#------------------------------------------------------------------------------ #$Date: 2025-07-01 13:56:09 +0300 (Tue, 01 Jul 2025) $ #$Revision: 1152 $ #$URL: svn://localhost/testcod/cif/7/70/00/7700032.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_7700032 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 Co N O6 P' _chemical_formula_sum 'C3 H6 Co N O6 P' _chemical_formula_weight 241.99 _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 ; 2017-09-12 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 5.202(4) _cell_length_b 7.7413(4) _cell_length_c 17.7009(13) _cell_measurement_reflns_used 1169 _cell_measurement_temperature 295(2) _cell_measurement_theta_max 27.0330 _cell_measurement_theta_min 4.8580 _cell_volume 712.8(6) _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 0.977 _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 0.0384 _diffrn_reflns_av_unetI/netI 0.0465 _diffrn_reflns_Laue_measured_fraction_full 0.977 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 2931 _diffrn_reflns_point_group_measured_fraction_full 0.907 _diffrn_reflns_point_group_measured_fraction_max 0.927 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.046 _diffrn_reflns_theta_min 3.496 _exptl_absorpt_coefficient_mu 2.622 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.92214 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Blessing, Acta Cryst. A51 (1995) 33-38' _exptl_crystal_colour blue _exptl_crystal_density_diffrn 2.255 _exptl_crystal_description needle _exptl_crystal_F_000 484 _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.03 _refine_diff_density_max 0.503 _refine_diff_density_min -0.402 _refine_diff_density_rms 0.110 _refine_ls_abs_structure_details ; Flack x determined using 348 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack -0.02(2) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 110 _refine_ls_number_reflns 1168 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.063 _refine_ls_R_factor_all 0.0363 _refine_ls_R_factor_gt 0.0296 _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^)+(0.0282P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0609 _refine_ls_wR_factor_ref 0.0637 _reflns_Friedel_coverage 0.517 _reflns_Friedel_fraction_full 0.796 _reflns_Friedel_fraction_max 0.816 _reflns_number_gt 1047 _reflns_number_total 1168 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c7dt03474a2.cif _cod_data_source_block vv138 _cod_original_cell_volume 712.9(6) _cod_database_code 7700032 _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 VV138 in P212121 #19 REM reset to P212121 #19 CELL 0.71073 5.2025 7.7413 17.7009 90 90 90 ZERR 4 0.004 0.0004 0.0013 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 Co UNIT 12 24 4 24 4 4 L.S. 50 BOND $H acta OMIT 0 50.1 REM REM REM WGHT 0.028200 FVAR 3.20184 CO1 6 -0.186696 -0.981643 -0.328226 11.00000 0.01788 0.01437 = 0.01410 0.00160 0.00064 0.00055 P1 5 -0.311778 -0.676289 -0.226081 11.00000 0.01541 0.01088 = 0.01230 0.00119 -0.00013 0.00128 O1 4 -0.206141 -0.987676 0.065654 11.00000 0.03831 0.03903 = 0.01103 0.00082 0.00072 -0.00963 O2 4 -0.548541 -1.117459 0.015490 11.00000 0.03211 0.03838 = 0.01991 0.00054 0.00806 -0.01248 O3 4 -0.236647 -0.842557 -0.175995 11.00000 0.03495 0.01439 = 0.01354 0.00607 0.00182 0.00681 O4 4 -0.225500 -0.731358 -0.304215 11.00000 0.02474 0.01276 = 0.01432 0.00209 0.00121 0.00406 O5 4 -0.599207 -0.652215 -0.222709 11.00000 0.01955 0.02037 = 0.01687 -0.00523 -0.00096 0.00076 O6 4 -0.171902 -0.522183 -0.194376 11.00000 0.01943 0.01343 = 0.02791 -0.00387 0.00449 -0.00232 N1 3 -0.293007 -1.169149 -0.115171 11.00000 0.02417 0.01881 = 0.01201 0.00104 -0.00344 0.00215 AFIX 137 H1A 2 -0.221827 -1.156830 -0.160573 11.00000 -1.20000 H1B 2 -0.463256 -1.172661 -0.119849 11.00000 -1.20000 H1C 2 -0.237910 -1.266882 -0.094220 11.00000 -1.20000 AFIX 0 C1 1 -0.337090 -1.047473 0.011865 11.00000 0.02776 0.01163 = 0.01378 0.00343 0.00003 0.00268 C2 1 -0.219888 -1.021280 -0.066730 11.00000 0.01676 0.01535 = 0.01538 0.00145 -0.00252 -0.00191 AFIX 13 H2 2 -0.032304 -1.013568 -0.062963 11.00000 -1.20000 AFIX 0 C3 1 -0.328458 -0.854264 -0.100117 11.00000 0.04241 0.01944 = 0.01613 0.00197 0.00957 0.00339 AFIX 23 H3A 2 -0.514853 -0.856845 -0.099451 11.00000 -1.20000 H3B 2 -0.270934 -0.755458 -0.070964 11.00000 -1.20000 AFIX 0 HKLF 4 REM VV138 in P212121 #19 REM R1 = 0.0296 for 1047 Fo > 4sig(Fo) and 0.0363 for all 1168 data REM 110 parameters refined using 0 restraints END WGHT 0.0282 0.0000 REM Highest difference peak 0.503, deepest hole -0.402, 1-sigma level 0.110 Q1 1 0.0053 -0.9478 -0.3245 11.00000 0.05 0.50 Q2 1 -0.4998 -0.6466 -0.1790 11.00000 0.05 0.39 Q3 1 -0.5305 -0.7222 -0.2040 11.00000 0.05 0.33 Q4 1 -0.4803 -1.2963 -0.1765 11.00000 0.05 0.33 Q5 1 -0.0849 -1.3105 -0.1604 11.00000 0.05 0.31 Q6 1 0.0650 -0.9341 -0.1348 11.00000 0.05 0.30 Q7 1 -0.0340 -1.0049 -0.0810 11.00000 0.05 0.30 Q8 1 -0.5141 -0.9153 0.0660 11.00000 0.05 0.30 Q9 1 0.0857 -0.8942 -0.1073 11.00000 0.05 0.29 Q10 1 0.0444 -0.9085 0.0607 11.00000 0.05 0.29 Q11 1 -0.0498 -1.0552 -0.0659 11.00000 0.05 0.29 Q12 1 -0.3997 -0.9417 -0.3232 11.00000 0.05 0.28 Q13 1 0.0361 -1.2134 -0.0860 11.00000 0.05 0.27 Q14 1 -0.5715 -1.2167 0.0416 11.00000 0.05 0.27 Q15 1 -0.5429 -1.0946 -0.0284 11.00000 0.05 0.27 Q16 1 -0.0366 -0.7223 -0.3026 11.00000 0.05 0.26 Q17 1 -0.0826 -0.7529 -0.3804 11.00000 0.05 0.26 Q18 1 -0.5066 -0.9229 -0.1172 11.00000 0.05 0.26 Q19 1 0.0088 -0.9170 -0.1844 11.00000 0.05 0.26 Q20 1 -0.0834 -0.5944 -0.0448 11.00000 0.05 0.26 ; _shelx_res_checksum 4682 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 Co1 Co -0.18670(14) -0.98164(9) -0.32823(4) 0.0155(2) Uani 1 1 d . . . . . P1 P -0.3118(3) -0.67629(16) -0.22608(7) 0.0129(3) Uani 1 1 d . . . . . O1 O -0.2061(8) -0.9877(6) 0.06565(19) 0.0295(10) Uani 1 1 d . . . . . O2 O -0.5485(9) -1.1175(6) 0.0155(2) 0.0301(11) Uani 1 1 d . . . . . O3 O -0.2366(7) -0.8426(4) -0.1760(2) 0.0210(10) Uani 1 1 d . . . . . O4 O -0.2255(7) -0.7314(4) -0.30421(19) 0.0173(9) Uani 1 1 d . . . . . O5 O -0.5992(7) -0.6522(5) -0.2227(2) 0.0189(9) Uani 1 1 d . . . . . O6 O -0.1719(7) -0.5222(5) -0.1944(2) 0.0203(8) Uani 1 1 d . . . . . N1 N -0.2930(10) -1.1691(5) -0.1152(2) 0.0183(11) Uani 1 1 d . . . . . H1A H -0.2218 -1.1568 -0.1606 0.022 Uiso 1 1 calc R U . . . H1B H -0.4633 -1.1727 -0.1198 0.022 Uiso 1 1 calc R U . . . H1C H -0.2379 -1.2669 -0.0942 0.022 Uiso 1 1 calc R U . . . C1 C -0.3371(13) -1.0475(6) 0.0119(3) 0.0177(13) Uani 1 1 d . . . . . C2 C -0.2199(10) -1.0213(7) -0.0667(3) 0.0158(12) Uani 1 1 d . . . . . H2 H -0.0323 -1.0136 -0.0630 0.019 Uiso 1 1 calc R U . . . C3 C -0.3285(15) -0.8543(7) -0.1001(3) 0.0260(14) Uani 1 1 d . . . . . H3A H -0.5149 -0.8568 -0.0995 0.031 Uiso 1 1 calc R U . . . H3B H -0.2709 -0.7555 -0.0710 0.031 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 Co1 0.0179(4) 0.0144(4) 0.0141(4) 0.0016(3) 0.0006(4) 0.0006(4) P1 0.0154(7) 0.0109(7) 0.0123(7) 0.0012(5) -0.0001(8) 0.0013(7) O1 0.038(2) 0.039(3) 0.0110(19) 0.0008(19) 0.001(2) -0.010(3) O2 0.032(3) 0.038(3) 0.020(2) 0.001(2) 0.008(2) -0.012(2) O3 0.035(3) 0.0144(19) 0.0135(19) 0.0061(16) 0.002(2) 0.0068(16) O4 0.025(2) 0.0128(19) 0.0143(19) 0.0021(14) 0.0012(18) 0.0041(16) O5 0.020(2) 0.020(2) 0.017(2) -0.0052(17) -0.0010(18) 0.0008(16) O6 0.0194(19) 0.0134(19) 0.028(2) -0.0039(16) 0.0045(18) -0.002(2) N1 0.024(3) 0.019(3) 0.012(2) 0.0010(18) -0.003(3) 0.002(2) C1 0.028(3) 0.012(3) 0.014(3) 0.003(2) 0.000(3) 0.003(3) C2 0.017(3) 0.015(3) 0.015(3) 0.001(2) -0.003(2) -0.002(3) C3 0.042(4) 0.019(3) 0.016(3) 0.002(2) 0.010(3) 0.003(3) 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' Co Co 0.3494 0.9721 '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 Co1 O5 110.23(16) 4_544 4_444 ? O6 Co1 O1 116.74(17) 4_544 2_434 ? O5 Co1 O1 101.38(17) 4_444 2_434 ? O6 Co1 O4 102.20(15) 4_544 . ? O5 Co1 O4 120.13(16) 4_444 . ? O1 Co1 O4 106.93(17) 2_434 . ? O6 P1 O5 111.5(2) . . ? O6 P1 O4 114.8(2) . . ? O5 P1 O4 111.4(2) . . ? O6 P1 O3 108.1(2) . . ? O5 P1 O3 108.5(2) . . ? O4 P1 O3 101.9(2) . . ? C1 O1 Co1 121.5(4) . 2_435 ? C3 O3 P1 119.1(4) . . ? P1 O4 Co1 119.9(2) . . ? P1 O5 Co1 132.0(2) . 4_454 ? P1 O6 Co1 132.2(2) . 4_554 ? 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 127.4(5) . . ? O2 C1 C2 117.5(5) . . ? O1 C1 C2 115.0(5) . . ? N1 C2 C3 109.6(4) . . ? N1 C2 C1 108.7(4) . . ? C3 C2 C1 108.4(4) . . ? N1 C2 H2 110.0 . . ? C3 C2 H2 110.0 . . ? C1 C2 H2 110.0 . . ? O3 C3 C2 107.1(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 Co1 O6 1.934(4) 4_544 ? Co1 O5 1.949(4) 4_444 ? Co1 O1 1.974(3) 2_434 ? Co1 O4 1.994(3) . ? P1 O6 1.506(4) . ? P1 O5 1.508(4) . ? P1 O4 1.515(4) . ? P1 O3 1.611(4) . ? O1 C1 1.259(7) . ? O1 Co1 1.974(3) 2_435 ? O2 C1 1.228(7) . ? O3 C3 1.428(7) . ? O5 Co1 1.949(4) 4_454 ? O6 Co1 1.934(4) 4_554 ? N1 C2 1.480(7) . ? N1 H1A 0.8900 . ? N1 H1B 0.8900 . ? N1 H1C 0.8900 . ? C1 C2 1.532(7) . ? C2 C3 1.530(8) . ? C2 H2 0.9800 . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ?