# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 1350 loop_ _publ_author_name 'Francesca Fabbiani' 'Gernot Buth' 'Birger Dittrich' 'Heidrun Sowa' _publ_contact_author_name 'Francesca Fabbiani' _publ_contact_author_email FFABBIA@GWDG.DE _publ_section_title ; Pressure-induced structural changes in wet vitamin B12 ; # Attachment 'b12_Fabbiani_combined.cif' data_B12_ambient_pressure _database_code_depnum_ccdc_archive 'CCDC 766943' #TrackingRef 'b12_Fabbiani_combined.cif' #B12_room_pressure_and_temperature _refine_special_details ; All H-atoms were placed geometrically and allowed to ride on the parent atoms. H-Uiso were assigned in the range 1.2-1.5 times Ueq of the parent atom. Water O atoms (OW) were assigned based on the peak height of Fourier difference peaks: OW1-OW5 were assigned full site occupancy and anisotropic displacement parameters were refined. OW6-OW13 were assigned half site occupancy and isotropic displacemen parameters were refined. Any attempt to add further water O-atoms resulted in unusally large displacement parameters and/or unreasonably small occupancy factors. A threshold of Uiso max. = 0.3 A^2^ was used for assignment of meaningful OW sites. The Following ALERTS were generated by PLATON checkcif<<< PLAT602_ALERT_2_A VERY LARGE Solvent Accessible VOID(S) in Structure ! PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) ....... OW1 PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) ....... OW2 PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) ....... OW3 PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) ....... OW4 PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) ....... OW5 PLAT430_ALERT_2_A Short Inter D...A Contact OW11 .. O51 .. 2.45 Ang. PLAT430_ALERT_2_B Short Inter D...A Contact OW1 .. O4P .. 2.71 Ang. PLAT430_ALERT_2_B Short Inter D...A Contact OW1 .. OW3 .. 2.78 Ang. PLAT430_ALERT_2_B Short Inter D...A Contact OW1 .. OW2 .. 2.79 Ang. PLAT430_ALERT_2_B Short Inter D...A Contact OW3 .. O39 .. 2.63 Ang. PLAT430_ALERT_2_B Short Inter D...A Contact OW3 .. O5P .. 2.68 Ang. PLAT430_ALERT_2_B Short Inter D...A Contact OW4 .. O4P .. 2.74 Ang. PLAT430_ALERT_2_B Short Inter D...A Contact OW4 .. O62 .. 2.77 Ang. PLAT430_ALERT_2_B Short Inter D...A Contact OW4 .. OW13 .. 2.78 Ang. PLAT430_ALERT_2_B Short Inter D...A Contact OW5 .. O58 .. 2.76 Ang. PLAT430_ALERT_2_B Short Inter D...A Contact OW7 .. OW9 .. 2.56 Ang. PLAT430_ALERT_2_B Short Inter D...A Contact OW7 .. OW8 .. 2.78 Ang. PLAT430_ALERT_2_B Short Inter D...A Contact OW8 .. O33 .. 2.57 Ang. PLAT430_ALERT_2_B Short Inter D...A Contact OW9 .. O33 .. 2.81 Ang. PLAT430_ALERT_2_B Short Inter D...A Contact OW10 .. OW13 .. 2.66 Ang. PLAT430_ALERT_2_C Short Inter D...A Contact OW3 .. OW5 .. 2.88 Ang. PLAT420_ALERT_2_C D-H Without Acceptor N45 - H45A ... ? These alerts arise because of missing water molecules in the model resulting in apparent large structural voids and missing H-bonds PLAT029_ALERT_3_B _diffrn_measured_fraction_theta_full Low ....... 0.96 PLAT952_ALERT_1_C Reported and Calculated Lmax Values Differ by .. 2 Resolution and completeness are reported below: #=============================================================================== Resolution & Completeness Statistics (Cumulative) #=============================================================================== Theta sin(th)/Lambda Complete Expected Measured Missing #------------------------------------------------------------------------------- 20.82 0.500 0.999 5236 5231 5 23.01 0.550 0.999 6911 6906 5 25.24 0.600 0.993 8893 8830 63 #----------------------------------------------------------- ACTA Min. Res. ---- 27.51 0.650 0.985 11255 11087 168 29.84 0.700 0.977 13991 13671 320 30.79 0.720 0.959 15211 14590 621 PLAT222_ALERT_3_A Large Non-Solvent H Ueq(max)/Ueq(min) ... 5.02 Ratio Some terminal H-atoms have high isotropic dispacement parameters. From this room- temperature data there is evidence of large thermal motion, as well as some unresolved disorder in some amide side chains. Both disodered density and thermal motion are modelled by the anisotropic displacement parameters, which as a reulst are comparably large. PLAT242_ALERT_2_A Check Low Ueq as Compared to Neighbors for C27 PLAT220_ALERT_2_B Large Non-Solvent O Ueq(max)/Ueq(min) ... 4.18 Ratio PLAT242_ALERT_2_B Check Low Ueq as Compared to Neighbors for C32 PLAT213_ALERT_2_C Atom O28 has ADP max/min Ratio ..... 3.70 prola PLAT230_ALERT_2_C Hirshfeld Test Diff for C2 -- C26 5.24 su PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C38 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C43 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C50 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C61 >From this room-temperature data there is evidence of large thermal motion, as well as some possible unresolved disorder in some amide side chains. The data indicate that O28 bound to C27 particularly affected. Both disodered density and thermal motion are modelled by the anisotropic displacement parameters, which as a reulst are comparably large. PLAT412_ALERT_2_C Short Intra XH3 .. XHn H3 .. H35A .. 1.88 Ang. PLAT412_ALERT_2_C Short Intra XH3 .. XHn H35B .. H36C .. 1.83 Ang. Alerts of short H .. H contact involving methyl H-atoms often arise from the fact that they involve H-atoms at not optimal calculated positions. PLAT043_ALERT_1_A Check Reported Molecular Weight ................ 1778.75 CHEMW03_ALERT_2_A ALERT: The ratio of given/expected molecular weight as calculated from the _atom_site* data lies outside the range 0.90 <> 1.10 From the CIF: _cell_formula_units_Z 4 From the CIF: _chemical_formula_weight 1778.75 TEST: Calculate formula weight from _atom_site_* atom mass num sum C 12.01 63.00 756.69 H 1.01 88.00 88.70 N 14.01 14.00 196.10 O 16.00 23.00 367.98 P 30.97 1.00 30.97 Co 58.93 1.00 58.93 Calculated formula weight 1499.38 PLAT041_ALERT_1_C Calc. and Reported SumFormula Strings Differ ? PLAT042_ALERT_1_C Calc. and Reported MoietyFormula Strings Differ ? The formula reflects the results of the PLATON squeeze calculation. Water H-atoms were included in the molecular formula but not in the model. PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for P1 PLAT234_ALERT_4_C Large Hirshfeld Difference C31 -- C32 .. 0.15 Ang PLAT234_ALERT_4_C Large Hirshfeld Difference C49 -- C50 .. 0.15 Ang PLAT731_ALERT_1_C Bond Calc 1.323(9), Rep 1.324(4) ...... 2.25 su-Ra C43 -N45 1.555 1.555 PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Co -- C1C .. 6.29 su PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 5 O PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 6 O PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 7 O PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 11 O All noted, all OK. The C43-N45 bond was subject to a distance restraint and the bond length reported in the .cif is correct. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; 5,6-Dimethylbenzimidazolyl cyanocobamide hydrate ; _chemical_name_common 'cyanocobalamin hydrate' _chemical_melting_point ? _chemical_formula_moiety 'C63 H88 Co N14 O14 P, 23.5 H2O' _chemical_formula_sum 'C63 H135 Co N14 O37.5 P' _chemical_formula_weight 1778.75 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' P P 0.1023 0.0942 '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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' loop_ _symmetry_equiv_pos_as_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' _cell_length_a 15.8260(9) _cell_length_b 22.4438(13) _cell_length_c 25.4429(16) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9037.2(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 9393 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 27.17 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.307 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3812 _exptl_absorpt_coefficient_mu 0.298 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'based on symmetry-related measuraments' # SADABS (Siemens, 2008) # The following data are from Sadabs: _exptl_absorpt_correction_T_min 0.6557 _exptl_absorpt_correction_T_max 0.7461 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_measurement_device 'Bruker AXS SMART APEX' _diffrn_measurement_device_type Area _diffrn_radiation_monochromator silicon _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method '\f & \w scans' _diffrn_reflns_number 101570 _diffrn_reflns_av_R_equivalents 0.0436 _diffrn_reflns_av_sigmaI/netI 0.0389 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_reduction_process ; Merged with XPREP ; #_diffrn_reflns_limit_h_min -20 #_diffrn_reflns_limit_h_max 22 #_diffrn_reflns_limit_k_min -32 #_diffrn_reflns_limit_k_max 27 #_diffrn_reflns_limit_l_min -34 #_diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.21 _diffrn_reflns_theta_max 30.79 _reflns_number_total 26484 _reflns_number_gt 19937 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex2 (Bruker AXS, 2006)' _computing_cell_refinement 'Apex2 (Bruker AXS, 2006)' _computing_data_reduction 'Apex2 (Bruker AXS, 2006)' _computing_structure_solution 'known coordinates' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_publication_material 'COOT, PLATON, XCIF, ENCIFER, MERCURY' _computing_molecular_graphics 'MERCURY, COOT' _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1552P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary 'known coordinates' _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _chemical_absolute_configuration rm _refine_ls_abs_structure_Flack 0.014(11) _refine_ls_number_reflns 26484 _refine_ls_number_parameters 917 _refine_ls_number_restraints 168 _refine_ls_R_factor_all 0.0932 _refine_ls_R_factor_gt 0.0731 _refine_ls_wR_factor_ref 0.2254 _refine_ls_wR_factor_gt 0.2060 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.022 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 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 Co Co 0.22928(2) 0.896943(14) 0.238729(15) 0.04515(9) Uani 1 1 d . . . C1 C 0.34507(16) 0.81117(12) 0.28317(12) 0.0488(5) Uani 1 1 d U . . C2 C 0.44203(18) 0.79662(13) 0.27333(13) 0.0550(6) Uani 1 1 d U . . C3 C 0.48164(18) 0.86035(15) 0.27466(14) 0.0593(7) Uani 1 1 d U . . H3 H 0.5293 0.8617 0.2501 0.071 Uiso 1 1 calc R . . C4 C 0.41016(16) 0.89777(13) 0.25277(12) 0.0529(6) Uani 1 1 d U . . C5 C 0.42275(18) 0.95440(15) 0.22837(15) 0.0632(8) Uani 1 1 d U . . C6 C 0.35617(18) 0.99133(13) 0.21839(14) 0.0576(6) Uani 1 1 d U . . C7 C 0.3591(2) 1.05491(15) 0.19596(16) 0.0659(8) Uani 1 1 d U . . C8 C 0.2718(2) 1.07841(13) 0.21211(15) 0.0628(7) Uani 1 1 d U . . H8 H 0.2490 1.1049 0.1850 0.075 Uiso 1 1 calc R . . C9 C 0.2212(2) 1.02169(12) 0.21499(14) 0.0585(7) Uani 1 1 d U . . C10 C 0.1349(2) 1.01833(13) 0.20564(16) 0.0654(8) Uani 1 1 d U . . H10 H 0.1070 1.0540 0.1989 0.079 Uiso 1 1 calc R . . C11 C 0.0864(2) 0.96692(13) 0.20545(15) 0.0608(7) Uani 1 1 d U . . C12 C -0.0029(2) 0.96341(16) 0.1851(2) 0.0800(11) Uani 1 1 d U . . C13 C -0.0341(2) 0.90596(14) 0.21178(17) 0.0663(8) Uani 1 1 d U . . H13 H -0.0709 0.8839 0.1877 0.080 Uiso 1 1 calc R . . C14 C 0.04784(17) 0.87249(13) 0.21928(14) 0.0537(6) Uani 1 1 d U . . C15 C 0.05403(18) 0.81232(12) 0.22779(13) 0.0550(6) Uani 1 1 d U . . C16 C 0.13332(16) 0.78501(10) 0.24176(12) 0.0474(5) Uani 1 1 d U . . C17 C 0.15184(19) 0.71730(11) 0.24630(12) 0.0509(6) Uani 1 1 d U . . C18 C 0.24014(18) 0.71829(11) 0.27274(12) 0.0526(6) Uani 1 1 d U . . H18 H 0.2318 0.7223 0.3107 0.063 Uiso 1 1 calc R . . C19 C 0.27762(16) 0.77638(11) 0.25258(11) 0.0487(5) Uani 1 1 d U . . H19 H 0.2990 0.7694 0.2170 0.058 Uiso 1 1 calc R . . C20 C 0.32126(18) 0.81226(13) 0.34145(12) 0.0533(6) Uani 1 1 d U . . H20A H 0.3636 0.8337 0.3608 0.080 Uiso 1 1 calc R . . H20B H 0.3177 0.7722 0.3544 0.080 Uiso 1 1 calc R . . H20C H 0.2676 0.8316 0.3457 0.080 Uiso 1 1 calc R . . N21 N 0.33788(13) 0.87221(10) 0.25993(10) 0.0473(4) Uani 1 1 d . . . N22 N 0.27183(15) 0.97563(10) 0.22563(10) 0.0533(5) Uani 1 1 d . . . N23 N 0.11359(14) 0.91362(10) 0.22041(11) 0.0501(5) Uani 1 1 d . . . N24 N 0.20251(13) 0.81566(9) 0.24864(9) 0.0462(5) Uani 1 1 d . . . C25 C 0.4814(2) 0.75384(17) 0.31299(17) 0.0705(9) Uani 1 1 d . . . H25A H 0.4725 0.7687 0.3479 0.106 Uiso 1 1 calc R . . H25B H 0.5409 0.7505 0.3064 0.106 Uiso 1 1 calc R . . H25C H 0.4555 0.7153 0.3096 0.106 Uiso 1 1 calc R . . C26 C 0.4534(2) 0.77231(18) 0.21583(17) 0.0691(9) Uani 1 1 d . . . H26A H 0.4220 0.7354 0.2123 0.083 Uiso 1 1 calc R . . H26B H 0.4294 0.8008 0.1914 0.083 Uiso 1 1 calc R . . C27 C 0.5443(3) 0.7611(2) 0.2011(2) 0.0902(13) Uani 1 1 d DU . . O28 O 0.5999(3) 0.7952(4) 0.2051(4) 0.266(6) Uani 1 1 d DU . . N29 N 0.5602(3) 0.7089(2) 0.1801(3) 0.125(2) Uani 1 1 d DU . . H29A H 0.6105 0.7004 0.1698 0.150 Uiso 1 1 calc R . . H29B H 0.5203 0.6831 0.1768 0.150 Uiso 1 1 calc R . . C30 C 0.5101(2) 0.88691(18) 0.32783(18) 0.0722(9) Uani 1 1 d U . . H30A H 0.5005 0.9296 0.3271 0.087 Uiso 1 1 calc R . . H30B H 0.4749 0.8704 0.3554 0.087 Uiso 1 1 calc R . . C31 C 0.6033(2) 0.8754(3) 0.3417(2) 0.0923(14) Uani 1 1 d . . . H31A H 0.6391 0.8878 0.3127 0.111 Uiso 1 1 calc R . . H31B H 0.6121 0.8331 0.3475 0.111 Uiso 1 1 calc R . . C32 C 0.6270(3) 0.9104(2) 0.3917(2) 0.0974(15) Uani 1 1 d DU . . O33 O 0.6535(5) 0.9606(2) 0.3904(3) 0.197(4) Uani 1 1 d DU . . N34 N 0.6195(3) 0.8811(3) 0.4360(2) 0.1194(17) Uani 1 1 d DU . . H34A H 0.6337 0.8977 0.4651 0.143 Uiso 1 1 calc R . . H34B H 0.6003 0.8453 0.4359 0.143 Uiso 1 1 calc R . . C35 C 0.5132(2) 0.9709(2) 0.2145(2) 0.0893(14) Uani 1 1 d . . . H35A H 0.5503 0.9390 0.2244 0.134 Uiso 1 1 calc R . . H35B H 0.5289 1.0065 0.2330 0.134 Uiso 1 1 calc R . . H35C H 0.5175 0.9777 0.1774 0.134 Uiso 1 1 calc R . . C36 C 0.4318(3) 1.09497(17) 0.2169(2) 0.0798(10) Uani 1 1 d . . . H36A H 0.4265 1.0993 0.2542 0.120 Uiso 1 1 calc R . . H36B H 0.4286 1.1334 0.2005 0.120 Uiso 1 1 calc R . . H36C H 0.4852 1.0769 0.2087 0.120 Uiso 1 1 calc R . . C37 C 0.3640(3) 1.0477(2) 0.13598(19) 0.0822(11) Uani 1 1 d U . . H37A H 0.4162 1.0275 0.1268 0.099 Uiso 1 1 calc R . . H37B H 0.3173 1.0232 0.1241 0.099 Uiso 1 1 calc R . . C38 C 0.3608(3) 1.1069(2) 0.10846(19) 0.0871(12) Uani 1 1 d U . . O39 O 0.2941(3) 1.1306(2) 0.1004(2) 0.1297(17) Uani 1 1 d U . . N40 N 0.4327(3) 1.1333(2) 0.09555(19) 0.0994(13) Uani 1 1 d U . . H40A H 0.4321 1.1680 0.0811 0.119 Uiso 1 1 calc R . . H40B H 0.4801 1.1158 0.1016 0.119 Uiso 1 1 calc R . . C41 C 0.2734(2) 1.11008(14) 0.26587(18) 0.0715(9) Uani 1 1 d . . . H41A H 0.3040 1.0853 0.2906 0.086 Uiso 1 1 calc R . . H41B H 0.3043 1.1471 0.2623 0.086 Uiso 1 1 calc R . . C42 C 0.1866(3) 1.1237(2) 0.2886(2) 0.0906(13) Uani 1 1 d . . . H42A H 0.1548 1.1482 0.2641 0.109 Uiso 1 1 calc R . . H42B H 0.1557 1.0869 0.2940 0.109 Uiso 1 1 calc R . . C43 C 0.1958(3) 1.1558(3) 0.3395(3) 0.1062(17) Uani 1 1 d DU . . O44 O 0.2540(4) 1.1891(3) 0.3507(2) 0.164(3) Uani 1 1 d DU . . N45 N 0.1310(4) 1.1510(3) 0.3721(3) 0.138(2) Uani 1 1 d DU . . H45A H 0.1302 1.1713 0.4008 0.166 Uiso 1 1 calc R . . H45B H 0.0896 1.1277 0.3646 0.166 Uiso 1 1 calc R . . C46 C -0.0535(3) 1.0199(2) 0.1969(4) 0.128(3) Uani 1 1 d U . . H46A H -0.1098 1.0156 0.1833 0.192 Uiso 1 1 calc R . . H46B H -0.0266 1.0534 0.1806 0.192 Uiso 1 1 calc R . . H46C H -0.0559 1.0260 0.2342 0.192 Uiso 1 1 calc R . . C47 C 0.0042(4) 0.9527(3) 0.1253(3) 0.1152(19) Uani 1 1 d U . . H47A H -0.0514 0.9495 0.1104 0.173 Uiso 1 1 calc R . . H47B H 0.0348 0.9164 0.1190 0.173 Uiso 1 1 calc R . . H47C H 0.0335 0.9854 0.1093 0.173 Uiso 1 1 calc R . . C48 C -0.0762(3) 0.9099(2) 0.2669(2) 0.0887(12) Uani 1 1 d . . . H48A H -0.0713 0.8710 0.2832 0.106 Uiso 1 1 calc R . . H48B H -0.0428 0.9373 0.2879 0.106 Uiso 1 1 calc R . . C49 C -0.1681(3) 0.9292(3) 0.2715(3) 0.1113(19) Uani 1 1 d . . . H49A H -0.1877 0.9205 0.3068 0.134 Uiso 1 1 calc R . . H49B H -0.1712 0.9720 0.2665 0.134 Uiso 1 1 calc R . . C50 C -0.2259(3) 0.9002(3) 0.2335(3) 0.1007(15) Uani 1 1 d U . . O51 O -0.2574(3) 0.9323(2) 0.2012(3) 0.1344(17) Uani 1 1 d U . . N52 N -0.2390(3) 0.8424(2) 0.2381(3) 0.1160(16) Uani 1 1 d U . . H52A H -0.2727 0.8246 0.2168 0.139 Uiso 1 1 calc R . . H52B H -0.2139 0.8225 0.2624 0.139 Uiso 1 1 calc R . . C53 C -0.0245(2) 0.77470(16) 0.22087(19) 0.0752(10) Uani 1 1 d . . . H53A H -0.0479 0.7654 0.2547 0.113 Uiso 1 1 calc R . . H53B H -0.0102 0.7385 0.2029 0.113 Uiso 1 1 calc R . . H53C H -0.0654 0.7964 0.2006 0.113 Uiso 1 1 calc R . . C54 C 0.1556(3) 0.69207(16) 0.19003(15) 0.0715(9) Uani 1 1 d . . . H54A H 0.1662 0.6500 0.1915 0.107 Uiso 1 1 calc R . . H54B H 0.2002 0.7113 0.1709 0.107 Uiso 1 1 calc R . . H54C H 0.1027 0.6992 0.1726 0.107 Uiso 1 1 calc R . . C55 C 0.0874(2) 0.68087(11) 0.27884(13) 0.0548(6) Uani 1 1 d . . . H55A H 0.0361 0.6770 0.2583 0.066 Uiso 1 1 calc R . . H55B H 0.1102 0.6411 0.2837 0.066 Uiso 1 1 calc R . . C56 C 0.0639(2) 0.70520(15) 0.33198(15) 0.0646(8) Uani 1 1 d . . . H56A H 0.0511 0.7473 0.3288 0.077 Uiso 1 1 calc R . . H56B H 0.1116 0.7011 0.3556 0.077 Uiso 1 1 calc R . . C57 C -0.0119(2) 0.67307(14) 0.35502(15) 0.0643(8) Uani 1 1 d . . . O58 O -0.08006(19) 0.67298(17) 0.33125(14) 0.0904(9) Uani 1 1 d . . . N59 N -0.0019(2) 0.64595(14) 0.39982(13) 0.0692(7) Uani 1 1 d . . . H59 H 0.0479 0.6462 0.4133 0.083 Uiso 1 1 calc R . . C60 C 0.2963(2) 0.66417(13) 0.26326(18) 0.0690(8) Uani 1 1 d U . . H60A H 0.2934 0.6538 0.2263 0.083 Uiso 1 1 calc R . . H60B H 0.3543 0.6752 0.2709 0.083 Uiso 1 1 calc R . . C61 C 0.2745(2) 0.61015(14) 0.29496(19) 0.0731(10) Uani 1 1 d U . . O62 O 0.2499(3) 0.61424(18) 0.34114(18) 0.1084(12) Uani 1 1 d U . . N63 N 0.2847(3) 0.55881(15) 0.2706(3) 0.1108(16) Uani 1 1 d U . . H63A H 0.2742 0.5260 0.2867 0.133 Uiso 1 1 calc R . . H63B H 0.3020 0.5582 0.2385 0.133 Uiso 1 1 calc R . . C1PR C -0.0682(3) 0.61513(16) 0.42903(16) 0.0727(9) Uani 1 1 d . . . H1P1 H -0.0448 0.5792 0.4444 0.087 Uiso 1 1 calc R . . H1P2 H -0.1125 0.6033 0.4048 0.087 Uiso 1 1 calc R . . C2PR C -0.1062(2) 0.65250(17) 0.47187(15) 0.0681(8) Uani 1 1 d . . . H2PR H -0.1342 0.6875 0.4567 0.082 Uiso 1 1 calc R . . C3PR C -0.1681(3) 0.6175(2) 0.5051(2) 0.0914(14) Uani 1 1 d . . . H3P1 H -0.1923 0.6433 0.5312 0.137 Uiso 1 1 calc R . . H3P2 H -0.1392 0.5852 0.5220 0.137 Uiso 1 1 calc R . . H3P3 H -0.2122 0.6020 0.4831 0.137 Uiso 1 1 calc R . . P1 P -0.02841(7) 0.73812(4) 0.52348(4) 0.0659(2) Uani 1 1 d . . . O2P O -0.0100(2) 0.76778(11) 0.46775(11) 0.0734(7) Uani 1 1 d . . . O3P O -0.03712(17) 0.67123(11) 0.50605(10) 0.0690(6) Uani 1 1 d . . . O4P O -0.1076(2) 0.76246(15) 0.54556(14) 0.0910(9) Uani 1 1 d . . . O5P O 0.0477(3) 0.74161(17) 0.55757(15) 0.0992(10) Uani 1 1 d . . . C1R C 0.0556(2) 0.91245(14) 0.42283(14) 0.0609(7) Uani 1 1 d U . . H1R H 0.0486 0.9437 0.4494 0.073 Uiso 1 1 calc R . . C2R C 0.0798(2) 0.85381(13) 0.44922(13) 0.0567(6) Uani 1 1 d U . . H2R H 0.1144 0.8601 0.4807 0.068 Uiso 1 1 calc R . . C3R C -0.0082(2) 0.83081(15) 0.46280(15) 0.0640(7) Uani 1 1 d U . . H3R H -0.0284 0.8495 0.4953 0.077 Uiso 1 1 calc R . . C4R C -0.0623(2) 0.85100(19) 0.41630(19) 0.0768(10) Uani 1 1 d U . . H4R H -0.0638 0.8197 0.3894 0.092 Uiso 1 1 calc R . . C5R C -0.1519(3) 0.8693(4) 0.4308(3) 0.127(2) Uani 1 1 d U . . H5R1 H -0.1821 0.8809 0.3992 0.152 Uiso 1 1 calc R . . H5R2 H -0.1812 0.8356 0.4462 0.152 Uiso 1 1 calc R . . O6R O -0.02237(15) 0.90249(14) 0.39604(13) 0.0792(7) Uani 1 1 d U . . O7R O 0.12057(16) 0.81774(10) 0.41232(10) 0.0635(5) Uani 1 1 d U . . H7R H 0.1543 0.7959 0.4274 0.095 Uiso 1 1 calc R . . O8R O -0.1519(5) 0.9188(4) 0.4680(4) 0.194(3) Uani 1 1 d U . . H8R H -0.1408 0.9064 0.4975 0.291 Uiso 1 1 calc R . . N1B N 0.11733(16) 0.93105(10) 0.38376(11) 0.0568(6) Uani 1 1 d U . . C2B C 0.12853(16) 0.90570(11) 0.33657(12) 0.0511(6) Uani 1 1 d U . . H2B H 0.0900 0.8795 0.3216 0.061 Uiso 1 1 calc R . . N3B N 0.19957(14) 0.92165(9) 0.31354(10) 0.0486(5) Uani 1 1 d U . . C4B C 0.31861(19) 0.98658(14) 0.35034(14) 0.0585(6) Uani 1 1 d U . . H4B H 0.3551 0.9820 0.3219 0.070 Uiso 1 1 calc R . . C5B C 0.3418(2) 1.02103(16) 0.39287(16) 0.0686(8) Uani 1 1 d U . . C6B C 0.2885(3) 1.02697(17) 0.43679(18) 0.0757(9) Uani 1 1 d U . . C7B C 0.2105(3) 0.99862(15) 0.43780(17) 0.0701(8) Uani 1 1 d U . . H7B H 0.1745 1.0021 0.4665 0.084 Uiso 1 1 calc R . . C8B C 0.18863(19) 0.96466(12) 0.39383(13) 0.0538(6) Uani 1 1 d U . . C9B C 0.23959(17) 0.95868(11) 0.35045(12) 0.0508(5) Uani 1 1 d U . . C10B C 0.4282(4) 1.0514(3) 0.3923(2) 0.1062(17) Uani 1 1 d U . . H10A H 0.4219 1.0925 0.4020 0.159 Uiso 1 1 calc R . . H10B H 0.4519 1.0490 0.3576 0.159 Uiso 1 1 calc R . . H10C H 0.4651 1.0319 0.4168 0.159 Uiso 1 1 calc R . . C11B C 0.3145(5) 1.0665(3) 0.4825(3) 0.122(2) Uani 1 1 d . . . H11A H 0.3682 1.0845 0.4750 0.183 Uiso 1 1 calc R . . H11B H 0.3191 1.0428 0.5138 0.183 Uiso 1 1 calc R . . H11C H 0.2728 1.0970 0.4876 0.183 Uiso 1 1 calc R . . C1C C 0.2526(2) 0.87878(16) 0.16876(15) 0.0636(8) Uani 1 1 d U . . N2C N 0.2668(4) 0.8671(2) 0.12501(16) 0.1011(12) Uani 1 1 d U . . OW1 O 0.2221(3) 0.7374(2) 0.46635(19) 0.1182(13) Uani 1 1 d . . . OW2 O 0.1653(3) 0.6225(4) 0.4439(3) 0.167(2) Uani 1 1 d . . . OW3 O -0.2866(4) 0.7440(3) 0.4258(3) 0.1497(19) Uani 1 1 d . . . OW4 O 0.6149(4) 1.1267(3) 0.0905(3) 0.172(3) Uani 1 1 d . . . OW5 O -0.1945(5) 0.7657(3) 0.3299(3) 0.183(3) Uani 1 1 d . . . OW6 O -0.0037(11) 1.0588(8) 0.3543(7) 0.190(6) Uiso 0.50 1 d P . . OW7 O 0.3970(10) 0.6582(7) 0.1302(6) 0.179(5) Uiso 0.50 1 d P . . OW8 O 0.3008(10) 0.5584(6) 0.1541(6) 0.165(4) Uiso 0.50 1 d P . . OW9 O 0.3745(13) 0.5581(9) 0.1767(8) 0.207(7) Uiso 0.50 1 d P . . OW10 O 0.0192(11) 1.0358(8) 0.5015(7) 0.192(6) Uiso 0.50 1 d P . . OW11 O -0.3177(18) 0.9072(12) 0.1154(11) 0.266(10) Uiso 0.50 1 d P . . OW12 O 0.1118(15) 0.8092(11) 0.0708(10) 0.251(9) Uiso 0.50 1 d P . . OW13 O -0.0726(16) 0.9932(10) 0.5807(9) 0.238(8) Uiso 0.50 1 d 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 Co 0.03838(14) 0.03872(14) 0.05836(19) 0.00930(13) 0.00336(13) -0.00190(12) C1 0.0419(11) 0.0432(11) 0.0613(15) 0.0060(10) 0.0061(10) 0.0035(9) C2 0.0465(12) 0.0545(13) 0.0638(18) 0.0035(11) 0.0063(11) 0.0066(10) C3 0.0394(12) 0.0632(15) 0.075(2) 0.0048(13) 0.0044(11) 0.0046(10) C4 0.0397(10) 0.0550(12) 0.0640(17) 0.0046(12) 0.0062(10) -0.0024(10) C5 0.0438(13) 0.0587(15) 0.087(2) 0.0147(14) 0.0094(13) -0.0076(11) C6 0.0476(13) 0.0519(14) 0.0733(18) 0.0153(12) 0.0086(12) -0.0098(10) C7 0.0615(16) 0.0519(15) 0.084(2) 0.0180(14) 0.0060(15) -0.0131(12) C8 0.0574(14) 0.0439(12) 0.087(2) 0.0182(13) -0.0008(15) -0.0079(12) C9 0.0551(14) 0.0412(11) 0.0792(19) 0.0159(11) 0.0002(13) -0.0037(10) C10 0.0555(15) 0.0427(13) 0.098(2) 0.0206(14) -0.0066(15) -0.0014(11) C11 0.0510(14) 0.0468(13) 0.085(2) 0.0138(13) -0.0102(13) -0.0015(11) C12 0.0559(17) 0.0532(16) 0.131(3) 0.0246(18) -0.0263(19) 0.0001(13) C13 0.0461(13) 0.0527(15) 0.100(2) 0.0111(15) -0.0105(14) -0.0015(11) C14 0.0419(12) 0.0481(12) 0.0711(17) 0.0100(11) -0.0058(11) -0.0039(9) C15 0.0455(12) 0.0451(12) 0.0745(19) 0.0069(11) -0.0011(11) -0.0058(9) C16 0.0475(12) 0.0387(10) 0.0559(14) 0.0014(10) 0.0051(10) -0.0057(8) C17 0.0566(13) 0.0384(10) 0.0577(16) -0.0013(9) 0.0052(11) -0.0024(9) C18 0.0538(13) 0.0372(10) 0.0668(17) 0.0016(9) 0.0041(11) 0.0041(9) C19 0.0446(11) 0.0438(11) 0.0578(15) 0.0043(9) 0.0069(10) 0.0034(9) C20 0.0487(13) 0.0519(13) 0.0592(16) 0.0077(11) 0.0019(11) 0.0053(10) N21 0.0404(9) 0.0460(10) 0.0556(12) 0.0073(9) 0.0044(9) 0.0009(7) N22 0.0442(10) 0.0444(10) 0.0713(15) 0.0143(9) 0.0017(10) -0.0049(9) N23 0.0396(10) 0.0414(10) 0.0693(15) 0.0086(9) -0.0016(9) -0.0027(7) N24 0.0429(9) 0.0384(9) 0.0574(14) 0.0056(8) 0.0037(8) -0.0015(7) C25 0.0559(17) 0.0672(19) 0.088(2) 0.0120(17) -0.0056(15) 0.0147(14) C26 0.0485(15) 0.075(2) 0.084(2) -0.0066(17) 0.0191(15) 0.0030(13) C27 0.054(2) 0.111(3) 0.105(3) -0.016(3) 0.023(2) 0.010(2) O28 0.076(3) 0.307(9) 0.414(12) -0.247(10) 0.104(5) -0.063(4) N29 0.079(3) 0.113(3) 0.183(5) -0.024(3) 0.045(3) 0.025(2) C30 0.0450(14) 0.076(2) 0.096(3) -0.0110(18) -0.0047(14) 0.0070(13) C31 0.0501(18) 0.117(4) 0.110(4) -0.013(3) -0.0098(19) 0.0073(19) C32 0.059(2) 0.090(3) 0.143(5) 0.008(3) -0.026(2) -0.0099(19) O33 0.224(7) 0.110(4) 0.256(8) 0.040(5) -0.111(7) -0.066(4) N34 0.107(3) 0.154(5) 0.097(3) -0.007(3) 0.003(3) -0.022(3) C35 0.0480(17) 0.080(2) 0.140(4) 0.031(3) 0.021(2) -0.0106(15) C36 0.0658(19) 0.066(2) 0.108(3) 0.0136(19) 0.0062(19) -0.0214(16) C37 0.082(2) 0.076(2) 0.088(3) 0.023(2) 0.004(2) -0.0163(19) C38 0.083(3) 0.094(3) 0.084(3) 0.036(2) -0.010(2) -0.017(2) O39 0.085(2) 0.144(3) 0.160(4) 0.083(3) -0.011(2) -0.005(2) N40 0.092(3) 0.101(3) 0.105(3) 0.044(2) 0.005(2) -0.018(2) C41 0.0609(17) 0.0500(14) 0.103(3) 0.0051(15) 0.0038(18) -0.0052(13) C42 0.073(2) 0.080(2) 0.119(4) -0.006(2) 0.013(2) -0.004(2) C43 0.094(3) 0.098(3) 0.127(5) -0.008(3) 0.024(3) -0.017(3) O44 0.134(4) 0.186(5) 0.171(5) -0.074(4) 0.060(4) -0.073(4) N45 0.136(5) 0.148(5) 0.131(4) -0.031(4) 0.052(4) -0.017(4) C46 0.059(2) 0.060(2) 0.265(8) 0.029(3) -0.027(3) 0.0106(17) C47 0.115(4) 0.114(4) 0.116(4) 0.044(3) -0.051(3) -0.030(3) C48 0.0523(17) 0.093(3) 0.120(4) -0.005(3) 0.004(2) 0.0023(17) C49 0.064(2) 0.102(4) 0.168(6) -0.002(4) 0.013(3) 0.012(2) C50 0.056(2) 0.100(3) 0.147(5) 0.005(3) 0.008(2) -0.009(2) O51 0.115(3) 0.097(3) 0.191(5) 0.011(3) -0.038(3) 0.002(2) N52 0.074(2) 0.101(3) 0.172(5) -0.005(3) -0.014(3) 0.007(2) C53 0.0558(17) 0.0566(16) 0.113(3) 0.0112(17) -0.0142(18) -0.0174(13) C54 0.086(2) 0.0607(18) 0.068(2) -0.0145(15) 0.0107(17) -0.0098(16) C55 0.0614(15) 0.0365(11) 0.0665(17) -0.0008(10) 0.0041(12) -0.0079(10) C56 0.0698(18) 0.0556(15) 0.0683(19) -0.0039(13) 0.0100(15) -0.0195(14) C57 0.0652(18) 0.0530(15) 0.075(2) -0.0037(13) 0.0122(15) -0.0109(13) O58 0.0651(15) 0.111(2) 0.095(2) 0.0210(17) -0.0023(14) -0.0217(15) N59 0.0709(18) 0.0706(17) 0.0662(17) -0.0020(13) 0.0101(13) -0.0176(14) C60 0.0648(17) 0.0432(13) 0.099(2) 0.0042(15) 0.0095(17) 0.0097(12) C61 0.0644(17) 0.0477(14) 0.107(3) 0.0148(15) -0.0139(19) 0.0037(14) O62 0.113(3) 0.099(2) 0.113(3) 0.040(2) -0.013(2) -0.003(2) N63 0.098(3) 0.0493(15) 0.185(5) 0.011(2) 0.019(3) 0.0084(16) C1PR 0.084(2) 0.0596(18) 0.075(2) 0.0010(14) 0.0138(17) -0.0217(16) C2PR 0.0683(19) 0.0633(18) 0.073(2) 0.0038(14) 0.0086(15) -0.0204(15) C3PR 0.091(3) 0.097(3) 0.086(3) 0.008(2) 0.018(2) -0.040(2) P1 0.0711(5) 0.0630(4) 0.0635(5) -0.0009(4) 0.0076(4) -0.0128(4) O2P 0.0944(18) 0.0557(12) 0.0700(15) -0.0017(10) 0.0253(13) -0.0193(12) O3P 0.0725(14) 0.0603(12) 0.0744(15) 0.0051(10) -0.0022(11) -0.0113(10) O4P 0.090(2) 0.0808(17) 0.102(2) -0.0019(16) 0.0368(17) -0.0094(15) O5P 0.105(2) 0.088(2) 0.104(2) -0.0149(18) -0.0285(19) -0.0126(18) C1R 0.0564(15) 0.0508(14) 0.076(2) -0.0054(12) 0.0211(13) -0.0015(11) C2R 0.0555(14) 0.0540(14) 0.0607(17) -0.0031(11) 0.0105(12) -0.0065(11) C3R 0.0654(17) 0.0540(15) 0.0725(19) -0.0013(13) 0.0212(14) -0.0120(13) C4R 0.0548(17) 0.078(2) 0.098(3) 0.0084(19) 0.0065(16) -0.0154(15) C5R 0.054(2) 0.183(6) 0.143(5) 0.049(4) 0.018(3) -0.001(3) O6R 0.0481(11) 0.0865(17) 0.1032(19) 0.0259(15) 0.0146(11) 0.0014(11) O7R 0.0651(12) 0.0533(11) 0.0723(14) 0.0023(9) 0.0175(10) 0.0046(9) O8R 0.149(5) 0.191(6) 0.243(8) 0.002(5) 0.079(5) 0.054(5) N1B 0.0542(12) 0.0428(11) 0.0735(16) -0.0024(10) 0.0148(11) -0.0060(9) C2B 0.0432(11) 0.0419(12) 0.0681(16) 0.0032(10) 0.0096(10) -0.0027(9) N3B 0.0402(9) 0.0383(9) 0.0673(14) 0.0058(8) 0.0042(9) -0.0022(7) C4B 0.0506(14) 0.0546(15) 0.0701(18) 0.0047(12) 0.0041(12) -0.0093(11) C5B 0.0651(18) 0.0586(17) 0.082(2) 0.0015(14) -0.0052(15) -0.0147(14) C6B 0.082(2) 0.0623(18) 0.083(2) -0.0101(16) -0.0008(17) -0.0115(16) C7B 0.078(2) 0.0533(15) 0.079(2) -0.0103(14) 0.0105(16) -0.0030(14) C8B 0.0538(14) 0.0388(11) 0.0688(17) 0.0000(10) 0.0082(12) -0.0026(10) C9B 0.0457(12) 0.0409(11) 0.0659(15) 0.0060(10) 0.0032(11) -0.0009(9) C10B 0.088(3) 0.122(4) 0.109(4) -0.002(3) -0.007(3) -0.049(3) C11B 0.122(5) 0.126(5) 0.119(4) -0.057(4) 0.008(4) -0.032(4) C1C 0.0589(17) 0.0627(16) 0.069(2) 0.0114(13) 0.0065(13) -0.0014(12) N2C 0.127(3) 0.111(3) 0.065(2) 0.0012(19) 0.018(2) -0.002(3) OW1 0.118(3) 0.112(3) 0.125(3) 0.010(2) -0.009(2) 0.033(3) OW2 0.100(3) 0.227(7) 0.174(5) 0.007(5) 0.004(3) -0.005(4) OW3 0.142(4) 0.124(4) 0.183(5) -0.019(4) -0.019(4) -0.013(3) OW4 0.154(5) 0.146(4) 0.218(7) 0.024(4) -0.081(5) 0.017(4) OW5 0.188(6) 0.169(6) 0.191(6) 0.033(5) 0.033(5) 0.053(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 Co C1C 1.863(4) . ? Co N21 1.885(2) . ? Co N24 1.890(2) . ? Co N22 1.919(2) . ? Co N23 1.926(2) . ? Co N3B 2.037(3) . ? C1 N21 1.496(3) . ? C1 C20 1.530(4) . ? C1 C19 1.535(4) . ? C1 C2 1.589(4) . ? C2 C25 1.526(5) . ? C2 C3 1.562(4) . ? C2 C26 1.572(5) . ? C3 C4 1.515(4) . ? C3 C30 1.545(5) . ? C3 H3 0.9800 . ? C4 N21 1.293(3) . ? C4 C5 1.428(4) . ? C5 C6 1.364(4) . ? C5 C35 1.520(4) . ? C6 N22 1.393(4) . ? C6 C7 1.538(4) . ? C7 C8 1.535(5) . ? C7 C37 1.537(7) . ? C7 C36 1.554(5) . ? C8 C9 1.506(4) . ? C8 C41 1.542(6) . ? C8 H8 0.9800 . ? C9 N22 1.336(4) . ? C9 C10 1.389(5) . ? C10 C11 1.386(4) . ? C10 H10 0.9300 . ? C11 N23 1.327(4) . ? C11 C12 1.507(5) . ? C12 C46 1.528(6) . ? C12 C13 1.538(5) . ? C12 C47 1.545(9) . ? C13 C14 1.511(4) . ? C13 C48 1.556(7) . ? C13 H13 0.9800 . ? C14 C15 1.371(4) . ? C14 N23 1.391(3) . ? C15 C16 1.441(4) . ? C15 C53 1.513(4) . ? C16 N24 1.305(3) . ? C16 C17 1.552(3) . ? C17 C54 1.541(5) . ? C17 C55 1.547(4) . ? C17 C18 1.551(4) . ? C18 C19 1.521(4) . ? C18 C60 1.524(4) . ? C18 H18 0.9800 . ? C19 N24 1.483(3) . ? C19 H19 0.9800 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 C27 1.508(5) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 O28 1.170(6) . ? C27 N29 1.312(4) . ? N29 H29A 0.8600 . ? N29 H29B 0.8600 . ? C30 C31 1.539(5) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 C32 1.543(8) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 O33 1.203(6) . ? C32 N34 1.310(4) . ? N34 H34A 0.8600 . ? N34 H34B 0.8600 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 C38 1.503(6) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 O39 1.200(6) . ? C38 N40 1.324(6) . ? N40 H40A 0.8600 . ? N40 H40B 0.8600 . ? C41 C42 1.522(6) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 C43 1.489(8) . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C43 O44 1.221(6) . ? C43 N45 1.324(4) . ? N45 H45A 0.8600 . ? N45 H45B 0.8600 . ? C46 H46A 0.9600 . ? C46 H46B 0.9600 . ? C46 H46C 0.9600 . ? C47 H47A 0.9600 . ? C47 H47B 0.9600 . ? C47 H47C 0.9600 . ? C48 C49 1.521(6) . ? C48 H48A 0.9700 . ? C48 H48B 0.9700 . ? C49 C50 1.480(9) . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? C50 O51 1.201(7) . ? C50 N52 1.319(7) . ? N52 H52A 0.8600 . ? N52 H52B 0.8600 . ? C53 H53A 0.9600 . ? C53 H53B 0.9600 . ? C53 H53C 0.9600 . ? C54 H54A 0.9600 . ? C54 H54B 0.9600 . ? C54 H54C 0.9600 . ? C55 C56 1.505(5) . ? C55 H55A 0.9700 . ? C55 H55B 0.9700 . ? C56 C57 1.517(4) . ? C56 H56A 0.9700 . ? C56 H56B 0.9700 . ? C57 O58 1.237(5) . ? C57 N59 1.302(5) . ? N59 C1PR 1.460(4) . ? N59 H59 0.8600 . ? C60 C61 1.497(5) . ? C60 H60A 0.9700 . ? C60 H60B 0.9700 . ? C61 O62 1.241(6) . ? C61 N63 1.319(6) . ? N63 H63A 0.8600 . ? N63 H63B 0.8600 . ? C1PR C2PR 1.501(6) . ? C1PR H1P1 0.9700 . ? C1PR H1P2 0.9700 . ? C2PR O3P 1.459(5) . ? C2PR C3PR 1.513(5) . ? C2PR H2PR 0.9800 . ? C3PR H3P1 0.9600 . ? C3PR H3P2 0.9600 . ? C3PR H3P3 0.9600 . ? P1 O4P 1.479(3) . ? P1 O5P 1.486(4) . ? P1 O3P 1.571(3) . ? P1 O2P 1.593(3) . ? O2P C3R 1.421(4) . ? C1R O6R 1.428(5) . ? C1R N1B 1.455(4) . ? C1R C2R 1.526(5) . ? C1R H1R 0.9800 . ? C2R O7R 1.398(4) . ? C2R C3R 1.525(4) . ? C2R H2R 0.9800 . ? C3R C4R 1.529(6) . ? C3R H3R 0.9800 . ? C4R O6R 1.415(5) . ? C4R C5R 1.521(7) . ? C4R H4R 0.9800 . ? C5R O8R 1.459(12) . ? C5R H5R1 0.9700 . ? C5R H5R2 0.9700 . ? O7R H7R 0.8200 . ? O8R H8R 0.8200 . ? N1B C2B 1.340(4) . ? N1B C8B 1.381(4) . ? C2B N3B 1.317(3) . ? C2B H2B 0.9300 . ? N3B C9B 1.405(4) . ? C4B C5B 1.380(5) . ? C4B C9B 1.399(4) . ? C4B H4B 0.9300 . ? C5B C6B 1.407(6) . ? C5B C10B 1.528(6) . ? C6B C7B 1.388(6) . ? C6B C11B 1.520(6) . ? C7B C8B 1.397(5) . ? C7B H7B 0.9300 . ? C8B C9B 1.373(4) . ? C10B H10A 0.9600 . ? C10B H10B 0.9600 . ? C10B H10C 0.9600 . ? C11B H11A 0.9600 . ? C11B H11B 0.9600 . ? C11B H11C 0.9600 . ? C1C N2C 1.165(6) . ? OW8 OW9 1.30(2) . ? 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 C1C Co N21 91.61(13) . . ? C1C Co N24 87.76(13) . . ? N21 Co N24 83.22(9) . . ? C1C Co N22 88.03(13) . . ? N21 Co N22 90.04(10) . . ? N24 Co N22 171.95(10) . . ? C1C Co N23 90.00(13) . . ? N21 Co N23 173.34(9) . . ? N24 Co N23 90.39(9) . . ? N22 Co N23 96.47(10) . . ? C1C Co N3B 176.22(12) . . ? N21 Co N3B 91.33(10) . . ? N24 Co N3B 94.95(9) . . ? N22 Co N3B 89.59(10) . . ? N23 Co N3B 87.36(10) . . ? N21 C1 C20 110.5(2) . . ? N21 C1 C19 102.3(2) . . ? C20 C1 C19 109.2(2) . . ? N21 C1 C2 101.5(2) . . ? C20 C1 C2 113.2(2) . . ? C19 C1 C2 119.2(2) . . ? C25 C2 C3 113.5(3) . . ? C25 C2 C26 110.5(3) . . ? C3 C2 C26 107.0(3) . . ? C25 C2 C1 114.8(3) . . ? C3 C2 C1 101.3(2) . . ? C26 C2 C1 109.2(3) . . ? C4 C3 C30 109.0(3) . . ? C4 C3 C2 101.5(2) . . ? C30 C3 C2 119.3(3) . . ? C4 C3 H3 108.8 . . ? C30 C3 H3 108.8 . . ? C2 C3 H3 108.8 . . ? N21 C4 C5 125.4(3) . . ? N21 C4 C3 111.3(2) . . ? C5 C4 C3 123.3(2) . . ? C6 C5 C4 120.9(2) . . ? C6 C5 C35 122.4(3) . . ? C4 C5 C35 116.7(3) . . ? C5 C6 N22 124.2(2) . . ? C5 C6 C7 127.5(3) . . ? N22 C6 C7 108.2(3) . . ? C8 C7 C37 110.3(3) . . ? C8 C7 C6 101.1(2) . . ? C37 C7 C6 105.8(3) . . ? C8 C7 C36 112.1(3) . . ? C37 C7 C36 111.3(3) . . ? C6 C7 C36 115.6(3) . . ? C9 C8 C7 101.6(3) . . ? C9 C8 C41 110.8(3) . . ? C7 C8 C41 112.4(3) . . ? C9 C8 H8 110.6 . . ? C7 C8 H8 110.6 . . ? C41 C8 H8 110.6 . . ? N22 C9 C10 125.6(3) . . ? N22 C9 C8 110.2(3) . . ? C10 C9 C8 124.1(3) . . ? C11 C10 C9 126.2(3) . . ? C11 C10 H10 116.9 . . ? C9 C10 H10 116.9 . . ? N23 C11 C10 124.7(3) . . ? N23 C11 C12 110.8(3) . . ? C10 C11 C12 124.3(3) . . ? C11 C12 C46 112.3(4) . . ? C11 C12 C13 101.1(3) . . ? C46 C12 C13 116.1(4) . . ? C11 C12 C47 106.2(4) . . ? C46 C12 C47 111.2(5) . . ? C13 C12 C47 109.1(4) . . ? C14 C13 C12 101.4(3) . . ? C14 C13 C48 106.4(3) . . ? C12 C13 C48 119.2(4) . . ? C14 C13 H13 109.8 . . ? C12 C13 H13 109.8 . . ? C48 C13 H13 109.8 . . ? C15 C14 N23 126.6(3) . . ? C15 C14 C13 124.8(2) . . ? N23 C14 C13 108.3(2) . . ? C14 C15 C16 121.3(2) . . ? C14 C15 C53 118.2(3) . . ? C16 C15 C53 120.5(2) . . ? N24 C16 C15 122.6(2) . . ? N24 C16 C17 110.4(2) . . ? C15 C16 C17 126.8(2) . . ? C54 C17 C55 109.2(2) . . ? C54 C17 C18 111.9(3) . . ? C55 C17 C18 111.7(2) . . ? C54 C17 C16 107.3(3) . . ? C55 C17 C16 115.6(2) . . ? C18 C17 C16 100.9(2) . . ? C19 C18 C60 113.7(2) . . ? C19 C18 C17 102.5(2) . . ? C60 C18 C17 116.4(3) . . ? C19 C18 H18 107.9 . . ? C60 C18 H18 107.9 . . ? C17 C18 H18 107.9 . . ? N24 C19 C18 102.7(2) . . ? N24 C19 C1 106.8(2) . . ? C18 C19 C1 122.4(2) . . ? N24 C19 H19 108.0 . . ? C18 C19 H19 108.0 . . ? C1 C19 H19 108.0 . . ? C1 C20 H20A 109.5 . . ? C1 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C1 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C4 N21 C1 113.3(2) . . ? C4 N21 Co 129.48(19) . . ? C1 N21 Co 116.87(16) . . ? C9 N22 C6 110.6(2) . . ? C9 N22 Co 122.47(19) . . ? C6 N22 Co 126.3(2) . . ? C11 N23 C14 110.4(2) . . ? C11 N23 Co 123.58(19) . . ? C14 N23 Co 125.95(18) . . ? C16 N24 C19 111.6(2) . . ? C16 N24 Co 132.78(18) . . ? C19 N24 Co 113.78(16) . . ? C2 C25 H25A 109.5 . . ? C2 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C2 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C27 C26 C2 113.5(3) . . ? C27 C26 H26A 108.9 . . ? C2 C26 H26A 108.9 . . ? C27 C26 H26B 108.9 . . ? C2 C26 H26B 108.9 . . ? H26A C26 H26B 107.7 . . ? O28 C27 N29 118.4(4) . . ? O28 C27 C26 125.9(4) . . ? N29 C27 C26 115.7(4) . . ? C27 N29 H29A 120.0 . . ? C27 N29 H29B 120.0 . . ? H29A N29 H29B 120.0 . . ? C31 C30 C3 114.5(3) . . ? C31 C30 H30A 108.6 . . ? C3 C30 H30A 108.6 . . ? C31 C30 H30B 108.6 . . ? C3 C30 H30B 108.6 . . ? H30A C30 H30B 107.6 . . ? C30 C31 C32 109.6(4) . . ? C30 C31 H31A 109.8 . . ? C32 C31 H31A 109.8 . . ? C30 C31 H31B 109.8 . . ? C32 C31 H31B 109.8 . . ? H31A C31 H31B 108.2 . . ? O33 C32 N34 121.7(7) . . ? O33 C32 C31 122.7(6) . . ? N34 C32 C31 115.5(5) . . ? C32 N34 H34A 120.0 . . ? C32 N34 H34B 120.0 . . ? H34A N34 H34B 120.0 . . ? C5 C35 H35A 109.5 . . ? C5 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C5 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C7 C36 H36A 109.5 . . ? C7 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C7 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C38 C37 C7 111.6(4) . . ? C38 C37 H37A 109.3 . . ? C7 C37 H37A 109.3 . . ? C38 C37 H37B 109.3 . . ? C7 C37 H37B 109.3 . . ? H37A C37 H37B 108.0 . . ? O39 C38 N40 121.0(4) . . ? O39 C38 C37 120.1(4) . . ? N40 C38 C37 118.8(4) . . ? C38 N40 H40A 120.0 . . ? C38 N40 H40B 120.0 . . ? H40A N40 H40B 120.0 . . ? C42 C41 C8 114.5(3) . . ? C42 C41 H41A 108.6 . . ? C8 C41 H41A 108.6 . . ? C42 C41 H41B 108.6 . . ? C8 C41 H41B 108.6 . . ? H41A C41 H41B 107.6 . . ? C43 C42 C41 109.8(4) . . ? C43 C42 H42A 109.7 . . ? C41 C42 H42A 109.7 . . ? C43 C42 H42B 109.7 . . ? C41 C42 H42B 109.7 . . ? H42A C42 H42B 108.2 . . ? O44 C43 N45 119.2(6) . . ? O44 C43 C42 125.0(5) . . ? N45 C43 C42 115.5(5) . . ? C43 N45 H45A 120.0 . . ? C43 N45 H45B 120.0 . . ? H45A N45 H45B 120.0 . . ? C12 C46 H46A 109.5 . . ? C12 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C12 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C12 C47 H47A 109.5 . . ? C12 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C12 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C49 C48 C13 119.6(5) . . ? C49 C48 H48A 107.4 . . ? C13 C48 H48A 107.4 . . ? C49 C48 H48B 107.4 . . ? C13 C48 H48B 107.4 . . ? H48A C48 H48B 106.9 . . ? C50 C49 C48 114.6(5) . . ? C50 C49 H49A 108.6 . . ? C48 C49 H49A 108.6 . . ? C50 C49 H49B 108.6 . . ? C48 C49 H49B 108.6 . . ? H49A C49 H49B 107.6 . . ? O51 C50 N52 125.8(6) . . ? O51 C50 C49 116.0(5) . . ? N52 C50 C49 118.2(6) . . ? C50 N52 H52A 120.0 . . ? C50 N52 H52B 120.0 . . ? H52A N52 H52B 120.0 . . ? C15 C53 H53A 109.5 . . ? C15 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C15 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C17 C54 H54A 109.5 . . ? C17 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C17 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C56 C55 C17 116.9(2) . . ? C56 C55 H55A 108.1 . . ? C17 C55 H55A 108.1 . . ? C56 C55 H55B 108.1 . . ? C17 C55 H55B 108.1 . . ? H55A C55 H55B 107.3 . . ? C55 C56 C57 111.7(3) . . ? C55 C56 H56A 109.3 . . ? C57 C56 H56A 109.3 . . ? C55 C56 H56B 109.3 . . ? C57 C56 H56B 109.3 . . ? H56A C56 H56B 107.9 . . ? O58 C57 N59 122.2(3) . . ? O58 C57 C56 120.1(3) . . ? N59 C57 C56 117.7(3) . . ? C57 N59 C1PR 125.4(4) . . ? C57 N59 H59 117.3 . . ? C1PR N59 H59 117.3 . . ? C61 C60 C18 115.2(3) . . ? C61 C60 H60A 108.5 . . ? C18 C60 H60A 108.5 . . ? C61 C60 H60B 108.5 . . ? C18 C60 H60B 108.5 . . ? H60A C60 H60B 107.5 . . ? O62 C61 N63 123.3(4) . . ? O62 C61 C60 121.5(4) . . ? N63 C61 C60 115.2(4) . . ? C61 N63 H63A 120.0 . . ? C61 N63 H63B 120.0 . . ? H63A N63 H63B 120.0 . . ? N59 C1PR C2PR 113.1(3) . . ? N59 C1PR H1P1 109.0 . . ? C2PR C1PR H1P1 109.0 . . ? N59 C1PR H1P2 109.0 . . ? C2PR C1PR H1P2 109.0 . . ? H1P1 C1PR H1P2 107.8 . . ? O3P C2PR C1PR 107.1(3) . . ? O3P C2PR C3PR 107.6(3) . . ? C1PR C2PR C3PR 112.0(3) . . ? O3P C2PR H2PR 110.0 . . ? C1PR C2PR H2PR 110.0 . . ? C3PR C2PR H2PR 110.0 . . ? C2PR C3PR H3P1 109.5 . . ? C2PR C3PR H3P2 109.5 . . ? H3P1 C3PR H3P2 109.5 . . ? C2PR C3PR H3P3 109.5 . . ? H3P1 C3PR H3P3 109.5 . . ? H3P2 C3PR H3P3 109.5 . . ? O4P P1 O5P 116.5(2) . . ? O4P P1 O3P 112.70(18) . . ? O5P P1 O3P 106.62(19) . . ? O4P P1 O2P 109.82(19) . . ? O5P P1 O2P 110.4(2) . . ? O3P P1 O2P 99.44(14) . . ? C3R O2P P1 119.9(2) . . ? C2PR O3P P1 120.6(2) . . ? O6R C1R N1B 107.4(3) . . ? O6R C1R C2R 106.9(3) . . ? N1B C1R C2R 112.3(2) . . ? O6R C1R H1R 110.0 . . ? N1B C1R H1R 110.0 . . ? C2R C1R H1R 110.0 . . ? O7R C2R C3R 112.2(3) . . ? O7R C2R C1R 108.7(3) . . ? C3R C2R C1R 99.4(3) . . ? O7R C2R H2R 112.0 . . ? C3R C2R H2R 112.0 . . ? C1R C2R H2R 112.0 . . ? O2P C3R C2R 112.0(3) . . ? O2P C3R C4R 110.7(3) . . ? C2R C3R C4R 103.6(3) . . ? O2P C3R H3R 110.1 . . ? C2R C3R H3R 110.1 . . ? C4R C3R H3R 110.1 . . ? O6R C4R C5R 106.5(4) . . ? O6R C4R C3R 105.9(3) . . ? C5R C4R C3R 114.5(4) . . ? O6R C4R H4R 109.9 . . ? C5R C4R H4R 109.9 . . ? C3R C4R H4R 109.9 . . ? O8R C5R C4R 111.3(6) . . ? O8R C5R H5R1 109.4 . . ? C4R C5R H5R1 109.4 . . ? O8R C5R H5R2 109.4 . . ? C4R C5R H5R2 109.4 . . ? H5R1 C5R H5R2 108.0 . . ? C4R O6R C1R 109.9(3) . . ? C2R O7R H7R 109.5 . . ? C5R O8R H8R 109.5 . . ? C2B N1B C8B 106.9(2) . . ? C2B N1B C1R 125.4(2) . . ? C8B N1B C1R 125.3(3) . . ? N3B C2B N1B 113.3(3) . . ? N3B C2B H2B 123.3 . . ? N1B C2B H2B 123.3 . . ? C2B N3B C9B 104.4(2) . . ? C2B N3B Co 122.6(2) . . ? C9B N3B Co 132.96(18) . . ? C5B C4B C9B 119.2(3) . . ? C5B C4B H4B 120.4 . . ? C9B C4B H4B 120.4 . . ? C4B C5B C6B 121.1(3) . . ? C4B C5B C10B 118.7(4) . . ? C6B C5B C10B 120.2(4) . . ? C7B C6B C5B 120.3(4) . . ? C7B C6B C11B 119.6(4) . . ? C5B C6B C11B 120.0(4) . . ? C6B C7B C8B 117.1(4) . . ? C6B C7B H7B 121.4 . . ? C8B C7B H7B 121.4 . . ? C9B C8B N1B 106.1(3) . . ? C9B C8B C7B 123.4(3) . . ? N1B C8B C7B 130.5(3) . . ? C8B C9B C4B 118.9(3) . . ? C8B C9B N3B 109.3(2) . . ? C4B C9B N3B 131.8(3) . . ? C5B C10B H10A 109.5 . . ? C5B C10B H10B 109.5 . . ? H10A C10B H10B 109.5 . . ? C5B C10B H10C 109.5 . . ? H10A C10B H10C 109.5 . . ? H10B C10B H10C 109.5 . . ? C6B C11B H11A 109.5 . . ? C6B C11B H11B 109.5 . . ? H11A C11B H11B 109.5 . . ? C6B C11B H11C 109.5 . . ? H11A C11B H11C 109.5 . . ? H11B C11B H11C 109.5 . . ? N2C C1C Co 179.5(4) . . ? 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 N21 C1 C2 C25 151.9(3) . . . . ? C20 C1 C2 C25 33.5(4) . . . . ? C19 C1 C2 C25 -96.9(3) . . . . ? N21 C1 C2 C3 29.3(3) . . . . ? C20 C1 C2 C3 -89.1(3) . . . . ? C19 C1 C2 C3 140.5(3) . . . . ? N21 C1 C2 C26 -83.4(3) . . . . ? C20 C1 C2 C26 158.2(3) . . . . ? C19 C1 C2 C26 27.8(3) . . . . ? C25 C2 C3 C4 -155.4(3) . . . . ? C26 C2 C3 C4 82.5(3) . . . . ? C1 C2 C3 C4 -31.8(3) . . . . ? C25 C2 C3 C30 -35.7(4) . . . . ? C26 C2 C3 C30 -157.9(3) . . . . ? C1 C2 C3 C30 87.9(3) . . . . ? C30 C3 C4 N21 -102.3(3) . . . . ? C2 C3 C4 N21 24.5(3) . . . . ? C30 C3 C4 C5 76.7(4) . . . . ? C2 C3 C4 C5 -156.6(3) . . . . ? N21 C4 C5 C6 11.4(6) . . . . ? C3 C4 C5 C6 -167.4(3) . . . . ? N21 C4 C5 C35 -168.7(4) . . . . ? C3 C4 C5 C35 12.5(6) . . . . ? C4 C5 C6 N22 -6.8(6) . . . . ? C35 C5 C6 N22 173.4(4) . . . . ? C4 C5 C6 C7 175.6(4) . . . . ? C35 C5 C6 C7 -4.2(7) . . . . ? C5 C6 C7 C8 -161.3(4) . . . . ? N22 C6 C7 C8 20.8(4) . . . . ? C5 C6 C7 C37 83.7(5) . . . . ? N22 C6 C7 C37 -94.3(4) . . . . ? C5 C6 C7 C36 -40.0(6) . . . . ? N22 C6 C7 C36 142.0(3) . . . . ? C37 C7 C8 C9 84.8(3) . . . . ? C6 C7 C8 C9 -26.9(3) . . . . ? C36 C7 C8 C9 -150.6(3) . . . . ? C37 C7 C8 C41 -156.7(3) . . . . ? C6 C7 C8 C41 91.6(3) . . . . ? C36 C7 C8 C41 -32.1(4) . . . . ? C7 C8 C9 N22 26.7(4) . . . . ? C41 C8 C9 N22 -92.9(4) . . . . ? C7 C8 C9 C10 -150.8(4) . . . . ? C41 C8 C9 C10 89.5(4) . . . . ? N22 C9 C10 C11 -0.3(7) . . . . ? C8 C9 C10 C11 176.8(4) . . . . ? C9 C10 C11 N23 8.5(7) . . . . ? C9 C10 C11 C12 -167.7(4) . . . . ? N23 C11 C12 C46 147.1(5) . . . . ? C10 C11 C12 C46 -36.3(7) . . . . ? N23 C11 C12 C13 22.6(5) . . . . ? C10 C11 C12 C13 -160.8(4) . . . . ? N23 C11 C12 C47 -91.2(4) . . . . ? C10 C11 C12 C47 85.4(5) . . . . ? C11 C12 C13 C14 -26.6(4) . . . . ? C46 C12 C13 C14 -148.4(4) . . . . ? C47 C12 C13 C14 85.0(4) . . . . ? C11 C12 C13 C48 89.7(4) . . . . ? C46 C12 C13 C48 -32.2(6) . . . . ? C47 C12 C13 C48 -158.7(4) . . . . ? C12 C13 C14 C15 -160.7(4) . . . . ? C48 C13 C14 C15 74.0(5) . . . . ? C12 C13 C14 N23 24.2(4) . . . . ? C48 C13 C14 N23 -101.1(3) . . . . ? N23 C14 C15 C16 2.9(6) . . . . ? C13 C14 C15 C16 -171.3(3) . . . . ? N23 C14 C15 C53 -175.7(4) . . . . ? C13 C14 C15 C53 10.1(6) . . . . ? C14 C15 C16 N24 2.1(5) . . . . ? C53 C15 C16 N24 -179.3(3) . . . . ? C14 C15 C16 C17 -172.5(3) . . . . ? C53 C15 C16 C17 6.0(5) . . . . ? N24 C16 C17 C54 -101.8(3) . . . . ? C15 C16 C17 C54 73.4(4) . . . . ? N24 C16 C17 C55 136.1(3) . . . . ? C15 C16 C17 C55 -48.7(4) . . . . ? N24 C16 C17 C18 15.5(3) . . . . ? C15 C16 C17 C18 -169.3(3) . . . . ? C54 C17 C18 C19 84.0(3) . . . . ? C55 C17 C18 C19 -153.2(2) . . . . ? C16 C17 C18 C19 -29.9(3) . . . . ? C54 C17 C18 C60 -40.8(4) . . . . ? C55 C17 C18 C60 82.0(3) . . . . ? C16 C17 C18 C60 -154.6(3) . . . . ? C60 C18 C19 N24 160.5(3) . . . . ? C17 C18 C19 N24 33.9(3) . . . . ? C60 C18 C19 C1 -79.9(4) . . . . ? C17 C18 C19 C1 153.5(2) . . . . ? N21 C1 C19 N24 -42.2(3) . . . . ? C20 C1 C19 N24 74.8(3) . . . . ? C2 C1 C19 N24 -153.0(2) . . . . ? N21 C1 C19 C18 -159.8(2) . . . . ? C20 C1 C19 C18 -42.8(3) . . . . ? C2 C1 C19 C18 89.4(3) . . . . ? C5 C4 N21 C1 176.0(3) . . . . ? C3 C4 N21 C1 -5.1(4) . . . . ? C5 C4 N21 Co 3.5(5) . . . . ? C3 C4 N21 Co -177.5(2) . . . . ? C20 C1 N21 C4 104.1(3) . . . . ? C19 C1 N21 C4 -139.8(3) . . . . ? C2 C1 N21 C4 -16.2(3) . . . . ? C20 C1 N21 Co -82.4(3) . . . . ? C19 C1 N21 Co 33.7(3) . . . . ? C2 C1 N21 Co 157.24(19) . . . . ? C1C Co N21 C4 72.6(3) . . . . ? N24 Co N21 C4 160.1(3) . . . . ? N22 Co N21 C4 -15.5(3) . . . . ? N23 Co N21 C4 176.5(9) . . . . ? N3B Co N21 C4 -105.0(3) . . . . ? C1C Co N21 C1 -99.7(2) . . . . ? N24 Co N21 C1 -12.1(2) . . . . ? N22 Co N21 C1 172.3(2) . . . . ? N23 Co N21 C1 4.2(11) . . . . ? N3B Co N21 C1 82.7(2) . . . . ? C10 C9 N22 C6 163.3(4) . . . . ? C8 C9 N22 C6 -14.2(4) . . . . ? C10 C9 N22 Co -8.3(5) . . . . ? C8 C9 N22 Co 174.2(2) . . . . ? C5 C6 N22 C9 177.1(4) . . . . ? C7 C6 N22 C9 -4.9(4) . . . . ? C5 C6 N22 Co -11.7(5) . . . . ? C7 C6 N22 Co 166.4(2) . . . . ? C1C Co N22 C9 97.7(3) . . . . ? N21 Co N22 C9 -170.7(3) . . . . ? N24 Co N22 C9 156.2(7) . . . . ? N23 Co N22 C9 7.9(3) . . . . ? N3B Co N22 C9 -79.4(3) . . . . ? C1C Co N22 C6 -72.6(3) . . . . ? N21 Co N22 C6 19.0(3) . . . . ? N24 Co N22 C6 -14.1(9) . . . . ? N23 Co N22 C6 -162.4(3) . . . . ? N3B Co N22 C6 110.3(3) . . . . ? C10 C11 N23 C14 175.5(4) . . . . ? C12 C11 N23 C14 -7.9(5) . . . . ? C10 C11 N23 Co -6.2(6) . . . . ? C12 C11 N23 Co 170.3(3) . . . . ? C15 C14 N23 C11 174.0(4) . . . . ? C13 C14 N23 C11 -11.0(4) . . . . ? C15 C14 N23 Co -4.2(5) . . . . ? C13 C14 N23 Co 170.8(2) . . . . ? C1C Co N23 C11 -89.1(3) . . . . ? N21 Co N23 C11 166.9(9) . . . . ? N24 Co N23 C11 -176.9(3) . . . . ? N22 Co N23 C11 -1.1(3) . . . . ? N3B Co N23 C11 88.2(3) . . . . ? C1C Co N23 C14 88.8(3) . . . . ? N21 Co N23 C14 -15.1(12) . . . . ? N24 Co N23 C14 1.1(3) . . . . ? N22 Co N23 C14 176.9(3) . . . . ? N3B Co N23 C14 -93.9(3) . . . . ? C15 C16 N24 C19 -169.1(3) . . . . ? C17 C16 N24 C19 6.4(3) . . . . ? C15 C16 N24 Co -5.9(5) . . . . ? C17 C16 N24 Co 169.5(2) . . . . ? C18 C19 N24 C16 -26.1(3) . . . . ? C1 C19 N24 C16 -156.1(2) . . . . ? C18 C19 N24 Co 167.34(18) . . . . ? C1 C19 N24 Co 37.4(3) . . . . ? C1C Co N24 C16 -86.1(3) . . . . ? N21 Co N24 C16 -177.9(3) . . . . ? N22 Co N24 C16 -144.6(7) . . . . ? N23 Co N24 C16 3.9(3) . . . . ? N3B Co N24 C16 91.3(3) . . . . ? C1C Co N24 C19 76.8(2) . . . . ? N21 Co N24 C19 -15.08(19) . . . . ? N22 Co N24 C19 18.3(9) . . . . ? N23 Co N24 C19 166.79(19) . . . . ? N3B Co N24 C19 -105.83(19) . . . . ? C25 C2 C26 C27 -56.9(4) . . . . ? C3 C2 C26 C27 67.1(4) . . . . ? C1 C2 C26 C27 175.9(3) . . . . ? C2 C26 C27 O28 -52.1(10) . . . . ? C2 C26 C27 N29 130.5(5) . . . . ? C4 C3 C30 C31 -151.8(4) . . . . ? C2 C3 C30 C31 92.4(4) . . . . ? C3 C30 C31 C32 172.9(4) . . . . ? C30 C31 C32 O33 -89.3(8) . . . . ? C30 C31 C32 N34 93.4(6) . . . . ? C8 C7 C37 C38 67.2(4) . . . . ? C6 C7 C37 C38 175.8(3) . . . . ? C36 C7 C37 C38 -57.8(5) . . . . ? C7 C37 C38 O39 -82.5(7) . . . . ? C7 C37 C38 N40 94.6(6) . . . . ? C9 C8 C41 C42 -56.0(4) . . . . ? C7 C8 C41 C42 -168.9(3) . . . . ? C8 C41 C42 C43 -178.3(4) . . . . ? C41 C42 C43 O44 30.6(9) . . . . ? C41 C42 C43 N45 -156.0(6) . . . . ? C14 C13 C48 C49 -167.0(4) . . . . ? C12 C13 C48 C49 79.5(5) . . . . ? C13 C48 C49 C50 45.5(7) . . . . ? C48 C49 C50 O51 -114.0(7) . . . . ? C48 C49 C50 N52 66.6(8) . . . . ? C54 C17 C55 C56 -169.8(3) . . . . ? C18 C17 C55 C56 65.9(3) . . . . ? C16 C17 C55 C56 -48.7(4) . . . . ? C17 C55 C56 C57 168.3(3) . . . . ? C55 C56 C57 O58 -59.3(5) . . . . ? C55 C56 C57 N59 120.3(4) . . . . ? O58 C57 N59 C1PR -3.3(6) . . . . ? C56 C57 N59 C1PR 177.1(3) . . . . ? C19 C18 C60 C61 163.6(3) . . . . ? C17 C18 C60 C61 -77.5(4) . . . . ? C18 C60 C61 O62 -37.2(6) . . . . ? C18 C60 C61 N63 143.8(4) . . . . ? C57 N59 C1PR C2PR -97.5(5) . . . . ? N59 C1PR C2PR O3P -56.3(4) . . . . ? N59 C1PR C2PR C3PR -174.1(4) . . . . ? O4P P1 O2P C3R 53.3(3) . . . . ? O5P P1 O2P C3R -76.5(3) . . . . ? O3P P1 O2P C3R 171.8(3) . . . . ? C1PR C2PR O3P P1 132.3(3) . . . . ? C3PR C2PR O3P P1 -107.1(4) . . . . ? O4P P1 O3P C2PR 51.1(3) . . . . ? O5P P1 O3P C2PR -179.9(3) . . . . ? O2P P1 O3P C2PR -65.2(3) . . . . ? O6R C1R C2R O7R 83.3(3) . . . . ? N1B C1R C2R O7R -34.2(4) . . . . ? O6R C1R C2R C3R -34.1(3) . . . . ? N1B C1R C2R C3R -151.6(3) . . . . ? P1 O2P C3R C2R 113.7(3) . . . . ? P1 O2P C3R C4R -131.2(3) . . . . ? O7R C2R C3R O2P 40.7(4) . . . . ? C1R C2R C3R O2P 155.4(3) . . . . ? O7R C2R C3R C4R -78.6(3) . . . . ? C1R C2R C3R C4R 36.1(3) . . . . ? O2P C3R C4R O6R -147.4(3) . . . . ? C2R C3R C4R O6R -27.1(4) . . . . ? O2P C3R C4R C5R 95.6(5) . . . . ? C2R C3R C4R C5R -144.1(5) . . . . ? O6R C4R C5R O8R -56.8(7) . . . . ? C3R C4R C5R O8R 59.8(7) . . . . ? C5R C4R O6R C1R 127.7(5) . . . . ? C3R C4R O6R C1R 5.4(4) . . . . ? N1B C1R O6R C4R 139.4(3) . . . . ? C2R C1R O6R C4R 18.7(4) . . . . ? O6R C1R N1B C2B -44.7(4) . . . . ? C2R C1R N1B C2B 72.6(4) . . . . ? O6R C1R N1B C8B 155.3(3) . . . . ? C2R C1R N1B C8B -87.4(3) . . . . ? C8B N1B C2B N3B -2.7(3) . . . . ? C1R N1B C2B N3B -165.7(3) . . . . ? N1B C2B N3B C9B 2.8(3) . . . . ? N1B C2B N3B Co -174.05(19) . . . . ? C1C Co N3B C2B 87.5(19) . . . . ? N21 Co N3B C2B -131.5(2) . . . . ? N24 Co N3B C2B -48.2(2) . . . . ? N22 Co N3B C2B 138.4(2) . . . . ? N23 Co N3B C2B 41.9(2) . . . . ? C1C Co N3B C9B -88.4(19) . . . . ? N21 Co N3B C9B 52.7(2) . . . . ? N24 Co N3B C9B 136.0(2) . . . . ? N22 Co N3B C9B -37.4(2) . . . . ? N23 Co N3B C9B -133.9(2) . . . . ? C9B C4B C5B C6B 1.9(5) . . . . ? C9B C4B C5B C10B -179.8(4) . . . . ? C4B C5B C6B C7B -0.8(6) . . . . ? C10B C5B C6B C7B -179.0(4) . . . . ? C4B C5B C6B C11B -178.4(5) . . . . ? C10B C5B C6B C11B 3.4(7) . . . . ? C5B C6B C7B C8B 0.0(6) . . . . ? C11B C6B C7B C8B 177.7(5) . . . . ? C2B N1B C8B C9B 1.3(3) . . . . ? C1R N1B C8B C9B 164.4(3) . . . . ? C2B N1B C8B C7B -178.0(3) . . . . ? C1R N1B C8B C7B -15.0(5) . . . . ? C6B C7B C8B C9B -0.5(5) . . . . ? C6B C7B C8B N1B 178.8(3) . . . . ? N1B C8B C9B C4B -177.8(3) . . . . ? C7B C8B C9B C4B 1.7(5) . . . . ? N1B C8B C9B N3B 0.3(3) . . . . ? C7B C8B C9B N3B 179.7(3) . . . . ? C5B C4B C9B C8B -2.3(4) . . . . ? C5B C4B C9B N3B -179.9(3) . . . . ? C2B N3B C9B C8B -1.8(3) . . . . ? Co N3B C9B C8B 174.5(2) . . . . ? C2B N3B C9B C4B 175.9(3) . . . . ? Co N3B C9B C4B -7.7(5) . . . . ? N21 Co C1C N2C 115(60) . . . . ? N24 Co C1C N2C 32(60) . . . . ? N22 Co C1C N2C -155(100) . . . . ? N23 Co C1C N2C -58(60) . . . . ? N3B Co C1C N2C -104(60) . . . . ? _diffrn_measured_fraction_theta_max 0.959 _diffrn_reflns_theta_full 30.79 _diffrn_measured_fraction_theta_full 0.959 _refine_diff_density_max 0.821 _refine_diff_density_min -0.536 _refine_diff_density_rms 0.181 #===END data_B12_1.0_GPa _database_code_depnum_ccdc_archive 'CCDC 766944' #TrackingRef 'b12_Fabbiani_combined.cif' #B12_1.0_GPa_and_room_temperature _refine_special_details ; All H-atoms were placed geometrically and allowed to ride on the parent atoms. H-Uiso were assigned in the range 1.2-1.5 times Ueq of the parent atom. All water O-atoms were modelled with isotropic displacement parameters. Water O-atoms sites were assigned based the peak height of Fourier difference peaks. OW1-OW20 were assigned full site occupancy, whilst OW22-OW24 were assigned half site occupancy. A threshold of Uiso max. = 0.2 A^2^ was used for assignment of meaningful OW sites. The Following ALERTS were generated by PLATON checkcif<<< PLAT029_ALERT_3_A _diffrn_measured_fraction_theta_full Low ....... 0.80 THETM01_ALERT_3_C The value of sine(theta_max)/wavelength is less than 0.590 Calculated sin(theta_max)/wavelength = 0.5760 PLAT952_ALERT_1_C Reported and Calculated Lmax Values Differ by .. 5 Resolution and completeness are reported below: #=============================================================================== Resolution & Completeness Statistics (Cumulative) #=============================================================================== Theta sin(th)/Lambda Complete Expected Measured Missing #------------------------------------------------------------------------------- 21.10 0.500 0.851 4653 3958 695 23.33 0.550 0.824 6151 5067 1084 24.50 0.576 0.803 7031 5646 1385 #----------------------------------------------------------- ACTA Min. Res. --- PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) ....... OW1 PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) ....... OW2 PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) ....... OW3 PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) ....... OW4 PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) ....... OW5 PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) ....... OW6 PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) ....... OW7 PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) ....... OW8 PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) ....... OW9 PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) ....... OW10 PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) ....... OW11 PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) ....... OW12 PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) ....... OW13 PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) ....... OW14 PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) ....... OW15 PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) ....... OW16 PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) ....... OW17 PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) ....... OW18 PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) ....... OW19 PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) ....... OW20 PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) ....... OW21 PLAT430_ALERT_2_A Short Inter D...A Contact OW13 .. OW21 .. 2.45 Ang. PLAT430_ALERT_2_B Short Inter D...A Contact OW1 .. OW2 .. 2.68 Ang. PLAT430_ALERT_2_B Short Inter D...A Contact OW1 .. O4P .. 2.78 Ang. PLAT430_ALERT_2_B Short Inter D...A Contact OW3 .. O5P .. 2.67 Ang. PLAT430_ALERT_2_B Short Inter D...A Contact OW3 .. OW5 .. 2.80 Ang. PLAT430_ALERT_2_B Short Inter D...A Contact OW4 .. O4P .. 2.68 Ang. PLAT430_ALERT_2_B Short Inter D...A Contact OW4 .. O62 .. 2.79 Ang. PLAT430_ALERT_2_B Short Inter D...A Contact OW5 .. O58 .. 2.73 Ang. PLAT430_ALERT_2_B Short Inter D...A Contact OW7 .. OW16 .. 2.72 Ang. PLAT430_ALERT_2_B Short Inter D...A Contact OW8 .. OW23 .. 2.67 Ang. PLAT430_ALERT_2_B Short Inter D...A Contact OW8 .. OW15 .. 2.68 Ang. PLAT430_ALERT_2_B Short Inter D...A Contact OW8 .. OW10 .. 2.81 Ang. PLAT430_ALERT_2_B Short Inter D...A Contact OW9 .. OW24 .. 2.75 Ang. PLAT430_ALERT_2_B Short Inter D...A Contact OW10 .. OW20 .. 2.76 Ang. PLAT430_ALERT_2_B Short Inter D...A Contact OW13 .. OW18 .. 2.82 Ang. PLAT430_ALERT_2_B Short Inter D...A Contact OW15 .. O62 .. 2.75 Ang. PLAT430_ALERT_2_B Short Inter D...A Contact OW17 .. OW19 .. 2.60 Ang. PLAT430_ALERT_2_B Short Inter D...A Contact OW17 .. OW20 .. 2.62 Ang. PLAT430_ALERT_2_B Short Inter D...A Contact OW19 .. O44 .. 2.69 Ang. PLAT430_ALERT_2_B Short Inter D...A Contact OW21 .. O51 .. 2.70 Ang. PLAT430_ALERT_2_B Short Inter D...A Contact OW23 .. O28 .. 2.74 Ang. PLAT430_ALERT_2_C Short Inter D...A Contact OW2 .. OW15 .. 2.86 Ang. PLAT430_ALERT_2_C Short Inter D...A Contact OW9 .. OW13 .. 2.88 Ang. PLAT430_ALERT_2_C Short Inter D...A Contact OW11 .. OW12 .. 2.88 Ang. PLAT430_ALERT_2_C Short Inter D...A Contact OW11 .. O33 .. 2.89 Ang. PLAT430_ALERT_2_C Short Inter D...A Contact OW12 .. OW16 .. 2.87 Ang. PLAT430_ALERT_2_C Short Inter D...A Contact OW12 .. OW13 .. 2.88 Ang. PLAT430_ALERT_2_C Short Inter D...A Contact OW13 .. OW20 .. 2.85 Ang. PLAT430_ALERT_2_C Short Inter D...A Contact OW14 .. OW15 .. 2.86 Ang. H-atoms were not added to water molecules and H-bonds are hence missing. Alert level C CHEMW03_ALERT_2_C The ratio of given/expected molecular weight as calculated from the _atom_site* data lies outside the range 0.99 <> 1.01 From the CIF: _cell_formula_units_Z 4 From the CIF: _chemical_formula_weight 1751.73 TEST: Calculate formula weight from _atom_site_* atom mass num sum C 12.01 63.00 756.69 H 1.01 88.00 88.70 N 14.01 14.00 196.10 O 16.00 36.00 575.96 P 30.97 1.00 30.97 Co 58.93 1.00 58.93 Calculated formula weight 1707.37 PLAT041_ALERT_1_C Calc. and Reported SumFormula Strings Differ ? PLAT042_ALERT_1_C Calc. and Reported MoietyFormula Strings Differ ? PLAT043_ALERT_1_C Check Reported Molecular Weight ................ 1751.73 Water H-atoms were included in the molecular formula but not in the model. PLAT410_ALERT_2_C Short Intra H...H Contact H19 .. H26B .. 1.95 Ang. Alerts of short H .. H contact involving methyl H-atoms often arise from the fact that they involve H-atoms at not optimal calculated positions. PLAT202_ALERT_3_C Isotropic non-H Atoms in Anion/Solvent ......... 20 PLAT234_ALERT_4_C Large Hirshfeld Difference C12 -- C47 .. 0.16 Ang. PLAT220_ALERT_2_C Large Non-Solvent N Ueq(max)/Ueq(min) ... 3.12 Ratio PLAT222_ALERT_3_C Large Non-Solvent H Ueq(max)/Ueq(min) ... 3.55 Ratio PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for O2P PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C27 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C32 PLAT341_ALERT_3_C Low Bond Precision on C-C Bonds (x 1000) Ang .. 11 PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 2 O2 PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 5 O PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 6 O PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 7 O PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 10 O PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 11 O PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 13 O PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 15 O PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 19 O PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 20 O PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 21 O PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 22 O PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 23 O All noted, all OK. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; 5,6-Dimethylbenzimidazolyl cyanocobamide hydrate ; _chemical_name_common 'cyanocobalamin hydrate' _chemical_melting_point ? _chemical_formula_moiety 'C63 H88 Co N14 O14 P, 22 H2O' _chemical_formula_sum 'C63 H132 Co N14 O36 P' _chemical_formula_weight 1751.73 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' P P 0.1023 0.0942 '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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' loop_ _symmetry_equiv_pos_as_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' _cell_length_a 15.9455(4) _cell_length_b 21.0511(5) _cell_length_c 23.8739(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8013.8(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 9928 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 24.27 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.452 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3752 _exptl_absorpt_coefficient_mu 0.333 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'based on symmetry-related measuraments' # SHADE (Parsons, 2004) # SADABS (Siemens, 1996) # The following data are from Sadabs: _exptl_absorpt_correction_T_min 0.6461 _exptl_absorpt_correction_T_max 0.8619 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_measurement_device 'Bruker AXS SMART APEX' _diffrn_measurement_device_type Area _diffrn_radiation_monochromator silicon _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.72000 _diffrn_measurement_method '\f & \w scans' _diffrn_reflns_number 53048 _diffrn_reflns_av_R_equivalents 0.052 _diffrn_reflns_av_sigmaI/netI 0.0606 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.31 _diffrn_reflns_theta_max 24.50 _reflns_number_total 10032 _reflns_number_gt 7534 _reflns_threshold_expression >2sigma(I) _diffrn_reflns_reduction_process ; Scaled and merged with XPREP ; _computing_data_collection 'Apex2 (Bruker AXS, 2006)' _computing_cell_refinement 'Apex2 (Bruker AXS, 2006)' _computing_data_reduction 'Apex2 (Bruker AXS, 2006)' _computing_structure_solution 'known coordinates' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_publication_material 'COOT, PLATON, XCIF, ENCIFER, MERCURY' _computing_molecular_graphics 'MERCURY, COOT' _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1602P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary 'known coordinates' _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.02(2) _chemical_absolute_configuration rm _refine_ls_number_reflns 10032 _refine_ls_number_parameters 936 _refine_ls_number_restraints 168 _refine_ls_R_factor_all 0.0968 _refine_ls_R_factor_gt 0.0665 _refine_ls_wR_factor_ref 0.2165 _refine_ls_wR_factor_gt 0.1837 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 Co Co 0.22669(5) 0.88195(4) 0.21927(5) 0.0346(3) Uani 1 1 d . . . C1 C 0.3517(4) 0.8000(3) 0.2675(4) 0.047(2) Uani 1 1 d U . . C2 C 0.4484(4) 0.7877(3) 0.2535(4) 0.040(2) Uani 1 1 d U . . C3 C 0.4829(4) 0.8565(3) 0.2485(4) 0.0313(18) Uani 1 1 d U . . H3 H 0.5264 0.8573 0.2195 0.038 Uiso 1 1 calc R . . C4 C 0.4049(4) 0.8926(3) 0.2264(4) 0.039(2) Uani 1 1 d U . . C5 C 0.4115(4) 0.9528(3) 0.1988(4) 0.041(2) Uani 1 1 d U . . C6 C 0.3408(4) 0.9880(3) 0.1889(4) 0.036(2) Uani 1 1 d U . . C7 C 0.3314(4) 1.0541(3) 0.1614(4) 0.042(2) Uani 1 1 d U . . C8 C 0.2482(4) 1.0762(3) 0.1882(4) 0.042(2) Uani 1 1 d U . . H8 H 0.2177 1.1046 0.1629 0.051 Uiso 1 1 calc R . . C9 C 0.2030(4) 1.0135(3) 0.1941(4) 0.036(2) Uani 1 1 d U . . C10 C 0.1176(4) 1.0068(3) 0.1888(4) 0.040(2) Uani 1 1 d U . . H10 H 0.0859 1.0435 0.1837 0.048 Uiso 1 1 calc R . . C11 C 0.0754(4) 0.9487(3) 0.1905(4) 0.039(2) Uani 1 1 d U . . C12 C -0.0142(4) 0.9409(3) 0.1722(4) 0.0382(19) Uani 1 1 d U . . C13 C -0.0383(4) 0.8757(3) 0.1989(4) 0.042(2) Uani 1 1 d U . . H13 H -0.0742 0.8511 0.1736 0.050 Uiso 1 1 calc R . . C14 C 0.0486(4) 0.8445(3) 0.2050(3) 0.0302(19) Uani 1 1 d U . . C15 C 0.0607(4) 0.7830(3) 0.2166(4) 0.040(2) Uani 1 1 d U . . C16 C 0.1435(4) 0.7580(3) 0.2308(4) 0.037(2) Uani 1 1 d U . . C17 C 0.1660(4) 0.6889(3) 0.2411(4) 0.043(2) Uani 1 1 d U . . C18 C 0.2546(4) 0.6971(3) 0.2704(4) 0.044(2) Uani 1 1 d U . . H18 H 0.2461 0.7065 0.3102 0.053 Uiso 1 1 calc R . . C19 C 0.2866(4) 0.7567(3) 0.2410(4) 0.046(2) Uani 1 1 d U . . H19 H 0.3064 0.7447 0.2037 0.055 Uiso 1 1 calc R . . C20 C 0.3341(4) 0.8064(3) 0.3287(4) 0.052(2) Uani 1 1 d U . . H20A H 0.3751 0.8338 0.3455 0.078 Uiso 1 1 calc R . . H20B H 0.3366 0.7653 0.3461 0.078 Uiso 1 1 calc R . . H20C H 0.2792 0.8242 0.3339 0.078 Uiso 1 1 calc R . . N21 N 0.3384(3) 0.8620(2) 0.2386(3) 0.0330(17) Uani 1 1 d . . . N22 N 0.2591(3) 0.9671(2) 0.2018(3) 0.0342(17) Uani 1 1 d . . . N23 N 0.1100(3) 0.8932(2) 0.2038(3) 0.0358(18) Uani 1 1 d . . . N24 N 0.2094(3) 0.7948(3) 0.2345(3) 0.0374(18) Uani 1 1 d . . . C25 C 0.4943(4) 0.7488(3) 0.2986(4) 0.044(2) Uani 1 1 d . . . H25A H 0.4889 0.7697 0.3341 0.067 Uiso 1 1 calc R . . H25B H 0.5526 0.7454 0.2890 0.067 Uiso 1 1 calc R . . H25C H 0.4701 0.7072 0.3008 0.067 Uiso 1 1 calc R . . C26 C 0.4562(4) 0.7558(3) 0.1973(4) 0.044(2) Uani 1 1 d . . . H26A H 0.4333 0.7836 0.1688 0.053 Uiso 1 1 calc R . . H26B H 0.4230 0.7172 0.1975 0.053 Uiso 1 1 calc R . . C27 C 0.5471(4) 0.7390(4) 0.1817(4) 0.045(2) Uani 1 1 d U . . O28 O 0.6021(3) 0.7803(3) 0.1765(3) 0.075(2) Uani 1 1 d U . . N29 N 0.5638(4) 0.6778(3) 0.1760(4) 0.067(3) Uani 1 1 d U . . H29A H 0.6141 0.6657 0.1685 0.081 Uiso 1 1 calc R . . H29B H 0.5245 0.6502 0.1798 0.081 Uiso 1 1 calc R . . C30 C 0.5170(4) 0.8906(3) 0.3016(4) 0.043(2) Uani 1 1 d U . . H30A H 0.5053 0.9357 0.2986 0.052 Uiso 1 1 calc R . . H30B H 0.4874 0.8747 0.3342 0.052 Uiso 1 1 calc R . . C31 C 0.6110(4) 0.8813(4) 0.3103(4) 0.054(2) Uani 1 1 d . . . H31A H 0.6224 0.8385 0.3232 0.064 Uiso 1 1 calc R . . H31B H 0.6409 0.8882 0.2755 0.064 Uiso 1 1 calc R . . C32 C 0.6383(4) 0.9290(3) 0.3537(5) 0.057(3) Uani 1 1 d DU . . O33 O 0.6678(4) 0.9816(3) 0.3394(3) 0.072(2) Uani 1 1 d DU . . N34 N 0.6265(6) 0.9116(5) 0.4065(5) 0.103(4) Uani 1 1 d DU . . H34A H 0.6393 0.9372 0.4333 0.124 Uiso 1 1 calc R . . H34B H 0.6060 0.8748 0.4140 0.124 Uiso 1 1 calc R . . C35 C 0.4984(4) 0.9764(4) 0.1833(4) 0.053(3) Uani 1 1 d . . . H35A H 0.5394 0.9452 0.1940 0.079 Uiso 1 1 calc R . . H35B H 0.5096 1.0155 0.2026 0.079 Uiso 1 1 calc R . . H35C H 0.5013 0.9832 0.1436 0.079 Uiso 1 1 calc R . . C36 C 0.4019(4) 1.1027(3) 0.1712(4) 0.049(2) Uani 1 1 d . . . H36A H 0.4526 1.0878 0.1541 0.074 Uiso 1 1 calc R . . H36B H 0.4106 1.1080 0.2107 0.074 Uiso 1 1 calc R . . H36C H 0.3863 1.1427 0.1549 0.074 Uiso 1 1 calc R . . C37 C 0.3139(4) 1.0458(3) 0.0982(5) 0.051(2) Uani 1 1 d U . . H37A H 0.3008 1.0871 0.0825 0.061 Uiso 1 1 calc R . . H37B H 0.2647 1.0192 0.0939 0.061 Uiso 1 1 calc R . . C38 C 0.3863(5) 1.0164(3) 0.0641(5) 0.056(3) Uani 1 1 d DU . . O39 O 0.4421(4) 1.0498(3) 0.0454(3) 0.069(2) Uani 1 1 d U . . N40 N 0.3853(4) 0.9540(3) 0.0579(4) 0.068(3) Uani 1 1 d DU . . H40A H 0.4252 0.9354 0.0401 0.081 Uiso 1 1 calc R . . H40B H 0.3448 0.9320 0.0717 0.081 Uiso 1 1 calc R . . C41 C 0.2587(4) 1.1069(3) 0.2470(4) 0.050(3) Uani 1 1 d . . . H41A H 0.2962 1.0807 0.2692 0.060 Uiso 1 1 calc R . . H41B H 0.2849 1.1482 0.2426 0.060 Uiso 1 1 calc R . . C42 C 0.1782(4) 1.1148(4) 0.2779(4) 0.053(3) Uani 1 1 d . . . H42A H 0.1497 1.0741 0.2801 0.064 Uiso 1 1 calc R . . H42B H 0.1423 1.1439 0.2575 0.064 Uiso 1 1 calc R . . C43 C 0.1927(5) 1.1397(4) 0.3359(5) 0.053(3) Uani 1 1 d U . . O44 O 0.2566(4) 1.1683(3) 0.3500(3) 0.069(2) Uani 1 1 d U . . N45 N 0.1309(4) 1.1302(3) 0.3730(4) 0.067(2) Uani 1 1 d U . . H45A H 0.1360 1.1441 0.4067 0.080 Uiso 1 1 calc R . . H45B H 0.0862 1.1103 0.3631 0.080 Uiso 1 1 calc R . . C46 C -0.0710(5) 0.9959(4) 0.1857(5) 0.060(3) Uani 1 1 d U . . H46A H -0.1271 0.9862 0.1739 0.090 Uiso 1 1 calc R . . H46B H -0.0516 1.0332 0.1665 0.090 Uiso 1 1 calc R . . H46C H -0.0705 1.0035 0.2254 0.090 Uiso 1 1 calc R . . C47 C -0.0122(6) 0.9313(4) 0.1080(5) 0.065(3) Uani 1 1 d U . . H47A H 0.0229 0.8956 0.0991 0.097 Uiso 1 1 calc R . . H47B H 0.0098 0.9688 0.0904 0.097 Uiso 1 1 calc R . . H47C H -0.0680 0.9235 0.0946 0.097 Uiso 1 1 calc R . . C48 C -0.0757(4) 0.8780(4) 0.2578(4) 0.052(3) Uani 1 1 d . . . H48A H -0.0434 0.9081 0.2798 0.062 Uiso 1 1 calc R . . H48B H -0.0685 0.8365 0.2748 0.062 Uiso 1 1 calc R . . C49 C -0.1692(4) 0.8964(4) 0.2624(4) 0.054(3) Uani 1 1 d . . . H49A H -0.1894 0.8849 0.2994 0.065 Uiso 1 1 calc R . . H49B H -0.1743 0.9421 0.2586 0.065 Uiso 1 1 calc R . . C50 C -0.2220(4) 0.8661(3) 0.2207(4) 0.045(2) Uani 1 1 d U . . O51 O -0.2558(4) 0.8977(3) 0.1825(3) 0.067(2) Uani 1 1 d U . . N52 N -0.2339(4) 0.8033(3) 0.2249(4) 0.056(2) Uani 1 1 d U . . H52A H -0.2653 0.7840 0.2010 0.067 Uiso 1 1 calc R . . H52B H -0.2103 0.7822 0.2514 0.067 Uiso 1 1 calc R . . C53 C -0.0140(4) 0.7381(3) 0.2113(5) 0.055(3) Uani 1 1 d . . . H53A H 0.0040 0.6989 0.1946 0.082 Uiso 1 1 calc R . . H53B H -0.0562 0.7574 0.1881 0.082 Uiso 1 1 calc R . . H53C H -0.0369 0.7299 0.2478 0.082 Uiso 1 1 calc R . . C54 C 0.1703(5) 0.6530(3) 0.1871(4) 0.051(3) Uani 1 1 d . . . H54A H 0.1839 0.6094 0.1946 0.077 Uiso 1 1 calc R . . H54B H 0.2128 0.6713 0.1636 0.077 Uiso 1 1 calc R . . H54C H 0.1171 0.6552 0.1685 0.077 Uiso 1 1 calc R . . C55 C 0.1065(4) 0.6536(3) 0.2821(4) 0.039(2) Uani 1 1 d . . . H55A H 0.0543 0.6451 0.2625 0.047 Uiso 1 1 calc R . . H55B H 0.1316 0.6128 0.2908 0.047 Uiso 1 1 calc R . . C56 C 0.0853(5) 0.6858(4) 0.3365(4) 0.053(3) Uani 1 1 d . . . H56A H 0.1327 0.6822 0.3618 0.063 Uiso 1 1 calc R . . H56B H 0.0755 0.7306 0.3296 0.063 Uiso 1 1 calc R . . C57 C 0.0097(5) 0.6579(4) 0.3638(4) 0.056(3) Uani 1 1 d D . . O58 O -0.0602(3) 0.6603(3) 0.3411(3) 0.065(2) Uani 1 1 d . . . N59 N 0.0201(4) 0.6265(3) 0.4110(4) 0.055(2) Uani 1 1 d D . . H59 H 0.0703 0.6223 0.4236 0.066 Uiso 1 1 calc R . . C60 C 0.3134(4) 0.6394(3) 0.2649(5) 0.053(3) Uani 1 1 d U . . H60A H 0.3172 0.6277 0.2257 0.064 Uiso 1 1 calc R . . H60B H 0.3691 0.6517 0.2772 0.064 Uiso 1 1 calc R . . C61 C 0.2864(4) 0.5825(3) 0.2977(4) 0.047(3) Uani 1 1 d DU . . O62 O 0.2606(4) 0.5883(2) 0.3458(4) 0.061(2) Uani 1 1 d DU . . N63 N 0.2961(4) 0.5259(3) 0.2727(4) 0.054(2) Uani 1 1 d U . . H63A H 0.2840 0.4916 0.2905 0.065 Uiso 1 1 calc R . . H63B H 0.3143 0.5239 0.2388 0.065 Uiso 1 1 calc R . . C1PR C -0.0484(5) 0.5982(4) 0.4433(4) 0.053(3) Uani 1 1 d . . . H1P1 H -0.0276 0.5610 0.4628 0.064 Uiso 1 1 calc R . . H1P2 H -0.0920 0.5844 0.4177 0.064 Uiso 1 1 calc R . . C2PR C -0.0854(5) 0.6432(3) 0.4849(4) 0.049(3) Uani 1 1 d . . . H2PR H -0.1057 0.6817 0.4663 0.059 Uiso 1 1 calc R . . C3PR C -0.1559(5) 0.6114(4) 0.5176(4) 0.058(3) Uani 1 1 d . . . H3P1 H -0.1798 0.6413 0.5434 0.087 Uiso 1 1 calc R . . H3P2 H -0.1340 0.5757 0.5378 0.087 Uiso 1 1 calc R . . H3P3 H -0.1984 0.5972 0.4920 0.087 Uiso 1 1 calc R . . P1 P 0.00112(12) 0.72877(9) 0.54000(11) 0.0467(6) Uani 1 1 d . . . O2P O 0.0223(3) 0.7578(2) 0.4810(3) 0.0595(19) Uani 1 1 d . . . O3P O -0.0200(3) 0.6582(2) 0.5235(3) 0.0485(16) Uani 1 1 d . . . O4P O -0.0743(3) 0.7614(2) 0.5624(3) 0.063(2) Uani 1 1 d . . . O5P O 0.0760(3) 0.7249(3) 0.5759(3) 0.071(2) Uani 1 1 d . . . C1R C 0.0629(4) 0.9094(3) 0.4162(4) 0.040(2) Uani 1 1 d U . . H1R H 0.0527 0.9445 0.4423 0.048 Uiso 1 1 calc R . . C2R C 0.0963(4) 0.8517(3) 0.4480(4) 0.0374(18) Uani 1 1 d U . . H2R H 0.1335 0.8637 0.4789 0.045 Uiso 1 1 calc R . . C3R C 0.0132(4) 0.8244(3) 0.4688(4) 0.0418(18) Uani 1 1 d U . . H3R H -0.0067 0.8476 0.5019 0.050 Uiso 1 1 calc R . . C4R C -0.0455(4) 0.8351(3) 0.4190(4) 0.0434(19) Uani 1 1 d U . . H4R H -0.0420 0.7985 0.3938 0.052 Uiso 1 1 calc R . . C5R C -0.1362(5) 0.8459(4) 0.4348(5) 0.062(3) Uani 1 1 d U . . H5R1 H -0.1695 0.8478 0.4009 0.074 Uiso 1 1 calc R . . H5R2 H -0.1556 0.8099 0.4566 0.074 Uiso 1 1 calc R . . O6R O -0.0142(3) 0.8901(2) 0.3908(3) 0.0476(15) Uani 1 1 d U . . O7R O 0.1365(3) 0.8120(2) 0.4089(3) 0.0515(16) Uani 1 1 d U . . H7R H 0.1689 0.7881 0.4253 0.077 Uiso 1 1 calc R . . O8R O -0.1493(4) 0.9012(3) 0.4655(4) 0.090(3) Uani 1 1 d U . . H8R H -0.1214 0.8999 0.4944 0.135 Uiso 1 1 calc R . . N1B N 0.1179(3) 0.9299(3) 0.3718(3) 0.0428(17) Uani 1 1 d U . . C2B C 0.1287(4) 0.8976(3) 0.3233(4) 0.0398(18) Uani 1 1 d U . . H2B H 0.0900 0.8682 0.3100 0.048 Uiso 1 1 calc R . . N3B N 0.2000(3) 0.9115(2) 0.2961(3) 0.0397(16) Uani 1 1 d U . . C4B C 0.3215(4) 0.9799(3) 0.3332(4) 0.043(2) Uani 1 1 d U . . H4B H 0.3554 0.9752 0.3018 0.052 Uiso 1 1 calc R . . C5B C 0.3486(4) 1.0151(3) 0.3804(4) 0.045(2) Uani 1 1 d U . . C6B C 0.2946(4) 1.0270(3) 0.4246(4) 0.047(2) Uani 1 1 d U . . C7B C 0.2155(4) 1.0007(3) 0.4259(4) 0.0439(19) Uani 1 1 d U . . H7B H 0.1799 1.0077 0.4561 0.053 Uiso 1 1 calc R . . C8B C 0.1906(4) 0.9638(3) 0.3811(4) 0.0424(19) Uani 1 1 d U . . C9B C 0.2419(4) 0.9524(3) 0.3357(4) 0.0385(17) Uani 1 1 d U . . C10B C 0.4382(5) 1.0366(4) 0.3815(5) 0.060(3) Uani 1 1 d U . . H10A H 0.4659 1.0231 0.3478 0.089 Uiso 1 1 calc R . . H10B H 0.4661 1.0184 0.4133 0.089 Uiso 1 1 calc R . . H10C H 0.4402 1.0821 0.3840 0.089 Uiso 1 1 calc R . . C11B C 0.3257(6) 1.0641(4) 0.4748(5) 0.074(3) Uani 1 1 d . . . H11A H 0.2809 1.0689 0.5013 0.111 Uiso 1 1 calc R . . H11B H 0.3446 1.1052 0.4629 0.111 Uiso 1 1 calc R . . H11C H 0.3713 1.0416 0.4920 0.111 Uiso 1 1 calc R . . C1C C 0.2473(4) 0.8609(3) 0.1469(5) 0.045(3) Uani 1 1 d DU . . N2C N 0.2577(5) 0.8502(4) 0.1002(5) 0.075(3) Uani 1 1 d DU . . OW1 O 0.2554(4) 0.7435(3) 0.4613(3) 0.0714(17) Uiso 1 1 d . . . OW2 O 0.1832(6) 0.6289(4) 0.4720(5) 0.124(3) Uiso 1 1 d . . . OW3 O 0.2813(4) 1.2085(3) 0.0745(3) 0.0659(16) Uiso 1 1 d . . . OW4 O -0.1061(5) 0.8843(4) 0.5827(4) 0.102(2) Uiso 1 1 d . . . OW5 O -0.1903(4) 0.7440(3) 0.3300(4) 0.0759(18) Uiso 1 1 d . . . OW6 O -0.0153(6) 1.0381(4) 0.3375(5) 0.129(3) Uiso 1 1 d . . . OW7 O 0.3946(4) 0.6095(4) 0.1412(4) 0.091(2) Uiso 1 1 d . . . OW8 O -0.1029(5) 1.0175(4) 0.5431(5) 0.117(3) Uiso 1 1 d . . . OW9 O 0.1557(6) 1.1773(5) 0.4885(5) 0.135(3) Uiso 1 1 d . . . OW10 O 0.5090(8) 0.9246(6) -0.0424(7) 0.178(5) Uiso 1 1 d . . . OW11 O -0.1785(6) 1.0099(5) 0.3985(5) 0.134(3) Uiso 1 1 d . . . OW12 O 0.2131(9) 0.6219(7) 0.0363(8) 0.204(6) Uiso 1 1 d . . . OW13 O -0.1074(8) 0.7877(7) 0.0747(8) 0.189(5) Uiso 1 1 d . . . OW14 O 0.6067(6) 1.0195(5) 0.4857(6) 0.151(4) Uiso 1 1 d . . . OW15 O 0.2356(8) 0.5065(6) 0.4341(7) 0.171(5) Uiso 1 1 d . . . OW16 O 0.3263(8) 0.7107(6) 0.0869(7) 0.172(5) Uiso 1 1 d . . . OW17 O 0.3846(9) 1.2071(7) 0.5302(8) 0.209(6) Uiso 1 1 d . . . OW18 O 0.5341(9) 1.1459(7) 0.4847(8) 0.196(6) Uiso 1 1 d . . . OW19 O 0.3100(8) 1.2379(6) 0.4375(6) 0.165(4) Uiso 1 1 d . . . OW20 O 0.4711(8) 1.2997(7) 0.5748(8) 0.184(5) Uiso 1 1 d . . . OW21 O -0.2254(17) 0.8620(13) 0.0760(15) 0.188(11) Uiso 0.50 1 d P . . OW22 O -0.035(2) 1.1390(14) 0.5835(16) 0.193(11) Uiso 0.50 1 d P . . OW23 O -0.1100(14) 1.1305(10) 0.5932(11) 0.137(7) Uiso 0.50 1 d P . . OW24 O 0.0237(12) 1.2039(9) 0.5587(11) 0.130(7) Uiso 0.50 1 d 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 Co 0.0281(4) 0.0294(4) 0.0464(9) 0.0007(4) 0.0002(4) -0.0015(4) C1 0.036(3) 0.034(3) 0.071(8) 0.004(4) 0.007(4) -0.001(3) C2 0.029(3) 0.032(3) 0.059(8) -0.009(3) 0.000(3) 0.004(3) C3 0.031(3) 0.039(3) 0.024(6) 0.010(3) -0.004(3) 0.003(2) C4 0.028(3) 0.037(3) 0.052(8) 0.001(3) 0.007(3) 0.005(3) C5 0.027(3) 0.031(3) 0.063(8) 0.002(3) 0.004(3) -0.003(2) C6 0.037(3) 0.032(3) 0.039(7) 0.004(3) 0.005(3) -0.005(3) C7 0.035(3) 0.025(3) 0.065(7) 0.004(3) -0.006(3) -0.005(3) C8 0.041(4) 0.023(3) 0.062(8) 0.007(3) -0.002(3) -0.003(2) C9 0.036(3) 0.031(3) 0.043(7) -0.004(3) 0.001(3) -0.006(3) C10 0.036(3) 0.031(3) 0.052(7) 0.008(3) -0.005(3) 0.005(3) C11 0.029(3) 0.037(3) 0.052(8) 0.000(4) -0.002(3) -0.006(3) C12 0.028(3) 0.039(3) 0.047(7) 0.012(3) -0.002(3) 0.003(3) C13 0.024(3) 0.031(3) 0.071(8) 0.009(3) -0.001(3) -0.002(2) C14 0.032(3) 0.038(3) 0.020(7) -0.001(3) 0.001(3) -0.001(3) C15 0.035(3) 0.034(3) 0.053(7) -0.007(4) -0.001(4) 0.000(3) C16 0.032(3) 0.025(3) 0.054(8) -0.003(3) 0.000(3) -0.006(2) C17 0.037(3) 0.029(3) 0.062(8) 0.008(4) -0.003(3) -0.002(3) C18 0.031(3) 0.033(3) 0.069(8) 0.002(3) -0.001(3) -0.001(3) C19 0.032(3) 0.031(3) 0.075(8) 0.005(3) -0.003(3) 0.006(3) C20 0.032(4) 0.040(4) 0.083(8) 0.005(4) 0.010(4) -0.001(3) N21 0.029(3) 0.026(3) 0.044(6) 0.011(2) -0.001(3) 0.002(2) N22 0.023(3) 0.036(3) 0.044(6) 0.003(3) 0.002(2) -0.004(2) N23 0.026(3) 0.030(3) 0.052(6) 0.002(3) -0.001(3) -0.003(2) N24 0.032(3) 0.039(3) 0.042(6) 0.000(3) 0.007(3) 0.004(2) C25 0.041(4) 0.039(4) 0.053(8) 0.006(3) 0.012(4) 0.002(3) C26 0.025(3) 0.039(4) 0.069(9) -0.001(4) 0.002(3) 0.000(3) C27 0.039(4) 0.051(4) 0.047(8) -0.002(4) 0.010(4) 0.006(4) O28 0.035(3) 0.063(3) 0.127(8) -0.028(4) 0.020(3) -0.013(3) N29 0.050(4) 0.051(4) 0.100(9) -0.006(4) 0.020(4) 0.011(3) C30 0.025(3) 0.049(4) 0.056(8) -0.010(4) 0.005(3) 0.006(3) C31 0.037(4) 0.062(5) 0.062(9) 0.001(5) -0.004(4) -0.004(4) C32 0.034(4) 0.050(5) 0.088(12) -0.001(5) -0.010(4) -0.006(4) O33 0.076(4) 0.070(4) 0.069(7) 0.002(3) -0.012(4) -0.018(3) N34 0.117(7) 0.113(7) 0.079(12) 0.005(6) -0.014(6) -0.071(6) C35 0.035(4) 0.055(4) 0.069(9) 0.011(4) 0.004(4) -0.014(4) C36 0.043(4) 0.039(4) 0.066(9) 0.005(4) 0.004(4) -0.006(3) C37 0.039(4) 0.035(4) 0.077(8) 0.002(4) -0.005(4) -0.009(3) C38 0.061(5) 0.057(5) 0.052(9) 0.006(5) 0.000(4) 0.002(4) O39 0.068(4) 0.073(4) 0.067(7) 0.008(3) 0.021(3) -0.019(3) N40 0.063(4) 0.046(4) 0.093(9) -0.015(4) 0.009(4) -0.005(3) C41 0.037(4) 0.038(4) 0.076(9) 0.011(4) -0.002(4) 0.011(3) C42 0.038(4) 0.063(5) 0.058(9) -0.007(5) 0.001(4) -0.003(4) C43 0.060(5) 0.041(4) 0.058(10) -0.005(4) 0.002(5) 0.002(4) O44 0.058(4) 0.082(4) 0.068(7) -0.022(4) 0.006(3) -0.020(3) N45 0.055(4) 0.077(5) 0.070(8) 0.001(4) 0.015(4) 0.001(4) C46 0.038(4) 0.052(4) 0.090(9) 0.023(4) -0.002(4) 0.010(3) C47 0.065(5) 0.055(5) 0.073(8) 0.010(4) -0.014(5) -0.005(4) C48 0.025(4) 0.046(4) 0.083(9) 0.008(4) 0.002(4) 0.003(3) C49 0.038(4) 0.052(4) 0.073(10) -0.009(4) 0.005(4) 0.002(3) C50 0.032(3) 0.056(4) 0.048(8) -0.003(4) 0.012(4) -0.002(3) O51 0.065(4) 0.054(3) 0.083(7) 0.005(3) -0.017(4) 0.002(3) N52 0.045(3) 0.046(3) 0.077(7) 0.004(3) -0.005(4) 0.001(3) C53 0.032(4) 0.037(4) 0.095(9) 0.004(4) -0.003(4) -0.003(3) C54 0.046(4) 0.043(4) 0.064(9) -0.018(4) 0.005(4) -0.005(3) C55 0.045(4) 0.040(4) 0.033(7) 0.010(4) 0.005(4) 0.005(3) C56 0.050(4) 0.049(4) 0.058(9) -0.008(4) 0.005(4) -0.012(4) C57 0.047(5) 0.041(4) 0.081(10) -0.004(5) 0.003(5) -0.014(4) O58 0.049(3) 0.069(4) 0.079(7) 0.006(3) 0.004(3) -0.010(3) N59 0.052(4) 0.053(4) 0.059(8) -0.002(4) 0.003(3) 0.000(3) C60 0.030(3) 0.031(3) 0.098(10) 0.022(4) 0.008(4) 0.006(3) C61 0.031(4) 0.043(4) 0.065(10) 0.000(4) 0.007(4) 0.002(3) O62 0.063(4) 0.050(3) 0.071(8) 0.000(3) -0.012(4) 0.000(3) N63 0.053(4) 0.037(3) 0.073(8) -0.001(3) -0.005(4) -0.001(3) C1PR 0.067(5) 0.044(4) 0.048(9) 0.004(4) 0.015(4) -0.020(4) C2PR 0.054(5) 0.038(4) 0.055(9) 0.007(4) -0.004(4) -0.006(3) C3PR 0.058(5) 0.058(5) 0.059(9) -0.003(5) 0.005(4) -0.013(4) P1 0.0450(10) 0.0424(10) 0.053(2) 0.0016(10) 0.0050(10) -0.0053(9) O2P 0.078(4) 0.034(3) 0.067(6) 0.009(3) 0.023(3) -0.005(3) O3P 0.048(3) 0.044(3) 0.053(6) 0.012(3) -0.003(3) -0.006(2) O4P 0.053(3) 0.052(3) 0.083(7) 0.002(3) 0.025(3) -0.002(3) O5P 0.052(3) 0.083(4) 0.079(7) 0.007(4) -0.004(3) -0.013(3) C1R 0.032(3) 0.047(4) 0.042(8) 0.005(3) 0.007(3) 0.000(3) C2R 0.048(4) 0.039(4) 0.025(7) 0.003(3) 0.002(3) -0.006(3) C3R 0.047(4) 0.043(4) 0.035(6) -0.009(3) 0.006(3) -0.006(3) C4R 0.049(4) 0.049(4) 0.032(7) -0.001(3) 0.008(3) -0.009(3) C5R 0.039(3) 0.055(5) 0.092(10) -0.002(4) 0.001(4) -0.014(3) O6R 0.039(3) 0.062(3) 0.042(5) 0.011(3) -0.001(2) -0.009(2) O7R 0.049(3) 0.049(3) 0.057(6) 0.004(3) 0.013(3) 0.015(2) O8R 0.083(4) 0.102(5) 0.085(8) -0.015(4) 0.015(4) 0.022(4) N1B 0.039(3) 0.036(3) 0.053(6) -0.001(3) 0.007(3) -0.002(2) C2B 0.039(3) 0.038(4) 0.043(7) 0.007(3) 0.000(3) 0.000(3) N3B 0.030(3) 0.031(3) 0.057(6) -0.005(3) 0.003(2) -0.001(2) C4B 0.037(3) 0.027(3) 0.066(7) 0.003(3) 0.009(3) 0.001(3) C5B 0.039(3) 0.043(4) 0.054(7) 0.006(4) -0.004(3) 0.001(3) C6B 0.048(4) 0.035(4) 0.057(7) 0.000(4) -0.002(4) 0.003(3) C7B 0.049(3) 0.040(4) 0.042(6) 0.003(3) 0.001(4) 0.000(3) C8B 0.038(3) 0.034(4) 0.055(6) -0.005(3) 0.003(3) 0.002(3) C9B 0.034(3) 0.034(3) 0.048(6) -0.002(3) -0.004(3) -0.002(3) C10B 0.044(4) 0.050(4) 0.085(10) -0.004(4) -0.009(4) -0.009(3) C11B 0.071(6) 0.067(6) 0.084(12) -0.014(5) -0.005(6) -0.012(5) C1C 0.036(4) 0.034(3) 0.064(10) -0.010(4) 0.011(4) -0.006(3) N2C 0.069(5) 0.079(5) 0.077(10) -0.012(5) 0.006(5) 0.004(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 Co C1C 1.813(11) . ? Co N21 1.888(5) . ? Co N24 1.890(5) . ? Co N22 1.911(5) . ? Co N23 1.912(5) . ? Co N3B 1.984(7) . ? C1 N21 1.492(9) . ? C1 C20 1.495(13) . ? C1 C19 1.519(11) . ? C1 C2 1.599(9) . ? C2 C26 1.505(12) . ? C2 C25 1.537(12) . ? C2 C3 1.554(9) . ? C3 C4 1.549(9) . ? C3 C30 1.555(12) . ? C3 H3 0.9800 . ? C4 N21 1.272(8) . ? C4 C5 1.434(10) . ? C5 C6 1.370(10) . ? C5 C35 1.518(9) . ? C6 N22 1.410(8) . ? C6 C7 1.545(9) . ? C7 C36 1.537(9) . ? C7 C37 1.543(13) . ? C7 C8 1.544(10) . ? C8 C9 1.510(9) . ? C8 C41 1.555(13) . ? C8 H8 0.9800 . ? C9 N22 1.336(8) . ? C9 C10 1.374(9) . ? C10 C11 1.397(9) . ? C10 H10 0.9300 . ? C11 N23 1.331(9) . ? C11 C12 1.504(9) . ? C12 C46 1.505(10) . ? C12 C47 1.547(14) . ? C12 C13 1.562(9) . ? C13 C48 1.528(12) . ? C13 C14 1.541(9) . ? C13 H13 0.9800 . ? C14 C15 1.337(9) . ? C14 N23 1.418(8) . ? C15 C16 1.460(9) . ? C15 C53 1.526(9) . ? C16 N24 1.309(8) . ? C16 C17 1.518(9) . ? C17 C54 1.496(12) . ? C17 C55 1.554(11) . ? C17 C18 1.586(10) . ? C18 C19 1.525(10) . ? C18 C60 1.541(9) . ? C18 H18 0.9800 . ? C19 N24 1.478(8) . ? C19 H19 0.9800 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 C27 1.537(9) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 O28 1.240(9) . ? C27 N29 1.322(9) . ? N29 H29A 0.8600 . ? N29 H29B 0.8600 . ? C30 C31 1.526(9) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 C32 1.505(13) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 O33 1.252(7) . ? C32 N34 1.327(8) . ? N34 H34A 0.8600 . ? N34 H34B 0.8600 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 C38 1.543(12) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 O39 1.219(10) . ? C38 N40 1.321(7) . ? N40 H40A 0.8600 . ? N40 H40B 0.8600 . ? C41 C42 1.490(11) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 C43 1.499(14) . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C43 O44 1.230(10) . ? C43 N45 1.340(12) . ? N45 H45A 0.8600 . ? N45 H45B 0.8600 . ? C46 H46A 0.9600 . ? C46 H46B 0.9600 . ? C46 H46C 0.9600 . ? C47 H47A 0.9600 . ? C47 H47B 0.9600 . ? C47 H47C 0.9600 . ? C48 C49 1.544(9) . ? C48 H48A 0.9700 . ? C48 H48B 0.9700 . ? C49 C50 1.451(13) . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? C50 O51 1.252(11) . ? C50 N52 1.340(9) . ? N52 H52A 0.8600 . ? N52 H52B 0.8600 . ? C53 H53A 0.9600 . ? C53 H53B 0.9600 . ? C53 H53C 0.9600 . ? C54 H54A 0.9600 . ? C54 H54B 0.9600 . ? C54 H54C 0.9600 . ? C55 C56 1.504(13) . ? C55 H55A 0.9700 . ? C55 H55B 0.9700 . ? C56 C57 1.491(11) . ? C56 H56A 0.9700 . ? C56 H56B 0.9700 . ? C57 O58 1.241(10) . ? C57 N59 1.317(8) . ? N59 C1PR 1.463(10) . ? N59 H59 0.8600 . ? C60 C61 1.494(11) . ? C60 H60A 0.9700 . ? C60 H60B 0.9700 . ? C61 O62 1.226(7) . ? C61 N63 1.341(10) . ? N63 H63A 0.8600 . ? N63 H63B 0.8600 . ? C1PR C2PR 1.495(13) . ? C1PR H1P1 0.9700 . ? C1PR H1P2 0.9700 . ? C2PR O3P 1.427(10) . ? C2PR C3PR 1.524(12) . ? C2PR H2PR 0.9800 . ? C3PR H3P1 0.9600 . ? C3PR H3P2 0.9600 . ? C3PR H3P3 0.9600 . ? P1 O5P 1.473(7) . ? P1 O4P 1.485(6) . ? P1 O2P 1.572(7) . ? P1 O3P 1.573(5) . ? O2P C3R 1.440(8) . ? C1R O6R 1.430(9) . ? C1R N1B 1.444(11) . ? C1R C2R 1.529(10) . ? C1R H1R 0.9800 . ? C2R O7R 1.407(10) . ? C2R C3R 1.527(10) . ? C2R H2R 0.9800 . ? C3R C4R 1.530(12) . ? C3R H3R 0.9800 . ? C4R O6R 1.429(9) . ? C4R C5R 1.510(10) . ? C4R H4R 0.9800 . ? C5R O8R 1.392(11) . ? C5R H5R1 0.9700 . ? C5R H5R2 0.9700 . ? O7R H7R 0.8200 . ? O8R H8R 0.8200 . ? N1B C2B 1.353(11) . ? N1B C8B 1.380(9) . ? C2B N3B 1.342(9) . ? C2B H2B 0.9300 . ? N3B C9B 1.442(10) . ? C4B C9B 1.395(9) . ? C4B C5B 1.416(12) . ? C4B H4B 0.9300 . ? C5B C6B 1.385(12) . ? C5B C10B 1.500(10) . ? C6B C7B 1.377(10) . ? C6B C11B 1.513(14) . ? C7B C8B 1.380(12) . ? C7B H7B 0.9300 . ? C8B C9B 1.379(12) . ? C10B H10A 0.9600 . ? C10B H10B 0.9600 . ? C10B H10C 0.9600 . ? C11B H11A 0.9600 . ? C11B H11B 0.9600 . ? C11B H11C 0.9600 . ? C1C N2C 1.150(8) . ? OW22 OW23 1.23(3) . ? OW22 OW24 1.76(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 C1C Co N21 90.4(3) . . ? C1C Co N24 88.4(3) . . ? N21 Co N24 82.9(2) . . ? C1C Co N22 88.4(3) . . ? N21 Co N22 90.4(2) . . ? N24 Co N22 172.5(2) . . ? C1C Co N23 91.3(3) . . ? N21 Co N23 173.4(2) . . ? N24 Co N23 90.8(2) . . ? N22 Co N23 96.0(2) . . ? C1C Co N3B 175.3(3) . . ? N21 Co N3B 92.7(3) . . ? N24 Co N3B 95.5(3) . . ? N22 Co N3B 88.0(3) . . ? N23 Co N3B 86.0(3) . . ? N21 C1 C20 110.3(6) . . ? N21 C1 C19 103.6(6) . . ? C20 C1 C19 109.4(7) . . ? N21 C1 C2 100.4(6) . . ? C20 C1 C2 113.6(7) . . ? C19 C1 C2 118.4(7) . . ? C26 C2 C25 110.3(6) . . ? C26 C2 C3 108.6(7) . . ? C25 C2 C3 112.4(6) . . ? C26 C2 C1 109.8(6) . . ? C25 C2 C1 113.5(7) . . ? C3 C2 C1 101.9(5) . . ? C4 C3 C2 101.5(5) . . ? C4 C3 C30 109.4(6) . . ? C2 C3 C30 119.5(7) . . ? C4 C3 H3 108.6 . . ? C2 C3 H3 108.6 . . ? C30 C3 H3 108.6 . . ? N21 C4 C5 127.8(6) . . ? N21 C4 C3 110.1(6) . . ? C5 C4 C3 122.1(5) . . ? C6 C5 C4 119.9(5) . . ? C6 C5 C35 122.2(6) . . ? C4 C5 C35 117.9(6) . . ? C5 C6 N22 123.6(6) . . ? C5 C6 C7 129.8(6) . . ? N22 C6 C7 106.6(5) . . ? C36 C7 C37 110.9(7) . . ? C36 C7 C8 111.4(6) . . ? C37 C7 C8 106.5(6) . . ? C36 C7 C6 117.6(6) . . ? C37 C7 C6 109.3(6) . . ? C8 C7 C6 100.2(6) . . ? C9 C8 C7 100.7(5) . . ? C9 C8 C41 109.3(7) . . ? C7 C8 C41 114.0(6) . . ? C9 C8 H8 110.8 . . ? C7 C8 H8 110.8 . . ? C41 C8 H8 110.8 . . ? N22 C9 C10 127.0(6) . . ? N22 C9 C8 109.4(5) . . ? C10 C9 C8 123.5(6) . . ? C9 C10 C11 124.3(6) . . ? C9 C10 H10 117.9 . . ? C11 C10 H10 117.9 . . ? N23 C11 C10 125.2(6) . . ? N23 C11 C12 111.5(5) . . ? C10 C11 C12 123.0(6) . . ? C11 C12 C46 115.1(7) . . ? C11 C12 C47 106.4(7) . . ? C46 C12 C47 109.0(7) . . ? C11 C12 C13 102.2(6) . . ? C46 C12 C13 116.2(6) . . ? C47 C12 C13 107.2(6) . . ? C48 C13 C14 106.2(6) . . ? C48 C13 C12 116.4(6) . . ? C14 C13 C12 101.1(5) . . ? C48 C13 H13 110.9 . . ? C14 C13 H13 110.9 . . ? C12 C13 H13 110.9 . . ? C15 C14 N23 127.2(6) . . ? C15 C14 C13 124.2(6) . . ? N23 C14 C13 108.1(5) . . ? C14 C15 C16 121.8(6) . . ? C14 C15 C53 118.0(6) . . ? C16 C15 C53 120.1(5) . . ? N24 C16 C15 121.8(5) . . ? N24 C16 C17 111.5(5) . . ? C15 C16 C17 126.6(5) . . ? C54 C17 C16 110.9(7) . . ? C54 C17 C55 109.2(6) . . ? C16 C17 C55 114.6(6) . . ? C54 C17 C18 113.2(6) . . ? C16 C17 C18 100.3(5) . . ? C55 C17 C18 108.6(7) . . ? C19 C18 C60 114.0(6) . . ? C19 C18 C17 100.6(6) . . ? C60 C18 C17 114.8(6) . . ? C19 C18 H18 109.0 . . ? C60 C18 H18 109.0 . . ? C17 C18 H18 109.0 . . ? N24 C19 C1 106.8(5) . . ? N24 C19 C18 102.6(5) . . ? C1 C19 C18 122.1(8) . . ? N24 C19 H19 108.2 . . ? C1 C19 H19 108.2 . . ? C18 C19 H19 108.2 . . ? C1 C20 H20A 109.5 . . ? C1 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C1 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C4 N21 C1 115.4(5) . . ? C4 N21 Co 128.2(5) . . ? C1 N21 Co 116.2(4) . . ? C9 N22 C6 111.1(5) . . ? C9 N22 Co 122.3(4) . . ? C6 N22 Co 126.2(4) . . ? C11 N23 C14 110.7(5) . . ? C11 N23 Co 123.9(4) . . ? C14 N23 Co 125.3(4) . . ? C16 N24 C19 110.8(5) . . ? C16 N24 Co 132.8(5) . . ? C19 N24 Co 115.2(4) . . ? C2 C25 H25A 109.5 . . ? C2 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C2 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C2 C26 C27 113.4(6) . . ? C2 C26 H26A 108.9 . . ? C27 C26 H26A 108.9 . . ? C2 C26 H26B 108.9 . . ? C27 C26 H26B 108.9 . . ? H26A C26 H26B 107.7 . . ? O28 C27 N29 122.0(7) . . ? O28 C27 C26 122.0(6) . . ? N29 C27 C26 116.0(7) . . ? C27 N29 H29A 120.0 . . ? C27 N29 H29B 120.0 . . ? H29A N29 H29B 120.0 . . ? C31 C30 C3 113.3(6) . . ? C31 C30 H30A 108.9 . . ? C3 C30 H30A 108.9 . . ? C31 C30 H30B 108.9 . . ? C3 C30 H30B 108.9 . . ? H30A C30 H30B 107.7 . . ? C32 C31 C30 107.0(7) . . ? C32 C31 H31A 110.3 . . ? C30 C31 H31A 110.3 . . ? C32 C31 H31B 110.3 . . ? C30 C31 H31B 110.3 . . ? H31A C31 H31B 108.6 . . ? O33 C32 N34 123.8(9) . . ? O33 C32 C31 120.7(10) . . ? N34 C32 C31 115.4(8) . . ? C32 N34 H34A 120.0 . . ? C32 N34 H34B 120.0 . . ? H34A N34 H34B 120.0 . . ? C5 C35 H35A 109.5 . . ? C5 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C5 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C7 C36 H36A 109.5 . . ? C7 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C7 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C7 C37 C38 115.3(7) . . ? C7 C37 H37A 108.5 . . ? C38 C37 H37A 108.5 . . ? C7 C37 H37B 108.5 . . ? C38 C37 H37B 108.5 . . ? H37A C37 H37B 107.5 . . ? O39 C38 N40 122.8(8) . . ? O39 C38 C37 120.5(7) . . ? N40 C38 C37 116.7(7) . . ? C38 N40 H40A 120.0 . . ? C38 N40 H40B 120.0 . . ? H40A N40 H40B 120.0 . . ? C42 C41 C8 113.6(6) . . ? C42 C41 H41A 108.9 . . ? C8 C41 H41A 108.9 . . ? C42 C41 H41B 108.9 . . ? C8 C41 H41B 108.9 . . ? H41A C41 H41B 107.7 . . ? C41 C42 C43 111.3(7) . . ? C41 C42 H42A 109.4 . . ? C43 C42 H42A 109.4 . . ? C41 C42 H42B 109.4 . . ? C43 C42 H42B 109.4 . . ? H42A C42 H42B 108.0 . . ? O44 C43 N45 120.1(10) . . ? O44 C43 C42 123.5(8) . . ? N45 C43 C42 116.5(8) . . ? C43 N45 H45A 120.0 . . ? C43 N45 H45B 120.0 . . ? H45A N45 H45B 120.0 . . ? C12 C46 H46A 109.5 . . ? C12 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C12 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C12 C47 H47A 109.5 . . ? C12 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C12 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C13 C48 C49 116.8(7) . . ? C13 C48 H48A 108.1 . . ? C49 C48 H48A 108.1 . . ? C13 C48 H48B 108.1 . . ? C49 C48 H48B 108.1 . . ? H48A C48 H48B 107.3 . . ? C50 C49 C48 113.6(7) . . ? C50 C49 H49A 108.8 . . ? C48 C49 H49A 108.8 . . ? C50 C49 H49B 108.8 . . ? C48 C49 H49B 108.8 . . ? H49A C49 H49B 107.7 . . ? O51 C50 N52 121.1(8) . . ? O51 C50 C49 121.1(7) . . ? N52 C50 C49 117.7(9) . . ? C50 N52 H52A 120.0 . . ? C50 N52 H52B 120.0 . . ? H52A N52 H52B 120.0 . . ? C15 C53 H53A 109.5 . . ? C15 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C15 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C17 C54 H54A 109.5 . . ? C17 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C17 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C56 C55 C17 117.7(6) . . ? C56 C55 H55A 107.9 . . ? C17 C55 H55A 107.9 . . ? C56 C55 H55B 107.9 . . ? C17 C55 H55B 107.9 . . ? H55A C55 H55B 107.2 . . ? C57 C56 C55 112.4(7) . . ? C57 C56 H56A 109.1 . . ? C55 C56 H56A 109.1 . . ? C57 C56 H56B 109.1 . . ? C55 C56 H56B 109.1 . . ? H56A C56 H56B 107.9 . . ? O58 C57 N59 120.6(7) . . ? O58 C57 C56 121.2(9) . . ? N59 C57 C56 118.0(8) . . ? C57 N59 C1PR 124.1(7) . . ? C57 N59 H59 118.0 . . ? C1PR N59 H59 118.0 . . ? C61 C60 C18 114.4(6) . . ? C61 C60 H60A 108.7 . . ? C18 C60 H60A 108.7 . . ? C61 C60 H60B 108.7 . . ? C18 C60 H60B 108.7 . . ? H60A C60 H60B 107.6 . . ? O62 C61 N63 123.0(8) . . ? O62 C61 C60 120.5(7) . . ? N63 C61 C60 116.5(9) . . ? C61 N63 H63A 120.0 . . ? C61 N63 H63B 120.0 . . ? H63A N63 H63B 120.0 . . ? N59 C1PR C2PR 112.8(6) . . ? N59 C1PR H1P1 109.0 . . ? C2PR C1PR H1P1 109.0 . . ? N59 C1PR H1P2 109.0 . . ? C2PR C1PR H1P2 109.0 . . ? H1P1 C1PR H1P2 107.8 . . ? O3P C2PR C1PR 106.4(7) . . ? O3P C2PR C3PR 107.8(8) . . ? C1PR C2PR C3PR 110.7(6) . . ? O3P C2PR H2PR 110.6 . . ? C1PR C2PR H2PR 110.6 . . ? C3PR C2PR H2PR 110.6 . . ? C2PR C3PR H3P1 109.5 . . ? C2PR C3PR H3P2 109.5 . . ? H3P1 C3PR H3P2 109.5 . . ? C2PR C3PR H3P3 109.5 . . ? H3P1 C3PR H3P3 109.5 . . ? H3P2 C3PR H3P3 109.5 . . ? O5P P1 O4P 118.2(4) . . ? O5P P1 O2P 111.7(4) . . ? O4P P1 O2P 108.6(4) . . ? O5P P1 O3P 105.4(3) . . ? O4P P1 O3P 110.7(3) . . ? O2P P1 O3P 100.9(3) . . ? C3R O2P P1 122.5(5) . . ? C2PR O3P P1 121.8(5) . . ? O6R C1R N1B 107.1(7) . . ? O6R C1R C2R 106.6(6) . . ? N1B C1R C2R 113.0(6) . . ? O6R C1R H1R 110.0 . . ? N1B C1R H1R 110.0 . . ? C2R C1R H1R 110.0 . . ? O7R C2R C3R 112.9(6) . . ? O7R C2R C1R 107.5(7) . . ? C3R C2R C1R 99.1(5) . . ? O7R C2R H2R 112.2 . . ? C3R C2R H2R 112.2 . . ? C1R C2R H2R 112.2 . . ? O2P C3R C2R 110.1(5) . . ? O2P C3R C4R 111.2(6) . . ? C2R C3R C4R 102.9(7) . . ? O2P C3R H3R 110.8 . . ? C2R C3R H3R 110.8 . . ? C4R C3R H3R 110.8 . . ? O6R C4R C5R 109.3(6) . . ? O6R C4R C3R 105.8(6) . . ? C5R C4R C3R 114.4(8) . . ? O6R C4R H4R 109.1 . . ? C5R C4R H4R 109.1 . . ? C3R C4R H4R 109.1 . . ? O8R C5R C4R 113.6(7) . . ? O8R C5R H5R1 108.8 . . ? C4R C5R H5R1 108.8 . . ? O8R C5R H5R2 108.8 . . ? C4R C5R H5R2 108.8 . . ? H5R1 C5R H5R2 107.7 . . ? C4R O6R C1R 109.3(6) . . ? C2R O7R H7R 109.5 . . ? C5R O8R H8R 109.5 . . ? C2B N1B C8B 107.0(6) . . ? C2B N1B C1R 123.7(6) . . ? C8B N1B C1R 123.1(8) . . ? N3B C2B N1B 114.2(7) . . ? N3B C2B H2B 122.9 . . ? N1B C2B H2B 122.9 . . ? C2B N3B C9B 102.0(7) . . ? C2B N3B Co 124.1(5) . . ? C9B N3B Co 133.9(5) . . ? C9B C4B C5B 117.5(8) . . ? C9B C4B H4B 121.3 . . ? C5B C4B H4B 121.3 . . ? C6B C5B C4B 120.8(7) . . ? C6B C5B C10B 121.6(8) . . ? C4B C5B C10B 117.6(8) . . ? C7B C6B C5B 120.8(8) . . ? C7B C6B C11B 119.3(8) . . ? C5B C6B C11B 119.6(7) . . ? C6B C7B C8B 118.2(8) . . ? C6B C7B H7B 120.9 . . ? C8B C7B H7B 120.9 . . ? C9B C8B N1B 106.3(7) . . ? C9B C8B C7B 122.4(7) . . ? N1B C8B C7B 131.2(8) . . ? C8B C9B C4B 120.0(7) . . ? C8B C9B N3B 110.1(6) . . ? C4B C9B N3B 129.9(8) . . ? C5B C10B H10A 109.5 . . ? C5B C10B H10B 109.5 . . ? H10A C10B H10B 109.5 . . ? C5B C10B H10C 109.5 . . ? H10A C10B H10C 109.5 . . ? H10B C10B H10C 109.5 . . ? C6B C11B H11A 109.5 . . ? C6B C11B H11B 109.5 . . ? H11A C11B H11B 109.5 . . ? C6B C11B H11C 109.5 . . ? H11A C11B H11C 109.5 . . ? H11B C11B H11C 109.5 . . ? N2C C1C Co 176.3(8) . . ? OW23 OW22 OW24 134(3) . . ? 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 N21 C1 C2 C26 -85.6(7) . . . . ? C20 C1 C2 C26 156.7(6) . . . . ? C19 C1 C2 C26 26.3(10) . . . . ? N21 C1 C2 C25 150.4(6) . . . . ? C20 C1 C2 C25 32.7(8) . . . . ? C19 C1 C2 C25 -97.7(9) . . . . ? N21 C1 C2 C3 29.4(8) . . . . ? C20 C1 C2 C3 -88.4(7) . . . . ? C19 C1 C2 C3 141.2(8) . . . . ? C26 C2 C3 C4 85.0(7) . . . . ? C25 C2 C3 C4 -152.7(7) . . . . ? C1 C2 C3 C4 -30.9(8) . . . . ? C26 C2 C3 C30 -154.7(6) . . . . ? C25 C2 C3 C30 -32.4(9) . . . . ? C1 C2 C3 C30 89.4(7) . . . . ? C2 C3 C4 N21 22.4(9) . . . . ? C30 C3 C4 N21 -104.7(7) . . . . ? C2 C3 C4 C5 -159.9(8) . . . . ? C30 C3 C4 C5 72.9(10) . . . . ? N21 C4 C5 C6 8.7(14) . . . . ? C3 C4 C5 C6 -168.5(8) . . . . ? N21 C4 C5 C35 -173.5(8) . . . . ? C3 C4 C5 C35 9.3(12) . . . . ? C4 C5 C6 N22 -3.4(13) . . . . ? C35 C5 C6 N22 178.9(8) . . . . ? C4 C5 C6 C7 178.5(9) . . . . ? C35 C5 C6 C7 0.8(14) . . . . ? C5 C6 C7 C36 -33.9(13) . . . . ? N22 C6 C7 C36 147.7(7) . . . . ? C5 C6 C7 C37 93.6(9) . . . . ? N22 C6 C7 C37 -84.8(7) . . . . ? C5 C6 C7 C8 -154.8(9) . . . . ? N22 C6 C7 C8 26.8(8) . . . . ? C36 C7 C8 C9 -158.0(7) . . . . ? C37 C7 C8 C9 81.0(7) . . . . ? C6 C7 C8 C9 -32.8(8) . . . . ? C36 C7 C8 C41 -41.0(9) . . . . ? C37 C7 C8 C41 -162.0(5) . . . . ? C6 C7 C8 C41 84.2(7) . . . . ? C7 C8 C9 N22 30.5(9) . . . . ? C41 C8 C9 N22 -89.8(7) . . . . ? C7 C8 C9 C10 -146.1(8) . . . . ? C41 C8 C9 C10 93.6(9) . . . . ? N22 C9 C10 C11 -0.2(15) . . . . ? C8 C9 C10 C11 175.7(9) . . . . ? C9 C10 C11 N23 8.1(15) . . . . ? C9 C10 C11 C12 -166.0(9) . . . . ? N23 C11 C12 C46 148.5(8) . . . . ? C10 C11 C12 C46 -36.6(12) . . . . ? N23 C11 C12 C47 -90.5(8) . . . . ? C10 C11 C12 C47 84.3(9) . . . . ? N23 C11 C12 C13 21.7(9) . . . . ? C10 C11 C12 C13 -163.5(8) . . . . ? C11 C12 C13 C48 90.4(7) . . . . ? C46 C12 C13 C48 -35.8(10) . . . . ? C47 C12 C13 C48 -157.9(6) . . . . ? C11 C12 C13 C14 -24.1(8) . . . . ? C46 C12 C13 C14 -150.2(7) . . . . ? C47 C12 C13 C14 87.6(7) . . . . ? C48 C13 C14 C15 70.9(10) . . . . ? C12 C13 C14 C15 -167.3(8) . . . . ? C48 C13 C14 N23 -101.2(7) . . . . ? C12 C13 C14 N23 20.7(8) . . . . ? N23 C14 C15 C16 0.7(14) . . . . ? C13 C14 C15 C16 -169.9(8) . . . . ? N23 C14 C15 C53 -175.8(8) . . . . ? C13 C14 C15 C53 13.7(13) . . . . ? C14 C15 C16 N24 2.0(14) . . . . ? C53 C15 C16 N24 178.4(8) . . . . ? C14 C15 C16 C17 -175.8(9) . . . . ? C53 C15 C16 C17 0.6(14) . . . . ? N24 C16 C17 C54 -102.6(8) . . . . ? C15 C16 C17 C54 75.4(10) . . . . ? N24 C16 C17 C55 133.3(8) . . . . ? C15 C16 C17 C55 -48.7(12) . . . . ? N24 C16 C17 C18 17.2(9) . . . . ? C15 C16 C17 C18 -164.8(9) . . . . ? C54 C17 C18 C19 85.7(7) . . . . ? C16 C17 C18 C19 -32.4(8) . . . . ? C55 C17 C18 C19 -152.9(6) . . . . ? C54 C17 C18 C60 -37.1(10) . . . . ? C16 C17 C18 C60 -155.3(7) . . . . ? C55 C17 C18 C60 84.2(9) . . . . ? N21 C1 C19 N24 -40.3(9) . . . . ? C20 C1 C19 N24 77.4(8) . . . . ? C2 C1 C19 N24 -150.3(7) . . . . ? N21 C1 C19 C18 -157.4(6) . . . . ? C20 C1 C19 C18 -39.8(8) . . . . ? C2 C1 C19 C18 92.5(10) . . . . ? C60 C18 C19 N24 160.0(7) . . . . ? C17 C18 C19 N24 36.6(8) . . . . ? C60 C18 C19 C1 -80.8(10) . . . . ? C17 C18 C19 C1 155.8(7) . . . . ? C5 C4 N21 C1 179.8(9) . . . . ? C3 C4 N21 C1 -2.7(10) . . . . ? C5 C4 N21 Co 5.5(13) . . . . ? C3 C4 N21 Co -177.1(5) . . . . ? C20 C1 N21 C4 102.6(8) . . . . ? C19 C1 N21 C4 -140.4(7) . . . . ? C2 C1 N21 C4 -17.6(9) . . . . ? C20 C1 N21 Co -82.4(7) . . . . ? C19 C1 N21 Co 34.6(8) . . . . ? C2 C1 N21 Co 157.5(5) . . . . ? C1C Co N21 C4 71.6(8) . . . . ? N24 Co N21 C4 159.9(8) . . . . ? N22 Co N21 C4 -16.8(8) . . . . ? N23 Co N21 C4 177(2) . . . . ? N3B Co N21 C4 -104.9(7) . . . . ? C1C Co N21 C1 -102.7(6) . . . . ? N24 Co N21 C1 -14.4(6) . . . . ? N22 Co N21 C1 168.8(6) . . . . ? N23 Co N21 C1 2(3) . . . . ? N3B Co N21 C1 80.8(6) . . . . ? C10 C9 N22 C6 162.4(9) . . . . ? C8 C9 N22 C6 -14.0(9) . . . . ? C10 C9 N22 Co -10.6(12) . . . . ? C8 C9 N22 Co 173.0(6) . . . . ? C5 C6 N22 C9 172.5(8) . . . . ? C7 C6 N22 C9 -9.0(9) . . . . ? C5 C6 N22 Co -14.8(11) . . . . ? C7 C6 N22 Co 163.7(6) . . . . ? C1C Co N22 C9 102.5(6) . . . . ? N21 Co N22 C9 -167.1(6) . . . . ? N24 Co N22 C9 168(2) . . . . ? N23 Co N22 C9 11.4(7) . . . . ? N3B Co N22 C9 -74.4(6) . . . . ? C1C Co N22 C6 -69.4(7) . . . . ? N21 Co N22 C6 21.0(7) . . . . ? N24 Co N22 C6 -4(3) . . . . ? N23 Co N22 C6 -160.6(7) . . . . ? N3B Co N22 C6 113.7(7) . . . . ? C10 C11 N23 C14 176.4(8) . . . . ? C12 C11 N23 C14 -8.9(10) . . . . ? C10 C11 N23 Co -3.5(12) . . . . ? C12 C11 N23 Co 171.2(6) . . . . ? C15 C14 N23 C11 179.9(9) . . . . ? C13 C14 N23 C11 -8.3(9) . . . . ? C15 C14 N23 Co -0.2(12) . . . . ? C13 C14 N23 Co 171.5(6) . . . . ? C1C Co N23 C11 -93.5(7) . . . . ? N21 Co N23 C11 161(2) . . . . ? N24 Co N23 C11 178.1(7) . . . . ? N22 Co N23 C11 -4.9(7) . . . . ? N3B Co N23 C11 82.7(7) . . . . ? C1C Co N23 C14 86.7(6) . . . . ? N21 Co N23 C14 -18(3) . . . . ? N24 Co N23 C14 -1.7(7) . . . . ? N22 Co N23 C14 175.3(6) . . . . ? N3B Co N23 C14 -97.2(6) . . . . ? C15 C16 N24 C19 -171.6(8) . . . . ? C17 C16 N24 C19 6.5(10) . . . . ? C15 C16 N24 Co -5.5(13) . . . . ? C17 C16 N24 Co 172.7(6) . . . . ? C1 C19 N24 C16 -157.9(8) . . . . ? C18 C19 N24 C16 -28.5(9) . . . . ? C1 C19 N24 Co 33.2(9) . . . . ? C18 C19 N24 Co 162.7(6) . . . . ? C1C Co N24 C16 -86.6(8) . . . . ? N21 Co N24 C16 -177.2(8) . . . . ? N22 Co N24 C16 -152(2) . . . . ? N23 Co N24 C16 4.7(8) . . . . ? N3B Co N24 C16 90.8(8) . . . . ? C1C Co N24 C19 79.1(6) . . . . ? N21 Co N24 C19 -11.5(6) . . . . ? N22 Co N24 C19 14(3) . . . . ? N23 Co N24 C19 170.4(6) . . . . ? N3B Co N24 C19 -103.5(6) . . . . ? C25 C2 C26 C27 -51.3(8) . . . . ? C3 C2 C26 C27 72.3(7) . . . . ? C1 C2 C26 C27 -177.1(6) . . . . ? C2 C26 C27 O28 -61.2(11) . . . . ? C2 C26 C27 N29 116.6(9) . . . . ? C4 C3 C30 C31 -152.2(7) . . . . ? C2 C3 C30 C31 91.6(8) . . . . ? C3 C30 C31 C32 166.3(7) . . . . ? C30 C31 C32 O33 -94.8(9) . . . . ? C30 C31 C32 N34 83.3(10) . . . . ? C36 C7 C37 C38 65.5(7) . . . . ? C8 C7 C37 C38 -173.2(6) . . . . ? C6 C7 C37 C38 -65.7(7) . . . . ? C7 C37 C38 O39 -85.9(11) . . . . ? C7 C37 C38 N40 92.2(9) . . . . ? C9 C8 C41 C42 -55.3(8) . . . . ? C7 C8 C41 C42 -167.1(6) . . . . ? C8 C41 C42 C43 175.5(6) . . . . ? C41 C42 C43 O44 21.1(12) . . . . ? C41 C42 C43 N45 -159.7(7) . . . . ? C14 C13 C48 C49 -169.5(6) . . . . ? C12 C13 C48 C49 78.9(8) . . . . ? C13 C48 C49 C50 42.9(10) . . . . ? C48 C49 C50 O51 -111.7(9) . . . . ? C48 C49 C50 N52 69.0(11) . . . . ? C54 C17 C55 C56 -173.0(7) . . . . ? C16 C17 C55 C56 -47.9(10) . . . . ? C18 C17 C55 C56 63.2(8) . . . . ? C17 C55 C56 C57 162.6(7) . . . . ? C55 C56 C57 O58 -63.3(11) . . . . ? C55 C56 C57 N59 112.0(10) . . . . ? O58 C57 N59 C1PR -6.6(14) . . . . ? C56 C57 N59 C1PR 178.1(7) . . . . ? C19 C18 C60 C61 174.9(8) . . . . ? C17 C18 C60 C61 -69.8(11) . . . . ? C18 C60 C61 O62 -43.3(12) . . . . ? C18 C60 C61 N63 140.0(8) . . . . ? C57 N59 C1PR C2PR -88.9(11) . . . . ? N59 C1PR C2PR O3P -62.8(10) . . . . ? N59 C1PR C2PR C3PR -179.6(8) . . . . ? O5P P1 O2P C3R -94.1(6) . . . . ? O4P P1 O2P C3R 38.0(7) . . . . ? O3P P1 O2P C3R 154.3(5) . . . . ? C1PR C2PR O3P P1 130.7(6) . . . . ? C3PR C2PR O3P P1 -110.5(6) . . . . ? O5P P1 O3P C2PR -174.9(7) . . . . ? O4P P1 O3P C2PR 56.2(8) . . . . ? O2P P1 O3P C2PR -58.6(7) . . . . ? O6R C1R C2R O7R 80.9(7) . . . . ? N1B C1R C2R O7R -36.5(9) . . . . ? O6R C1R C2R C3R -36.7(8) . . . . ? N1B C1R C2R C3R -154.1(7) . . . . ? P1 O2P C3R C2R 123.7(7) . . . . ? P1 O2P C3R C4R -123.0(7) . . . . ? O7R C2R C3R O2P 43.9(10) . . . . ? C1R C2R C3R O2P 157.3(7) . . . . ? O7R C2R C3R C4R -74.8(7) . . . . ? C1R C2R C3R C4R 38.7(7) . . . . ? O2P C3R C4R O6R -146.7(6) . . . . ? C2R C3R C4R O6R -28.9(7) . . . . ? O2P C3R C4R C5R 92.9(8) . . . . ? C2R C3R C4R C5R -149.3(6) . . . . ? O6R C4R C5R O8R -53.9(11) . . . . ? C3R C4R C5R O8R 64.5(10) . . . . ? C5R C4R O6R C1R 129.4(8) . . . . ? C3R C4R O6R C1R 5.7(8) . . . . ? N1B C1R O6R C4R 141.3(6) . . . . ? C2R C1R O6R C4R 20.1(8) . . . . ? O6R C1R N1B C2B -45.2(9) . . . . ? C2R C1R N1B C2B 71.9(10) . . . . ? O6R C1R N1B C8B 166.1(6) . . . . ? C2R C1R N1B C8B -76.9(9) . . . . ? C8B N1B C2B N3B -6.1(9) . . . . ? C1R N1B C2B N3B -159.1(6) . . . . ? N1B C2B N3B C9B 6.5(8) . . . . ? N1B C2B N3B Co -170.9(5) . . . . ? C1C Co N3B C2B 92(3) . . . . ? N21 Co N3B C2B -137.2(5) . . . . ? N24 Co N3B C2B -54.1(6) . . . . ? N22 Co N3B C2B 132.5(6) . . . . ? N23 Co N3B C2B 36.3(5) . . . . ? C1C Co N3B C9B -85(3) . . . . ? N21 Co N3B C9B 46.3(6) . . . . ? N24 Co N3B C9B 129.4(6) . . . . ? N22 Co N3B C9B -44.0(6) . . . . ? N23 Co N3B C9B -140.2(6) . . . . ? C9B C4B C5B C6B -6.4(11) . . . . ? C9B C4B C5B C10B 171.3(7) . . . . ? C4B C5B C6B C7B 5.2(12) . . . . ? C10B C5B C6B C7B -172.5(7) . . . . ? C4B C5B C6B C11B 179.2(7) . . . . ? C10B C5B C6B C11B 1.6(12) . . . . ? C5B C6B C7B C8B -2.0(11) . . . . ? C11B C6B C7B C8B -176.0(8) . . . . ? C2B N1B C8B C9B 2.6(8) . . . . ? C1R N1B C8B C9B 155.7(6) . . . . ? C2B N1B C8B C7B -174.7(8) . . . . ? C1R N1B C8B C7B -21.5(12) . . . . ? C6B C7B C8B C9B 0.2(12) . . . . ? C6B C7B C8B N1B 177.0(7) . . . . ? N1B C8B C9B C4B -179.2(6) . . . . ? C7B C8B C9B C4B -1.7(12) . . . . ? N1B C8B C9B N3B 1.4(8) . . . . ? C7B C8B C9B N3B 178.9(7) . . . . ? C5B C4B C9B C8B 4.7(10) . . . . ? C5B C4B C9B N3B -176.0(7) . . . . ? C2B N3B C9B C8B -4.7(8) . . . . ? Co N3B C9B C8B 172.4(5) . . . . ? C2B N3B C9B C4B 175.9(7) . . . . ? Co N3B C9B C4B -7.0(12) . . . . ? N21 Co C1C N2C -143(11) . . . . ? N24 Co C1C N2C 134(11) . . . . ? N22 Co C1C N2C -52(11) . . . . ? N23 Co C1C N2C 44(11) . . . . ? N3B Co C1C N2C -12(13) . . . . ? _diffrn_measured_fraction_theta_max 0.803 _diffrn_reflns_theta_full 24.50 _diffrn_measured_fraction_theta_full 0.803 _refine_diff_density_max 0.579 _refine_diff_density_min -0.520 _refine_diff_density_rms 0.092