#------------------------------------------------------------------------------ #$Date: 2025-07-01 13:56:09 +0300 (Tue, 01 Jul 2025) $ #$Revision: 1152 $ #$URL: svn://localhost/testcod/cif/7/70/00/7700031.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_7700031 loop_ _publ_author_name 'Vallejo, J.' 'Salcedo, I. R.' 'Colodrero, R. M. P.' 'Cabeza, A.' '\'Switlicka, A.' 'Cano, J.' 'Viciano-Chumillas, M.' _publ_section_title ; Zinc(ii), cobalt(ii) and manganese(ii) networks with phosphoserine ligand: synthesis, crystal structures and magnetic and proton conductivity properties ; _journal_issue 47 _journal_name_full 'Dalton Transactions' _journal_page_first 16570 _journal_page_last 16579 _journal_paper_doi 10.1039/C7DT03474A _journal_volume 46 _journal_year 2017 _chemical_absolute_configuration ad _chemical_formula_moiety 'C3 H6 N O6 P Zn' _chemical_formula_sum 'C3 H6 N O6 P Zn' _chemical_formula_weight 248.43 _space_group_crystal_system orthorhombic _space_group_IT_number 19 _space_group_name_Hall 'P 2ac 2ab' _space_group_name_H-M_alt 'P 21 21 21' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2014/6 _audit_update_record ; 2017-08-08 deposited with the CCDC. 2017-11-07 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 5.1818(6) _cell_length_b 7.6909(9) _cell_length_c 17.7166(15) _cell_measurement_reflns_used 1017 _cell_measurement_temperature 295(2) _cell_measurement_theta_max 27.6750 _cell_measurement_theta_min 4.3380 _cell_volume 706.05(13) _computing_cell_refinement 'CrysAlis RED v. 1.163 (UNIL IC & KUMA 2000)' _computing_data_collection 'CrysAlis CCD v. 1.163 (UNIL IC & KUMA 2000)' _computing_data_reduction 'CrysAlis RED v. 1.163 (UNIL IC & KUMA 2000)' _computing_structure_refinement 'SHELXL-2014/6 (Sheldrick, 2014)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 295(2) _diffrn_measured_fraction_theta_full 0.981 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device_type 'Oxford Diffraction Gemini A Ultra' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0421 _diffrn_reflns_av_unetI/netI 0.0631 _diffrn_reflns_Laue_measured_fraction_full 0.981 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 2462 _diffrn_reflns_point_group_measured_fraction_full 0.974 _diffrn_reflns_point_group_measured_fraction_max 0.994 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.094 _diffrn_reflns_theta_min 3.508 _exptl_absorpt_coefficient_mu 3.695 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.45337 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Blessing, Acta Cryst. A51 (1995) 33-38' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 2.337 _exptl_crystal_description needle _exptl_crystal_F_000 496 _exptl_crystal_size_max 0.22692 _exptl_crystal_size_mid 0.05909 _exptl_crystal_size_min 0.04843 _refine_diff_density_max 0.456 _refine_diff_density_min -0.453 _refine_diff_density_rms 0.106 _refine_ls_abs_structure_details ; Flack x determined using 403 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.032(19) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 110 _refine_ls_number_reflns 1248 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.055 _refine_ls_R_factor_all 0.0419 _refine_ls_R_factor_gt 0.0335 _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^)+(0.0224P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0635 _refine_ls_wR_factor_ref 0.0666 _reflns_Friedel_coverage 0.623 _reflns_Friedel_fraction_full 0.964 _reflns_Friedel_fraction_max 0.988 _reflns_number_gt 1132 _reflns_number_total 1248 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c7dt03474a2.cif _cod_data_source_block vv55a _cod_database_code 7700031 _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. ; _shelxl_version_number 2014/6 _shelx_res_file ; TITL CELL 0.71073 5.181756 7.690884 17.716605 90 90 90 ZERR 4 0.000613 0.000943 0.001519 0 0 0 LATT -1 SYMM 0.5-X,-Y,0.5+Z SYMM 0.5+X,0.5-Y,-Z SYMM -X,0.5+Y,0.5-Z SFAC C H N O P Zn UNIT 12 24 4 24 4 4 L.S. 10 PLAN 20 BOND $H fmap 2 53 acta OMIT 0 50.2 REM REM REM WGHT 0.022400 FVAR 4.93877 ZN1 6 -0.315867 1.019791 0.327678 11.00000 0.01480 0.01574 = 0.01157 -0.00106 0.00057 -0.00072 P1 5 0.185720 0.825897 0.275056 11.00000 0.01291 0.01044 = 0.00984 0.00073 0.00098 0.00126 O1 4 0.289679 0.508230 0.566449 11.00000 0.03342 0.04234 = 0.00878 -0.00004 0.00186 -0.00902 O2 4 -0.056257 0.385737 0.514779 11.00000 0.03087 0.04051 = 0.02013 -0.00213 0.00987 -0.01471 O3 4 0.260643 0.659960 0.325587 11.00000 0.03156 0.01393 = 0.01206 0.00309 0.00547 0.00618 O4 4 -0.101734 0.851188 0.277481 11.00000 0.01388 0.02511 = 0.01621 -0.00410 -0.00029 0.00127 O5 4 0.275815 0.769887 0.197001 11.00000 0.01629 0.01172 = 0.01121 0.00187 0.00222 0.00554 O6 4 0.327048 0.981548 0.306769 11.00000 0.01255 0.01507 = 0.02537 -0.00312 -0.00041 0.00050 N1 3 0.204464 0.330778 0.385347 11.00000 0.02820 0.02015 = 0.00766 0.00091 -0.00173 -0.00231 AFIX 137 H1A 2 0.277082 0.342612 0.340113 11.00000 -1.20000 H1B 2 0.033660 0.327140 0.380307 11.00000 -1.20000 H1C 2 0.259295 0.232690 0.406638 11.00000 -1.20000 AFIX 0 C1 1 0.158453 0.451239 0.512080 11.00000 0.02259 0.01052 = 0.01341 -0.00084 0.00266 -0.00365 C2 1 0.276530 0.480193 0.433520 11.00000 0.01723 0.02280 = 0.00885 0.00194 0.00122 0.00296 AFIX 13 H2 2 0.464797 0.488286 0.437435 11.00000 -1.20000 AFIX 0 C3 1 0.168183 0.647301 0.400724 11.00000 0.03934 0.01882 = 0.01452 0.00411 0.00542 0.00867 AFIX 23 H3A 2 -0.018957 0.644435 0.401187 11.00000 -1.20000 H3B 2 0.225297 0.746474 0.430138 11.00000 -1.20000 AFIX 0 HKLF 4 REM REM R1 = 0.0335 for 1132 Fo > 4sig(Fo) and 0.0419 for all 1248 data REM 110 parameters refined using 0 restraints END WGHT 0.0224 0.0000 REM Highest difference peak 0.456, deepest hole -0.453, 1-sigma level 0.106 Q1 1 -0.1402 0.8837 0.3239 11.00000 0.05 0.46 Q2 1 0.4717 1.0219 0.3305 11.00000 0.05 0.45 Q3 1 -0.0363 1.0253 0.3283 11.00000 0.05 0.44 Q4 1 0.1346 0.6620 0.1765 11.00000 0.05 0.43 Q5 1 0.4642 0.1061 0.3822 11.00000 0.05 0.40 Q6 1 -0.4836 1.1606 0.3259 11.00000 0.05 0.39 Q7 1 0.0139 1.0990 0.2616 11.00000 0.05 0.36 Q8 1 0.1900 0.7512 0.2950 11.00000 0.05 0.35 Q9 1 0.7510 0.5086 0.4390 11.00000 0.05 0.34 Q10 1 -0.0103 0.8232 0.2807 11.00000 0.05 0.34 Q11 1 -0.2033 0.7891 0.2745 11.00000 0.05 0.33 Q12 1 0.4851 0.8955 0.3205 11.00000 0.05 0.33 Q13 1 -0.1973 1.0505 0.2753 11.00000 0.05 0.31 Q14 1 0.5528 0.4649 0.4014 11.00000 0.05 0.31 Q15 1 0.2737 0.7540 0.5071 11.00000 0.05 0.30 Q16 1 0.4052 0.7593 0.1223 11.00000 0.05 0.30 Q17 1 -0.0387 0.9536 0.2677 11.00000 0.05 0.29 Q18 1 0.1759 1.0348 0.2226 11.00000 0.05 0.29 Q19 1 0.2004 0.2398 0.3266 11.00000 0.05 0.28 Q20 1 0.0938 0.2384 0.5370 11.00000 0.05 0.28 ; _shelx_res_checksum 81600 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' 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 Zn1 Zn -0.31587(14) 1.01979(9) 0.32768(4) 0.0140(2) Uani 1 1 d . . . . . P1 P 0.1857(4) 0.8259(2) 0.27506(8) 0.0111(4) Uani 1 1 d . . . . . O1 O 0.2897(9) 0.5082(7) 0.5664(2) 0.0282(12) Uani 1 1 d . . . . . O2 O -0.0563(11) 0.3857(7) 0.5148(3) 0.0305(14) Uani 1 1 d . . . . . O3 O 0.2606(9) 0.6600(5) 0.3256(2) 0.0192(11) Uani 1 1 d . . . . . O4 O -0.1017(9) 0.8512(6) 0.2775(2) 0.0184(11) Uani 1 1 d . . . . . O5 O 0.2758(8) 0.7699(5) 0.1970(2) 0.0131(11) Uani 1 1 d . . . . . O6 O 0.3270(8) 0.9815(5) 0.3068(2) 0.0177(10) Uani 1 1 d . . . . . N1 N 0.2045(12) 0.3308(6) 0.3853(3) 0.0187(13) Uani 1 1 d . . . . . H1A H 0.2771 0.3426 0.3401 0.022 Uiso 1 1 calc R U . . . H1B H 0.0337 0.3271 0.3803 0.022 Uiso 1 1 calc R U . . . H1C H 0.2593 0.2327 0.4066 0.022 Uiso 1 1 calc R U . . . C1 C 0.1585(15) 0.4512(8) 0.5121(3) 0.0155(15) Uani 1 1 d . . . . . C2 C 0.2765(12) 0.4802(9) 0.4335(3) 0.0163(15) Uani 1 1 d . . . . . H2 H 0.4648 0.4883 0.4374 0.020 Uiso 1 1 calc R U . . . C3 C 0.1682(18) 0.6473(8) 0.4007(3) 0.0242(17) Uani 1 1 d . . . . . H3A H -0.0190 0.6444 0.4012 0.029 Uiso 1 1 calc R U . . . H3B H 0.2253 0.7465 0.4301 0.029 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 Zn1 0.0148(4) 0.0157(4) 0.0116(3) -0.0011(3) 0.0006(4) -0.0007(4) P1 0.0129(9) 0.0104(8) 0.0098(7) 0.0007(6) 0.0010(9) 0.0013(9) O1 0.033(3) 0.042(3) 0.0088(19) 0.000(2) 0.002(2) -0.009(3) O2 0.031(3) 0.041(3) 0.020(3) -0.002(2) 0.010(3) -0.015(3) O3 0.032(3) 0.014(2) 0.0121(19) 0.003(2) 0.005(2) 0.006(2) O4 0.014(3) 0.025(3) 0.016(2) -0.004(2) 0.000(2) 0.001(2) O5 0.016(3) 0.012(2) 0.0112(19) 0.0019(16) 0.0022(19) 0.006(2) O6 0.013(2) 0.015(2) 0.025(2) -0.0031(19) 0.000(2) 0.001(3) N1 0.028(4) 0.020(3) 0.008(2) 0.001(2) -0.002(3) -0.002(3) C1 0.023(4) 0.011(3) 0.013(3) -0.001(3) 0.003(3) -0.004(4) C2 0.017(4) 0.023(4) 0.009(3) 0.002(3) 0.001(3) 0.003(3) C3 0.039(5) 0.019(4) 0.015(3) 0.004(3) 0.005(4) 0.009(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' 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' P P 0.1023 0.0942 '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 _geom_angle_publ_flag O6 Zn1 O4 111.42(19) 1_455 . ? O6 Zn1 O1 115.96(19) 1_455 3_466 ? O4 Zn1 O1 101.9(2) . 3_466 ? O6 Zn1 O5 102.00(18) 1_455 4 ? O4 Zn1 O5 119.42(18) . 4 ? O1 Zn1 O5 106.7(2) 3_466 4 ? O4 P1 O6 111.5(3) . . ? O4 P1 O5 111.5(3) . . ? O6 P1 O5 114.4(2) . . ? O4 P1 O3 109.1(3) . . ? O6 P1 O3 107.8(2) . . ? O5 P1 O3 102.0(2) . . ? C1 O1 Zn1 122.8(4) . 3_566 ? C3 O3 P1 119.7(4) . . ? P1 O4 Zn1 132.2(3) . . ? P1 O5 Zn1 120.5(2) . 4_545 ? P1 O6 Zn1 131.6(3) . 1_655 ? C2 N1 H1A 109.5 . . ? C2 N1 H1B 109.5 . . ? H1A N1 H1B 109.5 . . ? C2 N1 H1C 109.5 . . ? H1A N1 H1C 109.5 . . ? H1B N1 H1C 109.5 . . ? O2 C1 O1 127.3(6) . . ? O2 C1 C2 117.2(6) . . ? O1 C1 C2 115.3(6) . . ? N1 C2 C3 110.1(5) . . ? N1 C2 C1 108.0(5) . . ? C3 C2 C1 108.8(5) . . ? N1 C2 H2 110.0 . . ? C3 C2 H2 110.0 . . ? C1 C2 H2 110.0 . . ? O3 C3 C2 107.0(5) . . ? O3 C3 H3A 110.3 . . ? C2 C3 H3A 110.3 . . ? O3 C3 H3B 110.3 . . ? C2 C3 H3B 110.3 . . ? H3A C3 H3B 108.6 . . ? 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 Zn1 O6 1.910(4) 1_455 ? Zn1 O4 1.924(4) . ? Zn1 O1 1.966(4) 3_466 ? Zn1 O5 1.983(4) 4 ? P1 O4 1.503(5) . ? P1 O6 1.512(4) . ? P1 O5 1.522(4) . ? P1 O3 1.607(4) . ? O1 C1 1.258(7) . ? O1 Zn1 1.966(4) 3_566 ? O2 C1 1.222(9) . ? O3 C3 1.418(7) . ? O5 Zn1 1.983(4) 4_545 ? O6 Zn1 1.910(4) 1_655 ? N1 C2 1.479(8) . ? N1 H1A 0.8900 . ? N1 H1B 0.8900 . ? N1 H1C 0.8900 . ? C1 C2 1.537(8) . ? C2 C3 1.518(9) . ? C2 H2 0.9800 . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ?