#------------------------------------------------------------------------------ #$Date: 2019-11-08 00:04:46 +0200 (Fri, 08 Nov 2019) $ #$Revision: 224181 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/04/96/7049648.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_7049648 loop_ _publ_author_name 'Hua, Xiu-Ni' 'Gao, Ji-Xing' 'Chen, Xiao-Gang' 'Li, Peng-Fei' 'Mei, Guang-Quan' 'Liao, Wei-Qiang' _publ_section_title ; Ultrahigh phase transition temperature in a metal-halide perovskite-type material containing unprecedented hydrogen bonding interactions. ; _journal_issue 19 _journal_name_full 'Dalton transactions (Cambridge, England : 2003)' _journal_page_first 6621 _journal_page_last 6626 _journal_paper_doi 10.1039/c9dt00945k _journal_volume 48 _journal_year 2019 _chemical_formula_moiety 'Cd Cl3, C4 H12 N O' _chemical_formula_sum 'C4 H12 Cd Cl3 N O' _chemical_formula_weight 308.91 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _audit_block_doi 10.5517/ccdc.csd.cc220bjz _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2019-04-01 deposited with the CCDC. 2019-04-09 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 95.511(4) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 10.0482(5) _cell_length_b 14.6113(7) _cell_length_c 6.8335(3) _cell_measurement_reflns_used 5983 _cell_measurement_temperature 413(2) _cell_measurement_theta_max 30.6950 _cell_measurement_theta_min 3.2860 _cell_volume 998.64(8) _computing_cell_refinement 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_data_collection 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_data_reduction 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_molecular_graphics 'DIAMOND (Brandenburg & Putz, 2005)' _computing_publication_material 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution 'SHELXL-2014/7 (Sheldrick, 2014)' _diffrn_ambient_temperature 413(2) _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measurement_device_type 'XtaLAB Synergy R, DW system, HyPix' _diffrn_measurement_method 'four-circle diffractometer' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0682 _diffrn_reflns_av_unetI/netI 0.0390 _diffrn_reflns_Laue_measured_fraction_full 0.994 _diffrn_reflns_Laue_measured_fraction_max 0.994 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_number 6964 _diffrn_reflns_point_group_measured_fraction_full 0.994 _diffrn_reflns_point_group_measured_fraction_max 0.994 _diffrn_reflns_theta_full 25.022 _diffrn_reflns_theta_max 25.022 _diffrn_reflns_theta_min 2.468 _diffrn_source 'Rotating-anode X-ray tube' _exptl_absorpt_coefficient_mu 2.932 _exptl_absorpt_correction_T_max 0.710 _exptl_absorpt_correction_T_min 0.703 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 2.055 _exptl_crystal_density_method 'not measured' _exptl_crystal_description strip _exptl_crystal_F_000 600 _exptl_crystal_size_max 0.120 _exptl_crystal_size_mid 0.120 _exptl_crystal_size_min 0.120 _refine_diff_density_max 0.876 _refine_diff_density_min -1.035 _refine_diff_density_rms 0.129 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 94 _refine_ls_number_reflns 1743 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.076 _refine_ls_R_factor_all 0.0438 _refine_ls_R_factor_gt 0.0414 _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^)+(0.0745P)^2^+0.9007P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1227 _refine_ls_wR_factor_ref 0.1248 _reflns_Friedel_coverage 0.000 _reflns_number_gt 1587 _reflns_number_total 1743 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9dt00945k2.cif _cod_data_source_block 413K _cod_depositor_comments 'Adding full bibliography for 7049642--7049648.cif.' _cod_database_code 7049648 _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_res_file ; 413K.res created by SHELXL-2014/7 TITL 413K in P2(1)/c New: P21/c CELL 0.71073 10.0482 14.6113 6.8335 90.000 95.511 90.000 ZERR 4 0.0005 0.0007 0.0003 0.000 0.004 0.000 LATT 1 SYMM - X , 0.50000 + Y , 0.50000 - Z SFAC C H Cd Cl N O UNIT 16 48 4 12 4 4 OMIT 0.00 50.05 L.S. 50 ACTA BOND $H FMAP 2 PLAN 0 CONF TEMP 140 WGHT 0.074500 0.900700 FVAR 0.27876 CD1 3 0.234175 0.250330 0.588444 11.00000 0.06383 0.05605 = 0.02468 -0.00131 0.00370 -0.00139 CL1 4 0.253824 0.114374 0.343329 11.00000 0.09112 0.04603 = 0.03725 -0.00003 0.00500 0.00524 CL2 4 0.058159 0.317450 0.312199 11.00000 0.06388 0.07957 = 0.04101 0.00254 0.00433 0.02042 CL3 4 0.407726 0.328036 0.362379 11.00000 0.06103 0.06945 = 0.04298 -0.00020 0.00415 -0.01272 O1 6 0.682052 0.231937 0.475019 11.00000 0.10433 0.09071 = 0.09188 -0.02918 -0.01363 0.02777 AFIX 147 H1 2 0.608029 0.254674 0.447321 11.00000 -1.50000 AFIX 0 N1 5 0.770070 0.103993 0.202965 11.00000 0.07780 0.04552 = 0.04940 -0.00019 0.00864 -0.00196 AFIX 13 H1D 2 0.767060 0.169528 0.172337 11.00000 -1.20000 AFIX 0 C1 1 0.901611 0.084076 0.308177 11.00000 0.07294 0.11775 = 0.10765 -0.02458 -0.00973 -0.00122 AFIX 137 H1A 2 0.917396 0.124772 0.418251 11.00000 -1.50000 H1B 2 0.969947 0.092515 0.220841 11.00000 -1.50000 H1C 2 0.903291 0.021950 0.354067 11.00000 -1.50000 AFIX 0 C2 1 0.754907 0.052904 0.013425 11.00000 0.13660 0.09070 = 0.05553 -0.00996 0.01221 0.00596 AFIX 137 H2A 2 0.761124 -0.011622 0.039163 11.00000 -1.50000 H2B 2 0.824444 0.070851 -0.065664 11.00000 -1.50000 H2C 2 0.669384 0.066565 -0.055343 11.00000 -1.50000 AFIX 0 C3 1 0.658009 0.083464 0.320285 11.00000 0.08420 0.06574 = 0.06939 0.00224 0.01199 0.00141 AFIX 23 H3A 2 0.657859 0.018593 0.350423 11.00000 -1.20000 H3B 2 0.574281 0.097953 0.243873 11.00000 -1.20000 AFIX 0 C4 1 0.668234 0.137220 0.508259 11.00000 0.11473 0.09922 = 0.05871 0.00721 0.02726 0.02454 AFIX 23 H4A 2 0.588725 0.126733 0.575158 11.00000 -1.20000 H4B 2 0.744704 0.115757 0.593329 11.00000 -1.20000 AFIX 0 HKLF 4 REM 413K in P2(1)/c New: P21/c REM R1 = 0.0414 for 1587 Fo > 4sig(Fo) and 0.0438 for all 1743 data REM 94 parameters refined using 0 restraints END WGHT 0.0745 0.9007 REM Highest difference peak 0.876, deepest hole -1.035, 1-sigma level 0.129 Q1 1 0.1538 0.2484 0.6383 11.00000 0.05 0.88 Q2 1 0.3091 0.2493 0.5240 11.00000 0.05 0.72 Q3 1 0.1642 0.1207 0.3584 11.00000 0.05 0.56 Q4 1 0.2299 0.0830 0.2516 11.00000 0.05 0.43 Q5 1 0.2366 0.3641 0.5892 11.00000 0.05 0.41 Q6 1 0.1844 0.2981 0.4925 11.00000 0.05 0.40 Q7 1 0.1952 0.2037 0.4956 11.00000 0.05 0.40 Q8 1 0.1349 0.3205 0.2453 11.00000 0.05 0.37 Q9 1 0.0471 0.4356 0.3164 11.00000 0.05 0.37 Q10 1 0.4240 0.4250 0.3407 11.00000 0.05 0.36 Q11 1 0.2221 0.1757 0.3137 11.00000 0.05 0.36 Q12 1 0.2620 0.1787 0.3899 11.00000 0.05 0.35 Q13 1 0.8172 0.0999 0.4434 11.00000 0.05 0.35 Q14 1 0.3195 0.1218 0.3027 11.00000 0.05 0.35 Q15 1 0.7647 -0.0306 0.4308 11.00000 0.05 0.35 Q16 1 0.2365 0.1360 0.5872 11.00000 0.05 0.35 Q17 1 0.4823 0.3382 0.2933 11.00000 0.05 0.34 Q18 1 0.5827 0.0359 0.2731 11.00000 0.05 0.34 Q19 1 0.3350 0.3206 0.4334 11.00000 0.05 0.34 Q20 1 0.9789 0.0806 -0.0502 11.00000 0.05 0.33 ; _shelx_res_checksum 70019 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp Cd1 Cd 0.23418(4) 0.25033(2) 0.58844(5) 0.0482(2) Uani 1 1 d . . Cl1 Cl 0.25382(13) 0.11437(8) 0.34333(15) 0.0582(3) Uani 1 1 d . . Cl2 Cl 0.05816(12) 0.31745(9) 0.31220(16) 0.0615(4) Uani 1 1 d . . Cl3 Cl 0.40773(12) 0.32804(9) 0.36238(16) 0.0579(3) Uani 1 1 d . . O1 O 0.6821(6) 0.2319(4) 0.4750(9) 0.0971(17) Uani 1 1 d . . H1 H 0.6080 0.2547 0.4473 0.146 Uiso 1 1 calc R U N1 N 0.7701(4) 0.1040(3) 0.2030(6) 0.0574(10) Uani 1 1 d . . H1D H 0.7671 0.1695 0.1723 0.069 Uiso 1 1 calc R U C1 C 0.9016(7) 0.0841(6) 0.3082(11) 0.101(2) Uani 1 1 d . . H1A H 0.9174 0.1248 0.4183 0.151 Uiso 1 1 calc R U H1B H 0.9699 0.0925 0.2208 0.151 Uiso 1 1 calc R U H1C H 0.9033 0.0220 0.3541 0.151 Uiso 1 1 calc R U C2 C 0.7549(8) 0.0529(5) 0.0134(9) 0.094(2) Uani 1 1 d . . H2A H 0.7611 -0.0116 0.0392 0.141 Uiso 1 1 calc R U H2B H 0.8244 0.0709 -0.0657 0.141 Uiso 1 1 calc R U H2C H 0.6694 0.0666 -0.0553 0.141 Uiso 1 1 calc R U C3 C 0.6580(6) 0.0835(4) 0.3203(9) 0.0728(14) Uani 1 1 d . . H3A H 0.6579 0.0186 0.3504 0.087 Uiso 1 1 calc R U H3B H 0.5743 0.0980 0.2439 0.087 Uiso 1 1 calc R U C4 C 0.6682(8) 0.1372(5) 0.5083(9) 0.090(2) Uani 1 1 d . . H4A H 0.5887 0.1267 0.5752 0.108 Uiso 1 1 calc R U H4B H 0.7447 0.1158 0.5933 0.108 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 Cd1 0.0638(3) 0.0560(3) 0.0247(3) -0.00131(10) 0.0037(2) -0.00139(12) Cl1 0.0911(9) 0.0460(6) 0.0372(6) 0.0000(4) 0.0050(5) 0.0052(5) Cl2 0.0639(7) 0.0796(8) 0.0410(6) 0.0025(5) 0.0043(5) 0.0204(6) Cl3 0.0610(7) 0.0695(8) 0.0430(6) -0.0002(5) 0.0041(5) -0.0127(5) O1 0.104(4) 0.091(3) 0.092(4) -0.029(3) -0.014(3) 0.028(3) N1 0.078(3) 0.046(2) 0.049(2) -0.0002(17) 0.0086(19) -0.0020(17) C1 0.073(4) 0.118(6) 0.108(5) -0.025(5) -0.010(4) -0.001(4) C2 0.137(6) 0.091(5) 0.056(3) -0.010(3) 0.012(4) 0.006(4) C3 0.084(4) 0.066(3) 0.069(3) 0.002(3) 0.012(3) 0.001(3) C4 0.115(5) 0.099(5) 0.059(3) 0.007(3) 0.027(3) 0.025(4) 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' Cd Cd -0.8075 1.2024 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 Cl1 Cd1 Cl1 171.39(6) . 4_566 Cl1 Cd1 Cl2 100.48(4) . 4_566 Cl1 Cd1 Cl2 84.85(4) 4_566 4_566 Cl1 Cd1 Cl2 84.90(4) . . Cl1 Cd1 Cl2 101.32(4) 4_566 . Cl2 Cd1 Cl2 96.49(5) 4_566 . Cl1 Cd1 Cl3 92.21(4) . 4_566 Cl1 Cd1 Cl3 81.75(4) 4_566 4_566 Cl2 Cd1 Cl3 82.11(4) 4_566 4_566 Cl2 Cd1 Cl3 176.53(4) . 4_566 Cl1 Cd1 Cl3 81.95(4) . . Cl1 Cd1 Cl3 92.95(4) 4_566 . Cl2 Cd1 Cl3 177.01(4) 4_566 . Cl2 Cd1 Cl3 81.94(4) . . Cl3 Cd1 Cl3 99.60(5) 4_566 . Cl1 Cd1 Cd1 130.16(3) . 4_566 Cl1 Cd1 Cd1 49.23(2) 4_566 4_566 Cl2 Cd1 Cd1 49.86(3) 4_566 4_566 Cl2 Cd1 Cd1 130.52(3) . 4_566 Cl3 Cd1 Cd1 50.57(2) 4_566 4_566 Cl3 Cd1 Cd1 129.63(2) . 4_566 Cl1 Cd1 Cd1 49.52(2) . 4_565 Cl1 Cd1 Cd1 131.09(3) 4_566 4_565 Cl2 Cd1 Cd1 129.99(3) 4_566 4_565 Cl2 Cd1 Cd1 49.63(3) . 4_565 Cl3 Cd1 Cd1 129.25(3) 4_566 4_565 Cl3 Cd1 Cd1 50.55(2) . 4_565 Cd1 Cd1 Cd1 179.678(18) 4_566 4_565 Cd1 Cl1 Cd1 81.25(3) . 4_565 Cd1 Cl2 Cd1 80.51(3) 4_565 . Cd1 Cl3 Cd1 78.88(3) 4_565 . C4 O1 H1 109.5 . . C1 N1 C3 113.0(5) . . C1 N1 C2 109.7(5) . . C3 N1 C2 110.6(5) . . C1 N1 H1D 107.8 . . C3 N1 H1D 107.8 . . C2 N1 H1D 107.8 . . N1 C1 H1A 109.5 . . N1 C1 H1B 109.5 . . H1A C1 H1B 109.5 . . N1 C1 H1C 109.5 . . H1A C1 H1C 109.5 . . H1B C1 H1C 109.5 . . N1 C2 H2A 109.5 . . N1 C2 H2B 109.5 . . H2A C2 H2B 109.5 . . N1 C2 H2C 109.5 . . H2A C2 H2C 109.5 . . H2B C2 H2C 109.5 . . N1 C3 C4 111.5(5) . . N1 C3 H3A 109.3 . . C4 C3 H3A 109.3 . . N1 C3 H3B 109.3 . . C4 C3 H3B 109.3 . . H3A C3 H3B 108.0 . . O1 C4 C3 112.0(5) . . O1 C4 H4A 109.2 . . C3 C4 H4A 109.2 . . O1 C4 H4B 109.2 . . C3 C4 H4B 109.2 . . H4A C4 H4B 107.9 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Cd1 Cl1 2.6181(11) . Cd1 Cl1 2.6296(11) 4_566 Cd1 Cl2 2.6394(12) 4_566 Cd1 Cl2 2.6480(12) . Cd1 Cl3 2.6887(11) 4_566 Cd1 Cl3 2.6896(11) . Cd1 Cd1 3.41674(15) 4_566 Cd1 Cd1 3.41679(15) 4_565 Cl1 Cd1 2.6296(11) 4_565 Cl2 Cd1 2.6394(12) 4_565 Cl3 Cd1 2.6887(11) 4_565 O1 C4 1.411(8) . O1 H1 0.8200 . N1 C1 1.472(8) . N1 C3 1.474(7) . N1 C2 1.490(7) . N1 H1D 0.9800 . C1 H1A 0.9600 . C1 H1B 0.9600 . C1 H1C 0.9600 . C2 H2A 0.9600 . C2 H2B 0.9600 . C2 H2C 0.9600 . C3 C4 1.501(9) . C3 H3A 0.9700 . C3 H3B 0.9700 . C4 H4A 0.9700 . C4 H4B 0.9700 . 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 C1 N1 C3 C4 58.9(7) C2 N1 C3 C4 -177.6(5) N1 C3 C4 O1 53.2(7)