# Electronic Supplementary Material for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Avinash S Kumbhar' _publ_contact_author_email ASKUM@CHEM.UNIPUNE.ERNET.IN _publ_section_title ; Hydrogen bond directed Open-Framework of Bis(Bipyridine-glycoluril) Phosphatocobalt(III) with Solvent Accessible Void Space ; loop_ _publ_author_name 'Avinash S Kumbhar' 'R Butcher' 'Megha S Deshpande' # Attachment 'ask1crystengcomm_Jul_2008.cif' data_ask1 _database_code_depnum_ccdc_archive 'CCDC 666141' _audit_update_record ; 2008-06-24 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'phosphatocobalt(iii) Bipyridine-glycoluril complex' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H24 Co N12 O10 P' _chemical_formula_weight 778.49 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 n a 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z' _cell_length_a 21.8959(6) _cell_length_b 13.8979(3) _cell_length_c 13.7164(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4174.00(17) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 7800 _cell_measurement_theta_min 4.5477 _cell_measurement_theta_max 32.4671 _exptl_crystal_description chunk _exptl_crystal_colour 'dark pink' _exptl_crystal_size_max 0.47 _exptl_crystal_size_mid 0.41 _exptl_crystal_size_min 0.34 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.239 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1592 _exptl_absorpt_coefficient_mu 0.510 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.80923 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.8 (release 12-01-2007 CrysAlis171 .NET) (compiled Jan 12 2007,17:49:11) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 10.5081 _diffrn_standards_number 2 _diffrn_standards_interval_count 50 _diffrn_standards_interval_time ? _diffrn_standards_decay_% <2% _diffrn_reflns_number 28020 _diffrn_reflns_av_R_equivalents 0.0406 _diffrn_reflns_av_sigmaI/netI 0.1149 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 4.64 _diffrn_reflns_theta_max 32.51 _reflns_number_total 12296 _reflns_number_gt 6115 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.31.8 (release 12-01-2007 CrysAlis171 .NET) (compiled Jan 12 2007,17:49:11) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.8 (release 12-01-2007 CrysAlis171 .NET) (compiled Jan 12 2007,17:49:11) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.8 (release 12-01-2007 CrysAlis171 .NET) (compiled Jan 12 2007,17:49:11) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The water H's are restrained otherwise they tend to drift into chemically unfeasible positions during the extended refinement needed to converge the structure. These were lose restraints were: O-H distance constrained to 0.82 Ang.H-H distance constrained so the H-O-H angle was close to 104.5 deg. ; _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^)+(0.0859P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _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 -0.004(15) _refine_ls_number_reflns 12296 _refine_ls_number_parameters 469 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.1042 _refine_ls_R_factor_gt 0.0558 _refine_ls_wR_factor_ref 0.1580 _refine_ls_wR_factor_gt 0.1390 _refine_ls_goodness_of_fit_ref 0.926 _refine_ls_restrained_S_all 0.950 _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 0.734790(19) 0.55375(3) 0.66798(3) 0.03482(12) Uani 1 1 d . . . P P 0.77638(5) 0.72398(6) 0.67027(9) 0.0492(2) Uani 1 1 d . . . O1A O 0.95419(19) 0.3659(3) 0.2869(3) 0.0981(13) Uani 1 1 d . . . O2A O 0.8287(2) 0.0625(3) 0.5088(3) 0.0860(12) Uani 1 1 d . . . O1B O 0.48766(16) 0.5861(3) 1.0548(2) 0.0764(10) Uani 1 1 d . . . O2B O 0.42613(19) 0.3272(3) 0.7327(2) 0.0818(11) Uani 1 1 d . . . O11 O 0.76212(13) 0.6532(2) 0.5837(2) 0.0469(8) Uani 1 1 d . . . O12 O 0.76021(13) 0.65311(19) 0.75554(19) 0.0408(7) Uani 1 1 d . . . O13 O 0.73420(15) 0.81110(18) 0.6722(4) 0.0701(8) Uani 1 1 d . . . O14 O 0.84293(14) 0.7502(2) 0.6740(3) 0.0672(8) Uani 1 1 d . . . O1W O 0.93064(15) 0.7369(3) 0.8200(3) 0.0749(9) Uani 1 1 d D . . H1W1 H 0.9019 0.7513 0.7775 0.112 Uiso 1 1 d RD . . H1W2 H 0.9640 0.6827 0.8138 0.112 Uiso 1 1 d RD . . O2W O 0.88540(16) 0.9258(2) 0.6298(2) 0.0683(9) Uani 1 1 d D . . H2W1 H 0.8805 0.8691 0.6253 0.102 Uiso 1 1 d RD . . H2W2 H 0.8595 0.9625 0.6065 0.102 Uiso 1 1 d RD . . N1A N 0.65200(12) 0.60124(17) 0.6657(2) 0.0350(5) Uani 1 1 d . . . N2A N 0.70407(16) 0.4682(2) 0.7676(2) 0.0393(7) Uani 1 1 d . . . N3A N 0.49773(16) 0.5889(3) 0.8882(2) 0.0515(8) Uani 1 1 d . . . H3AB H 0.4863 0.6474 0.8790 0.062 Uiso 1 1 calc R . . N4A N 0.52826(17) 0.4601(3) 0.9672(2) 0.0594(10) Uani 1 1 d . . . H4AA H 0.5348 0.4209 1.0146 0.071 Uiso 1 1 calc R . . N5A N 0.46036(15) 0.4819(3) 0.7658(2) 0.0477(8) Uani 1 1 d . . . H5AA H 0.4309 0.5133 0.7392 0.057 Uiso 1 1 calc R . . N6A N 0.50999(17) 0.3574(3) 0.8277(3) 0.0624(10) Uani 1 1 d . . . H6AA H 0.5190 0.2988 0.8416 0.075 Uiso 1 1 calc R . . N1B N 0.81479(11) 0.49548(19) 0.6679(3) 0.0378(6) Uani 1 1 d . . . N2B N 0.71829(16) 0.4647(3) 0.5613(2) 0.0422(8) Uani 1 1 d . . . N3B N 0.93189(17) 0.3166(3) 0.4440(3) 0.0656(11) Uani 1 1 d . . . H3BB H 0.9688 0.3086 0.4638 0.079 Uiso 1 1 calc R . . N4B N 0.85597(18) 0.3414(3) 0.3415(3) 0.0665(11) Uani 1 1 d . . . H4BA H 0.8363 0.3616 0.2913 0.080 Uiso 1 1 calc R . . N5B N 0.87481(17) 0.2061(3) 0.5457(3) 0.0586(9) Uani 1 1 d . . . H5BA H 0.8928 0.1881 0.5983 0.070 Uiso 1 1 calc R . . N6B N 0.81486(19) 0.1968(3) 0.4198(3) 0.0612(11) Uani 1 1 d . . . H6BA H 0.7941 0.1712 0.3733 0.073 Uiso 1 1 calc R . . C1A C 0.63036(19) 0.6698(3) 0.6085(3) 0.0450(9) Uani 1 1 d . . . H1AA H 0.6565 0.7024 0.5664 0.054 Uiso 1 1 calc R . . C2A C 0.5669(2) 0.6941(3) 0.6109(3) 0.0528(10) Uani 1 1 d . . . H2AA H 0.5515 0.7411 0.5694 0.063 Uiso 1 1 calc R . . C3A C 0.52956(17) 0.6484(2) 0.6740(3) 0.0456(8) Uani 1 1 d . . . H3AA H 0.4883 0.6639 0.6765 0.055 Uiso 1 1 calc R . . C4A C 0.55340(18) 0.5779(3) 0.7355(3) 0.0400(8) Uani 1 1 d . . . C5A C 0.51329(17) 0.5267(3) 0.8113(2) 0.0397(8) Uani 1 1 d . . . C6A C 0.54419(19) 0.4383(3) 0.8643(3) 0.0444(9) Uani 1 1 d . . . C7A C 0.61079(18) 0.4238(2) 0.8518(3) 0.0379(8) Uani 1 1 d . . . C8A C 0.6426(2) 0.3536(3) 0.9030(3) 0.0524(11) Uani 1 1 d . . . H8AA H 0.6223 0.3147 0.9477 0.063 Uiso 1 1 calc R . . C9A C 0.7056(2) 0.3416(3) 0.8870(4) 0.0558(11) Uani 1 1 d . . . H9AA H 0.7278 0.2961 0.9218 0.067 Uiso 1 1 calc R . . C10A C 0.7334(2) 0.3989(3) 0.8187(3) 0.0530(10) Uani 1 1 d . . . H10A H 0.7748 0.3895 0.8068 0.064 Uiso 1 1 calc R . . C11A C 0.64287(17) 0.4795(2) 0.7856(2) 0.0357(7) Uani 1 1 d . . . C12A C 0.61335(17) 0.5552(2) 0.7279(2) 0.0358(8) Uani 1 1 d . . . C13A C 0.50227(19) 0.5485(4) 0.9790(3) 0.0524(11) Uani 1 1 d . . . C14A C 0.4633(2) 0.3811(4) 0.7707(3) 0.0600(12) Uani 1 1 d . . . C1B C 0.8614(2) 0.5145(3) 0.7272(3) 0.0497(10) Uani 1 1 d . . . H1BA H 0.8569 0.5621 0.7744 0.060 Uiso 1 1 calc R . . C2B C 0.9162(2) 0.4656(3) 0.7206(3) 0.0578(11) Uani 1 1 d . . . H2BA H 0.9477 0.4787 0.7641 0.069 Uiso 1 1 calc R . . C3B C 0.92358(19) 0.3964(3) 0.6484(3) 0.0573(11) Uani 1 1 d . . . H3BA H 0.9599 0.3621 0.6432 0.069 Uiso 1 1 calc R . . C4B C 0.87555(18) 0.3792(3) 0.5836(3) 0.0423(8) Uani 1 1 d . . . C5B C 0.88015(18) 0.3023(3) 0.5051(3) 0.0496(10) Uani 1 1 d . . . C6B C 0.8278(2) 0.3001(4) 0.4276(3) 0.0566(12) Uani 1 1 d . . . C7B C 0.76919(18) 0.3554(3) 0.4540(3) 0.0484(10) Uani 1 1 d . . . C8B C 0.7166(2) 0.3476(4) 0.3985(4) 0.0815(19) Uani 1 1 d . . . H8BA H 0.7157 0.3086 0.3434 0.098 Uiso 1 1 calc R . . C9B C 0.6658(3) 0.3987(5) 0.4266(5) 0.101(2) Uani 1 1 d . . . H9BA H 0.6302 0.3953 0.3896 0.121 Uiso 1 1 calc R . . C10B C 0.66740(19) 0.4557(3) 0.5104(3) 0.0581(12) Uani 1 1 d . . . H10B H 0.6323 0.4877 0.5305 0.070 Uiso 1 1 calc R . . C11B C 0.76866(16) 0.4149(3) 0.5340(3) 0.0348(7) Uani 1 1 d . . . C12B C 0.82242(17) 0.4302(3) 0.5960(2) 0.0367(8) Uani 1 1 d . . . C13B C 0.9179(3) 0.3441(4) 0.3511(4) 0.0729(14) Uani 1 1 d . . . C14B C 0.8388(2) 0.1482(4) 0.4924(4) 0.0631(13) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co 0.0348(2) 0.0351(2) 0.0346(2) -0.0060(2) 0.0054(2) -0.00224(18) P 0.0626(6) 0.0420(5) 0.0431(5) -0.0040(6) 0.0032(6) -0.0138(4) O1A 0.080(3) 0.135(4) 0.079(2) -0.006(2) 0.036(2) 0.015(3) O2A 0.105(3) 0.060(2) 0.093(3) -0.030(2) -0.019(2) 0.014(2) O1B 0.069(2) 0.124(3) 0.0363(15) -0.0159(18) 0.0107(15) 0.010(2) O2B 0.092(3) 0.091(2) 0.0614(19) 0.0013(18) -0.0144(18) -0.050(2) O11 0.0451(18) 0.059(2) 0.0367(15) -0.0013(13) 0.0043(12) -0.0127(14) O12 0.0584(19) 0.0362(15) 0.0280(14) -0.0105(11) 0.0048(11) -0.0050(13) O13 0.086(2) 0.0445(14) 0.080(2) 0.007(2) -0.005(2) 0.0056(14) O14 0.0641(18) 0.0801(19) 0.0574(15) 0.003(2) -0.0001(18) -0.0259(15) O1W 0.055(2) 0.094(2) 0.075(2) -0.013(2) -0.0081(16) -0.0027(18) O2W 0.071(2) 0.0582(17) 0.076(2) 0.0165(15) -0.0169(16) -0.0205(16) N1A 0.0434(14) 0.0312(12) 0.0302(12) 0.0007(15) 0.0076(15) 0.0022(11) N2A 0.0417(19) 0.0334(16) 0.0428(16) -0.0027(14) 0.0033(14) 0.0017(14) N3A 0.054(2) 0.063(2) 0.0384(17) 0.0029(16) 0.0093(15) -0.0002(18) N4A 0.045(2) 0.092(3) 0.0409(17) 0.0235(18) 0.0106(15) 0.002(2) N5A 0.0413(18) 0.064(2) 0.0384(16) 0.0030(15) -0.0073(14) -0.0083(16) N6A 0.051(2) 0.055(2) 0.081(3) 0.006(2) -0.011(2) -0.0125(18) N1B 0.0313(13) 0.0439(14) 0.0382(13) -0.0094(17) 0.0018(15) -0.0057(11) N2B 0.0357(17) 0.0461(18) 0.0449(17) -0.0123(15) -0.0001(14) -0.0012(15) N3B 0.041(2) 0.099(3) 0.057(2) -0.019(2) -0.0041(17) 0.020(2) N4B 0.056(2) 0.092(3) 0.051(2) -0.009(2) 0.0052(18) 0.023(2) N5B 0.060(2) 0.059(2) 0.0568(19) -0.0122(17) -0.0237(17) 0.0098(19) N6B 0.078(3) 0.054(2) 0.0514(19) -0.0208(17) -0.0236(19) 0.0192(19) C1A 0.052(2) 0.040(2) 0.0435(19) 0.0075(17) 0.0067(17) 0.0010(17) C2A 0.063(3) 0.055(2) 0.041(2) 0.0100(18) 0.0009(19) 0.009(2) C3A 0.0402(18) 0.0476(18) 0.0491(19) -0.008(2) 0.003(2) 0.0036(15) C4A 0.046(2) 0.0366(18) 0.0370(18) 0.0012(15) 0.0024(15) -0.0085(16) C5A 0.0366(19) 0.050(2) 0.0330(17) -0.0009(16) 0.0020(14) -0.0050(16) C6A 0.045(2) 0.050(2) 0.0377(19) 0.0078(16) -0.0017(16) -0.0072(18) C7A 0.043(2) 0.0350(17) 0.0361(18) -0.0027(14) 0.0022(15) -0.0077(15) C8A 0.073(3) 0.039(2) 0.046(2) 0.0061(17) 0.003(2) 0.000(2) C9A 0.053(3) 0.043(2) 0.071(3) 0.006(2) 0.011(2) 0.003(2) C10A 0.046(2) 0.048(2) 0.065(3) 0.000(2) 0.005(2) 0.013(2) C11A 0.0364(19) 0.0340(16) 0.0367(18) -0.0005(15) 0.0003(14) 0.0006(15) C12A 0.041(2) 0.0335(17) 0.0326(16) -0.0017(14) 0.0074(14) -0.0031(15) C13A 0.037(2) 0.081(3) 0.040(2) 0.000(2) 0.0005(17) 0.001(2) C14A 0.057(3) 0.076(3) 0.047(2) 0.008(2) 0.005(2) -0.026(3) C1B 0.054(2) 0.054(2) 0.041(2) -0.0194(18) -0.0064(18) -0.001(2) C2B 0.058(3) 0.066(3) 0.050(2) -0.013(2) -0.021(2) -0.006(2) C3B 0.039(2) 0.064(3) 0.069(3) -0.013(2) -0.0151(19) 0.0041(19) C4B 0.041(2) 0.045(2) 0.0412(18) -0.0029(16) -0.0067(15) 0.0076(17) C5B 0.037(2) 0.065(3) 0.047(2) -0.019(2) -0.0073(17) 0.0143(19) C6B 0.048(2) 0.078(3) 0.044(2) -0.028(2) -0.0113(18) 0.027(2) C7B 0.039(2) 0.059(2) 0.047(2) -0.0149(18) -0.0056(17) 0.0103(19) C8B 0.059(3) 0.116(5) 0.069(3) -0.059(3) -0.027(3) 0.027(3) C9B 0.060(3) 0.128(5) 0.115(4) -0.078(4) -0.046(3) 0.034(4) C10B 0.031(2) 0.081(3) 0.062(2) -0.030(2) -0.0081(19) 0.006(2) C11B 0.0352(19) 0.0344(17) 0.0348(18) -0.0050(14) -0.0017(14) 0.0022(15) C12B 0.0346(19) 0.044(2) 0.0314(16) -0.0044(15) 0.0004(14) 0.0014(15) C13B 0.071(3) 0.082(3) 0.066(3) -0.017(3) 0.008(3) 0.026(3) C14B 0.058(3) 0.060(3) 0.071(3) -0.033(2) -0.015(2) 0.018(2) _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 O11 1.899(3) . ? Co O12 1.913(3) . ? Co N1A 1.929(3) . ? Co N1B 1.930(3) . ? Co N2A 1.932(3) . ? Co N2B 1.950(3) . ? Co P 2.5352(9) . ? P O14 1.503(3) . ? P O13 1.523(3) . ? P O12 1.570(3) . ? P O11 1.574(3) . ? O1A C13B 1.225(6) . ? O2A C14B 1.232(6) . ? O1B C13A 1.207(5) . ? O2B C14A 1.222(5) . ? O1W H1W1 0.8810 . ? O1W H1W2 1.0530 . ? O2W H2W1 0.7977 . ? O2W H2W2 0.8273 . ? N1A C1A 1.323(5) . ? N1A C12A 1.361(4) . ? N2A C10A 1.354(5) . ? N2A C11A 1.372(5) . ? N3A C13A 1.370(5) . ? N3A C5A 1.405(5) . ? N3A H3AB 0.8600 . ? N4A C13A 1.364(6) . ? N4A C6A 1.484(5) . ? N4A H4AA 0.8600 . ? N5A C14A 1.404(6) . ? N5A C5A 1.457(5) . ? N5A H5AA 0.8600 . ? N6A C14A 1.329(6) . ? N6A C6A 1.441(5) . ? N6A H6AA 0.8600 . ? N1B C1B 1.331(5) . ? N1B C12B 1.350(5) . ? N2B C10B 1.321(5) . ? N2B C11B 1.355(5) . ? N3B C13B 1.365(7) . ? N3B C5B 1.424(6) . ? N3B H3BB 0.8600 . ? N4B C13B 1.362(7) . ? N4B C6B 1.450(6) . ? N4B H4BA 0.8600 . ? N5B C14B 1.342(5) . ? N5B C5B 1.453(6) . ? N5B H5BA 0.8600 . ? N6B C14B 1.313(6) . ? N6B C6B 1.467(6) . ? N6B H6BA 0.8600 . ? C1A C2A 1.430(6) . ? C1A H1AA 0.9300 . ? C2A C3A 1.349(6) . ? C2A H2AA 0.9300 . ? C3A C4A 1.395(6) . ? C3A H3AA 0.9300 . ? C4A C12A 1.354(5) . ? C4A C5A 1.535(5) . ? C5A C6A 1.581(5) . ? C6A C7A 1.482(6) . ? C7A C11A 1.386(5) . ? C7A C8A 1.389(6) . ? C8A C9A 1.406(6) . ? C8A H8AA 0.9300 . ? C9A C10A 1.372(6) . ? C9A H9AA 0.9300 . ? C10A H10A 0.9300 . ? C11A C12A 1.467(5) . ? C1B C2B 1.382(6) . ? C1B H1BA 0.9300 . ? C2B C3B 1.391(6) . ? C2B H2BA 0.9300 . ? C3B C4B 1.397(5) . ? C3B H3BA 0.9300 . ? C4B C12B 1.373(5) . ? C4B C5B 1.521(5) . ? C5B C6B 1.563(6) . ? C6B C7B 1.540(5) . ? C7B C11B 1.373(5) . ? C7B C8B 1.385(6) . ? C8B C9B 1.376(7) . ? C8B H8BA 0.9300 . ? C9B C10B 1.397(7) . ? C9B H9BA 0.9300 . ? C10B H10B 0.9300 . ? C11B C12B 1.468(5) . ? 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 O11 Co O12 76.43(9) . . ? O11 Co N1A 92.14(12) . . ? O12 Co N1A 92.10(12) . . ? O11 Co N1B 91.08(13) . . ? O12 Co N1B 92.26(12) . . ? N1A Co N1B 175.10(11) . . ? O11 Co N2A 171.24(13) . . ? O12 Co N2A 95.83(13) . . ? N1A Co N2A 83.97(14) . . ? N1B Co N2A 93.35(14) . . ? O11 Co N2B 93.63(15) . . ? O12 Co N2B 169.46(14) . . ? N1A Co N2B 91.77(14) . . ? N1B Co N2B 84.33(14) . . ? N2A Co N2B 94.33(12) . . ? O11 Co P 38.29(10) . . ? O12 Co P 38.19(9) . . ? N1A Co P 91.06(8) . . ? N1B Co P 93.76(8) . . ? N2A Co P 133.67(10) . . ? N2B Co P 131.92(12) . . ? O14 P O13 113.23(18) . . ? O14 P O12 110.24(18) . . ? O13 P O12 110.4(2) . . ? O14 P O11 111.69(18) . . ? O13 P O11 112.9(2) . . ? O12 P O11 97.21(12) . . ? O14 P Co 125.11(14) . . ? O13 P Co 121.62(13) . . ? O12 P Co 48.90(10) . . ? O11 P Co 48.39(11) . . ? P O11 Co 93.31(15) . . ? P O12 Co 92.91(13) . . ? H1W1 O1W H1W2 127.3 . . ? H2W1 O2W H2W2 119.1 . . ? C1A N1A C12A 119.2(3) . . ? C1A N1A Co 126.3(3) . . ? C12A N1A Co 114.4(2) . . ? C10A N2A C11A 116.9(3) . . ? C10A N2A Co 129.7(3) . . ? C11A N2A Co 113.4(3) . . ? C13A N3A C5A 114.4(4) . . ? C13A N3A H3AB 122.8 . . ? C5A N3A H3AB 122.8 . . ? C13A N4A C6A 113.3(3) . . ? C13A N4A H4AA 123.3 . . ? C6A N4A H4AA 123.3 . . ? C14A N5A C5A 111.7(3) . . ? C14A N5A H5AA 124.1 . . ? C5A N5A H5AA 124.1 . . ? C14A N6A C6A 114.4(4) . . ? C14A N6A H6AA 122.8 . . ? C6A N6A H6AA 122.8 . . ? C1B N1B C12B 119.0(3) . . ? C1B N1B Co 127.7(3) . . ? C12B N1B Co 113.2(2) . . ? C10B N2B C11B 119.5(3) . . ? C10B N2B Co 127.8(3) . . ? C11B N2B Co 112.4(3) . . ? C13B N3B C5B 114.2(4) . . ? C13B N3B H3BB 122.9 . . ? C5B N3B H3BB 122.9 . . ? C13B N4B C6B 110.8(4) . . ? C13B N4B H4BA 124.6 . . ? C6B N4B H4BA 124.6 . . ? C14B N5B C5B 113.0(4) . . ? C14B N5B H5BA 123.5 . . ? C5B N5B H5BA 123.5 . . ? C14B N6B C6B 111.7(4) . . ? C14B N6B H6BA 124.1 . . ? C6B N6B H6BA 124.1 . . ? N1A C1A C2A 120.3(3) . . ? N1A C1A H1AA 119.9 . . ? C2A C1A H1AA 119.9 . . ? C3A C2A C1A 119.5(4) . . ? C3A C2A H2AA 120.2 . . ? C1A C2A H2AA 120.2 . . ? C2A C3A C4A 119.5(4) . . ? C2A C3A H3AA 120.3 . . ? C4A C3A H3AA 120.3 . . ? C12A C4A C3A 118.6(3) . . ? C12A C4A C5A 120.0(3) . . ? C3A C4A C5A 121.4(3) . . ? N3A C5A N5A 113.1(3) . . ? N3A C5A C4A 111.2(3) . . ? N5A C5A C4A 111.3(3) . . ? N3A C5A C6A 103.7(3) . . ? N5A C5A C6A 101.8(3) . . ? C4A C5A C6A 115.3(3) . . ? N6A C6A C7A 111.4(3) . . ? N6A C6A N4A 111.6(3) . . ? C7A C6A N4A 111.7(3) . . ? N6A C6A C5A 102.9(3) . . ? C7A C6A C5A 118.3(3) . . ? N4A C6A C5A 100.2(3) . . ? C11A C7A C8A 118.0(4) . . ? C11A C7A C6A 119.9(3) . . ? C8A C7A C6A 122.0(4) . . ? C7A C8A C9A 119.7(4) . . ? C7A C8A H8AA 120.1 . . ? C9A C8A H8AA 120.1 . . ? C10A C9A C8A 118.3(4) . . ? C10A C9A H9AA 120.8 . . ? C8A C9A H9AA 120.8 . . ? N2A C10A C9A 123.7(4) . . ? N2A C10A H10A 118.2 . . ? C9A C10A H10A 118.2 . . ? N2A C11A C7A 123.3(3) . . ? N2A C11A C12A 114.6(3) . . ? C7A C11A C12A 122.1(3) . . ? C4A C12A N1A 122.9(3) . . ? C4A C12A C11A 123.5(3) . . ? N1A C12A C11A 113.7(3) . . ? O1B C13A N4A 127.2(4) . . ? O1B C13A N3A 125.9(5) . . ? N4A C13A N3A 106.9(4) . . ? O2B C14A N6A 127.7(5) . . ? O2B C14A N5A 124.1(5) . . ? N6A C14A N5A 108.1(4) . . ? N1B C1B C2B 121.8(3) . . ? N1B C1B H1BA 119.1 . . ? C2B C1B H1BA 119.1 . . ? C1B C2B C3B 119.2(4) . . ? C1B C2B H2BA 120.4 . . ? C3B C2B H2BA 120.4 . . ? C2B C3B C4B 118.9(4) . . ? C2B C3B H3BA 120.5 . . ? C4B C3B H3BA 120.5 . . ? C12B C4B C3B 118.1(3) . . ? C12B C4B C5B 120.4(3) . . ? C3B C4B C5B 121.4(3) . . ? N3B C5B N5B 114.7(4) . . ? N3B C5B C4B 111.8(4) . . ? N5B C5B C4B 111.8(3) . . ? N3B C5B C6B 100.7(3) . . ? N5B C5B C6B 100.6(3) . . ? C4B C5B C6B 116.5(3) . . ? N4B C6B N6B 114.2(3) . . ? N4B C6B C7B 110.4(4) . . ? N6B C6B C7B 110.1(4) . . ? N4B C6B C5B 103.6(4) . . ? N6B C6B C5B 102.2(3) . . ? C7B C6B C5B 116.2(3) . . ? C11B C7B C8B 118.7(4) . . ? C11B C7B C6B 119.7(3) . . ? C8B C7B C6B 121.6(4) . . ? C9B C8B C7B 118.5(4) . . ? C9B C8B H8BA 120.7 . . ? C7B C8B H8BA 120.7 . . ? C8B C9B C10B 120.2(5) . . ? C8B C9B H9BA 119.9 . . ? C10B C9B H9BA 119.9 . . ? N2B C10B C9B 120.7(4) . . ? N2B C10B H10B 119.7 . . ? C9B C10B H10B 119.7 . . ? N2B C11B C7B 122.4(3) . . ? N2B C11B C12B 114.7(3) . . ? C7B C11B C12B 122.9(3) . . ? N1B C12B C4B 122.8(3) . . ? N1B C12B C11B 114.9(3) . . ? C4B C12B C11B 122.2(3) . . ? O1A C13B N4B 125.7(5) . . ? O1A C13B N3B 126.4(5) . . ? N4B C13B N3B 107.9(5) . . ? O2A C14B N6B 124.3(4) . . ? O2A C14B N5B 125.8(5) . . ? N6B C14B N5B 109.9(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 O11 Co P O14 -88.8(2) . . . . ? O12 Co P O14 87.0(2) . . . . ? N1A Co P O14 179.0(2) . . . . ? N1B Co P O14 -1.9(2) . . . . ? N2A Co P O14 96.4(2) . . . . ? N2B Co P O14 -87.6(2) . . . . ? O11 Co P O13 93.8(3) . . . . ? O12 Co P O13 -90.4(3) . . . . ? N1A Co P O13 1.6(2) . . . . ? N1B Co P O13 -179.3(2) . . . . ? N2A Co P O13 -81.0(3) . . . . ? N2B Co P O13 95.0(3) . . . . ? O11 Co P O12 -175.85(18) . . . . ? N1A Co P O12 92.04(17) . . . . ? N1B Co P O12 -88.87(18) . . . . ? N2A Co P O12 9.4(2) . . . . ? N2B Co P O12 -174.6(2) . . . . ? O12 Co P O11 175.85(18) . . . . ? N1A Co P O11 -92.11(18) . . . . ? N1B Co P O11 86.97(18) . . . . ? N2A Co P O11 -174.8(2) . . . . ? N2B Co P O11 1.2(2) . . . . ? O14 P O11 Co 118.34(17) . . . . ? O13 P O11 Co -112.67(19) . . . . ? O12 P O11 Co 3.15(14) . . . . ? O12 Co O11 P -2.64(11) . . . . ? N1A Co O11 P 89.00(15) . . . . ? N1B Co O11 P -94.70(15) . . . . ? N2A Co O11 P 25.6(10) . . . . ? N2B Co O11 P -179.09(16) . . . . ? O14 P O12 Co -119.47(17) . . . . ? O13 P O12 Co 114.67(18) . . . . ? O11 P O12 Co -3.13(13) . . . . ? O11 Co O12 P 2.65(11) . . . . ? N1A Co O12 P -89.05(15) . . . . ? N1B Co O12 P 93.21(15) . . . . ? N2A Co O12 P -173.19(15) . . . . ? N2B Co O12 P 22.4(9) . . . . ? O11 Co N1A C1A 8.9(3) . . . . ? O12 Co N1A C1A 85.4(3) . . . . ? N1B Co N1A C1A -122.0(17) . . . . ? N2A Co N1A C1A -179.0(3) . . . . ? N2B Co N1A C1A -84.8(3) . . . . ? P Co N1A C1A 47.2(3) . . . . ? O11 Co N1A C12A -173.5(3) . . . . ? O12 Co N1A C12A -97.0(2) . . . . ? N1B Co N1A C12A 55.6(18) . . . . ? N2A Co N1A C12A -1.4(2) . . . . ? N2B Co N1A C12A 92.8(3) . . . . ? P Co N1A C12A -135.2(2) . . . . ? O11 Co N2A C10A -116.5(9) . . . . ? O12 Co N2A C10A -88.9(4) . . . . ? N1A Co N2A C10A 179.6(4) . . . . ? N1B Co N2A C10A 3.7(4) . . . . ? N2B Co N2A C10A 88.2(4) . . . . ? P Co N2A C10A -94.8(4) . . . . ? O11 Co N2A C11A 65.5(10) . . . . ? O12 Co N2A C11A 93.0(3) . . . . ? N1A Co N2A C11A 1.5(3) . . . . ? N1B Co N2A C11A -174.4(3) . . . . ? N2B Co N2A C11A -89.8(3) . . . . ? P Co N2A C11A 87.2(3) . . . . ? O11 Co N1B C1B 88.2(3) . . . . ? O12 Co N1B C1B 11.7(3) . . . . ? N1A Co N1B C1B -140.9(16) . . . . ? N2A Co N1B C1B -84.3(3) . . . . ? N2B Co N1B C1B -178.3(4) . . . . ? P Co N1B C1B 49.9(3) . . . . ? O11 Co N1B C12B -89.8(3) . . . . ? O12 Co N1B C12B -166.3(2) . . . . ? N1A Co N1B C12B 41.1(18) . . . . ? N2A Co N1B C12B 97.7(3) . . . . ? N2B Co N1B C12B 3.7(3) . . . . ? P Co N1B C12B -128.1(2) . . . . ? O11 Co N2B C10B -88.1(4) . . . . ? O12 Co N2B C10B -107.3(8) . . . . ? N1A Co N2B C10B 4.2(4) . . . . ? N1B Co N2B C10B -178.8(4) . . . . ? N2A Co N2B C10B 88.2(4) . . . . ? P Co N2B C10B -88.8(4) . . . . ? O11 Co N2B C11B 85.2(3) . . . . ? O12 Co N2B C11B 66.0(9) . . . . ? N1A Co N2B C11B 177.5(3) . . . . ? N1B Co N2B C11B -5.5(3) . . . . ? N2A Co N2B C11B -98.5(3) . . . . ? P Co N2B C11B 84.4(3) . . . . ? C12A N1A C1A C2A -1.0(5) . . . . ? Co N1A C1A C2A 176.5(3) . . . . ? N1A C1A C2A C3A 1.8(6) . . . . ? C1A C2A C3A C4A -0.3(6) . . . . ? C2A C3A C4A C12A -2.0(6) . . . . ? C2A C3A C4A C5A 177.5(4) . . . . ? C13A N3A C5A N5A 97.6(4) . . . . ? C13A N3A C5A C4A -136.4(4) . . . . ? C13A N3A C5A C6A -11.9(4) . . . . ? C14A N5A C5A N3A -121.3(4) . . . . ? C14A N5A C5A C4A 112.7(4) . . . . ? C14A N5A C5A C6A -10.7(4) . . . . ? C12A C4A C5A N3A 108.4(4) . . . . ? C3A C4A C5A N3A -71.1(4) . . . . ? C12A C4A C5A N5A -124.5(4) . . . . ? C3A C4A C5A N5A 56.0(5) . . . . ? C12A C4A C5A C6A -9.2(5) . . . . ? C3A C4A C5A C6A 171.2(3) . . . . ? C14A N6A C6A C7A -132.4(4) . . . . ? C14A N6A C6A N4A 102.0(4) . . . . ? C14A N6A C6A C5A -4.7(5) . . . . ? C13A N4A C6A N6A -116.5(4) . . . . ? C13A N4A C6A C7A 118.0(4) . . . . ? C13A N4A C6A C5A -8.1(4) . . . . ? N3A C5A C6A N6A 126.4(3) . . . . ? N5A C5A C6A N6A 8.8(4) . . . . ? C4A C5A C6A N6A -111.8(3) . . . . ? N3A C5A C6A C7A -110.3(4) . . . . ? N5A C5A C6A C7A 132.1(3) . . . . ? C4A C5A C6A C7A 11.5(4) . . . . ? N3A C5A C6A N4A 11.2(4) . . . . ? N5A C5A C6A N4A -106.4(3) . . . . ? C4A C5A C6A N4A 133.1(3) . . . . ? N6A C6A C7A C11A 111.0(4) . . . . ? N4A C6A C7A C11A -123.4(4) . . . . ? C5A C6A C7A C11A -7.9(5) . . . . ? N6A C6A C7A C8A -67.3(4) . . . . ? N4A C6A C7A C8A 58.2(5) . . . . ? C5A C6A C7A C8A 173.7(3) . . . . ? C11A C7A C8A C9A 0.4(6) . . . . ? C6A C7A C8A C9A 178.8(4) . . . . ? C7A C8A C9A C10A -1.6(6) . . . . ? C11A N2A C10A C9A -0.9(6) . . . . ? Co N2A C10A C9A -178.9(3) . . . . ? C8A C9A C10A N2A 1.9(7) . . . . ? C10A N2A C11A C7A -0.4(5) . . . . ? Co N2A C11A C7A 177.9(3) . . . . ? C10A N2A C11A C12A -179.7(3) . . . . ? Co N2A C11A C12A -1.4(4) . . . . ? C8A C7A C11A N2A 0.6(5) . . . . ? C6A C7A C11A N2A -177.8(3) . . . . ? C8A C7A C11A C12A 179.9(3) . . . . ? C6A C7A C11A C12A 1.5(5) . . . . ? C3A C4A C12A N1A 2.9(5) . . . . ? C5A C4A C12A N1A -176.6(3) . . . . ? C3A C4A C12A C11A -177.3(3) . . . . ? C5A C4A C12A C11A 3.2(5) . . . . ? C1A N1A C12A C4A -1.4(5) . . . . ? Co N1A C12A C4A -179.2(3) . . . . ? C1A N1A C12A C11A 178.8(3) . . . . ? Co N1A C12A C11A 1.0(4) . . . . ? N2A C11A C12A C4A -179.5(3) . . . . ? C7A C11A C12A C4A 1.2(5) . . . . ? N2A C11A C12A N1A 0.3(4) . . . . ? C7A C11A C12A N1A -179.0(3) . . . . ? C6A N4A C13A O1B -176.2(4) . . . . ? C6A N4A C13A N3A 1.6(5) . . . . ? C5A N3A C13A O1B -175.1(4) . . . . ? C5A N3A C13A N4A 7.1(5) . . . . ? C6A N6A C14A O2B -177.7(5) . . . . ? C6A N6A C14A N5A -1.9(5) . . . . ? C5A N5A C14A O2B -175.6(4) . . . . ? C5A N5A C14A N6A 8.4(5) . . . . ? C12B N1B C1B C2B -3.6(6) . . . . ? Co N1B C1B C2B 178.4(3) . . . . ? N1B C1B C2B C3B 1.9(7) . . . . ? C1B C2B C3B C4B 0.7(7) . . . . ? C2B C3B C4B C12B -1.5(6) . . . . ? C2B C3B C4B C5B -178.0(4) . . . . ? C13B N3B C5B N5B 120.9(4) . . . . ? C13B N3B C5B C4B -110.5(4) . . . . ? C13B N3B C5B C6B 13.9(5) . . . . ? C14B N5B C5B N3B -94.6(4) . . . . ? C14B N5B C5B C4B 136.7(4) . . . . ? C14B N5B C5B C6B 12.4(5) . . . . ? C12B C4B C5B N3B 127.4(4) . . . . ? C3B C4B C5B N3B -56.1(5) . . . . ? C12B C4B C5B N5B -102.4(4) . . . . ? C3B C4B C5B N5B 74.0(5) . . . . ? C12B C4B C5B C6B 12.4(6) . . . . ? C3B C4B C5B C6B -171.1(4) . . . . ? C13B N4B C6B N6B -95.4(5) . . . . ? C13B N4B C6B C7B 139.9(4) . . . . ? C13B N4B C6B C5B 14.9(5) . . . . ? C14B N6B C6B N4B 126.2(4) . . . . ? C14B N6B C6B C7B -109.0(4) . . . . ? C14B N6B C6B C5B 15.0(5) . . . . ? N3B C5B C6B N4B -16.4(4) . . . . ? N5B C5B C6B N4B -134.3(3) . . . . ? C4B C5B C6B N4B 104.7(4) . . . . ? N3B C5B C6B N6B 102.6(4) . . . . ? N5B C5B C6B N6B -15.3(4) . . . . ? C4B C5B C6B N6B -136.3(4) . . . . ? N3B C5B C6B C7B -137.6(4) . . . . ? N5B C5B C6B C7B 104.5(4) . . . . ? C4B C5B C6B C7B -16.4(6) . . . . ? N4B C6B C7B C11B -107.3(4) . . . . ? N6B C6B C7B C11B 125.6(4) . . . . ? C5B C6B C7B C11B 10.1(6) . . . . ? N4B C6B C7B C8B 72.0(6) . . . . ? N6B C6B C7B C8B -55.0(6) . . . . ? C5B C6B C7B C8B -170.5(5) . . . . ? C11B C7B C8B C9B -0.9(9) . . . . ? C6B C7B C8B C9B 179.7(6) . . . . ? C7B C8B C9B C10B -1.1(11) . . . . ? C11B N2B C10B C9B -2.7(8) . . . . ? Co N2B C10B C9B 170.2(5) . . . . ? C8B C9B C10B N2B 3.0(11) . . . . ? C10B N2B C11B C7B 0.6(6) . . . . ? Co N2B C11B C7B -173.3(3) . . . . ? C10B N2B C11B C12B -179.9(4) . . . . ? Co N2B C11B C12B 6.2(4) . . . . ? C8B C7B C11B N2B 1.2(7) . . . . ? C6B C7B C11B N2B -179.4(4) . . . . ? C8B C7B C11B C12B -178.3(5) . . . . ? C6B C7B C11B C12B 1.1(6) . . . . ? C1B N1B C12B C4B 2.9(5) . . . . ? Co N1B C12B C4B -178.9(3) . . . . ? C1B N1B C12B C11B -179.5(3) . . . . ? Co N1B C12B C11B -1.3(4) . . . . ? C3B C4B C12B N1B -0.3(6) . . . . ? C5B C4B C12B N1B 176.3(3) . . . . ? C3B C4B C12B C11B -177.8(4) . . . . ? C5B C4B C12B C11B -1.2(6) . . . . ? N2B C11B C12B N1B -3.4(5) . . . . ? C7B C11B C12B N1B 176.2(4) . . . . ? N2B C11B C12B C4B 174.3(4) . . . . ? C7B C11B C12B C4B -6.2(6) . . . . ? C6B N4B C13B O1A 172.1(5) . . . . ? C6B N4B C13B N3B -6.8(6) . . . . ? C5B N3B C13B O1A 175.6(5) . . . . ? C5B N3B C13B N4B -5.4(6) . . . . ? C6B N6B C14B O2A 171.3(5) . . . . ? C6B N6B C14B N5B -8.0(6) . . . . ? C5B N5B C14B O2A 177.0(5) . . . . ? C5B N5B C14B N6B -3.7(5) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H1W1 O14 0.88 1.92 2.781(5) 165.6 . O1W H1W2 O1A 1.05 1.95 2.934(6) 154.3 2_765 O2W H2W1 O14 0.80 1.96 2.681(4) 149.6 . O2W H2W2 O2A 0.83 2.05 2.812(5) 153.9 1_565 N3A H3AB O1W 0.86 2.17 2.982(5) 156.5 4_465 N4A H4AA O2W 0.86 2.36 2.962(5) 127.7 3_645 N5A H5AA O2W 0.86 1.99 2.797(5) 155.7 4_465 N4B H4BA O13 0.86 2.35 3.077(6) 142.0 3_644 N5B H5BA O2B 0.86 1.99 2.839(5) 167.2 4 N6B H6BA O12 0.86 2.02 2.854(4) 162.7 3_644 C3A H3AA O2W 0.93 2.65 3.376(5) 135.1 4_465 C8B H8BA O12 0.93 2.53 3.377(5) 151.6 3_644 _diffrn_measured_fraction_theta_max 0.928 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.003 _refine_diff_density_min -0.488 _refine_diff_density_rms 0.075