#------------------------------------------------------------------------------ #$Date: 2016-03-26 03:36:43 +0200 (Sat, 26 Mar 2016) $ #$Revision: 180189 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/10/85/7108551.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_7108551 loop_ _publ_author_name 'Samir Barman' 'Jai Anand Garg' 'Olivier Blacque' 'Koushik Venkatesan' 'Heinz Berke' _publ_section_title ; Triptycene based luminescent metal-organic gels for chemosensing ; _journal_name_full Chem.Commun. _journal_page_first 11127 _journal_paper_doi 10.1039/c2cc34430k _journal_volume 48 _journal_year 2012 _chemical_formula_moiety 'C27 H19 Co2 N O10' _chemical_formula_sum 'C27 H19 Co2 N O10' _chemical_formula_weight 635.29 _space_group_IT_number 15 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 98.302(3) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 17.1691(5) _cell_length_b 11.0334(5) _cell_length_c 16.3274(6) _cell_measurement_reflns_used 3441 _cell_measurement_temperature 183(2) _cell_measurement_theta_max 32.75 _cell_measurement_theta_min 2.44 _cell_volume 3060.5(2) _computing_cell_refinement ; CrysAlisPro, Version 1.171.33.55 (Agilent, 2011) ; _computing_data_collection ; CrysAlisPro, Version 1.171.33.55 (Agilent, 2011) ; _computing_data_reduction ; CrysAlisPro, Version 1.171.33.55 (Agilent, 2011) ; _computing_molecular_graphics ; DIAMOND (Brandenburg, 2006) ; _computing_publication_material ; WinGX (Farrugia, 1999), PLATON for Windows (Spek, 2003) and publCIF (Westrip, 2010) ; _computing_structure_refinement ' SHELXL97. Sheldrick (2008).' _computing_structure_solution ' SHELXS97. Sheldrick (2008)' _diffrn_ambient_temperature 183(2) _diffrn_detector_area_resol_mean 10.4498 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type ; Goniometer Xcalibur, detector: Ruby Oxford Diffraction (2007). Oxford Diffraction Ltd., Xcalibur CCD system ; _diffrn_measurement_method 'omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0431 _diffrn_reflns_av_sigmaI/netI 0.0650 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 9118 _diffrn_reflns_theta_full 25.00 _diffrn_reflns_theta_max 25.00 _diffrn_reflns_theta_min 2.45 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 1.135 _exptl_absorpt_correction_T_max 0.975 _exptl_absorpt_correction_T_min 0.864 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro, Version 1.171.33.66 (Agilent, 2011) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by Clark & Reid (1995). ; _exptl_crystal_colour violet _exptl_crystal_density_diffrn 1.379 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 1288 _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.02 _refine_diff_density_max 0.796 _refine_diff_density_min -0.728 _refine_diff_density_rms 0.129 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.107 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 254 _refine_ls_number_reflns 2691 _refine_ls_number_restraints 12 _refine_ls_restrained_S_all 1.105 _refine_ls_R_factor_all 0.1048 _refine_ls_R_factor_gt 0.0756 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1219P)^2^+11.3813P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2135 _refine_ls_wR_factor_ref 0.2256 _reflns_number_gt 1970 _reflns_number_total 2691 _reflns_threshold_expression >2sigma(I) _iucr_refine_instructions_details ; TITL sami1602 in C2/c CELL 0.71073 17.1691 11.0334 16.3274 90.000 98.302 90.000 ZERR 4.00 0.0005 0.0005 0.0006 0.000 0.003 0.000 LATT 7 SYMM - X, Y, 1/2 - Z SFAC C H CO N O UNIT 108 76 8 4 40 MERG 2 OMIT -2.00 50.00 OMIT 0 0 4 OMIT -2 0 2 SADI 0.005 N1 C17 N1 C18 N1 C19 SADI 0.010 C17 C18 C18 C19 C17 C19 EADP O6 C17 N1 C18 C19 DFIX 1.20 0.010 C17 O6 FREE C3A C3B C3A C4B FREE C4A C4B C4A C3B DFIX 0.95 0.005 O5 H5A O5 H5B DANG 2.50 0.005 CO2 H5A CO2 H5B DANG 1.60 0.010 H5A H5B FMAP 2 PLAN 20 ACTA BOND $H L.S. 8 WGHT 0.121900 11.381301 FVAR 0.49133 C1 1 0.095679 0.319963 0.133999 11.00000 0.02815 0.04872 = 0.03635 0.00021 0.01442 0.00362 C2 1 0.169266 0.248518 0.128957 11.00000 0.02963 0.05801 = 0.03318 0.00521 0.01666 0.01134 C5 1 0.308022 0.110663 0.128240 11.00000 0.02789 0.04768 = 0.03804 0.00852 0.01583 0.01172 C3A 1 0.184201 0.148895 0.177706 10.50000 0.02957 0.06224 = 0.05130 0.02818 0.02030 0.00484 AFIX 43 H3A 2 0.148311 0.126837 0.212600 10.50000 -1.20000 AFIX 0 C4A 1 0.252838 0.077559 0.176987 10.50000 0.05809 0.05478 = 0.06867 0.03897 0.04183 0.03046 AFIX 43 H4A 2 0.260439 0.008271 0.209597 10.50000 -1.20000 AFIX 0 C6A 1 0.296826 0.216143 0.080587 10.50000 0.01813 0.04614 = 0.03490 -0.00383 0.01485 0.00176 C7A 1 0.228546 0.288420 0.081561 10.50000 0.03158 0.03208 = 0.02842 -0.00443 0.00970 0.00346 C3B 1 0.213847 0.212355 0.202551 10.50000 0.03309 0.10174 = 0.02925 0.00474 0.01900 0.01911 AFIX 43 H3B 2 0.197012 0.231653 0.252602 10.50000 -1.20000 AFIX 0 C4B 1 0.283373 0.147642 0.202585 10.50000 0.04826 0.05934 = 0.04370 0.01686 0.01511 0.02668 AFIX 43 H4B 2 0.313985 0.128600 0.252667 10.50000 -1.20000 AFIX 0 C6B 1 0.258873 0.135252 0.054464 10.50000 0.02717 0.03027 = 0.03819 0.00266 0.01749 -0.00051 C7B 1 0.190065 0.204591 0.054361 10.50000 0.02821 0.03388 = 0.03204 0.00569 0.01646 0.00645 C8 1 0.384524 0.037847 0.133866 11.00000 0.02782 0.04598 = 0.04342 0.00560 0.01635 0.00504 C9 1 0.355343 0.276400 0.029648 10.50000 0.02193 0.03636 = 0.03228 0.00150 0.01151 0.00022 AFIX 13 H9 2 0.403413 0.228808 0.028795 10.50000 -1.20000 AFIX 0 C10 1 0.227547 0.401816 0.031990 10.50000 0.02705 0.04681 = 0.03177 -0.01097 0.01541 -0.00110 AFIX 13 H10 2 0.179500 0.449640 0.032356 10.50000 -1.20000 AFIX 66 C11 1 0.303417 0.472264 0.065924 10.50000 0.04205 0.04281 = 0.03498 0.00265 0.01337 -0.00159 C12 1 0.371427 0.404161 0.065218 10.50000 0.03790 0.02860 = 0.03103 -0.00365 0.01219 -0.00700 C13 1 0.444642 0.455484 0.091858 10.50000 0.04081 0.06250 = 0.05339 0.00533 0.01210 -0.00327 AFIX 43 H13 2 0.490145 0.409918 0.091385 10.50000 -1.20000 AFIX 65 C14 1 0.449847 0.574909 0.119205 10.50000 0.06278 0.08576 = 0.07128 -0.01197 0.00315 -0.05083 AFIX 43 H14 2 0.498833 0.609247 0.137029 10.50000 -1.20000 AFIX 65 C15 1 0.381838 0.643013 0.119912 10.50000 0.05654 0.05223 = 0.06128 -0.03066 0.01893 -0.01774 AFIX 43 H15 2 0.385321 0.722917 0.138209 10.50000 -1.20000 AFIX 65 C16 1 0.308623 0.591692 0.093271 10.50000 0.07115 0.03239 = 0.03782 -0.00518 0.01286 0.00575 AFIX 43 H16 2 0.263120 0.637259 0.093744 10.50000 -1.20000 AFIX 0 O1 5 0.060857 0.296646 0.193935 11.00000 0.04819 0.06536 = 0.05545 0.01432 0.03722 0.02041 O2 5 0.075315 0.398119 0.083499 11.00000 0.06065 0.12156 = 0.06779 0.05733 0.04290 0.05777 O3 5 0.408215 0.004127 0.070251 11.00000 0.05698 0.12722 = 0.05835 0.03213 0.03273 0.05642 O4 5 0.415338 0.014955 0.204372 11.00000 0.07071 0.12641 = 0.04025 -0.00076 0.00030 0.07049 PART -1 O5 5 -0.050468 0.354744 -0.071596 10.50000 0.07326 0.07510 = 0.08821 -0.04393 0.00893 0.02245 PART -2 O6 5 0.053977 0.658536 0.034913 10.50000 0.20157 0.08858 = 0.11470 0.02705 -0.00317 -0.04368 N1 4 0.109112 0.792288 0.133687 10.50000 0.20157 0.08858 = 0.11470 0.02705 -0.00317 -0.04368 C17 1 0.073932 0.698535 0.102065 10.50000 0.20157 0.08858 = 0.11470 0.02705 -0.00317 -0.04368 AFIX 43 H17 2 0.059992 0.647144 0.142702 10.50000 -1.20000 AFIX 0 C18 1 0.153216 0.851678 0.092153 10.50000 0.20157 0.08858 = 0.11470 0.02705 -0.00317 -0.04368 AFIX 137 H18A 2 0.167088 0.801742 0.048324 10.50000 -1.50000 H18B 2 0.200123 0.875831 0.127709 10.50000 -1.50000 H18C 2 0.125796 0.922383 0.069011 10.50000 -1.50000 AFIX 0 C19 1 0.112778 0.811949 0.210759 10.50000 0.20157 0.08858 = 0.11470 0.02705 -0.00317 -0.04368 AFIX 137 H19A 2 0.096801 0.893762 0.219479 10.50000 -1.50000 H19B 2 0.165849 0.800143 0.237366 10.50000 -1.50000 H19C 2 0.078457 0.756810 0.233715 10.50000 -1.50000 AFIX 0 PART 0 CO1 3 0.000000 0.409583 0.250000 10.50000 0.02072 0.05317 = 0.02595 0.00000 0.00855 0.00000 CO2 3 0.000000 0.500000 0.000000 10.50000 0.03510 0.05128 = 0.03951 0.00974 0.01920 0.01728 PART -1 H5A 2 -0.085163 0.392797 -0.114569 10.50000 -1.50000 H5B 2 -0.075789 0.308612 -0.034033 10.50000 -1.50000 HKLF 4 REM sami1602 in C2/c REM R1 = 0.0756 for 1970 Fo > 4sig(Fo) and 0.1048 for all 2691 data REM 254 parameters refined using 12 restraints END WGHT 0.1200 13.3751 REM Highest difference peak 0.796, deepest hole -0.728, 1-sigma level 0.129 Q1 1 0.0000 0.4991 0.2500 10.50000 0.05 0.80 Q2 1 0.0984 0.7022 0.0757 11.00000 0.05 0.72 Q3 1 0.3310 0.5538 0.0802 11.00000 0.05 0.71 Q4 1 0.2506 0.5691 0.0679 11.00000 0.05 0.70 Q5 1 -0.0026 0.5923 0.0071 11.00000 0.05 0.58 Q6 1 0.2295 0.6593 0.0806 11.00000 0.05 0.55 Q7 1 0.3985 0.6095 0.0998 11.00000 0.05 0.53 Q8 1 0.4325 0.0769 0.0928 11.00000 0.05 0.53 Q9 1 0.0425 0.7650 0.2045 11.00000 0.05 0.52 Q10 1 -0.0164 0.3398 -0.0667 11.00000 0.05 0.47 Q11 1 0.0568 0.8507 0.1024 11.00000 0.05 0.47 Q12 1 0.1812 0.8690 0.1483 11.00000 0.05 0.41 Q13 1 -0.0607 0.4165 -0.0793 11.00000 0.05 0.41 Q14 1 0.0314 0.7666 0.0708 11.00000 0.05 0.41 Q15 1 0.4289 0.4050 0.0824 11.00000 0.05 0.40 Q16 1 0.4408 0.5679 0.1387 11.00000 0.05 0.39 Q17 1 0.3773 0.4612 0.0529 11.00000 0.05 0.38 Q18 1 0.0469 0.3199 0.0773 11.00000 0.05 0.36 Q19 1 0.0883 0.9198 0.2817 11.00000 0.05 0.33 Q20 1 0.1584 0.7764 0.0671 11.00000 0.05 0.31 ; _cod_data_source_file c2cc34430k.txt _cod_data_source_block 1 _cod_original_sg_symbol_H-M 'C 2/c' _cod_database_code 7108551 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -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 _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.0957(4) 0.3200(6) 0.1340(4) 0.0368(15) Uani 1 1 d . . . C2 C 0.1693(4) 0.2485(7) 0.1290(4) 0.0391(16) Uani 1 1 d . . . C5 C 0.3080(4) 0.1107(6) 0.1282(4) 0.0368(16) Uani 1 1 d . . . C3A C 0.1842(9) 0.1489(17) 0.1777(11) 0.046(4) Uani 0.50 1 d P . . H3A H 0.1483 0.1268 0.2126 0.056 Uiso 0.50 1 calc PR . . C4A C 0.2528(11) 0.0776(18) 0.1770(12) 0.057(5) Uani 0.50 1 d P . . H4A H 0.2604 0.0083 0.2096 0.069 Uiso 0.50 1 calc PR . . C6A C 0.2968(6) 0.2161(12) 0.0806(8) 0.032(3) Uani 0.50 1 d P . . C7A C 0.2285(7) 0.2884(11) 0.0816(7) 0.030(3) Uani 0.50 1 d P . . C3B C 0.2138(9) 0.212(2) 0.2026(10) 0.053(5) Uani 0.50 1 d P . . H3B H 0.1970 0.2317 0.2526 0.064 Uiso 0.50 1 calc PR . . C4B C 0.2834(10) 0.1476(17) 0.2026(10) 0.050(4) Uani 0.50 1 d P . . H4B H 0.3140 0.1286 0.2527 0.060 Uiso 0.50 1 calc PR . . C6B C 0.2589(7) 0.1353(11) 0.0545(8) 0.031(3) Uani 0.50 1 d P . . C7B C 0.1901(7) 0.2046(12) 0.0544(8) 0.030(3) Uani 0.50 1 d P . . C8 C 0.3845(4) 0.0378(6) 0.1339(4) 0.0380(16) Uani 1 1 d . . . C9 C 0.3553(7) 0.2764(11) 0.0296(7) 0.029(3) Uani 0.50 1 d P . . H9 H 0.4034 0.2288 0.0288 0.035 Uiso 0.50 1 calc PR . . C10 C 0.2275(7) 0.4018(12) 0.0320(8) 0.034(3) Uani 0.50 1 d P . . H10 H 0.1795 0.4496 0.0324 0.041 Uiso 0.50 1 calc PR . . C11 C 0.3034(4) 0.4723(7) 0.0659(6) 0.039(3) Uani 0.50 1 d PG . . C12 C 0.3714(5) 0.4042(6) 0.0652(6) 0.032(3) Uani 0.50 1 d PG . . C13 C 0.4446(4) 0.4555(8) 0.0919(6) 0.052(4) Uani 0.50 1 d PG . . H13 H 0.4901 0.4099 0.0914 0.062 Uiso 0.50 1 calc PR . . C14 C 0.4498(4) 0.5749(9) 0.1192(7) 0.074(6) Uani 0.50 1 d PG . . H14 H 0.4988 0.6092 0.1370 0.089 Uiso 0.50 1 calc PR . . C15 C 0.3818(6) 0.6430(6) 0.1199(7) 0.056(4) Uani 0.50 1 d PG . . H15 H 0.3853 0.7229 0.1382 0.067 Uiso 0.50 1 calc PR . . C16 C 0.3086(5) 0.5917(7) 0.0933(6) 0.047(4) Uani 0.50 1 d PG . . H16 H 0.2631 0.6373 0.0937 0.056 Uiso 0.50 1 calc PR . . O1 O 0.0609(3) 0.2966(5) 0.1939(3) 0.0534(14) Uani 1 1 d . . . O2 O 0.0753(3) 0.3981(6) 0.0835(4) 0.080(2) Uani 1 1 d . A . O3 O 0.4082(3) 0.0041(6) 0.0703(4) 0.078(2) Uani 1 1 d . . . O4 O 0.4153(4) 0.0150(6) 0.2044(3) 0.080(2) Uani 1 1 d . . . O5 O -0.0505(10) 0.3547(16) -0.0716(9) 0.079(5) Uani 0.50 1 d PD A -1 O6 O 0.054(2) 0.659(2) 0.0349(12) 0.138(5) Uani 0.50 1 d PD A -2 N1 N 0.1091(13) 0.7923(16) 0.1337(10) 0.138(5) Uani 0.50 1 d PD A -2 C17 C 0.0739(19) 0.699(2) 0.1021(12) 0.138(5) Uani 0.50 1 d PD A -2 H17 H 0.0600 0.6471 0.1427 0.165 Uiso 0.50 1 calc PR A -2 C18 C 0.1532(16) 0.852(2) 0.0922(14) 0.138(5) Uani 0.50 1 d PD A -2 H18A H 0.1671 0.8017 0.0483 0.206 Uiso 0.50 1 calc PR A -2 H18B H 0.2001 0.8758 0.1277 0.206 Uiso 0.50 1 calc PR A -2 H18C H 0.1258 0.9224 0.0690 0.206 Uiso 0.50 1 calc PR A -2 C19 C 0.1128(18) 0.812(2) 0.2108(13) 0.138(5) Uani 0.50 1 d PD A -2 H19A H 0.0968 0.8938 0.2195 0.206 Uiso 0.50 1 calc PR A -2 H19B H 0.1658 0.8001 0.2374 0.206 Uiso 0.50 1 calc PR A -2 H19C H 0.0785 0.7568 0.2337 0.206 Uiso 0.50 1 calc PR A -2 Co1 Co 0.0000 0.40958(12) 0.2500 0.0328(4) Uani 1 2 d S . . Co2 Co 0.0000 0.5000 0.0000 0.0406(4) Uani 1 2 d SD . . H5A H -0.085(6) 0.3928(17) -0.115(4) 0.061 Uiso 0.50 1 d PD B -1 H5B H -0.076(6) 0.309(6) -0.034(2) 0.061 Uiso 0.50 1 d PD C -1 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 C1 0.028(3) 0.049(4) 0.036(4) 0.000(3) 0.014(3) 0.004(3) C2 0.030(3) 0.058(4) 0.033(4) 0.005(3) 0.017(3) 0.011(3) C5 0.028(3) 0.048(4) 0.038(4) 0.009(3) 0.016(3) 0.012(3) C3A 0.030(8) 0.062(11) 0.051(11) 0.028(9) 0.020(7) 0.005(8) C4A 0.058(11) 0.055(12) 0.069(13) 0.039(10) 0.042(10) 0.030(9) C6A 0.018(6) 0.046(8) 0.035(7) -0.004(6) 0.015(5) 0.002(6) C7A 0.032(6) 0.032(7) 0.028(6) -0.004(5) 0.010(5) 0.003(6) C3B 0.033(9) 0.102(16) 0.029(8) 0.005(9) 0.019(7) 0.019(10) C4B 0.048(10) 0.059(12) 0.044(9) 0.017(9) 0.015(7) 0.027(9) C6B 0.027(6) 0.030(7) 0.038(7) 0.003(6) 0.017(5) -0.001(6) C7B 0.028(6) 0.034(7) 0.032(6) 0.006(6) 0.016(5) 0.006(6) C8 0.028(3) 0.046(4) 0.043(4) 0.006(3) 0.016(3) 0.005(3) C9 0.022(5) 0.036(7) 0.032(6) 0.002(5) 0.012(5) 0.000(5) C10 0.027(6) 0.047(8) 0.032(7) -0.011(6) 0.015(5) -0.001(6) C11 0.042(8) 0.043(8) 0.035(7) 0.003(6) 0.013(6) -0.002(6) C12 0.038(7) 0.029(6) 0.031(6) -0.004(5) 0.012(5) -0.007(6) C13 0.041(8) 0.063(10) 0.053(9) 0.005(8) 0.012(7) -0.003(8) C14 0.063(11) 0.086(14) 0.071(12) -0.012(10) 0.003(9) -0.051(11) C15 0.057(9) 0.052(9) 0.061(10) -0.031(8) 0.019(8) -0.018(8) C16 0.071(10) 0.032(8) 0.038(8) -0.005(6) 0.013(7) 0.006(8) O1 0.048(3) 0.065(3) 0.055(3) 0.014(3) 0.037(2) 0.020(3) O2 0.061(3) 0.122(5) 0.068(4) 0.057(4) 0.043(3) 0.058(4) O3 0.057(3) 0.127(6) 0.058(4) 0.032(4) 0.033(3) 0.056(4) O4 0.071(4) 0.126(6) 0.040(3) -0.001(3) 0.000(3) 0.070(4) O5 0.073(8) 0.075(11) 0.088(11) -0.044(10) 0.009(9) 0.022(8) O6 0.202(13) 0.089(7) 0.115(10) 0.027(8) -0.003(10) -0.044(8) N1 0.202(13) 0.089(7) 0.115(10) 0.027(8) -0.003(10) -0.044(8) C17 0.202(13) 0.089(7) 0.115(10) 0.027(8) -0.003(10) -0.044(8) C18 0.202(13) 0.089(7) 0.115(10) 0.027(8) -0.003(10) -0.044(8) C19 0.202(13) 0.089(7) 0.115(10) 0.027(8) -0.003(10) -0.044(8) Co1 0.0207(6) 0.0532(8) 0.0259(7) 0.000 0.0086(5) 0.000 Co2 0.0351(7) 0.0513(9) 0.0395(8) 0.0097(6) 0.0192(6) 0.0173(6) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 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' 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 O2 C1 O1 124.0(6) . . O2 C1 C2 120.0(6) . . O1 C1 C2 116.0(6) . . C3A C2 C7B 100.3(10) . . C3B C2 C7B 118.3(9) . . C3A C2 C7A 118.4(9) . . C3B C2 C7A 102.1(9) . . C3A C2 C1 118.8(8) . . C3B C2 C1 117.8(8) . . C7B C2 C1 123.4(7) . . C7A C2 C1 122.5(7) . . C4A C5 C6B 99.8(10) . . C4A C5 C6A 119.6(9) . . C6B C5 C4B 118.1(9) . . C6A C5 C4B 101.8(10) . . C4A C5 C8 118.9(8) . . C6B C5 C8 124.1(7) . . C6A C5 C8 121.2(7) . . C4B C5 C8 117.7(8) . . C2 C3A C4A 122.0(13) . . C2 C3A H3A 119.0 . . C4A C3A H3A 119.0 . . C5 C4A C3A 120.1(13) . . C5 C4A H4A 120.0 . . C3A C4A H4A 120.0 . . C6B C6A C5 65.5(10) . . C6B C6A C7A 90.9(10) . . C5 C6A C7A 120.6(10) . . C6B C6A C9 120.8(12) . . C5 C6A C9 127.6(9) . . C7A C6A C9 111.5(11) . . C5 C6A C7B 97.2(8) . . C9 C6A C7B 127.8(10) . . C7B C7A C6A 88.5(10) . . C6A C7A C2 119.0(10) . . C7B C7A C10 119.3(12) . . C6A C7A C10 114.2(11) . . C2 C7A C10 126.7(10) . . C2 C7A C6B 95.5(8) . . C10 C7A C6B 128.5(9) . . C2 C3B C4B 121.0(13) . . C2 C3B H3B 119.5 . . C4B C3B H3B 119.5 . . C3B C4B C5 121.0(14) . . C3B C4B H4B 119.5 . . C5 C4B H4B 119.5 . . C6A C6B C5 65.8(9) . . C6A C6B C7B 90.5(11) . . C5 C6B C7B 120.7(11) . . C6A C6B C10 113.5(12) . 7 C5 C6B C10 126.5(10) . 7 C7B C6B C10 112.7(11) . 7 C5 C6B C7A 97.3(9) . . C10 C6B C7A 123.8(10) 7 . C7A C7B C6B 90.1(11) . . C2 C7B C6B 120.3(10) . . C7A C7B C9 115.1(11) . 7 C2 C7B C9 125.8(9) . 7 C6B C7B C9 113.9(11) . 7 C2 C7B C6A 98.3(9) . . C9 C7B C6A 125.4(9) 7 . O4 C8 O3 125.7(6) . . O4 C8 C5 114.6(6) . . O3 C8 C5 119.7(6) . . C7B C9 C12 105.1(10) 7 . C7B C9 C6A 105.2(9) 7 . C12 C9 C6A 106.7(9) . . C7B C9 H9 113.1 7 . C12 C9 H9 113.1 . . C6A C9 H9 113.1 . . C7A C10 C6B 106.7(10) . 7 C7A C10 C11 106.5(10) . . C6B C10 C11 103.5(9) 7 . C7A C10 H10 113.1 . . C6B C10 H10 113.1 7 . C11 C10 H10 113.1 . . C12 C11 C16 120.0 . . C12 C11 C10 112.9(7) . . C16 C11 C10 127.0(7) . . C11 C12 C13 120.0 . . C11 C12 C9 113.2(7) . . C13 C12 C9 126.7(7) . . C14 C13 C12 120.0 . . C14 C13 H13 120.0 . . C12 C13 H13 120.0 . . C15 C14 C13 120.0 . . C15 C14 H14 120.0 . . C13 C14 H14 120.0 . . C14 C15 C16 120.0 . . C14 C15 H15 120.0 . . C16 C15 H15 120.0 . . C15 C16 C11 120.0 . . C15 C16 H16 120.0 . . C11 C16 H16 120.0 . . C1 O1 Co1 126.2(5) . . C1 O2 Co2 158.1(6) . . C8 O3 Co2 147.6(6) . 3_545 C8 O4 Co1 133.6(5) . 3_545 Co2 O5 H5A 103.8(12) . . Co2 O5 H5B 103.9(12) . . H5A O5 H5B 114.7(14) . . C17 O6 Co2 130(2) . . C18 N1 C17 119.3(7) . . C18 N1 C19 119.6(7) . . C17 N1 C19 119.7(7) . . O6 C17 N1 137(2) . . O6 C17 H17 111.3 . . N1 C17 H17 111.3 . . N1 C18 H18A 109.5 . . N1 C18 H18B 109.5 . . H18A C18 H18B 109.5 . . N1 C18 H18C 109.5 . . H18A C18 H18C 109.5 . . H18B C18 H18C 109.5 . . N1 C19 H19A 109.5 . . N1 C19 H19B 109.5 . . H19A C19 H19B 109.5 . . N1 C19 H19C 109.5 . . H19A C19 H19C 109.5 . . H19B C19 H19C 109.5 . . O4 Co1 O4 105.7(4) 4 3_455 O4 Co1 O1 98.2(3) 4 . O4 Co1 O1 129.3(2) 3_455 . O4 Co1 O1 129.3(2) 4 2 O4 Co1 O1 98.2(3) 3_455 2 O1 Co1 O1 100.0(3) . 2 O6 Co2 O6 180.000(2) . 5_565 O6 Co2 O2 93.8(8) . . O6 Co2 O2 86.2(8) 5_565 . O6 Co2 O2 86.2(8) . 5_565 O6 Co2 O2 93.8(8) 5_565 5_565 O2 Co2 O2 180.0 . 5_565 O6 Co2 O3 100.3(9) . 3_455 O6 Co2 O3 79.7(9) 5_565 3_455 O2 Co2 O3 95.7(2) . 3_455 O2 Co2 O3 84.3(2) 5_565 3_455 O6 Co2 O3 79.7(9) . 7 O6 Co2 O3 100.3(9) 5_565 7 O2 Co2 O3 84.3(2) . 7 O2 Co2 O3 95.7(2) 5_565 7 O3 Co2 O3 180.0(5) 3_455 7 O6 Co2 O5 17.4(8) . 5_565 O6 Co2 O5 162.6(8) 5_565 5_565 O2 Co2 O5 83.1(5) . 5_565 O2 Co2 O5 96.9(5) 5_565 5_565 O3 Co2 O5 87.8(5) 3_455 5_565 O3 Co2 O5 92.2(5) 7 5_565 O6 Co2 O5 162.6(8) . . O6 Co2 O5 17.4(8) 5_565 . O2 Co2 O5 96.9(5) . . O2 Co2 O5 83.1(5) 5_565 . O3 Co2 O5 92.2(5) 3_455 . O3 Co2 O5 87.8(5) 7 . O5 Co2 O5 180.000(1) 5_565 . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 C1 O2 1.209(8) . C1 O1 1.245(8) . C1 C2 1.501(9) . C2 C3A 1.360(17) . C2 C3B 1.387(17) . C2 C7B 1.404(14) . C2 C7A 1.434(14) . C5 C4A 1.372(17) . C5 C6B 1.394(14) . C5 C6A 1.398(15) . C5 C4B 1.403(18) . C5 C8 1.531(8) . C3A C4A 1.42(2) . C3A H3A 0.9300 . C4A H4A 0.9300 . C6A C6B 1.150(17) . C6A C7A 1.420(16) . C6A C9 1.544(16) . C6A C7B 1.826(16) . C7A C7B 1.185(17) . C7A C10 1.489(18) . C7A C6B 1.841(17) . C3B C4B 1.39(2) . C3B H3B 0.9300 . C4B H4B 0.9300 . C6B C7B 1.407(16) . C6B C10 1.520(17) 7 C7B C9 1.491(17) 7 C8 O4 1.222(9) . C8 O3 1.227(9) . C9 C7B 1.491(17) 7 C9 C12 1.534(14) . C9 H9 0.9800 . C10 C6B 1.520(17) 7 C10 C11 1.549(13) . C10 H10 0.9800 . C11 C12 1.3900 . C11 C16 1.3900 . C12 C13 1.3900 . C13 C14 1.3900 . C13 H13 0.9300 . C14 C15 1.3900 . C14 H14 0.9300 . C15 C16 1.3900 . C15 H15 0.9300 . C16 H16 0.9300 . O1 Co1 1.939(5) . O2 Co2 2.070(5) . O3 Co2 2.079(5) 3_545 O4 Co1 1.925(5) 3_545 O5 Co2 2.096(16) . O5 H5A 0.950(5) . O5 H5B 0.949(5) . O6 C17 1.186(10) . O6 Co2 2.02(2) . N1 C18 1.269(16) . N1 C17 1.269(16) . N1 C19 1.270(16) . C17 H17 0.9300 . C18 H18A 0.9600 . C18 H18B 0.9600 . C18 H18C 0.9600 . C19 H19A 0.9600 . C19 H19B 0.9600 . C19 H19C 0.9600 . Co1 O4 1.925(5) 4 Co1 O4 1.925(5) 3_455 Co1 O1 1.939(5) 2 Co2 O6 2.02(2) 5_565 Co2 O2 2.070(5) 5_565 Co2 O3 2.079(5) 3_455 Co2 O3 2.079(5) 7 Co2 O5 2.096(16) 5_565