00N C00W C019 C00O 149.4(15) . . . . C00N C00W C019 C016 -31(2) . . . . C00O C23 C013 C24 1(3) . . . . C00O C23 C013 C017 178.8(15) . . . . C00Q C26 C00V C00K -178.5(16) . . . . C00Q C26 C00V C010 2(2) . . . . C00Q C011 C012 C010 0(2) . . . . C00R C25 C00K C00J 3(2) . . . . C00R C25 C00K C00V -177.4(15) . . . . C00R C015 C01A C00Y -179.2(18) . . . . C00T C001 C27 C011 -175.5(18) . . . . C00U C00J C00K C25 -1(3) . . . . C00U C00J C00K C00V 179.4(15) . . . . C00U C015 C01A C00Y -2(3) . . . . C00V C26 C00Q C011 -1(3) . . . . C00V C010 C012 C011 1(2) . . . . C00W C21 C20 C22 -1(2) . . . . C013 C24 C016 C019 1(3) . . . . C013 C23 C00O C019 -3(3) . . . . C013 C017 C01C C014 -1(3) . . . . C013 C017 C01C C01B -179.5(17) . . . . C016 C24 C013 C23 0(2) . . . . C016 C24 C013 C017 -177.7(16) . . . . C018 C00Y C01A C015 180.0(17) . . . . loop_ _twin_individual_id _twin_individual_mass_fraction_refined _oxdiff_twin_reflns_isolated _oxdiff_twin_reflns_overlapped _twin_individual_twin_lattice_type _twin_individual_twin_matrix_11 _twin_individual_twin_matrix_12 _twin_individual_twin_matrix_13 _twin_individual_twin_matrix_21 _twin_individual_twin_matrix_22 _twin_individual_twin_matrix_23 _twin_individual_twin_matrix_31 _twin_individual_twin_matrix_32 _twin_individual_twin_matrix_33 1 0.643(6) 6966 11126 ref 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 2 0.357(6) 0 11126 nmt 0.9980 -0.0002 0.0002 0.0003 -1.0003 0.0004 -0.8233 -0.0033 -0.9990