#------------------------------------------------------------------------------ #$Date: 2024-07-25 01:14:29 +0300 (Thu, 25 Jul 2024) $ #$Revision: 293532 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/21/1572162.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_1572162 loop_ _publ_author_name 'Madron du Vign\'e, Adrien' 'Cramer, Nicolai' _publ_section_title ; Streamlined Synthetic Assembly of \a-Chiral CAAC Ligands and Catalytic Performance of Their Copper and Ruthenium Complexes ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/D4SC04278F _journal_year 2024 _chemical_absolute_configuration rmad _chemical_formula_moiety 'C21 H31 Cl Cu N' _chemical_formula_sum 'C21 H31 Cl Cu N' _chemical_formula_weight 396.46 _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 _atom_sites_solution_secondary difmap _audit_creation_date 2022-07-27 _audit_creation_method ; Olex2 1.5 (compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498) ; _audit_update_record ; 2022-07-27 deposited with the CCDC. 2024-07-24 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 98.352(2) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 9.6227(3) _cell_length_b 8.2304(3) _cell_length_c 12.9158(3) _cell_measurement_reflns_used 6895 _cell_measurement_temperature 140.00(10) _cell_measurement_theta_max 76.2390 _cell_measurement_theta_min 3.3950 _cell_volume 1012.07(5) _computing_cell_refinement 'CrysAlisPro 1.171.42.61a (Rigaku OD, 2022)' _computing_data_collection 'CrysAlisPro 1.171.42.61a (Rigaku OD, 2022)' _computing_data_reduction 'CrysAlisPro 1.171.42.61a (Rigaku OD, 2022)' _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 2018/2 (Sheldrick, 2015)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 140.00(10) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 10.2665 _diffrn_detector_type Atlas _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.991 _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 -50.00 -25.00 1.00 1.00 -- -43.01 17.00-148.00 25 2 \w -112.00 4.00 1.00 1.00 -- -43.01 -17.00 42.00 116 3 \w 36.00 63.00 1.00 1.00 -- 43.01 17.00-148.00 27 4 \w 97.00 122.00 1.00 3.00 -- 112.00 17.00-148.00 25 5 \w 79.00 104.00 1.00 3.00 -- 112.00 -17.00 42.00 25 6 \w -108.00 -15.00 1.00 1.00 -- -43.01 -57.00 -60.00 93 7 \w -82.00 -15.00 1.00 1.00 -- -43.01 -57.00-120.00 67 8 \w -114.00 -28.00 1.00 1.00 -- -43.01 -57.00-150.00 86 9 \w 22.00 65.00 1.00 1.00 -- 43.01 37.00-120.00 43 10 \w 29.00 96.00 1.00 1.00 -- 43.01-125.00 60.00 67 11 \w 7.00 58.00 1.00 1.00 -- 43.01 -99.00 0.00 51 12 \w 83.00 112.00 1.00 3.00 -- 112.00 61.00 0.00 29 13 \w 41.00 140.00 1.00 3.00 -- 112.00 -61.00 90.00 99 14 \w 147.00 178.00 1.00 3.00 -- 112.00 61.00-120.00 31 15 \w 40.00 104.00 1.00 3.00 -- 112.00-111.00 -30.00 64 16 \w 84.00 110.00 1.00 3.00 -- 112.00 61.00 -30.00 26 17 \w 121.00 178.00 1.00 3.00 -- 112.00 61.00 -30.00 57 18 \w 84.00 109.00 1.00 3.00 -- 112.00 61.00 -53.98 25 19 \w 152.00 177.00 1.00 3.00 -- 112.00 61.00 -53.98 25 20 \w 117.00 170.00 1.00 3.00 -- 112.00 45.00 -90.00 53 21 \w 84.00 109.00 1.00 3.00 -- 112.00 61.00 -90.00 25 22 \w 87.00 112.00 1.00 3.00 -- 112.00 45.00 -90.00 25 23 \w 84.00 125.00 1.00 3.00 -- 112.00 66.00 48.83 41 24 \w 86.00 113.00 1.00 3.00 -- 112.00 58.00 -77.30 27 25 \w 84.00 110.00 1.00 3.00 -- 112.00 58.00 -9.49 26 26 \w 83.00 109.00 1.00 3.00 -- 112.00 61.00 30.00 26 27 \w 119.00 178.00 1.00 3.00 -- 112.00 61.00 30.00 59 28 \w 83.00 109.00 1.00 3.00 -- 112.00 61.00 -60.00 26 29 \w 78.00 118.00 1.00 3.00 -- 112.00 -61.00 -90.00 40 30 \w 88.00 148.00 1.00 3.00 -- 112.00 45.00 30.00 60 31 \w 127.00 154.00 1.00 3.00 -- 112.00 30.00 -90.00 27 32 \w 61.00 125.00 1.00 3.00 -- 112.00 178.00 0.00 64 33 \w 90.00 117.00 1.00 3.00 -- 112.00 45.00-120.00 27 34 \w 84.00 110.00 1.00 3.00 -- 112.00 30.00 0.00 26 35 \w 87.00 112.00 1.00 3.00 -- 112.00 45.00 0.00 25 36 \w 87.00 114.00 1.00 3.00 -- 112.00 30.00 -90.00 27 37 \w 39.00 106.00 1.00 3.00 -- 112.00-111.00 -90.00 67 38 \w 88.00 178.00 1.00 3.00 -- 112.00 30.00 -60.00 90 39 \w 102.00 127.00 1.00 3.00 -- 112.00 30.00 -30.00 25 40 \w 142.00 167.00 1.00 3.00 -- 112.00 61.00 0.00 25 41 \w 83.00 110.00 1.00 3.00 -- 112.00 61.00-120.00 27 42 \w 41.00 66.00 1.00 3.00 -- 112.00-111.00-150.00 25 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at home/near, Atlas' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0028014000 _diffrn_orient_matrix_UB_12 -0.0255556000 _diffrn_orient_matrix_UB_13 -0.1177898000 _diffrn_orient_matrix_UB_21 0.1593102000 _diffrn_orient_matrix_UB_22 0.0328099000 _diffrn_orient_matrix_UB_23 0.0164581000 _diffrn_orient_matrix_UB_31 0.0281350000 _diffrn_orient_matrix_UB_32 -0.1825855000 _diffrn_orient_matrix_UB_33 0.0194902000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0330 _diffrn_reflns_av_unetI/netI 0.0354 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.991 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 11385 _diffrn_reflns_point_group_measured_fraction_full 0.938 _diffrn_reflns_point_group_measured_fraction_max 0.922 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 76.457 _diffrn_reflns_theta_min 3.459 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 2.725 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.403 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.42.61a (Rigaku Oxford Diffraction, 2022) Numerical absorption correction based on Gaussian integration over a multifaceted crystal model. Empirical absorption correction using spherical harmonics as implemented in SCALE3 ABSPACK scaling algorithm ; _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.301 _exptl_crystal_description needle _exptl_crystal_F_000 420 _exptl_crystal_size_max 0.66 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _refine_diff_density_max 0.298 _refine_diff_density_min -0.294 _refine_diff_density_rms 0.044 _refine_ls_abs_structure_details ; Flack x determined using 1464 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack -0.028(16) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 221 _refine_ls_number_reflns 3906 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.046 _refine_ls_R_factor_all 0.0343 _refine_ls_R_factor_gt 0.0310 _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^)+(0.0363P)^2^+0.2887P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0756 _refine_ls_wR_factor_ref 0.0777 _reflns_Friedel_coverage 0.734 _reflns_Friedel_fraction_full 0.866 _reflns_Friedel_fraction_max 0.841 _reflns_number_gt 3671 _reflns_number_total 3906 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc04278f2.cif _cod_data_source_block amd-r855_2 _cod_depositor_comments ; The following automatic conversions were performed: data item '_exptl_absorpt_correction_type' value 'Gaussian' was changed to 'gaussian' in accordance with the /home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.2 last updated on 2011-04-26. Automatic conversion script Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas ; _cod_original_cell_volume 1012.06(5) _cod_database_code 1572162 _shelx_shelxl_version_number 2018/3 _audit_contact_author 'Farzaneh Fadaei Tirani' _chemical_oxdiff_formula 'C21 H31 Cl Cu N' _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 0.899 _shelx_estimated_absorpt_t_min 0.266 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2.a Ternary CH refined with riding coordinates: C5(H5), C6(H6) 2.b Secondary CH2 refined with riding coordinates: C3(H3A,H3B), C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A, H11B) 2.c Aromatic/amide H refined with riding coordinates: C14(H14), C15(H15), C16(H16), C17(H17), C18(H18) 2.d Idealised Me refined as rotating group: C12(H12A,H12B,H12C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C21(H21A,H21B, H21C) ; _shelx_res_file ; TITL amd-r855_2.res in P2(1) amd-r855_2.res created by SHELXL-2018/3 at 13:41:22 on 27-Jul-2022 CELL 1.54184 9.622667 8.230384 12.915788 90 98.3521 90 ZERR 2 0.000255 0.000263 0.000327 0 0.0024 0 LATT -1 SYMM -X,0.5+Y,-Z SFAC C H Cl Cu N UNIT 42 62 2 2 2 L.S. 20 PLAN 5 SIZE 0.04 0.06 0.66 TEMP -133.15 CONF wpdb -2 MORE -1 BOND $H fmap 2 acta REM REM REM WGHT 0.036300 0.288700 FVAR 0.98587 CU1 4 0.407934 0.694250 0.813693 11.00000 0.02632 0.02578 = 0.03205 -0.00194 0.00448 -0.00028 CL1 3 0.554554 0.886363 0.826792 11.00000 0.03722 0.02735 = 0.04658 -0.00190 0.01185 -0.00556 N1 5 0.320857 0.363743 0.802496 11.00000 0.02245 0.02887 = 0.02358 0.00033 0.00220 -0.00190 C1 1 0.285223 0.514405 0.811419 11.00000 0.02431 0.03203 = 0.02344 0.00108 0.00115 0.00025 C2 1 0.132629 0.522753 0.830168 11.00000 0.02582 0.03846 = 0.02832 0.00035 0.00552 0.00069 C3 1 0.079931 0.346779 0.812598 11.00000 0.02474 0.04082 = 0.04310 0.00539 0.00459 -0.00478 AFIX 23 H3A 2 0.024926 0.314295 0.868312 11.00000 -1.20000 H3B 2 0.019042 0.337163 0.744176 11.00000 -1.20000 AFIX 0 C4 1 0.210108 0.237340 0.815087 11.00000 0.02891 0.02887 = 0.03064 0.00419 0.00484 -0.00431 C5 1 0.469135 0.310321 0.796119 11.00000 0.02227 0.02839 = 0.02916 0.00130 0.00137 0.00160 AFIX 13 H5 2 0.468675 0.189078 0.791045 11.00000 -1.20000 AFIX 0 C6 1 0.520602 0.376704 0.697297 11.00000 0.02374 0.02170 = 0.02991 -0.00118 0.00481 -0.00056 AFIX 13 H6 2 0.507048 0.497189 0.696062 11.00000 -1.20000 AFIX 0 C7 1 0.677013 0.342366 0.697870 11.00000 0.02308 0.06273 = 0.03671 -0.00636 0.00318 -0.00126 AFIX 23 H7A 2 0.693732 0.223795 0.703483 11.00000 -1.20000 H7B 2 0.731819 0.394822 0.759711 11.00000 -1.20000 AFIX 0 C8 1 0.727306 0.406123 0.598362 11.00000 0.02907 0.06064 = 0.04733 -0.00614 0.01351 -0.01223 AFIX 23 H8A 2 0.716491 0.525720 0.595294 11.00000 -1.20000 H8B 2 0.828281 0.380725 0.600732 11.00000 -1.20000 AFIX 0 C9 1 0.645428 0.331667 0.500972 11.00000 0.03359 0.03532 = 0.03466 0.00143 0.01129 -0.00225 AFIX 23 H9A 2 0.663448 0.213268 0.500368 11.00000 -1.20000 H9B 2 0.677209 0.379615 0.438132 11.00000 -1.20000 AFIX 0 C10 1 0.488339 0.361971 0.497662 11.00000 0.03282 0.04670 = 0.03165 0.00717 0.00651 0.00156 AFIX 23 H10A 2 0.436149 0.302962 0.437412 11.00000 -1.20000 H10B 2 0.468996 0.479418 0.487157 11.00000 -1.20000 AFIX 0 C11 1 0.435989 0.306554 0.598189 11.00000 0.02604 0.03357 = 0.02761 0.00109 0.00315 -0.00126 AFIX 23 H11A 2 0.336483 0.339194 0.595336 11.00000 -1.20000 H11B 2 0.440112 0.186475 0.601947 11.00000 -1.20000 AFIX 0 C12 1 0.562418 0.356181 0.897782 11.00000 0.02705 0.04761 = 0.02843 -0.00025 -0.00327 0.00274 AFIX 137 H12A 2 0.580458 0.473394 0.898554 11.00000 -1.50000 H12B 2 0.651678 0.297360 0.902638 11.00000 -1.50000 H12C 2 0.515009 0.327231 0.957424 11.00000 -1.50000 AFIX 0 C13 1 0.049766 0.640723 0.753618 11.00000 0.02127 0.03441 = 0.03101 -0.00035 0.00218 -0.00395 C14 1 0.079824 0.649932 0.650663 11.00000 0.02611 0.05158 = 0.03351 -0.00026 0.00537 0.00204 AFIX 43 H14 2 0.153187 0.585083 0.630710 11.00000 -1.20000 AFIX 0 C15 1 0.004623 0.751714 0.577580 11.00000 0.03024 0.06600 = 0.03395 0.00936 -0.00018 -0.00588 AFIX 43 H15 2 0.026970 0.756418 0.508376 11.00000 -1.20000 AFIX 0 C16 1 -0.102943 0.846546 0.605079 11.00000 0.02893 0.04818 = 0.05189 0.01461 -0.00618 -0.00594 AFIX 43 H16 2 -0.153575 0.917738 0.555338 11.00000 -1.20000 AFIX 0 C17 1 -0.136031 0.836993 0.704951 11.00000 0.02454 0.04003 = 0.06510 0.00389 0.00430 0.00433 AFIX 43 H17 2 -0.211329 0.899749 0.723822 11.00000 -1.20000 AFIX 0 C18 1 -0.058974 0.734942 0.778946 11.00000 0.02796 0.03990 = 0.03943 0.00238 0.00896 0.00225 AFIX 43 H18 2 -0.082076 0.730544 0.847946 11.00000 -1.20000 AFIX 0 C19 1 0.136358 0.578519 0.944836 11.00000 0.03651 0.05373 = 0.02905 -0.00003 0.00654 0.00710 AFIX 137 H19A 2 0.203470 0.511541 0.990677 11.00000 -1.50000 H19B 2 0.042659 0.566706 0.965192 11.00000 -1.50000 H19C 2 0.165309 0.692662 0.951329 11.00000 -1.50000 AFIX 0 C20 1 0.250703 0.150497 0.919655 11.00000 0.03920 0.03890 = 0.03455 0.01026 0.00897 -0.00052 AFIX 137 H20A 2 0.338678 0.090906 0.918693 11.00000 -1.50000 H20B 2 0.176193 0.074202 0.931006 11.00000 -1.50000 H20C 2 0.263278 0.230678 0.976339 11.00000 -1.50000 AFIX 0 C21 1 0.193094 0.115127 0.726077 11.00000 0.03753 0.03651 = 0.03560 -0.00171 0.00264 -0.01387 AFIX 137 H21A 2 0.175477 0.172824 0.659080 11.00000 -1.50000 H21B 2 0.113725 0.043190 0.732749 11.00000 -1.50000 H21C 2 0.279099 0.050488 0.728952 11.00000 -1.50000 AFIX 0 HKLF 4 REM amd-r855_2.res in P2(1) REM wR2 = 0.0777, GooF = S = 1.046, Restrained GooF = 1.046 for all data REM R1 = 0.0310 for 3671 Fo > 4sig(Fo) and 0.0343 for all 3906 data REM 221 parameters refined using 1 restraints END WGHT 0.0363 0.2884 REM Highest difference peak 0.298, deepest hole -0.294, 1-sigma level 0.044 Q1 1 0.2946 0.6840 0.7969 11.00000 0.05 0.30 Q2 1 0.3252 0.6907 0.7463 11.00000 0.05 0.27 Q3 1 0.4841 0.6972 0.8785 11.00000 0.05 0.27 Q4 1 0.2625 -0.1274 0.8051 11.00000 0.05 0.22 Q5 1 0.3776 0.3556 0.8032 11.00000 0.05 0.21 ; _shelx_res_checksum 62846 _shelx_hkl_file ; 0 -10 0 41.20 4.50 0 -10 -1 40.21 4.61 0 -10 -2 41.15 4.66 0 -10 -3 83.75 5.82 0 -10 -4 14.03 2.47 0 -9 0 0.96 5.64 0 -9 0 1.71 5.21 0 -9 1 108.58 10.77 0 -9 -1 81.16 9.84 0 -9 1 103.58 9.23 0 -9 -1 84.07 9.52 0 -9 2 213.95 13.89 0 -9 -2 217.91 13.70 0 -9 2 210.36 11.44 0 -9 3 15.91 3.97 0 -9 -3 24.04 6.41 0 -9 -3 20.79 4.65 0 -9 3 18.74 5.71 0 -9 -4 76.78 7.38 0 -9 -4 65.09 7.69 0 -9 4 71.55 7.49 0 -9 -5 49.74 6.31 0 -9 5 39.84 5.24 0 -9 -5 32.92 5.77 0 -9 -6 9.21 3.30 0 -9 -6 8.80 3.56 0 -9 -7 143.59 8.02 0 -8 0 35.79 8.74 0 -8 0 54.27 9.03 0 -8 1 0.65 7.30 0 -8 -1 3.44 5.82 0 -8 1 8.54 6.20 0 -8 -1 1.55 6.48 0 -8 2 15.59 6.88 0 -8 -2 12.42 6.88 0 -8 -2 15.24 7.15 0 -8 2 3.18 5.41 0 -8 -3 6.51 5.98 0 -8 3 10.76 6.06 0 -8 -3 12.94 6.84 0 -8 3 6.32 4.65 0 -8 4 44.64 7.68 0 -8 -4 40.77 7.90 0 -8 4 39.20 5.72 0 -8 -5 58.08 8.69 0 -8 5 57.96 7.64 0 -8 6 -0.44 4.27 0 -8 -6 -3.37 5.04 0 -8 -7 43.33 7.58 0 -8 -7 35.19 5.50 0 -8 -8 13.33 5.00 0 -8 -9 2.89 3.59 0 -8 -10 60.16 4.67 0 -7 0 15.46 11.01 0 -7 0 -0.54 5.98 0 -7 0 -1.44 6.18 0 -7 1 95.12 11.39 0 -7 -1 111.74 11.56 0 -7 1 59.53 10.64 0 -7 -1 70.04 17.49 0 -7 -1 102.89 11.43 0 -7 1 108.98 11.23 0 -7 -2 24.33 11.82 0 -7 -2 43.18 8.24 0 -7 2 45.69 8.00 0 -7 -2 45.39 8.63 0 -7 2 39.32 8.58 0 -7 -3 45.07 15.49 0 -7 -3 55.33 9.14 0 -7 3 67.80 9.62 0 -7 -3 75.56 10.70 0 -7 3 69.43 8.44 0 -7 4 107.46 11.19 0 -7 -4 100.99 11.62 0 -7 4 97.88 8.55 0 -7 -4 71.82 9.92 0 -7 -5 4.73 6.12 0 -7 5 14.06 6.42 0 -7 -6 41.14 7.40 0 -7 6 51.08 7.57 0 -7 6 51.96 7.12 0 -7 7 66.79 8.26 0 -7 -7 67.55 8.56 0 -7 7 86.02 8.24 0 -7 8 22.97 5.82 0 -7 -9 61.77 8.98 0 -7 9 66.91 7.59 0 -7 -10 68.15 7.50 0 -7 10 75.77 7.31 0 -7 -11 19.77 3.68 0 -7 11 22.88 3.99 0 -6 0 2789.15 85.55 0 -6 1 241.78 25.29 0 -6 -1 249.22 26.69 0 -6 -1 200.40 24.85 0 -6 1 245.80 15.46 0 -6 -1 226.81 14.54 0 -6 -1 236.85 15.03 0 -6 -2 632.55 43.52 0 -6 2 657.55 39.27 0 -6 -2 726.08 47.36 0 -6 2 725.76 24.90 0 -6 2 738.88 26.59 0 -6 -2 683.08 24.66 0 -6 -2 666.79 25.13 0 -6 2 723.46 23.67 0 -6 -3 1552.80 71.64 0 -6 -3 1414.97 66.69 0 -6 3 1525.63 38.00 0 -6 3 1465.00 35.07 0 -6 -3 1444.21 35.63 0 -6 -3 1566.21 38.46 0 -6 3 1555.09 33.24 0 -6 -4 31.94 10.53 0 -6 4 10.25 4.98 0 -6 -4 9.21 4.32 0 -6 4 14.21 6.38 0 -6 -4 13.53 6.15 0 -6 4 15.43 5.81 0 -6 5 563.89 26.81 0 -6 -5 545.85 44.60 0 -6 5 530.32 21.63 0 -6 5 533.98 22.48 0 -6 -5 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4 7 62.63 4.94 -9 5 9 51.98 5.15 9 5 -9 64.50 4.78 9 5 -8 130.10 7.36 9 5 -8 134.00 7.84 -9 5 8 126.99 9.01 9 5 -8 124.43 6.69 9 5 -8 144.16 8.17 9 5 -7 22.93 4.42 9 5 -7 23.88 5.04 9 5 -7 21.66 4.90 -9 5 7 16.58 5.40 9 5 -7 24.96 4.76 9 5 -6 58.97 6.46 9 5 -6 57.83 6.80 9 5 -6 65.44 6.96 -9 5 6 40.03 6.86 9 5 -6 56.34 7.10 9 5 -5 76.61 7.51 -9 5 5 59.10 7.81 9 5 -5 73.78 7.65 9 5 -5 80.38 8.42 9 5 -4 3.94 5.12 -9 5 4 1.02 4.13 9 5 -4 2.17 5.24 9 5 -3 169.49 11.09 9 5 -3 156.31 11.39 9 5 -2 0.12 5.03 9 5 -2 -1.83 6.00 9 5 -2 4.09 5.84 9 5 -2 -2.61 5.23 9 5 -1 1.16 5.80 9 5 -1 5.01 5.49 9 5 -1 11.22 6.14 9 5 -1 8.30 5.76 9 5 0 98.26 9.45 9 5 0 90.83 9.15 9 5 0 78.59 9.23 9 5 0 88.20 8.31 9 5 1 18.34 5.71 9 5 1 23.42 6.24 9 5 1 16.53 6.08 9 5 1 16.57 5.12 9 5 1 23.71 5.04 9 5 1 20.11 4.71 9 5 2 36.58 6.61 9 5 2 38.31 6.72 9 5 2 38.60 6.09 9 5 2 30.63 5.29 9 5 2 32.96 5.47 9 5 2 19.17 4.51 9 5 3 9.93 4.50 9 5 3 17.63 5.68 9 5 3 19.90 4.45 9 5 3 17.76 4.27 9 5 3 21.01 4.83 9 5 4 21.34 4.56 9 5 4 18.09 3.73 9 5 4 23.24 4.44 9 5 5 41.11 4.75 9 6 -7 107.00 5.55 9 6 -6 61.14 5.19 9 6 -6 56.36 5.16 9 6 -6 47.90 4.52 9 6 -5 24.77 4.15 9 6 -5 24.15 4.31 9 6 -4 119.13 7.85 9 6 -4 111.81 7.61 9 6 -4 103.11 7.62 9 6 -3 73.69 6.81 9 6 -3 72.37 6.88 9 6 -3 50.24 5.84 9 6 -3 63.37 6.45 9 6 -2 31.82 5.55 9 6 -2 36.69 5.68 9 6 -2 23.27 4.45 9 6 -1 158.77 9.35 9 6 -1 149.38 8.93 9 6 -1 130.86 8.06 9 6 -1 125.76 8.49 9 6 0 8.45 3.12 9 6 0 7.39 4.04 9 6 0 8.81 4.14 9 6 0 11.58 3.04 9 6 0 15.65 3.83 9 6 1 53.88 5.50 9 6 1 73.43 6.46 9 6 1 61.21 5.38 9 6 1 62.58 5.68 9 6 2 67.28 5.33 9 6 2 74.41 6.32 9 6 2 82.43 5.56 9 6 2 84.59 5.99 9 6 3 47.26 4.20 9 6 3 54.01 4.53 -10 -5 6 28.60 4.31 -10 -5 5 13.64 4.00 -10 -5 5 12.56 3.48 -10 -5 4 4.31 4.21 -10 -5 4 3.30 3.48 -10 -5 3 40.85 5.80 -10 -5 3 39.89 5.99 -10 -5 2 19.72 4.94 -10 -5 1 25.39 4.82 -10 -5 0 -0.40 3.44 -10 -5 -1 5.19 2.96 -10 -5 -1 16.94 3.31 -10 -5 -2 0.88 2.59 -10 -4 8 96.95 6.74 -10 -4 8 60.23 4.97 -10 -4 7 76.36 7.25 -10 -4 7 51.69 5.35 -10 -4 6 37.38 6.64 -10 -4 6 29.08 4.77 -10 -4 6 19.50 3.86 -10 -4 5 119.94 10.24 -10 -4 5 110.03 8.74 -10 -4 4 49.58 7.57 -10 -4 4 38.90 7.27 -10 -4 3 64.67 8.24 -10 -4 3 56.10 8.61 -10 -4 2 107.98 9.86 -10 -4 2 93.60 9.98 -10 -4 1 38.20 6.30 -10 -4 1 39.07 7.69 -10 -4 0 157.76 11.58 10 -4 1 162.12 9.57 -10 -4 -1 160.14 10.98 -10 -4 -2 2.23 3.59 10 -4 2 0.43 3.16 10 -4 3 145.89 9.58 10 -4 4 35.85 4.85 -10 -3 9 116.85 7.58 -10 -3 9 162.29 9.23 -10 -3 8 16.00 5.26 -10 -3 7 345.11 16.71 -10 -3 6 30.60 5.77 -10 -3 6 33.97 7.23 -10 -3 5 9.05 5.48 -10 -3 5 11.22 6.42 -10 -3 4 107.18 10.92 -10 -3 4 130.35 11.90 -10 -3 3 73.50 9.98 -10 -3 3 58.25 8.80 -10 -3 2 28.77 8.78 10 -3 -2 27.23 5.36 -10 -3 2 37.58 6.64 -10 -3 1 171.17 13.85 -10 -3 1 149.13 11.22 10 -3 0 52.24 7.95 -10 -3 0 58.91 7.24 -10 -3 0 51.74 9.00 10 -3 1 161.24 12.11 -10 -3 -1 161.28 12.21 10 -3 2 256.27 14.53 -10 -3 -2 251.89 13.81 10 -3 3 2.09 4.61 -10 -3 -3 -8.37 4.53 10 -3 4 91.07 8.22 10 -3 4 71.96 7.88 10 -3 5 145.63 8.94 -10 -2 10 84.61 6.71 -10 -2 9 10.52 4.47 -10 -2 8 175.79 12.55 -10 -2 7 36.28 7.96 -10 -2 6 162.16 13.52 -10 -2 6 138.64 10.09 -10 -2 5 205.37 15.06 -10 -2 5 171.71 12.53 -10 -2 4 15.53 7.25 -10 -2 4 21.46 6.78 -10 -2 3 127.81 12.07 -10 -2 3 110.35 11.95 -10 -2 2 413.94 19.50 -10 -2 2 355.33 19.12 -10 -2 1 -1.31 3.84 10 -2 0 140.60 12.67 10 -2 1 106.81 11.79 -10 -2 -2 1.63 5.61 10 -2 2 -5.77 6.80 -10 -2 -3 203.68 12.36 10 -2 3 234.28 14.74 -10 -2 -4 98.28 7.59 10 -2 4 119.09 10.54 10 -2 5 54.18 6.71 10 -2 5 63.14 7.02 10 -2 6 121.48 7.47 -10 -1 10 23.25 4.81 -10 -1 9 217.89 13.43 -10 -1 8 50.82 8.76 -10 -1 7 229.51 15.74 -10 -1 7 235.36 16.25 -10 -1 6 65.99 10.67 -10 -1 6 46.89 7.00 -10 -1 6 68.06 9.97 -10 -1 5 0.96 7.97 -10 -1 5 3.26 4.92 -10 -1 5 3.30 6.49 -10 -1 4 92.37 12.32 -10 -1 4 90.66 11.03 -10 -1 3 15.25 5.73 -10 -1 2 32.00 6.40 10 -1 -2 34.58 6.05 10 -1 -1 79.00 8.49 10 -1 0 46.20 6.55 10 -1 0 50.59 7.51 10 -1 1 36.65 6.48 10 -1 1 21.23 5.88 10 -1 2 80.49 8.82 10 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10 0 4 63.33 8.06 10 0 4 63.28 6.39 10 0 4 67.28 8.74 10 0 5 92.21 8.39 10 0 5 92.70 8.75 10 0 6 117.59 8.11 10 0 6 100.57 7.46 10 0 7 0.06 2.37 -10 1 10 18.87 4.27 -10 1 10 14.15 4.12 -10 1 10 21.65 4.68 10 1 -10 24.40 3.23 -10 1 9 215.96 12.54 -10 1 9 203.84 12.88 -10 1 9 207.43 12.05 10 1 -9 175.79 9.36 -10 1 8 49.88 8.20 -10 1 8 40.06 7.56 -10 1 8 38.85 6.54 10 1 -8 38.16 6.18 -10 1 7 226.75 15.52 10 1 -7 213.95 10.88 -10 1 7 214.17 14.68 -10 1 7 217.62 13.73 10 1 -7 217.59 12.66 -10 1 6 77.66 11.16 10 1 -6 77.59 7.70 -10 1 6 73.71 9.43 10 1 -6 77.91 8.46 10 1 -5 12.70 5.13 -10 1 5 12.36 7.27 -10 1 5 16.82 6.09 10 1 -5 18.34 6.18 -10 1 4 94.26 11.69 10 1 -4 85.34 8.96 -10 1 4 103.20 10.54 10 1 -4 97.34 10.40 10 1 -3 17.84 6.10 -10 1 3 12.34 6.33 10 1 -3 7.82 5.27 -10 1 2 42.93 8.68 10 1 -2 24.14 6.61 -10 1 1 108.18 11.28 10 1 -1 107.63 10.37 10 1 0 45.92 7.25 10 1 0 47.49 8.42 10 1 0 49.03 8.98 10 1 1 22.77 5.98 10 1 1 32.29 7.31 10 1 1 21.12 7.29 10 1 2 89.89 10.25 10 1 2 74.99 8.60 10 1 2 86.59 10.05 10 1 3 203.50 14.01 10 1 3 218.87 13.82 10 1 3 203.72 12.30 10 1 3 204.36 13.48 10 1 4 124.55 10.57 10 1 4 148.78 11.11 10 1 4 132.74 9.68 10 1 4 129.55 10.57 10 1 5 73.79 7.08 10 1 5 89.71 8.43 10 1 5 78.62 6.89 10 1 6 21.61 4.62 10 1 6 13.73 3.14 10 1 7 33.15 3.94 -10 2 10 64.97 5.90 -10 2 10 62.89 5.97 10 2 -10 68.33 4.93 -10 2 9 8.14 4.44 -10 2 9 7.74 4.14 -10 2 9 5.54 3.18 10 2 -9 12.07 4.00 -10 2 8 176.54 12.29 10 2 -8 165.86 8.99 -10 2 8 174.00 11.77 -10 2 8 155.60 9.88 10 2 -8 170.07 10.51 10 2 -7 17.21 5.09 -10 2 7 21.82 6.22 -10 2 7 21.02 7.07 -10 2 7 16.97 4.28 10 2 -7 20.38 6.00 -10 2 6 144.86 12.72 10 2 -6 136.30 10.18 -10 2 6 130.46 10.80 10 2 -6 131.92 10.97 10 2 -5 201.34 13.64 10 2 -5 197.36 10.69 -10 2 5 206.33 14.99 10 2 -5 215.14 13.01 10 2 -4 19.94 7.13 10 2 -4 14.85 6.09 -10 2 4 15.36 6.96 10 2 -4 19.68 5.90 10 2 -3 125.90 9.93 -10 2 3 145.33 12.74 10 2 -3 144.09 11.74 10 2 -2 400.19 16.99 -10 2 2 385.48 19.15 10 2 -2 383.63 18.25 10 2 -2 395.47 15.35 10 2 -2 381.24 18.39 10 2 -1 7.63 4.26 -10 2 1 -0.79 5.61 10 2 -1 4.67 5.85 10 2 -1 -1.94 4.95 10 2 0 171.75 13.32 10 2 0 165.63 10.90 10 2 0 179.17 13.06 10 2 1 118.95 11.64 10 2 1 109.23 9.37 10 2 1 113.05 11.60 10 2 1 108.56 10.57 10 2 2 8.91 6.27 10 2 2 4.37 5.09 10 2 2 4.99 5.79 10 2 3 224.17 13.25 10 2 3 270.35 14.86 10 2 3 240.84 13.69 10 2 3 236.71 14.09 10 2 4 108.90 8.56 10 2 4 136.55 10.37 10 2 4 138.02 10.49 10 2 4 128.31 9.86 10 2 5 65.81 7.06 10 2 5 65.69 6.85 10 2 6 160.56 8.56 10 2 6 156.69 8.03 -10 3 9 131.32 8.63 10 3 -9 119.83 6.14 10 3 -9 137.40 7.39 10 3 -8 14.03 3.93 -10 3 8 11.08 3.60 -10 3 8 14.97 4.88 10 3 -8 12.18 4.29 -10 3 7 293.81 15.16 10 3 -7 316.96 13.29 10 3 -7 299.37 13.43 10 3 -6 37.72 6.82 10 3 -6 37.00 6.61 -10 3 6 35.21 7.17 10 3 -6 29.63 4.91 10 3 -5 14.10 5.69 10 3 -5 9.75 5.37 10 3 -5 9.56 3.61 -10 3 5 9.59 5.37 10 3 -5 9.40 4.59 10 3 -4 127.61 10.98 10 3 -4 124.05 8.60 -10 3 4 108.70 10.59 10 3 -4 116.90 9.22 10 3 -4 112.98 10.35 10 3 -3 68.98 7.16 10 3 -3 69.20 8.16 -10 3 3 52.48 7.87 10 3 -3 66.01 9.16 10 3 -2 29.88 7.58 10 3 -2 21.79 5.13 -10 3 2 23.27 5.32 10 3 -2 25.43 6.32 10 3 -2 31.78 7.15 10 3 -1 164.35 11.55 10 3 -1 157.55 10.49 10 3 -1 164.44 12.33 10 3 0 59.68 8.26 10 3 0 65.18 7.93 10 3 0 53.15 8.65 10 3 0 60.02 8.19 10 3 1 180.54 12.76 10 3 1 186.04 11.45 10 3 1 168.26 12.34 10 3 1 170.29 12.32 10 3 2 282.03 14.89 10 3 2 288.00 13.73 10 3 2 277.62 14.80 10 3 2 273.45 14.24 10 3 3 1.61 4.27 10 3 3 -6.86 5.51 10 3 3 3.58 4.13 10 3 4 89.92 7.58 10 3 4 94.25 8.00 10 3 4 88.59 8.05 10 3 5 140.80 7.05 10 3 5 146.18 8.54 10 3 5 161.77 8.63 10 4 -8 81.72 5.62 10 4 -8 86.12 5.68 10 4 -7 63.27 6.05 -10 4 7 53.42 6.19 10 4 -7 50.66 4.25 10 4 -6 17.79 4.36 10 4 -6 27.06 5.00 10 4 -6 23.71 3.68 -10 4 6 18.64 5.14 10 4 -6 19.82 4.12 10 4 -5 108.96 7.04 -10 4 5 102.21 8.76 10 4 -5 117.66 7.95 10 4 -5 115.42 8.96 10 4 -4 36.65 6.56 10 4 -4 45.94 5.64 -10 4 4 35.20 5.85 10 4 -4 35.31 5.88 10 4 -3 64.23 6.78 10 4 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5 -1 15.79 3.26 10 5 0 0.58 3.29 10 5 0 7.69 3.69 10 5 0 4.51 3.35 10 5 0 -2.67 2.27 10 5 0 5.02 2.32 10 5 1 11.00 3.36 10 5 1 17.35 3.93 10 5 1 10.43 3.27 10 5 1 11.77 2.54 10 5 2 3.58 2.61 -11 -4 4 12.98 3.26 -11 -4 3 131.91 7.33 -11 -4 2 46.60 5.08 -11 -4 1 25.44 4.52 -11 -4 0 39.10 4.28 -11 -3 7 195.83 8.63 -11 -3 6 198.79 9.66 -11 -3 5 20.01 3.67 -11 -3 5 35.36 4.75 -11 -3 4 215.63 10.42 -11 -3 4 209.30 10.57 -11 -3 3 111.82 8.48 -11 -3 3 111.64 7.82 -11 -3 2 20.59 5.42 -11 -3 2 24.38 3.85 11 -3 -1 26.50 4.01 -11 -3 1 202.91 11.36 11 -3 0 3.21 2.50 -11 -3 0 -0.80 4.63 11 -3 1 66.42 5.81 -11 -3 -1 78.89 6.51 11 -3 2 142.15 7.37 -11 -2 8 70.62 5.63 -11 -2 7 12.54 3.67 -11 -2 6 37.74 5.71 -11 -2 5 251.91 11.20 -11 -2 5 298.06 13.43 -11 -2 4 6.52 4.54 -11 -2 4 13.81 3.97 -11 -2 3 314.87 14.76 -11 -2 3 312.57 13.07 -11 -2 2 128.00 10.29 11 -2 -2 112.88 8.75 11 -2 -1 40.22 6.32 -11 -2 1 44.57 7.36 11 -2 0 159.79 10.60 -11 -2 0 178.28 11.47 11 -2 1 40.23 6.20 -11 -2 -1 47.47 6.28 11 -2 2 95.78 7.84 -11 -2 -2 85.52 6.98 11 -2 3 97.18 7.14 -11 -1 8 13.52 3.35 -11 -1 7 122.70 8.79 -11 -1 6 51.22 6.45 -11 -1 5 -5.53 3.91 -11 -1 5 10.50 3.99 -11 -1 4 48.81 6.19 -11 -1 4 42.36 6.53 -11 -1 3 13.73 5.52 -11 -1 2 95.04 9.48 11 -1 -1 74.83 6.35 11 -1 0 0.40 5.29 11 -1 0 2.70 2.74 11 -1 1 157.02 11.13 11 -1 1 135.57 8.05 11 -1 2 116.35 9.39 -11 -1 -2 108.84 8.41 11 -1 3 64.18 6.57 -11 -1 -3 56.91 5.41 11 -1 4 52.78 5.32 -11 0 8 67.39 6.11 -11 0 7 0.41 3.12 -11 0 6 41.20 5.55 -11 0 5 8.97 2.65 -11 0 5 -6.41 4.74 -11 0 4 -1.57 3.57 11 0 -3 96.65 7.99 11 0 -2 -0.99 3.41 11 0 -2 -1.79 4.08 11 0 -1 132.01 9.60 11 0 -1 126.48 8.63 11 0 0 42.98 5.88 11 0 0 42.96 5.97 11 0 1 4.32 3.72 11 0 1 1.27 4.64 11 0 1 2.65 3.66 11 0 2 338.97 12.84 11 0 2 348.94 13.37 11 0 3 5.40 3.35 11 0 3 -3.64 4.12 11 0 4 149.00 7.31 11 0 4 150.69 8.12 -11 1 7 112.74 9.21 -11 1 7 101.09 7.17 -11 1 6 79.50 8.62 -11 1 6 62.11 5.42 11 1 -5 2.10 3.10 -11 1 5 14.00 5.60 11 1 -4 62.14 5.66 -11 1 4 68.56 8.31 11 1 -4 55.95 6.10 11 1 -3 29.68 4.59 11 1 -3 32.24 5.24 11 1 -2 107.64 8.63 11 1 -2 87.65 7.21 11 1 -2 110.45 9.12 11 1 -1 103.19 8.61 11 1 -1 93.33 7.38 11 1 -1 109.72 9.17 11 1 0 2.76 2.84 11 1 0 -0.88 4.14 11 1 0 0.05 4.48 11 1 1 171.61 10.68 11 1 1 167.57 10.26 11 1 2 134.31 9.15 11 1 2 112.74 9.17 11 1 2 110.20 6.93 11 1 2 130.46 8.85 11 1 3 55.29 5.91 11 1 3 53.75 5.69 11 1 4 53.24 4.85 -11 2 8 82.74 6.35 -11 2 7 8.33 3.96 -11 2 6 52.20 6.84 11 2 -6 44.30 4.52 -11 2 5 283.45 13.87 11 2 -5 267.19 11.01 -11 2 4 22.97 5.43 11 2 -4 15.62 3.72 11 2 -3 323.40 13.73 11 2 -3 311.22 12.95 11 2 -2 131.04 9.66 11 2 -2 130.81 8.87 11 2 -2 151.04 10.43 11 2 -1 41.18 5.71 11 2 -1 45.03 6.24 11 2 -1 41.74 6.57 11 2 0 174.43 10.91 11 2 0 167.31 10.58 11 2 0 164.09 9.64 11 2 1 45.95 6.40 11 2 1 36.40 5.81 11 2 1 44.26 6.09 11 2 1 34.94 4.96 11 2 2 112.16 7.92 11 2 2 92.76 7.19 11 2 2 113.89 8.13 11 2 2 97.50 6.89 11 2 3 101.17 7.01 11 2 3 85.60 5.86 -11 3 6 169.12 9.12 11 3 -6 174.00 7.73 -11 3 5 32.26 4.94 11 3 -5 41.97 4.84 -11 3 4 185.60 9.81 11 3 -4 200.05 9.79 11 3 -3 120.95 8.23 11 3 -3 104.40 7.80 11 3 -2 20.70 4.57 11 3 -2 26.36 5.10 11 3 -2 28.51 5.28 11 3 -1 186.07 10.23 11 3 -1 183.53 9.92 11 3 -1 187.07 10.42 11 3 0 2.40 3.22 11 3 0 5.04 3.73 11 3 0 2.75 3.10 11 3 1 81.06 6.55 11 3 1 62.49 5.65 11 3 1 68.63 6.02 11 3 2 173.82 8.42 11 3 2 177.31 8.33 11 3 2 171.56 8.04 11 4 -4 28.45 3.56 11 4 -4 26.66 3.77 11 4 -4 22.86 3.51 11 4 -3 133.31 7.26 11 4 -3 125.16 7.00 11 4 -3 110.38 6.64 11 4 -2 39.62 4.56 11 4 -2 32.23 4.24 11 4 -2 36.23 4.13 11 4 -1 42.31 4.47 11 4 -1 40.20 4.40 11 4 -1 40.36 4.08 11 4 0 36.73 4.03 11 4 0 39.46 4.16 -12 -1 2 31.15 4.03 -12 -1 1 12.91 2.99 12 0 -3 3.20 2.52 12 0 -2 146.20 7.84 -12 0 2 131.35 7.12 -12 0 1 28.43 3.97 12 0 -1 32.72 4.12 -12 0 0 6.43 2.72 12 0 0 5.60 3.10 12 1 -2 32.52 4.44 12 1 -1 10.12 2.77 0 0 0 0.00 0.00 TITL AMD-R855_2 in P2(1) REM P2(1) (#4 in standard setting) CELL 1.54184 9.622667 8.230384 12.915788 90.0000 98.3521 90.0000 ZERR 2.00 0.000255 0.000263 0.000327 0.0000 0.0024 0.0000 LATT -1 SYMM -x, y+1/2,-z SFAC C H N Cl Cu UNIT 42.00 62.00 2.00 2.00 2.00 REM CrysAlisPro recorded range (K): Min=139.9; max=140.1; aver:140.0 TEMP -133 SIZE 0.04 0.06 0.66 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 65234 _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 - Detector area scaling - B-factor correction ; _oxdiff_exptl_absorpt_empirical_full_max 1.523 _oxdiff_exptl_absorpt_empirical_full_min 0.741 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 Cu1 Cu 0.40793(5) 0.69425(6) 0.81369(4) 0.02803(13) Uani 1 1 d . . . . . Cl1 Cl 0.55455(9) 0.88636(11) 0.82679(7) 0.0365(2) Uani 1 1 d . . . . . N1 N 0.3209(3) 0.3637(4) 0.8025(2) 0.0251(6) Uani 1 1 d . . . . . C1 C 0.2852(3) 0.5144(5) 0.8114(2) 0.0268(7) Uani 1 1 d . . . . . C2 C 0.1326(3) 0.5228(5) 0.8302(3) 0.0307(8) Uani 1 1 d . . . . . C3 C 0.0799(4) 0.3468(5) 0.8126(3) 0.0363(9) Uani 1 1 d . . . . . H3A H 0.024926 0.314295 0.868312 0.044 Uiso 1 1 calc R U . . . H3B H 0.019042 0.337163 0.744176 0.044 Uiso 1 1 calc R U . . . C4 C 0.2101(4) 0.2373(4) 0.8151(3) 0.0294(8) Uani 1 1 d . . . . . C5 C 0.4691(3) 0.3103(5) 0.7961(2) 0.0268(7) Uani 1 1 d . . . . . H5 H 0.468675 0.189078 0.791045 0.032 Uiso 1 1 calc R U . . . C6 C 0.5206(3) 0.3767(4) 0.6973(2) 0.0250(6) Uani 1 1 d . . . . . H6 H 0.507048 0.497189 0.696062 0.030 Uiso 1 1 calc R U . . . C7 C 0.6770(4) 0.3424(6) 0.6979(3) 0.0410(10) Uani 1 1 d . . . . . H7A H 0.693732 0.223795 0.703483 0.049 Uiso 1 1 calc R U . . . H7B H 0.731819 0.394822 0.759711 0.049 Uiso 1 1 calc R U . . . C8 C 0.7273(4) 0.4061(6) 0.5984(3) 0.0449(10) Uani 1 1 d . . . . . H8A H 0.716491 0.525720 0.595294 0.054 Uiso 1 1 calc R U . . . H8B H 0.828281 0.380725 0.600732 0.054 Uiso 1 1 calc R U . . . C9 C 0.6454(4) 0.3317(5) 0.5010(3) 0.0339(8) Uani 1 1 d . . . . . H9A H 0.663448 0.213268 0.500368 0.041 Uiso 1 1 calc R U . . . H9B H 0.677209 0.379615 0.438132 0.041 Uiso 1 1 calc R U . . . C10 C 0.4883(4) 0.3620(6) 0.4977(3) 0.0369(9) Uani 1 1 d . . . . . H10A H 0.436149 0.302962 0.437412 0.044 Uiso 1 1 calc R U . . . H10B H 0.468996 0.479418 0.487157 0.044 Uiso 1 1 calc R U . . . C11 C 0.4360(3) 0.3066(5) 0.5982(3) 0.0291(7) Uani 1 1 d . . . . . H11A H 0.336483 0.339194 0.595336 0.035 Uiso 1 1 calc R U . . . H11B H 0.440112 0.186475 0.601947 0.035 Uiso 1 1 calc R U . . . C12 C 0.5624(4) 0.3562(5) 0.8978(3) 0.0351(8) Uani 1 1 d . . . . . H12A H 0.580458 0.473394 0.898554 0.053 Uiso 1 1 calc R U . . . H12B H 0.651678 0.297360 0.902638 0.053 Uiso 1 1 calc R U . . . H12C H 0.515009 0.327231 0.957424 0.053 Uiso 1 1 calc R U . . . C13 C 0.0498(3) 0.6407(4) 0.7536(3) 0.0291(7) Uani 1 1 d . . . . . C14 C 0.0798(3) 0.6499(5) 0.6507(3) 0.0370(9) Uani 1 1 d . . . . . H14 H 0.153187 0.585083 0.630710 0.044 Uiso 1 1 calc R U . . . C15 C 0.0046(4) 0.7517(6) 0.5776(3) 0.0439(11) Uani 1 1 d . . . . . H15 H 0.026970 0.756418 0.508376 0.053 Uiso 1 1 calc R U . . . C16 C -0.1029(4) 0.8465(6) 0.6051(4) 0.0442(10) Uani 1 1 d . . . . . H16 H -0.153575 0.917738 0.555338 0.053 Uiso 1 1 calc R U . . . C17 C -0.1360(4) 0.8370(6) 0.7050(4) 0.0434(10) Uani 1 1 d . . . . . H17 H -0.211329 0.899749 0.723822 0.052 Uiso 1 1 calc R U . . . C18 C -0.0590(4) 0.7349(5) 0.7789(3) 0.0354(9) Uani 1 1 d . . . . . H18 H -0.082076 0.730544 0.847946 0.042 Uiso 1 1 calc R U . . . C19 C 0.1364(4) 0.5785(6) 0.9448(3) 0.0396(9) Uani 1 1 d . . . . . H19A H 0.203470 0.511541 0.990677 0.059 Uiso 1 1 calc R U . . . H19B H 0.042659 0.566706 0.965192 0.059 Uiso 1 1 calc R U . . . H19C H 0.165309 0.692662 0.951329 0.059 Uiso 1 1 calc R U . . . C20 C 0.2507(4) 0.1505(5) 0.9197(3) 0.0372(9) Uani 1 1 d . . . . . H20A H 0.338678 0.090906 0.918693 0.056 Uiso 1 1 calc R U . . . H20B H 0.176193 0.074202 0.931006 0.056 Uiso 1 1 calc R U . . . H20C H 0.263278 0.230678 0.976339 0.056 Uiso 1 1 calc R U . . . C21 C 0.1931(4) 0.1151(5) 0.7261(3) 0.0368(8) Uani 1 1 d . . . . . H21A H 0.175477 0.172824 0.659080 0.055 Uiso 1 1 calc R U . . . H21B H 0.113725 0.043190 0.732749 0.055 Uiso 1 1 calc R U . . . H21C H 0.279099 0.050488 0.728952 0.055 Uiso 1 1 calc R U . . . 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 Cu1 0.0263(2) 0.0258(3) 0.0321(2) -0.0019(2) 0.00448(15) -0.0003(2) Cl1 0.0372(4) 0.0273(5) 0.0466(5) -0.0019(4) 0.0119(3) -0.0056(4) N1 0.0225(12) 0.0289(17) 0.0236(12) 0.0003(11) 0.0022(9) -0.0019(12) C1 0.0243(15) 0.032(2) 0.0234(14) 0.0011(13) 0.0011(12) 0.0003(13) C2 0.0258(16) 0.038(2) 0.0283(16) 0.0004(14) 0.0055(12) 0.0007(14) C3 0.0247(16) 0.041(2) 0.0431(19) 0.0054(17) 0.0046(14) -0.0048(15) C4 0.0289(16) 0.029(2) 0.0306(16) 0.0042(13) 0.0048(12) -0.0043(13) C5 0.0223(15) 0.0284(19) 0.0292(16) 0.0013(13) 0.0014(12) 0.0016(13) C6 0.0237(14) 0.0217(17) 0.0299(14) -0.0012(13) 0.0048(11) -0.0006(13) C7 0.0231(16) 0.063(3) 0.0367(18) -0.0064(18) 0.0032(13) -0.0013(16) C8 0.0291(17) 0.061(3) 0.047(2) -0.006(2) 0.0135(15) -0.0122(18) C9 0.0336(18) 0.035(2) 0.0347(17) 0.0014(15) 0.0113(14) -0.0022(15) C10 0.0328(17) 0.047(3) 0.0317(16) 0.0072(16) 0.0065(13) 0.0016(17) C11 0.0260(16) 0.034(2) 0.0276(15) 0.0011(13) 0.0031(12) -0.0013(14) C12 0.0270(16) 0.048(3) 0.0284(16) -0.0003(15) -0.0033(12) 0.0027(16) C13 0.0213(14) 0.034(2) 0.0310(16) -0.0004(13) 0.0022(12) -0.0039(13) C14 0.0261(15) 0.052(3) 0.0335(17) -0.0003(15) 0.0054(13) 0.0020(15) C15 0.0302(18) 0.066(3) 0.0340(18) 0.0094(17) -0.0002(14) -0.0059(17) C16 0.0289(17) 0.048(3) 0.052(2) 0.015(2) -0.0062(15) -0.0059(17) C17 0.0245(16) 0.040(2) 0.065(3) 0.004(2) 0.0043(16) 0.0043(15) C18 0.0280(16) 0.040(3) 0.0394(18) 0.0024(15) 0.0090(13) 0.0023(14) C19 0.0365(18) 0.054(3) 0.0290(17) 0.0000(17) 0.0065(14) 0.0071(18) C20 0.0392(18) 0.039(3) 0.0346(17) 0.0103(14) 0.0090(14) -0.0005(15) C21 0.0375(18) 0.037(2) 0.0356(18) -0.0017(15) 0.0026(14) -0.0139(16) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1 0 0 0.0251 -1 0 0 0.0100 0 0 1 0.0415 0 0 -1 0.0132 0 -1 0 0.2660 0 1 0 0.3952 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 C1 Cu1 Cl1 175.41(11) . . ? C1 N1 C4 116.6(3) . . ? C1 N1 C5 123.3(3) . . ? C5 N1 C4 119.5(3) . . ? N1 C1 Cu1 125.3(2) . . ? N1 C1 C2 109.3(3) . . ? C2 C1 Cu1 125.2(3) . . ? C1 C2 C3 103.8(3) . . ? C1 C2 C13 110.5(3) . . ? C1 C2 C19 106.1(3) . . ? C3 C2 C19 112.4(3) . . ? C13 C2 C3 111.9(3) . . ? C13 C2 C19 111.7(3) . . ? C2 C3 H3A 110.3 . . ? C2 C3 H3B 110.3 . . ? H3A C3 H3B 108.5 . . ? C4 C3 C2 107.3(3) . . ? C4 C3 H3A 110.3 . . ? C4 C3 H3B 110.3 . . ? N1 C4 C3 100.3(3) . . ? N1 C4 C20 108.8(3) . . ? N1 C4 C21 112.0(3) . . ? C20 C4 C3 113.3(3) . . ? C21 C4 C3 112.0(3) . . ? C21 C4 C20 110.2(3) . . ? N1 C5 H5 107.4 . . ? N1 C5 C6 111.3(3) . . ? N1 C5 C12 108.9(3) . . ? C6 C5 H5 107.4 . . ? C12 C5 H5 107.4 . . ? C12 C5 C6 114.0(3) . . ? C5 C6 H6 108.0 . . ? C7 C6 C5 111.5(3) . . ? C7 C6 H6 108.0 . . ? C11 C6 C5 111.4(3) . . ? C11 C6 H6 108.0 . . ? C11 C6 C7 109.8(3) . . ? C6 C7 H7A 109.4 . . ? C6 C7 H7B 109.4 . . ? C6 C7 C8 111.3(3) . . ? H7A C7 H7B 108.0 . . ? C8 C7 H7A 109.4 . . ? C8 C7 H7B 109.4 . . ? C7 C8 H8A 109.3 . . ? C7 C8 H8B 109.3 . . ? H8A C8 H8B 107.9 . . ? C9 C8 C7 111.7(3) . . ? C9 C8 H8A 109.3 . . ? C9 C8 H8B 109.3 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? C8 C9 C10 110.5(3) . . ? H9A C9 H9B 108.1 . . ? C10 C9 H9A 109.5 . . ? C10 C9 H9B 109.5 . . ? C9 C10 H10A 109.2 . . ? C9 C10 H10B 109.2 . . ? C9 C10 C11 112.0(3) . . ? H10A C10 H10B 107.9 . . ? C11 C10 H10A 109.2 . . ? C11 C10 H10B 109.2 . . ? C6 C11 C10 113.4(3) . . ? C6 C11 H11A 108.9 . . ? C6 C11 H11B 108.9 . . ? C10 C11 H11A 108.9 . . ? C10 C11 H11B 108.9 . . ? H11A C11 H11B 107.7 . . ? C5 C12 H12A 109.5 . . ? C5 C12 H12B 109.5 . . ? C5 C12 H12C 109.5 . . ? H12A C12 H12B 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 C2 119.2(3) . . ? C18 C13 C2 123.2(3) . . ? C18 C13 C14 117.5(3) . . ? C13 C14 H14 119.4 . . ? C15 C14 C13 121.3(4) . . ? C15 C14 H14 119.4 . . ? C14 C15 H15 119.9 . . ? C16 C15 C14 120.2(4) . . ? C16 C15 H15 119.9 . . ? C15 C16 H16 120.2 . . ? C17 C16 C15 119.5(4) . . ? C17 C16 H16 120.2 . . ? C16 C17 H17 119.9 . . ? C16 C17 C18 120.2(4) . . ? C18 C17 H17 119.9 . . ? C13 C18 C17 121.3(4) . . ? C13 C18 H18 119.3 . . ? C17 C18 H18 119.3 . . ? C2 C19 H19A 109.5 . . ? C2 C19 H19B 109.5 . . ? C2 C19 H19C 109.5 . . ? H19A C19 H19B 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C4 C20 H20A 109.5 . . ? C4 C20 H20B 109.5 . . ? C4 C20 H20C 109.5 . . ? H20A C20 H20B 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C4 C21 H21A 109.5 . . ? C4 C21 H21B 109.5 . . ? C4 C21 H21C 109.5 . . ? H21A C21 H21B 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 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 Cu1 Cl1 2.1095(10) . ? Cu1 C1 1.891(4) . ? N1 C1 1.296(5) . ? N1 C4 1.515(4) . ? N1 C5 1.507(4) . ? C1 C2 1.524(4) . ? C2 C3 1.540(6) . ? C2 C13 1.525(5) . ? C2 C19 1.546(5) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C3 C4 1.539(5) . ? C4 C20 1.528(5) . ? C4 C21 1.518(5) . ? C5 H5 1.0000 . ? C5 C6 1.535(4) . ? C5 C12 1.526(4) . ? C6 H6 1.0000 . ? C6 C7 1.530(4) . ? C6 C11 1.527(4) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C7 C8 1.530(5) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C8 C9 1.513(5) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C9 C10 1.527(5) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C10 C11 1.529(5) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.403(5) . ? C13 C18 1.379(5) . ? C14 H14 0.9500 . ? C14 C15 1.385(6) . ? C15 H15 0.9500 . ? C15 C16 1.383(7) . ? C16 H16 0.9500 . ? C16 C17 1.375(7) . ? C17 H17 0.9500 . ? C17 C18 1.401(6) . ? C18 H18 0.9500 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cu1 C1 C2 C3 176.5(2) . . . . ? Cu1 C1 C2 C13 56.4(4) . . . . ? Cu1 C1 C2 C19 -64.8(4) . . . . ? N1 C1 C2 C3 -8.8(3) . . . . ? N1 C1 C2 C13 -128.9(3) . . . . ? N1 C1 C2 C19 109.9(3) . . . . ? N1 C5 C6 C7 172.3(3) . . . . ? N1 C5 C6 C11 -64.7(4) . . . . ? C1 N1 C4 C3 11.1(4) . . . . ? C1 N1 C4 C20 -108.0(3) . . . . ? C1 N1 C4 C21 130.0(3) . . . . ? C1 N1 C5 C6 -63.7(4) . . . . ? C1 N1 C5 C12 62.9(4) . . . . ? C1 C2 C3 C4 15.4(4) . . . . ? C1 C2 C13 C14 36.7(5) . . . . ? C1 C2 C13 C18 -146.4(3) . . . . ? C2 C3 C4 N1 -15.6(3) . . . . ? C2 C3 C4 C20 100.2(3) . . . . ? C2 C3 C4 C21 -134.5(3) . . . . ? C2 C13 C14 C15 178.1(4) . . . . ? C2 C13 C18 C17 -177.4(4) . . . . ? C3 C2 C13 C14 -78.4(4) . . . . ? C3 C2 C13 C18 98.5(4) . . . . ? C4 N1 C1 Cu1 173.1(2) . . . . ? C4 N1 C1 C2 -1.6(4) . . . . ? C4 N1 C5 C6 125.6(3) . . . . ? C4 N1 C5 C12 -107.9(3) . . . . ? C5 N1 C1 Cu1 2.1(4) . . . . ? C5 N1 C1 C2 -172.6(3) . . . . ? C5 N1 C4 C3 -177.6(3) . . . . ? C5 N1 C4 C20 63.4(4) . . . . ? C5 N1 C4 C21 -58.7(4) . . . . ? C5 C6 C7 C8 179.0(3) . . . . ? C5 C6 C11 C10 -176.9(3) . . . . ? C6 C7 C8 C9 -58.2(5) . . . . ? C7 C6 C11 C10 -52.9(4) . . . . ? C7 C8 C9 C10 56.3(5) . . . . ? C8 C9 C10 C11 -53.2(5) . . . . ? C9 C10 C11 C6 52.7(5) . . . . ? C11 C6 C7 C8 55.1(5) . . . . ? C12 C5 C6 C7 48.6(4) . . . . ? C12 C5 C6 C11 171.6(3) . . . . ? C13 C2 C3 C4 134.6(3) . . . . ? C13 C14 C15 C16 -0.3(6) . . . . ? C14 C13 C18 C17 -0.4(6) . . . . ? C14 C15 C16 C17 -1.0(6) . . . . ? C15 C16 C17 C18 1.6(7) . . . . ? C16 C17 C18 C13 -0.8(6) . . . . ? C18 C13 C14 C15 1.0(6) . . . . ? C19 C2 C3 C4 -98.8(3) . . . . ? C19 C2 C13 C14 154.5(3) . . . . ? C19 C2 C13 C18 -28.6(5) . . . . ? loop_ _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z 1.0000 -0.0000 -0.0000 0.0028 0.1593 0.0281 -1.0000 0.0000 0.0000 -0.0028 -0.1593 -0.0281 0.0000 -0.0000 1.0000 -0.1178 0.0165 0.0195 -0.0000 0.0000 -1.0000 0.1178 -0.0165 -0.0195 0.0000 -1.0000 0.0000 0.0256 -0.0328 0.1826 -0.0000 1.0000 -0.0000 -0.0256 0.0328 -0.1826