#------------------------------------------------------------------------------ #$Date: 2020-10-06 10:13:18 +0300 (Tue, 06 Oct 2020) $ #$Revision: 257329 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/78/1557898.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_1557898 loop_ _publ_author_name 'Das, Sandip' Kulbir, 'Ghosh, Somnath' 'Chandra Sahoo, Subash' 'Kumar, Pankaj' _publ_section_title ; Nitric oxide monooxygenation (NOM) reaction of cobalt-nitrosyl {Co(NO)}8 to CoII-nitrito {CoII(NO2−)}: base induced hydrogen gas (H2) evolution ; _journal_issue 19 _journal_name_full 'Chemical Science' _journal_page_first 5037 _journal_page_last 5042 _journal_paper_doi 10.1039/D0SC01572E _journal_volume 11 _journal_year 2020 _chemical_compound_source synthesized _chemical_formula_moiety 'C12 H28 Co N5 O2, B F4' _chemical_formula_sum 'C12 H28 B Co F4 N5 O2' _chemical_formula_weight 420.13 _space_group_crystal_system orthorhombic _space_group_IT_number 61 _space_group_name_Hall '-P 2ac 2ab' _space_group_name_H-M_alt 'P b c a' _atom_sites_solution_hydrogens geom _audit_creation_date 2019-12-28 _audit_creation_method ; Olex2 1.2-ac3 (compiled 2017.02.24 svn.r3390 for Rigaku Oxford Diffraction, GUI svn.r5318) ; _audit_update_record ; 2019-12-28 deposited with the CCDC. 2020-04-24 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 13.0883(2) _cell_length_b 14.8329(3) _cell_length_c 19.5325(3) _cell_measurement_reflns_used 30109 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 27.3180 _cell_measurement_theta_min 3.3190 _cell_volume 3791.99(11) _computing_cell_refinement 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_data_collection 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_data_reduction 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 293(2) _diffrn_detector 'CCD plate' _diffrn_detector_type HyPix3000 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.977 _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 7.00 56.00 0.50 15.00 -- -9.95 30.00 154.00 98 2 \w -48.00 -20.00 0.50 15.00 -- -9.95 -30.00 -5.00 56 3 \w -56.00 -11.00 0.50 15.00 -- 10.22 -30.00 -5.00 90 4 \w 35.00 61.00 0.50 15.00 -- 10.22 30.00 154.00 52 5 \w -56.00 -19.00 0.50 15.00 -- -9.95 125.00 120.00 74 6 \w -58.00 -23.00 0.50 15.00 -- -9.95 125.00 -90.00 70 7 \w -73.00 -27.00 0.50 15.00 -- -9.95 -57.00 60.00 92 8 \w -47.00 -22.00 0.50 15.00 -- -9.95 125.00 0.00 50 9 \w -49.00 7.00 0.50 15.00 -- -9.95 -57.00 -30.00 112 10 \w -49.00 -23.00 0.50 15.00 -- -9.95 125.00-120.00 52 11 \w -30.00 1.00 0.50 15.00 -- 10.22 121.00 147.94 62 12 \w -33.00 0.00 0.50 15.00 -- 10.22 118.00-135.82 66 13 \w 49.00 74.00 0.50 15.00 -- 10.22 38.00 -60.00 50 14 \w -37.00 -5.00 0.50 15.00 -- 10.22 124.00 -37.75 64 15 \w -60.00 22.00 0.50 15.00 -- 10.22 -19.00-150.00 164 16 \w 5.00 36.00 0.50 15.00 -- 10.22 38.00 -60.00 62 17 \w -2.00 77.00 0.50 15.00 -- 10.22 19.00 30.00 158 18 \w -5.00 56.00 0.50 15.00 -- 10.22 57.00 150.00 122 19 \w -9.00 40.00 0.50 15.00 -- 10.22 -99.00-150.00 98 20 \w -32.00 -2.00 0.50 15.00 -- 10.22 116.00 71.85 60 21 \w 8.00 43.00 0.50 15.00 -- 10.22 -99.00 -90.00 70 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Single source at offset/far, HyPix3000' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0196854000 _diffrn_orient_matrix_UB_12 0.0442373000 _diffrn_orient_matrix_UB_13 0.0038917000 _diffrn_orient_matrix_UB_21 0.0459669000 _diffrn_orient_matrix_UB_22 -0.0179698000 _diffrn_orient_matrix_UB_23 0.0135951000 _diffrn_orient_matrix_UB_31 0.0209650000 _diffrn_orient_matrix_UB_32 -0.0021481000 _diffrn_orient_matrix_UB_33 -0.0334459000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0394 _diffrn_reflns_av_unetI/netI 0.0168 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.977 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_number 57112 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.977 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.390 _diffrn_reflns_theta_min 3.325 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 0.958 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.70839 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour red _exptl_crystal_density_diffrn 1.472 _exptl_crystal_description block _exptl_crystal_F_000 1752 _exptl_crystal_recrystallization_method 'slow evaporation' _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.05 _refine_diff_density_max 0.698 _refine_diff_density_min -0.397 _refine_diff_density_rms 0.072 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.129 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 302 _refine_ls_number_reflns 4208 _refine_ls_number_restraints 72 _refine_ls_restrained_S_all 1.177 _refine_ls_R_factor_all 0.0792 _refine_ls_R_factor_gt 0.0623 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0964P)^2^+3.7491P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1908 _refine_ls_wR_factor_ref 0.2051 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3007 _reflns_number_total 4208 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; TITL sub-pankj-sd12_a.res in Pbca sub-pankj-sd12.res created by SHELXL-2018/3 at 20:17:59 on 28-Dec-2019 REM Old TITL sub-Pankj-SD12 in Pbca REM SHELXT solution in Pbca REM R1 0.190, Rweak 0.002, Alpha 0.040, Orientation as input REM Formula found by SHELXT: C15 N4 O F4 Co CELL 0.71073 13.0883 14.8329 19.5325 90 90 90 ZERR 8 0.0002 0.0003 0.0003 0 0 0 LATT 1 SYMM 0.5-X,-Y,0.5+Z SYMM -X,0.5+Y,0.5-Z SYMM 0.5+X,0.5-Y,-Z SFAC C H B Co F N O UNIT 96 224 8 8 32 40 16 RIGU 0.00005 0.00005 C2 C3 C5 C6 C8 C9 C11 C12 N3 C6 N3 C8 N2 C3 N2 C5 N4 C9 = N4 C11 N1 C2 N1 C12 C6 C5 C6 C9 C8 C3 C2 C5 C12 C11 C11 C12 C2 C3 C9 C11 C2 = C9 C11 C11 C8 C9 C5 C6 RIGU 0.0001 0.0001 C2A C3A C5A C6A C8A C9A C11A C12A N3 C6A N3 C8A N2 C3A N2 = C5A N4 C9A N4 C11A N1 C2A N1 C12A C6A C5A C9A C8A C3A C2A C5A C12A C11A C11A = C12A C2A C3A C12A C8A C9A C11A C9A C11A C9A C11A C8A C5A C6A L.S. 22 PLAN 20 BOND $H LIST 6 fmap 2 acta REM REM REM WGHT 0.096400 3.749100 FVAR 0.29472 CO1 4 0.360727 0.749710 0.629593 11.00000 0.03573 0.04357 = 0.04328 0.00532 0.00240 0.00108 N3 6 0.470913 0.651369 0.594361 11.00000 0.06347 0.07226 = 0.08309 -0.00735 0.00533 0.00320 N5 6 0.173230 0.689356 0.633071 11.00000 0.04974 0.10724 = 0.09240 0.00847 0.01300 -0.01334 N2 6 0.443851 0.728943 0.725176 11.00000 0.08568 0.07907 = 0.06296 -0.00044 -0.01288 0.00153 F1 5 0.285539 0.356334 0.866464 11.00000 0.12353 0.09677 = 0.15185 -0.01891 0.01065 0.02388 N4 6 0.396807 0.808008 0.530962 11.00000 0.07090 0.09385 = 0.06866 0.01285 -0.00025 -0.00907 O2 7 0.248564 0.652097 0.653265 11.00000 0.07689 0.09676 = 0.19518 0.04063 -0.00071 -0.02081 N1 6 0.374317 0.887780 0.661853 11.00000 0.08889 0.05589 = 0.09094 -0.00744 0.00054 0.00735 O1 7 0.195566 0.763540 0.612180 11.00000 0.06799 0.14190 = 0.15677 0.04826 -0.00519 -0.00237 F3 5 0.157010 0.440867 0.893176 11.00000 0.09119 0.17922 = 0.20152 0.00792 0.00648 0.04956 F2 5 0.290589 0.432794 0.959579 11.00000 0.20160 0.24151 = 0.10920 -0.02587 -0.03529 -0.03306 F4 5 0.302364 0.502179 0.861481 11.00000 0.28658 0.12634 = 0.20149 0.03182 0.10116 -0.05278 C10 1 0.310177 0.811616 0.483584 11.00000 0.11586 0.14255 = 0.06685 0.03292 -0.02715 -0.02219 AFIX 137 H10A 2 0.285757 0.751626 0.475071 11.00000 -1.50000 H10B 2 0.331601 0.838518 0.441250 11.00000 -1.50000 H10C 2 0.256388 0.847070 0.503375 11.00000 -1.50000 AFIX 0 B1 3 0.259158 0.436588 0.893592 11.00000 0.06917 0.07128 = 0.07245 -0.00587 -0.00169 0.00389 C1 1 0.277952 0.925121 0.690030 11.00000 0.14784 0.08204 = 0.13547 -0.01588 0.02233 0.05243 AFIX 137 H1A 2 0.229037 0.932039 0.653785 11.00000 -1.50000 H1B 2 0.291237 0.982757 0.710540 11.00000 -1.50000 H1C 2 0.251217 0.884732 0.724000 11.00000 -1.50000 AFIX 0 C7 1 0.427658 0.563058 0.578617 11.00000 0.09825 0.07305 = 0.13568 -0.03882 0.01379 0.00415 AFIX 137 H7A 2 0.398696 0.537461 0.619374 11.00000 -1.50000 H7B 2 0.480477 0.524130 0.561615 11.00000 -1.50000 H7C 2 0.375357 0.569506 0.544509 11.00000 -1.50000 AFIX 0 C4 1 0.389794 0.682565 0.778713 11.00000 0.16707 0.16424 = 0.05979 0.04584 -0.00657 -0.00597 AFIX 137 H4A 2 0.326319 0.712823 0.787577 11.00000 -1.50000 H4B 2 0.430564 0.682257 0.819569 11.00000 -1.50000 H4C 2 0.376405 0.621651 0.764738 11.00000 -1.50000 AFIX 0 PART 1 C2 1 0.459300 0.895501 0.701540 10.60000 0.16469 0.06738 = 0.08874 -0.01526 -0.00834 -0.03856 AFIX 23 H2A 2 0.461834 0.954926 0.722201 10.60000 -1.20000 H2B 2 0.520073 0.887577 0.673762 10.60000 -1.20000 AFIX 0 PART 0 PART 2 C2A 1 0.437633 0.879518 0.737038 10.40000 0.09158 0.07912 = 0.09304 -0.00085 -0.00192 0.00058 AFIX 23 H2AA 2 0.474872 0.935032 0.745185 10.40000 -1.20000 H2AB 2 0.388566 0.872177 0.773836 10.40000 -1.20000 AFIX 0 PART 0 PART 1 C3 1 0.455311 0.822773 0.757702 10.60000 0.10129 0.11932 = 0.05763 -0.02930 -0.02613 -0.00288 AFIX 23 H3A 2 0.517458 0.824912 0.784710 10.60000 -1.20000 H3B 2 0.397996 0.834333 0.787937 10.60000 -1.20000 AFIX 0 PART 0 PART 2 C3A 1 0.507214 0.805968 0.738098 10.40000 0.08850 0.08058 = 0.09107 -0.00658 -0.01175 0.00004 AFIX 23 H3AA 2 0.540613 0.801142 0.782279 10.40000 -1.20000 H3AB 2 0.558839 0.812581 0.702823 10.40000 -1.20000 AFIX 0 PART 0 PART 1 C5 1 0.544076 0.694541 0.705280 10.60000 0.05463 0.16554 = 0.08644 0.03199 -0.02436 0.00993 AFIX 23 H5A 2 0.583824 0.743113 0.685372 10.60000 -1.20000 H5B 2 0.579808 0.673464 0.745736 10.60000 -1.20000 AFIX 0 PART 0 PART 2 C5A 1 0.516237 0.651056 0.711332 10.40000 0.08648 0.07658 = 0.08418 0.00323 0.00105 -0.00106 AFIX 23 H5AA 2 0.480523 0.594118 0.716227 10.40000 -1.20000 H5AB 2 0.572463 0.652188 0.743673 10.40000 -1.20000 AFIX 0 PART 0 PART 1 C6 1 0.537217 0.628899 0.661397 10.60000 0.06943 0.10200 = 0.10032 0.00330 -0.01133 0.05436 AFIX 23 H6A 2 0.507156 0.577170 0.684141 10.60000 -1.20000 H6B 2 0.605597 0.612030 0.647161 10.60000 -1.20000 AFIX 0 PART 0 PART 2 C6A 1 0.562398 0.662694 0.627700 10.40000 0.06786 0.07755 = 0.08701 0.00497 0.00058 -0.00510 AFIX 23 H6AA 2 0.591829 0.721748 0.619566 10.40000 -1.20000 H6AB 2 0.611520 0.616224 0.615977 10.40000 -1.20000 AFIX 0 PART 0 PART 1 C8 1 0.533193 0.689437 0.545448 10.60000 0.04300 0.14491 = 0.09645 -0.03387 0.02322 0.00930 AFIX 23 H8A 2 0.573318 0.642862 0.523260 10.60000 -1.20000 H8B 2 0.579801 0.731747 0.566860 10.60000 -1.20000 AFIX 0 PART 0 PART 2 C8A 1 0.493560 0.689603 0.514814 10.40000 0.06363 0.09594 = 0.08722 0.00334 -0.00078 -0.01218 AFIX 23 H8AA 2 0.559197 0.667270 0.499189 10.40000 -1.20000 H8AB 2 0.441434 0.666864 0.484023 10.40000 -1.20000 AFIX 0 PART 0 PART 1 C9 1 0.471015 0.735826 0.495063 10.60000 0.09060 0.10286 = 0.06010 0.00329 0.04930 0.00053 AFIX 23 H9A 2 0.430337 0.692172 0.470078 10.60000 -1.20000 H9B 2 0.515042 0.766444 0.462578 10.60000 -1.20000 AFIX 0 PART 0 PART 2 C9A 1 0.493701 0.790639 0.512764 10.40000 0.07097 0.09611 = 0.08651 0.00703 0.00227 -0.01076 AFIX 23 H9AA 2 0.542013 0.815868 0.545184 10.40000 -1.20000 H9AB 2 0.508791 0.813162 0.467251 10.40000 -1.20000 AFIX 0 PART 0 PART 1 C11 1 0.446887 0.888551 0.540981 10.60000 0.09091 0.07522 = 0.07273 0.01758 0.02228 -0.02401 AFIX 23 H11A 2 0.451607 0.921523 0.498212 10.60000 -1.20000 H11B 2 0.515500 0.877725 0.557859 10.60000 -1.20000 AFIX 0 PART 0 PART 2 C11A 1 0.398213 0.920584 0.556261 10.40000 0.08172 0.09751 = 0.09366 0.00242 -0.00098 -0.00774 AFIX 23 H11C 2 0.435372 0.955315 0.522340 10.40000 -1.20000 H11D 2 0.328522 0.942804 0.557113 10.40000 -1.20000 AFIX 0 PART 0 PART 1 C12 1 0.386770 0.941609 0.592363 10.60000 0.17536 0.03402 = 0.09490 0.01105 0.00635 -0.01706 AFIX 23 H12A 2 0.319760 0.955033 0.573759 10.60000 -1.20000 H12B 2 0.421185 0.998328 0.601260 10.60000 -1.20000 AFIX 0 PART 0 PART 2 C12A 1 0.445851 0.936584 0.625305 10.40000 0.09577 0.08818 = 0.09522 0.00396 -0.00616 -0.00903 AFIX 23 H12C 2 0.514027 0.911368 0.628848 10.40000 -1.20000 H12D 2 0.446756 0.999848 0.637864 10.40000 -1.20000 AFIX 0 HKLF 4 REM sub-pankj-sd12_a.res in Pbca REM wR2 = 0.2051, GooF = S = 1.129, Restrained GooF = 1.177 for all data REM R1 = 0.0623 for 3007 Fo > 4sig(Fo) and 0.0792 for all 4208 data REM 302 parameters refined using 72 restraints END WGHT 0.0964 3.7388 REM Highest difference peak 0.698, deepest hole -0.397, 1-sigma level 0.072 Q1 1 0.2064 0.4876 0.9448 11.00000 0.05 0.70 Q2 1 0.4667 0.6294 0.6159 11.00000 0.05 0.56 Q3 1 0.2009 0.4840 0.8461 11.00000 0.05 0.49 Q4 1 0.3790 0.8482 0.5476 11.00000 0.05 0.49 Q5 1 0.3462 0.4793 0.9148 11.00000 0.05 0.48 Q6 1 0.2202 0.7229 0.6800 11.00000 0.05 0.48 Q7 1 0.2299 0.6713 0.5853 11.00000 0.05 0.44 Q8 1 0.4768 0.6815 0.5734 11.00000 0.05 0.42 Q9 1 0.4198 0.7728 0.5205 11.00000 0.05 0.41 Q10 1 0.3063 0.3727 0.9238 11.00000 0.05 0.38 Q11 1 0.3023 0.4254 0.8308 11.00000 0.05 0.35 Q12 1 0.4744 0.6464 0.7362 11.00000 0.05 0.35 Q13 1 0.4832 0.8433 0.5200 11.00000 0.05 0.32 Q14 1 0.3012 0.5077 0.8369 11.00000 0.05 0.31 Q15 1 0.4338 0.7541 0.7317 11.00000 0.05 0.30 Q16 1 0.5426 0.6397 0.6891 11.00000 0.05 0.30 Q17 1 0.4963 0.6479 0.5296 11.00000 0.05 0.29 Q18 1 0.1866 0.3731 0.8880 11.00000 0.05 0.28 Q19 1 0.4864 0.8553 0.7296 11.00000 0.05 0.28 Q20 1 0.1340 0.4299 0.8946 11.00000 0.05 0.27 REM The information below was added by Olex2. REM REM R1 = 0.0623 for 3007 Fo > 4sig(Fo) and 0.0792 for all 61370 data REM n/a parameters refined using n/a restraints REM Highest difference peak 0.70, deepest hole -0.40 REM Mean Shift 0, Max Shift 0.001. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0792 REM R1_gt = 0.0623 REM wR_ref = 0.2051 REM GOOF = 1.129 REM Shift_max = 0.001 REM Shift_mean = 0 REM Reflections_all = 61370 REM Reflections_gt = 3007 REM Parameters = n/a REM Hole = -0.40 REM Peak = 0.70 REM Flack = n/a ; _cod_data_source_file d0sc01572e2.cif _cod_data_source_block Co-BF4 _cod_depositor_comments ;Adding full bibliography for 1557898.cif. Adding full bibliography for 1557898.cif. ; _cod_database_code 1557898 _shelx_shelxl_version_number 2018/3 _chemical_oxdiff_formula 'Co B F C H N O' _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. ; _diffrn_oxdiff_ac3_digest_frames ; 0197eeb08c3a60edf726793378415987da000253582 ; _diffrn_oxdiff_ac3_digest_hkl ; 01a427163ced6726a2332d16e91ade0b193575 ; _reflns_odcompleteness_completeness 99.63 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 26.32 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2. Rigid body (RIGU) restrains C2, C3, C5, C6, C8, C9, C11, C12, N3, C6, N3, C8, N2, C3, N2, C5, N4, C9, N4, C11, N1, C2, N1, C12, C6, C5, C6, C9, C8, C3, C2, C5, C12, C11, C11, C12, C2, C3, C9, C11, C2, C9, C11, C11, C8, C9, C5, C6 with sigma for 1-2 distances of 0.00005 and sigma for 1-3 distances of 0.00005 C2A, C3A, C5A, C6A, C8A, C9A, C11A, C12A, N3, C6A, N3, C8A, N2, C3A, N2, C5A, N4, C9A, N4, C11A, N1, C2A, N1, C12A, C6A, C5A, C9A, C8A, C3A, C2A, C5A, C12A, C11A, C11A, C12A, C2A, C3A, C12A, C8A, C9A, C11A, C9A, C11A, C9A, C11A, C8A, C5A, C6A with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001 3. Others Fixed Sof: C2(0.6) H2A(0.6) H2B(0.6) C2A(0.4) H2AA(0.4) H2AB(0.4) C3(0.6) H3A(0.6) H3B(0.6) C3A(0.4) H3AA(0.4) H3AB(0.4) C5(0.6) H5A(0.6) H5B(0.6) C5A(0.4) H5AA(0.4) H5AB(0.4) C6(0.6) H6A(0.6) H6B(0.6) C6A(0.4) H6AA(0.4) H6AB(0.4) C8(0.6) H8A(0.6) H8B(0.6) C8A(0.4) H8AA(0.4) H8AB(0.4) C9(0.6) H9A(0.6) H9B(0.6) C9A(0.4) H9AA(0.4) H9AB(0.4) C11(0.6) H11A(0.6) H11B(0.6) C11A(0.4) H11C(0.4) H11D(0.4) C12(0.6) H12A(0.6) H12B(0.6) C12A(0.4) H12C(0.4) H12D(0.4) 4.a Secondary CH2 refined with riding coordinates: C2(H2A,H2B), C2A(H2AA,H2AB), C3(H3A,H3B), C3A(H3AA,H3AB), C5(H5A,H5B), C5A(H5AA,H5AB), C6(H6A,H6B), C6A(H6AA,H6AB), C8(H8A,H8B), C8A(H8AA,H8AB), C9(H9A,H9B), C9A(H9AA,H9AB), C11(H11A,H11B), C11A(H11C,H11D), C12(H12A,H12B), C12A(H12C,H12D) 4.b Idealised Me refined as rotating group: C10(H10A,H10B,H10C), C1(H1A,H1B,H1C), C7(H7A,H7B,H7C), C4(H4A,H4B,H4C) ; _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 1.448 _oxdiff_exptl_absorpt_empirical_full_min 0.774 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' 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 0.36073(3) 0.74971(3) 0.62959(2) 0.0409(2) Uani 1 1 d . . . . . N3 N 0.4709(3) 0.6514(2) 0.59436(19) 0.0729(8) Uani 1 1 d . U . . . N5 N 0.1732(3) 0.6894(4) 0.6331(2) 0.0831(12) Uani 1 1 d . . . . . N2 N 0.4439(3) 0.7289(3) 0.72518(18) 0.0759(8) Uani 1 1 d . U . . . F1 F 0.2855(3) 0.3563(2) 0.86646(19) 0.1241(13) Uani 1 1 d . . . . . N4 N 0.3968(3) 0.8080(3) 0.53096(18) 0.0778(9) Uani 1 1 d . U . . . O2 O 0.2486(3) 0.6521(3) 0.6533(3) 0.1229(15) Uani 1 1 d . . . . . N1 N 0.3743(3) 0.8878(2) 0.6619(2) 0.0786(8) Uani 1 1 d . U . . . O1 O 0.1956(4) 0.7635(4) 0.6122(3) 0.1222(18) Uani 1 1 d . . . . . F3 F 0.1570(3) 0.4409(4) 0.8932(3) 0.1573(18) Uani 1 1 d . . . . . F2 F 0.2906(4) 0.4328(4) 0.9596(2) 0.184(2) Uani 1 1 d . . . . . F4 F 0.3024(6) 0.5022(3) 0.8615(3) 0.205(3) Uani 1 1 d . . . . . C10 C 0.3102(5) 0.8116(4) 0.4836(2) 0.1084(19) Uani 1 1 d . . . . . H10A H 0.285757 0.751626 0.475071 0.163 Uiso 1 1 calc GR . . . . H10B H 0.331601 0.838518 0.441250 0.163 Uiso 1 1 calc GR . . . . H10C H 0.256388 0.847070 0.503375 0.163 Uiso 1 1 calc GR . . . . B1 B 0.2592(4) 0.4366(4) 0.8936(3) 0.0710(12) Uani 1 1 d . . . . . C1 C 0.2780(5) 0.9251(4) 0.6900(3) 0.122(2) Uani 1 1 d . . . . . H1A H 0.229037 0.932039 0.653785 0.183 Uiso 1 1 calc GR . . . . H1B H 0.291237 0.982757 0.710540 0.183 Uiso 1 1 calc GR . . . . H1C H 0.251217 0.884732 0.724000 0.183 Uiso 1 1 calc GR . . . . C7 C 0.4277(4) 0.5631(3) 0.5786(3) 0.1023(18) Uani 1 1 d . . . . . H7A H 0.398696 0.537461 0.619374 0.153 Uiso 1 1 calc GR . . . . H7B H 0.480477 0.524130 0.561615 0.153 Uiso 1 1 calc GR . . . . H7C H 0.375357 0.569506 0.544509 0.153 Uiso 1 1 calc GR . . . . C4 C 0.3898(6) 0.6826(5) 0.7787(3) 0.130(2) Uani 1 1 d . . . . . H4A H 0.326319 0.712823 0.787577 0.196 Uiso 1 1 calc GR . . . . H4B H 0.430564 0.682257 0.819569 0.196 Uiso 1 1 calc GR . . . . H4C H 0.376405 0.621651 0.764738 0.196 Uiso 1 1 calc GR . . . . C2 C 0.4593(10) 0.8955(6) 0.7015(6) 0.107(4) Uani 0.6 1 d . U P A 1 H2A H 0.461834 0.954926 0.722201 0.128 Uiso 0.6 1 calc R . P A 1 H2B H 0.520073 0.887577 0.673762 0.128 Uiso 0.6 1 calc R . P A 1 C2A C 0.4376(13) 0.8795(12) 0.7370(9) 0.0879(11) Uani 0.4 1 d . U P A 2 H2AA H 0.474872 0.935032 0.745185 0.105 Uiso 0.4 1 calc R . P A 2 H2AB H 0.388566 0.872177 0.773836 0.105 Uiso 0.4 1 calc R . P A 2 C3 C 0.4553(8) 0.8228(8) 0.7577(4) 0.093(3) Uani 0.6 1 d . U P A 1 H3A H 0.517458 0.824912 0.784710 0.111 Uiso 0.6 1 calc R . P A 1 H3B H 0.397996 0.834333 0.787937 0.111 Uiso 0.6 1 calc R . P A 1 C3A C 0.5072(12) 0.8060(10) 0.7381(8) 0.0867(14) Uani 0.4 1 d . U P A 2 H3AA H 0.540613 0.801142 0.782279 0.104 Uiso 0.4 1 calc R . P A 2 H3AB H 0.558839 0.812581 0.702823 0.104 Uiso 0.4 1 calc R . P A 2 C5 C 0.5441(6) 0.6945(9) 0.7053(5) 0.102(4) Uani 0.6 1 d . U P A 1 H5A H 0.583824 0.743113 0.685372 0.123 Uiso 0.6 1 calc R . P A 1 H5B H 0.579808 0.673464 0.745736 0.123 Uiso 0.6 1 calc R . P A 1 C5A C 0.5162(12) 0.6511(10) 0.7113(9) 0.0824(10) Uani 0.4 1 d . U P A 2 H5AA H 0.480523 0.594118 0.716227 0.099 Uiso 0.4 1 calc R . P A 2 H5AB H 0.572463 0.652188 0.743673 0.099 Uiso 0.4 1 calc R . P A 2 C6 C 0.5372(7) 0.6289(7) 0.6614(5) 0.091(3) Uani 0.6 1 d . U P A 1 H6A H 0.507156 0.577170 0.684141 0.109 Uiso 0.6 1 calc R . P A 1 H6B H 0.605597 0.612030 0.647161 0.109 Uiso 0.6 1 calc R . P A 1 C6A C 0.5624(10) 0.6627(10) 0.6277(7) 0.0775(13) Uani 0.4 1 d . U P A 2 H6AA H 0.591829 0.721748 0.619566 0.093 Uiso 0.4 1 calc R . P A 2 H6AB H 0.611520 0.616224 0.615977 0.093 Uiso 0.4 1 calc R . P A 2 C8 C 0.5332(6) 0.6894(7) 0.5454(5) 0.095(3) Uani 0.6 1 d . U P A 1 H8A H 0.573318 0.642862 0.523260 0.114 Uiso 0.6 1 calc R . P A 1 H8B H 0.579801 0.731747 0.566860 0.114 Uiso 0.6 1 calc R . P A 1 C8A C 0.4936(12) 0.6896(11) 0.5148(8) 0.0823(11) Uani 0.4 1 d . U P A 2 H8AA H 0.559197 0.667270 0.499189 0.099 Uiso 0.4 1 calc R . P A 2 H8AB H 0.441434 0.666864 0.484023 0.099 Uiso 0.4 1 calc R . P A 2 C9 C 0.4710(7) 0.7358(7) 0.4951(4) 0.085(3) Uani 0.6 1 d . U P A 1 H9A H 0.430337 0.692172 0.470078 0.101 Uiso 0.6 1 calc R . P A 1 H9B H 0.515042 0.766444 0.462578 0.101 Uiso 0.6 1 calc R . P A 1 C9A C 0.4937(10) 0.7906(10) 0.5128(8) 0.0845(14) Uani 0.4 1 d . U P A 2 H9AA H 0.542013 0.815868 0.545184 0.101 Uiso 0.4 1 calc R . P A 2 H9AB H 0.508791 0.813162 0.467251 0.101 Uiso 0.4 1 calc R . P A 2 C11 C 0.4469(7) 0.8886(6) 0.5410(4) 0.080(2) Uani 0.6 1 d . U P A 1 H11A H 0.451607 0.921523 0.498212 0.096 Uiso 0.6 1 calc R . P A 1 H11B H 0.515500 0.877725 0.557859 0.096 Uiso 0.6 1 calc R . P A 1 C11A C 0.3982(14) 0.9206(12) 0.5563(10) 0.0910(12) Uani 0.4 1 d . U P A 2 H11C H 0.435372 0.955315 0.522340 0.109 Uiso 0.4 1 calc R . P A 2 H11D H 0.328522 0.942804 0.557113 0.109 Uiso 0.4 1 calc R . P A 2 C12 C 0.3868(11) 0.9416(5) 0.5924(6) 0.101(3) Uani 0.6 1 d . U P A 1 H12A H 0.319760 0.955033 0.573759 0.122 Uiso 0.6 1 calc R . P A 1 H12B H 0.421185 0.998328 0.601260 0.122 Uiso 0.6 1 calc R . P A 1 C12A C 0.4459(13) 0.9366(11) 0.6253(7) 0.0931(16) Uani 0.4 1 d . U P A 2 H12C H 0.514027 0.911368 0.628848 0.112 Uiso 0.4 1 calc R . P A 2 H12D H 0.446756 0.999848 0.637864 0.112 Uiso 0.4 1 calc R . P A 2 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 0.0357(3) 0.0436(3) 0.0433(3) 0.00532(16) 0.00240(14) 0.00108(16) N3 0.0635(15) 0.0723(19) 0.0831(17) -0.0074(13) 0.0053(13) 0.0032(14) N5 0.050(2) 0.107(3) 0.092(3) 0.008(2) 0.0130(18) -0.013(2) N2 0.0857(18) 0.0791(17) 0.0630(16) -0.0004(13) -0.0129(14) 0.0015(14) F1 0.124(3) 0.097(2) 0.152(3) -0.019(2) 0.011(2) 0.024(2) N4 0.0709(17) 0.0938(19) 0.0687(18) 0.0129(14) -0.0003(14) -0.0091(14) O2 0.077(2) 0.097(3) 0.195(4) 0.041(3) -0.001(3) -0.021(2) N1 0.0889(17) 0.0559(17) 0.0909(19) -0.0074(13) 0.0005(15) 0.0074(14) O1 0.068(3) 0.142(4) 0.157(4) 0.048(3) -0.005(2) -0.002(2) F3 0.091(3) 0.179(4) 0.202(4) 0.008(3) 0.006(3) 0.050(3) F2 0.202(5) 0.242(5) 0.109(3) -0.026(3) -0.035(3) -0.033(4) F4 0.287(7) 0.126(4) 0.201(5) 0.032(3) 0.101(5) -0.053(4) C10 0.116(4) 0.143(5) 0.067(3) 0.033(3) -0.027(3) -0.022(4) B1 0.069(3) 0.071(3) 0.072(3) -0.006(2) -0.002(2) 0.004(2) C1 0.148(5) 0.082(3) 0.135(5) -0.016(3) 0.022(4) 0.052(4) C7 0.098(4) 0.073(3) 0.136(5) -0.039(3) 0.014(3) 0.004(3) C4 0.167(6) 0.164(6) 0.060(3) 0.046(3) -0.007(3) -0.006(5) C2 0.165(10) 0.067(5) 0.089(6) -0.015(5) -0.008(7) -0.039(6) C2A 0.092(2) 0.0791(18) 0.0930(19) -0.0009(15) -0.0019(17) 0.0006(15) C3 0.101(7) 0.119(8) 0.058(4) -0.029(5) -0.026(4) -0.003(6) C3A 0.0885(19) 0.0806(18) 0.091(3) -0.0066(14) -0.0118(19) 0.0000(14) C5 0.055(5) 0.166(11) 0.086(6) 0.032(7) -0.024(4) 0.010(5) C5A 0.086(2) 0.0766(18) 0.0842(16) 0.0032(15) 0.0010(15) -0.0011(17) C6 0.069(5) 0.102(7) 0.100(7) 0.003(5) -0.011(5) 0.054(5) C6A 0.0679(16) 0.078(4) 0.0870(17) 0.0050(17) 0.0006(14) -0.0051(14) C8 0.043(4) 0.145(9) 0.096(6) -0.034(6) 0.023(4) 0.009(5) C8A 0.064(2) 0.096(2) 0.0872(17) 0.0033(16) -0.0008(14) -0.0122(16) C9 0.091(6) 0.103(7) 0.060(4) 0.003(4) 0.049(5) 0.001(5) C9A 0.0710(18) 0.096(2) 0.087(4) 0.0070(17) 0.0023(19) -0.0108(16) C11 0.091(6) 0.075(5) 0.073(5) 0.018(4) 0.022(4) -0.024(4) C11A 0.082(3) 0.0975(19) 0.0937(18) 0.0024(15) -0.0010(17) -0.0077(16) C12 0.175(11) 0.034(4) 0.095(6) 0.011(4) 0.006(7) -0.017(5) C12A 0.096(2) 0.088(3) 0.0952(19) 0.0040(15) -0.0062(18) -0.009(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' B B 0.0013 0.0007 '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' F F 0.0171 0.0103 '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 N3 Co1 N2 81.06(15) . . ? N3 Co1 N4 80.84(15) . . ? N3 Co1 O1 132.01(18) . . ? N2 Co1 O1 129.48(17) . . ? N4 Co1 N2 135.17(15) . . ? N4 Co1 O1 92.27(16) . . ? O2 Co1 N3 94.05(17) . . ? O2 Co1 N2 93.58(18) . . ? O2 Co1 N4 128.33(18) . . ? O2 Co1 N1 130.24(18) . . ? O2 Co1 O1 54.16(17) . . ? N1 Co1 N3 132.86(14) . . ? N1 Co1 N2 80.94(15) . . ? N1 Co1 N4 82.08(15) . . ? N1 Co1 O1 92.17(18) . . ? C7 N3 Co1 114.4(3) . . ? C7 N3 C6 101.3(5) . . ? C7 N3 C8A 100.2(6) . . ? C6 N3 Co1 103.9(4) . . ? C6A N3 Co1 110.4(6) . . ? C6A N3 C7 123.2(7) . . ? C6A N3 C8A 104.1(8) . . ? C8 N3 Co1 109.8(5) . . ? C8 N3 C7 116.8(6) . . ? C8 N3 C6 109.3(6) . . ? C8A N3 Co1 100.6(6) . . ? O2 N5 O1 109.4(4) . . ? C4 N2 Co1 116.4(4) . . ? C4 N2 C3 100.4(5) . . ? C4 N2 C5 117.9(6) . . ? C4 N2 C5A 94.2(7) . . ? C3 N2 Co1 105.9(4) . . ? C3A N2 Co1 109.0(7) . . ? C3A N2 C4 122.5(8) . . ? C3A N2 C5A 106.1(9) . . ? C5 N2 Co1 105.6(4) . . ? C5 N2 C3 109.8(7) . . ? C5A N2 Co1 105.4(7) . . ? C10 N4 Co1 114.1(3) . . ? C10 N4 C9 102.5(5) . . ? C10 N4 C11A 98.8(7) . . ? C9 N4 Co1 104.7(4) . . ? C9A N4 Co1 111.4(6) . . ? C9A N4 C10 124.8(7) . . ? C9A N4 C11A 104.4(9) . . ? C11 N4 Co1 108.9(4) . . ? C11 N4 C10 115.3(5) . . ? C11 N4 C9 110.6(6) . . ? C11A N4 Co1 97.6(6) . . ? N5 O2 Co1 100.6(3) . . ? C1 N1 Co1 113.2(3) . . ? C1 N1 C2A 97.0(6) . . ? C1 N1 C12 102.6(6) . . ? C2 N1 Co1 108.3(5) . . ? C2 N1 C1 116.9(6) . . ? C2 N1 C12 111.2(7) . . ? C2A N1 Co1 103.1(6) . . ? C12 N1 Co1 103.7(4) . . ? C12A N1 Co1 113.8(7) . . ? C12A N1 C1 124.9(8) . . ? C12A N1 C2A 98.9(9) . . ? N5 O1 Co1 95.8(3) . . ? N4 C10 H10A 109.5 . . ? N4 C10 H10B 109.5 . . ? N4 C10 H10C 109.5 . . ? H10A C10 H10B 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? F1 B1 F2 105.0(5) . . ? F3 B1 F1 107.2(5) . . ? F3 B1 F2 108.1(5) . . ? F4 B1 F1 111.3(5) . . ? F4 B1 F3 113.6(6) . . ? F4 B1 F2 111.2(6) . . ? N1 C1 H1A 109.5 . . ? N1 C1 H1B 109.5 . . ? N1 C1 H1C 109.5 . . ? H1A C1 H1B 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N3 C7 H7A 109.5 . . ? N3 C7 H7B 109.5 . . ? N3 C7 H7C 109.5 . . ? H7A C7 H7B 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N2 C4 H4A 109.5 . . ? N2 C4 H4B 109.5 . . ? N2 C4 H4C 109.5 . . ? H4A C4 H4B 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N1 C2 H2A 110.0 . . ? N1 C2 H2B 110.0 . . ? N1 C2 C3 108.6(8) . . ? H2A C2 H2B 108.3 . . ? C3 C2 H2A 110.0 . . ? C3 C2 H2B 110.0 . . ? N1 C2A H2AA 109.1 . . ? N1 C2A H2AB 109.1 . . ? H2AA C2A H2AB 107.8 . . ? C3A C2A N1 112.5(12) . . ? C3A C2A H2AA 109.1 . . ? C3A C2A H2AB 109.1 . . ? N2 C3 C2 110.1(6) . . ? N2 C3 H3A 109.6 . . ? N2 C3 H3B 109.6 . . ? C2 C3 H3A 109.6 . . ? C2 C3 H3B 109.6 . . ? H3A C3 H3B 108.2 . . ? N2 C3A H3AA 111.0 . . ? N2 C3A H3AB 111.0 . . ? C2A C3A N2 103.8(12) . . ? C2A C3A H3AA 111.0 . . ? C2A C3A H3AB 111.0 . . ? H3AA C3A H3AB 109.0 . . ? N2 C5 H5A 109.2 . . ? N2 C5 H5B 109.2 . . ? H5A C5 H5B 107.9 . . ? C6 C5 N2 112.0(8) . . ? C6 C5 H5A 109.2 . . ? C6 C5 H5B 109.2 . . ? N2 C5A H5AA 110.1 . . ? N2 C5A H5AB 110.1 . . ? N2 C5A C6A 107.9(10) . . ? H5AA C5A H5AB 108.4 . . ? C6A C5A H5AA 110.1 . . ? C6A C5A H5AB 110.1 . . ? N3 C6 H6A 108.6 . . ? N3 C6 H6B 108.6 . . ? C5 C6 N3 114.8(7) . . ? C5 C6 H6A 108.6 . . ? C5 C6 H6B 108.6 . . ? H6A C6 H6B 107.5 . . ? N3 C6A C5A 97.4(9) . . ? N3 C6A H6AA 112.3 . . ? N3 C6A H6AB 112.3 . . ? C5A C6A H6AA 112.3 . . ? C5A C6A H6AB 112.3 . . ? H6AA C6A H6AB 109.9 . . ? N3 C8 H8A 109.8 . . ? N3 C8 H8B 109.8 . . ? N3 C8 C9 109.5(6) . . ? H8A C8 H8B 108.2 . . ? C9 C8 H8A 109.8 . . ? C9 C8 H8B 109.8 . . ? N3 C8A H8AA 109.4 . . ? N3 C8A H8AB 109.4 . . ? H8AA C8A H8AB 108.0 . . ? C9A C8A N3 111.2(11) . . ? C9A C8A H8AA 109.4 . . ? C9A C8A H8AB 109.4 . . ? N4 C9 H9A 109.4 . . ? N4 C9 H9B 109.4 . . ? C8 C9 N4 111.0(6) . . ? C8 C9 H9A 109.4 . . ? C8 C9 H9B 109.4 . . ? H9A C9 H9B 108.0 . . ? N4 C9A C8A 100.6(11) . . ? N4 C9A H9AA 111.7 . . ? N4 C9A H9AB 111.7 . . ? C8A C9A H9AA 111.7 . . ? C8A C9A H9AB 111.7 . . ? H9AA C9A H9AB 109.4 . . ? N4 C11 H11A 110.2 . . ? N4 C11 H11B 110.2 . . ? N4 C11 C12 107.5(7) . . ? H11A C11 H11B 108.5 . . ? C12 C11 H11A 110.2 . . ? C12 C11 H11B 110.2 . . ? N4 C11A H11C 108.7 . . ? N4 C11A H11D 108.7 . . ? H11C C11A H11D 107.6 . . ? C12A C11A N4 114.2(13) . . ? C12A C11A H11C 108.7 . . ? C12A C11A H11D 108.7 . . ? N1 C12 H12A 109.4 . . ? N1 C12 H12B 109.4 . . ? C11 C12 N1 111.3(6) . . ? C11 C12 H12A 109.4 . . ? C11 C12 H12B 109.4 . . ? H12A C12 H12B 108.0 . . ? N1 C12A C11A 95.7(12) . . ? N1 C12A H12C 112.6 . . ? N1 C12A H12D 112.6 . . ? C11A C12A H12C 112.6 . . ? C11A C12A H12D 112.6 . . ? H12C C12A H12D 110.1 . . ? 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 N3 2.164(3) . ? Co1 N2 2.183(4) . ? Co1 N4 2.164(4) . ? Co1 O2 2.113(4) . ? Co1 N1 2.150(4) . ? Co1 O1 2.198(5) . ? N3 C7 1.460(6) . ? N3 C6 1.606(9) . ? N3 C6A 1.373(13) . ? N3 C8 1.377(9) . ? N3 C8A 1.680(16) . ? N5 O2 1.197(6) . ? N5 O1 1.209(6) . ? N2 C4 1.438(7) . ? N2 C3 1.537(10) . ? N2 C3A 1.434(15) . ? N2 C5 1.460(10) . ? N2 C5A 1.518(16) . ? F1 B1 1.348(6) . ? N4 C10 1.465(6) . ? N4 C9 1.607(9) . ? N4 C9A 1.342(13) . ? N4 C11 1.377(8) . ? N4 C11A 1.742(19) . ? N1 C1 1.483(6) . ? N1 C2 1.361(11) . ? N1 C2A 1.691(18) . ? N1 C12 1.583(10) . ? N1 C12A 1.382(16) . ? F3 B1 1.338(6) . ? F2 B1 1.354(7) . ? F4 B1 1.288(7) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C2 C3 1.539(14) . ? C2A H2AA 0.9700 . ? C2A H2AB 0.9700 . ? C2A C3A 1.42(2) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C3A H3AA 0.9700 . ? C3A H3AB 0.9700 . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C5 C6 1.300(14) . ? C5A H5AA 0.9700 . ? C5A H5AB 0.9700 . ? C5A C6A 1.75(2) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C6A H6AA 0.9700 . ? C6A H6AB 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C8 C9 1.451(13) . ? C8A H8AA 0.9700 . ? C8A H8AB 0.9700 . ? C8A C9A 1.50(2) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C9A H9AA 0.9700 . ? C9A H9AB 0.9700 . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C11 C12 1.499(13) . ? C11A H11C 0.9700 . ? C11A H11D 0.9700 . ? C11A C12A 1.50(2) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C12A H12C 0.9700 . ? C12A H12D 0.9700 . ?