#------------------------------------------------------------------------------ #$Date: 2021-05-07 05:26:07 +0300 (Fri, 07 May 2021) $ #$Revision: 265025 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/73/7707353.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_7707353 loop_ _publ_author_name 'Wang, Kuiyuan' 'Prior, Timothy J.' 'Hughes, David L.' 'Arbaoui, Abdessamad' 'Redshaw, Carl' _publ_section_title ; Coordination chemistry of [2+2] Schiff-base macrocycles derived from the dianilines [(2-NH2C6H4)2X] (X = CH2CH2, O): Structural studies and ROP capability towards cyclic esters. ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D1DT00711D _journal_year 2021 _chemical_formula_moiety ; C32 H38 Co2 N4 O6, 2(C2 H3 Br3 Co N) ; _chemical_formula_sum 'C36 H44 Br6 Co4 N6 O6' _chemical_formula_weight 1371.95 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2021-01-05 deposited with the CCDC. 2021-05-04 downloaded from the CCDC. ; _cell_angle_alpha 78.04(3) _cell_angle_beta 70.59(2) _cell_angle_gamma 87.78(2) _cell_formula_units_Z 1 _cell_length_a 10.416(2) _cell_length_b 11.156(4) _cell_length_c 11.738(4) _cell_measurement_reflns_used 6138 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 29.7 _cell_measurement_theta_min 1.85 _cell_volume 1257.8(7) _computing_cell_refinement 'Stoe X-AREA' _computing_data_collection 'Stoe X-AREA' _computing_data_reduction ; Scaled and merged with Sortav R.H. Blessing, (1987) Cryst. Rev. 1, 3-58 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397 ; _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT (Sheldrick, 2015)' _diffrn_ambient_temperature 150(2) _diffrn_detector_area_resol_mean 6.67 _diffrn_measured_fraction_theta_full 0.987 _diffrn_measured_fraction_theta_max 0.972 _diffrn_measurement_device_type 'Stoe IPDS2' _diffrn_measurement_method \w-scans _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0442 _diffrn_reflns_av_unetI/netI 0.0815 _diffrn_reflns_Laue_measured_fraction_full 0.987 _diffrn_reflns_Laue_measured_fraction_max 0.972 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 11602 _diffrn_reflns_point_group_measured_fraction_full 0.987 _diffrn_reflns_point_group_measured_fraction_max 0.972 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 29.190 _diffrn_reflns_theta_min 1.867 _diffrn_source 'fine-focus sealed tube' _exptl_absorpt_coefficient_mu 6.105 _exptl_absorpt_correction_T_max 0.820 _exptl_absorpt_correction_T_min 0.725 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; R.H. Blessing, Acta Cryst. (1995), A51, 33-38 ; _exptl_crystal_colour green _exptl_crystal_density_diffrn 1.811 _exptl_crystal_description block _exptl_crystal_F_000 668 _exptl_crystal_size_max 0.310 _exptl_crystal_size_mid 0.130 _exptl_crystal_size_min 0.090 _refine_diff_density_max 0.842 _refine_diff_density_min -0.633 _refine_diff_density_rms 0.107 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.823 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 268 _refine_ls_number_reflns 6632 _refine_ls_number_restraints 36 _refine_ls_restrained_S_all 0.822 _refine_ls_R_factor_all 0.0746 _refine_ls_R_factor_gt 0.0351 _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^)+(0.0312P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0650 _refine_ls_wR_factor_ref 0.0715 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4069 _reflns_number_total 6632 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1dt00711d2.cif _cod_data_source_block FeROP11 _cod_database_code 7707353 _shelx_shelxl_version_number 2018/3 _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_min 0.253 _shelx_estimated_absorpt_t_max 0.610 _shelx_res_file ; TITL shelxt_a.res in P-1 shelx.res created by SHELXL-2018/3 at 17:34:08 on 11-Oct-2019 CELL 0.71073 10.4161 11.1558 11.7379 78.039 70.587 87.777 ZERR 1.00 0.0023 0.0035 0.0040 0.025 0.022 0.022 LATT 1 SFAC C H N O CO BR UNIT 36 44 6 6 4 6 MERG 2 OMIT 10 -1 5 OMIT 8 -4 5 OMIT 11 -2 6 OMIT 2 1 6 rigu c9 > C12 isor c10 > c12 FMAP 2 PLAN 16 SIZE 0.090 0.130 0.310 ACTA BOND $H LIST 6 L.S. 15 TEMP -123.00 WGHT 0.031200 FVAR 0.37305 C1 1 -0.027690 0.581103 0.700659 11.00000 0.02305 0.01407 = 0.02130 -0.00093 -0.00866 -0.00041 C2 1 0.072334 0.662394 0.706528 11.00000 0.02541 0.02020 = 0.01986 -0.00448 -0.00576 -0.00301 C3 1 0.049410 0.711325 0.813238 11.00000 0.03082 0.01807 = 0.02703 -0.00601 -0.01225 -0.00286 AFIX 43 H3 2 0.118021 0.763920 0.814964 11.00000 -1.20000 AFIX 0 C4 1 -0.066992 0.686869 0.914807 11.00000 0.03226 0.01883 = 0.02243 -0.00850 -0.00885 0.00187 C5 1 -0.162355 0.606162 0.908663 11.00000 0.02936 0.01804 = 0.02089 -0.00483 -0.00458 -0.00118 AFIX 43 H5 2 -0.243144 0.585881 0.977790 11.00000 -1.20000 AFIX 0 C6 1 -0.146020 0.553223 0.806526 11.00000 0.02656 0.01532 = 0.02227 -0.00231 -0.00643 -0.00153 C7 1 0.201223 0.696891 0.610954 11.00000 0.02856 0.02494 = 0.02781 -0.00828 -0.01066 -0.00457 AFIX 43 H7 2 0.259850 0.748084 0.628629 11.00000 -1.20000 AFIX 0 C8 1 -0.252592 0.465962 0.819965 11.00000 0.02122 0.02753 = 0.01993 -0.00453 -0.00288 0.00048 AFIX 43 H8 2 -0.325827 0.453130 0.896044 11.00000 -1.20000 AFIX 0 C9 1 -0.089874 0.748187 1.025487 11.00000 0.04097 0.02598 = 0.02278 -0.01135 -0.00406 -0.00653 C10 1 -0.177723 0.665971 1.143715 11.00000 0.16298 0.09999 = 0.02343 -0.02455 0.01751 -0.08663 AFIX 137 H10A 2 -0.177983 0.699590 1.214584 11.00000 -1.50000 H10B 2 -0.140958 0.583582 1.150513 11.00000 -1.50000 H10C 2 -0.271025 0.661588 1.142481 11.00000 -1.50000 AFIX 0 C11 1 0.045740 0.770509 1.045455 11.00000 0.06796 0.08050 = 0.05093 -0.03830 -0.02957 0.00619 AFIX 137 H11A 2 0.101325 0.833012 0.976680 11.00000 -1.50000 H11B 2 0.095035 0.693962 1.049403 11.00000 -1.50000 H11C 2 0.026938 0.798720 1.122955 11.00000 -1.50000 AFIX 0 C12 1 -0.153738 0.869850 1.000273 11.00000 0.11754 0.06144 = 0.06942 -0.04989 -0.05267 0.04505 AFIX 137 H12A 2 -0.236840 0.857537 0.981888 11.00000 -1.50000 H12B 2 -0.089464 0.924324 0.929484 11.00000 -1.50000 H12C 2 -0.176480 0.906886 1.073033 11.00000 -1.50000 AFIX 0 C13 1 0.327304 0.347842 0.498069 11.00000 0.02083 0.03518 = 0.02254 -0.00480 -0.00103 -0.00391 C14 1 0.421295 0.255365 0.525037 11.00000 0.03068 0.04660 = 0.03830 -0.00390 -0.01238 0.00850 AFIX 137 H14A 2 0.502419 0.295557 0.526806 11.00000 -1.50000 H14B 2 0.447983 0.206416 0.460973 11.00000 -1.50000 H14C 2 0.376817 0.201808 0.605504 11.00000 -1.50000 AFIX 0 C15 1 0.001556 0.836057 0.380476 11.00000 0.02275 0.03065 = 0.02573 -0.00287 -0.00546 -0.00658 C16 1 -0.057589 0.956026 0.364280 11.00000 0.03250 0.03124 = 0.05065 -0.00070 -0.01222 0.00614 AFIX 137 H16A 2 0.013351 1.019933 0.342814 11.00000 -1.50000 H16B 2 -0.129181 0.964001 0.441240 11.00000 -1.50000 H16C 2 -0.096788 0.964981 0.297874 11.00000 -1.50000 AFIX 0 C17 1 0.558942 0.171817 -0.084208 11.00000 0.03444 0.04521 = 0.03409 -0.00411 -0.00770 -0.01736 C18 1 0.578627 0.158881 -0.209384 11.00000 0.06947 0.07033 = 0.03579 -0.01359 -0.00734 -0.03785 AFIX 137 H18A 2 0.497506 0.118867 -0.211363 11.00000 -1.50000 H18B 2 0.657993 0.108964 -0.237215 11.00000 -1.50000 H18C 2 0.593674 0.240081 -0.264082 11.00000 -1.50000 AFIX 0 N1 3 0.253739 0.419638 0.478258 11.00000 0.02192 0.03558 = 0.02946 -0.01051 -0.00575 0.00056 N2 3 0.047494 0.743108 0.392273 11.00000 0.03004 0.02637 = 0.03387 -0.00806 -0.01033 0.00030 N3 3 0.540973 0.180680 0.014527 11.00000 0.04089 0.04834 = 0.03663 -0.00777 -0.01473 -0.00667 O1 4 -0.007709 0.531875 0.604924 11.00000 0.02227 0.02388 = 0.01839 -0.00915 -0.00217 -0.00466 O2 4 0.245556 0.668635 0.508973 11.00000 0.02456 0.03111 = 0.02694 -0.01063 -0.00256 -0.00942 O3 4 -0.259379 0.406255 0.744026 11.00000 0.02531 0.02638 = 0.02259 -0.00892 -0.00316 -0.00661 CO1 5 0.140312 0.572611 0.435264 11.00000 0.02030 0.02169 = 0.02096 -0.00814 -0.00400 -0.00335 CO2 5 0.504541 0.196842 0.191281 11.00000 0.02665 0.03126 = 0.02824 -0.00382 -0.00957 -0.00345 BR1 6 0.567604 0.401152 0.185318 11.00000 0.03721 0.02855 = 0.03589 -0.00106 -0.00395 -0.00524 BR2 6 0.271307 0.138603 0.299632 11.00000 0.02687 0.04743 = 0.04603 -0.00084 -0.01061 -0.00732 BR3 6 0.647464 0.055887 0.271189 11.00000 0.03402 0.02536 = 0.05408 -0.00901 -0.02325 -0.00062 HKLF 4 REM shelxt_a.res in P-1 REM wR2 = 0.0715, GooF = S = 0.823, Restrained GooF = 0.822 for all data REM R1 = 0.0351 for 4069 Fo > 4sig(Fo) and 0.0746 for all 6632 data REM 268 parameters refined using 36 restraints END WGHT 0.0312 0.0000 REM Highest difference peak 0.842, deepest hole -0.633, 1-sigma level 0.107 Q1 1 0.3005 0.1158 0.2218 11.00000 0.05 0.84 Q2 1 0.5811 0.3790 0.1015 11.00000 0.05 0.80 Q3 1 0.6288 0.0960 0.3433 11.00000 0.05 0.79 Q4 1 0.1673 0.5467 0.3642 11.00000 0.05 0.75 Q5 1 0.5142 0.1876 0.1082 11.00000 0.05 0.72 Q6 1 0.5533 0.4281 0.2657 11.00000 0.05 0.68 Q7 1 0.6783 0.0367 0.1879 11.00000 0.05 0.67 Q8 1 0.5496 0.3913 0.2691 11.00000 0.05 0.67 Q9 1 0.1144 0.6055 0.5055 11.00000 0.05 0.65 Q10 1 0.2565 0.1731 0.3818 11.00000 0.05 0.63 Q11 1 0.4909 0.2067 0.2741 11.00000 0.05 0.52 Q12 1 0.2794 0.1287 0.3797 11.00000 0.05 0.50 Q13 1 0.5385 0.2733 0.0978 11.00000 0.05 0.46 Q14 1 0.5803 0.4373 0.0992 11.00000 0.05 0.42 Q15 1 0.5885 0.0412 0.3599 11.00000 0.05 0.41 Q16 1 0.0690 0.6651 0.7788 11.00000 0.05 0.41 ; _shelx_res_checksum 11927 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -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 C1 C -0.0277(3) 0.5811(3) 0.7007(3) 0.0195(7) Uani 1 1 d . . . . . C2 C 0.0723(4) 0.6624(3) 0.7065(3) 0.0221(7) Uani 1 1 d . . . . . C3 C 0.0494(4) 0.7113(3) 0.8132(3) 0.0243(7) Uani 1 1 d . . . . . H3 H 0.118021 0.763920 0.814964 0.029 Uiso 1 1 calc R U . . . C4 C -0.0670(4) 0.6869(3) 0.9148(3) 0.0239(7) Uani 1 1 d . . . . . C5 C -0.1624(4) 0.6062(3) 0.9087(3) 0.0235(7) Uani 1 1 d . . . . . H5 H -0.243144 0.585881 0.977790 0.028 Uiso 1 1 calc R U . . . C6 C -0.1460(4) 0.5532(3) 0.8065(3) 0.0220(7) Uani 1 1 d . . . . . C7 C 0.2012(4) 0.6969(3) 0.6110(3) 0.0262(8) Uani 1 1 d . . . . . H7 H 0.259850 0.748084 0.628629 0.031 Uiso 1 1 calc R U . . . C8 C -0.2526(4) 0.4660(3) 0.8200(3) 0.0239(7) Uani 1 1 d . . . . . H8 H -0.325827 0.453130 0.896044 0.029 Uiso 1 1 calc R U . . . C9 C -0.0899(4) 0.7482(3) 1.0255(3) 0.0304(8) Uani 1 1 d . . . . . C10 C -0.1777(8) 0.6660(6) 1.1437(4) 0.103(3) Uani 1 1 d . U . . . H10A H -0.177983 0.699590 1.214584 0.155 Uiso 1 1 calc R U . . . H10B H -0.140958 0.583582 1.150513 0.155 Uiso 1 1 calc R U . . . H10C H -0.271025 0.661588 1.142481 0.155 Uiso 1 1 calc R U . . . C11 C 0.0457(5) 0.7705(5) 1.0455(5) 0.0603(14) Uani 1 1 d . U . . . H11A H 0.101325 0.833012 0.976680 0.090 Uiso 1 1 calc R U . . . H11B H 0.095035 0.693962 1.049403 0.090 Uiso 1 1 calc R U . . . H11C H 0.026938 0.798720 1.122955 0.090 Uiso 1 1 calc R U . . . C12 C -0.1537(7) 0.8699(5) 1.0003(5) 0.0729(18) Uani 1 1 d . U . . . H12A H -0.236840 0.857537 0.981888 0.109 Uiso 1 1 calc R U . . . H12B H -0.089464 0.924324 0.929484 0.109 Uiso 1 1 calc R U . . . H12C H -0.176480 0.906886 1.073033 0.109 Uiso 1 1 calc R U . . . C13 C 0.3273(4) 0.3478(3) 0.4981(3) 0.0278(8) Uani 1 1 d . . . . . C14 C 0.4213(4) 0.2554(4) 0.5250(4) 0.0392(9) Uani 1 1 d . . . . . H14A H 0.502419 0.295557 0.526806 0.059 Uiso 1 1 calc R U . . . H14B H 0.447983 0.206416 0.460973 0.059 Uiso 1 1 calc R U . . . H14C H 0.376817 0.201808 0.605504 0.059 Uiso 1 1 calc R U . . . C15 C 0.0016(4) 0.8361(3) 0.3805(3) 0.0273(8) Uani 1 1 d . . . . . C16 C -0.0576(4) 0.9560(4) 0.3643(4) 0.0399(10) Uani 1 1 d . . . . . H16A H 0.013351 1.019933 0.342814 0.060 Uiso 1 1 calc R U . . . H16B H -0.129181 0.964001 0.441240 0.060 Uiso 1 1 calc R U . . . H16C H -0.096788 0.964981 0.297874 0.060 Uiso 1 1 calc R U . . . C17 C 0.5589(4) 0.1718(4) -0.0842(4) 0.0389(10) Uani 1 1 d . . . . . C18 C 0.5786(5) 0.1589(5) -0.2094(4) 0.0596(15) Uani 1 1 d . . . . . H18A H 0.497506 0.118867 -0.211363 0.089 Uiso 1 1 calc R U . . . H18B H 0.657993 0.108964 -0.237215 0.089 Uiso 1 1 calc R U . . . H18C H 0.593674 0.240081 -0.264082 0.089 Uiso 1 1 calc R U . . . N1 N 0.2537(3) 0.4196(3) 0.4783(3) 0.0291(7) Uani 1 1 d . . . . . N2 N 0.0475(3) 0.7431(3) 0.3923(3) 0.0299(7) Uani 1 1 d . . . . . N3 N 0.5410(4) 0.1807(3) 0.0145(3) 0.0414(8) Uani 1 1 d . . . . . O1 O -0.0077(2) 0.5319(2) 0.60492(19) 0.0218(5) Uani 1 1 d . . . . . O2 O 0.2456(2) 0.6686(2) 0.5090(2) 0.0281(6) Uani 1 1 d . . . . . O3 O -0.2594(2) 0.4063(2) 0.7440(2) 0.0252(5) Uani 1 1 d . . . . . Co1 Co 0.14031(5) 0.57261(4) 0.43526(4) 0.02102(11) Uani 1 1 d . . . . . Co2 Co 0.50454(5) 0.19684(5) 0.19128(5) 0.02883(12) Uani 1 1 d . . . . . Br1 Br 0.56760(4) 0.40115(4) 0.18532(4) 0.03664(10) Uani 1 1 d . . . . . Br2 Br 0.27131(4) 0.13860(4) 0.29963(4) 0.04160(11) Uani 1 1 d . . . . . Br3 Br 0.64746(4) 0.05589(3) 0.27119(4) 0.03545(10) 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 C1 0.0231(18) 0.0141(15) 0.0213(16) -0.0009(12) -0.0087(14) -0.0004(13) C2 0.0254(19) 0.0202(17) 0.0199(16) -0.0045(13) -0.0058(14) -0.0030(14) C3 0.031(2) 0.0181(17) 0.0270(18) -0.0060(14) -0.0122(16) -0.0029(14) C4 0.032(2) 0.0188(17) 0.0224(17) -0.0085(13) -0.0088(15) 0.0019(14) C5 0.029(2) 0.0180(16) 0.0209(16) -0.0048(13) -0.0046(15) -0.0012(14) C6 0.0266(19) 0.0153(16) 0.0223(17) -0.0023(13) -0.0064(15) -0.0015(14) C7 0.029(2) 0.0249(18) 0.0278(19) -0.0083(15) -0.0107(16) -0.0046(15) C8 0.0212(18) 0.0275(18) 0.0199(17) -0.0045(14) -0.0029(14) 0.0005(14) C9 0.041(2) 0.0260(18) 0.0228(17) -0.0114(14) -0.0041(16) -0.0065(16) C10 0.163(7) 0.100(5) 0.023(2) -0.025(3) 0.018(3) -0.087(5) C11 0.068(3) 0.081(4) 0.051(3) -0.038(3) -0.030(3) 0.006(3) C12 0.118(5) 0.061(3) 0.069(3) -0.050(3) -0.053(4) 0.045(3) C13 0.021(2) 0.035(2) 0.0225(18) -0.0048(15) -0.0010(15) -0.0039(17) C14 0.031(2) 0.047(2) 0.038(2) -0.0039(19) -0.0124(19) 0.0085(19) C15 0.0228(19) 0.031(2) 0.0257(19) -0.0029(15) -0.0055(15) -0.0066(16) C16 0.032(2) 0.031(2) 0.051(3) -0.0007(18) -0.012(2) 0.0061(18) C17 0.034(2) 0.045(2) 0.034(2) -0.0041(18) -0.0077(18) -0.0174(19) C18 0.069(4) 0.070(3) 0.036(2) -0.014(2) -0.007(2) -0.038(3) N1 0.0219(17) 0.0356(18) 0.0295(16) -0.0105(14) -0.0058(13) 0.0006(14) N2 0.0300(18) 0.0264(17) 0.0339(17) -0.0081(13) -0.0103(14) 0.0003(14) N3 0.041(2) 0.048(2) 0.037(2) -0.0078(16) -0.0147(17) -0.0067(17) O1 0.0223(13) 0.0239(12) 0.0184(11) -0.0091(9) -0.0022(10) -0.0047(10) O2 0.0246(14) 0.0311(14) 0.0269(13) -0.0106(11) -0.0026(11) -0.0094(11) O3 0.0253(14) 0.0264(13) 0.0226(12) -0.0089(10) -0.0032(10) -0.0066(10) Co1 0.0203(3) 0.0217(2) 0.0210(2) -0.00814(18) -0.00400(19) -0.00335(18) Co2 0.0266(3) 0.0313(3) 0.0282(3) -0.0038(2) -0.0096(2) -0.0035(2) Br1 0.0372(2) 0.0286(2) 0.0359(2) -0.00106(16) -0.00395(18) -0.00524(17) Br2 0.0269(2) 0.0474(3) 0.0460(2) -0.00084(19) -0.01061(18) -0.00732(18) Br3 0.0340(2) 0.0254(2) 0.0541(3) -0.00901(17) -0.02325(19) -0.00062(16) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 '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 O1 C1 C6 122.1(3) . . ? O1 C1 C2 121.5(3) . . ? C6 C1 C2 116.4(3) . . ? C3 C2 C1 120.1(3) . . ? C3 C2 C7 115.3(3) . . ? C1 C2 C7 124.5(3) . . ? C4 C3 C2 123.5(3) . . ? C4 C3 H3 118.2 . . ? C2 C3 H3 118.2 . . ? C3 C4 C5 115.7(3) . . ? C3 C4 C9 121.3(3) . . ? C5 C4 C9 123.0(3) . . ? C4 C5 C6 123.9(3) . . ? C4 C5 H5 118.1 . . ? C6 C5 H5 118.1 . . ? C5 C6 C1 120.3(3) . . ? C5 C6 C8 115.9(3) . . ? C1 C6 C8 123.7(3) . . ? O2 C7 C2 128.4(3) . . ? O2 C7 H7 115.8 . . ? C2 C7 H7 115.8 . . ? O3 C8 C6 127.7(3) . . ? O3 C8 H8 116.1 . . ? C6 C8 H8 116.1 . . ? C12 C9 C10 111.6(5) . . ? C12 C9 C4 108.4(3) . . ? C10 C9 C4 110.7(3) . . ? C12 C9 C11 108.6(4) . . ? C10 C9 C11 106.1(4) . . ? C4 C9 C11 111.4(3) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N1 C13 C14 179.4(4) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N2 C15 C16 179.6(4) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N3 C17 C18 178.6(4) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C13 N1 Co1 171.5(3) . . ? C15 N2 Co1 172.3(3) . . ? C17 N3 Co2 178.8(4) . . ? C1 O1 Co1 129.2(2) . . ? C1 O1 Co1 129.4(2) . 2_566 ? Co1 O1 Co1 99.59(9) . 2_566 ? C7 O2 Co1 126.0(2) . . ? C8 O3 Co1 127.5(2) . 2_566 ? O3 Co1 O1 167.74(8) 2_566 . ? O3 Co1 O2 103.68(10) 2_566 . ? O1 Co1 O2 88.56(9) . . ? O3 Co1 O1 87.35(9) 2_566 2_566 ? O1 Co1 O1 80.41(9) . 2_566 ? O2 Co1 O1 168.96(9) . 2_566 ? O3 Co1 N1 88.92(11) 2_566 . ? O1 Co1 N1 92.50(11) . . ? O2 Co1 N1 87.22(11) . . ? O1 Co1 N1 92.82(10) 2_566 . ? O3 Co1 N2 89.89(11) 2_566 . ? O1 Co1 N2 90.32(11) . . ? O2 Co1 N2 85.44(11) . . ? O1 Co1 N2 94.95(11) 2_566 . ? N1 Co1 N2 172.07(11) . . ? N3 Co2 Br1 107.23(10) . . ? N3 Co2 Br2 106.48(10) . . ? Br1 Co2 Br2 115.68(4) . . ? N3 Co2 Br3 106.79(11) . . ? Br1 Co2 Br3 110.03(3) . . ? Br2 Co2 Br3 110.17(4) . . ? 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 C1 O1 1.304(4) . ? C1 C6 1.418(5) . ? C1 C2 1.435(4) . ? C2 C3 1.414(4) . ? C2 C7 1.438(5) . ? C3 C4 1.377(5) . ? C3 H3 0.9500 . ? C4 C5 1.395(5) . ? C4 C9 1.537(4) . ? C5 C6 1.402(4) . ? C5 H5 0.9500 . ? C6 C8 1.452(5) . ? C7 O2 1.234(4) . ? C7 H7 0.9500 . ? C8 O3 1.239(4) . ? C8 H8 0.9500 . ? C9 C12 1.506(6) . ? C9 C10 1.516(6) . ? C9 C11 1.544(6) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 N1 1.130(5) . ? C13 C14 1.454(6) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 N2 1.127(5) . ? C15 C16 1.454(5) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 N3 1.136(5) . ? C17 C18 1.452(6) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? N1 Co1 2.108(3) . ? N2 Co1 2.143(3) . ? N3 Co2 2.027(4) . ? O1 Co1 2.046(2) . ? O1 Co1 2.068(2) 2_566 ? O2 Co1 2.050(2) . ? O3 Co1 2.026(2) 2_566 ? Co2 Br1 2.3771(10) . ? Co2 Br2 2.3807(10) . ? Co2 Br3 2.3883(9) . ?