# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 #TrackingRef '- CIFs.cif' # #------------------------------------------------------------------------- #2 Person making the deposition # _publ_contact_author 'Dr. Blacque, Olivier' _publ_contact_author_email oblacque@aci.uzh.ch _publ_contact_author_fax '+41 44 63 54 681' _publ_contact_author_phone '+41 44 63 54 651' #------------------------------------------------------------------------- #3 Publication details # # Provide these details if the structure has been published, # accepted or submitted for publication # # The CCDC journal deposition number, eg. 182/357, # should be included only if it has been assigned by the journal # # #------------------------------------------------------------------------- #4 Chemical and physical data # # Note that the units for melting point are Kelvin # The compound_id is the identifier for the compound in the published # paper, eg. 4a, II, etc. # Provide a brief description of any significant biological activity, # eg. antimalarial activity # If the compound exhibits polymorphism provide brief details, # eg. monoclinic form, low-temperature phase, etc. # For chemdiag leave blank - no longer necessary # #------------------------------------------------------------------------- #5 Other data relating to the structure determination and refinement # # Record the radiation type if not X-rays, eg. neutron # Record the temperature of the data collection (Kelvin) # if not room-temperature # Record R_squared if this is the only reliability factor given by # your refinement program # Describe briefly any disorder, eg. t-Butyl C31-33 disordered over # two sites with occupancies 0.6 and 0.4 # Under ccdc_comments record any other important information #------------------------------------------------------------------------- #6 Include your "standard" CIF file here # It should contain the following data items: # unit cell parameters and volume, z value, space group symbol, # R-factor(s), atomic coordinates with standard deviations, # occupancy factors, bond lengths and bond angles # Other data items may be present but will not necessarily be # included in the Cambridge Structural Database # # Do NOT include structure factors # # #------------------------------------------------------------------------- #SUBMISSION INFORMATION # # For a journal send the form to the address specified by the journal # # For a private communication to the CCDC send the form to the address # deposit@ccdc.cam.ac.uk # # For up-to-date information on deposition procedures, check the website # http://www.ccdc.cam.ac.uk/ _publ_section_comment ; (type here to add) ; _publ_section_abstract ; (type here to add abstract) ; _publ_contact_letter ; Please consider this CIF for publication. I certify that this contibution is the original work of those listed as authors; that it has not been published before (in any language or medium) and is not being considered for publication elsewhere; that all authors concur with and are aware of the submission; that all workers involved in the study are listed as authors or given proper credit in the acknowledgements; that I have obtained permission for and acknowledged the source of any excerpts from other copyright works; and that to the best of my knowledge the paper contains no statements which are libellous, unlawful or in any way actionable. All coauthors have made significant scientific contributions to the work reported, including the ideas and their execution, and share responsibility and accountability for the results. ; _publ_requested_category FM #============================================================================== # TITLE AND AUTHOR LIST _publ_section_title ; Incorporation of active metal sites in MOFs via in situ generated ligand deficient metal-linker complexes ; loop_ _publ_author_name _publ_author_address #Corresponding author of the paper #Corresponding author of the paper S.Barman ; Anorganisch-Chemisches Institut, Universitat Zurich, Winterthurerstrasse 190, CH-8037, Zurich, Switzerland ; H.Furukawa ; Center for Reticular Chemistry, Department of Chemistry and Biochemistry, University of California-Los Angeles, 607 Charles E. Young Drive East, Los Angeles, California 90095 ; O.Blacque ; Anorganisch-Chemisches Institut, Universitat Zurich, Winterthurerstrasse 190, CH-8037, Zurich, Switzerland ; K.Venkatesan ; Anorganisch-Chemisches Institut, Universitat Zurich, Winterthurerstrasse 190, CH-8037, Zurich, Switzerland ; O.M.Yaghi ; Center for Reticular Chemistry, Department of Chemistry and Biochemistry, University of California-Los Angeles, 607 Charles E. Young Drive East, Los Angeles, California 90095 ; G.-X.Jin ; Shanghai Key Laboratory of Molecular Catalysis and Innovative Material, Department of Chemistry, Fudan University, 200433, Shanghai, P. R. China ; ; H.Berke ; ; Anorganisch-Chemisches Institut, Universitat Zurich, Winterthurerstrasse 190, CH-8037, Zurich, Switzerland ; _publ_contact_author_name 'Dr. Blacque, Olivier' #============================================================================== data_MOF-647A _database_code_depnum_ccdc_archive 'CCDC 829034' #TrackingRef '- CIFs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C15.71 H21.51 Cu3 N5.90 O13' _chemical_formula_sum 'C15.71 H21.51 Cu3 N5.90 O13' _chemical_formula_weight 691.65 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'I 41/a c d' _symmetry_space_group_name_Hall '-I 4bd 2c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+1/4, x+3/4, z+1/4' 'y+1/4, -x+1/4, z+3/4' '-x+1/2, y, -z' 'x, -y, -z+1/2' 'y+1/4, x+3/4, -z+3/4' '-y+1/4, -x+1/4, -z+1/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+3/4, x+5/4, z+3/4' 'y+3/4, -x+3/4, z+5/4' '-x+1, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1' 'y+3/4, x+5/4, -z+5/4' '-y+3/4, -x+3/4, -z+3/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-1/4, -x-3/4, -z-1/4' '-y-1/4, x-1/4, -z-3/4' 'x-1/2, -y, z' '-x, y, z-1/2' '-y-1/4, -x-3/4, z-3/4' 'y-1/4, x-1/4, z-1/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y+1/4, -x-1/4, -z+1/4' '-y+1/4, x+1/4, -z-1/4' 'x, -y+1/2, z+1/2' '-x+1/2, y+1/2, z' '-y+1/4, -x-1/4, z-1/4' 'y+1/4, x+1/4, z+1/4' _cell_length_a 17.6342(6) _cell_length_b 17.6342(6) _cell_length_c 33.4999(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 10417.3(6) _cell_formula_units_Z 16 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 2770 _cell_measurement_theta_min 2.4263 _cell_measurement_theta_max 24.9984 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.762 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5568.8 _exptl_absorpt_coefficient_mu 2.499 _exptl_absorpt_correction_T_min 0.604 _exptl_absorpt_correction_T_max 0.788 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; Oxford Diffraction (2007). Oxford Diffraction Ltd., Xcalibur CCD system ; _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 10.4498 _diffrn_standards_number 2 _diffrn_standards_interval_count 50 _diffrn_standards_interval_time 180 _diffrn_standards_decay_% 0 _diffrn_reflns_number 24570 _diffrn_reflns_av_R_equivalents 0.1413 _diffrn_reflns_av_sigmaI/netI 0.1496 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 2.43 _diffrn_reflns_theta_max 25.68 _reflns_number_total 2480 _reflns_number_gt 978 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) ; _computing_structure_solution ; SHELXS97. Program for Crystal Structure solution. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122. ; _computing_structure_refinement ; SHELXL97. Program for crystal structure refinement. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122. ; _computing_molecular_graphics ; ORTEP-3 for Windows, Version 2.01. Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565. ; _computing_publication_material ; WinGX -- An integrated system of Windows programs for the solution, refinment and analysis of single crystal X-ray diffraction data, Version 1.80.00. Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837-838. SHELXL97. Program for crystal structure refinement. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122. PLATON for Windows, Version 1.12. Spek, A. L. (2003). J. Appl. Cryst. 36, 7-13. ; _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 'w=1/[\s^2^(Fo^2^)+(0.0422P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2480 _refine_ls_number_parameters 181 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.1357 _refine_ls_R_factor_gt 0.0399 _refine_ls_wR_factor_ref 0.0930 _refine_ls_wR_factor_gt 0.0800 _refine_ls_goodness_of_fit_ref 0.738 _refine_ls_restrained_S_all 0.737 _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 C1 C 0.4622(4) 0.3988(4) 1.05050(15) 0.0436(17) Uani 1 1 d . . . C2 C 0.4764(4) 0.4081(3) 1.01061(15) 0.0471(18) Uani 1 1 d . . . H2 H 0.5230 0.4073 0.9976 0.056 Uiso 1 1 calc R . . C3 C 0.4058(4) 0.4188(3) 0.99434(15) 0.0380(15) Uani 1 1 d . . . C4 C 0.3774(4) 0.4290(3) 0.95271(16) 0.0428(17) Uani 1 1 d . . . C5 C 0.5117(4) 0.3885(4) 1.08575(17) 0.0455(18) Uani 1 1 d . . . N1 N 0.3874(3) 0.4044(3) 1.05787(11) 0.0433(15) Uani 1 1 d . A . N2 N 0.3516(3) 0.4157(2) 1.02250(12) 0.0371(13) Uani 1 1 d . . . O1 O 0.2577(3) 0.3628(3) 1.10834(11) 0.0633(13) Uani 1 1 d D A . H1A H 0.236(3) 0.387(3) 1.0911(14) 0.076 Uiso 1 1 d D . . H1B H 0.237(3) 0.362(4) 1.1300(9) 0.076 Uiso 1 1 d D . . O2 O 0.5800(3) 0.3902(2) 1.08274(10) 0.0503(12) Uani 1 1 d . . . O3A O 0.3665(10) 0.4969(12) 1.1394(5) 0.084(3) Uani 0.451(6) 1 d P A 1 N4 N 0.4181(9) 0.6071(8) 1.1596(4) 0.084(3) Uani 0.451(6) 1 d P A 1 C8 C 0.4159(11) 0.5423(10) 1.1428(5) 0.084(3) Uani 0.451(6) 1 d P A 1 H8 H 0.4614 0.5279 1.1309 0.101 Uiso 0.451(6) 1 calc PR A 1 C9 C 0.3516(10) 0.6358(9) 1.1782(5) 0.084(3) Uani 0.451(6) 1 d P A 1 H9A H 0.3620 0.6849 1.1893 0.126 Uiso 0.451(6) 1 calc PR A 1 H9B H 0.3360 0.6019 1.1990 0.126 Uiso 0.451(6) 1 calc PR A 1 H9C H 0.3118 0.6400 1.1587 0.126 Uiso 0.451(6) 1 calc PR A 1 C10 C 0.4769(9) 0.6528(9) 1.1637(5) 0.084(3) Uani 0.451(6) 1 d P A 1 H10A H 0.4615 0.6978 1.1777 0.126 Uiso 0.451(6) 1 calc PR A 1 H10B H 0.4960 0.6664 1.1379 0.126 Uiso 0.451(6) 1 calc PR A 1 H10C H 0.5160 0.6275 1.1786 0.126 Uiso 0.451(6) 1 calc PR A 1 O3B O 0.3326(6) 0.4899(9) 1.1462(4) 0.084(3) Uani 0.549(6) 1 d PD A 2 H3A H 0.290(2) 0.499(4) 1.139(3) 0.101 Uiso 0.549(6) 1 d PD A 2 H3B H 0.353(5) 0.5231(12) 1.133(2) 0.101 Uiso 0.549(6) 1 d PD A 2 O4 O 0.4763(2) 0.3821(2) 1.11925(11) 0.0530(11) Uani 1 1 d . A . O5 O 0.4229(2) 0.4283(2) 0.92440(10) 0.0529(13) Uani 1 1 d . . . O6 O 0.3056(3) 0.4363(2) 0.94993(10) 0.0486(11) Uani 1 1 d . . . Cu1 Cu 0.36495(5) 0.38031(5) 1.114916(18) 0.0498(3) Uani 1 1 d D . . Cu2 Cu 0.2500 0.43729(6) 1.0000 0.0393(3) Uani 1 2 d S . . C6 C 0.2768(9) 0.6050(8) 0.9930(4) 0.069(2) Uani 0.50 1 d P . . H6 H 0.3074 0.5886 0.9721 0.083 Uiso 0.50 1 calc PR . . C7A C 0.2236(8) 0.7184(8) 1.0305(4) 0.069(2) Uani 0.50 1 d P . . H7A1 H 0.2193 0.7715 1.0247 0.104 Uiso 0.50 1 calc PR . . H7A2 H 0.2468 0.7118 1.0562 0.104 Uiso 0.50 1 calc PR . . H7A3 H 0.1741 0.6958 1.0306 0.104 Uiso 0.50 1 calc PR . . C7B C 0.3213(9) 0.7337(8) 0.9795(4) 0.069(2) Uani 0.50 1 d P . . H7B1 H 0.3034 0.7847 0.9830 0.104 Uiso 0.50 1 calc PR . . H7B2 H 0.3227 0.7217 0.9516 0.104 Uiso 0.50 1 calc PR . . H7B3 H 0.3713 0.7291 0.9906 0.104 Uiso 0.50 1 calc PR . . O7 O 0.2454(8) 0.5590(5) 1.0123(2) 0.069(2) Uani 0.50 1 d P . . N3 N 0.2707(6) 0.6817(5) 0.9998(5) 0.069(2) 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 C1 0.045(5) 0.066(5) 0.020(3) 0.012(3) -0.006(3) -0.013(4) C2 0.053(5) 0.060(5) 0.029(4) 0.000(3) 0.001(3) 0.000(4) C3 0.047(4) 0.044(4) 0.023(3) 0.001(3) -0.001(3) 0.001(3) C4 0.058(5) 0.045(4) 0.025(3) 0.005(3) -0.007(3) 0.002(4) C5 0.052(5) 0.062(5) 0.023(3) 0.007(3) 0.000(3) 0.001(4) N1 0.066(4) 0.051(4) 0.013(2) 0.009(2) -0.008(2) -0.004(3) N2 0.050(4) 0.039(3) 0.023(2) 0.003(2) 0.000(2) -0.003(2) O1 0.055(3) 0.100(4) 0.035(3) 0.023(3) 0.016(2) 0.018(3) O2 0.055(3) 0.074(3) 0.021(2) 0.012(2) -0.009(2) -0.003(3) O3A 0.084(8) 0.071(4) 0.097(4) -0.024(3) -0.014(5) 0.008(5) N4 0.084(8) 0.071(4) 0.097(4) -0.024(3) -0.014(5) 0.008(5) C8 0.084(8) 0.071(4) 0.097(4) -0.024(3) -0.014(5) 0.008(5) C9 0.084(8) 0.071(4) 0.097(4) -0.024(3) -0.014(5) 0.008(5) C10 0.084(8) 0.071(4) 0.097(4) -0.024(3) -0.014(5) 0.008(5) O3B 0.084(8) 0.071(4) 0.097(4) -0.024(3) -0.014(5) 0.008(5) O4 0.060(3) 0.071(3) 0.028(2) 0.010(2) -0.007(2) -0.008(2) O5 0.054(3) 0.084(4) 0.021(2) 0.010(2) 0.004(2) 0.007(3) O6 0.045(3) 0.077(3) 0.024(2) 0.010(2) -0.0033(19) 0.007(3) Cu1 0.0669(6) 0.0624(6) 0.0202(3) 0.0076(4) 0.0024(4) 0.0001(5) Cu2 0.0487(7) 0.0470(7) 0.0222(4) 0.000 -0.0017(5) 0.000 C6 0.088(6) 0.058(4) 0.062(4) 0.006(3) 0.012(5) 0.004(3) C7A 0.088(6) 0.058(4) 0.062(4) 0.006(3) 0.012(5) 0.004(3) C7B 0.088(6) 0.058(4) 0.062(4) 0.006(3) 0.012(5) 0.004(3) O7 0.088(6) 0.058(4) 0.062(4) 0.006(3) 0.012(5) 0.004(3) N3 0.088(6) 0.058(4) 0.062(4) 0.006(3) 0.012(5) 0.004(3) _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 C1 N1 1.346(7) . ? C1 C2 1.369(7) . ? C1 C5 1.479(8) . ? C2 C3 1.372(8) . ? C2 H2 0.9300 . ? C3 N2 1.344(7) . ? C3 C4 1.493(7) . ? C4 O5 1.243(7) . ? C4 O6 1.276(7) . ? C5 O2 1.209(7) . ? C5 O4 1.288(6) . ? N1 N2 1.358(5) . ? N1 Cu1 1.997(4) . ? N2 Cu2 1.981(5) . ? O1 Cu1 1.928(5) . ? O1 H1A 0.81(5) . ? O1 H1B 0.81(4) . ? O2 Cu1 1.967(3) 27_567 ? O3A C8 1.19(2) . ? O3A Cu1 2.21(2) . ? N4 C8 1.275(18) . ? N4 C10 1.322(19) . ? N4 C9 1.420(19) . ? C8 H8 0.9300 . ? C8 H3B 1.20(10) . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? O3B Cu1 2.271(15) . ? O3B H3A 0.814(10) . ? O3B H3B 0.816(10) . ? O4 Cu1 1.970(4) . ? O6 Cu2 1.943(4) . ? Cu1 O2 1.967(3) 20_658 ? Cu2 O6 1.943(4) 5_557 ? Cu2 N2 1.981(5) 5_557 ? Cu2 O7 2.187(8) . ? Cu2 O7 2.187(8) 5_557 ? C6 O7 1.177(14) . ? C6 N3 1.377(15) . ? C6 H6 0.9300 . ? C7A N3 1.471(18) . ? C7A H7A1 0.9600 . ? C7A H7A2 0.9600 . ? C7A H7A3 0.9600 . ? C7B N3 1.448(16) . ? C7B H7B1 0.9600 . ? C7B H7B2 0.9600 . ? C7B H7B3 0.9600 . ? N3 C6 1.610(15) 5_557 ? 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 N1 C1 C2 110.5(5) . . ? N1 C1 C5 116.1(5) . . ? C2 C1 C5 133.3(6) . . ? C1 C2 C3 103.8(6) . . ? C1 C2 H2 128.1 . . ? C3 C2 H2 128.1 . . ? N2 C3 C2 111.2(5) . . ? N2 C3 C4 114.9(6) . . ? C2 C3 C4 133.8(6) . . ? O5 C4 O6 125.9(5) . . ? O5 C4 C3 119.7(6) . . ? O6 C4 C3 114.4(5) . . ? O2 C5 O4 123.8(5) . . ? O2 C5 C1 121.2(6) . . ? O4 C5 C1 114.9(6) . . ? C1 N1 N2 107.9(4) . . ? C1 N1 Cu1 110.8(3) . . ? N2 N1 Cu1 140.7(4) . . ? C3 N2 N1 106.7(5) . . ? C3 N2 Cu2 111.6(4) . . ? N1 N2 Cu2 141.4(4) . . ? Cu1 O1 H1A 118(5) . . ? Cu1 O1 H1B 110(5) . . ? H1A O1 H1B 115(7) . . ? C5 O2 Cu1 111.9(4) . 27_567 ? C8 O3A Cu1 132.0(15) . . ? C8 O3A H3A 136(3) . . ? Cu1 O3A H3A 90.4(19) . . ? C8 O3A H3B 77(10) . . ? Cu1 O3A H3B 129(10) . . ? H3A O3A H3B 64(5) . . ? C8 N4 C10 128.0(19) . . ? C8 N4 C9 119.3(17) . . ? C10 N4 C9 112.6(15) . . ? O3A C8 N4 132(2) . . ? O3A C8 H8 114.1 . . ? N4 C8 H8 114.1 . . ? N4 C8 H3B 113(2) . . ? H8 C8 H3B 127.2 . . ? N4 C9 H9A 109.5 . . ? N4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N4 C10 H10A 109.5 . . ? N4 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? N4 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? Cu1 O3B H3A 105(2) . . ? Cu1 O3B H3B 105(2) . . ? H3A O3B H3B 96(2) . . ? C5 O4 Cu1 114.8(4) . . ? C4 O6 Cu2 116.0(3) . . ? O1 Cu1 O2 89.10(17) . 20_658 ? O1 Cu1 O4 171.3(2) . . ? O2 Cu1 O4 89.28(17) 20_658 . ? O1 Cu1 N1 96.86(19) . . ? O2 Cu1 N1 163.3(2) 20_658 . ? O4 Cu1 N1 82.49(19) . . ? O1 Cu1 O3A 101.7(5) . . ? O2 Cu1 O3A 95.1(5) 20_658 . ? O4 Cu1 O3A 86.9(5) . . ? N1 Cu1 O3A 98.9(5) . . ? O1 Cu1 O3B 86.7(3) . . ? O2 Cu1 O3B 87.7(4) 20_658 . ? O4 Cu1 O3B 101.7(3) . . ? N1 Cu1 O3B 108.1(4) . . ? O3A Cu1 O3B 16.6(6) . . ? O6 Cu2 O6 179.0(3) 5_557 . ? O6 Cu2 N2 82.56(17) 5_557 5_557 ? O6 Cu2 N2 97.25(17) . 5_557 ? O6 Cu2 N2 97.25(17) 5_557 . ? O6 Cu2 N2 82.56(17) . . ? N2 Cu2 N2 157.9(3) 5_557 . ? O6 Cu2 O7 80.0(2) 5_557 . ? O6 Cu2 O7 101.0(3) . . ? N2 Cu2 O7 103.1(4) 5_557 . ? N2 Cu2 O7 98.6(4) . . ? O6 Cu2 O7 101.0(3) 5_557 5_557 ? O6 Cu2 O7 80.0(2) . 5_557 ? N2 Cu2 O7 98.6(4) 5_557 5_557 ? N2 Cu2 O7 103.1(4) . 5_557 ? O7 Cu2 O7 22.2(4) . 5_557 ? O7 C6 N3 123.3(13) . . ? O7 C6 H6 118.3 . . ? N3 C6 H6 118.3 . . ? N3 C7A H7A1 109.5 . . ? N3 C7A H7A2 109.5 . . ? H7A1 C7A H7A2 109.5 . . ? N3 C7A H7A3 109.5 . . ? H7A1 C7A H7A3 109.5 . . ? H7A2 C7A H7A3 109.5 . . ? N3 C7B H7B1 109.5 . . ? N3 C7B H7B2 109.5 . . ? H7B1 C7B H7B2 109.5 . . ? N3 C7B H7B3 109.5 . . ? H7B1 C7B H7B3 109.5 . . ? H7B2 C7B H7B3 109.5 . . ? C6 O7 Cu2 123.7(8) . . ? C6 N3 C7B 119.7(13) . . ? C6 N3 C7A 126.3(12) . . ? C7B N3 C7A 113.4(10) . . ? C7B N3 C6 157.4(13) . 5_557 ? C7A N3 C6 88.3(10) . 5_557 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1A O6 0.81(5) 1.78(5) 2.596(6) 174(7) 5_557 O1 H1B O5 0.81(5) 1.91(2) 2.694(5) 161(6) 12_454 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.382 _refine_diff_density_min -0.466 _refine_diff_density_rms 0.077 #===END data_MOF-647B _database_code_depnum_ccdc_archive 'CCDC 829035' #TrackingRef '- CIFs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H22 Cu3 N4 O12' _chemical_formula_sum 'C18 H22 Cu3 N4 O12' _chemical_formula_weight 677.05 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'I 41/a c d' _symmetry_space_group_name_Hall '-I 4bd 2c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y+1/2, z' 'x, -y, -z+1/2' '-x+1/2, y, -z' '-y+1/4, -x+1/4, -z+1/4' 'y+3/4, x+1/4, -z+1/4' 'y+1/4, -x+1/4, z+3/4' '-y+1/4, x+3/4, z+1/4' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1, z+1/2' 'x+1/2, -y+1/2, -z+1' '-x+1, y+1/2, -z+1/2' '-y+3/4, -x+3/4, -z+3/4' 'y+5/4, x+3/4, -z+3/4' 'y+3/4, -x+3/4, z+5/4' '-y+3/4, x+5/4, z+3/4' '-x, -y, -z' 'x, y-1/2, -z' '-x, y, z-1/2' 'x-1/2, -y, z' 'y-1/4, x-1/4, z-1/4' '-y-3/4, -x-1/4, z-1/4' '-y-1/4, x-1/4, -z-3/4' 'y-1/4, -x-3/4, -z-1/4' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y, -z+1/2' '-x+1/2, y+1/2, z' 'x, -y+1/2, z+1/2' 'y+1/4, x+1/4, z+1/4' '-y-1/4, -x+1/4, z+1/4' '-y+1/4, x+1/4, -z-1/4' 'y+1/4, -x-1/4, -z+1/4' _cell_length_a 17.1637(5) _cell_length_b 17.1637(5) _cell_length_c 34.0665(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 10035.7(5) _cell_formula_units_Z 16 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 3219 _cell_measurement_theta_min 2.65 _cell_measurement_theta_max 30.81 _exptl_crystal_description plate _exptl_crystal_colour blue _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.792 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5456 _exptl_absorpt_coefficient_mu 2.587 _exptl_absorpt_correction_T_min 0.746 _exptl_absorpt_correction_T_max 0.917 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; Goniometer Xcalibur, detector: Ruby Oxford Diffraction (2007). Oxford Diffraction Ltd., Xcalibur CCD system ; _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 10.4498 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 11076 _diffrn_reflns_av_R_equivalents 0.0433 _diffrn_reflns_av_sigmaI/netI 0.0647 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_theta_min 2.66 _diffrn_reflns_theta_max 25.68 _reflns_number_total 2325 _reflns_number_gt 1155 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_structure_solution ; SHELXS97. Program for Crystal Structure solution. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122. ; _computing_structure_refinement ; SHELXL97. Program for crystal structure refinement. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122. ; _computing_molecular_graphics ; ORTEP-3 for Windows, Version 2.01. Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565. ; _computing_publication_material ; WinGX -- An integrated system of Windows programs for the solution, refinment and analysis of single crystal X-ray diffraction data, Version 1.80.00. Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837-838. SHELXL97. Program for crystal structure refinement. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122. PLATON for Windows, Version 1.12. Spek, A. L. (2003). J. Appl. Cryst. 36, 7-13. ; _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 'w=1/[\s^2^(Fo^2^)+(0.1552P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2325 _refine_ls_number_parameters 158 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1319 _refine_ls_R_factor_gt 0.0731 _refine_ls_wR_factor_ref 0.2363 _refine_ls_wR_factor_gt 0.2122 _refine_ls_goodness_of_fit_ref 0.921 _refine_ls_restrained_S_all 0.921 _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 C1 C 0.3658(5) 0.2693(6) 0.16539(17) 0.049(2) Uani 1 1 d . . . C2 C 0.3570(5) 0.2183(5) 0.20016(19) 0.053(2) Uani 1 1 d . . . C3 C 0.3472(5) 0.2336(5) 0.24012(18) 0.049(2) Uani 1 1 d . . . H3 H 0.3461 0.2815 0.2528 0.059 Uiso 1 1 calc R . . C4 C 0.3397(5) 0.1608(5) 0.25596(19) 0.052(2) Uani 1 1 d . . . C5 C 0.3303(6) 0.1294(5) 0.2967(2) 0.053(2) Uani 1 1 d . . . C6 C 0.5308(8) 0.0574(8) 0.2317(5) 0.141(6) Uani 1 1 d . . . H6A H 0.5154 0.1091 0.2402 0.170 Uiso 1 1 calc R . . H6B H 0.5260 0.0543 0.2034 0.170 Uiso 1 1 calc R . . C7 C 0.6115(8) 0.0403(9) 0.2441(5) 0.143(7) Uani 1 1 d . . . H7A H 0.6474 0.0484 0.2225 0.172 Uiso 1 1 calc R . . H7B H 0.6266 0.0736 0.2657 0.172 Uiso 1 1 calc R . . N1 N 0.3558(4) 0.1422(4) 0.19335(17) 0.055(2) Uani 1 1 d . . . N2 N 0.3455(5) 0.1054(4) 0.22763(17) 0.054(2) Uani 1 1 d . . . O1 O 0.3706(4) 0.2342(4) 0.13261(13) 0.0627(18) Uani 1 1 d . . . O2 O 0.3647(4) 0.3408(4) 0.16825(14) 0.0560(16) Uani 1 1 d . . . O3 O 0.3298(4) 0.0566(4) 0.29896(14) 0.0648(18) Uani 1 1 d . . . O4 O 0.3208(4) 0.1753(4) 0.32494(14) 0.0681(19) Uani 1 1 d . . . O5 O 0.4845(6) 0.0000 0.2500 0.082(3) Uani 1 2 d S . . O6 O 0.3767(6) 0.0094(4) 0.13807(19) 0.108(3) Uani 1 1 d . . . H1 H 0.3818 -0.0060 0.1116 0.162 Uiso 1 1 d . . . H2 H 0.3686 -0.0159 0.1570 0.162 Uiso 1 1 d . . . Cu1 Cu 0.37019(7) 0.11986(7) 0.13648(3) 0.0628(5) Uani 1 1 d . . . Cu2 Cu 0.34815(10) 0.0000 0.2500 0.0558(6) Uani 1 2 d S . . O7 O 0.2373(7) 0.1138(11) 0.1171(7) 0.147(7) Uani 0.50 1 d PG . . C8 C 0.1907(12) 0.1821(9) 0.1168(7) 0.147(7) Uani 0.50 1 d PG . . H8A H 0.1953 0.2092 0.1416 0.177 Uiso 0.50 1 calc PR . . H8B H 0.2078 0.2169 0.0960 0.177 Uiso 0.50 1 calc PR . . C9 C 0.1122(10) 0.1594(13) 0.1103(8) 0.147(7) Uani 0.50 1 d PG . . H9A H 0.0799 0.1758 0.1322 0.177 Uiso 0.50 1 calc PR . . H9B H 0.0924 0.1835 0.0866 0.177 Uiso 0.50 1 calc PR . . C10 C 0.1103(8) 0.0770(13) 0.1067(8) 0.147(7) Uani 0.50 1 d PG . . H10A H 0.0896 0.0624 0.0812 0.177 Uiso 0.50 1 calc PR . . H10B H 0.0771 0.0548 0.1268 0.177 Uiso 0.50 1 calc PR . . C11 C 0.1876(10) 0.0488(9) 0.1109(8) 0.147(7) Uani 0.50 1 d PG . . H11A H 0.2033 0.0210 0.0874 0.177 Uiso 0.50 1 calc PR . . H11B H 0.1908 0.0133 0.1330 0.177 Uiso 0.50 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.069(6) 0.063(6) 0.014(3) 0.000(4) 0.002(3) 0.014(5) C2 0.079(7) 0.056(6) 0.023(3) 0.002(3) 0.007(3) 0.011(5) C3 0.081(6) 0.049(5) 0.018(3) 0.001(3) 0.009(3) 0.015(5) C4 0.079(6) 0.057(6) 0.020(3) -0.005(4) 0.005(4) 0.012(5) C5 0.078(7) 0.057(6) 0.024(4) 0.000(4) 0.007(4) 0.004(5) C6 0.079(10) 0.130(12) 0.215(17) 0.072(12) 0.030(10) -0.004(9) C7 0.098(11) 0.129(12) 0.203(17) 0.090(13) 0.010(11) -0.003(9) N1 0.085(6) 0.062(5) 0.018(3) 0.001(3) 0.006(3) 0.010(4) N2 0.087(5) 0.058(4) 0.018(3) 0.003(3) -0.004(3) 0.000(4) O1 0.105(5) 0.057(4) 0.027(3) 0.008(3) 0.003(3) 0.009(3) O2 0.087(5) 0.063(4) 0.018(2) 0.003(3) 0.001(2) 0.001(4) O3 0.118(6) 0.055(4) 0.022(2) 0.003(2) 0.005(3) 0.000(4) O4 0.102(5) 0.080(4) 0.022(2) -0.004(3) 0.018(3) -0.001(4) O5 0.080(7) 0.077(7) 0.088(6) 0.026(6) 0.000 0.000 O6 0.210(9) 0.081(5) 0.032(3) -0.011(3) 0.043(4) -0.028(5) Cu1 0.0970(11) 0.0700(9) 0.0215(5) -0.0010(4) 0.0121(5) 0.0019(7) Cu2 0.0942(13) 0.0552(10) 0.0179(6) 0.0005(6) 0.000 0.000 O7 0.091(8) 0.173(14) 0.177(16) -0.063(12) -0.011(10) -0.041(8) C8 0.091(8) 0.173(14) 0.177(16) -0.063(12) -0.011(10) -0.041(8) C9 0.091(8) 0.173(14) 0.177(16) -0.063(12) -0.011(10) -0.041(8) C10 0.091(8) 0.173(14) 0.177(16) -0.063(12) -0.011(10) -0.041(8) C11 0.091(8) 0.173(14) 0.177(16) -0.063(12) -0.011(10) -0.041(8) _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 C1 O2 1.232(10) . ? C1 O1 1.272(8) . ? C1 C2 1.480(10) . ? C2 N1 1.326(11) . ? C2 C3 1.397(9) . ? C3 C4 1.367(11) . ? C3 H3 0.9300 . ? C4 N2 1.359(10) . ? C4 C5 1.497(10) . ? C5 O3 1.251(10) . ? C5 O4 1.255(9) . ? C6 O5 1.411(13) . ? C6 C7 1.476(18) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C7 1.44(3) 3 ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? N1 N2 1.340(8) . ? N1 Cu1 1.991(6) . ? N2 Cu2 1.963(6) . ? O1 Cu1 1.967(6) . ? O2 Cu1 1.983(5) 32_565 ? O3 Cu2 1.956(5) . ? O5 C6 1.411(13) 3 ? O5 Cu2 2.340(10) . ? O6 Cu1 1.900(7) . ? O6 H1 0.94 . ? O6 H2 0.79 . ? Cu1 O2 1.983(5) 23_656 ? Cu1 O7 2.376(13) . ? Cu2 O3 1.956(5) 3 ? Cu2 N2 1.963(6) 3 ? O7 C8 1.4200 . ? O7 C11 1.4200 . ? C8 C9 1.4200 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.4200 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.4200 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? 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 O2 C1 O1 122.9(7) . . ? O2 C1 C2 121.7(6) . . ? O1 C1 C2 115.4(8) . . ? N1 C2 C3 110.7(7) . . ? N1 C2 C1 116.4(6) . . ? C3 C2 C1 132.9(8) . . ? C4 C3 C2 102.9(7) . . ? C4 C3 H3 128.5 . . ? C2 C3 H3 128.5 . . ? N2 C4 C3 110.6(6) . . ? N2 C4 C5 114.5(7) . . ? C3 C4 C5 134.8(7) . . ? O3 C5 O4 125.4(7) . . ? O3 C5 C4 114.7(7) . . ? O4 C5 C4 119.9(8) . . ? O5 C6 C7 105.3(11) . . ? O5 C6 H6A 110.7 . . ? C7 C6 H6A 110.7 . . ? O5 C6 H6B 110.7 . . ? C7 C6 H6B 110.7 . . ? H6A C6 H6B 108.8 . . ? C7 C7 C6 105.7(9) 3 . ? C7 C7 H7A 110.6 3 . ? C6 C7 H7A 110.6 . . ? C7 C7 H7B 110.6 3 . ? C6 C7 H7B 110.6 . . ? H7A C7 H7B 108.7 . . ? C2 N1 N2 108.3(6) . . ? C2 N1 Cu1 111.0(5) . . ? N2 N1 Cu1 140.7(6) . . ? N1 N2 C4 107.4(6) . . ? N1 N2 Cu2 140.4(5) . . ? C4 N2 Cu2 111.8(5) . . ? C1 O1 Cu1 114.4(5) . . ? C1 O2 Cu1 105.2(4) . 32_565 ? C5 O3 Cu2 116.3(4) . . ? C6 O5 C6 111.4(13) 3 . ? C6 O5 Cu2 124.3(7) 3 . ? C6 O5 Cu2 124.3(7) . . ? Cu1 O6 H1 105 . . ? Cu1 O6 H2 124 . . ? H1 O6 H2 130 . . ? O6 Cu1 O1 175.8(3) . . ? O6 Cu1 O2 87.9(3) . 23_656 ? O1 Cu1 O2 88.9(2) . 23_656 ? O6 Cu1 N1 99.9(3) . . ? O1 Cu1 N1 82.7(3) . . ? O2 Cu1 N1 165.0(3) 23_656 . ? O6 Cu1 O7 91.2(5) . . ? O1 Cu1 O7 91.7(5) . . ? O2 Cu1 O7 93.5(6) 23_656 . ? N1 Cu1 O7 99.2(6) . . ? O3 Cu2 O3 161.5(4) 3 . ? O3 Cu2 N2 97.1(2) 3 . ? O3 Cu2 N2 82.5(2) . . ? O3 Cu2 N2 82.5(2) 3 3 ? O3 Cu2 N2 97.1(2) . 3 ? N2 Cu2 N2 177.3(5) . 3 ? O3 Cu2 O5 99.3(2) 3 . ? O3 Cu2 O5 99.3(2) . . ? N2 Cu2 O5 91.3(2) . . ? N2 Cu2 O5 91.3(2) 3 . ? C8 O7 C11 108.0 . . ? C8 O7 Cu1 120.4(10) . . ? C11 O7 Cu1 130.7(10) . . ? C9 C8 O7 108.0 . . ? C9 C8 H8A 110.1 . . ? O7 C8 H8A 110.1 . . ? C9 C8 H8B 110.1 . . ? O7 C8 H8B 110.1 . . ? H8A C8 H8B 108.4 . . ? C10 C9 C8 108.0 . . ? C10 C9 H9A 110.1 . . ? C8 C9 H9A 110.1 . . ? C10 C9 H9B 110.1 . . ? C8 C9 H9B 110.1 . . ? H9A C9 H9B 108.4 . . ? C9 C10 C11 108.0 . . ? C9 C10 H10A 110.1 . . ? C11 C10 H10A 110.1 . . ? C9 C10 H10B 110.1 . . ? C11 C10 H10B 110.1 . . ? H10A C10 H10B 108.4 . . ? C10 C11 O7 108.0 . . ? C10 C11 H11A 110.1 . . ? O7 C11 H11A 110.1 . . ? C10 C11 H11B 110.1 . . ? O7 C11 H11B 110.1 . . ? H11A C11 H11B 108.4 . . ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 2.318 _refine_diff_density_min -0.906 _refine_diff_density_rms 0.146 #===END data_MOF-648 _database_code_depnum_ccdc_archive 'CCDC 829036' #TrackingRef '- CIFs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C67 H71 Cu12 N25 O41, 2(C3 H7 N O), 2(O)' _chemical_formula_sum 'C73 H85 Cu12 N27 O45' _chemical_formula_weight 2823.28 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' Cu Cu 0.3201 1.2651 '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 b c m' _symmetry_space_group_name_Hall '-P 2c 2b' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, y, -z-1/2' '-x, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 15.3345(1) _cell_length_b 14.5465(1) _cell_length_c 26.2229(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5849.37(9) _cell_formula_units_Z 2 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 26187 _cell_measurement_theta_min 2.3252 _cell_measurement_theta_max 32.7325 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.603 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2840 _exptl_absorpt_coefficient_mu 2.224 _exptl_absorpt_correction_T_min 0.591 _exptl_absorpt_correction_T_max 0.741 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; Oxford Diffraction (2007). Oxford Diffraction Ltd., Xcalibur CCD system ; _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 10.4498 _diffrn_standards_number 2 _diffrn_standards_interval_count 50 _diffrn_standards_interval_time 90 _diffrn_standards_decay_% 0 _diffrn_reflns_number 87527 _diffrn_reflns_av_R_equivalents 0.0721 _diffrn_reflns_av_sigmaI/netI 0.0520 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 2.48 _diffrn_reflns_theta_max 30.51 _reflns_number_total 9101 _reflns_number_gt 6196 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) ; _computing_structure_solution ; SHELXS97. Program for Crystal Structure solution. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122. ; _computing_structure_refinement ; SHELXL97. Program for crystal structure refinement. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122. ; _computing_molecular_graphics ; ORTEP-3 for Windows, Version 2.01. Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565. ; _computing_publication_material ; WinGX -- An integrated system of Windows programs for the solution, refinment and analysis of single crystal X-ray diffraction data, Version 1.80.00. Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837-838. SHELXL97. Program for crystal structure refinement. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122. PLATON for Windows, Version 1.12. Spek, A. L. (2003). J. Appl. Cryst. 36, 7-13. ; _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 'w=1/[\s^2^(Fo^2^)+(0.1162P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9101 _refine_ls_number_parameters 363 _refine_ls_number_restraints 16 _refine_ls_R_factor_all 0.0773 _refine_ls_R_factor_gt 0.0535 _refine_ls_wR_factor_ref 0.1820 _refine_ls_wR_factor_gt 0.1738 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _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 C1 C 0.2654(3) 0.8524(3) 0.59122(15) 0.0262(8) Uani 1 1 d . . . C2 C 0.2059(2) 0.8051(3) 0.62177(15) 0.0253(8) Uani 1 1 d . . . H2 H 0.2032 0.7424 0.6285 0.030 Uiso 1 1 calc R . . C3 C 0.1512(3) 0.8750(3) 0.63978(15) 0.0250(8) Uani 1 1 d . . . C4 C 0.3442(2) 0.8331(2) 0.55970(14) 0.0227(7) Uani 1 1 d . . . C5 C 0.0782(2) 0.8851(2) 0.67685(14) 0.0228(7) Uani 1 1 d . . . C6 C 0.3262(3) 1.2089(3) 0.59252(15) 0.0278(8) Uani 1 1 d . . . C7 C 0.2854(2) 1.2751(3) 0.62296(15) 0.0251(8) Uani 1 1 d . . . H7 H 0.3036 1.3348 0.6297 0.030 Uiso 1 1 calc R . . C8 C 0.2113(3) 1.2304(2) 0.64070(15) 0.0252(8) Uani 1 1 d . . . C9 C 0.4077(3) 1.1983(3) 0.56173(15) 0.0252(8) Uani 1 1 d . . . C10 C 0.1393(3) 1.2458(3) 0.67810(15) 0.0249(8) Uani 1 1 d . . . C14 C 0.3453(5) 1.0238(4) 0.4523(2) 0.0678(18) Uani 1 1 d . . . H14 H 0.4001 1.0417 0.4639 0.081 Uiso 1 1 calc R . . C15 C 0.2534(10) 0.9580(7) 0.3910(4) 0.162(6) Uani 1 1 d . . . H15A H 0.2205 0.9398 0.4205 0.243 Uiso 1 1 calc R . . H15B H 0.2592 0.9065 0.3683 0.243 Uiso 1 1 calc R . . H15C H 0.2237 1.0071 0.3738 0.243 Uiso 1 1 calc R . . C16 C 0.4196(10) 0.9703(9) 0.3748(4) 0.188(7) Uani 1 1 d . . . H16A H 0.4249 1.0167 0.3490 0.282 Uiso 1 1 calc R . . H16B H 0.4149 0.9110 0.3589 0.282 Uiso 1 1 calc R . . H16C H 0.4702 0.9715 0.3963 0.282 Uiso 1 1 calc R . . N1 N 0.1758(2) 0.9559(2) 0.62016(14) 0.0294(8) Uani 1 1 d . . . N2 N 0.2453(2) 0.9431(2) 0.59063(14) 0.0304(8) Uani 1 1 d . . . N3 N 0.2093(2) 1.1445(2) 0.62216(14) 0.0327(8) Uani 1 1 d . . . N4 N 0.2781(2) 1.1322(2) 0.59252(15) 0.0352(9) Uani 1 1 d . . . N6 N 0.3386(5) 0.9885(3) 0.40659(19) 0.0731(18) Uani 1 1 d . . . O1 O 0.38569(18) 0.90236(17) 0.54369(11) 0.0278(6) Uani 1 1 d . . . O2 O 0.36642(17) 0.75097(17) 0.55147(10) 0.0248(6) Uani 1 1 d . . . O3 O 0.05098(19) 0.96548(18) 0.68468(11) 0.0301(6) Uani 1 1 d . . . O4 O 0.05081(18) 0.81421(17) 0.69841(10) 0.0261(6) Uani 1 1 d . . . O5 O 0.42434(19) 1.11777(17) 0.54609(11) 0.0303(6) Uani 1 1 d . . . O6 O 0.45243(17) 1.26737(18) 0.55189(10) 0.0254(6) Uani 1 1 d . . . O7 O 0.09048(18) 1.17721(17) 0.68717(11) 0.0287(6) Uani 1 1 d . . . O8 O 0.13037(17) 1.32356(17) 0.69812(10) 0.0241(5) Uani 1 1 d . . . O10 O 0.2806(3) 1.0345(3) 0.48141(14) 0.0573(10) Uani 1 1 d . . . Cu1 Cu 0.11812(3) 1.06384(3) 0.64668(2) 0.02996(15) Uani 1 1 d . . . Cu2 Cu -0.03893(4) 0.82137(4) 0.7500 0.01380(13) Uani 1 2 d S . . Cu3 Cu 0.32932(3) 1.02484(3) 0.56070(2) 0.03161(15) Uani 1 1 d . . . Cu4 Cu 0.45869(4) 0.7500 0.5000 0.01359(13) Uani 1 2 d S . . O9 O 0.0258(3) 1.0901(3) 0.58146(14) 0.0552(9) Uani 1 1 d D . . C11 C 0.0581(4) 1.1065(4) 0.5371(2) 0.0609(15) Uani 1 1 d D . . H11 H 0.1185 1.1075 0.5340 0.073 Uiso 1 1 calc R . . C12 C 0.0542(6) 1.1357(5) 0.4485(3) 0.100(3) Uani 1 1 d D . . H12A H 0.1163 1.1352 0.4531 0.150 Uiso 1 1 calc R . . H12B H 0.0366 1.1939 0.4346 0.150 Uiso 1 1 calc R . . H12C H 0.0377 1.0875 0.4254 0.150 Uiso 1 1 calc R . . C13 C -0.0803(4) 1.1209(6) 0.5000(3) 0.085(2) Uani 1 1 d D . . H13A H -0.1015 1.0602 0.4926 0.128 Uiso 1 1 calc R . . H13B H -0.1042 1.1636 0.4758 0.128 Uiso 1 1 calc R . . H13C H -0.0978 1.1384 0.5338 0.128 Uiso 1 1 calc R . . N5 N 0.0123(4) 1.1218(3) 0.49660(17) 0.0640(14) Uani 1 1 d D . . O12 O 0.4026(11) 1.0162(14) 0.6582(5) 0.084(4) Uani 0.25 1 d PD . . C20 C 0.3700(14) 0.9678(11) 0.6944(7) 0.084(4) Uani 0.25 1 d PD . . H20 H 0.3857 0.9062 0.6961 0.101 Uiso 0.25 1 calc PR . . C21 C 0.3118(14) 1.0948(12) 0.7392(7) 0.084(4) Uani 0.25 1 d PD . . H21A H 0.2737 1.1050 0.7677 0.126 Uiso 0.25 1 calc PR . . H21B H 0.2895 1.1264 0.7098 0.126 Uiso 0.25 1 calc PR . . H21C H 0.3689 1.1177 0.7472 0.126 Uiso 0.25 1 calc PR . . C22 C 0.2734(14) 0.9344(14) 0.7610(7) 0.084(4) Uani 0.25 1 d PD . . H22A H 0.2404 0.9670 0.7863 0.126 Uiso 0.25 1 calc PR . . H22B H 0.3158 0.8960 0.7775 0.126 Uiso 0.25 1 calc PR . . H22C H 0.2349 0.8970 0.7409 0.126 Uiso 0.25 1 calc PR . . N8 N 0.3168(11) 0.9985(11) 0.7287(5) 0.084(4) Uani 0.25 1 d PD . . O11 O 0.3260(5) 0.9805(5) 0.2500 0.0917(13) Uani 1 2 d SD . . C17 C 0.2423(6) 0.9845(6) 0.2500 0.0917(13) Uani 1 2 d SD . . H17 H 0.2155 1.0418 0.2500 0.110 Uiso 1 2 calc SR . . C18 C 0.1009(6) 0.9205(7) 0.2500 0.0917(13) Uani 1 2 d SD . . H18A H 0.0859 0.9844 0.2474 0.138 Uiso 0.50 1 calc PR . . H18B H 0.0776 0.8958 0.2811 0.138 Uiso 0.50 1 calc PR . . H18C H 0.0768 0.8878 0.2215 0.138 Uiso 0.50 1 calc PR . . C19 C 0.2342(7) 0.8227(6) 0.2500 0.0917(13) Uani 1 2 d SD . . H19A H 0.2574 0.8101 0.2167 0.138 Uiso 0.50 1 calc PR . . H19B H 0.1919 0.7766 0.2587 0.138 Uiso 0.50 1 calc PR . . H19C H 0.2806 0.8219 0.2746 0.138 Uiso 0.50 1 calc PR . . N7 N 0.1937(5) 0.9108(5) 0.2500 0.0917(13) Uani 1 2 d SD . . O13A O 0.455(2) 1.153(2) 0.2500 0.212(13) Uiso 0.50 2 d SP A 1 O13B O 0.503(3) 1.229(3) 0.2500 0.257(17) Uiso 0.50 2 d SP B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0231(19) 0.0215(16) 0.034(2) -0.0008(15) 0.0108(16) 0.0019(14) C2 0.0212(18) 0.0256(17) 0.029(2) 0.0008(15) 0.0102(16) 0.0011(14) C3 0.0221(18) 0.0255(17) 0.0275(19) -0.0030(15) 0.0129(15) -0.0022(14) C4 0.0205(18) 0.0249(17) 0.0228(18) -0.0018(14) 0.0089(14) 0.0033(14) C5 0.0176(17) 0.0267(17) 0.0241(18) 0.0000(14) 0.0066(14) -0.0017(14) C6 0.027(2) 0.0242(17) 0.033(2) 0.0003(16) 0.0154(17) -0.0020(15) C7 0.0230(19) 0.0221(16) 0.030(2) -0.0004(15) 0.0089(16) -0.0012(14) C8 0.0234(19) 0.0232(17) 0.029(2) -0.0024(14) 0.0118(16) 0.0024(14) C9 0.0202(18) 0.0274(18) 0.0279(19) 0.0005(14) 0.0101(15) -0.0004(14) C10 0.0195(18) 0.0300(18) 0.0253(19) 0.0000(15) 0.0077(14) 0.0049(15) C14 0.082(5) 0.070(4) 0.052(4) 0.015(3) 0.004(3) 0.019(4) C15 0.282(17) 0.124(8) 0.081(6) -0.025(6) 0.014(8) -0.114(10) C16 0.260(16) 0.238(13) 0.065(6) 0.045(7) 0.064(8) 0.167(12) N1 0.0271(17) 0.0249(15) 0.0360(19) -0.0008(14) 0.0202(15) 0.0015(13) N2 0.0258(17) 0.0234(15) 0.042(2) -0.0028(14) 0.0204(16) -0.0003(13) N3 0.0284(18) 0.0274(16) 0.042(2) -0.0060(15) 0.0237(16) -0.0010(14) N4 0.0290(19) 0.0287(17) 0.048(2) -0.0061(15) 0.0262(16) -0.0026(14) N6 0.131(6) 0.044(3) 0.045(3) 0.004(2) 0.004(3) 0.009(3) O1 0.0265(14) 0.0202(12) 0.0367(15) -0.0004(11) 0.0183(12) 0.0005(11) O2 0.0212(13) 0.0228(12) 0.0305(14) -0.0015(10) 0.0104(11) 0.0019(10) O3 0.0268(15) 0.0248(13) 0.0386(16) -0.0016(11) 0.0199(12) -0.0012(11) O4 0.0202(13) 0.0297(13) 0.0285(14) 0.0023(11) 0.0107(11) -0.0029(10) O5 0.0270(15) 0.0222(13) 0.0416(16) -0.0008(11) 0.0195(13) 0.0004(11) O6 0.0196(13) 0.0277(13) 0.0290(14) -0.0035(11) 0.0100(11) -0.0056(10) O7 0.0259(14) 0.0242(12) 0.0362(15) -0.0003(11) 0.0194(12) 0.0030(11) O8 0.0181(13) 0.0285(13) 0.0258(13) -0.0065(11) 0.0098(11) 0.0016(10) O10 0.069(3) 0.060(2) 0.044(2) 0.0051(17) 0.007(2) 0.001(2) Cu1 0.0258(3) 0.0235(2) 0.0406(3) -0.00210(19) 0.0202(2) -0.00039(18) Cu2 0.0103(3) 0.0168(3) 0.0143(3) 0.000 0.000 -0.0039(2) Cu3 0.0289(3) 0.0215(2) 0.0445(3) -0.0029(2) 0.0248(2) -0.00082(19) Cu4 0.0086(2) 0.0153(2) 0.0168(3) -0.0012(2) 0.000 0.000 O9 0.051(2) 0.061(2) 0.053(2) 0.0066(19) -0.0006(19) 0.0036(19) C11 0.062(4) 0.060(3) 0.061(4) -0.002(3) 0.007(3) -0.004(3) C12 0.148(9) 0.076(5) 0.076(5) 0.009(4) -0.015(5) -0.025(6) C13 0.075(5) 0.099(6) 0.080(5) 0.011(4) -0.027(4) 0.000(4) N5 0.075(4) 0.068(3) 0.049(3) 0.005(2) -0.003(3) -0.004(3) O12 0.058(6) 0.153(11) 0.041(6) 0.016(6) -0.010(4) -0.031(7) C20 0.058(6) 0.153(11) 0.041(6) 0.016(6) -0.010(4) -0.031(7) C21 0.058(6) 0.153(11) 0.041(6) 0.016(6) -0.010(4) -0.031(7) C22 0.058(6) 0.153(11) 0.041(6) 0.016(6) -0.010(4) -0.031(7) N8 0.058(6) 0.153(11) 0.041(6) 0.016(6) -0.010(4) -0.031(7) O11 0.081(3) 0.089(3) 0.105(3) 0.000 0.000 -0.002(3) C17 0.081(3) 0.089(3) 0.105(3) 0.000 0.000 -0.002(3) C18 0.081(3) 0.089(3) 0.105(3) 0.000 0.000 -0.002(3) C19 0.081(3) 0.089(3) 0.105(3) 0.000 0.000 -0.002(3) N7 0.081(3) 0.089(3) 0.105(3) 0.000 0.000 -0.002(3) _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 C1 N2 1.355(5) . ? C1 C2 1.395(5) . ? C1 C4 1.491(5) . ? C2 C3 1.400(5) . ? C2 H2 0.9300 . ? C3 N1 1.339(5) . ? C3 C5 1.489(5) . ? C4 O2 1.260(4) . ? C4 O1 1.264(4) . ? C5 O4 1.249(4) . ? C5 O3 1.259(4) . ? C6 N4 1.337(5) . ? C6 C7 1.398(5) . ? C6 C9 1.496(5) . ? C7 C8 1.389(5) . ? C7 H7 0.9300 . ? C8 N3 1.341(5) . ? C8 C10 1.495(5) . ? C9 O6 1.244(4) . ? C9 O5 1.267(4) . ? C10 O8 1.254(4) . ? C10 O7 1.270(5) . ? C14 O10 1.261(8) . ? C14 N6 1.308(8) . ? C14 H14 0.9300 . ? C15 N6 1.440(13) . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 N6 1.519(12) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? N1 N2 1.331(4) . ? N1 Cu1 1.931(3) . ? N2 Cu3 1.921(3) . ? N3 N4 1.322(4) . ? N3 Cu1 1.936(3) . ? N4 Cu3 1.937(3) . ? O1 Cu3 2.030(3) . ? O2 Cu4 1.955(3) . ? O3 Cu1 2.025(3) . ? O4 Cu2 1.932(3) . ? O5 Cu3 2.024(3) . ? O6 Cu4 1.942(3) 5_676 ? O7 Cu1 2.007(3) . ? O8 Cu2 1.954(2) 7_565 ? O10 Cu3 2.214(4) . ? Cu1 O9 2.253(4) . ? Cu2 O4 1.932(3) 6_557 ? Cu2 O8 1.954(2) 7 ? Cu2 O8 1.954(2) 4_546 ? Cu4 O6 1.942(3) 7_655 ? Cu4 O6 1.942(3) 5_676 ? Cu4 O2 1.955(3) 3_566 ? O9 C11 1.286(6) . ? C11 N5 1.294(7) . ? C11 H11 0.9300 . ? C12 N5 1.431(7) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 N5 1.423(8) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? O12 C20 1.284(6) . ? C20 N8 1.294(7) . ? C20 C22 1.95(3) 6_557 ? C20 H20 0.9300 . ? C21 N8 1.430(8) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 N8 1.424(8) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? O11 C17 1.285(7) . ? C17 N7 1.305(8) . ? C17 H17 0.9300 . ? C18 N7 1.431(8) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 N7 1.424(8) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? 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 N2 C1 C2 109.7(3) . . ? N2 C1 C4 111.2(3) . . ? C2 C1 C4 139.1(3) . . ? C1 C2 C3 103.2(3) . . ? C1 C2 H2 128.4 . . ? C3 C2 H2 128.4 . . ? N1 C3 C2 109.9(3) . . ? N1 C3 C5 112.1(3) . . ? C2 C3 C5 137.9(3) . . ? O2 C4 O1 124.2(3) . . ? O2 C4 C1 119.5(3) . . ? O1 C4 C1 116.2(3) . . ? O4 C5 O3 125.5(3) . . ? O4 C5 C3 117.8(3) . . ? O3 C5 C3 116.6(3) . . ? N4 C6 C7 109.1(3) . . ? N4 C6 C9 112.0(3) . . ? C7 C6 C9 138.9(4) . . ? C8 C7 C6 103.6(3) . . ? C8 C7 H7 128.2 . . ? C6 C7 H7 128.2 . . ? N3 C8 C7 109.4(3) . . ? N3 C8 C10 111.2(3) . . ? C7 C8 C10 139.0(3) . . ? O6 C9 O5 124.6(3) . . ? O6 C9 C6 119.3(3) . . ? O5 C9 C6 116.0(3) . . ? O8 C10 O7 124.5(3) . . ? O8 C10 C8 119.4(3) . . ? O7 C10 C8 116.1(3) . . ? O10 C14 N6 122.8(7) . . ? O10 C14 H14 118.6 . . ? N6 C14 H14 118.6 . . ? N6 C15 H15A 109.5 . . ? N6 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? N6 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N6 C16 H16A 109.5 . . ? N6 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? N6 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N2 N1 C3 109.0(3) . . ? N2 N1 Cu1 133.7(3) . . ? C3 N1 Cu1 116.6(2) . . ? N1 N2 C1 108.2(3) . . ? N1 N2 Cu3 133.5(3) . . ? C1 N2 Cu3 117.1(3) . . ? N4 N3 C8 108.7(3) . . ? N4 N3 Cu1 133.6(3) . . ? C8 N3 Cu1 117.4(3) . . ? N3 N4 C6 109.1(3) . . ? N3 N4 Cu3 133.3(3) . . ? C6 N4 Cu3 116.7(3) . . ? C14 N6 C15 116.9(7) . . ? C14 N6 C16 120.5(9) . . ? C15 N6 C16 122.1(8) . . ? C4 O1 Cu3 114.4(2) . . ? C4 O2 Cu4 108.7(2) . . ? C5 O3 Cu1 114.0(2) . . ? C5 O4 Cu2 120.8(2) . . ? C9 O5 Cu3 114.3(2) . . ? C9 O6 Cu4 115.3(2) . 5_676 ? C10 O7 Cu1 115.0(2) . . ? C10 O8 Cu2 110.8(2) . 7_565 ? C14 O10 Cu3 107.1(4) . . ? N1 Cu1 N3 92.42(13) . . ? N1 Cu1 O7 162.79(15) . . ? N3 Cu1 O7 80.22(12) . . ? N1 Cu1 O3 80.55(12) . . ? N3 Cu1 O3 163.58(15) . . ? O7 Cu1 O3 102.29(11) . . ? N1 Cu1 O9 98.76(16) . . ? N3 Cu1 O9 95.69(16) . . ? O7 Cu1 O9 97.45(13) . . ? O3 Cu1 O9 100.01(14) . . ? O4 Cu2 O4 88.86(17) 6_557 . ? O4 Cu2 O8 177.82(11) 6_557 7 ? O4 Cu2 O8 91.41(12) . 7 ? O4 Cu2 O8 91.41(12) 6_557 4_546 ? O4 Cu2 O8 177.82(11) . 4_546 ? O8 Cu2 O8 88.24(17) 7 4_546 ? N2 Cu3 N4 92.95(13) . . ? N2 Cu3 O5 166.79(14) . . ? N4 Cu3 O5 80.48(12) . . ? N2 Cu3 O1 80.33(12) . . ? N4 Cu3 O1 167.15(15) . . ? O5 Cu3 O1 103.77(10) . . ? N2 Cu3 O10 101.33(17) . . ? N4 Cu3 O10 102.52(17) . . ? O5 Cu3 O10 91.32(14) . . ? O1 Cu3 O10 89.60(14) . . ? O6 Cu4 O6 90.88(17) 7_655 5_676 ? O6 Cu4 O2 172.82(10) 7_655 3_566 ? O6 Cu4 O2 91.33(12) 5_676 3_566 ? O6 Cu4 O2 91.33(12) 7_655 . ? O6 Cu4 O2 172.82(10) 5_676 . ? O2 Cu4 O2 87.30(17) 3_566 . ? C11 O9 Cu1 118.4(4) . . ? O9 C11 N5 124.4(5) . . ? O9 C11 H11 117.8 . . ? N5 C11 H11 117.8 . . ? N5 C12 H12A 109.5 . . ? N5 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? N5 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N5 C13 H13A 109.5 . . ? N5 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? N5 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 N5 C13 119.3(5) . . ? C11 N5 C12 120.4(5) . . ? C13 N5 C12 120.3(5) . . ? O12 C20 N8 124.9(7) . . ? O12 C20 C22 151.4(14) . 6_557 ? O12 C20 H20 117.6 . . ? N8 C20 H20 117.6 . . ? C22 C20 H20 85.8 6_557 . ? N8 C21 H21A 109.5 . . ? N8 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? N8 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N8 C22 H22A 109.5 . . ? N8 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? N8 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C20 N8 C22 118.8(6) . . ? C20 N8 C21 120.3(6) . . ? C22 N8 C21 120.2(6) . . ? O11 C17 N7 122.2(8) . . ? O11 C17 H17 118.9 . . ? N7 C17 H17 118.9 . . ? N7 C18 H18A 109.5 . . ? N7 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? N7 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N7 C19 H19A 109.5 . . ? N7 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? N7 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C17 N7 C19 119.3(7) . . ? C17 N7 C18 119.2(7) . . ? C19 N7 C18 121.5(7) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 30.51 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.375 _refine_diff_density_min -2.413 _refine_diff_density_rms 0.156 #===END