# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_at1bpin _database_code_depnum_ccdc_archive 'CCDC 898276' #TrackingRef 'at1bpin.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C4 H14 N2 O5 P2, 0.5(H2 O)' _chemical_formula_sum 'C4 H15 N2 O5.50 P2' _chemical_formula_weight 241.12 _chemical_compound_source 'synthesized by the authors' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 16.4183(4) _cell_length_b 6.7200(2) _cell_length_c 17.8230(4) _cell_angle_alpha 90.00 _cell_angle_beta 101.2530(10) _cell_angle_gamma 90.00 _cell_volume 1928.62(9) _cell_formula_units_Z 8 _cell_measurement_temperature 150(1) _cell_measurement_reflns_used 6599 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.661 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1016 _exptl_absorpt_coefficient_mu 0.454 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8209 _exptl_absorpt_correction_T_max 0.9569 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(1) _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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11754 _diffrn_reflns_av_R_equivalents 0.0200 _diffrn_reflns_av_sigmaI/netI 0.0165 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.33 _diffrn_reflns_theta_max 27.50 _reflns_number_total 2218 _reflns_number_gt 2003 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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. ; _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^)+(0.0376P)^2^+2.6664P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2218 _refine_ls_number_parameters 124 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0302 _refine_ls_R_factor_gt 0.0261 _refine_ls_wR_factor_ref 0.0739 _refine_ls_wR_factor_gt 0.0713 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.077 _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 N1 N 0.46343(8) 0.4900(2) 0.62716(8) 0.0140(3) Uani 1 1 d . . . H11 H 0.4693 0.5538 0.6725 0.017 Uiso 1 1 d R . . H12 H 0.4121 0.5050 0.6016 0.017 Uiso 1 1 d R . . H13 H 0.5021 0.5506 0.5989 0.017 Uiso 1 1 d R . . C2 C 0.48594(9) 0.2764(2) 0.63704(9) 0.0134(3) Uani 1 1 d . . . H21 H 0.4675 0.2076 0.5875 0.016 Uiso 1 1 calc R . . H22 H 0.4552 0.2173 0.6742 0.016 Uiso 1 1 calc R . . P3 P 0.59688(2) 0.22964(6) 0.67026(2) 0.00983(11) Uani 1 1 d . . . O31 O 0.60302(7) 0.01584(16) 0.69587(7) 0.0171(2) Uani 1 1 d . . . O32 O 0.63223(6) 0.38398(16) 0.72945(6) 0.0129(2) Uani 1 1 d . . . C4 C 0.65005(9) 0.2502(2) 0.58836(8) 0.0111(3) Uani 1 1 d . . . O41 O 0.73138(7) 0.17507(17) 0.62010(6) 0.0161(2) Uani 1 1 d . . . H41O H 0.7532 0.1179 0.5826 0.019 Uiso 1 1 d R . . C41 C 0.60640(10) 0.1225(2) 0.52104(9) 0.0155(3) Uani 1 1 d . . . H411 H 0.6406 0.1174 0.4817 0.019 Uiso 1 1 calc R . . H412 H 0.5523 0.1810 0.4993 0.019 Uiso 1 1 calc R . . H413 H 0.5985 -0.0126 0.5391 0.019 Uiso 1 1 calc R . . P5 P 0.65949(2) 0.50816(5) 0.55414(2) 0.00919(11) Uani 1 1 d . . . O51 O 0.68854(7) 0.49553(16) 0.47891(6) 0.0138(2) Uani 1 1 d . . . O52 O 0.58008(6) 0.61972(16) 0.55361(6) 0.0126(2) Uani 1 1 d . . . C6 C 0.74319(9) 0.6296(2) 0.62042(9) 0.0149(3) Uani 1 1 d . . . H61 H 0.7878 0.5314 0.6378 0.018 Uiso 1 1 calc R . . H62 H 0.7667 0.7368 0.5930 0.018 Uiso 1 1 calc R . . N7 N 0.71643(8) 0.7165(2) 0.68862(7) 0.0137(3) Uani 1 1 d . . . H71 H 0.6799 0.8232 0.6786 0.016 Uiso 1 1 d R . . H72 H 0.7611 0.7621 0.7220 0.016 Uiso 1 1 d R . . H73 H 0.6932 0.6238 0.7132 0.016 Uiso 1 1 d R . . O1W O 0.0000 0.2626(2) 0.7500 0.0193(3) Uani 1 2 d S . . H1W H 0.0333 0.3379 0.7345 0.023 Uiso 1 1 d R . . 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 N1 0.0102(6) 0.0183(7) 0.0132(6) 0.0008(5) 0.0016(5) 0.0036(5) C2 0.0109(6) 0.0145(7) 0.0146(7) 0.0002(6) 0.0019(5) -0.0010(6) P3 0.01004(18) 0.00907(19) 0.01070(19) 0.00146(14) 0.00279(13) 0.00096(13) O31 0.0203(6) 0.0109(5) 0.0222(6) 0.0055(4) 0.0094(5) 0.0021(4) O32 0.0129(5) 0.0144(5) 0.0108(5) -0.0004(4) 0.0006(4) 0.0000(4) C4 0.0114(6) 0.0097(7) 0.0129(7) 0.0009(5) 0.0037(5) 0.0023(5) O41 0.0128(5) 0.0196(6) 0.0159(5) 0.0019(5) 0.0029(4) 0.0067(4) C41 0.0184(7) 0.0124(7) 0.0160(7) -0.0021(6) 0.0040(6) -0.0016(6) P5 0.00868(18) 0.00905(19) 0.00992(19) 0.00044(13) 0.00199(13) -0.00017(13) O51 0.0146(5) 0.0155(5) 0.0125(5) 0.0019(4) 0.0056(4) 0.0009(4) O52 0.0115(5) 0.0119(5) 0.0146(5) 0.0011(4) 0.0028(4) 0.0018(4) C6 0.0115(6) 0.0165(8) 0.0163(7) -0.0017(6) 0.0016(6) -0.0029(6) N7 0.0127(6) 0.0119(6) 0.0149(6) -0.0017(5) -0.0016(5) -0.0003(5) O1W 0.0241(8) 0.0112(7) 0.0271(9) 0.000 0.0160(7) 0.000 _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 N1 C2 1.484(2) . ? N1 H11 0.9027 . ? N1 H12 0.8820 . ? N1 H13 0.9724 . ? C2 P3 1.8293(15) . ? C2 H21 0.9900 . ? C2 H22 0.9900 . ? P3 O31 1.5049(11) . ? P3 O32 1.5121(11) . ? P3 C4 1.8463(15) . ? C4 O41 1.4364(17) . ? C4 C41 1.535(2) . ? C4 P5 1.8540(15) . ? O41 H41O 0.9038 . ? C41 H411 0.9800 . ? C41 H412 0.9800 . ? C41 H413 0.9800 . ? P5 O52 1.5024(11) . ? P5 O51 1.5106(11) . ? P5 C6 1.8211(16) . ? C6 N7 1.4899(19) . ? C6 H61 0.9900 . ? C6 H62 0.9900 . ? N7 H71 0.9296 . ? N7 H72 0.9026 . ? N7 H73 0.8888 . ? O1W H1W 0.8311 . ? 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 C2 N1 H11 111.9 . . ? C2 N1 H12 111.2 . . ? H11 N1 H12 109.4 . . ? C2 N1 H13 107.1 . . ? H11 N1 H13 107.3 . . ? H12 N1 H13 109.9 . . ? N1 C2 P3 114.43(10) . . ? N1 C2 H21 108.7 . . ? P3 C2 H21 108.7 . . ? N1 C2 H22 108.7 . . ? P3 C2 H22 108.7 . . ? H21 C2 H22 107.6 . . ? O31 P3 O32 116.70(7) . . ? O31 P3 C2 105.40(7) . . ? O32 P3 C2 109.29(7) . . ? O31 P3 C4 107.30(7) . . ? O32 P3 C4 108.89(6) . . ? C2 P3 C4 109.02(7) . . ? O41 C4 C41 111.56(12) . . ? O41 C4 P3 102.06(9) . . ? C41 C4 P3 110.82(10) . . ? O41 C4 P5 109.11(10) . . ? C41 C4 P5 108.79(10) . . ? P3 C4 P5 114.39(8) . . ? C4 O41 H41O 109.3 . . ? C4 C41 H411 109.5 . . ? C4 C41 H412 109.5 . . ? H411 C41 H412 109.5 . . ? C4 C41 H413 109.5 . . ? H411 C41 H413 109.5 . . ? H412 C41 H413 109.5 . . ? O52 P5 O51 116.51(6) . . ? O52 P5 C6 108.93(7) . . ? O51 P5 C6 105.78(7) . . ? O52 P5 C4 109.90(6) . . ? O51 P5 C4 107.50(6) . . ? C6 P5 C4 107.85(7) . . ? N7 C6 P5 113.55(10) . . ? N7 C6 H61 108.9 . . ? P5 C6 H61 108.9 . . ? N7 C6 H62 108.9 . . ? P5 C6 H62 108.9 . . ? H61 C6 H62 107.7 . . ? C6 N7 H71 115.3 . . ? C6 N7 H72 109.8 . . ? H71 N7 H72 106.0 . . ? C6 N7 H73 110.5 . . ? H71 N7 H73 108.3 . . ? H72 N7 H73 106.6 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.489 _refine_diff_density_min -0.262 _refine_diff_density_rms 0.058 data_bampin _database_code_depnum_ccdc_archive 'CCDC 898277' #TrackingRef 'bampin.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C3 H12 N2 O4 P2, H2 O' _chemical_formula_sum 'C3 H14 N2 O5 P2' _chemical_formula_weight 220.10 _chemical_compound_source 'synthesized by the authors' 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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbcn _symmetry_space_group_name_Hall '-P 2n 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y, -z+1/2' '-x+1/2, -y+1/2, z+1/2' '-x, -y, -z' '-x-1/2, y-1/2, z' 'x, -y, z-1/2' 'x-1/2, y-1/2, -z-1/2' _cell_length_a 11.5649(4) _cell_length_b 8.9009(3) _cell_length_c 8.3936(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 864.02(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150(1) _cell_measurement_reflns_used 3970 _cell_measurement_theta_min 3.5 _cell_measurement_theta_max 27.5 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.692 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 464 _exptl_absorpt_coefficient_mu 0.493 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7889 _exptl_absorpt_correction_T_max 0.9078 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(1) _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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5904 _diffrn_reflns_av_R_equivalents 0.0151 _diffrn_reflns_av_sigmaI/netI 0.0098 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.89 _diffrn_reflns_theta_max 27.47 _reflns_number_total 993 _reflns_number_gt 944 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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. ; _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^)+(0.0395P)^2^+0.4459P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 993 _refine_ls_number_parameters 56 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0246 _refine_ls_R_factor_gt 0.0232 _refine_ls_wR_factor_ref 0.0702 _refine_ls_wR_factor_gt 0.0690 _refine_ls_goodness_of_fit_ref 1.127 _refine_ls_restrained_S_all 1.127 _refine_ls_shift/su_max 0.000 _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 N1 N 0.64380(10) 0.11311(13) 0.36209(13) 0.0152(2) Uani 1 1 d . . . H11 H 0.5748 0.1369 0.4050 0.018 Uiso 1 1 d R . . H12 H 0.6380 0.0540 0.2843 0.018 Uiso 1 1 d R . . H13 H 0.6852 0.0743 0.4353 0.018 Uiso 1 1 d R . . C2 C 0.69706(11) 0.25527(14) 0.30678(16) 0.0147(3) Uani 1 1 d . . . H21 H 0.7753 0.2329 0.2651 0.018 Uiso 1 1 calc R . . H22 H 0.7063 0.3230 0.3994 0.018 Uiso 1 1 calc R . . P3 P 0.61570(3) 0.35363(4) 0.15329(3) 0.01007(13) Uani 1 1 d . . . O31 O 0.69866(8) 0.46735(10) 0.08574(11) 0.0161(2) Uani 1 1 d . . . O32 O 0.56423(8) 0.23700(10) 0.04358(10) 0.0154(2) Uani 1 1 d . . . C4 C 0.5000 0.45630(19) 0.2500 0.0112(3) Uani 1 2 d S . . H41 H 0.5357 0.5225 0.3310 0.013 Uiso 0.50 1 calc PR . . H42 H 0.4643 0.5225 0.1690 0.013 Uiso 0.50 1 calc PR . . O1W O 0.5000 0.12926(14) 0.7500 0.0213(3) Uani 1 2 d S . . H1W H 0.5136 0.1835 0.8204 0.026 Uiso 1 1 d R . . 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 N1 0.0178(5) 0.0123(5) 0.0155(5) 0.0008(4) -0.0074(4) 0.0001(4) C2 0.0121(6) 0.0151(6) 0.0168(6) 0.0013(5) -0.0032(5) -0.0006(4) P3 0.0095(2) 0.0118(2) 0.00890(19) 0.00003(10) 0.00107(10) 0.00053(11) O31 0.0147(4) 0.0158(4) 0.0177(5) 0.0011(4) 0.0066(3) -0.0008(3) O32 0.0172(5) 0.0171(4) 0.0119(4) -0.0036(3) -0.0016(3) 0.0004(4) C4 0.0108(7) 0.0107(7) 0.0122(7) 0.000 0.0018(6) 0.000 O1W 0.0343(8) 0.0134(6) 0.0161(6) 0.000 -0.0110(6) 0.000 _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 N1 C2 1.4818(16) . ? N1 H11 0.9005 . ? N1 H12 0.8413 . ? N1 H13 0.8525 . ? C2 P3 1.8198(13) . ? C2 H21 0.9900 . ? C2 H22 0.9900 . ? P3 O31 1.5055(9) . ? P3 O32 1.5100(9) . ? P3 C4 1.8123(9) . ? C4 P3 1.8123(9) 3_655 ? C4 H41 0.9900 . ? C4 H42 0.9900 . ? O1W H1W 0.7791 . ? 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 C2 N1 H11 107.0 . . ? C2 N1 H12 108.9 . . ? H11 N1 H12 112.8 . . ? C2 N1 H13 109.8 . . ? H11 N1 H13 107.8 . . ? H12 N1 H13 110.5 . . ? N1 C2 P3 114.69(8) . . ? N1 C2 H21 108.6 . . ? P3 C2 H21 108.6 . . ? N1 C2 H22 108.6 . . ? P3 C2 H22 108.6 . . ? H21 C2 H22 107.6 . . ? O31 P3 O32 118.93(5) . . ? O31 P3 C4 107.47(6) . . ? O32 P3 C4 109.19(5) . . ? O31 P3 C2 105.11(6) . . ? O32 P3 C2 107.75(6) . . ? C4 P3 C2 107.90(5) . . ? P3 C4 P3 119.44(9) 3_655 . ? P3 C4 H41 107.5 3_655 . ? P3 C4 H41 107.5 . . ? P3 C4 H42 107.5 3_655 . ? P3 C4 H42 107.5 . . ? H41 C4 H42 107.0 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.325 _refine_diff_density_min -0.368 _refine_diff_density_rms 0.059 data_cobisa _database_code_depnum_ccdc_archive 'CCDC 898278' #TrackingRef 'cobisa.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H42 Co4 Li2 N6 O20 P6, 13.5(H2 O) ' _chemical_formula_sum 'C12 H69 Co4 Li2 N6 O33.50 P6' _chemical_formula_weight 1269.15 _chemical_compound_source 'synthesized by the authors' 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' Li Li -0.0003 0.0001 '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+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, z+1/2' _cell_length_a 13.0426(3) _cell_length_b 13.2471(4) _cell_length_c 26.9972(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4664.5(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(1) _cell_measurement_reflns_used 186 _cell_measurement_theta_min 4.16 _cell_measurement_theta_max 24.50 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.56 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.807 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2620 _exptl_absorpt_coefficient_mu 1.706 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.4457 _exptl_absorpt_correction_T_max 0.7987 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(1) _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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30509 _diffrn_reflns_av_R_equivalents 0.0258 _diffrn_reflns_av_sigmaI/netI 0.0335 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 27.49 _reflns_number_total 10660 _reflns_number_gt 9956 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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. ; _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^)+(0.0369P)^2^+4.1094P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _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 0.000(8) _refine_ls_number_reflns 10660 _refine_ls_number_parameters 622 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0331 _refine_ls_R_factor_gt 0.0293 _refine_ls_wR_factor_ref 0.0737 _refine_ls_wR_factor_gt 0.0721 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _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 Co1 Co 0.02770(3) 0.29660(3) 0.868071(14) 0.01107(9) Uani 1 1 d . . . Co2 Co 0.19688(3) 0.32125(3) 0.785006(14) 0.00975(8) Uani 1 1 d . . . Co3 Co 0.14679(3) 0.50015(3) 0.856980(14) 0.01030(8) Uani 1 1 d . . . Co4 Co 0.26698(3) 0.30373(3) 0.897341(14) 0.01008(8) Uani 1 1 d . . . O1 O 0.07080(15) 0.39718(16) 0.81218(7) 0.0120(4) Uani 1 1 d . . . H11 H 0.0161 0.4237 0.7955 0.014 Uiso 1 1 d R . . N1A N -0.07754(18) 0.2121(2) 0.82568(10) 0.0156(5) Uani 1 1 d . . . H11A H -0.1321 0.1971 0.8460 0.019 Uiso 1 1 calc R . . H12A H -0.1020 0.2540 0.8012 0.019 Uiso 1 1 calc R . . C2A C -0.0459(2) 0.1170(3) 0.80161(11) 0.0155(6) Uani 1 1 d . . . H21A H -0.0961 0.1004 0.7753 0.019 Uiso 1 1 calc R . . H22A H -0.0482 0.0621 0.8265 0.019 Uiso 1 1 calc R . . P3A P 0.08149(6) 0.12006(6) 0.77432(3) 0.01135(15) Uani 1 1 d . . . O31A O 0.09692(16) 0.22007(17) 0.74712(8) 0.0145(4) Uani 1 1 d . . . O32A O 0.09351(17) 0.02601(17) 0.74376(8) 0.0162(5) Uani 1 1 d . . . C4A C 0.1730(2) 0.1251(2) 0.82684(11) 0.0104(6) Uani 1 1 d . . . O41A O 0.16515(15) 0.22490(15) 0.84778(7) 0.0099(4) Uani 1 1 d . . . C41A C 0.1509(2) 0.0400(2) 0.86403(11) 0.0149(6) Uani 1 1 d . . . H41A H 0.0780 0.0408 0.8729 0.018 Uiso 1 1 calc R . . H42A H 0.1923 0.0502 0.8939 0.018 Uiso 1 1 calc R . . H43A H 0.1682 -0.0252 0.8491 0.018 Uiso 1 1 calc R . . P5A P 0.30352(6) 0.11730(6) 0.80038(3) 0.01090(15) Uani 1 1 d . . . O51A O 0.31442(16) 0.21467(16) 0.77064(8) 0.0143(4) Uani 1 1 d . . . O52A O 0.31851(16) 0.01774(16) 0.77418(8) 0.0158(5) Uani 1 1 d . . . C6A C 0.3943(2) 0.1212(2) 0.85143(12) 0.0145(6) Uani 1 1 d . . . H61A H 0.3728 0.0721 0.8771 0.017 Uiso 1 1 calc R . . H62A H 0.4627 0.1006 0.8393 0.017 Uiso 1 1 calc R . . N7A N 0.40175(19) 0.22271(19) 0.87398(9) 0.0124(5) Uani 1 1 d . . . H71A H 0.4356 0.2632 0.8516 0.015 Uiso 1 1 calc R . . H72A H 0.4437 0.2169 0.9012 0.015 Uiso 1 1 calc R . . N1B N 0.2203(2) 0.41302(19) 0.72149(9) 0.0134(5) Uani 1 1 d . . . H11B H 0.2385 0.3705 0.6960 0.016 Uiso 1 1 calc R . . H12B H 0.1577 0.4402 0.7133 0.016 Uiso 1 1 calc R . . C2B C 0.2950(2) 0.4970(2) 0.72152(10) 0.0145(6) Uani 1 1 d . . . H21B H 0.2782 0.5436 0.6940 0.017 Uiso 1 1 calc R . . H22B H 0.3643 0.4693 0.7152 0.017 Uiso 1 1 calc R . . P3B P 0.29765(6) 0.56800(6) 0.77895(3) 0.01112(15) Uani 1 1 d . . . O31B O 0.18835(17) 0.58741(16) 0.79595(8) 0.0149(4) Uani 1 1 d . . . O32B O 0.36296(18) 0.66044(16) 0.77065(8) 0.0165(5) Uani 1 1 d . . . C4B C 0.3554(2) 0.4828(2) 0.82573(10) 0.0091(5) Uani 1 1 d . . . O41B O 0.27915(15) 0.40717(15) 0.83640(7) 0.0097(4) Uani 1 1 d . . . C41B C 0.4573(2) 0.4409(2) 0.80712(12) 0.0150(6) Uani 1 1 d . . . H41B H 0.4487 0.3699 0.7979 0.018 Uiso 1 1 calc R . . H42B H 0.5089 0.4464 0.8334 0.018 Uiso 1 1 calc R . . H43B H 0.4797 0.4796 0.7781 0.018 Uiso 1 1 calc R . . P5B P 0.36801(6) 0.55560(6) 0.88369(3) 0.01070(15) Uani 1 1 d . . . O51B O 0.25888(16) 0.57924(16) 0.89977(8) 0.0135(4) Uani 1 1 d . . . O52B O 0.43973(17) 0.64427(16) 0.87680(8) 0.0151(4) Uani 1 1 d . . . C6B C 0.4268(2) 0.4734(2) 0.92937(11) 0.0155(6) Uani 1 1 d . . . H61B H 0.4884 0.4416 0.9147 0.019 Uiso 1 1 calc R . . H62B H 0.4492 0.5144 0.9581 0.019 Uiso 1 1 calc R . . N7B N 0.3557(2) 0.3931(2) 0.94688(9) 0.0131(5) Uani 1 1 d . . . H71B H 0.3103 0.4235 0.9683 0.016 Uiso 1 1 calc R . . H72B H 0.3942 0.3490 0.9655 0.016 Uiso 1 1 calc R . . N1C N 0.0166(2) 0.5915(2) 0.86916(10) 0.0160(5) Uani 1 1 d . . . H11C H 0.0367 0.6576 0.8652 0.019 Uiso 1 1 calc R . . H12C H -0.0295 0.5777 0.8443 0.019 Uiso 1 1 calc R . . C2C C -0.0393(2) 0.5851(2) 0.91638(12) 0.0177(7) Uani 1 1 d . . . H21C H -0.1067 0.6186 0.9125 0.021 Uiso 1 1 calc R . . H22C H -0.0004 0.6223 0.9420 0.021 Uiso 1 1 calc R . . P3C P -0.05990(6) 0.45626(7) 0.93754(3) 0.01357(16) Uani 1 1 d . . . O31C O -0.09159(15) 0.39292(18) 0.89290(8) 0.0161(5) Uani 1 1 d . . . O32C O -0.13209(17) 0.46079(19) 0.98081(8) 0.0203(5) Uani 1 1 d . . . C4C C 0.0671(2) 0.4065(2) 0.95596(10) 0.0116(6) Uani 1 1 d . . . O41C O 0.12660(15) 0.39145(16) 0.91125(7) 0.0100(4) Uani 1 1 d . . . C41C C 0.1183(2) 0.4789(2) 0.99292(11) 0.0161(6) Uani 1 1 d . . . H41C H 0.1778 0.4457 1.0079 0.019 Uiso 1 1 calc R . . H42C H 0.0691 0.4970 1.0189 0.019 Uiso 1 1 calc R . . H43C H 0.1405 0.5400 0.9755 0.019 Uiso 1 1 calc R . . P5C P 0.04992(6) 0.27788(6) 0.98103(3) 0.01460(16) Uani 1 1 d . . . O51C O 0.01336(16) 0.21608(17) 0.93648(8) 0.0171(5) Uani 1 1 d . . . O52C O -0.0143(2) 0.2768(2) 1.02680(9) 0.0304(6) Uani 1 1 d . . . C6C C 0.1764(3) 0.2312(3) 0.99872(11) 0.0178(7) Uani 1 1 d . . . H61C H 0.2134 0.2852 1.0166 0.021 Uiso 1 1 calc R . . H62C H 0.1679 0.1737 1.0218 0.021 Uiso 1 1 calc R . . N7C N 0.23907(19) 0.1983(2) 0.95627(9) 0.0138(5) Uani 1 1 d . . . H71C H 0.2081 0.1423 0.9427 0.017 Uiso 1 1 calc R . . H72C H 0.3017 0.1778 0.9683 0.017 Uiso 1 1 calc R . . Li1 Li 0.2163(4) -0.0506(4) 0.7358(2) 0.0201(12) Uani 1 1 d . . . O1M O 0.25675(18) -0.07699(18) 0.66746(9) 0.0212(5) Uani 1 1 d . . . H11M H 0.2843 -0.0345 0.6563 0.025 Uiso 1 1 d R . . H12M H 0.2072 -0.0860 0.6493 0.025 Uiso 1 1 d R . . O2M O 0.1776(2) -0.18275(19) 0.76301(10) 0.0306(6) Uani 1 1 d . . . H21M H 0.1199 -0.1773 0.7824 0.037 Uiso 1 1 d R . . H22M H 0.2156 -0.2384 0.7723 0.037 Uiso 1 1 d R . . Li2 Li 0.4332(4) 0.7369(4) 0.8206(2) 0.0188(12) Uani 1 1 d . . . O3M O 0.3594(2) 0.85859(18) 0.84059(10) 0.0307(6) Uani 1 1 d . . . H31M H 0.2948 0.8512 0.8534 0.037 Uiso 1 1 d R . . H32M H 0.3473 0.9084 0.8198 0.037 Uiso 1 1 d R . . O4M O 0.5676(2) 0.7782(2) 0.80647(9) 0.0325(7) Uani 1 1 d . . . H41M H 0.6046 0.7584 0.7825 0.039 Uiso 1 1 d R . . H42M H 0.5968 0.8135 0.8268 0.039 Uiso 1 1 d R . . O1W O 0.62408(19) 0.24662(18) 0.82280(9) 0.0237(5) Uani 1 1 d . . . H11W H 0.6589 0.2956 0.8211 0.028 Uiso 1 1 d R . . H12W H 0.6277 0.2202 0.7942 0.028 Uiso 1 1 d R . . O2W O 0.2042(2) 0.2231(2) 0.65490(10) 0.0356(6) Uani 1 1 d . . . H21W H 0.1725 0.2221 0.6819 0.043 Uiso 1 1 d R . . H22W H 0.1740 0.2697 0.6380 0.043 Uiso 1 1 d R . . O3W O 0.3510(2) 0.0860(2) 0.62193(10) 0.0324(6) Uani 1 1 d . . . H31W H 0.3459 0.0653 0.5923 0.039 Uiso 1 1 d R . . H32W H 0.3070 0.1284 0.6320 0.039 Uiso 1 1 d R . . O4W O -0.0643(4) 0.3432(4) 0.53247(15) 0.0942(17) Uani 1 1 d . . . H41W H -0.0975 0.3212 0.5544 0.113 Uiso 1 1 d R . . H42W H -0.0546 0.3091 0.5076 0.113 Uiso 1 1 d R . . O5W O 0.0971(3) 0.3886(3) 0.59629(17) 0.0721(13) Uani 1 1 d . . . H51W H 0.0739 0.3578 0.5724 0.086 Uiso 1 1 d R . . H52W H 0.1308 0.4373 0.5948 0.086 Uiso 1 1 d R . . O6W O 0.3332(2) 0.0192(2) 0.52810(11) 0.0408(7) Uani 1 1 d . . . H61W H 0.3587 0.0601 0.5051 0.049 Uiso 1 1 d R . . H62W H 0.2703 -0.0100 0.5249 0.049 Uiso 1 1 d R . . O7W O 0.6553(4) 1.1149(3) 0.89612(12) 0.0727(13) Uani 1 1 d . . . H71W H 0.6976 1.1069 0.9134 0.087 Uiso 1 1 d R . . H72W H 0.6473 1.1537 0.8742 0.087 Uiso 1 1 d R . . O8W O 0.8540(3) 1.0828(3) 0.93049(15) 0.0643(11) Uani 1 1 d . . . H81W H 0.8365 1.0882 0.9029 0.077 Uiso 1 1 d R . . H82W H 0.9040 1.1236 0.9327 0.077 Uiso 1 1 d R . . O9W O 0.6565(4) 0.9003(4) 0.88427(17) 0.0401(12) Uani 0.70 1 d P A 1 O9X O 0.5937(9) 0.9131(8) 0.8884(4) 0.043(3) Uani 0.30 1 d P B 2 H91W H 0.6110 0.9726 0.8908 0.052 Uiso 1 1 d R . . H92W H 0.6376 0.8683 0.9080 0.052 Uiso 1 1 d R . . O10W O 0.3708(6) 0.9118(7) 0.9411(3) 0.049(2) Uani 0.60 1 d P C 1 O10X O 0.4150(7) 0.9308(10) 0.9343(4) 0.038(3) Uani 0.40 1 d P D 2 H10W H 0.3801 0.8967 0.9083 0.046 Uiso 1 1 d R D 1 H10X H 0.4059 0.8700 0.9570 0.046 Uiso 1 1 d R D 1 O11W O -0.0083(6) -0.1485(5) 0.8162(3) 0.0331(16) Uani 0.50 1 d P E 1 O11X O 0.0248(5) -0.1889(5) 0.8240(2) 0.0343(16) Uani 0.50 1 d P F 2 H11X H -0.0165 -0.1620 0.8479 0.041 Uiso 1 1 d R . . H11Y H -0.0204 -0.2169 0.8038 0.041 Uiso 1 1 d R . . O12W O 0.1820(5) 0.7661(4) 0.8924(2) 0.0548(16) Uani 0.60 1 d P . . O12X O 0.2181(6) 0.7519(5) 0.9541(3) 0.047(2) Uani 0.40 1 d P . . O13W O -0.0319(4) 0.2231(3) 0.44623(15) 0.0497(11) Uani 0.80 1 d P . . O13X O 0.0870(14) 0.2637(10) 0.4701(5) 0.039(4) Uani 0.20 1 d P . . O14W O 0.7305(7) 0.7858(7) 0.9460(4) 0.080(3) Uani 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 Co1 0.00886(17) 0.0153(2) 0.00904(18) -0.00191(16) 0.00040(14) -0.00098(16) Co2 0.01055(17) 0.01086(19) 0.00785(18) -0.00047(14) 0.00010(15) 0.00020(15) Co3 0.00995(17) 0.01327(19) 0.00766(17) 0.00057(16) 0.00014(14) 0.00169(16) Co4 0.00937(17) 0.0128(2) 0.00809(17) 0.00145(15) -0.00133(14) -0.00044(15) O1 0.0093(10) 0.0171(11) 0.0095(10) -0.0001(8) -0.0027(8) 0.0036(8) N1A 0.0080(11) 0.0198(14) 0.0190(13) -0.0038(11) 0.0004(10) -0.0017(10) C2A 0.0125(14) 0.0194(16) 0.0147(14) -0.0033(12) -0.0006(12) -0.0041(12) P3A 0.0114(3) 0.0131(4) 0.0095(3) -0.0014(3) -0.0027(3) -0.0004(3) O31A 0.0166(10) 0.0152(11) 0.0116(10) 0.0000(8) -0.0062(8) -0.0017(9) O32A 0.0163(11) 0.0167(12) 0.0157(11) -0.0065(9) -0.0036(9) 0.0005(9) C4A 0.0098(13) 0.0101(14) 0.0112(13) -0.0008(11) -0.0016(11) -0.0019(11) O41A 0.0096(9) 0.0107(10) 0.0094(9) -0.0026(8) -0.0005(8) -0.0013(8) C41A 0.0169(14) 0.0157(15) 0.0122(14) 0.0022(12) 0.0005(12) -0.0011(12) P5A 0.0100(3) 0.0112(4) 0.0115(3) -0.0012(3) -0.0003(3) 0.0010(3) O51A 0.0152(10) 0.0122(11) 0.0156(10) 0.0007(8) 0.0034(9) 0.0011(8) O52A 0.0165(11) 0.0141(11) 0.0166(11) -0.0050(9) -0.0033(9) 0.0019(8) C6A 0.0102(13) 0.0140(15) 0.0193(15) -0.0014(12) -0.0032(12) 0.0017(11) N7A 0.0135(12) 0.0142(13) 0.0096(11) -0.0014(9) -0.0024(10) -0.0008(10) N1B 0.0185(13) 0.0134(13) 0.0084(11) -0.0012(9) -0.0009(10) 0.0008(10) C2B 0.0201(15) 0.0149(14) 0.0085(13) 0.0004(12) 0.0014(12) -0.0030(13) P3B 0.0158(4) 0.0108(4) 0.0067(3) 0.0007(3) 0.0005(3) 0.0008(3) O31B 0.0168(11) 0.0174(11) 0.0104(10) 0.0018(8) 0.0004(9) 0.0047(9) O32B 0.0248(12) 0.0128(10) 0.0118(10) 0.0013(8) 0.0004(9) -0.0036(9) C4B 0.0078(12) 0.0080(13) 0.0115(13) 0.0004(10) 0.0016(11) 0.0002(11) O41B 0.0090(10) 0.0115(10) 0.0086(9) 0.0016(8) 0.0001(8) -0.0019(8) C41B 0.0116(14) 0.0146(15) 0.0189(15) 0.0015(12) 0.0047(12) 0.0038(12) P5B 0.0118(3) 0.0111(4) 0.0092(3) 0.0005(3) -0.0011(3) -0.0002(3) O51B 0.0132(10) 0.0164(11) 0.0107(10) -0.0015(8) 0.0010(9) 0.0010(8) O52B 0.0180(11) 0.0113(11) 0.0159(11) 0.0005(8) -0.0002(9) -0.0025(8) C6B 0.0153(15) 0.0165(16) 0.0147(15) 0.0043(12) -0.0025(12) -0.0036(12) N7B 0.0139(12) 0.0156(13) 0.0096(11) 0.0029(10) 0.0012(10) 0.0001(11) N1C 0.0147(12) 0.0172(14) 0.0162(13) 0.0029(10) 0.0019(11) 0.0051(10) C2C 0.0192(16) 0.0180(16) 0.0158(15) -0.0041(12) 0.0014(13) 0.0045(12) P3C 0.0092(3) 0.0202(4) 0.0113(4) -0.0030(3) 0.0015(3) 0.0010(3) O31C 0.0085(9) 0.0249(12) 0.0150(11) -0.0041(9) -0.0009(8) 0.0016(9) O32C 0.0146(11) 0.0303(13) 0.0159(11) -0.0051(10) 0.0062(9) -0.0013(10) C4C 0.0097(13) 0.0167(15) 0.0083(13) -0.0020(11) 0.0024(11) 0.0002(11) O41C 0.0093(9) 0.0147(10) 0.0059(9) -0.0004(8) 0.0014(8) 0.0005(8) C41C 0.0158(15) 0.0227(17) 0.0098(14) -0.0023(12) -0.0001(12) 0.0005(13) P5C 0.0168(4) 0.0172(4) 0.0098(3) 0.0015(3) 0.0053(3) -0.0008(3) O51C 0.0156(10) 0.0179(12) 0.0176(11) -0.0001(9) 0.0013(9) -0.0040(9) O52C 0.0422(15) 0.0283(14) 0.0207(13) 0.0066(11) 0.0218(12) 0.0043(12) C6C 0.0260(17) 0.0209(17) 0.0064(13) 0.0022(12) -0.0009(12) 0.0036(13) N7C 0.0134(12) 0.0156(13) 0.0122(12) 0.0024(10) -0.0011(10) -0.0008(11) Li1 0.023(3) 0.018(3) 0.019(3) -0.004(2) -0.002(2) 0.007(2) O1M 0.0198(11) 0.0237(13) 0.0200(11) -0.0010(9) -0.0074(10) 0.0004(10) O2M 0.0435(16) 0.0161(13) 0.0321(14) 0.0030(11) -0.0167(12) -0.0004(11) Li2 0.022(3) 0.021(3) 0.013(3) 0.004(2) 0.001(2) -0.006(2) O3M 0.0455(16) 0.0182(13) 0.0285(14) 0.0013(11) -0.0111(12) 0.0077(12) O4M 0.0341(14) 0.0437(17) 0.0197(12) -0.0112(12) 0.0106(11) -0.0179(13) O1W 0.0348(14) 0.0205(13) 0.0158(11) -0.0043(9) 0.0044(10) -0.0024(11) O2W 0.0392(15) 0.0393(16) 0.0283(14) 0.0002(12) 0.0025(12) 0.0020(13) O3W 0.0254(13) 0.0349(16) 0.0369(15) -0.0115(12) -0.0014(12) 0.0017(12) O4W 0.136(4) 0.095(3) 0.051(2) 0.034(2) 0.040(3) 0.048(3) O5W 0.048(2) 0.057(2) 0.111(3) 0.042(2) 0.016(2) 0.0085(18) O6W 0.0283(15) 0.053(2) 0.0409(17) 0.0034(15) -0.0018(13) -0.0119(13) O7W 0.138(4) 0.052(2) 0.0276(16) 0.0125(16) -0.033(2) -0.012(2) O8W 0.054(2) 0.054(2) 0.085(3) -0.020(2) 0.025(2) -0.0320(18) O9W 0.061(3) 0.038(3) 0.022(2) -0.0047(19) 0.006(2) -0.016(3) O9X 0.077(9) 0.015(5) 0.037(6) -0.008(4) -0.011(7) 0.008(6) O10W 0.062(5) 0.060(5) 0.026(3) -0.016(3) -0.014(4) 0.020(4) O10X 0.036(6) 0.056(6) 0.023(4) -0.007(4) -0.001(5) -0.009(5) O11W 0.041(4) 0.026(4) 0.032(4) -0.002(3) -0.012(3) 0.001(3) O11X 0.046(4) 0.036(4) 0.020(3) -0.005(3) -0.010(3) -0.021(3) O12W 0.066(4) 0.033(3) 0.065(4) 0.012(3) 0.029(3) 0.027(3) O12X 0.040(4) 0.022(4) 0.078(6) 0.000(4) -0.013(4) 0.001(3) O13W 0.070(3) 0.041(2) 0.038(2) 0.0073(18) 0.010(2) 0.000(2) O13X 0.085(12) 0.019(7) 0.012(6) -0.002(5) 0.011(7) 0.012(7) O14W 0.075(6) 0.074(6) 0.092(6) -0.015(5) 0.018(5) 0.003(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 Co1 O1 2.090(2) . ? Co1 O41A 2.101(2) . ? Co1 N1A 2.109(3) . ? Co1 O31C 2.121(2) . ? Co1 O51C 2.141(2) . ? Co1 O41C 2.145(2) . ? Co2 O1 2.062(2) . ? Co2 O41B 2.091(2) . ? Co2 O51A 2.120(2) . ? Co2 N1B 2.124(2) . ? Co2 O31A 2.131(2) . ? Co2 O41A 2.162(2) . ? Co3 O41C 2.071(2) . ? Co3 O1 2.075(2) . ? Co3 O31B 2.084(2) . ? Co3 N1C 2.111(3) . ? Co3 O51B 2.138(2) . ? Co3 O41B 2.192(2) . ? Co4 N7B 2.128(3) . ? Co4 O41B 2.147(2) . ? Co4 N7C 2.148(3) . ? Co4 N7A 2.154(3) . ? Co4 O41A 2.155(2) . ? Co4 O41C 2.201(2) . ? O1 H11 0.9146 . ? N1A C2A 1.476(4) . ? N1A H11A 0.9200 . ? N1A H12A 0.9200 . ? C2A P3A 1.818(3) . ? C2A H21A 0.9900 . ? C2A H22A 0.9900 . ? P3A O32A 1.503(2) . ? P3A O31A 1.528(2) . ? P3A C4A 1.855(3) . ? P3A Li1 3.047(5) . ? O32A Li1 1.908(6) . ? C4A O41A 1.442(3) . ? C4A C41A 1.536(4) . ? C4A P5A 1.849(3) . ? C41A H41A 0.9800 . ? C41A H42A 0.9800 . ? C41A H43A 0.9800 . ? P5A O52A 1.509(2) . ? P5A O51A 1.526(2) . ? P5A C6A 1.817(3) . ? P5A Li1 3.046(6) . ? O52A Li1 1.915(6) . ? C6A N7A 1.479(4) . ? C6A H61A 0.9900 . ? C6A H62A 0.9900 . ? N7A H71A 0.9200 . ? N7A H72A 0.9200 . ? N1B C2B 1.479(4) . ? N1B H11B 0.9200 . ? N1B H12B 0.9200 . ? C2B P3B 1.814(3) . ? C2B H21B 0.9900 . ? C2B H22B 0.9900 . ? P3B O32B 1.509(2) . ? P3B O31B 1.519(2) . ? P3B C4B 1.854(3) . ? P3B Li2 3.066(6) . ? O32B Li2 1.920(6) . ? C4B O41B 1.440(3) . ? C4B C41B 1.525(4) . ? C4B P5B 1.846(3) . ? C41B H41B 0.9800 . ? C41B H42B 0.9800 . ? C41B H43B 0.9800 . ? P5B O52B 1.513(2) . ? P5B O51B 1.521(2) . ? P5B C6B 1.815(3) . ? P5B Li2 3.064(5) . ? O52B Li2 1.953(6) . ? C6B N7B 1.488(4) . ? C6B H61B 0.9900 . ? C6B H62B 0.9900 . ? N7B H71B 0.9200 . ? N7B H72B 0.9200 . ? N1C C2C 1.471(4) . ? N1C H11C 0.9200 . ? N1C H12C 0.9200 . ? C2C P3C 1.819(3) . ? C2C H21C 0.9900 . ? C2C H22C 0.9900 . ? P3C O32C 1.502(2) . ? P3C O31C 1.525(2) . ? P3C C4C 1.851(3) . ? C4C O41C 1.449(3) . ? C4C C41C 1.536(4) . ? C4C P5C 1.847(3) . ? C41C H41C 0.9800 . ? C41C H42C 0.9800 . ? C41C H43C 0.9800 . ? P5C O52C 1.493(2) . ? P5C O51C 1.531(2) . ? P5C C6C 1.826(3) . ? C6C N7C 1.474(4) . ? C6C H61C 0.9900 . ? C6C H62C 0.9900 . ? N7C H71C 0.9200 . ? N7C H72C 0.9200 . ? Li1 O1M 1.951(6) . ? Li1 O2M 1.965(6) . ? Li1 H11M 2.3322 . ? O1M H11M 0.7329 . ? O1M H12M 0.8199 . ? O2M H21M 0.9186 . ? O2M H22M 0.9240 . ? Li2 O4M 1.875(6) . ? Li2 O3M 1.953(7) . ? O3M H31M 0.9156 . ? O3M H32M 0.8818 . ? O4M H41M 0.8497 . ? O4M H42M 0.8155 . ? O1W H11W 0.7935 . ? O1W H12W 0.8501 . ? O2W H21W 0.8394 . ? O2W H22W 0.8626 . ? O3W H31W 0.8478 . ? O3W H32W 0.8483 . ? O4W H41W 0.7894 . ? O4W H42W 0.8194 . ? O5W H51W 0.8204 . ? O5W H52W 0.7810 . ? O6W H61W 0.8887 . ? O6W H62W 0.9106 . ? O7W H71W 0.7286 . ? O7W H72W 0.7905 . ? O8W H81W 0.7815 . ? O8W H82W 0.8500 . ? O9W H91W 1.1407 . ? O9W H92W 0.8063 . ? O9X H91W 0.8220 . ? O9X H92W 0.9805 . ? O10W H10W 0.9151 . ? O10W H10X 0.8366 . ? O10X H10W 0.9512 . ? O10X H10X 1.0187 . ? O11W H11X 0.8818 . ? O11W H11Y 0.9786 . ? O11X H11X 0.9112 . ? O11X H11Y 0.8848 . ? O12W O12X 1.743(11) . ? O13W O13X 1.763(18) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Co1 O41A 82.56(8) . . ? O1 Co1 N1A 96.99(10) . . ? O41A Co1 N1A 100.01(9) . . ? O1 Co1 O31C 92.40(9) . . ? O41A Co1 O31C 168.56(8) . . ? N1A Co1 O31C 90.77(9) . . ? O1 Co1 O51C 164.57(8) . . ? O41A Co1 O51C 94.25(8) . . ? N1A Co1 O51C 98.44(10) . . ? O31C Co1 O51C 87.88(9) . . ? O1 Co1 O41C 81.79(8) . . ? O41A Co1 O41C 83.88(8) . . ? N1A Co1 O41C 175.77(9) . . ? O31C Co1 O41C 85.24(8) . . ? O51C Co1 O41C 82.85(8) . . ? O1 Co2 O41B 84.70(8) . . ? O1 Co2 O51A 165.12(8) . . ? O41B Co2 O51A 96.48(8) . . ? O1 Co2 N1B 97.05(9) . . ? O41B Co2 N1B 98.64(9) . . ? O51A Co2 N1B 97.43(9) . . ? O1 Co2 O31A 89.41(8) . . ? O41B Co2 O31A 167.09(8) . . ? O51A Co2 O31A 86.31(8) . . ? N1B Co2 O31A 93.47(9) . . ? O1 Co2 O41A 81.75(8) . . ? O41B Co2 O41A 84.22(8) . . ? O51A Co2 O41A 83.61(8) . . ? N1B Co2 O41A 176.80(9) . . ? O31A Co2 O41A 83.56(8) . . ? O41C Co3 O1 83.95(8) . . ? O41C Co3 O31B 167.91(8) . . ? O1 Co3 O31B 91.60(8) . . ? O41C Co3 N1C 100.73(9) . . ? O1 Co3 N1C 94.79(10) . . ? O31B Co3 N1C 90.82(9) . . ? O41C Co3 O51B 92.60(8) . . ? O1 Co3 O51B 164.54(8) . . ? O31B Co3 O51B 88.71(8) . . ? N1C Co3 O51B 100.65(10) . . ? O41C Co3 O41B 83.62(7) . . ? O1 Co3 O41B 81.90(8) . . ? O31B Co3 O41B 84.63(8) . . ? N1C Co3 O41B 174.28(9) . . ? O51B Co3 O41B 82.75(8) . . ? N7B Co4 O41B 94.95(9) . . ? N7B Co4 N7C 89.35(10) . . ? O41B Co4 N7C 174.28(9) . . ? N7B Co4 N7A 90.99(10) . . ? O41B Co4 N7A 91.91(9) . . ? N7C Co4 N7A 91.78(10) . . ? N7B Co4 O41A 174.15(9) . . ? O41B Co4 O41A 83.05(8) . . ? N7C Co4 O41A 92.30(9) . . ? N7A Co4 O41A 94.57(8) . . ? N7B Co4 O41C 92.96(9) . . ? O41B Co4 O41C 81.68(7) . . ? N7C Co4 O41C 94.36(9) . . ? N7A Co4 O41C 172.73(8) . . ? O41A Co4 O41C 81.32(7) . . ? Co2 O1 Co3 98.46(9) . . ? Co2 O1 Co1 99.22(9) . . ? Co3 O1 Co1 97.27(8) . . ? Co2 O1 H11 129.3 . . ? Co3 O1 H11 114.0 . . ? Co1 O1 H11 113.1 . . ? C2A N1A Co1 120.66(19) . . ? C2A N1A H11A 107.2 . . ? Co1 N1A H11A 107.2 . . ? C2A N1A H12A 107.2 . . ? Co1 N1A H12A 107.2 . . ? H11A N1A H12A 106.8 . . ? N1A C2A P3A 114.5(2) . . ? N1A C2A H21A 108.6 . . ? P3A C2A H21A 108.6 . . ? N1A C2A H22A 108.6 . . ? P3A C2A H22A 108.6 . . ? H21A C2A H22A 107.6 . . ? O32A P3A O31A 116.18(12) . . ? O32A P3A C2A 107.42(14) . . ? O31A P3A C2A 109.53(14) . . ? O32A P3A C4A 112.48(13) . . ? O31A P3A C4A 104.58(13) . . ? C2A P3A C4A 106.22(13) . . ? O32A P3A Li1 30.37(13) . . ? O31A P3A Li1 113.77(15) . . ? C2A P3A Li1 130.50(16) . . ? C4A P3A Li1 85.17(14) . . ? P3A O31A Co2 113.27(11) . . ? P3A O32A Li1 126.2(2) . . ? O41A C4A C41A 113.7(2) . . ? O41A C4A P5A 105.54(18) . . ? C41A C4A P5A 112.6(2) . . ? O41A C4A P3A 106.66(18) . . ? C41A C4A P3A 110.6(2) . . ? P5A C4A P3A 107.17(15) . . ? C4A O41A Co1 125.27(16) . . ? C4A O41A Co4 130.09(16) . . ? Co1 O41A Co4 98.33(8) . . ? C4A O41A Co2 102.74(15) . . ? Co1 O41A Co2 95.78(8) . . ? Co4 O41A Co2 94.74(8) . . ? C4A C41A H41A 109.5 . . ? C4A C41A H42A 109.5 . . ? H41A C41A H42A 109.5 . . ? C4A C41A H43A 109.5 . . ? H41A C41A H43A 109.5 . . ? H42A C41A H43A 109.5 . . ? O52A P5A O51A 118.69(12) . . ? O52A P5A C6A 107.21(13) . . ? O51A P5A C6A 108.32(14) . . ? O52A P5A C4A 110.42(13) . . ? O51A P5A C4A 104.01(13) . . ? C6A P5A C4A 107.75(14) . . ? O52A P5A Li1 30.92(13) . . ? O51A P5A Li1 110.54(14) . . ? C6A P5A Li1 134.26(15) . . ? C4A P5A Li1 85.30(14) . . ? P5A O51A Co2 113.53(12) . . ? P5A O52A Li1 125.2(2) . . ? N7A C6A P5A 112.4(2) . . ? N7A C6A H61A 109.1 . . ? P5A C6A H61A 109.1 . . ? N7A C6A H62A 109.1 . . ? P5A C6A H62A 109.1 . . ? H61A C6A H62A 107.9 . . ? C6A N7A Co4 121.30(19) . . ? C6A N7A H71A 107.0 . . ? Co4 N7A H71A 107.0 . . ? C6A N7A H72A 107.0 . . ? Co4 N7A H72A 107.0 . . ? H71A N7A H72A 106.7 . . ? C2B N1B Co2 121.68(18) . . ? C2B N1B H11B 106.9 . . ? Co2 N1B H11B 106.9 . . ? C2B N1B H12B 106.9 . . ? Co2 N1B H12B 106.9 . . ? H11B N1B H12B 106.7 . . ? N1B C2B P3B 113.75(19) . . ? N1B C2B H21B 108.8 . . ? P3B C2B H21B 108.8 . . ? N1B C2B H22B 108.8 . . ? P3B C2B H22B 108.8 . . ? H21B C2B H22B 107.7 . . ? O32B P3B O31B 115.93(13) . . ? O32B P3B C2B 107.72(13) . . ? O31B P3B C2B 109.17(13) . . ? O32B P3B C4B 111.49(13) . . ? O31B P3B C4B 106.16(12) . . ? C2B P3B C4B 105.92(14) . . ? O32B P3B Li2 30.28(13) . . ? O31B P3B Li2 107.86(14) . . ? C2B P3B Li2 134.66(14) . . ? C4B P3B Li2 87.72(14) . . ? P3B O31B Co3 112.89(12) . . ? P3B O32B Li2 126.4(2) . . ? O41B C4B C41B 114.5(2) . . ? O41B C4B P5B 104.80(18) . . ? C41B C4B P5B 113.1(2) . . ? O41B C4B P3B 106.22(18) . . ? C41B C4B P3B 110.5(2) . . ? P5B C4B P3B 107.19(14) . . ? C4B O41B Co2 126.88(16) . . ? C4B O41B Co4 130.39(16) . . ? Co2 O41B Co4 97.08(8) . . ? C4B O41B Co3 101.75(15) . . ? Co2 O41B Co3 94.01(8) . . ? Co4 O41B Co3 96.09(8) . . ? C4B C41B H41B 109.5 . . ? C4B C41B H42B 109.5 . . ? H41B C41B H42B 109.5 . . ? C4B C41B H43B 109.5 . . ? H41B C41B H43B 109.5 . . ? H42B C41B H43B 109.5 . . ? O52B P5B O51B 116.99(13) . . ? O52B P5B C6B 106.73(13) . . ? O51B P5B C6B 108.96(14) . . ? O52B P5B C4B 110.90(13) . . ? O51B P5B C4B 105.44(12) . . ? C6B P5B C4B 107.48(14) . . ? O52B P5B Li2 31.97(13) . . ? O51B P5B Li2 104.90(14) . . ? C6B P5B Li2 136.91(15) . . ? C4B P5B Li2 87.90(14) . . ? P5B O51B Co3 112.64(12) . . ? P5B O52B Li2 123.8(2) . . ? N7B C6B P5B 112.4(2) . . ? N7B C6B H61B 109.1 . . ? P5B C6B H61B 109.1 . . ? N7B C6B H62B 109.1 . . ? P5B C6B H62B 109.1 . . ? H61B C6B H62B 107.9 . . ? C6B N7B Co4 122.48(19) . . ? C6B N7B H71B 106.7 . . ? Co4 N7B H71B 106.7 . . ? C6B N7B H72B 106.7 . . ? Co4 N7B H72B 106.7 . . ? H71B N7B H72B 106.6 . . ? C2C N1C Co3 120.0(2) . . ? C2C N1C H11C 107.3 . . ? Co3 N1C H11C 107.3 . . ? C2C N1C H12C 107.3 . . ? Co3 N1C H12C 107.3 . . ? H11C N1C H12C 106.9 . . ? N1C C2C P3C 113.6(2) . . ? N1C C2C H21C 108.9 . . ? P3C C2C H21C 108.9 . . ? N1C C2C H22C 108.9 . . ? P3C C2C H22C 108.9 . . ? H21C C2C H22C 107.7 . . ? O32C P3C O31C 117.82(13) . . ? O32C P3C C2C 107.42(14) . . ? O31C P3C C2C 107.93(14) . . ? O32C P3C C4C 111.48(13) . . ? O31C P3C C4C 105.00(13) . . ? C2C P3C C4C 106.65(15) . . ? P3C O31C Co1 112.45(11) . . ? O41C C4C C41C 113.2(2) . . ? O41C C4C P5C 104.08(19) . . ? C41C C4C P5C 113.0(2) . . ? O41C C4C P3C 107.74(18) . . ? C41C C4C P3C 109.9(2) . . ? P5C C4C P3C 108.59(15) . . ? C4C O41C Co3 124.18(18) . . ? C4C O41C Co1 102.18(16) . . ? Co3 O41C Co1 95.69(8) . . ? C4C O41C Co4 131.34(17) . . ? Co3 O41C Co4 98.08(8) . . ? Co1 O41C Co4 95.64(8) . . ? C4C C41C H41C 109.5 . . ? C4C C41C H42C 109.5 . . ? H41C C41C H42C 109.5 . . ? C4C C41C H43C 109.5 . . ? H41C C41C H43C 109.5 . . ? H42C C41C H43C 109.5 . . ? O52C P5C O51C 118.07(15) . . ? O52C P5C C6C 106.67(15) . . ? O51C P5C C6C 107.80(14) . . ? O52C P5C C4C 112.35(15) . . ? O51C P5C C4C 104.07(13) . . ? C6C P5C C4C 107.40(15) . . ? P5C O51C Co1 112.58(12) . . ? N7C C6C P5C 113.5(2) . . ? N7C C6C H61C 108.9 . . ? P5C C6C H61C 108.9 . . ? N7C C6C H62C 108.9 . . ? P5C C6C H62C 108.9 . . ? H61C C6C H62C 107.7 . . ? C6C N7C Co4 118.5(2) . . ? C6C N7C H71C 107.7 . . ? Co4 N7C H71C 107.7 . . ? C6C N7C H72C 107.7 . . ? Co4 N7C H72C 107.7 . . ? H71C N7C H72C 107.1 . . ? O32A Li1 O52A 105.8(3) . . ? O32A Li1 O1M 115.4(3) . . ? O52A Li1 O1M 114.1(3) . . ? O32A Li1 O2M 102.5(3) . . ? O52A Li1 O2M 113.4(3) . . ? O1M Li1 O2M 105.3(3) . . ? O32A Li1 P5A 82.01(19) . . ? O52A Li1 P5A 23.89(10) . . ? O1M Li1 P5A 124.9(3) . . ? O2M Li1 P5A 122.2(2) . . ? O32A Li1 P3A 23.46(10) . . ? O52A Li1 P3A 82.33(19) . . ? O1M Li1 P3A 127.7(3) . . ? O2M Li1 P3A 112.7(2) . . ? P5A Li1 P3A 58.57(10) . . ? O32A Li1 H11M 112.0 . . ? O52A Li1 H11M 101.0 . . ? O1M Li1 H11M 16.9 . . ? O2M Li1 H11M 121.5 . . ? P5A Li1 H11M 108.6 . . ? P3A Li1 H11M 117.8 . . ? Li1 O1M H11M 112.6 . . ? Li1 O1M H12M 112.2 . . ? H11M O1M H12M 104.7 . . ? Li1 O2M H21M 110.7 . . ? Li1 O2M H22M 132.5 . . ? H21M O2M H22M 110.3 . . ? O4M Li2 O32B 117.2(3) . . ? O4M Li2 O52B 107.5(3) . . ? O32B Li2 O52B 103.6(3) . . ? O4M Li2 O3M 106.0(3) . . ? O32B Li2 O3M 113.2(3) . . ? O52B Li2 O3M 109.0(3) . . ? O4M Li2 P5B 127.0(3) . . ? O32B Li2 P5B 81.06(19) . . ? O52B Li2 P5B 24.22(10) . . ? O3M Li2 P5B 110.9(2) . . ? O4M Li2 P3B 132.6(3) . . ? O32B Li2 P3B 23.34(10) . . ? O52B Li2 P3B 81.46(19) . . ? O3M Li2 P3B 114.8(2) . . ? P5B Li2 P3B 58.12(10) . . ? Li2 O3M H31M 118.0 . . ? Li2 O3M H32M 122.0 . . ? H31M O3M H32M 99.0 . . ? Li2 O4M H41M 126.6 . . ? Li2 O4M H42M 117.8 . . ? H41M O4M H42M 115.1 . . ? H11W O1W H12W 104.7 . . ? H21W O2W H22W 104.3 . . ? H31W O3W H32W 117.6 . . ? H41W O4W H42W 119.8 . . ? H51W O5W H52W 125.3 . . ? H61W O6W H62W 121.9 . . ? H71W O7W H72W 132.2 . . ? H81W O8W H82W 103.3 . . ? H91W O9W H92W 99.1 . . ? H91W O9X H92W 112.1 . . ? H10W O10W H10X 106.2 . . ? H10W O10X H10X 90.7 . . ? H11X O11W H11Y 97.1 . . ? H11X O11X H11Y 102.0 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.839 _refine_diff_density_min -0.517 _refine_diff_density_rms 0.077 data_cubisampinph _database_code_depnum_ccdc_archive 'CCDC 898279' #TrackingRef 'cubisampinph.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H26 Cu2 N4 O10 P4, C O3, 4(C H6 N3), 10(H2 O)' _chemical_formula_sum 'C23 H70 Cu2 N16 O23 P4' _chemical_formula_weight 1189.91 _chemical_compound_source 'synthesized by the authors' 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P 1' _symmetry_space_group_name_Hall 'P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 14.1333(4) _cell_length_b 14.2073(4) _cell_length_c 14.4339(4) _cell_angle_alpha 69.8750(10) _cell_angle_beta 76.6460(10) _cell_angle_gamma 65.3910(10) _cell_volume 2461.05(12) _cell_formula_units_Z 2 _cell_measurement_temperature 150(1) _cell_measurement_reflns_used 9729 _cell_measurement_theta_min 2.7 _cell_measurement_theta_max 27.5 _exptl_crystal_description plate _exptl_crystal_colour 'brownish green' _exptl_crystal_size_max 0.69 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.606 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1244 _exptl_absorpt_coefficient_mu 1.086 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5193 _exptl_absorpt_correction_T_max 0.8807 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(1) _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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 68119 _diffrn_reflns_av_R_equivalents 0.0201 _diffrn_reflns_av_sigmaI/netI 0.0229 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 27.50 _reflns_number_total 22429 _reflns_number_gt 21349 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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. ; _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^)+(0.0321P)^2^+1.1003P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _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 0.00(4) _refine_ls_number_reflns 22429 _refine_ls_number_parameters 1226 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0262 _refine_ls_R_factor_gt 0.0237 _refine_ls_wR_factor_ref 0.0618 _refine_ls_wR_factor_gt 0.0604 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _refine_ls_shift/su_max 0.003 _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 Cu1 Cu 0.133497(19) 0.768998(19) 0.997880(18) 0.01214(5) Uani 1 1 d . . . Cu2 Cu 0.023018(19) 0.95918(2) 0.832745(18) 0.01260(5) Uani 1 1 d . . . N1A N 0.28701(15) 0.69874(15) 1.01166(14) 0.0147(4) Uani 1 1 d . . . H11A H 0.3153 0.7512 0.9924 0.018 Uiso 1 1 calc R . . H12A H 0.2968 0.6628 1.0773 0.018 Uiso 1 1 calc R . . C2A C 0.34331(18) 0.62119(18) 0.95116(17) 0.0154(4) Uani 1 1 d . . . H21A H 0.3451 0.5483 0.9911 0.018 Uiso 1 1 calc R . . H22A H 0.4163 0.6178 0.9314 0.018 Uiso 1 1 calc R . . P3A P 0.27761(5) 0.66375(4) 0.84132(4) 0.01373(11) Uani 1 1 d . . . O31A O 0.17303(14) 0.65127(14) 0.87649(14) 0.0249(4) Uani 1 1 d . . . O32A O 0.35053(15) 0.60415(14) 0.76951(14) 0.0241(4) Uani 1 1 d . . . C4A C 0.24683(17) 0.81219(17) 0.79631(16) 0.0119(4) Uani 1 1 d . . . O41A O 0.16208(12) 0.85909(12) 0.86278(11) 0.0127(3) Uani 1 1 d . . . C41A C 0.34126(17) 0.83900(18) 0.79369(16) 0.0133(4) Uani 1 1 d . . . C42A C 0.3320(2) 0.91559(19) 0.83929(18) 0.0195(5) Uani 1 1 d . . . H42A H 0.2668 0.9507 0.8722 0.023 Uiso 1 1 calc R . . C43A C 0.4186(2) 0.9400(2) 0.8362(2) 0.0279(6) Uani 1 1 d . . . H43A H 0.4122 0.9913 0.8677 0.034 Uiso 1 1 calc R . . C44A C 0.5142(2) 0.8903(2) 0.7876(2) 0.0263(6) Uani 1 1 d . . . H44A H 0.5729 0.9074 0.7859 0.032 Uiso 1 1 calc R . . C45A C 0.5232(2) 0.8157(2) 0.74184(19) 0.0231(5) Uani 1 1 d . . . H45A H 0.5883 0.7818 0.7079 0.028 Uiso 1 1 calc R . . C46A C 0.43798(18) 0.7903(2) 0.74518(17) 0.0175(5) Uani 1 1 d . . . H46A H 0.4455 0.7385 0.7137 0.021 Uiso 1 1 calc R . . P5A P 0.19829(4) 0.86666(4) 0.67209(4) 0.01211(11) Uani 1 1 d . . . O51A O 0.10092(13) 0.84345(13) 0.68254(12) 0.0163(3) Uani 1 1 d . . . O52A O 0.28466(13) 0.82913(13) 0.59394(12) 0.0166(3) Uani 1 1 d . . . C6A C 0.15939(18) 1.01120(18) 0.64934(17) 0.0154(4) Uani 1 1 d . . . H61A H 0.2106 1.0256 0.6737 0.019 Uiso 1 1 calc R . . H62A H 0.1585 1.0469 0.5772 0.019 Uiso 1 1 calc R . . N7A N 0.05396(15) 1.05573(15) 0.70079(14) 0.0152(4) Uani 1 1 d . . . H71A H 0.0048 1.0713 0.6602 0.018 Uiso 1 1 calc R . . H72A H 0.0466 1.1196 0.7097 0.018 Uiso 1 1 calc R . . N1B N -0.12975(15) 1.02512(16) 0.82072(14) 0.0145(4) Uani 1 1 d . . . H11B H -0.1407 1.0572 0.7549 0.017 Uiso 1 1 calc R . . H12B H -0.1573 0.9719 0.8444 0.017 Uiso 1 1 calc R . . C2B C -0.18437(19) 1.10639(19) 0.87621(17) 0.0178(5) Uani 1 1 d . . . H21B H -0.2587 1.1139 0.8940 0.021 Uiso 1 1 calc R . . H22B H -0.1820 1.1772 0.8341 0.021 Uiso 1 1 calc R . . P3B P -0.12208(5) 1.06543(5) 0.98892(4) 0.01527(12) Uani 1 1 d . . . O31B O -0.01883(16) 1.07881(16) 0.95940(15) 0.0338(5) Uani 1 1 d . . . O32B O -0.19986(16) 1.12498(14) 1.05949(13) 0.0261(4) Uani 1 1 d . . . C4B C -0.09248(17) 0.91671(17) 1.03317(16) 0.0120(4) Uani 1 1 d . . . O41B O -0.00523(12) 0.87052(13) 0.96825(11) 0.0147(3) Uani 1 1 d . . . C41B C -0.18406(17) 0.88504(17) 1.03587(16) 0.0129(4) Uani 1 1 d . . . C42B C -0.1698(2) 0.8027(2) 0.99726(19) 0.0209(5) Uani 1 1 d . . . H42B H -0.1033 0.7685 0.9656 0.025 Uiso 1 1 calc R . . C43B C -0.2515(2) 0.7691(2) 1.0041(2) 0.0270(6) Uani 1 1 d . . . H43B H -0.2404 0.7123 0.9776 0.032 Uiso 1 1 calc R . . C44B C -0.3489(2) 0.8189(2) 1.04969(19) 0.0275(6) Uani 1 1 d . . . H44B H -0.4050 0.7966 1.0544 0.033 Uiso 1 1 calc R . . C45B C -0.3641(2) 0.9012(2) 1.08822(19) 0.0245(5) Uani 1 1 d . . . H45B H -0.4309 0.9352 1.1197 0.029 Uiso 1 1 calc R . . C46B C -0.28301(18) 0.93476(19) 1.08155(17) 0.0169(5) Uani 1 1 d . . . H46B H -0.2946 0.9917 1.1081 0.020 Uiso 1 1 calc R . . P5B P -0.04998(4) 0.86225(5) 1.16063(4) 0.01229(11) Uani 1 1 d . . . O51B O 0.04171(13) 0.89104(14) 1.15825(12) 0.0187(3) Uani 1 1 d . . . O52B O -0.14131(13) 0.89370(14) 1.23680(12) 0.0167(3) Uani 1 1 d . . . C6B C -0.00576(18) 0.71753(18) 1.18323(17) 0.0162(5) Uani 1 1 d . . . H61B H -0.0006 0.6821 1.2551 0.019 Uiso 1 1 calc R . . H62B H -0.0580 0.7005 1.1633 0.019 Uiso 1 1 calc R . . N7B N 0.09754(15) 0.67361(15) 1.12772(14) 0.0151(4) Uani 1 1 d . . . H71B H 0.1013 0.6121 1.1165 0.018 Uiso 1 1 calc R . . H72B H 0.1484 0.6531 1.1682 0.018 Uiso 1 1 calc R . . Cu3 Cu 0.508931(19) 0.294749(19) 0.402894(18) 0.01194(5) Uani 1 1 d . . . Cu4 Cu 0.631432(19) 0.410547(19) 0.437279(18) 0.01260(6) Uani 1 1 d . . . N1C N 0.46505(16) 0.29402(15) 0.27877(14) 0.0165(4) Uani 1 1 d . . . H11C H 0.5244 0.2642 0.2400 0.020 Uiso 1 1 calc R . . H12C H 0.4273 0.2499 0.2973 0.020 Uiso 1 1 calc R . . C2C C 0.40147(19) 0.40133(18) 0.21723(17) 0.0158(4) Uani 1 1 d . . . H21C H 0.3362 0.3988 0.2059 0.019 Uiso 1 1 calc R . . H22C H 0.4412 0.4197 0.1519 0.019 Uiso 1 1 calc R . . P3C P 0.36958(4) 0.50427(4) 0.27979(4) 0.01053(10) Uani 1 1 d . . . O31C O 0.33812(13) 0.45607(13) 0.38706(12) 0.0152(3) Uani 1 1 d . . . O32C O 0.29184(12) 0.60918(12) 0.22512(12) 0.0148(3) Uani 1 1 d . . . C4C C 0.49888(17) 0.51304(17) 0.27267(15) 0.0107(4) Uani 1 1 d . . . O41C O 0.56084(12) 0.41176(11) 0.33310(11) 0.0112(3) Uani 1 1 d . . . C41C C 0.54906(17) 0.53470(18) 0.16505(16) 0.0123(4) Uani 1 1 d . . . C42C C 0.63768(18) 0.45468(19) 0.13553(18) 0.0183(5) Uani 1 1 d . . . H42C H 0.6659 0.3864 0.1819 0.022 Uiso 1 1 calc R . . C43C C 0.6850(2) 0.4740(2) 0.03881(19) 0.0241(5) Uani 1 1 d . . . H43C H 0.7463 0.4194 0.0199 0.029 Uiso 1 1 calc R . . C44C C 0.6437(2) 0.5717(2) -0.02990(18) 0.0227(5) Uani 1 1 d . . . H44C H 0.6756 0.5841 -0.0963 0.027 Uiso 1 1 calc R . . C45C C 0.5556(2) 0.6515(2) -0.00186(18) 0.0197(5) Uani 1 1 d . . . H45C H 0.5266 0.7189 -0.0491 0.024 Uiso 1 1 calc R . . C46C C 0.50924(18) 0.63349(18) 0.09574(17) 0.0145(4) Uani 1 1 d . . . H46C H 0.4498 0.6894 0.1149 0.017 Uiso 1 1 calc R . . P5C P 0.48833(4) 0.61967(4) 0.32656(4) 0.01109(11) Uani 1 1 d . . . O51C O 0.47614(12) 0.57277(12) 0.43811(11) 0.0138(3) Uani 1 1 d . . . O52C O 0.40906(12) 0.72826(13) 0.28157(12) 0.0163(3) Uani 1 1 d . . . C6C C 0.61974(17) 0.62270(18) 0.29724(18) 0.0160(4) Uani 1 1 d . . . H61C H 0.6346 0.6505 0.2247 0.019 Uiso 1 1 calc R . . H62C H 0.6256 0.6709 0.3296 0.019 Uiso 1 1 calc R . . N7C N 0.69573(15) 0.51142(15) 0.33350(15) 0.0152(4) Uani 1 1 d . . . H71C H 0.7475 0.5144 0.3599 0.018 Uiso 1 1 calc R . . H72C H 0.7266 0.4834 0.2804 0.018 Uiso 1 1 calc R . . N1D N 0.67413(19) 0.41501(17) 0.55977(17) 0.0245(5) Uani 1 1 d . . . H11D H 0.7125 0.4586 0.5402 0.029 Uiso 1 1 calc R . . H12D H 0.6146 0.4464 0.5975 0.029 Uiso 1 1 calc R . . C2D C 0.73661(18) 0.30819(18) 0.62330(17) 0.0159(4) Uani 1 1 d . . . H21D H 0.6949 0.2898 0.6873 0.019 Uiso 1 1 calc R . . H22D H 0.8004 0.3115 0.6372 0.019 Uiso 1 1 calc R . . P3D P 0.77317(4) 0.20492(4) 0.56029(4) 0.01142(11) Uani 1 1 d . . . O31D O 0.80564(13) 0.25444(13) 0.45343(12) 0.0160(3) Uani 1 1 d . . . O32D O 0.85168(12) 0.10125(13) 0.61493(12) 0.0153(3) Uani 1 1 d . . . C4D C 0.64562(16) 0.19206(17) 0.56638(16) 0.0110(4) Uani 1 1 d . . . O41D O 0.58097(12) 0.29213(12) 0.50645(11) 0.0117(3) Uani 1 1 d . . . C41D C 0.59764(17) 0.16885(18) 0.67359(16) 0.0128(4) Uani 1 1 d . . . C42D C 0.50259(19) 0.24250(19) 0.70277(18) 0.0191(5) Uani 1 1 d . . . H42D H 0.4675 0.3071 0.6553 0.023 Uiso 1 1 calc R . . C43D C 0.4589(2) 0.2219(2) 0.80097(19) 0.0249(5) Uani 1 1 d . . . H43D H 0.3935 0.2721 0.8196 0.030 Uiso 1 1 calc R . . C44D C 0.5093(2) 0.1296(2) 0.87158(18) 0.0222(5) Uani 1 1 d . . . H44D H 0.4797 0.1166 0.9388 0.027 Uiso 1 1 calc R . . C45D C 0.6037(2) 0.0560(2) 0.84291(18) 0.0189(5) Uani 1 1 d . . . H45D H 0.6392 -0.0076 0.8910 0.023 Uiso 1 1 calc R . . C46D C 0.64701(18) 0.07425(18) 0.74507(16) 0.0138(4) Uani 1 1 d . . . H46D H 0.7107 0.0221 0.7264 0.017 Uiso 1 1 calc R . . P5D P 0.65851(4) 0.08579(4) 0.51149(4) 0.01172(11) Uani 1 1 d . . . O51D O 0.67247(13) 0.13181(13) 0.40040(12) 0.0155(3) Uani 1 1 d . . . O52D O 0.73787(13) -0.02301(13) 0.55651(12) 0.0167(3) Uani 1 1 d . . . C6D C 0.52878(18) 0.07866(18) 0.54065(17) 0.0152(4) Uani 1 1 d . . . H61D H 0.5270 0.0253 0.5121 0.018 Uiso 1 1 calc R . . H62D H 0.5129 0.0546 0.6135 0.018 Uiso 1 1 calc R . . N7D N 0.44834(15) 0.18665(15) 0.49944(14) 0.0167(4) Uani 1 1 d . . . H71D H 0.4090 0.2141 0.5511 0.020 Uiso 1 1 calc R . . H72D H 0.4042 0.1780 0.4678 0.020 Uiso 1 1 calc R . . C1E C 0.98388(18) 0.97847(18) 0.38593(18) 0.0164(5) Uani 1 1 d . . . N1E N 1.04837(16) 0.98460(17) 0.30306(15) 0.0198(4) Uani 1 1 d . . . H11E H 1.0982 1.0062 0.2889 0.024 Uiso 1 1 d R . . H12E H 1.0393 0.9568 0.2588 0.024 Uiso 1 1 d R . . N2E N 0.91292(16) 0.93564(17) 0.39914(15) 0.0192(4) Uani 1 1 d . . . H21E H 0.9054 0.9233 0.3524 0.023 Uiso 1 1 d R . . H22E H 0.8603 0.9519 0.4434 0.023 Uiso 1 1 d R . . N3E N 0.99359(17) 1.01315(16) 0.45704(15) 0.0206(4) Uani 1 1 d . . . H31E H 0.9404 1.0342 0.4985 0.025 Uiso 1 1 d R . . H32E H 1.0301 1.0531 0.4278 0.025 Uiso 1 1 d R . . C1F C 0.16347(18) 0.72904(18) 0.46167(18) 0.0165(5) Uani 1 1 d . . . N1F N 0.10278(17) 0.73010(18) 0.54640(16) 0.0219(4) Uani 1 1 d . . . H11F H 0.0570 0.6997 0.5573 0.026 Uiso 1 1 d R . . H12F H 0.1060 0.7656 0.5839 0.026 Uiso 1 1 d R . . N2F N 0.23476(16) 0.77356(17) 0.43777(16) 0.0203(4) Uani 1 1 d . . . H21F H 0.2454 0.7966 0.4849 0.024 Uiso 1 1 d R . . H22F H 0.2863 0.7689 0.3926 0.024 Uiso 1 1 d R . . N3F N 0.14962(17) 0.68592(17) 0.39974(16) 0.0229(4) Uani 1 1 d . . . H31F H 0.1954 0.6779 0.3491 0.028 Uiso 1 1 d R . . H32F H 0.1029 0.6573 0.4159 0.028 Uiso 1 1 d R . . C1G C 0.8710(2) 0.2328(2) 0.19477(18) 0.0197(5) Uani 1 1 d . . . N1G N 0.92122(18) 0.24303(18) 0.10303(16) 0.0247(5) Uani 1 1 d . . . H11G H 0.9615 0.2844 0.0822 0.030 Uiso 1 1 d R . . H12G H 0.9123 0.1990 0.0676 0.030 Uiso 1 1 d R . . N2G N 0.81149(17) 0.17547(17) 0.22602(16) 0.0219(4) Uani 1 1 d . . . H21G H 0.8014 0.1549 0.1852 0.026 Uiso 1 1 d R . . H22G H 0.7778 0.1757 0.2820 0.026 Uiso 1 1 d R . . N3G N 0.88148(19) 0.28295(18) 0.25284(16) 0.0255(5) Uani 1 1 d . . . H31G H 0.8552 0.2760 0.3063 0.031 Uiso 1 1 d R . . H32G H 0.9239 0.3244 0.2291 0.031 Uiso 1 1 d R . . C1H C 0.28029(19) 0.4818(2) 0.64638(18) 0.0181(5) Uani 1 1 d . . . N1H N 0.26891(18) 0.42864(18) 0.59309(16) 0.0228(5) Uani 1 1 d . . . H11H H 0.2954 0.4396 0.5268 0.027 Uiso 1 1 d R . . H12H H 0.2421 0.3832 0.6186 0.027 Uiso 1 1 d R . . N2H N 0.23677(18) 0.47284(18) 0.73984(16) 0.0247(5) Uani 1 1 d . . . H21H H 0.1950 0.4319 0.7618 0.030 Uiso 1 1 d R . . H22H H 0.2387 0.5179 0.7674 0.030 Uiso 1 1 d R . . N3H N 0.33494(17) 0.54435(17) 0.60764(16) 0.0212(4) Uani 1 1 d . . . H31H H 0.3457 0.5780 0.6452 0.025 Uiso 1 1 d R . . H32H H 0.3746 0.5399 0.5495 0.025 Uiso 1 1 d R . . C1I C 0.25639(16) 0.94130(18) 0.12771(16) 0.0159(4) Uani 1 1 d . . . N1I N 0.25116(15) 0.84476(15) 0.14769(15) 0.0179(4) Uani 1 1 d . . . H11I H 0.2969 0.7993 0.1883 0.021 Uiso 1 1 d R . . H12I H 0.1937 0.8426 0.1525 0.021 Uiso 1 1 d R . . N2I N 0.18272(15) 1.02881(15) 0.07964(15) 0.0204(4) Uani 1 1 d . . . H21I H 0.1261 1.0215 0.0668 0.024 Uiso 1 1 d R . . H22I H 0.1817 1.0949 0.0744 0.024 Uiso 1 1 d R . . N3I N 0.33704(15) 0.94899(15) 0.15315(15) 0.0221(4) Uani 1 1 d . . . H31I H 0.3456 1.0060 0.1432 0.026 Uiso 1 1 d R . . H32I H 0.3804 0.8884 0.1954 0.026 Uiso 1 1 d R . . C1J C 0.45455(17) 0.93987(17) 0.37414(16) 0.0185(4) Uani 1 1 d . . . N1J N 0.35817(15) 0.94317(16) 0.40611(14) 0.0223(4) Uani 1 1 d . . . H11J H 0.3415 0.9057 0.4657 0.027 Uiso 1 1 d R . . H12J H 0.3169 0.9832 0.3760 0.027 Uiso 1 1 d R . . N2J N 0.47450(15) 1.00783(17) 0.28987(15) 0.0244(4) Uani 1 1 d . . . H21J H 0.4231 1.0617 0.2499 0.029 Uiso 1 1 d R . . H22J H 0.5330 1.0165 0.2785 0.029 Uiso 1 1 d R . . N3J N 0.53285(15) 0.86818(17) 0.42820(15) 0.0243(4) Uani 1 1 d . . . H31J H 0.6018 0.8605 0.4010 0.029 Uiso 1 1 d R . . H32J H 0.5232 0.8189 0.4720 0.029 Uiso 1 1 d R . . C1K C 0.54686(19) 0.29594(19) 0.98849(18) 0.0249(5) Uani 1 1 d . . . N1K N 0.54591(17) 0.21673(17) 1.07180(17) 0.0280(5) Uani 1 1 d . . . H11K H 0.6127 0.1712 1.0908 0.034 Uiso 1 1 d R . . H12K H 0.4935 0.1961 1.0858 0.034 Uiso 1 1 d R . . N2K N 0.45881(17) 0.35751(16) 0.94662(16) 0.0274(4) Uani 1 1 d . . . H21K H 0.4044 0.3408 0.9717 0.033 Uiso 1 1 d R . . H22K H 0.4552 0.4141 0.8772 0.033 Uiso 1 1 d R . . N3K N 0.63345(18) 0.3153(2) 0.9494(2) 0.0376(6) Uani 1 1 d . . . H31K H 0.6402 0.3635 0.8923 0.045 Uiso 1 1 d R . . H32K H 0.6832 0.2792 0.9850 0.045 Uiso 1 1 d R . . C1L C 0.91105(18) 0.7427(2) 0.74905(18) 0.0204(5) Uani 1 1 d . . . N1L N 0.90118(16) 0.84233(17) 0.69500(16) 0.0234(4) Uani 1 1 d . . . H11L H 0.8510 0.8786 0.6621 0.028 Uiso 1 1 d R . . H12L H 0.9578 0.8609 0.6929 0.028 Uiso 1 1 d R . . N2L N 0.98958(16) 0.68236(17) 0.80360(16) 0.0250(4) Uani 1 1 d . . . H21L H 1.0362 0.7077 0.7863 0.030 Uiso 1 1 d R . . H22L H 0.9926 0.6125 0.8328 0.030 Uiso 1 1 d R . . N3L N 0.83993(17) 0.70169(19) 0.75217(17) 0.0322(5) Uani 1 1 d . . . H31L H 0.8574 0.6255 0.7867 0.039 Uiso 1 1 d R . . H32L H 0.7980 0.7377 0.7036 0.039 Uiso 1 1 d R . . C1M C 0.28672(19) 0.21897(18) 0.08709(16) 0.0223(5) Uani 1 1 d . . . O1M O 0.20003(13) 0.20158(13) 0.12076(13) 0.0275(4) Uani 1 1 d . . . O2M O 0.28371(15) 0.30344(15) 0.01624(14) 0.0343(4) Uani 1 1 d . . . O3M O 0.37142(14) 0.14945(14) 0.12152(13) 0.0284(4) Uani 1 1 d . . . C1N C 0.98216(17) 0.35155(18) 0.61588(16) 0.0196(4) Uani 1 1 d . . . O1N O 0.96513(13) 0.29200(13) 0.70246(12) 0.0260(4) Uani 1 1 d . . . O2N O 0.91507(14) 0.44709(14) 0.58280(13) 0.0298(4) Uani 1 1 d . . . O3N O 1.06535(13) 0.31312(14) 0.55988(12) 0.0262(4) Uani 1 1 d . . . O1W O 0.29875(14) 0.21179(16) 0.36874(16) 0.0364(4) Uani 1 1 d . . . H11W H 0.2627 0.1962 0.3505 0.044 Uiso 1 1 d R . . H12W H 0.2561 0.2620 0.3891 0.044 Uiso 1 1 d R . . O2W O 0.66055(14) 0.04495(15) 0.26444(14) 0.0245(4) Uani 1 1 d . . . H21W H 0.7283 0.0026 0.2554 0.029 Uiso 1 1 d R . . H22W H 0.6638 0.0762 0.3065 0.029 Uiso 1 1 d R . . O3W O 0.48700(14) 0.68411(14) 0.55704(13) 0.0230(4) Uani 1 1 d . . . H31W H 0.4200 0.7155 0.5790 0.028 Uiso 1 1 d R . . H32W H 0.4832 0.6459 0.5307 0.028 Uiso 1 1 d R . . O4W O 0.02662(13) 0.21753(15) 0.44131(13) 0.0293(4) Uani 1 1 d . . . H41W H -0.0450 0.2423 0.4455 0.035 Uiso 1 1 d R . . H42W H 0.0424 0.2481 0.4760 0.035 Uiso 1 1 d R . . O5W O 0.85799(13) 0.54101(14) 0.39709(14) 0.0284(4) Uani 1 1 d . . . H51W H 0.9066 0.5212 0.3573 0.034 Uiso 1 1 d R . . H52W H 0.8800 0.5064 0.4536 0.034 Uiso 1 1 d R . . O6W O 0.17618(14) 0.11232(15) 0.31417(14) 0.0268(4) Uani 1 1 d . . . H61W H 0.1227 0.1558 0.3441 0.032 Uiso 1 1 d R . . H62W H 0.1811 0.1448 0.2537 0.032 Uiso 1 1 d R . . O7W O 0.16132(15) 0.40654(16) 0.39679(14) 0.0349(4) Uani 1 1 d . . . H71W H 0.1192 0.4073 0.4482 0.042 Uiso 1 1 d R . . H72W H 0.1984 0.4360 0.3961 0.042 Uiso 1 1 d R . . O8W O 0.56836(16) 0.48674(16) 0.75850(16) 0.0381(5) Uani 1 1 d . . . H81W H 0.5051 0.5358 0.7602 0.046 Uiso 1 1 d R . . H82W H 0.6095 0.5249 0.7212 0.046 Uiso 1 1 d R . . O9W O 0.75939(14) 0.76233(14) 0.37131(13) 0.0320(4) Uani 1 1 d . . . H91W H 0.7917 0.6984 0.3739 0.038 Uiso 1 1 d R . . H92W H 0.7981 0.8012 0.3370 0.038 Uiso 1 1 d R . . O10W O 0.14256(15) 0.33507(15) 0.88541(13) 0.0335(4) Uani 1 1 d . . . H101 H 0.1818 0.3205 0.9343 0.040 Uiso 1 1 d R . . H102 H 0.1290 0.2855 0.8918 0.040 Uiso 1 1 d R . . O11W O 0.02691(15) 0.37073(16) 0.12663(15) 0.0373(4) Uani 1 1 d . . . H111 H 0.0910 0.3220 0.1155 0.045 Uiso 1 1 d R . . H112 H 0.0596 0.4251 0.0917 0.045 Uiso 1 1 d R . . O12W O 0.13795(17) 0.50105(15) 0.03519(15) 0.0399(5) Uani 1 1 d . . . H121 H 0.1828 0.4466 0.0333 0.048 Uiso 1 1 d R . . H122 H 0.1649 0.5490 -0.0270 0.048 Uiso 1 1 d R . . O13W O 0.97514(16) 0.62606(17) 0.52733(18) 0.0398(5) Uani 1 1 d . . . H131 H 0.9661 0.5695 0.5467 0.048 Uiso 1 1 d R . . H132 H 0.9107 0.6733 0.5257 0.048 Uiso 1 1 d R . . O14W O 0.81960(16) 0.38344(17) 0.83679(15) 0.0411(5) Uani 1 1 d . . . H141 H 0.8601 0.3760 0.7814 0.049 Uiso 1 1 d R . . H142 H 0.7827 0.4487 0.7909 0.049 Uiso 1 1 d R . . O15W O 0.02187(17) 0.47892(17) 0.26250(15) 0.0436(5) Uani 1 1 d . . . H151 H 0.0248 0.4247 0.2473 0.052 Uiso 1 1 d R . . H152 H 0.0792 0.4413 0.3040 0.052 Uiso 1 1 d R . . O16W O 0.10872(14) 0.18179(15) 0.83732(13) 0.0313(4) Uani 1 1 d . . . H161 H 0.0638 0.2212 0.7936 0.038 Uiso 1 1 d R . . H162 H 0.0608 0.1555 0.8803 0.038 Uiso 1 1 d R . . O17W O 0.24449(14) 0.22318(15) 0.65100(14) 0.0316(4) Uani 1 1 d . . . H171 H 0.2278 0.2018 0.7164 0.038 Uiso 1 1 d R . . H172 H 0.1820 0.2416 0.6319 0.038 Uiso 1 1 d R . . O18W O 0.75184(15) 0.77678(14) 0.55669(14) 0.0334(4) Uani 1 1 d . . . H181 H 0.7449 0.8453 0.5460 0.040 Uiso 1 1 d R . . H182 H 0.7463 0.7828 0.5009 0.040 Uiso 1 1 d R . . O19W O 0.93544(18) 0.48039(17) 0.88427(18) 0.0491(6) Uani 1 1 d . . . H191 H 0.9014 0.4419 0.8753 0.059 Uiso 1 1 d R . . H192 H 0.9996 0.4341 0.8879 0.059 Uiso 1 1 d R . . O20W O 0.73280(17) 0.56242(17) 0.66539(19) 0.0544(6) Uani 1 1 d . . . H201 H 0.7977 0.5234 0.6486 0.065 Uiso 1 1 d R . . H202 H 0.7208 0.6341 0.6278 0.065 Uiso 1 1 d R . . 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 Cu1 0.01131(12) 0.01403(12) 0.00813(12) -0.00231(9) -0.00173(9) -0.00213(10) Cu2 0.01192(12) 0.01502(12) 0.00832(12) -0.00261(10) -0.00186(9) -0.00266(10) N1A 0.0164(10) 0.0165(9) 0.0107(9) -0.0048(7) -0.0020(7) -0.0044(8) C2A 0.0168(11) 0.0150(10) 0.0122(11) -0.0045(8) -0.0041(8) -0.0020(9) P3A 0.0161(3) 0.0139(3) 0.0124(3) -0.0040(2) -0.0038(2) -0.0053(2) O31A 0.0229(9) 0.0241(9) 0.0267(10) 0.0057(7) -0.0121(7) -0.0129(8) O32A 0.0337(11) 0.0188(8) 0.0204(9) -0.0112(7) -0.0023(8) -0.0062(8) C4A 0.0118(10) 0.0138(10) 0.0093(10) -0.0043(8) -0.0010(8) -0.0031(8) O41A 0.0106(7) 0.0161(7) 0.0082(7) -0.0048(6) -0.0001(6) -0.0012(6) C41A 0.0159(11) 0.0155(10) 0.0100(10) -0.0005(8) -0.0057(8) -0.0074(9) C42A 0.0258(13) 0.0171(11) 0.0185(12) -0.0076(9) -0.0044(9) -0.0076(10) C43A 0.0372(15) 0.0230(12) 0.0324(15) -0.0063(11) -0.0111(11) -0.0168(12) C44A 0.0273(13) 0.0302(13) 0.0250(14) 0.0031(10) -0.0083(10) -0.0199(11) C45A 0.0167(11) 0.0350(14) 0.0174(12) -0.0027(10) -0.0007(9) -0.0136(11) C46A 0.0165(11) 0.0239(12) 0.0136(11) -0.0063(9) -0.0009(9) -0.0083(10) P5A 0.0128(3) 0.0151(3) 0.0084(3) -0.0037(2) -0.0010(2) -0.0048(2) O51A 0.0157(8) 0.0215(8) 0.0156(8) -0.0075(6) -0.0032(6) -0.0078(6) O52A 0.0179(8) 0.0203(8) 0.0101(8) -0.0067(6) 0.0013(6) -0.0051(7) C6A 0.0168(11) 0.0151(10) 0.0132(11) -0.0031(8) -0.0010(9) -0.0057(9) N7A 0.0178(10) 0.0136(9) 0.0119(9) -0.0029(7) -0.0025(7) -0.0039(8) N1B 0.0133(9) 0.0170(9) 0.0096(9) -0.0022(7) -0.0040(7) -0.0018(8) C2B 0.0170(11) 0.0163(11) 0.0142(11) -0.0038(9) -0.0028(9) -0.0003(9) P3B 0.0202(3) 0.0146(3) 0.0124(3) -0.0022(2) -0.0037(2) -0.0078(2) O31B 0.0324(11) 0.0315(10) 0.0366(12) 0.0117(9) -0.0141(9) -0.0226(9) O32B 0.0430(12) 0.0168(8) 0.0164(9) -0.0080(7) -0.0033(8) -0.0061(8) C4B 0.0106(10) 0.0151(10) 0.0092(10) -0.0044(8) 0.0005(8) -0.0039(8) O41B 0.0115(7) 0.0197(8) 0.0082(7) -0.0041(6) 0.0003(6) -0.0018(6) C41B 0.0153(10) 0.0158(10) 0.0088(10) -0.0034(8) -0.0011(8) -0.0069(9) C42B 0.0223(12) 0.0207(12) 0.0217(13) -0.0081(10) -0.0025(10) -0.0078(10) C43B 0.0416(16) 0.0235(12) 0.0251(13) -0.0070(10) -0.0084(11) -0.0180(12) C44B 0.0344(14) 0.0371(15) 0.0195(13) 0.0035(11) -0.0081(10) -0.0275(12) C45B 0.0187(12) 0.0418(15) 0.0140(12) -0.0049(10) 0.0006(9) -0.0156(12) C46B 0.0182(11) 0.0222(11) 0.0124(11) -0.0060(9) -0.0020(9) -0.0084(10) P5B 0.0123(3) 0.0158(3) 0.0082(3) -0.0036(2) -0.0014(2) -0.0043(2) O51B 0.0163(8) 0.0266(9) 0.0148(8) -0.0054(7) -0.0039(6) -0.0085(7) O52B 0.0155(8) 0.0235(8) 0.0103(8) -0.0054(6) -0.0007(6) -0.0064(7) C6B 0.0161(11) 0.0163(11) 0.0133(11) -0.0006(8) -0.0006(9) -0.0065(9) N7B 0.0150(9) 0.0155(9) 0.0136(9) -0.0034(7) -0.0022(7) -0.0046(8) Cu3 0.01463(12) 0.01170(12) 0.00964(12) -0.00051(9) -0.00478(9) -0.00516(10) Cu4 0.01572(13) 0.01204(12) 0.01076(12) -0.00072(9) -0.00601(10) -0.00537(10) N1C 0.0205(10) 0.0138(9) 0.0147(10) -0.0045(7) -0.0072(8) -0.0029(8) C2C 0.0204(11) 0.0153(10) 0.0128(11) -0.0029(8) -0.0070(9) -0.0056(9) P3C 0.0113(3) 0.0115(2) 0.0087(3) -0.0018(2) -0.0029(2) -0.0039(2) O31C 0.0175(8) 0.0184(8) 0.0097(8) -0.0019(6) -0.0011(6) -0.0085(7) O32C 0.0144(8) 0.0149(8) 0.0129(8) -0.0006(6) -0.0052(6) -0.0039(7) C4C 0.0137(10) 0.0115(10) 0.0060(10) -0.0013(7) -0.0022(8) -0.0041(8) O41C 0.0136(7) 0.0089(7) 0.0095(7) 0.0006(6) -0.0058(6) -0.0028(6) C41C 0.0126(10) 0.0168(10) 0.0089(10) -0.0037(8) -0.0023(8) -0.0061(9) C42C 0.0178(11) 0.0185(11) 0.0145(11) -0.0057(9) 0.0001(9) -0.0027(9) C43C 0.0220(12) 0.0277(13) 0.0178(12) -0.0102(10) 0.0036(10) -0.0043(10) C44C 0.0261(13) 0.0342(14) 0.0116(11) -0.0089(10) 0.0055(10) -0.0167(11) C45C 0.0282(13) 0.0244(12) 0.0100(11) 0.0017(9) -0.0057(9) -0.0163(11) C46C 0.0153(10) 0.0165(10) 0.0130(11) -0.0036(8) -0.0015(8) -0.0075(9) P5C 0.0128(3) 0.0109(2) 0.0094(3) -0.0030(2) -0.0025(2) -0.0034(2) O51C 0.0174(8) 0.0160(7) 0.0079(7) -0.0037(6) -0.0013(6) -0.0057(6) O52C 0.0174(8) 0.0139(8) 0.0162(8) -0.0050(6) -0.0055(6) -0.0018(7) C6C 0.0158(11) 0.0158(10) 0.0167(11) -0.0022(9) -0.0042(8) -0.0066(9) N7C 0.0132(9) 0.0160(9) 0.0168(9) -0.0036(7) -0.0037(7) -0.0056(7) N1D 0.0366(13) 0.0161(10) 0.0223(11) -0.0059(8) -0.0140(9) -0.0051(9) C2D 0.0184(11) 0.0177(11) 0.0127(11) -0.0036(9) -0.0040(9) -0.0069(9) P3D 0.0121(3) 0.0132(3) 0.0084(3) -0.0021(2) -0.0024(2) -0.0042(2) O31D 0.0163(8) 0.0196(8) 0.0107(8) -0.0024(6) -0.0014(6) -0.0067(7) O32D 0.0139(8) 0.0176(8) 0.0110(8) -0.0032(6) -0.0032(6) -0.0022(7) C4D 0.0106(10) 0.0111(9) 0.0091(10) -0.0007(8) -0.0042(8) -0.0020(8) O41D 0.0131(7) 0.0106(7) 0.0097(7) -0.0001(6) -0.0044(6) -0.0032(6) C41D 0.0154(10) 0.0164(10) 0.0100(10) -0.0058(8) -0.0002(8) -0.0080(9) C42D 0.0184(11) 0.0196(11) 0.0169(11) -0.0052(9) -0.0030(9) -0.0042(9) C43D 0.0223(12) 0.0315(13) 0.0211(13) -0.0139(11) 0.0044(10) -0.0083(11) C44D 0.0294(13) 0.0310(13) 0.0109(11) -0.0062(10) 0.0031(9) -0.0181(11) C45D 0.0240(12) 0.0209(11) 0.0125(11) -0.0015(9) -0.0040(9) -0.0102(10) C46D 0.0169(11) 0.0165(10) 0.0098(10) -0.0013(8) -0.0052(8) -0.0076(9) P5D 0.0134(3) 0.0117(2) 0.0096(3) -0.0034(2) -0.0027(2) -0.0031(2) O51D 0.0186(8) 0.0164(8) 0.0110(8) -0.0041(6) -0.0019(6) -0.0058(7) O52D 0.0181(8) 0.0136(8) 0.0179(8) -0.0057(6) -0.0058(6) -0.0022(7) C6D 0.0175(11) 0.0129(10) 0.0142(11) -0.0011(8) -0.0033(8) -0.0059(9) N7D 0.0140(9) 0.0181(9) 0.0160(9) -0.0026(7) -0.0022(7) -0.0055(8) C1E 0.0173(11) 0.0134(10) 0.0145(11) -0.0036(8) -0.0048(9) -0.0006(9) N1E 0.0181(10) 0.0282(11) 0.0174(10) -0.0113(8) 0.0025(8) -0.0108(9) N2E 0.0192(10) 0.0250(10) 0.0137(10) -0.0078(8) -0.0004(8) -0.0072(9) N3E 0.0268(11) 0.0233(10) 0.0145(9) -0.0095(8) -0.0003(8) -0.0096(9) C1F 0.0157(11) 0.0145(10) 0.0162(11) -0.0059(8) -0.0065(9) 0.0011(9) N1F 0.0196(10) 0.0306(11) 0.0209(10) -0.0135(9) 0.0021(8) -0.0116(9) N2F 0.0193(10) 0.0249(11) 0.0185(11) -0.0092(8) 0.0006(8) -0.0086(9) N3F 0.0243(11) 0.0253(10) 0.0224(11) -0.0132(9) -0.0001(8) -0.0082(9) C1G 0.0221(12) 0.0181(11) 0.0152(12) -0.0044(9) -0.0025(9) -0.0039(10) N1G 0.0364(13) 0.0303(11) 0.0150(10) -0.0108(9) 0.0065(9) -0.0209(10) N2G 0.0271(11) 0.0237(10) 0.0155(11) -0.0065(8) -0.0018(8) -0.0092(9) N3G 0.0363(13) 0.0329(12) 0.0136(10) -0.0114(9) 0.0054(9) -0.0189(11) C1H 0.0194(12) 0.0177(11) 0.0142(11) -0.0046(9) -0.0021(9) -0.0036(10) N1H 0.0337(12) 0.0281(11) 0.0134(10) -0.0058(8) 0.0012(8) -0.0199(10) N2H 0.0356(13) 0.0277(11) 0.0180(10) -0.0109(9) 0.0066(9) -0.0199(10) N3H 0.0261(11) 0.0266(11) 0.0160(11) -0.0075(9) 0.0024(9) -0.0159(10) C1I 0.0150(10) 0.0191(11) 0.0136(10) -0.0072(8) 0.0008(8) -0.0055(9) N1I 0.0151(9) 0.0145(9) 0.0230(10) -0.0043(7) -0.0053(7) -0.0035(7) N2I 0.0198(9) 0.0149(9) 0.0236(10) -0.0012(7) -0.0076(8) -0.0042(8) N3I 0.0213(9) 0.0174(9) 0.0290(10) -0.0040(8) -0.0076(8) -0.0079(8) C1J 0.0209(10) 0.0190(10) 0.0166(10) -0.0067(8) 0.0000(8) -0.0078(8) N1J 0.0192(9) 0.0246(10) 0.0179(9) 0.0024(8) -0.0032(7) -0.0093(8) N2J 0.0180(9) 0.0311(11) 0.0209(10) -0.0007(8) -0.0004(7) -0.0122(8) N3J 0.0192(9) 0.0264(11) 0.0217(10) 0.0003(8) -0.0019(8) -0.0090(8) C1K 0.0261(12) 0.0221(11) 0.0301(13) -0.0185(10) 0.0047(10) -0.0074(9) N1K 0.0265(11) 0.0215(10) 0.0338(12) -0.0084(9) -0.0061(9) -0.0045(9) N2K 0.0310(11) 0.0217(10) 0.0257(10) -0.0050(8) 0.0022(9) -0.0101(9) N3K 0.0318(12) 0.0361(13) 0.0501(15) -0.0219(11) 0.0086(11) -0.0160(10) C1L 0.0173(11) 0.0291(12) 0.0202(12) -0.0140(10) 0.0033(9) -0.0107(10) N1L 0.0162(9) 0.0285(11) 0.0244(11) -0.0055(9) -0.0048(8) -0.0074(9) N2L 0.0216(10) 0.0266(11) 0.0276(11) -0.0072(8) -0.0053(8) -0.0086(8) N3L 0.0319(11) 0.0385(12) 0.0326(12) -0.0031(10) -0.0097(9) -0.0212(10) C1M 0.0288(12) 0.0199(11) 0.0171(11) -0.0046(9) -0.0006(9) -0.0093(9) O1M 0.0285(9) 0.0237(9) 0.0303(9) -0.0065(7) -0.0011(7) -0.0112(7) O2M 0.0313(10) 0.0270(9) 0.0317(10) 0.0051(8) -0.0011(8) -0.0104(8) O3M 0.0283(9) 0.0260(9) 0.0257(9) 0.0005(7) -0.0066(7) -0.0092(7) C1N 0.0212(11) 0.0222(11) 0.0174(10) -0.0068(9) -0.0023(8) -0.0088(9) O1N 0.0290(9) 0.0239(8) 0.0213(8) -0.0035(7) -0.0012(7) -0.0090(7) O2N 0.0328(10) 0.0226(9) 0.0266(9) -0.0029(7) -0.0029(7) -0.0063(7) O3N 0.0223(8) 0.0318(9) 0.0258(9) -0.0117(7) 0.0016(7) -0.0103(7) O1W 0.0268(9) 0.0361(10) 0.0565(13) -0.0190(10) -0.0112(9) -0.0128(8) O2W 0.0185(9) 0.0347(10) 0.0273(10) -0.0199(8) -0.0007(7) -0.0083(8) O3W 0.0241(9) 0.0264(9) 0.0231(9) -0.0141(7) -0.0005(7) -0.0088(8) O4W 0.0220(8) 0.0419(10) 0.0340(10) -0.0239(8) 0.0018(7) -0.0130(8) O5W 0.0261(9) 0.0302(9) 0.0317(10) -0.0089(8) -0.0092(7) -0.0095(7) O6W 0.0212(9) 0.0285(9) 0.0251(9) -0.0062(7) -0.0018(7) -0.0051(7) O7W 0.0333(10) 0.0508(12) 0.0315(10) -0.0157(9) 0.0052(8) -0.0269(9) O8W 0.0338(11) 0.0283(10) 0.0402(12) -0.0036(8) -0.0065(9) -0.0035(8) O9W 0.0329(10) 0.0261(9) 0.0328(10) -0.0100(8) 0.0115(8) -0.0131(8) O10W 0.0436(11) 0.0362(10) 0.0263(9) -0.0016(8) -0.0077(8) -0.0235(9) O11W 0.0306(10) 0.0324(10) 0.0468(12) -0.0111(9) 0.0053(8) -0.0145(8) O12W 0.0526(12) 0.0236(9) 0.0382(11) -0.0093(8) 0.0109(9) -0.0166(9) O13W 0.0256(10) 0.0313(11) 0.0665(15) -0.0145(10) -0.0061(10) -0.0130(9) O14W 0.0372(11) 0.0465(12) 0.0342(11) -0.0152(9) 0.0097(9) -0.0139(9) O15W 0.0484(12) 0.0383(11) 0.0368(11) -0.0086(9) -0.0073(9) -0.0092(10) O16W 0.0337(10) 0.0363(10) 0.0265(9) 0.0003(8) -0.0060(7) -0.0212(8) O17W 0.0293(9) 0.0367(10) 0.0311(10) -0.0075(8) -0.0023(8) -0.0164(8) O18W 0.0462(11) 0.0201(9) 0.0353(10) -0.0021(7) -0.0175(8) -0.0112(8) O19W 0.0481(13) 0.0296(11) 0.0653(15) -0.0108(10) -0.0081(11) -0.0111(10) O20W 0.0328(11) 0.0313(11) 0.0709(16) 0.0000(11) 0.0121(11) -0.0055(9) _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 Cu1 O41B 1.9275(16) . ? Cu1 O41A 1.9883(15) . ? Cu1 N7B 1.9982(19) . ? Cu1 N1A 2.001(2) . ? Cu1 Cu2 3.0321(3) . ? Cu2 O41A 1.9274(16) . ? Cu2 O41B 1.9835(15) . ? Cu2 N1B 1.9865(19) . ? Cu2 N7A 2.0044(19) . ? N1A C2A 1.490(3) . ? N1A H11A 0.9200 . ? N1A H12A 0.9200 . ? C2A P3A 1.815(2) . ? C2A H21A 0.9900 . ? C2A H22A 0.9900 . ? P3A O32A 1.4958(19) . ? P3A O31A 1.5112(17) . ? P3A C4A 1.866(2) . ? C4A O41A 1.429(3) . ? C4A C41A 1.522(3) . ? C4A P5A 1.859(2) . ? C41A C46A 1.393(3) . ? C41A C42A 1.403(3) . ? C42A C43A 1.391(3) . ? C42A H42A 0.9500 . ? C43A C44A 1.387(4) . ? C43A H43A 0.9500 . ? C44A C45A 1.380(4) . ? C44A H44A 0.9500 . ? C45A C46A 1.381(3) . ? C45A H45A 0.9500 . ? C46A H46A 0.9500 . ? P5A O51A 1.5076(16) . ? P5A O52A 1.5107(16) . ? P5A C6A 1.818(2) . ? C6A N7A 1.483(3) . ? C6A H61A 0.9900 . ? C6A H62A 0.9900 . ? N7A H71A 0.9200 . ? N7A H72A 0.9200 . ? N1B C2B 1.476(3) . ? N1B H11B 0.9200 . ? N1B H12B 0.9200 . ? C2B P3B 1.829(2) . ? C2B H21B 0.9900 . ? C2B H22B 0.9900 . ? P3B O31B 1.4951(19) . ? P3B O32B 1.5044(19) . ? P3B C4B 1.872(2) . ? C4B O41B 1.430(3) . ? C4B C41B 1.526(3) . ? C4B P5B 1.868(2) . ? C41B C42B 1.386(3) . ? C41B C46B 1.401(3) . ? C42B C43B 1.394(3) . ? C42B H42B 0.9500 . ? C43B C44B 1.386(4) . ? C43B H43B 0.9500 . ? C44B C45B 1.379(4) . ? C44B H44B 0.9500 . ? C45B C46B 1.387(3) . ? C45B H45B 0.9500 . ? C46B H46B 0.9500 . ? P5B O51B 1.5030(16) . ? P5B O52B 1.5089(17) . ? P5B C6B 1.813(2) . ? C6B N7B 1.486(3) . ? C6B H61B 0.9900 . ? C6B H62B 0.9900 . ? N7B H71B 0.9200 . ? N7B H72B 0.9200 . ? Cu3 O41C 1.9593(14) . ? Cu3 O41D 1.9762(15) . ? Cu3 N7D 2.0261(18) . ? Cu3 N1C 2.0311(19) . ? Cu3 Cu4 3.0466(3) . ? Cu4 O41D 1.9623(14) . ? Cu4 O41C 1.9792(15) . ? Cu4 N1D 2.024(2) . ? Cu4 N7C 2.0254(18) . ? Cu4 O51C 2.4337(16) . ? N1C C2C 1.489(3) . ? N1C H11C 0.9200 . ? N1C H12C 0.9200 . ? C2C P3C 1.825(2) . ? C2C H21C 0.9900 . ? C2C H22C 0.9900 . ? P3C O31C 1.5066(16) . ? P3C O32C 1.5095(16) . ? P3C C4C 1.860(2) . ? C4C O41C 1.428(3) . ? C4C C41C 1.534(3) . ? C4C P5C 1.868(2) . ? C41C C46C 1.387(3) . ? C41C C42C 1.394(3) . ? C42C C43C 1.389(3) . ? C42C H42C 0.9500 . ? C43C C44C 1.377(4) . ? C43C H43C 0.9500 . ? C44C C45C 1.381(4) . ? C44C H44C 0.9500 . ? C45C C46C 1.395(3) . ? C45C H45C 0.9500 . ? C46C H46C 0.9500 . ? P5C O52C 1.5047(17) . ? P5C O51C 1.5151(16) . ? P5C C6C 1.822(2) . ? C6C N7C 1.484(3) . ? C6C H61C 0.9900 . ? C6C H62C 0.9900 . ? N7C H71C 0.9200 . ? N7C H72C 0.9200 . ? N1D C2D 1.491(3) . ? N1D H11D 0.9200 . ? N1D H12D 0.9200 . ? C2D P3D 1.821(2) . ? C2D H21D 0.9900 . ? C2D H22D 0.9900 . ? P3D O32D 1.5054(17) . ? P3D O31D 1.5099(16) . ? P3D C4D 1.866(2) . ? C4D O41D 1.429(2) . ? C4D C41D 1.521(3) . ? C4D P5D 1.862(2) . ? C41D C42D 1.396(3) . ? C41D C46D 1.398(3) . ? C42D C43D 1.392(3) . ? C42D H42D 0.9500 . ? C43D C44D 1.380(4) . ? C43D H43D 0.9500 . ? C44D C45D 1.388(4) . ? C44D H44D 0.9500 . ? C45D C46D 1.385(3) . ? C45D H45D 0.9500 . ? C46D H46D 0.9500 . ? P5D O52D 1.5071(17) . ? P5D O51D 1.5090(16) . ? P5D C6D 1.822(2) . ? C6D N7D 1.494(3) . ? C6D H61D 0.9900 . ? C6D H62D 0.9900 . ? N7D H71D 0.9200 . ? N7D H72D 0.9200 . ? C1E N2E 1.324(3) . ? C1E N1E 1.327(3) . ? C1E N3E 1.336(3) . ? N1E H11E 0.8385 . ? N1E H12E 0.9125 . ? N2E H21E 0.7924 . ? N2E H22E 0.8678 . ? N3E H31E 0.8608 . ? N3E H32E 0.8630 . ? C1F N1F 1.323(3) . ? C1F N2F 1.325(3) . ? C1F N3F 1.330(3) . ? N1F H11F 0.8773 . ? N1F H12F 0.8759 . ? N2F H21F 0.9135 . ? N2F H22F 0.8545 . ? N3F H31F 0.8629 . ? N3F H32F 0.8619 . ? C1G N2G 1.311(3) . ? C1G N3G 1.336(3) . ? C1G N1G 1.341(3) . ? N1G H11G 0.9156 . ? N1G H12G 0.9916 . ? N2G H21G 0.8021 . ? N2G H22G 0.8381 . ? N3G H31G 0.7678 . ? N3G H32G 0.9397 . ? C1H N3H 1.315(3) . ? C1H N1H 1.321(3) . ? C1H N2H 1.333(3) . ? N1H H11H 0.9276 . ? N1H H12H 0.8196 . ? N2H H21H 0.9274 . ? N2H H22H 0.8735 . ? N3H H31H 0.9076 . ? N3H H32H 0.9006 . ? C1I N3I 1.331(3) . ? C1I N1I 1.331(3) . ? C1I N2I 1.332(3) . ? N1I H11I 0.8640 . ? N1I H12I 0.8113 . ? N2I H21I 0.9144 . ? N2I H22I 0.9103 . ? N3I H31I 0.8271 . ? N3I H32I 0.9282 . ? C1J N1J 1.320(3) . ? C1J N2J 1.323(3) . ? C1J N3J 1.336(3) . ? N1J H11J 0.8802 . ? N1J H12J 0.7240 . ? N2J H21J 0.9344 . ? N2J H22J 0.8570 . ? N3J H31J 0.9377 . ? N3J H32J 0.8027 . ? C1K N3K 1.321(3) . ? C1K N2K 1.325(3) . ? C1K N1K 1.337(3) . ? N1K H11K 0.9341 . ? N1K H12K 0.8643 . ? N2K H21K 0.8628 . ? N2K H22K 1.0429 . ? N3K H31K 0.8870 . ? N3K H32K 0.8410 . ? C1L N2L 1.317(3) . ? C1L N1L 1.326(3) . ? C1L N3L 1.342(3) . ? N1L H11L 0.8233 . ? N1L H12L 0.9324 . ? N2L H21L 0.8278 . ? N2L H22L 0.9218 . ? N3L H31L 0.9716 . ? N3L H32L 0.8925 . ? C1M O3M 1.268(3) . ? C1M O2M 1.273(3) . ? C1M O1M 1.301(3) . ? C1N O1N 1.280(3) . ? C1N O2N 1.289(3) . ? C1N O3N 1.290(3) . ? O1W H11W 0.7579 . ? O1W H12W 0.8146 . ? O2W H21W 0.9014 . ? O2W H22W 0.8847 . ? O3W H31W 0.8963 . ? O3W H32W 0.7869 . ? O4W H41W 0.9181 . ? O4W H42W 0.8776 . ? O5W H51W 0.8051 . ? O5W H52W 0.8476 . ? O6W H61W 0.8848 . ? O6W H62W 0.8370 . ? O7W H71W 0.8379 . ? O7W H72W 0.7929 . ? O8W H81W 0.8764 . ? O8W H82W 0.9155 . ? O9W H91W 0.8205 . ? O9W H92W 0.8884 . ? O10W H101 0.9128 . ? O10W H102 0.7755 . ? O11W H111 0.9016 . ? O11W H112 0.9931 . ? O12W H121 0.7741 . ? O12W H122 1.0260 . ? O13W H131 0.8088 . ? O13W H132 0.8779 . ? O14W H141 0.8797 . ? O14W H142 0.9509 . ? O15W H151 0.8534 . ? O15W H152 0.9714 . ? O16W H161 0.8722 . ? O16W H162 0.9160 . ? O17W H171 0.8929 . ? O17W H172 0.8912 . ? O18W H181 0.8978 . ? O18W H182 0.7987 . ? O19W H191 0.9184 . ? O19W H192 0.8715 . ? O20W H201 0.8794 . ? O20W H202 0.9374 . ? 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 O41B Cu1 O41A 78.37(6) . . ? O41B Cu1 N7B 99.38(7) . . ? O41A Cu1 N7B 174.52(7) . . ? O41B Cu1 N1A 164.70(7) . . ? O41A Cu1 N1A 90.02(7) . . ? N7B Cu1 N1A 93.02(8) . . ? O41B Cu1 Cu2 39.84(5) . . ? O41A Cu1 Cu2 38.53(4) . . ? N7B Cu1 Cu2 138.94(6) . . ? N1A Cu1 Cu2 127.96(6) . . ? O41A Cu2 O41B 78.49(6) . . ? O41A Cu2 N1B 163.77(7) . . ? O41B Cu2 N1B 89.05(7) . . ? O41A Cu2 N7A 101.00(7) . . ? O41B Cu2 N7A 175.49(8) . . ? N1B Cu2 N7A 92.23(8) . . ? O41A Cu2 Cu1 39.99(4) . . ? O41B Cu2 Cu1 38.50(5) . . ? N1B Cu2 Cu1 126.70(6) . . ? N7A Cu2 Cu1 140.86(6) . . ? C2A N1A Cu1 112.69(14) . . ? C2A N1A H11A 109.1 . . ? Cu1 N1A H11A 109.1 . . ? C2A N1A H12A 109.1 . . ? Cu1 N1A H12A 109.1 . . ? H11A N1A H12A 107.8 . . ? N1A C2A P3A 109.91(15) . . ? N1A C2A H21A 109.7 . . ? P3A C2A H21A 109.7 . . ? N1A C2A H22A 109.7 . . ? P3A C2A H22A 109.7 . . ? H21A C2A H22A 108.2 . . ? O32A P3A O31A 118.09(11) . . ? O32A P3A C2A 108.30(11) . . ? O31A P3A C2A 106.77(11) . . ? O32A P3A C4A 113.56(10) . . ? O31A P3A C4A 105.38(10) . . ? C2A P3A C4A 103.62(10) . . ? O41A C4A C41A 110.93(17) . . ? O41A C4A P5A 106.86(14) . . ? C41A C4A P5A 111.20(15) . . ? O41A C4A P3A 106.58(14) . . ? C41A C4A P3A 111.50(15) . . ? P5A C4A P3A 109.57(11) . . ? C4A O41A Cu2 127.72(13) . . ? C4A O41A Cu1 120.06(13) . . ? Cu2 O41A Cu1 101.48(7) . . ? C46A C41A C42A 118.2(2) . . ? C46A C41A C4A 121.5(2) . . ? C42A C41A C4A 120.2(2) . . ? C43A C42A C41A 119.9(2) . . ? C43A C42A H42A 120.1 . . ? C41A C42A H42A 120.1 . . ? C44A C43A C42A 120.9(2) . . ? C44A C43A H43A 119.5 . . ? C42A C43A H43A 119.5 . . ? C45A C44A C43A 119.3(2) . . ? C45A C44A H44A 120.3 . . ? C43A C44A H44A 120.3 . . ? C44A C45A C46A 120.2(2) . . ? C44A C45A H45A 119.9 . . ? C46A C45A H45A 119.9 . . ? C45A C46A C41A 121.4(2) . . ? C45A C46A H46A 119.3 . . ? C41A C46A H46A 119.3 . . ? O51A P5A O52A 117.02(9) . . ? O51A P5A C6A 107.89(10) . . ? O52A P5A C6A 109.47(10) . . ? O51A P5A C4A 107.84(9) . . ? O52A P5A C4A 111.30(10) . . ? C6A P5A C4A 102.24(10) . . ? N7A C6A P5A 110.12(14) . . ? N7A C6A H61A 109.6 . . ? P5A C6A H61A 109.6 . . ? N7A C6A H62A 109.6 . . ? P5A C6A H62A 109.6 . . ? H61A C6A H62A 108.2 . . ? C6A N7A Cu2 115.25(14) . . ? C6A N7A H71A 108.5 . . ? Cu2 N7A H71A 108.5 . . ? C6A N7A H72A 108.5 . . ? Cu2 N7A H72A 108.5 . . ? H71A N7A H72A 107.5 . . ? C2B N1B Cu2 111.84(14) . . ? C2B N1B H11B 109.2 . . ? Cu2 N1B H11B 109.2 . . ? C2B N1B H12B 109.2 . . ? Cu2 N1B H12B 109.2 . . ? H11B N1B H12B 107.9 . . ? N1B C2B P3B 109.94(16) . . ? N1B C2B H21B 109.7 . . ? P3B C2B H21B 109.7 . . ? N1B C2B H22B 109.7 . . ? P3B C2B H22B 109.7 . . ? H21B C2B H22B 108.2 . . ? O31B P3B O32B 118.00(12) . . ? O31B P3B C2B 108.12(11) . . ? O32B P3B C2B 107.72(11) . . ? O31B P3B C4B 106.36(11) . . ? O32B P3B C4B 113.00(10) . . ? C2B P3B C4B 102.44(10) . . ? O41B C4B C41B 111.14(17) . . ? O41B C4B P5B 107.63(14) . . ? C41B C4B P5B 108.26(14) . . ? O41B C4B P3B 105.89(14) . . ? C41B C4B P3B 114.40(15) . . ? P5B C4B P3B 109.32(11) . . ? C4B O41B Cu1 129.50(13) . . ? C4B O41B Cu2 120.23(13) . . ? Cu1 O41B Cu2 101.65(7) . . ? C42B C41B C46B 118.4(2) . . ? C42B C41B C4B 120.6(2) . . ? C46B C41B C4B 120.89(19) . . ? C41B C42B C43B 121.1(2) . . ? C41B C42B H42B 119.4 . . ? C43B C42B H42B 119.4 . . ? C44B C43B C42B 119.8(2) . . ? C44B C43B H43B 120.1 . . ? C42B C43B H43B 120.1 . . ? C45B C44B C43B 119.7(2) . . ? C45B C44B H44B 120.2 . . ? C43B C44B H44B 120.2 . . ? C44B C45B C46B 120.7(2) . . ? C44B C45B H45B 119.6 . . ? C46B C45B H45B 119.6 . . ? C45B C46B C41B 120.3(2) . . ? C45B C46B H46B 119.9 . . ? C41B C46B H46B 119.9 . . ? O51B P5B O52B 116.66(10) . . ? O51B P5B C6B 108.90(10) . . ? O52B P5B C6B 107.26(10) . . ? O51B P5B C4B 108.65(10) . . ? O52B P5B C4B 111.30(10) . . ? C6B P5B C4B 103.20(10) . . ? N7B C6B P5B 112.08(14) . . ? N7B C6B H61B 109.2 . . ? P5B C6B H61B 109.2 . . ? N7B C6B H62B 109.2 . . ? P5B C6B H62B 109.2 . . ? H61B C6B H62B 107.9 . . ? C6B N7B Cu1 117.97(14) . . ? C6B N7B H71B 107.8 . . ? Cu1 N7B H71B 107.8 . . ? C6B N7B H72B 107.8 . . ? Cu1 N7B H72B 107.8 . . ? H71B N7B H72B 107.2 . . ? O41C Cu3 O41D 78.72(6) . . ? O41C Cu3 N7D 167.96(7) . . ? O41D Cu3 N7D 92.08(7) . . ? O41C Cu3 N1C 94.04(7) . . ? O41D Cu3 N1C 167.67(7) . . ? N7D Cu3 N1C 96.32(8) . . ? O41C Cu3 Cu4 39.57(4) . . ? O41D Cu3 Cu4 39.16(4) . . ? N7D Cu3 Cu4 130.71(6) . . ? N1C Cu3 Cu4 132.94(6) . . ? O41D Cu4 O41C 78.58(6) . . ? O41D Cu4 N1D 95.30(8) . . ? O41C Cu4 N1D 168.18(9) . . ? O41D Cu4 N7C 163.04(7) . . ? O41C Cu4 N7C 89.13(7) . . ? N1D Cu4 N7C 98.75(9) . . ? O41D Cu4 O51C 104.19(6) . . ? O41C Cu4 O51C 80.38(6) . . ? N1D Cu4 O51C 91.49(7) . . ? N7C Cu4 O51C 84.96(7) . . ? O41D Cu4 Cu3 39.49(4) . . ? O41C Cu4 Cu3 39.09(4) . . ? N1D Cu4 Cu3 133.88(7) . . ? N7C Cu4 Cu3 127.38(6) . . ? O51C Cu4 Cu3 92.39(4) . . ? C2C N1C Cu3 115.58(14) . . ? C2C N1C H11C 108.4 . . ? Cu3 N1C H11C 108.4 . . ? C2C N1C H12C 108.4 . . ? Cu3 N1C H12C 108.4 . . ? H11C N1C H12C 107.4 . . ? N1C C2C P3C 110.04(15) . . ? N1C C2C H21C 109.7 . . ? P3C C2C H21C 109.7 . . ? N1C C2C H22C 109.7 . . ? P3C C2C H22C 109.7 . . ? H21C C2C H22C 108.2 . . ? O31C P3C O32C 117.46(9) . . ? O31C P3C C2C 106.20(10) . . ? O32C P3C C2C 109.79(10) . . ? O31C P3C C4C 107.58(9) . . ? O32C P3C C4C 112.12(9) . . ? C2C P3C C4C 102.49(10) . . ? O41C C4C C41C 111.40(18) . . ? O41C C4C P3C 105.68(13) . . ? C41C C4C P3C 110.82(14) . . ? O41C C4C P5C 107.30(14) . . ? C41C C4C P5C 109.69(14) . . ? P3C C4C P5C 111.84(11) . . ? C4C O41C Cu3 122.92(12) . . ? C4C O41C Cu4 118.81(12) . . ? Cu3 O41C Cu4 101.34(7) . . ? C46C C41C C42C 118.6(2) . . ? C46C C41C C4C 121.5(2) . . ? C42C C41C C4C 120.0(2) . . ? C43C C42C C41C 120.5(2) . . ? C43C C42C H42C 119.7 . . ? C41C C42C H42C 119.7 . . ? C44C C43C C42C 120.4(2) . . ? C44C C43C H43C 119.8 . . ? C42C C43C H43C 119.8 . . ? C43C C44C C45C 119.7(2) . . ? C43C C44C H44C 120.2 . . ? C45C C44C H44C 120.2 . . ? C44C C45C C46C 120.1(2) . . ? C44C C45C H45C 119.9 . . ? C46C C45C H45C 119.9 . . ? C41C C46C C45C 120.7(2) . . ? C41C C46C H46C 119.7 . . ? C45C C46C H46C 119.7 . . ? O52C P5C O51C 117.93(10) . . ? O52C P5C C6C 110.71(10) . . ? O51C P5C C6C 105.12(10) . . ? O52C P5C C4C 112.86(10) . . ? O51C P5C C4C 105.90(9) . . ? C6C P5C C4C 103.02(10) . . ? P5C O51C Cu4 93.69(8) . . ? N7C C6C P5C 108.52(14) . . ? N7C C6C H61C 110.0 . . ? P5C C6C H61C 110.0 . . ? N7C C6C H62C 110.0 . . ? P5C C6C H62C 110.0 . . ? H61C C6C H62C 108.4 . . ? C6C N7C Cu4 113.94(14) . . ? C6C N7C H71C 108.8 . . ? Cu4 N7C H71C 108.8 . . ? C6C N7C H72C 108.8 . . ? Cu4 N7C H72C 108.8 . . ? H71C N7C H72C 107.7 . . ? C2D N1D Cu4 115.20(15) . . ? C2D N1D H11D 108.5 . . ? Cu4 N1D H11D 108.5 . . ? C2D N1D H12D 108.5 . . ? Cu4 N1D H12D 108.5 . . ? H11D N1D H12D 107.5 . . ? N1D C2D P3D 109.77(16) . . ? N1D C2D H21D 109.7 . . ? P3D C2D H21D 109.7 . . ? N1D C2D H22D 109.7 . . ? P3D C2D H22D 109.7 . . ? H21D C2D H22D 108.2 . . ? O32D P3D O31D 117.20(9) . . ? O32D P3D C2D 110.18(10) . . ? O31D P3D C2D 105.97(10) . . ? O32D P3D C4D 111.75(9) . . ? O31D P3D C4D 108.31(9) . . ? C2D P3D C4D 102.25(10) . . ? O41D C4D C41D 111.59(18) . . ? O41D C4D P5D 106.43(14) . . ? C41D C4D P5D 110.13(14) . . ? O41D C4D P3D 106.40(13) . . ? C41D C4D P3D 109.61(15) . . ? P5D C4D P3D 112.60(11) . . ? C4D O41D Cu4 121.50(12) . . ? C4D O41D Cu3 120.57(12) . . ? Cu4 O41D Cu3 101.34(7) . . ? C42D C41D C46D 118.4(2) . . ? C42D C41D C4D 120.3(2) . . ? C46D C41D C4D 121.3(2) . . ? C43D C42D C41D 120.4(2) . . ? C43D C42D H42D 119.8 . . ? C41D C42D H42D 119.8 . . ? C44D C43D C42D 120.8(2) . . ? C44D C43D H43D 119.6 . . ? C42D C43D H43D 119.6 . . ? C43D C44D C45D 119.0(2) . . ? C43D C44D H44D 120.5 . . ? C45D C44D H44D 120.5 . . ? C46D C45D C44D 120.8(2) . . ? C46D C45D H45D 119.6 . . ? C44D C45D H45D 119.6 . . ? C45D C46D C41D 120.5(2) . . ? C45D C46D H46D 119.8 . . ? C41D C46D H46D 119.8 . . ? O52D P5D O51D 117.20(10) . . ? O52D P5D C6D 109.27(10) . . ? O51D P5D C6D 106.08(10) . . ? O52D P5D C4D 113.23(9) . . ? O51D P5D C4D 106.46(9) . . ? C6D P5D C4D 103.51(10) . . ? N7D C6D P5D 110.19(14) . . ? N7D C6D H61D 109.6 . . ? P5D C6D H61D 109.6 . . ? N7D C6D H62D 109.6 . . ? P5D C6D H62D 109.6 . . ? H61D C6D H62D 108.1 . . ? C6D N7D Cu3 113.98(13) . . ? C6D N7D H71D 108.8 . . ? Cu3 N7D H71D 108.8 . . ? C6D N7D H72D 108.8 . . ? Cu3 N7D H72D 108.8 . . ? H71D N7D H72D 107.7 . . ? N2E C1E N1E 120.4(2) . . ? N2E C1E N3E 120.5(2) . . ? N1E C1E N3E 119.1(2) . . ? C1E N1E H11E 128.0 . . ? C1E N1E H12E 114.5 . . ? H11E N1E H12E 117.3 . . ? C1E N2E H21E 116.4 . . ? C1E N2E H22E 116.9 . . ? H21E N2E H22E 119.7 . . ? C1E N3E H31E 119.7 . . ? C1E N3E H32E 104.8 . . ? H31E N3E H32E 119.5 . . ? N1F C1F N2F 120.1(2) . . ? N1F C1F N3F 119.2(2) . . ? N2F C1F N3F 120.7(2) . . ? C1F N1F H11F 115.3 . . ? C1F N1F H12F 119.6 . . ? H11F N1F H12F 124.8 . . ? C1F N2F H21F 117.4 . . ? C1F N2F H22F 130.7 . . ? H21F N2F H22F 109.3 . . ? C1F N3F H31F 117.5 . . ? C1F N3F H32F 120.0 . . ? H31F N3F H32F 121.6 . . ? N2G C1G N3G 120.8(2) . . ? N2G C1G N1G 120.0(2) . . ? N3G C1G N1G 119.2(2) . . ? C1G N1G H11G 118.6 . . ? C1G N1G H12G 113.0 . . ? H11G N1G H12G 128.3 . . ? C1G N2G H21G 116.0 . . ? C1G N2G H22G 116.4 . . ? H21G N2G H22G 126.1 . . ? C1G N3G H31G 120.5 . . ? C1G N3G H32G 119.8 . . ? H31G N3G H32G 119.6 . . ? N3H C1H N1H 120.2(2) . . ? N3H C1H N2H 119.2(2) . . ? N1H C1H N2H 120.6(2) . . ? C1H N1H H11H 119.7 . . ? C1H N1H H12H 120.9 . . ? H11H N1H H12H 119.3 . . ? C1H N2H H21H 115.5 . . ? C1H N2H H22H 115.6 . . ? H21H N2H H22H 127.1 . . ? C1H N3H H31H 120.2 . . ? C1H N3H H32H 118.6 . . ? H31H N3H H32H 119.4 . . ? N3I C1I N1I 119.6(2) . . ? N3I C1I N2I 120.6(2) . . ? N1I C1I N2I 119.7(2) . . ? C1I N1I H11I 107.7 . . ? C1I N1I H12I 117.4 . . ? H11I N1I H12I 122.4 . . ? C1I N2I H21I 118.6 . . ? C1I N2I H22I 118.8 . . ? H21I N2I H22I 120.8 . . ? C1I N3I H31I 125.1 . . ? C1I N3I H32I 117.7 . . ? H31I N3I H32I 116.1 . . ? N1J C1J N2J 120.9(2) . . ? N1J C1J N3J 119.7(2) . . ? N2J C1J N3J 119.5(2) . . ? C1J N1J H11J 122.5 . . ? C1J N1J H12J 117.7 . . ? H11J N1J H12J 119.2 . . ? C1J N2J H21J 123.8 . . ? C1J N2J H22J 119.0 . . ? H21J N2J H22J 114.8 . . ? C1J N3J H31J 118.8 . . ? C1J N3J H32J 118.9 . . ? H31J N3J H32J 118.3 . . ? N3K C1K N2K 119.9(2) . . ? N3K C1K N1K 120.9(2) . . ? N2K C1K N1K 119.2(2) . . ? C1K N1K H11K 113.3 . . ? C1K N1K H12K 117.0 . . ? H11K N1K H12K 123.5 . . ? C1K N2K H21K 117.9 . . ? C1K N2K H22K 123.6 . . ? H21K N2K H22K 117.1 . . ? C1K N3K H31K 125.1 . . ? C1K N3K H32K 113.9 . . ? H31K N3K H32K 120.9 . . ? N2L C1L N1L 120.6(2) . . ? N2L C1L N3L 118.2(2) . . ? N1L C1L N3L 121.2(2) . . ? C1L N1L H11L 118.7 . . ? C1L N1L H12L 114.5 . . ? H11L N1L H12L 126.3 . . ? C1L N2L H21L 110.6 . . ? C1L N2L H22L 113.2 . . ? H21L N2L H22L 131.0 . . ? C1L N3L H31L 115.8 . . ? C1L N3L H32L 114.7 . . ? H31L N3L H32L 124.4 . . ? O3M C1M O2M 122.3(2) . . ? O3M C1M O1M 119.6(2) . . ? O2M C1M O1M 118.0(2) . . ? O1N C1N O2N 120.7(2) . . ? O1N C1N O3N 119.2(2) . . ? O2N C1N O3N 120.0(2) . . ? H11W O1W H12W 100.1 . . ? H21W O2W H22W 100.8 . . ? H31W O3W H32W 101.9 . . ? H41W O4W H42W 107.1 . . ? H51W O5W H52W 105.9 . . ? H61W O6W H62W 108.1 . . ? H71W O7W H72W 109.1 . . ? H81W O8W H82W 104.4 . . ? H91W O9W H92W 110.7 . . ? H101 O10W H102 109.7 . . ? H111 O11W H112 85.0 . . ? H121 O12W H122 97.6 . . ? H131 O13W H132 102.0 . . ? H141 O14W H142 79.4 . . ? H151 O15W H152 97.6 . . ? H161 O16W H162 91.6 . . ? H171 O17W H172 97.9 . . ? H181 O18W H182 95.8 . . ? H191 O19W H192 102.4 . . ? H201 O20W H202 107.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.428 _refine_diff_density_min -0.338 _refine_diff_density_rms 0.052