#------------------------------------------------------------------------------ #$Date: 2018-03-17 07:53:13 +0200 (Sat, 17 Mar 2018) $ #$Revision: 207000 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/54/90/1549077.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_1549077 loop_ _publ_author_name 'Xu, Jiaxi' 'Liu, Jingjing' 'Li, Zhenjiang' 'Xu, Songquan' 'Wang, Haixin' 'Guo, Tianfo' 'Gao, Yu' 'Zhang, Lei' 'Zhang, Chan' 'Guo, Kai' _publ_section_title ; Opposite-charge repulsive cation and anion pair cooperative organocatalysis in ring-opening polymerization ; _journal_name_full 'Polymer Chemistry' _journal_paper_doi 10.1039/C8PY00338F _journal_year 2018 _chemical_formula_sum 'C21 H18 Cl N3' _chemical_formula_weight 347.83 _space_group_crystal_system cubic _space_group_IT_number 198 _space_group_name_Hall 'P 2ac 2ab 3' _space_group_name_H-M_alt 'P 21 3' _symmetry_space_group_name_Hall 'P 2ac 2ab 3' _symmetry_space_group_name_H-M 'P 21 3' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2016-10-14 deposited with the CCDC. 2018-03-14 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 13.4840(8) _cell_length_b 13.4840(8) _cell_length_c 13.4840(8) _cell_measurement_reflns_used 8242 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 28.28 _cell_measurement_theta_min 2.62 _cell_volume 2451.6(3) _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _diffrn_ambient_temperature 296(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0890 _diffrn_reflns_av_unetI/netI 0.0343 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 23175 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.319 _diffrn_reflns_theta_min 2.136 _exptl_absorpt_coefficient_mu 0.161 _exptl_absorpt_correction_T_max 0.9653 _exptl_absorpt_correction_T_min 0.9577 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 0.942 _exptl_crystal_description block _exptl_crystal_F_000 728 _exptl_crystal_size_max 0.270 _exptl_crystal_size_mid 0.250 _exptl_crystal_size_min 0.220 _refine_diff_density_max 0.703 _refine_diff_density_min -0.437 _refine_diff_density_rms 0.108 _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack 0.2(3) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.140 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 86 _refine_ls_number_reflns 2045 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.142 _refine_ls_R_factor_all 0.1140 _refine_ls_R_factor_gt 0.1082 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1820P)^2^+3.4136P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.3079 _refine_ls_wR_factor_ref 0.3135 _reflns_Friedel_coverage 0.788 _reflns_Friedel_fraction_full 0.998 _reflns_Friedel_fraction_max 0.999 _reflns_number_gt 1846 _reflns_number_total 2045 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c8py00338f2.cif _cod_data_source_block 20160728lmf_0m_a_sqd _cod_depositor_comments ; The following automatic conversions were performed: '_exptl_absorpt_correction_type' value 'MULTI-SCAN' changed to 'multi-scan' according to /home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26. Automatic conversion script Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas ; _cod_original_cell_volume 2451.6(4) _cod_database_code 1549077 _shelx_shelxl_version_number 2014/7 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_min 0.958 _shelx_estimated_absorpt_t_max 0.965 _platon_squeeze_void_probe_radius 1.20 _shelx_res_file ; 20160728lmf_0m_a_sqd.res created by SHELXL-2014/7 TITL 20160728LMF_0m_a.res in P2(1)2(1 New: P213 CELL 0.71073 13.4840 13.4840 13.4840 90.000 90.000 90.000 ZERR 4 0.0008 0.0008 0.0008 0.000 0.000 0.000 LATT -1 SYMM 0.50000 - X , - Y , 0.50000 + Z SYMM 0.50000 + X , 0.50000 - Y , - Z SYMM - X , 0.50000 + Y , 0.50000 - Z SYMM Z , X , Y SYMM 0.50000 - Z , - X , 0.50000 + Y SYMM 0.50000 + Z , 0.50000 - X , - Y SYMM - Z , 0.50000 + X , 0.50000 - Y SYMM Y , Z , X SYMM 0.50000 + Y , 0.50000 - Z , - X SYMM - Y , 0.50000 + Z , 0.50000 - X SYMM 0.50000 - Y , - Z , 0.50000 + X SFAC C H Cl N UNIT 84 72 4 12 L.S. 20 ACTA BOND $H FMAP 2 PLAN 0 DFIX 1.38 .01 C1 C6 WGHT 0.182000 3.413600 BASF 0.19349 FVAR 6.54521 RESI 0 SIZE .27 .25 .22 TWIN CONF TEMP 23 PART 1 N1 4 0.999765 0.808200 0.308224 10.50000 0.02434 0.02325 = 0.01201 0.00301 0.00341 -0.00245 AFIX 3 H1A 2 0.973925 0.761380 0.342974 11.00000 -1.20000 PART 2 AFIX 0 N1' 4 1.058055 0.939239 0.252149 10.50000 0.04762 0.04839 = 0.03294 0.01785 -0.00780 -0.01241 PART 1 C1 1 0.957464 0.931319 0.199748 11.00000 0.06487 0.14261 = 0.04039 0.03072 -0.00914 -0.07194 AFIX 43 H1 2 0.999953 0.969393 0.238503 11.00000 -1.20000 PART 0 AFIX 0 C2 1 0.905984 0.972881 0.124472 11.00000 0.07124 0.06554 = 0.08930 0.01750 0.01560 -0.03467 AFIX 43 H2 2 0.919643 1.038292 0.107392 11.00000 -1.20000 AFIX 0 C3 1 0.835764 0.923810 0.073061 11.00000 0.04139 0.08032 = 0.06040 0.04706 -0.01352 -0.02081 AFIX 43 H3 2 0.795378 0.956132 0.027441 11.00000 -1.20000 AFIX 0 C4 1 0.826561 0.825575 0.090665 11.00000 0.05133 0.08260 = 0.03597 0.00408 -0.00974 -0.02612 AFIX 43 H4 2 0.782874 0.788285 0.052483 11.00000 -1.20000 AFIX 0 C5 1 0.880415 0.779915 0.163731 11.00000 0.07283 0.05527 = 0.07520 0.03430 0.01140 -0.00236 AFIX 43 H5 2 0.871953 0.712615 0.176221 11.00000 -1.20000 AFIX 0 C6 1 0.946036 0.833487 0.217611 11.00000 0.04387 0.14172 = 0.05545 0.05982 -0.01998 -0.03080 C7 1 1.080881 0.847470 0.345445 11.00000 0.05369 0.04477 = 0.03928 -0.00415 -0.00449 -0.00631 PART 1 CL1 3 0.875949 0.624051 0.375949 10.33333 0.02984 0.02984 = 0.02984 -0.00929 0.00929 -0.00929 PART 0 HKLF 4 1 0.0000 0.0000 1.0000 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 REM 20160728LMF_0m_a.res in P2(1)2(1 New: P213 REM R1 = 0.1082 for 1846 Fo > 4sig(Fo) and 0.1140 for all 2045 data REM 86 parameters refined using 1 restraints END WGHT 0.1839 3.8143 REM Highest difference peak 0.703, deepest hole -0.437, 1-sigma level 0.108 Q1 1 1.1002 0.8971 0.3241 11.00000 0.05 0.70 Q2 1 0.9078 0.5840 0.3539 11.00000 0.05 0.50 Q3 1 0.8378 0.6446 0.3638 11.00000 0.05 0.50 Q4 1 0.7968 0.7032 0.2968 10.33333 0.05 0.45 Q5 1 0.8834 0.9299 0.1015 11.00000 0.05 0.44 Q6 1 0.6780 0.8165 -0.1702 11.00000 0.05 0.43 Q7 1 0.8421 0.8768 0.0957 11.00000 0.05 0.38 Q8 1 0.9670 0.8847 0.1989 11.00000 0.05 0.38 Q9 1 1.0360 1.0360 0.0360 10.33333 0.05 0.36 Q10 1 1.0655 0.7720 0.2399 11.00000 0.05 0.33 Q11 1 0.9074 0.8393 0.1785 11.00000 0.05 0.33 Q12 1 0.9246 0.9043 0.1478 11.00000 0.05 0.31 Q13 1 0.9488 0.9571 0.0604 11.00000 0.05 0.31 Q14 1 0.7735 0.7796 0.2097 11.00000 0.05 0.31 Q15 1 0.9018 1.1028 0.1475 11.00000 0.05 0.31 Q16 1 0.7317 0.7683 0.2317 10.33333 0.05 0.31 Q17 1 0.8977 0.6569 0.1480 11.00000 0.05 0.31 Q18 1 0.9847 0.9216 0.0635 11.00000 0.05 0.30 Q19 1 0.9342 0.9342 -0.0658 10.33333 0.05 0.29 Q20 1 0.9325 0.9554 0.0807 11.00000 0.05 0.29 ; _shelx_res_checksum 10707 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' 'z, x, y' '-z+1/2, -x, y+1/2' 'z+1/2, -x+1/2, -y' '-z, x+1/2, -y+1/2' 'y, z, x' 'y+1/2, -z+1/2, -x' '-y, z+1/2, -x+1/2' '-y+1/2, -z, x+1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group N1 N 0.9998(6) 0.8082(6) 0.3082(6) 0.0199(16) Uani 0.5 1 d . . P A 1 H1A H 0.9739 0.7614 0.3430 0.024 Uiso 1 1 d R U . A 1 N1' N 1.0581(10) 0.9392(9) 0.2521(8) 0.043(3) Uani 0.5 1 d . . P . 2 C1 C 0.9575(7) 0.9313(9) 0.1997(7) 0.083(4) Uani 1 1 d D . . B 1 H1 H 1.0000 0.9694 0.2385 0.099 Uiso 1 1 calc R U . B 1 C2 C 0.9060(8) 0.9729(8) 0.1245(9) 0.075(3) Uani 1 1 d . . . . . H2 H 0.9196 1.0383 0.1074 0.090 Uiso 1 1 calc R U . B 1 C3 C 0.8358(6) 0.9238(7) 0.0731(7) 0.061(3) Uani 1 1 d . . . . . H3 H 0.7954 0.9561 0.0274 0.073 Uiso 1 1 calc R U . . . C4 C 0.8266(7) 0.8256(8) 0.0907(6) 0.057(2) Uani 1 1 d . . . . . H4 H 0.7829 0.7883 0.0525 0.068 Uiso 1 1 calc R U . . . C5 C 0.8804(8) 0.7799(7) 0.1637(8) 0.068(3) Uani 1 1 d . . . . . H5 H 0.8720 0.7126 0.1762 0.081 Uiso 1 1 calc R U . . . C6 C 0.9460(7) 0.8335(9) 0.2176(7) 0.080(4) Uani 1 1 d D . . . . C7 C 1.0809(6) 0.8475(6) 0.3454(5) 0.0459(17) Uani 1 1 d . . . . . Cl1 Cl 0.87595(11) 0.62405(11) 0.37595(11) 0.0298(6) Uani 1 3 d S T P C 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.024(4) 0.023(4) 0.012(3) 0.003(3) 0.003(3) -0.002(3) N1' 0.048(6) 0.048(6) 0.033(5) 0.018(5) -0.008(5) -0.012(5) C1 0.065(5) 0.143(10) 0.040(4) 0.031(5) -0.009(4) -0.072(7) C2 0.071(6) 0.066(5) 0.089(7) 0.018(5) 0.016(6) -0.035(5) C3 0.041(4) 0.080(6) 0.060(5) 0.047(5) -0.014(3) -0.021(4) C4 0.051(4) 0.083(6) 0.036(3) 0.004(4) -0.010(3) -0.026(4) C5 0.073(6) 0.055(5) 0.075(6) 0.034(4) 0.011(5) -0.002(4) C6 0.044(4) 0.142(10) 0.055(5) 0.060(6) -0.020(4) -0.031(5) C7 0.054(4) 0.045(4) 0.039(3) -0.004(3) -0.004(3) -0.006(3) Cl1 0.0298(6) 0.0298(6) 0.0298(6) -0.0093(5) 0.0093(5) -0.0093(5) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 C7 N1 C6 129.6(8) . . C7 N1 H1A 115.1 . . C6 N1 H1A 115.2 . . C7 N1' C7 44.7(5) . 6_674 C6 C1 C2 118.7(9) . . C6 C1 H1 120.6 . . C2 C1 H1 120.6 . . C3 C2 C1 122.9(9) . . C3 C2 H2 118.5 . . C1 C2 H2 118.5 . . C4 C3 C2 117.1(8) . . C4 C3 H3 121.4 . . C2 C3 H3 121.4 . . C3 C4 C5 121.2(9) . . C3 C4 H4 119.4 . . C5 C4 H4 119.4 . . C4 C5 C6 119.5(8) . . C4 C5 H5 120.2 . . C6 C5 H5 120.2 . . C1 C6 C5 120.0(8) . . C1 C6 N1 108.7(9) . . C5 C6 N1 130.4(8) . . N1 C7 C7 147.7(9) . 11_756 N1 C7 C7 152.2(9) . 6_674 C7 C7 C7 59.999(2) 11_756 6_674 C7 C7 N1' 129.6(7) 11_756 . C7 C7 N1' 69.8(7) 6_674 . C7 C7 N1' 65.4(7) 11_756 11_756 C7 C7 N1' 125.2(7) 6_674 11_756 N1' C7 N1' 161.7(8) . 11_756 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 N1 C7 1.315(11) . N1 C6 1.461(11) . N1 H1A 0.8600 . N1' C7 1.791(13) . N1' C7 1.849(14) 6_674 C1 C6 1.350(11) . C1 C2 1.351(15) . C1 H1 0.9300 . C2 C3 1.347(14) . C2 H2 0.9300 . C3 C4 1.351(13) . C3 H3 0.9300 . C4 C5 1.370(13) . C4 H4 0.9300 . C5 C6 1.354(15) . C5 H5 0.9300 . C7 C7 1.386(13) 11_756 C7 C7 1.386(13) 6_674 C7 N1' 1.849(14) 11_756 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_4 C6 C1 C2 C3 7.3(17) . . C1 C2 C3 C4 -8.4(17) . . C2 C3 C4 C5 5.5(15) . . C3 C4 C5 C6 -1.8(16) . . C2 C1 C6 C5 -3.2(16) . . C2 C1 C6 N1 -173.7(10) . . C4 C5 C6 C1 0.5(16) . . C4 C5 C6 N1 168.8(11) . . C7 N1 C6 C1 -31.0(14) . . C7 N1 C6 C5 159.7(11) . . C6 N1 C7 C7 -176.6(8) . 11_756 C6 N1 C7 C7 8.9(18) . 6_674 C7 N1' C7 C7 6.4(6) 6_674 11_756 C7 N1' C7 N1' 147(3) 6_674 11_756 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.096 -0.118 0.590 963 355 ' '