#------------------------------------------------------------------------------ #$Date: 2018-09-26 06:29:44 +0300 (Wed, 26 Sep 2018) $ #$Revision: 211175 $ #$URL: file:///home/coder/svn-repositories/cod/cif/8/00/02/8000278.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_8000278 loop_ _publ_author_name 'Gui, Di' 'Ji, Lijun' 'Muhammad, Azeem' 'Li, Wei' 'Cai, Weizhao' 'Li, Yanchun' 'Li, Xiaodong' 'Wu, Xiang' 'Lu, Peixiang' _publ_section_title ; Jahn-Teller Effect on Framework Flexibility of Hybrid Organic-Inorganic Perovskites. ; _journal_name_full 'The journal of physical chemistry letters' _journal_page_first 751 _journal_page_last 755 _journal_paper_doi 10.1021/acs.jpclett.7b03229 _journal_year 2018 _chemical_formula_moiety '0.25(C12 H12 O24 Zn4), C H6 N3' _chemical_formula_sum 'C4 H9 N3 O6 Zn' _chemical_formula_weight 260.51 _space_group_crystal_system orthorhombic _space_group_IT_number 52 _space_group_name_Hall '-P 2a 2bc' _space_group_name_H-M_alt 'P n n a' _symmetry_space_group_name_Hall '-P 2a 2bc' _symmetry_space_group_name_H-M 'P n n a' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_date 2017-05-13 _audit_creation_method ; Olex2 1.2 (compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337) ; _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 8.3400(3) _cell_length_b 11.7244(5) _cell_length_c 8.9461(4) _cell_measurement_reflns_used 12435 _cell_measurement_temperature 240.02(10) _cell_measurement_theta_max 30.2600 _cell_measurement_theta_min 3.7530 _cell_volume 874.76(6) _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 240.02(10) _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.960 _diffrn_measurement_device_type 'XtaLAB Pro: Kappa single' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0206 _diffrn_reflns_av_unetI/netI 0.0070 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 21831 _diffrn_reflns_theta_full 30.24 _diffrn_reflns_theta_max 30.24 _diffrn_reflns_theta_min 3.77 _diffrn_source 'fine-focus sealed tube' _exptl_absorpt_coefficient_mu 2.819 _exptl_crystal_density_diffrn 1.978 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 528 _refine_diff_density_max 0.277 _refine_diff_density_min -0.271 _refine_diff_density_rms 0.065 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.130 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 66 _refine_ls_number_reflns 1260 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.130 _refine_ls_R_factor_all 0.0178 _refine_ls_R_factor_gt 0.0170 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0257P)^2^+0.3509P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0499 _refine_ls_wR_factor_ref 0.0503 _reflns_number_gt 1209 _reflns_number_total 1260 _reflns_threshold_expression >2sigma(I) _cod_data_source_file Zn-240K.cif _cod_data_source_block Zn_240_00-multiscan _cod_database_code 8000278 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All N(H,H) groups 2. Others Fixed Sof: H2A(0.5) H2B(0.5) 3.a Aromatic/amide H refined with riding coordinates: C2(H2), C1(H1) 3.b X=CH2 refined with riding coordinates: N1(H1A,H1B), N2(H2A,H2B) ; _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x+1/2, -y, z' 3 '-x+1/2, y+1/2, -z+1/2' 4 'x, -y+1/2, -z+1/2' 5 '-x, -y, -z' 6 'x-1/2, y, -z' 7 'x-1/2, -y-1/2, z-1/2' 8 '-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_calc_flag _atom_site_site_symmetry_order _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy Zn1 Zn 0.257234(17) 0.7500 0.2500 0.00990(7) Uani 1 d 2 S T P O2 O 0.40796(10) 0.81898(6) 0.41338(9) 0.01971(16) Uani 1 d 1 . . . O1 O 0.56435(9) 0.80778(6) 0.61324(8) 0.01710(15) Uani 1 d 1 . . . O3 O 0.25869(9) 0.59468(6) 0.36571(9) 0.01682(16) Uani 1 d 1 . . . N1 N 0.34174(13) 0.57327(9) 0.68274(10) 0.0266(2) Uani 1 d 1 . . . H1A H 0.4012 0.6207 0.7307 0.032 Uiso 1 calc 1 R . . H1B H 0.3417 0.5732 0.5866 0.032 Uiso 1 calc 1 R . . C2 C 0.52481(12) 0.77868(9) 0.48371(11) 0.01596(18) Uani 1 d 1 . . . H2 H 0.5865 0.7233 0.4364 0.019 Uiso 1 calc 1 R . . C1 C 0.2500 0.5000 0.30196(17) 0.0190(3) Uani 1 d 2 S T P H1 H 0.2500 0.5000 0.1980 0.023 Uiso 1 calc 2 RS T P N2 N 0.2500 0.5000 0.90505(16) 0.0225(3) Uani 1 d 2 S T P H2A H 0.1906 0.4526 0.9531 0.027 Uiso 0.50 calc 1 R . . H2B H 0.3094 0.5474 0.9531 0.027 Uiso 0.50 calc 1 R . . C3 C 0.2500 0.5000 0.75712(16) 0.0173(4) Uani 1 d 2 S T P 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 Zn1 0.01150(10) 0.00961(11) 0.00859(11) 0.00001(5) 0.000 0.000 O2 0.0206(4) 0.0183(3) 0.0201(4) -0.0038(3) -0.0097(3) 0.0027(3) O1 0.0166(3) 0.0214(3) 0.0133(3) -0.0009(3) -0.0037(3) 0.0038(3) O3 0.0278(4) 0.0106(3) 0.0120(3) 0.0002(3) -0.0009(3) 0.0005(2) N1 0.0317(5) 0.0330(5) 0.0151(4) 0.0038(4) -0.0034(4) -0.0172(4) C2 0.0166(4) 0.0164(4) 0.0149(4) -0.0010(3) -0.0016(3) 0.0030(4) C1 0.0340(9) 0.0137(7) 0.0093(7) 0.000 0.000 0.0002(5) N2 0.0328(8) 0.0225(7) 0.0121(6) 0.000 0.000 -0.0084(5) C3 0.0180(8) 0.0184(9) 0.0156(8) 0.000 0.000 -0.0010(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' 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' Zn Zn 0.2839 1.4301 '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 O2 Zn1 O2 106.08(5) . 4_565 O2 Zn1 O1 85.96(3) . 6_556 O2 Zn1 O1 167.96(3) 4_565 6_556 O2 Zn1 O1 167.96(3) . 7_575 O2 Zn1 O1 85.96(3) 4_565 7_575 O2 Zn1 O3 90.33(3) . 4_565 O2 Zn1 O3 89.27(3) . . O2 Zn1 O3 90.33(3) 4_565 . O2 Zn1 O3 89.27(3) 4_565 4_565 O1 Zn1 O1 82.00(4) 7_575 6_556 O3 Zn1 O1 89.83(3) . 6_556 O3 Zn1 O1 90.67(3) . 7_575 O3 Zn1 O1 89.83(3) 4_565 7_575 O3 Zn1 O1 90.67(3) 4_565 6_556 O3 Zn1 O3 179.33(4) 4_565 . C2 O2 Zn1 132.31(7) . . C2 O1 Zn1 130.04(7) . 6_656 C1 O3 Zn1 123.11(8) . . H1A N1 H1B 120.0 . . C3 N1 H1A 120.0 . . C3 N1 H1B 120.0 . . O2 C2 H2 117.7 . . O1 C2 O2 124.54(10) . . O1 C2 H2 117.7 . . O3 C1 O3 125.72(14) . 2_565 O3 C1 H1 117.1 . . O3 C1 H1 117.1 2_565 . H2A N2 H2B 120.0 . . C3 N2 H2A 120.0 . . C3 N2 H2B 120.0 . . N1 C3 N1 119.90(14) 2_565 . N2 C3 N1 120.05(7) . 2_565 N2 C3 N1 120.05(7) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Zn1 O2 2.0906(7) . Zn1 O2 2.0906(7) 4_565 Zn1 O1 2.1316(7) 6_556 Zn1 O1 2.1316(7) 7_575 Zn1 O3 2.0947(8) 4_565 Zn1 O3 2.0947(8) . O2 C2 1.2525(12) . O1 Zn1 2.1316(7) 6_656 O1 C2 1.2522(12) . O3 C1 1.2501(10) . N1 H1A 0.8600 . N1 H1B 0.8600 . N1 C3 1.3289(12) . C2 H2 0.9300 . C1 O3 1.2501(10) 2_565 C1 H1 0.9300 . N2 H2A 0.8600 . N2 H2B 0.8600 . N2 C3 1.323(2) . C3 N1 1.3289(12) 2_565