#------------------------------------------------------------------------------ #$Date: 2021-07-05 20:34:47 +0300 (Mon, 05 Jul 2021) $ #$Revision: 267163 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/71/7707185.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_7707185 loop_ _publ_author_name 'Zenno, Hikaru' 'Kobayashi, Fumiya' 'Nakamura, Masaaki' 'Sekine, Yoshihiro' 'Lindoy, Leonard F.' 'Hayami, Shinya' _publ_section_title ; Hydrogen bond-induced abrupt spin crossover behaviour in 1-D cobalt(II) complexes - the key role of solvate water molecules. ; _journal_issue 22 _journal_name_full 'Dalton transactions (Cambridge, England : 2003)' _journal_page_first 7843 _journal_page_last 7853 _journal_paper_doi 10.1039/d1dt01069g _journal_volume 50 _journal_year 2021 _chemical_formula_moiety 'C20 H14 Cl2 Co N4, H4 O2' _chemical_formula_sum 'C20 H18 Cl2 Co N4 O2' _chemical_formula_weight 476.21 _space_group_crystal_system orthorhombic _space_group_IT_number 54 _space_group_name_Hall '-P 2a 2ac' _space_group_name_H-M_alt 'P c c a' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _audit_creation_date 2021-01-21 _audit_creation_method ; Olex2 1.3 (compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226) ; _audit_update_record ; 2021-01-28 deposited with the CCDC. 2021-04-22 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 10.7848(18) _cell_length_b 7.5554(18) _cell_length_c 21.527(4) _cell_measurement_reflns_used 619 _cell_measurement_temperature 250 _cell_measurement_theta_max 25.2700 _cell_measurement_theta_min 2.6820 _cell_volume 1754.1(6) _computing_cell_refinement 'CrysAlisPro 1.171.40.15 (Rigaku OD, 2018)' _computing_data_collection 'CrysAlisPro 1.171.40.15 (Rigaku OD, 2018)' _computing_data_reduction 'CrysAlisPro 1.171.40.15 (Rigaku OD, 2018)' _computing_molecular_graphics 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2014/7 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 250 _diffrn_detector 'CCD plate' _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.993 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w -14.00 39.00 0.50 105.00 -- 20.00 54.00-150.00 106 2 \w 63.00 90.00 0.50 105.00 -- 20.00 54.00-150.00 54 3 \w -73.00 -32.00 0.50 105.00 -- 20.00 54.00 -90.00 82 4 \w -24.00 30.00 0.50 105.00 -- 20.00 54.00 -90.00 108 5 \w 83.00 110.00 0.50 105.00 -- 20.00 54.00 -90.00 54 6 \w -52.00 -27.00 0.50 105.00 -- 20.00 54.00 -60.00 50 7 \w -21.00 6.00 0.50 105.00 -- 20.00 54.00 -60.00 54 8 \w -67.00 23.00 0.50 105.00 -- 20.00 54.00 -30.00 180 9 \w -71.00 -43.00 0.50 105.00 -- 20.00 54.00-150.00 56 ; _diffrn_measurement_device 'two-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB Mini II' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0035045000 _diffrn_orient_matrix_UB_12 0.0933242000 _diffrn_orient_matrix_UB_13 0.0032476000 _diffrn_orient_matrix_UB_21 -0.0019062000 _diffrn_orient_matrix_UB_22 0.0092349000 _diffrn_orient_matrix_UB_23 -0.0327743000 _diffrn_orient_matrix_UB_31 -0.0656288000 _diffrn_orient_matrix_UB_32 0.0047337000 _diffrn_orient_matrix_UB_33 0.0010718000 _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1008 _diffrn_reflns_av_unetI/netI 0.1063 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.993 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_number 8067 _diffrn_reflns_point_group_measured_fraction_full 0.996 _diffrn_reflns_point_group_measured_fraction_max 0.993 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.367 _diffrn_reflns_theta_min 2.674 _diffrn_source 'fine-focus sealed X-ray tube' _diffrn_source_type 'Rigaku (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 1.311 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.22023 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.15 (Rigaku Oxford Diffraction, 2018) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'clear dark orange' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier dark _exptl_crystal_colour_primary orange _exptl_crystal_density_diffrn 1.803 _exptl_crystal_description needle _exptl_crystal_F_000 972 _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.01 _refine_diff_density_max 1.557 _refine_diff_density_min -0.858 _refine_diff_density_rms 0.147 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 141 _refine_ls_number_reflns 1799 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.012 _refine_ls_R_factor_all 0.1678 _refine_ls_R_factor_gt 0.0891 _refine_ls_shift/su_max 0.029 _refine_ls_shift/su_mean 0.002 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1274P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2017 _refine_ls_wR_factor_ref 0.2397 _reflns_Friedel_coverage 0.000 _reflns_number_gt 943 _reflns_number_total 1799 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1dt01069g2.cif _cod_data_source_block 210105_pyterpycoclhs_2 _cod_depositor_comments 'Adding full bibliography for 7707184--7707187.cif.' _cod_database_code 7707185 _shelx_shelxl_version_number 2014/7 _chemical_oxdiff_formula 'Co N C H O' _chemical_oxdiff_usercomment '250 K' _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_estimated_absorpt_t_max 0.987 _shelx_estimated_absorpt_t_min 0.560 _diffrn_oxdiff_ac4_digest_frames ; 019c3d8ba86c467764afb6ecd4f735051400744b4cc ; _diffrn_oxdiff_ac4_digest_hkl ; 018967a02be97c3c7867138772e9eea4805069 ; _reflns_odcompleteness_completeness 98.86 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 26.32 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All O(H,H) groups 2. Others Fixed Sof: H2A(0.5) H2B(0.5) H1A(0.5) H1B(0.5) 3.a Free rotating group: O2(H2A,H2B), O1(H1A,H1B) 3.b Aromatic/amide H refined with riding coordinates: C7(H7), C4(H4), C3(H3), C10(H10), C2(H2), C11(H11), C1(H1) ; _shelx_res_file ; 210105_pyterpycoclhs_2.res created by SHELXL-2014/7 TITL 210105_pyterpycoclhs_2_a.res in Pcca REM Old TITL 210105_pyterpyCoClHS_2 in Pcca REM SHELXT solution in Pcca REM R1 0.280, Rweak 0.028, Alpha 0.062, Orientation as input REM Formula found by SHELXT: C20 N5 O3 Co CELL 0.71073 10.7848 7.5554 21.5267 90 90 90 ZERR 4 0.0018 0.0018 0.0036 0 0 0 LATT 1 SYMM 0.5-X,-Y,+Z SYMM -X,+Y,0.5-Z SYMM 0.5+X,-Y,0.5-Z SFAC C H Cl Co N O UNIT 80 72 8 4 16 8 L.S. 30 0 0 PLAN 5 SIZE 0.5 0.1 0.01 TEMP -23.15 CONF list 4 MORE -1 BOND $H fmap 2 53 acta REM REM REM WGHT 0.127400 FVAR 0.30425 CO1 4 0.750000 0.500000 0.366254 10.50000 0.02922 0.06121 = 0.03270 0.00000 0.00000 0.00268 CL00 3 0.886704 0.751849 0.371074 11.00000 0.03597 0.06397 = 0.04368 -0.00224 -0.00096 -0.00155 N2 5 0.750000 0.500000 0.457651 10.50000 0.02804 0.05641 = 0.04205 0.00000 0.00000 0.01235 N3 5 0.750000 0.500000 0.771796 10.50000 0.02530 0.05924 = 0.03652 0.00000 0.00000 0.00274 N1 5 0.604626 0.665673 0.387899 11.00000 0.03768 0.04917 = 0.03123 -0.00618 0.00142 -0.00015 C5 1 0.582939 0.683675 0.446368 11.00000 0.02837 0.03804 = 0.04037 0.00391 -0.00348 -0.00461 C9 1 0.750000 0.500000 0.646175 10.50000 0.02505 0.05631 = 0.03773 0.00000 0.00000 -0.00252 C7 1 0.665247 0.593394 0.547865 11.00000 0.02802 0.04548 = 0.03883 -0.00575 -0.00080 -0.00356 AFIX 43 H7 2 0.604823 0.660252 0.568835 11.00000 -1.20000 AFIX 0 C8 1 0.750000 0.500000 0.580218 10.50000 0.02604 0.05698 = 0.03030 0.00000 0.00000 0.00617 C6 1 0.667671 0.590337 0.486277 11.00000 0.02652 0.04797 = 0.04061 0.00181 0.00239 -0.00493 C4 1 0.490769 0.783077 0.468094 11.00000 0.03349 0.05660 = 0.04490 0.00337 0.00452 -0.00176 AFIX 43 H4 2 0.476105 0.791968 0.511025 11.00000 -1.20000 AFIX 0 C3 1 0.420121 0.869256 0.427802 11.00000 0.04048 0.05752 = 0.05122 0.00046 -0.00180 -0.00077 AFIX 43 H3 2 0.354404 0.940640 0.441769 11.00000 -1.20000 AFIX 0 C10 1 0.832388 0.411749 0.679236 11.00000 0.04636 0.09489 = 0.03299 -0.00054 0.00538 0.02617 AFIX 43 H10 2 0.894366 0.345930 0.659013 11.00000 -1.20000 AFIX 0 C2 1 0.443098 0.853679 0.367954 11.00000 0.03360 0.04941 = 0.05569 -0.00033 -0.00796 0.00417 AFIX 43 H2 2 0.395387 0.916301 0.338759 11.00000 -1.20000 AFIX 0 C11 1 0.828471 0.415165 0.739485 11.00000 0.05768 0.09730 = 0.03693 0.01265 -0.00157 0.02847 AFIX 43 H11 2 0.888743 0.349358 0.760968 11.00000 -1.20000 AFIX 0 C1 1 0.534594 0.748306 0.349329 11.00000 0.03407 0.07174 = 0.03789 0.00987 -0.00527 -0.00715 AFIX 43 H1 2 0.548476 0.733817 0.306521 11.00000 -1.20000 AFIX 6 O2 6 0.250000 1.000000 0.537464 10.50000 0.05492 0.06326 = 0.05307 0.00000 0.00000 0.00531 H2A 2 0.207452 1.040397 0.568162 10.50000 -1.50000 H2B 2 0.256051 0.888368 0.544680 10.50000 -1.50000 AFIX 6 O1 6 0.250000 1.000000 0.230095 10.50000 0.11808 0.10741 = 0.08241 0.00000 0.00000 -0.04902 H1A 2 0.203775 0.946445 0.203512 10.50000 -1.50000 H1B 2 0.294031 1.071453 0.208174 10.50000 -1.50000 AFIX 0 HKLF 4 REM 210105_pyterpycoclhs_2_a.res in Pcca REM R1 = 0.0891 for 943 Fo > 4sig(Fo) and 0.1678 for all 1799 data REM 141 parameters refined using 0 restraints END WGHT 0.1272 0.0000 REM Highest difference peak 1.557, deepest hole -0.858, 1-sigma level 0.147 Q1 1 0.7500 0.5000 0.3195 10.50000 0.05 1.56 Q2 1 0.7500 0.5000 0.4161 10.50000 0.05 1.28 Q3 1 0.7451 0.3633 0.3474 11.00000 0.05 0.98 Q4 1 0.7508 0.6486 0.3743 11.00000 0.05 0.93 Q5 1 0.8866 0.8680 0.3969 11.00000 0.05 0.60 ; _shelx_res_checksum 30506 _shelx_hkl_file ; 0 0 -3 3.84 3.44 0 0 -3 0.15 2.38 0 0 3 2.99 2.81 0 0 3 -4.54 3.77 0 0 -3 3.85 3.93 0 0 -4 2552.44 158.26 0 0 -4 2650.48 158.37 0 0 -4 2840.73 158.22 0 0 4 2684.71 158.13 0 0 5 11.60 4.99 0 0 -5 -6.55 5.96 0 0 -5 9.32 7.35 0 0 -5 18.72 8.09 0 0 -6 43.68 7.43 0 0 -6 43.91 7.75 0 0 -6 34.44 6.41 0 0 6 35.25 5.88 0 0 7 6.62 5.06 0 0 -7 0.79 6.58 0 0 -7 2.47 6.22 0 0 -7 3.95 5.34 0 0 -8 2291.28 137.89 0 0 -8 2397.72 137.59 0 0 -8 2261.66 137.82 0 0 8 2292.22 137.50 0 0 9 3.20 4.81 0 0 9 1.56 5.38 0 0 -9 12.80 7.67 0 0 -9 6.57 5.83 0 0 -9 15.95 7.30 0 0 10 2308.60 137.02 0 0 10 2560.82 137.59 0 0 -10 2492.09 138.09 0 0 -10 2612.15 137.02 0 0 -10 2432.75 138.01 0 0 -10 2587.30 137.63 0 0 -11 11.72 6.13 0 0 11 -4.01 5.42 0 0 -11 11.53 6.82 0 0 -11 25.20 9.04 0 0 11 -4.65 6.21 0 0 -11 17.91 9.10 0 0 -12 1422.60 92.43 0 0 -12 1558.70 92.03 0 0 -12 1636.67 91.59 0 0 12 1372.97 91.12 0 0 -12 1501.01 92.57 0 0 12 1611.74 92.05 0 0 -13 9.26 7.02 0 0 -13 12.24 8.87 0 0 -13 19.27 8.83 0 0 -13 9.42 6.73 0 0 13 3.88 6.29 0 0 -14 97.84 12.39 0 0 -14 94.93 12.65 0 0 -14 97.60 10.74 0 0 -14 91.61 11.06 0 0 -15 -1.65 7.05 0 0 -15 4.79 9.50 0 0 -15 8.79 9.33 0 0 -15 26.69 7.99 0 0 -16 440.55 33.35 0 0 -16 471.52 33.56 0 0 -16 486.55 32.28 0 0 -17 29.28 9.22 0 0 -17 17.10 10.95 0 0 -17 14.59 11.67 0 0 -18 182.19 16.90 0 0 -18 146.45 18.60 0 0 -18 182.95 19.22 0 0 -19 40.59 13.73 0 0 -19 8.62 13.23 0 0 -20 154.10 18.83 0 0 -20 130.41 18.84 0 0 -21 3.96 14.67 0 0 -22 177.96 21.95 0 0 -23 14.22 16.00 0 0 -24 -4.76 17.31 0 0 -25 -5.02 17.44 0 0 -26 12.39 18.71 -1 0 1 -0.14 1.70 1 0 -1 -0.07 1.77 -1 0 -1 3.32 3.39 -1 0 -2 2329.03 128.25 1 0 -2 2050.61 128.04 -1 0 2 1845.03 127.99 1 0 -2 2013.63 128.62 1 0 3 1.08 3.05 1 0 -3 -1.60 4.22 -1 0 -3 -1.77 2.63 1 0 -3 -2.93 4.31 1 0 3 2.16 2.90 -1 0 -3 2.91 4.67 1 0 4 9.88 4.42 1 0 -4 -1.93 5.55 -1 0 4 1.20 5.82 1 0 -4 11.65 6.15 1 0 4 5.78 6.13 -1 0 -4 8.34 5.94 1 0 -4 4.82 3.09 -1 0 4 3.94 3.20 -1 0 -4 -10.45 7.70 -1 0 -4 5.33 4.87 1 0 -4 -8.39 6.57 1 0 5 20.72 4.86 -1 0 5 -0.17 5.38 1 0 -5 -12.21 3.78 -1 0 -5 8.54 5.78 -1 0 -5 4.43 4.90 1 0 -5 0.71 6.97 -1 0 5 -4.81 4.93 -1 0 5 6.55 3.09 -1 0 -5 -16.39 7.76 1 0 -5 5.25 5.51 1 0 5 17.34 6.66 1 0 -5 21.63 7.23 1 0 6 1056.45 59.58 1 0 -6 984.17 60.38 -1 0 6 1012.70 60.01 -1 0 6 942.62 58.99 -1 0 -6 1055.07 59.53 1 0 -6 955.37 60.13 1 0 6 1016.17 59.97 -1 0 -6 925.05 60.29 -1 0 6 994.88 60.45 -1 0 -6 988.56 60.15 -1 0 -7 -1.52 4.75 -1 0 7 2.46 5.64 1 0 7 -0.18 5.66 1 0 -7 2.74 6.23 -1 0 7 0.64 5.51 1 0 -7 11.15 5.55 -1 0 7 8.56 6.34 -1 0 -7 3.96 5.59 1 0 7 -4.51 4.88 -1 0 -7 -3.54 6.68 -1 0 7 8.66 3.35 -1 0 -8 149.59 11.89 -1 0 -8 127.34 12.17 -1 0 8 135.83 11.58 -1 0 -8 136.19 11.58 -1 0 8 148.46 12.01 1 0 8 130.71 11.52 1 0 -8 131.36 11.66 -1 0 8 128.57 9.69 1 0 -8 132.27 12.44 -1 0 -8 140.72 10.85 -1 0 8 133.22 11.62 1 0 -8 133.97 11.96 1 0 8 120.76 10.69 -1 0 -9 6.01 6.23 -1 0 -9 0.56 5.95 -1 0 9 -5.04 7.09 -1 0 9 10.17 4.11 1 0 9 -5.59 6.91 1 0 -9 -5.34 7.83 1 0 -9 1.86 6.31 -1 0 -9 -1.88 7.68 1 0 -9 6.92 7.40 -1 0 -9 8.40 6.88 -1 0 9 5.31 6.11 1 0 9 -5.63 5.28 -1 0 9 11.65 7.29 -1 0 10 3593.78 200.82 -1 0 10 3634.81 201.34 1 0 10 3292.64 200.17 -1 0 10 3486.02 200.67 1 0 -10 3242.62 200.99 -1 0 -10 3373.31 201.23 -1 0 -10 3539.79 200.77 1 0 10 3518.57 200.89 -1 0 10 3119.40 199.47 1 0 -10 3304.80 201.00 -1 0 -10 3434.65 200.20 -1 0 -10 3314.85 200.88 1 0 -10 3343.93 201.51 -1 0 -11 1.93 6.60 1 0 -11 9.20 8.90 -1 0 -11 13.82 8.82 1 0 -11 -9.80 7.30 1 0 11 -1.69 5.56 -1 0 11 1.98 4.32 1 0 -11 -7.82 9.11 1 0 11 -12.65 8.78 -1 0 11 4.20 6.68 -1 0 -11 -3.64 9.04 -1 0 -11 -5.89 7.14 1 0 -12 58.01 10.79 1 0 -12 53.14 9.30 -1 0 12 61.83 9.53 -1 0 -12 48.28 10.40 -1 0 -12 61.16 10.15 1 0 12 52.16 7.88 -1 0 -12 58.97 8.92 -1 0 -12 40.72 8.59 1 0 -12 70.80 11.01 1 0 -13 1.48 7.24 -1 0 -13 -0.79 8.87 -1 0 -13 0.37 7.95 -1 0 -13 -2.60 6.91 1 0 -13 1.24 8.64 -1 0 -13 -4.24 7.30 1 0 -13 3.80 8.71 -1 0 -14 317.45 22.51 1 0 -14 304.45 24.23 1 0 -14 304.19 24.09 1 0 -14 312.73 23.29 -1 0 -14 321.22 24.61 -1 0 -14 312.21 23.09 1 0 -15 10.09 9.97 1 0 -15 15.84 10.02 -1 0 -15 -1.13 7.50 -1 0 -15 6.11 10.12 -1 0 -15 -1.64 8.01 1 0 -15 7.03 7.91 -1 0 -16 101.41 12.41 -1 0 -16 73.80 13.75 1 0 -16 108.55 12.37 1 0 -16 79.40 13.86 -1 0 -16 82.21 11.49 1 0 -16 77.83 13.33 -1 0 -17 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13.92 1 8 0 18.97 11.74 -1 8 0 21.73 10.53 1 8 -1 -1.47 11.32 1 8 1 22.85 11.86 -1 8 -1 11.57 9.94 -1 8 1 20.34 9.98 1 8 -2 35.14 13.39 1 8 2 42.44 12.30 -1 8 -2 28.20 11.72 -1 8 2 45.60 10.91 1 8 -3 4.74 12.54 -1 8 -3 25.09 11.03 1 8 3 14.19 10.29 -1 8 -4 18.27 10.89 1 8 4 7.69 9.63 1 8 -4 14.67 12.48 -1 8 -5 -13.56 11.34 1 8 -5 17.02 13.02 1 8 5 17.74 10.02 -1 8 -6 21.88 12.31 1 8 -6 55.36 15.07 -1 8 -7 0.80 11.41 1 8 -7 27.07 14.53 -1 8 -8 5.77 11.63 1 8 -8 15.73 13.73 -1 8 -9 9.36 12.51 1 8 -9 -6.57 13.36 -1 8 -10 27.71 13.61 1 8 -10 35.54 15.11 -1 8 -11 -1.76 12.26 1 8 -11 17.37 14.23 -1 8 -12 3.67 13.31 1 8 -12 -3.87 13.03 -1 8 -13 -8.43 13.62 1 8 -13 -6.78 13.97 1 8 -14 4.83 13.84 -1 8 -14 -11.55 14.03 -2 8 0 18.80 10.68 2 8 0 32.46 14.70 -2 8 -1 -0.68 10.05 2 8 -1 7.11 13.73 2 8 1 7.32 12.51 2 8 2 14.00 13.19 -2 8 -2 0.70 10.30 2 8 -2 10.13 15.41 2 8 3 16.33 11.83 -2 8 -3 -3.56 10.53 2 8 -3 9.48 14.76 2 8 -4 -1.93 15.01 -2 8 -4 -4.40 10.49 2 8 4 15.64 11.95 2 8 -5 19.64 15.49 -2 8 -5 2.25 10.80 2 8 5 9.59 11.60 2 8 -6 6.90 14.37 -2 8 -6 -12.98 11.04 2 8 6 -5.29 11.26 -2 8 -7 -12.59 11.91 2 8 -7 7.02 14.45 -2 8 -8 -9.63 11.14 2 8 -8 22.19 15.75 -2 8 -9 -9.08 11.69 2 8 -9 -12.13 14.08 -2 8 -10 -12.95 12.77 2 8 -10 13.08 14.54 -2 8 -11 -14.30 13.18 2 8 -11 16.13 15.00 2 -8 -12 10.81 24.09 2 8 -12 8.11 14.79 -2 8 -12 4.56 12.59 2 -8 -13 -40.40 25.59 2 8 -13 -6.03 14.23 -2 8 -13 -16.95 13.92 3 8 0 -5.35 17.05 3 8 -1 24.45 18.30 -3 8 -1 -18.35 11.78 3 8 1 1.02 15.59 -3 8 -2 -10.35 11.33 3 8 2 5.87 14.92 3 8 -2 6.85 17.46 -3 8 -3 -4.48 11.40 3 8 -3 18.65 18.43 3 8 3 -4.64 15.01 -3 8 -4 -3.76 11.05 3 8 4 2.66 13.91 3 8 -4 9.39 18.32 -3 8 -5 -3.82 11.10 3 8 -5 25.75 19.01 3 8 5 11.82 13.81 -3 8 -6 -12.68 11.69 3 8 -6 19.63 18.07 -3 8 -7 -6.53 11.65 3 8 -7 3.40 17.62 3 8 7 11.83 12.50 3 8 -8 20.98 16.61 -3 8 -8 -11.65 12.17 3 -8 -9 -5.58 22.33 3 8 -9 1.09 15.28 -3 8 -9 -14.60 12.42 3 -8 -10 -13.66 23.20 3 8 -10 -3.22 14.86 -3 8 -10 -10.51 12.00 3 -8 -11 -4.65 23.14 3 8 -11 26.38 16.16 3 -8 -12 1.19 23.58 3 8 -12 5.21 14.72 4 8 0 9.10 19.84 4 8 1 -13.72 20.12 4 8 -1 37.67 22.56 4 8 -2 2.75 20.75 4 8 2 -10.64 17.97 4 8 -3 1.39 20.54 -4 8 -3 -14.65 12.49 4 8 4 -4.26 17.03 4 8 -4 2.76 20.71 -4 8 -4 -16.46 12.40 4 8 5 7.06 15.87 4 8 -5 19.04 22.45 -4 8 -5 -5.78 11.53 4 8 -6 14.53 20.15 4 8 6 -19.24 15.03 -4 8 -6 -9.11 11.90 4 8 -7 16.57 19.61 4 8 -8 1.22 18.36 4 8 -9 -1.17 17.62 4 -8 -10 21.32 23.45 4 8 -10 39.15 17.03 4 -8 -11 20.70 23.08 4 8 -11 26.22 17.16 5 8 0 8.54 21.59 5 8 -1 5.92 22.61 5 8 -2 33.18 23.24 5 8 2 -18.19 20.23 5 8 -3 18.19 23.79 5 8 3 -12.26 19.67 5 8 -4 1.50 22.18 5 8 4 -23.21 18.46 5 8 -5 22.05 22.51 5 8 -6 -4.26 21.64 5 8 -7 -5.45 20.33 5 8 -8 19.46 21.20 5 8 -9 -1.23 19.25 5 8 -10 3.52 17.60 6 8 1 5.36 19.90 6 8 2 -15.35 20.33 6 8 -2 -7.41 22.44 6 8 -3 11.97 23.20 6 8 -4 22.37 22.71 6 8 -5 -10.29 23.19 6 8 -6 -7.14 21.54 6 8 -7 6.87 21.17 7 8 0 -23.26 20.93 7 8 1 26.13 21.25 7 8 -1 5.36 20.07 7 8 -3 13.92 21.75 0 9 0 33.01 11.08 0 9 -1 20.40 11.00 0 9 1 15.41 9.95 0 9 -2 -1.48 10.27 0 9 -3 13.97 11.27 0 9 -4 22.12 12.22 0 9 -5 5.15 12.02 0 9 -6 6.33 12.56 0 9 -7 -4.68 13.16 0 9 -8 9.72 13.89 1 9 0 0.73 11.32 -1 9 0 16.10 10.54 1 9 -1 10.70 11.32 1 9 1 7.00 11.02 -1 9 -1 11.80 10.28 1 9 2 4.02 10.58 -1 9 -2 5.10 10.48 1 9 -2 26.03 12.42 -1 9 -3 -9.87 11.00 1 9 -3 10.23 12.79 -1 9 -4 14.94 11.98 1 9 -4 26.06 13.97 -1 9 -5 -12.22 12.32 1 9 -5 5.65 13.12 -1 9 -6 2.55 11.90 1 9 -6 16.65 13.94 -1 9 -7 -16.67 13.35 1 9 -7 5.10 14.22 2 9 0 41.68 15.23 2 9 -1 65.44 16.87 2 9 1 40.56 14.70 2 9 -2 9.52 15.29 -2 9 -2 1.49 11.00 2 9 2 22.12 13.20 2 9 -3 30.78 16.46 -2 9 -3 12.19 11.60 2 9 3 15.91 12.55 -2 9 -4 1.57 11.35 2 9 4 15.25 12.40 2 9 -4 42.07 16.33 -2 9 -5 -11.23 12.23 2 9 -5 26.89 16.18 -2 9 -6 -5.80 12.22 2 9 -6 20.97 16.92 -2 9 -7 -17.81 12.48 2 9 -7 28.36 17.39 3 9 0 7.47 16.32 3 9 -1 -8.91 17.13 3 9 1 25.38 16.30 3 9 -2 11.59 17.93 3 9 2 20.36 16.25 3 9 3 9.27 14.71 3 9 -3 21.56 18.67 -3 9 -4 -9.12 12.51 3 9 -4 -2.45 18.66 3 9 4 3.56 14.27 -3 9 -5 -4.21 12.38 3 9 -5 -5.01 19.39 3 9 5 -2.57 13.43 4 9 0 45.10 21.34 4 9 1 32.09 21.03 4 9 -1 -1.34 20.91 0 0 0 0.00 0.00 TITL 210105_pyterpyCoClHS_2 in Pcca REM Pcca (#54, found as Pccb in ba-c setting) CELL 0.71073 10.784773 7.555438 21.526691 90.0000 90.0000 90.0000 ZERR 25.00 0.001798 0.001839 0.003567 0.0000 0.0000 0.0000 LATT 1 SYMM -x+1/2,-y, z SYMM -x, y,-z+1/2 SYMM x+1/2,-y,-z+1/2 SFAC C H N O Co UNIT 25.00 25.00 25.00 25.00 25.00 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 50926 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 2.732 _oxdiff_exptl_absorpt_empirical_full_min 0.586 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z' '-x, y, -z+1/2' 'x+1/2, -y, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z' 'x, -y, z-1/2' '-x-1/2, y, 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 0.7500 0.5000 0.36625(6) 0.0410(5) Uani 1 2 d S T P . . Cl00 Cl 0.88670(19) 0.7518(3) 0.37107(8) 0.0479(7) Uani 1 1 d . . . . . N2 N 0.7500 0.5000 0.4577(4) 0.042(2) Uani 1 2 d S T P . . N3 N 0.7500 0.5000 0.7718(4) 0.040(2) Uani 1 2 d S T P . . N1 N 0.6046(6) 0.6657(9) 0.3879(3) 0.0394(16) Uani 1 1 d . . . . . C5 C 0.5829(7) 0.6837(10) 0.4464(3) 0.0356(18) Uani 1 1 d . . . . . C9 C 0.7500 0.5000 0.6462(5) 0.040(3) Uani 1 2 d S T P . . C7 C 0.6652(7) 0.5934(10) 0.5479(3) 0.0374(18) Uani 1 1 d . . . . . H7 H 0.6048 0.6603 0.5688 0.045 Uiso 1 1 calc R U . . . C8 C 0.7500 0.5000 0.5802(4) 0.038(3) Uani 1 2 d S T P . . C6 C 0.6677(7) 0.5903(11) 0.4863(3) 0.0384(19) Uani 1 1 d . . . . . C4 C 0.4908(7) 0.7831(10) 0.4681(4) 0.045(2) Uani 1 1 d . . . . . H4 H 0.4761 0.7920 0.5110 0.054 Uiso 1 1 calc R U . . . C3 C 0.4201(8) 0.8693(11) 0.4278(4) 0.050(2) Uani 1 1 d . . . . . H3 H 0.3544 0.9406 0.4418 0.060 Uiso 1 1 calc R U . . . C10 C 0.8324(8) 0.4117(12) 0.6792(4) 0.058(3) Uani 1 1 d . . . . . H10 H 0.8944 0.3459 0.6590 0.070 Uiso 1 1 calc R U . . . C2 C 0.4431(7) 0.8537(11) 0.3680(4) 0.046(2) Uani 1 1 d . . . . . H2 H 0.3954 0.9163 0.3388 0.055 Uiso 1 1 calc R U . . . C11 C 0.8285(9) 0.4152(13) 0.7395(4) 0.064(3) Uani 1 1 d . . . . . H11 H 0.8887 0.3494 0.7610 0.077 Uiso 1 1 calc R U . . . C1 C 0.5346(7) 0.7483(12) 0.3493(3) 0.048(2) Uani 1 1 d . . . . . H1 H 0.5485 0.7338 0.3065 0.057 Uiso 1 1 calc R U . . . O2 O 0.2500 1.0000 0.5375(4) 0.057(2) Uani 1 2 d GS T P . . H2A H 0.2075 1.0404 0.5682 0.086 Uiso 0.5 1 d G U P . . H2B H 0.2561 0.8884 0.5447 0.086 Uiso 0.5 1 d G U P . . O1 O 0.2500 1.0000 0.2301(5) 0.103(4) Uani 1 2 d GS T P . . H1A H 0.2038 0.9464 0.2035 0.154 Uiso 0.5 1 d G U P . . H1B H 0.2940 1.0715 0.2082 0.154 Uiso 0.5 1 d G U 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 Co1 0.0292(8) 0.0612(12) 0.0327(8) 0.000 0.000 0.0027(9) Cl00 0.0360(11) 0.0640(15) 0.0437(11) -0.0022(10) -0.0010(8) -0.0015(11) N2 0.028(5) 0.056(6) 0.042(5) 0.000 0.000 0.012(5) N3 0.025(5) 0.059(7) 0.037(5) 0.000 0.000 0.003(5) N1 0.038(4) 0.049(4) 0.031(3) -0.006(3) 0.001(3) 0.000(3) C5 0.028(4) 0.038(5) 0.040(4) 0.004(4) -0.003(3) -0.005(4) C9 0.025(5) 0.056(8) 0.038(6) 0.000 0.000 -0.003(6) C7 0.028(4) 0.045(5) 0.039(4) -0.006(4) -0.001(3) -0.004(4) C8 0.026(5) 0.057(8) 0.030(6) 0.000 0.000 0.006(6) C6 0.027(4) 0.048(5) 0.041(4) 0.002(4) 0.002(3) -0.005(4) C4 0.033(5) 0.057(6) 0.045(4) 0.003(4) 0.005(3) -0.002(4) C3 0.040(5) 0.058(6) 0.051(5) 0.000(5) -0.002(4) -0.001(5) C10 0.046(5) 0.095(8) 0.033(4) -0.001(5) 0.005(4) 0.026(5) C2 0.034(5) 0.049(6) 0.056(5) 0.000(4) -0.008(4) 0.004(4) C11 0.058(6) 0.097(8) 0.037(5) 0.013(5) -0.002(4) 0.028(6) C1 0.034(4) 0.072(6) 0.038(4) 0.010(4) -0.005(3) -0.007(5) O2 0.055(6) 0.063(6) 0.053(5) 0.000 0.000 0.005(6) O1 0.118(11) 0.107(11) 0.082(8) 0.000 0.000 -0.049(8) 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' Cl Cl 0.1484 0.1585 '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' 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' 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 Cl00 Co1 Cl00 175.06(10) . 2_665 ? N2 Co1 Cl00 87.53(5) . 2_665 ? N2 Co1 Cl00 87.53(5) . . ? N2 Co1 N3 180.0 . 7_565 ? N2 Co1 N1 76.93(17) . . ? N2 Co1 N1 76.92(17) . 2_665 ? N3 Co1 Cl00 92.47(5) 7_565 2_665 ? N3 Co1 Cl00 92.47(5) 7_565 . ? N3 Co1 N1 103.08(17) 7_565 2_665 ? N3 Co1 N1 103.07(17) 7_565 . ? N1 Co1 Cl00 90.3(2) . 2_665 ? N1 Co1 Cl00 88.6(2) . . ? N1 Co1 Cl00 90.3(2) 2_665 . ? N1 Co1 Cl00 88.6(2) 2_665 2_665 ? N1 Co1 N1 153.8(3) 2_665 . ? C6 N2 Co1 118.8(5) 2_665 . ? C6 N2 Co1 118.8(5) . . ? C6 N2 C6 122.4(9) . 2_665 ? C11 N3 Co1 123.2(5) 2_665 7_566 ? C11 N3 Co1 123.2(5) . 7_566 ? C11 N3 C11 113.5(9) 2_665 . ? C5 N1 Co1 115.1(5) . . ? C1 N1 Co1 126.6(5) . . ? C1 N1 C5 118.3(7) . . ? N1 C5 C6 114.6(7) . . ? N1 C5 C4 122.6(7) . . ? C4 C5 C6 122.8(7) . . ? C10 C9 C8 122.6(5) 2_665 . ? C10 C9 C8 122.6(5) . . ? C10 C9 C10 114.7(10) 2_665 . ? C8 C7 H7 120.2 . . ? C6 C7 H7 120.2 . . ? C6 C7 C8 119.6(7) . . ? C7 C8 C9 121.1(5) . . ? C7 C8 C9 121.1(5) 2_665 . ? C7 C8 C7 117.8(9) . 2_665 ? N2 C6 C5 114.5(7) . . ? N2 C6 C7 120.3(8) . . ? C7 C6 C5 125.2(7) . . ? C5 C4 H4 120.8 . . ? C3 C4 C5 118.5(8) . . ? C3 C4 H4 120.8 . . ? C4 C3 H3 120.4 . . ? C2 C3 C4 119.2(8) . . ? C2 C3 H3 120.4 . . ? C9 C10 H10 119.8 . . ? C11 C10 C9 120.5(9) . . ? C11 C10 H10 119.8 . . ? C3 C2 H2 120.4 . . ? C3 C2 C1 119.2(8) . . ? C1 C2 H2 120.4 . . ? N3 C11 C10 125.4(9) . . ? N3 C11 H11 117.3 . . ? C10 C11 H11 117.3 . . ? N1 C1 C2 122.2(7) . . ? N1 C1 H1 118.9 . . ? C2 C1 H1 118.9 . . ? H2A O2 H2B 104.5 . . ? H1A O1 H1B 104.5 . . ? 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 Cl00 2.409(2) 2_665 ? Co1 Cl00 2.409(2) . ? Co1 N2 1.967(8) . ? Co1 N3 2.033(8) 7_565 ? Co1 N1 2.060(6) 2_665 ? Co1 N1 2.060(6) . ? N2 C6 1.278(8) . ? N2 C6 1.278(8) 2_665 ? N3 Co1 2.033(8) 7_566 ? N3 C11 1.269(9) 2_665 ? N3 C11 1.269(9) . ? N1 C5 1.287(8) . ? N1 C1 1.284(9) . ? C5 C6 1.439(10) . ? C5 C4 1.331(10) . ? C9 C8 1.420(13) . ? C9 C10 1.319(9) . ? C9 C10 1.319(9) 2_665 ? C7 H7 0.9400 . ? C7 C8 1.348(9) . ? C7 C6 1.326(9) . ? C8 C7 1.349(9) 2_665 ? C4 H4 0.9400 . ? C4 C3 1.325(10) . ? C3 H3 0.9400 . ? C3 C2 1.317(10) . ? C10 H10 0.9400 . ? C10 C11 1.298(10) . ? C2 H2 0.9400 . ? C2 C1 1.330(11) . ? C11 H11 0.9400 . ? C1 H1 0.9400 . ? O2 H2A 0.8605 . ? O2 H2B 0.8601 . ? O1 H1A 0.8601 . ? O1 H1B 0.8600 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Co1 N2 C6 C5 -0.1(7) . . . . ? Co1 N2 C6 C7 -179.9(5) . . . . ? Co1 N3 C11 C10 -179.7(8) 7_566 . . . ? Co1 N1 C5 C6 2.5(9) . . . . ? Co1 N1 C5 C4 -178.6(6) . . . . ? Co1 N1 C1 C2 -179.6(6) . . . . ? N1 C5 C6 N2 -1.6(10) . . . . ? N1 C5 C6 C7 178.2(8) . . . . ? N1 C5 C4 C3 -1.2(12) . . . . ? C5 N1 C1 C2 1.5(12) . . . . ? C5 C4 C3 C2 0.1(13) . . . . ? C9 C10 C11 N3 -0.5(16) . . . . ? C8 C9 C10 C11 -179.8(7) . . . . ? C8 C7 C6 N2 -0.2(11) . . . . ? C8 C7 C6 C5 180.0(6) . . . . ? C6 N2 C6 C5 179.9(7) 2_665 . . . ? C6 N2 C6 C7 0.1(5) 2_665 . . . ? C6 C5 C4 C3 177.6(7) . . . . ? C6 C7 C8 C9 -179.9(5) . . . . ? C6 C7 C8 C7 0.1(5) . . . 2_665 ? C4 C5 C6 N2 179.5(7) . . . . ? C4 C5 C6 C7 -0.8(13) . . . . ? C4 C3 C2 C1 1.7(13) . . . . ? C3 C2 C1 N1 -2.6(13) . . . . ? C10 C9 C8 C7 0.8(6) 2_665 . . . ? C10 C9 C8 C7 0.8(6) . . . 2_665 ? C10 C9 C8 C7 -179.2(6) . . . . ? C10 C9 C8 C7 -179.2(6) 2_665 . . 2_665 ? C10 C9 C10 C11 0.2(7) 2_665 . . . ? C11 N3 C11 C10 0.3(8) 2_665 . . . ? C1 N1 C5 C6 -178.5(7) . . . . ? C1 N1 C5 C4 0.5(12) . . . . ?