# 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_mgo_mr160_01_0m _database_code_depnum_ccdc_archive 'CCDC 901474' #TrackingRef 'web_deposit_cif_file_0_RaulSanz_1352310836.mgo_mr160_01_0m.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C11.17 H18.02 Cu2 N0.25 O10' _chemical_formula_weight 442.85 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M R-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 25.9972(11) _cell_length_b 25.9972(11) _cell_length_c 6.2587(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 3663.3(3) _cell_formula_units_Z 9 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 751 _cell_measurement_theta_min 3.4 _cell_measurement_theta_max 62.4 _exptl_crystal_description rods _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.807 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2023 _exptl_absorpt_coefficient_mu 3.695 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5255 _exptl_absorpt_correction_T_max 0.9298 _exptl_absorpt_process_details 'SADABS; (Sheldrick, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BRUKER SMART APEXII CCD' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3601 _diffrn_reflns_av_R_equivalents 0.0668 _diffrn_reflns_av_sigmaI/netI 0.0781 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -5 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 5.90 _diffrn_reflns_theta_max 65.34 _reflns_number_total 1332 _reflns_number_gt 984 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2010)' _computing_cell_refinement 'APEX2 (Bruker, 2010); SAINT (Bruker, 2009)' _computing_data_reduction 'SAINT (Bruker, 2009);XPREP(Sheldrick,2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material 'APEX2 (Bruker, 2010)' _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^)+(0.0629P)^2^+0.0000P] 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 1332 _refine_ls_number_parameters 125 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0689 _refine_ls_R_factor_gt 0.0454 _refine_ls_wR_factor_ref 0.1198 _refine_ls_wR_factor_gt 0.1107 _refine_ls_goodness_of_fit_ref 0.994 _refine_ls_restrained_S_all 0.993 _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 Cu1 Cu 0.29095(3) 0.01523(3) 0.34667(11) 0.0099(3) Uani 1 1 d . . . O1 O 0.25019(14) -0.05673(14) 0.1687(5) 0.0094(7) Uani 1 1 d . . . O2 O 0.28480(15) -0.03077(15) 0.5989(6) 0.0135(8) Uani 1 1 d . . . O3 O 0.26622(15) -0.10919(15) 0.7890(5) 0.0115(8) Uani 1 1 d . . . C4 C 0.1698(2) -0.1831(2) 0.5385(8) 0.0101(11) Uani 1 1 d . . . H4 H 0.1725 -0.1939 0.6812 0.012 Uiso 1 1 calc R . . C6 C 0.2577(2) -0.0861(2) 0.6256(8) 0.0117(11) Uani 1 1 d . . . C8 C 0.2096(2) -0.1095(2) 0.2552(8) 0.0104(11) Uani 1 1 d . . . C11 C 0.2121(2) -0.1273(2) 0.4669(8) 0.0111(11) Uani 1 1 d . . . O22 O 0.0573(7) -0.1054(7) 0.853(3) 0.052(4) Uani 0.3333 1 d P . . C21 C 0.1944(5) 0.0629(5) 0.469(2) 0.048(3) Uani 0.6667 1 d P A 1 O7 O 0.2099(2) 0.0174(2) 0.4841(8) 0.0400(12) Uani 1 1 d D A 1 O12 O 0.1802(3) -0.0266(3) 0.8931(11) 0.0410(19) Uani 0.6667 1 d P B 1 C23 C 0.1896(13) 0.0078(14) 0.668(3) 0.072(8) Uiso 0.3333 1 d PD C 2 N26 N 0.162(2) 0.0246(17) 0.803(5) 0.042(12) Uiso 0.125 1 d PD C 2 C24 C 0.1446(14) -0.0151(13) 0.984(4) 0.108(9) Uiso 0.4583 1 d PD C 2 C25 C 0.151(3) 0.067(3) 0.698(10) 0.07(2) Uiso 0.125 1 d PD C 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 Cu1 0.0119(4) 0.0062(4) 0.0101(4) 0.0004(3) -0.0006(3) 0.0034(3) O1 0.0050(17) 0.0045(17) 0.0160(18) 0.0001(14) 0.0001(14) 0.0003(14) O2 0.0115(18) 0.0077(19) 0.018(2) -0.0022(14) -0.0024(15) 0.0021(16) O3 0.0095(18) 0.0093(18) 0.0111(19) -0.0006(14) -0.0002(14) 0.0011(15) C4 0.003(2) 0.011(3) 0.016(3) -0.001(2) -0.001(2) 0.004(2) C6 0.008(3) 0.012(3) 0.018(3) 0.000(2) 0.001(2) 0.007(2) C8 0.012(3) 0.013(3) 0.011(3) -0.001(2) -0.001(2) 0.010(2) C11 0.009(2) 0.011(3) 0.013(3) -0.003(2) -0.005(2) 0.005(2) O22 0.045(10) 0.030(9) 0.077(12) -0.016(8) -0.010(8) 0.015(7) C21 0.052(8) 0.050(7) 0.054(8) 0.014(6) 0.010(6) 0.034(7) O7 0.039(3) 0.045(3) 0.042(3) 0.011(2) 0.010(2) 0.025(3) O12 0.035(4) 0.040(4) 0.040(5) 0.013(3) -0.001(3) 0.013(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O2 1.938(4) . ? Cu1 O3 1.944(3) 6_554 ? Cu1 O1 1.970(3) . ? Cu1 O1 2.026(3) 6 ? Cu1 O7 2.303(5) . ? O1 C8 1.358(6) . ? O1 Cu1 2.026(3) 8_544 ? O2 C6 1.257(6) . ? O3 C6 1.261(6) . ? O3 Cu1 1.944(3) 8_545 ? C4 C8 1.385(7) 16_545 ? C4 C11 1.385(7) . ? C4 H4 0.9500 . ? C6 C11 1.506(7) . ? C8 C4 1.385(7) 16_545 ? C8 C11 1.415(7) . ? C21 O7 1.430(12) . ? C23 N26 1.311(19) . ? N26 C25 1.44(2) . ? N26 C24 1.447(19) . ? 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 Cu1 O3 170.64(15) . 6_554 ? O2 Cu1 O1 92.02(14) . . ? O3 Cu1 O1 93.68(14) 6_554 . ? O2 Cu1 O1 84.91(14) . 6 ? O3 Cu1 O1 92.66(14) 6_554 6 ? O1 Cu1 O1 156.98(13) . 6 ? O2 Cu1 O7 85.23(16) . . ? O3 Cu1 O7 86.49(16) 6_554 . ? O1 Cu1 O7 99.81(16) . . ? O1 Cu1 O7 102.65(16) 6 . ? C8 O1 Cu1 120.8(3) . . ? C8 O1 Cu1 114.9(3) . 8_544 ? Cu1 O1 Cu1 102.96(15) . 8_544 ? C6 O2 Cu1 129.8(3) . . ? C6 O3 Cu1 119.0(3) . 8_545 ? C8 C4 C11 123.0(5) 16_545 . ? C8 C4 H4 118.5 16_545 . ? C11 C4 H4 118.5 . . ? O2 C6 O3 121.4(5) . . ? O2 C6 C11 121.2(5) . . ? O3 C6 C11 117.4(4) . . ? O1 C8 C4 118.8(5) . 16_545 ? O1 C8 C11 124.3(5) . . ? C4 C8 C11 116.8(5) 16_545 . ? C4 C11 C8 120.2(5) . . ? C4 C11 C6 117.5(5) . . ? C8 C11 C6 122.3(5) . . ? C21 O7 Cu1 129.5(6) . . ? C23 N26 C25 108(4) . . ? C23 N26 C24 107(3) . . ? C25 N26 C24 143(4) . . ? _diffrn_measured_fraction_theta_max 0.947 _diffrn_reflns_theta_full 65.34 _diffrn_measured_fraction_theta_full 0.947 _refine_diff_density_max 0.561 _refine_diff_density_min -0.472 _refine_diff_density_rms 0.125 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 -0.019 101 22 ' ' 2 0.333 0.667 -0.027 95 21 ' ' 3 0.667 0.333 -0.018 95 21 ' ' _platon_squeeze_details ; ;