data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name M.Schroder 'Sihai Yang' 'Chenrong Tan' 'Alexander Blake' 'William Lewis' 'Neil Champness' 'Xiang Lin' _publ_contact_author_email m.schroder@nottingham.ac.uk _publ_contact_author_name M.Schroder data_CUTPDM #TrackingRef '- NOTT-140.cif' #8146 NOTT-140 _database_code_depnum_ccdc_archive 'CCDC 809180' _refine_special_details ; Due to the small size of the crystal, especially in its thickness (0.04 x 0.04 x 0.002 mm), and the large pore voids (\~71% - see PLATON SQUEEZE details below) contained in the structure, even data collected using synchrotron radiation showed weak diffraction, with almost no diffraction at high resolution (< 0.95 Angstrom). We believe that this represents an inherent limit of the data quality, and during the final data reduction using the Rigaku CrystalClear software the high-angle data were therefore excluded. ; 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 1 -0.012 -0.004 -0.004 8297 3175 _platon_squeeze_details ; Approximately 71% of the unit cell volume comprises a large region of disordered solvent which could not be modelled as discrete atomic sites. We employed PLATON SQUEEZE to calculate the contribution to the diffraction from the solvent region and thereby produced a set of solvent-free diffraction intensities. SQUEEZE estimated a total count of 3175 electrons per unit cell, which were assigned to be 40 DMF, 4 dioxane and 32 water molecules per unit cell. The final formula was calculated from TGA combined with elemental analysis data. ; _audit_creation_method 'enCIFer editing of SHELXL97 CIF output' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C57 H36 Cu4 O20), 10(C3 H7 N O), (C4 H8 O2), 8(H2 O)' _chemical_formula_sum 'C91 H130 Cu4 N10 O40' _chemical_formula_weight 2258.21 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' 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P 4/n c c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-y+1/2, x, z' 'y, -x+1/2, z' '-x, y+1/2, -z+1/2' 'x+1/2, -y, -z+1/2' 'y+1/2, x+1/2, -z+1/2' '-y, -x, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'y-1/2, -x, -z' '-y, x-1/2, -z' 'x, -y-1/2, z-1/2' '-x-1/2, y, z-1/2' '-y-1/2, -x-1/2, z-1/2' 'y, x, z-1/2' _cell_length_a 18.900(3) _cell_length_b 18.900(3) _cell_length_c 33.561(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 11988(3) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 752 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 20.43 _exptl_crystal_description plate _exptl_crystal_colour blue _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.002 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.251 _exptl_crystal_density_method ? _exptl_crystal_F_000 4728 _exptl_absorpt_coefficient_mu 0.779 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.839 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details 'Jacobson, R. (1998). Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.6889 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Diamond Light Source Beamline I19' _diffrn_radiation_monochromator 'silicon double crystal' _diffrn_measurement_device_type 'Rigaku Saturn724+' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 51240 _diffrn_reflns_av_R_equivalents 0.194 _diffrn_reflns_av_sigmaI/netI 0.093 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 2.40 _diffrn_reflns_theta_max 21.26 _reflns_number_total 3660 _reflns_number_gt 2142 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Rigaku CrystalClear' _computing_cell_refinement 'Rigaku CrystalClear' _computing_data_reduction 'Rigaku CrystalClear' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_publication_material 'enCIFer (Allen et al., 2004); PLATON (Spek, 2009)' _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^)+(0.012P)^2^+1.00P] 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 3660 _refine_ls_number_parameters 183 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.113 _refine_ls_R_factor_gt 0.0463 _refine_ls_wR_factor_ref 0.0773 _refine_ls_wR_factor_gt 0.0680 _refine_ls_goodness_of_fit_ref 1.00 _refine_ls_restrained_S_all 1.00 _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 0.04988(3) 0.48508(2) 0.219622(15) 0.03376(16) Uani 1 1 d . . . C1 C 0.2500 0.7500 0.5000 0.041(3) Uani 1 4 d S . . O1 O 0.08454(16) 0.55577(15) 0.29807(8) 0.0442(9) Uani 1 1 d . . . O2 O 0.13711(14) 0.49453(15) 0.24841(9) 0.0410(8) Uani 1 1 d . . . C2 C 0.2616(3) 0.6886(3) 0.47110(14) 0.0451(13) Uani 1 1 d . . . C3 C 0.3233(2) 0.6863(2) 0.44756(14) 0.0436(13) Uani 1 1 d . . . H3A H 0.3618 0.7146 0.4544 0.052 Uiso 1 1 calc R . . O3 O 0.39934(14) 0.47415(15) 0.25124(9) 0.0447(9) Uani 1 1 d . . . C4 C 0.3279(3) 0.6430(2) 0.41457(14) 0.0486(14) Uani 1 1 d . . . H4A H 0.3700 0.6414 0.4003 0.058 Uiso 1 1 calc R . . O4 O 0.45738(16) 0.52024(14) 0.30439(8) 0.0463(8) Uani 1 1 d . . . O5 O 0.09571(15) 0.43230(15) 0.16920(9) 0.0539(9) Uani 1 1 d . . . C5 C 0.2706(3) 0.6013(3) 0.40201(14) 0.0496(14) Uani 1 1 d . . . C6 C 0.2109(2) 0.5994(3) 0.42704(14) 0.0471(14) Uani 1 1 d . . . H6A H 0.1737 0.5689 0.4210 0.057 Uiso 1 1 calc R . . C7 C 0.2065(3) 0.6421(3) 0.46049(15) 0.0508(13) Uani 1 1 d . . . H7A H 0.1662 0.6399 0.4763 0.061 Uiso 1 1 calc R . . C8 C 0.2714(3) 0.5660(2) 0.36293(14) 0.0438(13) Uani 1 1 d . . . C9 C 0.3327(2) 0.5458(2) 0.34409(15) 0.0475(13) Uani 1 1 d . . . H9A H 0.3754 0.5505 0.3575 0.057 Uiso 1 1 calc R . . C10 C 0.3331(2) 0.5183(2) 0.30563(14) 0.0370(12) Uani 1 1 d . . . C11 C 0.2692(3) 0.5104(2) 0.28651(14) 0.0398(12) Uani 1 1 d . . . H11A H 0.2689 0.4904 0.2612 0.048 Uiso 1 1 calc R . . C12 C 0.2051(2) 0.5307(2) 0.30339(14) 0.0414(13) Uani 1 1 d . . . C13 C 0.2072(2) 0.5586(2) 0.34223(15) 0.0490(13) Uani 1 1 d . . . H13A H 0.1652 0.5723 0.3545 0.059 Uiso 1 1 calc R . . C14 C 0.4007(2) 0.5019(2) 0.28498(18) 0.0462(13) Uani 1 1 d . . . C15 C 0.1372(2) 0.5267(2) 0.28172(17) 0.0393(11) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0334(4) 0.0327(3) 0.0352(3) -0.0031(3) 0.0035(3) -0.0022(2) C1 0.042(4) 0.042(4) 0.041(6) 0.000 0.000 0.000 O1 0.032(2) 0.058(2) 0.042(2) -0.0143(16) -0.0010(16) 0.0046(16) O2 0.041(2) 0.045(2) 0.037(2) -0.0120(18) -0.0040(15) -0.0009(15) C2 0.057(4) 0.048(4) 0.030(3) -0.004(3) -0.006(3) 0.004(3) C3 0.033(3) 0.059(4) 0.039(3) -0.013(3) -0.009(3) -0.010(2) O3 0.046(2) 0.060(2) 0.0280(19) -0.0246(18) -0.0005(15) 0.0111(15) C4 0.043(4) 0.063(4) 0.039(3) -0.001(3) 0.000(3) -0.005(3) O4 0.026(2) 0.068(2) 0.0449(19) -0.0091(15) 0.0034(16) -0.0004(16) O5 0.063(2) 0.051(2) 0.048(2) -0.0165(17) 0.0267(17) -0.0112(17) C5 0.033(3) 0.073(4) 0.042(3) -0.011(3) 0.006(3) 0.004(3) C6 0.045(4) 0.064(4) 0.032(3) -0.004(3) -0.003(3) -0.003(3) C7 0.055(4) 0.059(4) 0.038(3) 0.001(3) 0.000(3) -0.003(3) C8 0.045(3) 0.048(4) 0.039(3) -0.008(3) 0.008(3) 0.000(3) C9 0.035(3) 0.058(4) 0.050(4) -0.002(3) 0.003(3) 0.006(3) C10 0.030(3) 0.045(3) 0.036(3) 0.000(3) 0.004(3) 0.004(2) C11 0.046(3) 0.037(3) 0.037(3) -0.011(3) 0.000(3) -0.004(2) C12 0.034(3) 0.055(4) 0.036(3) -0.003(3) 0.007(3) 0.008(3) C13 0.040(3) 0.061(4) 0.046(4) 0.002(3) -0.002(3) 0.004(3) C14 0.034(3) 0.047(3) 0.057(4) 0.015(3) 0.004(3) 0.007(2) C15 0.038(3) 0.028(3) 0.052(3) 0.009(3) -0.006(3) -0.004(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O2 1.919(3) . ? Cu1 O4 1.928(3) 6_465 ? Cu1 O1 1.974(3) 7_455 ? Cu1 O3 1.990(3) 3 ? Cu1 O5 2.147(3) . ? C1 C2 1.529(5) . ? O1 C15 1.263(5) . ? O2 C15 1.273(6) . ? C2 C7 1.408(6) . ? C2 C3 1.410(6) . ? C3 C4 1.379(6) . ? O3 C14 1.248(6) . ? C4 C5 1.404(6) . ? O4 C14 1.302(5) . ? C5 C6 1.407(6) . ? C5 C8 1.471(6) . ? C6 C7 1.385(6) . ? C8 C9 1.374(6) . ? C8 C13 1.406(6) . ? C9 C10 1.391(6) . ? C10 C11 1.376(5) . ? C10 C14 1.486(6) . ? C11 C12 1.392(5) . ? C12 C13 1.406(6) . ? C12 C15 1.476(6) . ? 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 O4 173.93(13) . 6_465 ? O2 Cu1 O1 90.82(12) . 7_455 ? O4 Cu1 O1 88.57(12) 6_465 7_455 ? O2 Cu1 O3 90.19(11) . 3 ? O4 Cu1 O3 88.48(11) 6_465 3 ? O1 Cu1 O3 161.57(12) 7_455 3 ? O2 Cu1 O5 95.35(12) . . ? O4 Cu1 O5 90.70(12) 6_465 . ? O1 Cu1 O5 100.52(12) 7_455 . ? O3 Cu1 O5 97.70(12) 3 . ? C2 C1 C2 113.74(19) . 11_566 ? C2 C1 C2 101.2(3) . 2_565 ? C2 C1 C2 113.74(18) 11_566 2_565 ? C15 O1 Cu1 126.5(3) . 7_455 ? C15 O2 Cu1 119.2(3) . . ? C7 C2 C3 116.8(4) . . ? C7 C2 C1 121.9(4) . . ? C3 C2 C1 119.8(4) . . ? C4 C3 C2 121.2(4) . . ? C14 O3 Cu1 124.3(3) . 4 ? C3 C4 C5 121.8(5) . . ? C14 O4 Cu1 121.6(3) . 6_565 ? C4 C5 C6 117.0(5) . . ? C4 C5 C8 120.9(5) . . ? C6 C5 C8 121.9(5) . . ? C7 C6 C5 121.1(5) . . ? C6 C7 C2 121.7(5) . . ? C9 C8 C13 118.2(4) . . ? C9 C8 C5 123.1(5) . . ? C13 C8 C5 118.5(5) . . ? C8 C9 C10 122.4(4) . . ? C11 C10 C9 117.9(4) . . ? C11 C10 C14 120.9(5) . . ? C9 C10 C14 121.1(5) . . ? C10 C11 C12 123.0(4) . . ? C11 C12 C13 117.2(4) . . ? C11 C12 C15 122.8(5) . . ? C13 C12 C15 120.0(5) . . ? C8 C13 C12 121.3(4) . . ? O3 C14 O4 125.6(4) . . ? O3 C14 C10 119.6(5) . . ? O4 C14 C10 114.7(5) . . ? O1 C15 O2 126.0(4) . . ? O1 C15 C12 116.6(5) . . ? O2 C15 C12 117.3(4) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 21.26 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.24 _refine_diff_density_min -0.32 _refine_diff_density_rms 0.05 #=== END of CIF