#------------------------------------------------------------------------------ #$Date: 2024-09-29 03:59:32 +0300 (Sun, 29 Sep 2024) $ #$Revision: 294939 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/94/7249406.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_7249406 loop_ _publ_author_name 'Gishan, Md' 'Middya, Puspendu' 'Drew, Michael G. B.' 'Frontera, Antonio' 'Chattopadhyay, Shouvik' _publ_section_title ; Synthesis, structural characterization, and theoretical analysis of novel zinc(ii) schiff base complexes with halogen and hydrogen bonding interactions ; _journal_issue 42 _journal_name_full 'RSC Advances' _journal_page_first 30896 _journal_page_last 30911 _journal_paper_doi 10.1039/D4RA06217E _journal_volume 14 _journal_year 2024 _chemical_formula_sum 'C20 H20 Br4 N2 O4 Zn' _chemical_formula_weight 737.37 _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-C 2yc' _space_group_name_H-M_alt 'C 1 2/c 1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2024-04-05 deposited with the CCDC. 2024-09-09 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 110.3680(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 21.5606(9) _cell_length_b 4.5954(2) _cell_length_c 25.0465(10) _cell_measurement_reflns_used 900 _cell_measurement_temperature 273(2) _cell_measurement_theta_max 34.054 _cell_measurement_theta_min 3.084 _cell_volume 2326.44(17) _computing_cell_refinement 'SAINT (Bruker, 2000)' _computing_data_collection 'SMART (Bruker, 2000)' _computing_data_reduction SAINT _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1999) and CAMERON (Watkin et al., 1993)' _computing_publication_material 'PLATON (Spek, 2003)' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 273(2) _diffrn_measured_fraction_theta_full 0.983 _diffrn_measured_fraction_theta_max 0.930 _diffrn_measurement_device_type 'BRUKER D8 QUEST AREA DETECTOR' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0595 _diffrn_reflns_av_unetI/netI 0.0315 _diffrn_reflns_Laue_measured_fraction_full 0.983 _diffrn_reflns_Laue_measured_fraction_max 0.930 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_number 48908 _diffrn_reflns_point_group_measured_fraction_full 0.983 _diffrn_reflns_point_group_measured_fraction_max 0.930 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 34.054 _diffrn_reflns_theta_min 3.084 _exptl_absorpt_coefficient_mu 7.956 _exptl_absorpt_correction_T_max 0.204 _exptl_absorpt_correction_T_min 0.071 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_crystal_colour YELLOW _exptl_crystal_density_diffrn 2.105 _exptl_crystal_description BLOCK _exptl_crystal_F_000 1424.0 _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _refine_diff_density_max 1.149 _refine_diff_density_min -1.284 _refine_diff_density_rms 0.375 _refine_ls_extinction_coef 0.0181(9) _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 1.201 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 148 _refine_ls_number_reflns 4432 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.201 _refine_ls_R_factor_all 0.0619 _refine_ls_R_factor_gt 0.0449 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0667P)^2^+3.4496P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1099 _refine_ls_wR_factor_ref 0.1341 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3638 _reflns_number_total 4764 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4ra06217e2.cif _cod_data_source_block shelx _cod_depositor_comments ; The following automatic conversions were performed: data item '_exptl_absorpt_correction_type' value 'MULTI-SCAN' was changed to 'multi-scan' 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_sg_symbol_H-M 'C 2/c' _cod_database_code 7249406 _shelx_shelxl_version_number 2018/3 _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 ; TITL SC_MG_66_0m_a.res in C2/c shelx.res created by SHELXL-2018/3 at 15:47:22 on 09-Oct-2023 CELL 0.71073 21.5606 4.5954 25.0465 90.000 110.368 90.000 ZERR 4.00 0.0009 0.0002 0.0010 0.000 0.001 0.000 LATT 7 SYMM - X, Y, 1/2 - Z SFAC C H N O ZN BR UNIT 88 0 8 24 4 16 MERG 2 FMAP 2 PLAN 20 ACTA BOND $H L.S. 70 TEMP 0.00 WGHT 0.066700 3.449600 EXTI 0.018131 FVAR 0.33088 0.55947 PART 1 O2 4 0.293763 0.021964 0.557758 21.00000 0.08199 0.06688 = 0.03068 0.00169 0.00114 -0.01059 AFIX 83 H2 2 0.282961 0.061178 0.523796 21.00000 -1.50000 AFIX 0 PART 2 O2A 4 0.253347 0.433639 0.562930 -21.00000 0.04085 AFIX 147 H2A 2 0.258876 0.595922 0.577448 -21.00000 -1.50000 PART 0 AFIX 0 BR1 6 0.679606 0.909362 0.712516 11.00000 0.03560 0.04777 = 0.03819 -0.00778 0.01389 -0.00997 ZN1 5 0.500000 0.391799 0.750000 10.50000 0.02794 0.04333 = 0.01800 0.00000 0.00961 0.00000 BR2 6 0.613233 0.307961 0.504816 11.00000 0.07713 0.09049 = 0.04035 -0.01761 0.04168 -0.01619 O1 4 0.559059 0.591570 0.719328 11.00000 0.03743 0.04482 = 0.02535 -0.00880 0.01744 -0.00869 N1 3 0.450356 0.180558 0.677376 11.00000 0.02631 0.03737 = 0.02188 0.00201 0.00749 -0.00230 C7 1 0.472201 0.173882 0.635811 11.00000 0.03272 0.03991 = 0.02293 -0.00334 0.00956 -0.00468 AFIX 43 H7 2 0.449515 0.053223 0.605489 11.00000 -1.20000 AFIX 0 C1 1 0.567986 0.528330 0.671942 11.00000 0.02651 0.03241 = 0.02170 0.00006 0.01055 0.00106 C2 1 0.621063 0.655921 0.659038 11.00000 0.02769 0.03427 = 0.02550 0.00066 0.01139 0.00006 C3 1 0.633700 0.597297 0.609809 11.00000 0.03323 0.04498 = 0.03040 0.00358 0.01820 -0.00001 AFIX 43 H3 2 0.668754 0.687584 0.602873 11.00000 -1.20000 AFIX 0 C8 1 0.391044 0.005943 0.671475 11.00000 0.02921 0.04330 = 0.02781 0.00639 0.00862 -0.00470 AFIX 23 H8A 2 0.395485 -0.079731 0.708018 11.00000 -1.20000 H8B 2 0.387655 -0.151264 0.644760 11.00000 -1.20000 AFIX 0 C5 1 0.541225 0.269805 0.580329 11.00000 0.04255 0.05020 = 0.02549 -0.00886 0.01678 -0.00824 AFIX 43 H5 2 0.514612 0.139515 0.553755 11.00000 -1.20000 AFIX 0 C10 1 0.308177 0.267636 0.588309 11.00000 0.04034 0.05797 = 0.03797 0.01490 0.00206 0.00008 AFIX 23 H10A 2 0.269946 0.395195 0.577347 11.00000 -1.20000 H10B 2 0.344219 0.368452 0.581453 11.00000 -1.20000 AFIX 0 C6 1 0.527879 0.331433 0.630415 11.00000 0.03236 0.03877 = 0.02199 -0.00231 0.01275 -0.00362 C4 1 0.593506 0.402118 0.570784 11.00000 0.04253 0.04962 = 0.02638 -0.00294 0.02100 -0.00004 C9 1 0.327868 0.188899 0.650603 11.00000 0.03051 0.05096 = 0.03350 0.00522 0.01084 -0.00193 AFIX 23 H9A 2 0.292122 0.081140 0.656531 11.00000 -1.20000 H9B 2 0.334585 0.365979 0.672984 11.00000 -1.20000 AFIX 0 HKLF 4 1.0 1.00 0.00 0.00 0.00 1.00 0.00 0.00 0.00 1.00 REM SC_MG_66_0m_a.res in C2/c REM wR2 = 0.1341, GooF = S = 1.201, Restrained GooF = 1.201 for all data REM R1 = 0.0449 for 3638 Fo > 4sig(Fo) and 0.0619 for all 4432 data REM 148 parameters refined using 0 restraints END WGHT 0.0668 3.4277 REM Highest difference peak 1.149, deepest hole -1.284, 1-sigma level 0.375 Q1 1 0.6185 0.4392 0.5113 11.00000 0.05 0.90 Q2 1 0.3620 -0.1021 0.6088 11.00000 0.05 0.90 Q3 1 0.4019 0.4755 0.6441 11.00000 0.05 0.85 Q4 1 0.3586 -0.0818 0.6729 11.00000 0.05 0.84 Q5 1 0.4068 -0.3208 0.6438 11.00000 0.05 0.83 Q6 1 0.5100 0.2091 0.6327 11.00000 0.05 0.83 Q7 1 0.2979 0.6839 0.6356 11.00000 0.05 0.82 Q8 1 0.3090 0.5466 0.6403 11.00000 0.05 0.80 Q9 1 0.3899 -0.0130 0.6239 11.00000 0.05 0.79 Q10 1 0.3600 -0.2829 0.6133 11.00000 0.05 0.79 Q11 1 0.3235 0.2358 0.6192 11.00000 0.05 0.78 Q12 1 0.6276 0.6245 0.6393 11.00000 0.05 0.77 Q13 1 0.3247 -0.2036 0.6188 11.00000 0.05 0.76 Q14 1 0.2821 -0.0187 0.6382 11.00000 0.05 0.76 Q15 1 0.3962 0.4300 0.6185 11.00000 0.05 0.74 Q16 1 0.3916 0.3233 0.6299 11.00000 0.05 0.74 Q17 1 0.4770 0.0224 0.6101 11.00000 0.05 0.74 Q18 1 0.4202 -0.1087 0.6198 11.00000 0.05 0.74 Q19 1 0.4305 0.3946 0.6503 11.00000 0.05 0.73 Q20 1 0.3727 -0.4368 0.6261 11.00000 0.05 0.73 ; _shelx_res_checksum 15458 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -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 _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group O2 O 0.2938(3) 0.0220(13) 0.5578(2) 0.0647(18) Uani 0.559(8) 1 d . . P A 1 H2 H 0.282961 0.061178 0.523796 0.097 Uiso 0.559(8) 1 calc R U P A 1 O2A O 0.2533(3) 0.4336(11) 0.5629(2) 0.0409(14) Uiso 0.441(8) 1 d . . P A 2 H2A H 0.258876 0.595922 0.577448 0.061 Uiso 0.441(8) 1 calc R U P A 2 Br1 Br 0.67961(2) 0.90936(7) 0.71252(2) 0.04024(13) Uani 1 1 d . . . . . Zn1 Zn 0.500000 0.39180(10) 0.750000 0.02933(13) Uani 1 2 d S T P . . Br2 Br 0.61323(2) 0.30796(12) 0.50482(2) 0.06372(17) Uani 1 1 d . . . . . O1 O 0.55906(10) 0.5916(5) 0.71933(8) 0.0342(4) Uani 1 1 d . . . . . N1 N 0.45036(10) 0.1806(5) 0.67738(9) 0.0288(4) Uani 1 1 d . . . . . C7 C 0.47220(13) 0.1739(6) 0.63581(11) 0.0319(5) Uani 1 1 d . . . . . H7 H 0.449515 0.053223 0.605489 0.038 Uiso 1 1 calc R U . . . C1 C 0.56799(12) 0.5283(6) 0.67194(10) 0.0263(4) Uani 1 1 d . . . . . C2 C 0.62106(13) 0.6559(6) 0.65904(11) 0.0286(4) Uani 1 1 d . . . . . C3 C 0.63370(14) 0.5973(6) 0.60981(12) 0.0343(5) Uani 1 1 d . . . . . H3 H 0.668754 0.687584 0.602873 0.041 Uiso 1 1 calc R U . . . C8 C 0.39104(13) 0.0059(7) 0.67147(11) 0.0338(5) Uani 1 1 d . . . . . H8A H 0.395485 -0.079731 0.708018 0.041 Uiso 1 1 calc R U . . . H8B H 0.387655 -0.151264 0.644760 0.041 Uiso 1 1 calc R U . . . C5 C 0.54123(16) 0.2698(7) 0.58033(12) 0.0381(6) Uani 1 1 d . . . . . H5 H 0.514612 0.139515 0.553755 0.046 Uiso 1 1 calc R U . . . C10 C 0.30818(17) 0.2676(9) 0.58831(15) 0.0485(8) Uani 1 1 d . . . . . H10A H 0.269946 0.395195 0.577347 0.058 Uiso 1 1 calc R U . A 1 H10B H 0.344219 0.368452 0.581453 0.058 Uiso 1 1 calc R U . A 1 C6 C 0.52788(13) 0.3314(6) 0.63041(10) 0.0302(5) Uani 1 1 d . . . . . C4 C 0.59351(16) 0.4021(7) 0.57078(12) 0.0371(6) Uani 1 1 d . . . . . C9 C 0.32787(14) 0.1889(8) 0.65060(13) 0.0384(6) Uani 1 1 d . . . . . H9A H 0.292122 0.081140 0.656531 0.046 Uiso 1 1 calc R U . . . H9B H 0.334585 0.365979 0.672984 0.046 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 O2 0.082(4) 0.067(3) 0.031(2) 0.002(2) 0.001(2) -0.011(3) Br1 0.03560(18) 0.0478(2) 0.03819(18) -0.00778(11) 0.01389(12) -0.00997(11) Zn1 0.0279(2) 0.0433(3) 0.01800(18) 0.000 0.00961(14) 0.000 Br2 0.0771(3) 0.0905(3) 0.0404(2) -0.01761(18) 0.04168(19) -0.0162(2) O1 0.0374(10) 0.0448(11) 0.0254(8) -0.0088(7) 0.0174(7) -0.0087(8) N1 0.0263(9) 0.0374(10) 0.0219(8) 0.0020(8) 0.0075(7) -0.0023(8) C7 0.0327(11) 0.0399(12) 0.0229(10) -0.0033(9) 0.0096(9) -0.0047(10) C1 0.0265(10) 0.0324(11) 0.0217(9) 0.0001(8) 0.0106(8) 0.0011(9) C2 0.0277(10) 0.0343(11) 0.0255(10) 0.0007(9) 0.0114(8) 0.0001(9) C3 0.0332(12) 0.0450(14) 0.0304(11) 0.0036(10) 0.0182(10) 0.0000(10) C8 0.0292(11) 0.0433(14) 0.0278(11) 0.0064(10) 0.0086(9) -0.0047(10) C5 0.0426(14) 0.0502(16) 0.0255(11) -0.0089(11) 0.0168(10) -0.0082(12) C10 0.0403(15) 0.0580(19) 0.0380(15) 0.0149(14) 0.0021(12) 0.0001(14) C6 0.0324(11) 0.0388(12) 0.0220(9) -0.0023(9) 0.0128(8) -0.0036(10) C4 0.0425(14) 0.0496(16) 0.0264(11) -0.0029(10) 0.0210(11) 0.0000(12) C9 0.0305(12) 0.0510(16) 0.0335(12) 0.0052(12) 0.0108(10) -0.0019(11) 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' Br Br -0.2901 2.4595 '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 _geom_angle_publ_flag C10 O2 H2 109.5 . . ? C10 O2A H2A 109.5 . . ? O1 Zn1 O1 123.28(13) . 2_656 ? O1 Zn1 N1 111.84(9) . 2_656 ? O1 Zn1 N1 94.97(8) 2_656 2_656 ? O1 Zn1 N1 94.97(8) . . ? O1 Zn1 N1 111.84(9) 2_656 . ? N1 Zn1 N1 122.25(14) 2_656 . ? C1 O1 Zn1 125.75(17) . . ? C7 N1 C8 117.2(2) . . ? C7 N1 Zn1 121.01(18) . . ? C8 N1 Zn1 121.61(17) . . ? N1 C7 C6 127.9(2) . . ? N1 C7 H7 116.1 . . ? C6 C7 H7 116.1 . . ? O1 C1 C2 120.2(2) . . ? O1 C1 C6 124.4(2) . . ? C2 C1 C6 115.4(2) . . ? C3 C2 C1 123.3(2) . . ? C3 C2 Br1 117.6(2) . . ? C1 C2 Br1 119.08(18) . . ? C2 C3 C4 119.2(3) . . ? C2 C3 H3 120.4 . . ? C4 C3 H3 120.4 . . ? N1 C8 C9 111.9(3) . . ? N1 C8 H8A 109.2 . . ? C9 C8 H8A 109.2 . . ? N1 C8 H8B 109.2 . . ? C9 C8 H8B 109.2 . . ? H8A C8 H8B 107.9 . . ? C4 C5 C6 120.0(3) . . ? C4 C5 H5 120.0 . . ? C6 C5 H5 120.0 . . ? O2 C10 C9 108.3(4) . . ? O2A C10 C9 120.1(4) . . ? O2 C10 H10A 110.0 . . ? C9 C10 H10A 110.0 . . ? O2 C10 H10B 110.0 . . ? C9 C10 H10B 110.0 . . ? H10A C10 H10B 108.4 . . ? C5 C6 C1 121.2(2) . . ? C5 C6 C7 114.5(2) . . ? C1 C6 C7 124.2(2) . . ? C5 C4 C3 120.9(2) . . ? C5 C4 Br2 119.9(2) . . ? C3 C4 Br2 119.2(2) . . ? C10 C9 C8 112.4(3) . . ? C10 C9 H9A 109.1 . . ? C8 C9 H9A 109.1 . . ? C10 C9 H9B 109.1 . . ? C8 C9 H9B 109.1 . . ? H9A C9 H9B 107.9 . . ? 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 O2 C10 1.338(7) . ? O2 H2 0.8200 . ? O2A C10 1.364(6) . ? O2A H2A 0.8200 . ? Br1 C2 1.889(3) . ? Zn1 O1 1.933(2) . ? Zn1 O1 1.933(2) 2_656 ? Zn1 N1 2.010(2) 2_656 ? Zn1 N1 2.010(2) . ? Br2 C4 1.894(3) . ? O1 C1 1.300(3) . ? N1 C7 1.284(3) . ? N1 C8 1.473(3) . ? C7 C6 1.448(4) . ? C7 H7 0.9300 . ? C1 C2 1.420(3) . ? C1 C6 1.422(4) . ? C2 C3 1.379(4) . ? C3 C4 1.386(4) . ? C3 H3 0.9300 . ? C8 C9 1.530(4) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C5 C4 1.373(4) . ? C5 C6 1.410(4) . ? C5 H5 0.9300 . ? C10 C9 1.511(4) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ?