#------------------------------------------------------------------------------ #$Date: 2019-11-07 21:35:52 +0200 (Thu, 07 Nov 2019) $ #$Revision: 223554 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/23/45/7234530.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_7234530 loop_ _publ_author_name 'Galadzhun, Iurii' 'Capel Berdiell, Izar' 'Shahid, Namrah' 'Halcrow, Malcolm A.' _publ_section_title ; An iron(ii) coordination polymer of a triazolyl tris-heterocycle showing a spin state conversion triggered by loss of lattice solvent ; _journal_issue 42 _journal_name_full CrystEngComm _journal_page_first 6330 _journal_paper_doi 10.1039/C9CE01496A _journal_volume 21 _journal_year 2019 _chemical_absolute_configuration unk _chemical_formula_moiety 'C8 H6 F N3' _chemical_formula_sum 'C8 H6 F N3' _chemical_formula_weight 163.16 _chemical_name_systematic ; 2-Fluoro-6-(pyrazol-1-yl)pyridine ; _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' _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_space_group_name_H-M 'P 21 21 21' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_date 2019-07-18 _audit_creation_method ; Olex2 1.2 (compiled Apr 23 2013 17:54:37, GUI svn.r4466) ; _audit_update_record ; 2019-08-30 deposited with the CCDC. 2019-10-10 downloaded from the CCDC. ; _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 4.0393(1) _cell_length_b 11.2187(4) _cell_length_c 16.2922(4) _cell_measurement_reflns_used 1216 _cell_measurement_temperature 120(2) _cell_measurement_theta_max 73.52 _cell_measurement_theta_min 4.75 _cell_volume 738.29(4) _computing_cell_refinement 'CrysAlisPro, Agilent Technologies' _computing_data_collection 'CrysAlisPro, Agilent Technologies' _computing_data_reduction 'CrysAlisPro, Agilent Technologies' _computing_molecular_graphics 'XSEED (Barbour, 2001)' _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 120(2) _diffrn_detector_area_resol_mean 5.3095 _diffrn_measured_fraction_theta_full 0.976 _diffrn_measured_fraction_theta_max 0.960 _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator mirror _diffrn_radiation_source 'SuperNova (Cu) X-ray Source' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0134 _diffrn_reflns_av_unetI/netI 0.0154 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_h_min -2 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 1711 _diffrn_reflns_theta_full 72.00 _diffrn_reflns_theta_max 73.66 _diffrn_reflns_theta_min 4.79 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.943 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.781 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.468 _exptl_crystal_density_method 'not measured' _exptl_crystal_description lath _exptl_crystal_F_000 336 _exptl_crystal_recrystallization_method 'From the Melt' _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.15 _refine_diff_density_max 0.150 _refine_diff_density_min -0.153 _refine_diff_density_rms 0.035 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.5(3) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_hydrogen_treatment refxyz _refine_ls_matrix_type full _refine_ls_number_parameters 127 _refine_ls_number_reflns 870 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.079 _refine_ls_R_factor_all 0.0293 _refine_ls_R_factor_gt 0.0277 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0525P)^2^+0.1020P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0770 _refine_ls_wR_factor_ref 0.0786 _reflns_number_gt 829 _reflns_number_total 870 _reflns_threshold_expression >2sigma(I) _cod_data_source_file c9ce01496a2.cif _cod_data_source_block ig11 _cod_depositor_comments 'Adding full bibliography for 7234530--7234535.cif.' _cod_database_code 7234530 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups ; _shelx_res_file ; TITL ig11_a.res in P2(1)2(1)2(1) CELL 1.54184 4.0393 11.2187 16.2922 90 90 90 ZERR 4 0.0001 0.0004 0.0004 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 F N UNIT 32 24 4 12 L.S. 10 PLAN 20 TEMP -153 REM Old TITL IG11 in P2(1)2(1)2(1) REM SHELXT solution in P2(1)2(1)2(1) REM R1 0.095, Rweak 0.019, Alpha 0.000, Orientation as input REM Flack x = -0.121 ( 0.130 ) from Parsons' quotients REM Formula found by SHELXT: C9 N2 O REM ig11_a.res in P2(1)2(1)2(1) REM 109 parameters refined using 0 restraints REM Highest difference peak 0.140, deepest hole -0.145, 1-sigma level 0.035 GRID BOND $H fmap 2 acta 144 MERG 3 REM C:\Users\chmmah\Desktop\ig13Cn%20and%20ig14Cn%20paper\ig11\ig11.hkl WGHT 0.052500 0.102000 FVAR 1.22574 N1 4 1.121662 0.916612 0.597371 11.00000 0.02660 0.02124 = 0.02361 0.00121 0.00246 0.00191 C2 1 1.040733 1.012278 0.553151 11.00000 0.02033 0.02148 = 0.02067 -0.00050 0.00338 0.00042 C3 1 1.132894 1.128068 0.572917 11.00000 0.02535 0.02037 = 0.02671 0.00172 0.00248 -0.00007 H3 2 1.071165 1.193155 0.540564 11.00000 -1.20000 C4 1 1.318123 1.143834 0.643605 11.00000 0.02705 0.02459 = 0.02858 -0.00333 0.00137 -0.00341 H4 2 1.387517 1.223711 0.658519 11.00000 -1.20000 C5 1 1.402644 1.047014 0.691720 11.00000 0.02697 0.03237 = 0.02394 -0.00254 -0.00013 -0.00005 H5 2 1.518644 1.051918 0.741154 11.00000 -1.20000 C6 1 1.297455 0.937525 0.663654 11.00000 0.02881 0.02565 = 0.02428 0.00499 0.00164 0.00494 N7 4 0.846305 0.988368 0.482995 11.00000 0.02208 0.01877 = 0.02259 0.00070 0.00160 0.00144 N8 4 0.736759 1.080058 0.435149 11.00000 0.03088 0.02277 = 0.02347 0.00317 -0.00073 0.00441 C9 1 0.562313 1.026709 0.376920 11.00000 0.02961 0.03006 = 0.02281 0.00005 -0.00062 0.00502 H9 2 0.466160 1.074105 0.335739 11.00000 -1.20000 C10 1 0.558030 0.901960 0.386022 11.00000 0.02544 0.02858 = 0.02644 -0.00617 -0.00060 -0.00078 H10 2 0.456467 0.845919 0.351619 11.00000 -1.20000 C11 1 0.743642 0.880572 0.454709 11.00000 0.02324 0.02048 = 0.02883 -0.00130 0.00249 -0.00090 H11 2 0.792681 0.807185 0.481010 11.00000 -1.20000 F12 3 1.377214 0.838954 0.707615 11.00000 0.05442 0.02915 = 0.03156 0.00648 -0.00932 0.00561 HKLF 4 REM ig11_a.res in P2(1)2(1)2(1) REM R1 = 0.0277 for 829 Fo > 4sig(Fo) and 0.0293 for all 870 data REM 127 parameters refined using 0 restraints END WGHT 0.0525 0.1020 REM Highest difference peak 0.150, deepest hole -0.153, 1-sigma level 0.035 Q1 1 1.3570 1.0008 0.6777 11.00000 0.05 0.15 Q2 1 1.1069 1.0709 0.5623 11.00000 0.05 0.13 Q3 1 0.7308 0.8839 0.3981 11.00000 0.05 0.11 Q4 1 1.3134 0.9851 0.5055 11.00000 0.05 0.11 Q5 1 1.0121 1.0028 0.5013 11.00000 0.05 0.11 Q6 1 0.5848 1.0081 0.5453 11.00000 0.05 0.11 Q7 1 1.1132 0.7801 0.7011 11.00000 0.05 0.11 Q8 1 1.0140 0.8471 0.5805 11.00000 0.05 0.11 Q9 1 0.6770 1.0197 0.5651 11.00000 0.05 0.10 Q10 1 0.2614 0.8838 0.4401 11.00000 0.05 0.10 Q11 1 0.8681 1.0006 0.5266 11.00000 0.05 0.10 Q12 1 0.9219 0.9351 0.6611 11.00000 0.05 0.10 Q13 1 1.4514 1.0940 0.6611 11.00000 0.05 0.10 Q14 1 0.5451 0.8856 0.4333 11.00000 0.05 0.10 Q15 1 0.6074 0.9639 0.3635 11.00000 0.05 0.10 Q16 1 0.7545 1.0268 0.5926 11.00000 0.05 0.10 Q17 1 1.0765 0.9273 0.6405 11.00000 0.05 0.10 Q18 1 0.7615 1.0604 0.3848 11.00000 0.05 0.10 Q19 1 0.4832 0.9633 0.3802 11.00000 0.05 0.09 Q20 1 1.1223 1.1374 0.6240 11.00000 0.05 0.09 REM The information below was added by Olex2. REM REM R1 = 0.0277 for 829 Fo > 4sig(Fo) and 0.0293 for all 1729 data REM n/a parameters refined using n/a restraints REM Highest difference peak 0.15, deepest hole -0.15 REM Mean Shift 0, Max Shift 0. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0293 REM R1_gt = 0.0277 REM wR_ref = 0.0786 REM GOOF = 1.079 REM Shift_max = 0 REM Shift_mean = 0 REM Reflections_all = 1729 REM Reflections_gt = 829 REM Parameters = n/a REM Hole = 0.15 REM Peak = -0.15 REM Flack = 0.5(3) ; loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x+1/2, -y, z+1/2' 3 'x+1/2, -y+1/2, -z' 4 '-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_symmetry_multiplicity _atom_site_calc_flag N1 N 1.1217(4) 0.91661(13) 0.59737(8) 0.0238(3) Uani 1 1 d C2 C 1.0407(4) 1.01228(15) 0.55315(10) 0.0208(4) Uani 1 1 d C3 C 1.1329(5) 1.12807(15) 0.57292(10) 0.0241(4) Uani 1 1 d H3 H 1.071(6) 1.1932(17) 0.5406(12) 0.029 Uiso 1 1 d C4 C 1.3181(5) 1.14383(17) 0.64361(11) 0.0267(4) Uani 1 1 d H4 H 1.388(7) 1.2237(18) 0.6585(13) 0.032 Uiso 1 1 d C5 C 1.4026(5) 1.04701(17) 0.69172(11) 0.0278(4) Uani 1 1 d H5 H 1.519(6) 1.052(2) 0.7412(14) 0.033 Uiso 1 1 d C6 C 1.2975(5) 0.93753(16) 0.66365(10) 0.0262(4) Uani 1 1 d N7 N 0.8463(4) 0.98837(12) 0.48299(8) 0.0211(3) Uani 1 1 d N8 N 0.7368(4) 1.08006(13) 0.43515(8) 0.0257(4) Uani 1 1 d C9 C 0.5623(5) 1.02671(17) 0.37692(10) 0.0275(4) Uani 1 1 d H9 H 0.466(6) 1.0741(19) 0.3357(13) 0.033 Uiso 1 1 d C10 C 0.5580(5) 0.90196(17) 0.38602(11) 0.0268(4) Uani 1 1 d H10 H 0.456(6) 0.8459(18) 0.3516(13) 0.032 Uiso 1 1 d C11 C 0.7436(5) 0.88057(16) 0.45471(11) 0.0242(4) Uani 1 1 d H11 H 0.793(6) 0.8072(17) 0.4810(12) 0.029 Uiso 1 1 d F12 F 1.3772(4) 0.83895(10) 0.70761(6) 0.0384(3) Uani 1 1 d 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 N1 0.0266(8) 0.0212(7) 0.0236(7) 0.0012(5) 0.0025(7) 0.0019(7) C2 0.0203(8) 0.0215(8) 0.0207(7) -0.0005(6) 0.0034(7) 0.0004(7) C3 0.0253(9) 0.0204(8) 0.0267(8) 0.0017(7) 0.0025(7) -0.0001(8) C4 0.0271(10) 0.0246(8) 0.0286(8) -0.0033(7) 0.0014(7) -0.0034(9) C5 0.0270(9) 0.0324(10) 0.0239(8) -0.0025(7) -0.0001(8) -0.0001(9) C6 0.0288(9) 0.0257(8) 0.0243(8) 0.0050(7) 0.0016(7) 0.0049(8) N7 0.0221(7) 0.0188(7) 0.0226(6) 0.0007(5) 0.0016(6) 0.0014(6) N8 0.0309(8) 0.0228(7) 0.0235(7) 0.0032(6) -0.0007(6) 0.0044(7) C9 0.0296(9) 0.0301(9) 0.0228(8) 0.0001(7) -0.0006(8) 0.0050(9) C10 0.0254(9) 0.0286(9) 0.0264(8) -0.0062(7) -0.0006(8) -0.0008(9) C11 0.0232(9) 0.0205(8) 0.0288(8) -0.0013(7) 0.0025(7) -0.0009(7) F12 0.0544(8) 0.0292(6) 0.0316(6) 0.0065(4) -0.0093(6) 0.0056(6) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 '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 C6 N1 C2 115.66(15) N1 C2 C3 124.18(16) N1 C2 N7 114.88(15) C3 C2 N7 120.94(15) C2 C3 H3 121.9(13) C4 C3 C2 117.20(16) C4 C3 H3 120.9(13) C3 C4 H4 118.9(13) C5 C4 C3 120.31(17) C5 C4 H4 120.8(13) C4 C5 H5 124.5(14) C6 C5 C4 115.86(16) C6 C5 H5 119.6(14) N1 C6 C5 126.78(16) N1 C6 F12 114.64(15) F12 C6 C5 118.58(16) N8 N7 C2 119.96(13) C11 N7 C2 127.81(14) C11 N7 N8 112.22(13) C9 N8 N7 103.95(14) N8 C9 H9 118.4(13) N8 C9 C10 112.36(17) C10 C9 H9 129.2(13) C9 C10 H10 127.6(13) C11 C10 C9 104.70(17) C11 C10 H10 127.7(13) N7 C11 C10 106.77(16) N7 C11 H11 123.7(13) C10 C11 H11 129.5(13) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance N1 C2 1.333(2) N1 C6 1.314(2) C2 C3 1.389(2) C2 N7 1.413(2) C3 H3 0.93(2) C3 C4 1.385(3) C4 H4 0.97(2) C4 C5 1.382(3) C5 H5 0.93(2) C5 C6 1.378(3) C6 F12 1.3563(19) N7 N8 1.3644(19) N7 C11 1.359(2) N8 C9 1.325(2) C9 H9 0.94(2) C9 C10 1.407(3) C10 H10 0.94(2) C10 C11 1.368(2) C11 H11 0.949(19)