# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # 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_Rh_2_L1_2_CF3COO_2 _audit_creation_date 2013-05-01T17:14:53-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; Rh_2_L1_2_CF3COO_2 ; _chemical_formula_moiety 'C44 H28 F16 O10 Rh2' _chemical_formula_sum 'C44 H28 F16 O10 Rh2' _chemical_formula_weight 1226.48 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.510(5) _cell_length_b 9.693(6) _cell_length_c 13.597(8) _cell_angle_alpha 103.857(5) _cell_angle_beta 100.543(4) _cell_angle_gamma 107.060(8) _cell_volume 1119.1(11) _cell_formula_units_Z 1 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 3104 _cell_measurement_theta_min 3.0491 _cell_measurement_theta_max 27.4816 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description platelet _exptl_crystal_colour green _exptl_crystal_size_max 0.104 _exptl_crystal_size_mid 0.097 _exptl_crystal_size_min 0.034 _exptl_crystal_density_diffrn 1.82 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 606 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.862 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.8540 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_process_details 'REQAB (Rigaku, 1998)' #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.710747 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator 'Graphite Monochromator' _diffrn_detector_area_resol_mean 7.31 _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_reflns_av_R_equivalents 0.0278 _diffrn_reflns_av_unetI/netI 0.0498 _diffrn_reflns_number 7154 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 25 _diffrn_reflns_theta_full 25 _diffrn_measured_fraction_theta_full 0.959 _diffrn_measured_fraction_theta_max 0.959 _reflns_number_total 3772 _reflns_number_gt 3231 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008), ' _computing_structure_solution 'SIR97 (Giacovazzo et al, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^ > 2\s(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^)+(0.0001P)^2^+13.9331P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 3772 _refine_ls_number_parameters 327 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0684 _refine_ls_R_factor_gt 0.0587 _refine_ls_wR_factor_ref 0.1615 _refine_ls_wR_factor_gt 0.1575 _refine_ls_goodness_of_fit_ref 1.229 _refine_ls_restrained_S_all 1.229 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.409 _refine_diff_density_min -0.8 _refine_diff_density_rms 0.137 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.7156(9) 0.1753(10) 0.6649(7) 0.0277(19) Uani 1 1 d . . . C2 C 0.8468(10) 0.2815(11) 0.7646(7) 0.036(2) Uani 1 1 d . . . C3 C 0.3169(9) -0.0607(9) 0.6167(7) 0.0274(19) Uani 1 1 d . . . C4 C 0.2176(10) -0.0952(9) 0.6888(6) 0.0289(19) Uani 1 1 d . . . C5 C 0.1075(10) -0.0287(10) 0.6982(7) 0.032(2) Uani 1 1 d . . . H5 H 0.0954 0.0385 0.6595 0.039 Uiso 1 1 calc R . . C6 C 0.0161(10) -0.0599(10) 0.7634(7) 0.035(2) Uani 1 1 d . . . H6 H -0.0611 -0.0167 0.7682 0.042 Uiso 1 1 calc R . . C7 C 0.0372(11) -0.1549(11) 0.8222(7) 0.036(2) Uani 1 1 d . . . C8 C 0.1468(11) -0.2215(11) 0.8131(7) 0.040(2) Uani 1 1 d . . . H8 H 0.1595 -0.2881 0.8523 0.047 Uiso 1 1 calc R . . C9 C 0.2377(10) -0.1905(10) 0.7464(7) 0.035(2) Uani 1 1 d . . . H9 H 0.3137 -0.235 0.7405 0.042 Uiso 1 1 calc R . . C10 C -0.0593(11) -0.1903(11) 0.8894(8) 0.038(2) Uani 1 1 d . . . C11 C -0.1427(10) -0.2223(11) 0.9435(7) 0.036(2) Uani 1 1 d . . . C12 C -0.2421(10) -0.2627(11) 1.0075(7) 0.037(2) Uani 1 1 d . . . C13 C -0.3432(11) -0.1858(11) 1.0275(8) 0.041(2) Uani 1 1 d . . . C14 C -0.4391(11) -0.2214(11) 1.0884(8) 0.038(2) Uani 1 1 d . . . C15 C -0.4318(11) -0.3348(12) 1.1346(8) 0.044(3) Uani 1 1 d . . . C16 C -0.3357(11) -0.4143(11) 1.1149(7) 0.039(2) Uani 1 1 d . . . C17 C -0.2438(10) -0.3778(10) 1.0502(7) 0.031(2) Uani 1 1 d . . . C18 C 0.2987(11) 0.3623(10) 0.4367(7) 0.038(2) Uani 1 1 d . . . C19 C 0.3345(12) 0.3994(12) 0.3451(9) 0.048(3) Uani 1 1 d . . . H19A H 0.3931 0.5096 0.3659 0.057 Uiso 1 1 calc R . . H19B H 0.2377 0.3779 0.2922 0.057 Uiso 1 1 calc R . . C20 C 0.4240(12) 0.3147(14) 0.2954(10) 0.057(3) Uani 1 1 d . . . H20A H 0.517 0.33 0.3483 0.085 Uiso 1 1 calc R . . H20B H 0.4518 0.3521 0.2382 0.085 Uiso 1 1 calc R . . H20C H 0.3622 0.2062 0.2671 0.085 Uiso 1 1 calc R . . C21 C 0.1843(13) 0.4259(13) 0.4786(10) 0.058(3) Uani 1 1 d . . . H21A H 0.0927 0.3986 0.4196 0.07 Uiso 1 1 calc R . . H21B H 0.2308 0.5381 0.5053 0.07 Uiso 1 1 calc R . . C22 C 0.1339(16) 0.3678(16) 0.5675(10) 0.072(4) Uani 1 1 d . . . H22A H 0.0896 0.2566 0.5424 0.107 Uiso 1 1 calc R . . H22B H 0.0573 0.4091 0.588 0.107 Uiso 1 1 calc R . . H22C H 0.2227 0.4009 0.6284 0.107 Uiso 1 1 calc R . . O1 O 0.6332(6) 0.2382(6) 0.6244(4) 0.0269(13) Uani 1 1 d . . . O2 O 0.2910(7) -0.0402(6) 0.3619(5) 0.0307(14) Uani 1 1 d . . . O3 O 0.3182(7) 0.0506(6) 0.5833(5) 0.0317(14) Uani 1 1 d . . . O4 O 0.6066(7) 0.1482(6) 0.4037(5) 0.0301(13) Uani 1 1 d . . . O5 O 0.3580(7) 0.2920(7) 0.4862(5) 0.0341(15) Uani 1 1 d . . . F1 F 0.8544(8) 0.4230(7) 0.7896(5) 0.067(2) Uani 1 1 d . . . F2 F 0.9805(6) 0.2782(7) 0.7496(5) 0.0544(16) Uani 1 1 d . . . F3 F 0.8338(7) 0.2309(8) 0.8452(4) 0.0600(17) Uani 1 1 d . . . F4 F -0.3524(7) -0.0774(7) 0.9832(5) 0.0530(15) Uani 1 1 d . . . F5 F -0.5349(7) -0.1479(7) 1.1068(5) 0.0590(17) Uani 1 1 d . . . F6 F -0.5252(7) -0.3712(8) 1.1940(5) 0.0606(18) Uani 1 1 d . . . F7 F -0.3340(7) -0.5259(7) 1.1549(5) 0.0514(15) Uani 1 1 d . . . F8 F -0.1523(6) -0.4579(6) 1.0317(4) 0.0410(13) Uani 1 1 d . . . Rh1 Rh 0.45959(8) 0.10442(8) 0.49266(5) 0.0246(2) 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 C1 0.028(5) 0.029(5) 0.030(5) 0.011(4) 0.012(4) 0.012(4) C2 0.034(5) 0.041(6) 0.035(5) 0.008(4) 0.005(4) 0.023(4) C3 0.027(4) 0.022(4) 0.027(4) 0.006(4) 0.006(4) 0.004(4) C4 0.033(5) 0.024(4) 0.025(4) 0.004(4) 0.009(4) 0.006(4) C5 0.036(5) 0.028(5) 0.033(5) 0.009(4) 0.012(4) 0.011(4) C6 0.032(5) 0.034(5) 0.044(6) 0.010(4) 0.018(4) 0.015(4) C7 0.037(5) 0.038(5) 0.034(5) 0.010(4) 0.013(4) 0.015(4) C8 0.046(6) 0.045(6) 0.037(5) 0.022(5) 0.018(5) 0.019(5) C9 0.034(5) 0.036(5) 0.039(5) 0.012(4) 0.014(4) 0.017(4) C10 0.038(5) 0.038(5) 0.046(6) 0.016(5) 0.015(5) 0.020(5) C11 0.033(5) 0.040(6) 0.038(5) 0.013(4) 0.013(4) 0.014(4) C12 0.029(5) 0.042(6) 0.029(5) 0.000(4) 0.005(4) 0.010(4) C13 0.036(5) 0.047(6) 0.041(6) 0.006(5) 0.013(4) 0.019(5) C14 0.033(5) 0.044(6) 0.036(5) 0.008(4) 0.012(4) 0.012(5) C15 0.031(5) 0.055(7) 0.034(5) -0.003(5) 0.013(4) 0.008(5) C16 0.038(5) 0.042(6) 0.032(5) 0.005(4) 0.007(4) 0.012(5) C17 0.030(5) 0.036(5) 0.025(4) 0.006(4) 0.009(4) 0.012(4) C18 0.044(6) 0.027(5) 0.036(5) 0.011(4) -0.003(4) 0.009(4) C19 0.036(6) 0.042(6) 0.060(7) 0.021(5) 0.002(5) 0.010(5) C20 0.045(6) 0.070(8) 0.067(8) 0.039(7) 0.016(6) 0.023(6) C21 0.055(7) 0.045(7) 0.074(8) 0.015(6) -0.003(6) 0.032(6) C22 0.096(10) 0.101(11) 0.065(8) 0.043(8) 0.048(8) 0.072(9) O1 0.032(3) 0.023(3) 0.026(3) 0.006(2) 0.007(3) 0.011(3) O2 0.033(3) 0.025(3) 0.033(3) 0.008(3) 0.003(3) 0.012(3) O3 0.035(3) 0.027(3) 0.043(4) 0.018(3) 0.017(3) 0.016(3) O4 0.037(3) 0.030(3) 0.037(3) 0.016(3) 0.018(3) 0.020(3) O5 0.041(4) 0.029(3) 0.033(3) 0.004(3) 0.004(3) 0.023(3) F1 0.072(4) 0.032(3) 0.070(5) -0.006(3) -0.024(4) 0.023(3) F2 0.031(3) 0.072(4) 0.045(3) -0.002(3) 0.007(3) 0.015(3) F3 0.061(4) 0.073(4) 0.031(3) 0.017(3) 0.009(3) 0.004(3) F4 0.064(4) 0.052(4) 0.055(4) 0.028(3) 0.021(3) 0.025(3) F5 0.049(4) 0.070(4) 0.071(4) 0.020(4) 0.032(3) 0.033(3) F6 0.058(4) 0.073(4) 0.054(4) 0.020(3) 0.040(3) 0.011(3) F7 0.060(4) 0.055(4) 0.047(4) 0.029(3) 0.024(3) 0.016(3) F8 0.039(3) 0.047(3) 0.041(3) 0.012(3) 0.014(3) 0.020(3) Rh1 0.0268(4) 0.0242(4) 0.0300(4) 0.0120(3) 0.0114(3) 0.0141(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 1.252(10) 2_656 ? C1 O1 1.254(10) . ? C1 C2 1.554(12) . ? C2 F1 1.308(11) . ? C2 F3 1.314(11) . ? C2 F2 1.332(10) . ? C3 O3 1.265(10) . ? C3 O4 1.284(10) 2_656 ? C3 C4 1.508(11) . ? C4 C9 1.378(12) . ? C4 C5 1.390(12) . ? C5 C6 1.373(12) . ? C5 H5 0.95 . ? C6 C7 1.389(13) . ? C6 H6 0.95 . ? C7 C8 1.386(13) . ? C7 C10 1.438(13) . ? C8 C9 1.387(13) . ? C8 H8 0.95 . ? C9 H9 0.95 . ? C10 C11 1.202(13) . ? C11 C12 1.432(13) . ? C12 C17 1.374(13) . ? C12 C13 1.404(13) . ? C13 F4 1.347(11) . ? C13 C14 1.366(13) . ? C14 F5 1.334(11) . ? C14 C15 1.403(15) . ? C15 F6 1.334(11) . ? C15 C16 1.379(14) . ? C16 F7 1.326(11) . ? C16 C17 1.382(13) . ? C17 F8 1.344(10) . ? C18 O5 1.241(10) . ? C18 C19 1.448(14) . ? C18 C21 1.530(15) . ? C19 C20 1.487(15) . ? C19 H19A 0.99 . ? C19 H19B 0.99 . ? C20 H20A 0.98 . ? C20 H20B 0.98 . ? C20 H20C 0.98 . ? C21 C22 1.545(16) . ? C21 H21A 0.99 . ? C21 H21B 0.99 . ? C22 H22A 0.98 . ? C22 H22B 0.98 . ? C22 H22C 0.98 . ? O1 Rh1 2.041(6) . ? O2 C1 1.252(10) 2_656 ? O2 Rh1 2.035(6) . ? O3 Rh1 2.025(6) . ? O4 C3 1.284(10) 2_656 ? O4 Rh1 2.029(6) . ? O5 Rh1 2.307(6) . ? Rh1 Rh1 2.4037(17) 2_656 ? 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 130.4(8) 2_656 . ? O2 C1 C2 114.5(7) 2_656 . ? O1 C1 C2 115.1(7) . . ? F1 C2 F3 109.6(8) . . ? F1 C2 F2 108.0(8) . . ? F3 C2 F2 105.2(7) . . ? F1 C2 C1 113.6(7) . . ? F3 C2 C1 110.5(8) . . ? F2 C2 C1 109.7(7) . . ? O3 C3 O4 126.5(8) . 2_656 ? O3 C3 C4 117.8(7) . . ? O4 C3 C4 115.7(7) 2_656 . ? C9 C4 C5 120.1(8) . . ? C9 C4 C3 120.0(8) . . ? C5 C4 C3 119.8(8) . . ? C6 C5 C4 120.3(8) . . ? C6 C5 H5 119.9 . . ? C4 C5 H5 119.9 . . ? C5 C6 C7 119.6(8) . . ? C5 C6 H6 120.2 . . ? C7 C6 H6 120.2 . . ? C8 C7 C6 120.3(9) . . ? C8 C7 C10 119.5(8) . . ? C6 C7 C10 120.1(8) . . ? C7 C8 C9 119.7(9) . . ? C7 C8 H8 120.2 . . ? C9 C8 H8 120.2 . . ? C4 C9 C8 119.9(8) . . ? C4 C9 H9 120 . . ? C8 C9 H9 120 . . ? C11 C10 C7 178.4(11) . . ? C10 C11 C12 179.1(10) . . ? C17 C12 C13 117.7(9) . . ? C17 C12 C11 121.8(8) . . ? C13 C12 C11 120.5(9) . . ? F4 C13 C14 117.7(8) . . ? F4 C13 C12 120.4(9) . . ? C14 C13 C12 121.9(10) . . ? F5 C14 C13 121.4(9) . . ? F5 C14 C15 120.1(8) . . ? C13 C14 C15 118.5(9) . . ? F6 C15 C16 119.8(10) . . ? F6 C15 C14 119.1(9) . . ? C16 C15 C14 121.0(9) . . ? F7 C16 C15 120.8(9) . . ? F7 C16 C17 120.5(9) . . ? C15 C16 C17 118.7(9) . . ? F8 C17 C12 120.5(8) . . ? F8 C17 C16 117.4(8) . . ? C12 C17 C16 122.1(9) . . ? O5 C18 C19 126.1(9) . . ? O5 C18 C21 118.3(9) . . ? C19 C18 C21 115.5(8) . . ? C18 C19 C20 114.0(9) . . ? C18 C19 H19A 108.7 . . ? C20 C19 H19A 108.7 . . ? C18 C19 H19B 108.7 . . ? C20 C19 H19B 108.7 . . ? H19A C19 H19B 107.6 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C18 C21 C22 113.9(8) . . ? C18 C21 H21A 108.8 . . ? C22 C21 H21A 108.8 . . ? C18 C21 H21B 108.8 . . ? C22 C21 H21B 108.8 . . ? H21A C21 H21B 107.7 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C1 O1 Rh1 116.8(5) . . ? C1 O2 Rh1 116.5(5) 2_656 . ? C3 O3 Rh1 118.0(5) . . ? C3 O4 Rh1 119.1(5) 2_656 . ? C18 O5 Rh1 151.5(6) . . ? O3 Rh1 O4 176.4(2) . . ? O3 Rh1 O2 89.8(3) . . ? O4 Rh1 O2 90.5(2) . . ? O3 Rh1 O1 90.2(2) . . ? O4 Rh1 O1 89.2(2) . . ? O2 Rh1 O1 176.3(2) . . ? O3 Rh1 O5 84.3(2) . . ? O4 Rh1 O5 99.3(2) . . ? O2 Rh1 O5 89.8(2) . . ? O1 Rh1 O5 93.9(2) . . ? O3 Rh1 Rh1 88.99(16) . 2_656 ? O4 Rh1 Rh1 87.40(16) . 2_656 ? O2 Rh1 Rh1 88.49(17) . 2_656 ? O1 Rh1 Rh1 87.86(16) . 2_656 ? O5 Rh1 Rh1 173.12(17) . 2_656 ? # The following lines are used to test the character set of files sent by # network email or other means. They are not part of the CIF data set # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];'`,./ # END of CIF _database_code_depnum_ccdc_archive 'CCDC 936777' ####################################################################### # # 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_Cu_2_L1_4 _audit_creation_date 2013-05-01T17:16:36-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; Cu_2_L1_4 ; _chemical_formula_moiety 'C68 H32 Cu2 F20 O10' _chemical_formula_sum 'C68 H32 Cu2 F20 O10' _chemical_formula_weight 1516.02 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/m' _symmetry_space_group_name_Hall '-P 2yb' _symmetry_Int_Tables_number 11 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 9.0904(5) _cell_length_b 26.7064(2) _cell_length_c 17.9565(8) _cell_angle_alpha 90 _cell_angle_beta 101.5050(10) _cell_angle_gamma 90 _cell_volume 4271.7(3) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 12394 _cell_measurement_theta_min 3.01 _cell_measurement_theta_max 27.535 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description platet _exptl_crystal_colour blue _exptl_crystal_size_max 0.373 _exptl_crystal_size_mid 0.149 _exptl_crystal_size_min 0.042 _exptl_crystal_density_diffrn 1.179 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1516 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.586 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'ABSCOR (Rigaku, 1955)' _exptl_absorpt_correction_T_min 0.6246 _exptl_absorpt_correction_T_max 1.0000 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71074 _diffrn_radiation_type MoK\a _diffrn_measurement_device_type 'Rigaku R-AXIS RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.000 _diffrn_radiation_monochromator confocal _diffrn_reflns_av_R_equivalents 0.071 _diffrn_reflns_av_unetI/netI 0.0616 _diffrn_reflns_number 33173 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 25 _diffrn_reflns_theta_full 25 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _reflns_number_total 7682 _reflns_number_gt 6213 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'RAPID AUTO (Rigaku)' _computing_cell_refinement 'RAPID AUTO (Rigaku)' _computing_data_reduction 'RAPID AUTO (Rigaku)' _computing_structure_solution 'SIR92 (Giacovazzo et al, 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^ > 2\s(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^)+(0.1401P)^2^+3.1549P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 7682 _refine_ls_number_parameters 475 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0818 _refine_ls_R_factor_gt 0.0759 _refine_ls_wR_factor_ref 0.2472 _refine_ls_wR_factor_gt 0.2422 _refine_ls_goodness_of_fit_ref 1.143 _refine_ls_restrained_S_all 1.143 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.939 _refine_diff_density_min -0.603 _refine_diff_density_rms 0.098 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' 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 0.1448(4) 0.31539(13) 0.3279(2) 0.0330(7) Uani 1 1 d . . . C2 C 0.0679(4) 0.35212(13) 0.3696(2) 0.0330(7) Uani 1 1 d . . . C3 C 0.1101(4) 0.35676(14) 0.4477(2) 0.0382(8) Uani 1 1 d . . . H3 H 0.1894 0.3368 0.4751 0.046 Uiso 1 1 calc R . . C4 C 0.0357(5) 0.39086(16) 0.4863(2) 0.0448(9) Uani 1 1 d . . . H4 H 0.0638 0.394 0.5399 0.054 Uiso 1 1 calc R . . C5 C -0.0798(4) 0.42012(14) 0.4458(2) 0.0391(8) Uani 1 1 d . . . C6 C -0.1211(4) 0.41506(15) 0.3672(2) 0.0400(8) Uani 1 1 d . . . H6 H -0.199 0.4353 0.3394 0.048 Uiso 1 1 calc R . . C7 C -0.0501(4) 0.38103(14) 0.3298(2) 0.0363(8) Uani 1 1 d . . . H7 H -0.0811 0.377 0.2764 0.044 Uiso 1 1 calc R . . C8 C -0.1576(5) 0.45606(16) 0.4834(2) 0.0461(10) Uani 1 1 d . . . C9 C -0.2292(5) 0.48637(16) 0.5107(2) 0.0475(10) Uani 1 1 d . . . C10 C -0.3177(5) 0.52362(15) 0.5380(2) 0.0455(10) Uani 1 1 d . . . C11 C -0.3423(5) 0.52422(17) 0.6107(3) 0.0543(11) Uani 1 1 d . . . C12 C -0.4302(6) 0.55987(18) 0.6357(3) 0.0564(11) Uani 1 1 d . . . C13 C -0.4906(5) 0.59769(16) 0.5879(3) 0.0484(10) Uani 1 1 d . . . C14 C -0.4702(5) 0.59739(17) 0.5149(3) 0.0512(10) Uani 1 1 d . . . C15 C -0.3864(5) 0.56122(17) 0.4898(2) 0.0515(11) Uani 1 1 d . . . C16 C 0.3653(4) 0.18465(13) 0.1779(2) 0.0331(8) Uani 1 1 d . . . C17 C 0.4414(4) 0.14817(13) 0.1353(2) 0.0330(7) Uani 1 1 d . . . C18 C 0.5646(4) 0.12091(14) 0.1736(2) 0.0365(8) Uani 1 1 d . . . H18 H 0.6005 0.1261 0.2264 0.044 Uiso 1 1 calc R . . C19 C 0.6336(4) 0.08681(15) 0.1353(2) 0.0403(8) Uani 1 1 d . . . H19 H 0.7158 0.0679 0.1621 0.048 Uiso 1 1 calc R . . C20 C 0.5852(4) 0.07951(14) 0.0577(2) 0.0390(8) Uani 1 1 d . . . C21 C 0.4632(5) 0.10704(15) 0.0186(2) 0.0421(9) Uani 1 1 d . . . H21 H 0.429 0.1024 -0.0344 0.051 Uiso 1 1 calc R . . C22 C 0.3915(4) 0.14156(14) 0.0581(2) 0.0380(8) Uani 1 1 d . . . H22 H 0.3086 0.1604 0.0318 0.046 Uiso 1 1 calc R . . C23 C 0.6593(5) 0.04323(15) 0.0191(2) 0.0457(10) Uani 1 1 d . . . C24 C 0.7259(5) 0.01266(16) -0.0105(2) 0.0469(10) Uani 1 1 d . . . C25 C 0.8079(5) -0.02444(15) -0.0423(2) 0.0444(9) Uani 1 1 d . . . C26 C 0.9006(5) -0.05757(17) 0.0042(2) 0.0503(10) Uani 1 1 d . . . C27 C 0.9795(5) -0.09347(16) -0.0257(2) 0.0495(10) Uani 1 1 d . . . C28 C 0.9687(5) -0.09781(15) -0.1023(2) 0.0451(9) Uani 1 1 d . . . C29 C 0.8758(6) -0.06567(18) -0.1498(3) 0.0584(12) Uani 1 1 d . . . C30 C 0.7973(6) -0.02994(17) -0.1197(3) 0.0542(11) Uani 1 1 d . . . O1 O 0.2745(3) 0.30090(10) 0.35918(15) 0.0389(6) Uani 1 1 d . . . O2 O 0.0730(3) 0.30141(9) 0.26348(14) 0.0356(6) Uani 1 1 d . . . O3 O 0.4377(3) 0.19836(10) 0.24241(14) 0.0369(6) Uani 1 1 d . . . O4 O 0.2360(3) 0.19919(10) 0.14717(15) 0.0384(6) Uani 1 1 d . . . F1 F -0.2840(4) 0.48749(12) 0.65901(17) 0.0887(11) Uani 1 1 d . . . F2 F -0.4555(5) 0.55857(13) 0.70656(18) 0.0965(13) Uani 1 1 d . . . F3 F -0.5755(3) 0.63243(9) 0.61247(17) 0.0603(7) Uani 1 1 d . . . F4 F -0.5356(4) 0.63285(12) 0.46708(18) 0.0830(10) Uani 1 1 d . . . F5 F -0.3670(4) 0.56251(12) 0.41837(16) 0.0767(9) Uani 1 1 d . . . F6 F 0.9147(4) -0.05426(12) 0.07883(15) 0.0782(10) Uani 1 1 d . . . F7 F 1.0712(4) -0.12440(11) 0.02099(16) 0.0722(8) Uani 1 1 d . . . F8 F 1.0478(3) -0.13229(9) -0.13056(16) 0.0551(6) Uani 1 1 d . . . F9 F 0.8602(5) -0.07020(13) -0.22559(16) 0.0928(12) Uani 1 1 d . . . F10 F 0.7071(4) 0.00180(12) -0.16764(17) 0.0829(10) Uani 1 1 d . . . Cu1 Cu 0.37409(6) 0.25 0.30750(3) 0.0287(2) Uani 1 2 d S . . Cu2 Cu 0.13616(6) 0.25 0.19835(3) 0.0288(2) Uani 1 2 d S . . C31 C 0.6016(7) 0.25 0.4670(3) 0.0513(15) Uani 1 2 d S . . H31A H 0.5866 0.216 0.4863 0.062 Uiso 0.5 1 calc PR A . H31B H 0.5295 0.2733 0.4834 0.062 Uiso 0.5 1 calc PR . . C32 C 0.7654(10) 0.2679(4) 0.4947(5) 0.059(3) Uani 0.5 1 d P A -1 H32A H 0.7704 0.3049 0.4979 0.07 Uiso 0.5 1 calc PR A -1 H32B H 0.8087 0.2536 0.5452 0.07 Uiso 0.5 1 calc PR A -1 C33 C 0.8417(8) 0.25 0.4390(4) 0.075(2) Uani 1 2 d S . . H33A H 0.8796 0.2157 0.4518 0.09 Uiso 0.5 1 calc PR A . H33B H 0.928 0.272 0.4358 0.09 Uiso 0.5 1 calc PR . . C34 C 0.7295(6) 0.25 0.3637(3) 0.0447(13) Uani 1 2 d S A . H34A H 0.742 0.2802 0.3335 0.054 Uiso 0.5 1 calc PR . . H34B H 0.742 0.2198 0.3335 0.054 Uiso 0.5 1 calc PR . . O5 O 0.5848(4) 0.25 0.3853(2) 0.0383(8) Uani 1 2 d S A . C35 C -0.0982(7) 0.25 0.0402(3) 0.0572(17) Uani 1 2 d S . . H35A H -0.0881 0.2159 0.0204 0.069 Uiso 0.5 1 calc PR B . H35B H -0.026 0.2726 0.0224 0.069 Uiso 0.5 1 calc PR . . C36 C -0.2644(10) 0.2700(4) 0.0157(5) 0.057(2) Uani 0.5 1 d P B -1 H36A H -0.2675 0.3071 0.0163 0.069 Uiso 0.5 1 calc PR B -1 H36B H -0.3116 0.2579 -0.0356 0.069 Uiso 0.5 1 calc PR B -1 C37 C -0.3334(8) 0.25 0.0703(4) 0.075(2) Uani 1 2 d S . . H37A H -0.3674 0.2154 0.0563 0.09 Uiso 0.5 1 calc PR B . H37B H -0.4219 0.2704 0.0753 0.09 Uiso 0.5 1 calc PR . . C38 C -0.2194(7) 0.25 0.1443(3) 0.0449(13) Uani 1 2 d S B . H38A H -0.2307 0.2802 0.1747 0.054 Uiso 0.5 1 calc PR . . H38B H -0.2307 0.2198 0.1747 0.054 Uiso 0.5 1 calc PR . . O6 O -0.0764(4) 0.25 0.1214(2) 0.0371(8) Uani 1 2 d S B . 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 0.0296(18) 0.0287(17) 0.0415(19) 0.0024(13) 0.0092(14) -0.0018(14) C2 0.0321(18) 0.0282(17) 0.0397(18) -0.0032(13) 0.0097(14) -0.0052(14) C3 0.0336(19) 0.0363(19) 0.0423(19) -0.0031(15) 0.0015(15) 0.0007(16) C4 0.046(2) 0.044(2) 0.044(2) -0.0140(16) 0.0085(17) -0.0034(18) C5 0.035(2) 0.0322(19) 0.055(2) -0.0102(15) 0.0192(16) -0.0086(16) C6 0.034(2) 0.041(2) 0.047(2) 0.0019(16) 0.0111(15) 0.0031(16) C7 0.0346(19) 0.0377(19) 0.0368(18) 0.0017(14) 0.0073(14) -0.0006(15) C8 0.040(2) 0.043(2) 0.059(2) -0.0151(18) 0.0168(18) -0.0094(18) C9 0.040(2) 0.047(2) 0.057(2) -0.0162(18) 0.0142(18) -0.0074(19) C10 0.041(2) 0.040(2) 0.058(2) -0.0141(17) 0.0178(18) -0.0065(17) C11 0.058(3) 0.047(2) 0.061(3) -0.0012(19) 0.019(2) 0.013(2) C12 0.064(3) 0.058(3) 0.053(2) -0.0034(19) 0.025(2) 0.006(2) C13 0.038(2) 0.042(2) 0.069(3) -0.0132(19) 0.0212(19) -0.0012(17) C14 0.043(2) 0.048(2) 0.061(3) -0.0032(19) 0.0046(19) -0.0011(19) C15 0.050(3) 0.054(3) 0.052(2) -0.0125(19) 0.0131(19) -0.012(2) C16 0.0275(18) 0.0311(18) 0.0419(19) 0.0006(14) 0.0100(14) -0.0025(14) C17 0.0291(18) 0.0282(17) 0.0428(19) -0.0031(13) 0.0095(14) -0.0050(14) C18 0.035(2) 0.0350(19) 0.0398(18) -0.0008(14) 0.0087(15) -0.0023(15) C19 0.034(2) 0.037(2) 0.051(2) -0.0002(16) 0.0123(16) 0.0001(16) C20 0.035(2) 0.0326(19) 0.054(2) -0.0114(16) 0.0214(16) -0.0084(16) C21 0.043(2) 0.042(2) 0.044(2) -0.0132(16) 0.0135(16) -0.0069(17) C22 0.0318(19) 0.0376(19) 0.0433(19) -0.0039(15) 0.0047(15) -0.0005(15) C23 0.043(2) 0.038(2) 0.060(2) -0.0147(18) 0.0215(19) -0.0112(18) C24 0.044(2) 0.042(2) 0.059(2) -0.0143(18) 0.0195(19) -0.0107(18) C25 0.042(2) 0.036(2) 0.059(2) -0.0128(17) 0.0204(18) -0.0073(17) C26 0.048(2) 0.053(3) 0.051(2) -0.0176(19) 0.0120(18) -0.012(2) C27 0.041(2) 0.047(2) 0.058(2) -0.0057(19) 0.0020(18) -0.0002(19) C28 0.038(2) 0.038(2) 0.064(2) -0.0139(17) 0.0216(18) -0.0021(17) C29 0.078(3) 0.051(2) 0.052(2) -0.0053(19) 0.028(2) 0.009(2) C30 0.062(3) 0.046(2) 0.058(3) -0.0058(19) 0.021(2) 0.007(2) O1 0.0324(14) 0.0392(14) 0.0429(14) -0.0055(11) 0.0022(11) 0.0007(11) O2 0.0308(13) 0.0350(13) 0.0390(13) -0.0049(10) 0.0017(10) 0.0012(11) O3 0.0314(13) 0.0343(13) 0.0434(14) -0.0051(10) 0.0036(10) 0.0027(11) O4 0.0313(14) 0.0403(14) 0.0416(14) -0.0067(10) 0.0025(10) -0.0004(11) F1 0.128(3) 0.077(2) 0.0663(17) 0.0086(14) 0.0313(18) 0.045(2) F2 0.144(3) 0.089(2) 0.0731(19) 0.0112(16) 0.061(2) 0.049(2) F3 0.0521(15) 0.0443(13) 0.0914(19) -0.0158(12) 0.0312(13) 0.0013(11) F4 0.099(3) 0.0719(19) 0.0738(19) 0.0003(15) 0.0060(16) 0.0288(18) F5 0.103(3) 0.0761(19) 0.0530(15) -0.0094(13) 0.0218(15) 0.0123(17) F6 0.108(3) 0.080(2) 0.0473(15) -0.0117(13) 0.0173(14) 0.0189(18) F7 0.082(2) 0.0658(17) 0.0638(16) -0.0036(13) 0.0016(14) 0.0208(15) F8 0.0507(14) 0.0451(13) 0.0749(16) -0.0167(11) 0.0257(12) 0.0005(11) F9 0.140(3) 0.090(2) 0.0539(16) -0.0045(14) 0.0321(18) 0.052(2) F10 0.111(3) 0.0742(19) 0.0642(17) -0.0013(14) 0.0196(16) 0.0418(19) Cu1 0.0235(4) 0.0265(4) 0.0350(4) 0 0.0037(2) 0 Cu2 0.0237(4) 0.0274(4) 0.0343(4) 0 0.0038(2) 0 C31 0.036(3) 0.079(4) 0.037(3) 0 0.003(2) 0 C32 0.043(5) 0.065(6) 0.056(5) -0.014(4) -0.018(4) 0.007(4) C33 0.034(4) 0.128(7) 0.060(4) 0 0.004(3) 0 C34 0.028(3) 0.054(3) 0.050(3) 0 0.004(2) 0 O5 0.0269(19) 0.047(2) 0.0384(19) 0 -0.0005(14) 0 C35 0.033(3) 0.101(5) 0.035(3) 0 0.000(2) 0 C36 0.038(5) 0.072(6) 0.053(5) 0.013(4) -0.013(4) -0.008(4) C37 0.037(4) 0.128(7) 0.059(4) 0 0.006(3) 0 C38 0.036(3) 0.053(3) 0.046(3) 0 0.007(2) 0 O6 0.0236(18) 0.049(2) 0.0367(18) 0 0.0008(14) 0 #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 O1 1.262(5) . ? C1 O2 1.266(4) . ? C1 C2 1.489(5) . ? C2 C3 1.385(5) . ? C2 C7 1.397(5) . ? C3 C4 1.397(6) . ? C3 H3 0.95 . ? C4 C5 1.392(6) . ? C4 H4 0.95 . ? C5 C6 1.393(5) . ? C5 C8 1.439(5) . ? C6 C7 1.366(5) . ? C6 H6 0.95 . ? C7 H7 0.95 . ? C8 C9 1.202(6) . ? C9 C10 1.426(6) . ? C10 C11 1.368(6) . ? C10 C15 1.389(7) . ? C11 F1 1.346(5) . ? C11 C12 1.375(6) . ? C12 F2 1.337(5) . ? C12 C13 1.367(7) . ? C13 F3 1.336(5) . ? C13 C14 1.361(6) . ? C14 F4 1.336(5) . ? C14 C15 1.362(6) . ? C15 F5 1.330(5) . ? C16 O4 1.257(4) . ? C16 O3 1.267(4) . ? C16 C17 1.491(5) . ? C17 C22 1.381(5) . ? C17 C18 1.396(5) . ? C18 C19 1.367(5) . ? C18 H18 0.95 . ? C19 C20 1.388(6) . ? C19 H19 0.95 . ? C20 C21 1.397(6) . ? C20 C23 1.436(5) . ? C21 C22 1.400(5) . ? C21 H21 0.95 . ? C22 H22 0.95 . ? C23 C24 1.202(6) . ? C24 C25 1.426(6) . ? C25 C30 1.381(6) . ? C25 C26 1.381(7) . ? C26 F6 1.324(5) . ? C26 C27 1.369(6) . ? C27 F7 1.342(5) . ? C27 C28 1.365(6) . ? C28 F8 1.330(4) . ? C28 C29 1.374(7) . ? C29 F9 1.345(5) . ? C29 C30 1.366(6) . ? C30 F10 1.361(5) . ? O1 Cu1 1.966(3) . ? O2 Cu2 1.962(3) . ? O3 Cu1 1.968(3) . ? O4 Cu2 1.960(3) . ? Cu1 O1 1.966(3) 4_565 ? Cu1 O3 1.968(3) 4_565 ? Cu1 O5 2.134(4) . ? Cu1 Cu2 2.6131(9) . ? Cu2 O4 1.960(3) 4_565 ? Cu2 O2 1.962(3) 4_565 ? Cu2 O6 2.139(3) . ? C31 O5 1.444(7) . ? C31 C32 1.549(10) . ? C31 C32 1.549(10) 4_565 ? C31 H31A 0.99 . ? C31 H31B 0.99 . ? C32 C33 1.410(12) . ? C32 H32A 0.99 . ? C32 H32B 0.99 . ? C33 C32 1.410(12) 4_565 ? C33 C34 1.522(9) . ? C33 H33A 0.99 . ? C33 H33B 0.99 . ? C34 O5 1.444(7) . ? C34 H34A 0.99 . ? C34 H34B 0.99 . ? C35 O6 1.432(7) . ? C35 C36 1.580(10) . ? C35 C36 1.580(10) 4_565 ? C35 H35A 0.99 . ? C35 H35B 0.99 . ? C36 C37 1.373(12) . ? C36 H36A 0.99 . ? C36 H36B 0.99 . ? C37 C36 1.373(12) 4_565 ? C37 C38 1.514(9) . ? C37 H37A 0.99 . ? C37 H37B 0.99 . ? C38 O6 1.439(7) . ? C38 H38A 0.99 . ? C38 H38B 0.99 . ? 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 C1 O2 125.6(3) . . ? O1 C1 C2 118.0(3) . . ? O2 C1 C2 116.4(3) . . ? C3 C2 C7 119.9(3) . . ? C3 C2 C1 120.3(3) . . ? C7 C2 C1 119.8(3) . . ? C2 C3 C4 119.8(4) . . ? C2 C3 H3 120.1 . . ? C4 C3 H3 120.1 . . ? C5 C4 C3 119.8(4) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 120.1 . . ? C4 C5 C6 119.8(3) . . ? C4 C5 C8 121.3(4) . . ? C6 C5 C8 118.9(4) . . ? C7 C6 C5 120.3(4) . . ? C7 C6 H6 119.9 . . ? C5 C6 H6 119.9 . . ? C6 C7 C2 120.4(3) . . ? C6 C7 H7 119.8 . . ? C2 C7 H7 119.8 . . ? C9 C8 C5 175.9(5) . . ? C8 C9 C10 176.1(5) . . ? C11 C10 C15 116.6(4) . . ? C11 C10 C9 123.1(4) . . ? C15 C10 C9 120.3(4) . . ? F1 C11 C10 119.2(4) . . ? F1 C11 C12 118.3(4) . . ? C10 C11 C12 122.4(4) . . ? F2 C12 C13 119.5(4) . . ? F2 C12 C11 120.9(4) . . ? C13 C12 C11 119.6(4) . . ? F3 C13 C14 121.4(4) . . ? F3 C13 C12 119.5(4) . . ? C14 C13 C12 119.0(4) . . ? F4 C14 C13 119.1(4) . . ? F4 C14 C15 119.8(4) . . ? C13 C14 C15 121.1(4) . . ? F5 C15 C14 119.4(4) . . ? F5 C15 C10 119.3(4) . . ? C14 C15 C10 121.2(4) . . ? O4 C16 O3 125.6(3) . . ? O4 C16 C17 117.8(3) . . ? O3 C16 C17 116.7(3) . . ? C22 C17 C18 119.9(3) . . ? C22 C17 C16 120.3(3) . . ? C18 C17 C16 119.8(3) . . ? C19 C18 C17 120.2(3) . . ? C19 C18 H18 119.9 . . ? C17 C18 H18 119.9 . . ? C18 C19 C20 120.9(4) . . ? C18 C19 H19 119.6 . . ? C20 C19 H19 119.6 . . ? C19 C20 C21 119.4(3) . . ? C19 C20 C23 119.6(4) . . ? C21 C20 C23 121.0(4) . . ? C20 C21 C22 119.7(3) . . ? C20 C21 H21 120.2 . . ? C22 C21 H21 120.2 . . ? C17 C22 C21 120.0(4) . . ? C17 C22 H22 120 . . ? C21 C22 H22 120 . . ? C24 C23 C20 177.2(5) . . ? C23 C24 C25 177.4(5) . . ? C30 C25 C26 116.8(4) . . ? C30 C25 C24 122.6(4) . . ? C26 C25 C24 120.5(4) . . ? F6 C26 C27 119.4(4) . . ? F6 C26 C25 119.5(4) . . ? C27 C26 C25 121.1(4) . . ? F7 C27 C28 119.2(4) . . ? F7 C27 C26 119.7(4) . . ? C28 C27 C26 121.1(4) . . ? F8 C28 C27 120.5(4) . . ? F8 C28 C29 120.6(4) . . ? C27 C28 C29 119.0(4) . . ? F9 C29 C30 120.3(4) . . ? F9 C29 C28 119.9(4) . . ? C30 C29 C28 119.7(4) . . ? F10 C30 C29 118.8(4) . . ? F10 C30 C25 118.9(4) . . ? C29 C30 C25 122.4(4) . . ? C1 O1 Cu1 118.7(2) . . ? C1 O2 Cu2 126.3(2) . . ? C16 O3 Cu1 125.8(2) . . ? C16 O4 Cu2 119.2(2) . . ? O1 Cu1 O1 87.51(16) . 4_565 ? O1 Cu1 O3 169.32(10) . . ? O1 Cu1 O3 90.76(12) 4_565 . ? O1 Cu1 O3 90.76(12) . 4_565 ? O1 Cu1 O3 169.32(10) 4_565 4_565 ? O3 Cu1 O3 89.00(16) . 4_565 ? O1 Cu1 O5 97.40(11) . . ? O1 Cu1 O5 97.40(11) 4_565 . ? O3 Cu1 O5 93.28(11) . . ? O3 Cu1 O5 93.28(11) 4_565 . ? O1 Cu1 Cu2 87.93(8) . . ? O1 Cu1 Cu2 87.93(8) 4_565 . ? O3 Cu1 Cu2 81.48(8) . . ? O3 Cu1 Cu2 81.48(8) 4_565 . ? O5 Cu1 Cu2 172.60(11) . . ? O4 Cu2 O4 87.63(16) 4_565 . ? O4 Cu2 O2 90.74(12) 4_565 . ? O4 Cu2 O2 169.03(11) . . ? O4 Cu2 O2 169.03(11) 4_565 4_565 ? O4 Cu2 O2 90.74(12) . 4_565 ? O2 Cu2 O2 88.81(15) . 4_565 ? O4 Cu2 O6 98.06(10) 4_565 . ? O4 Cu2 O6 98.06(10) . . ? O2 Cu2 O6 92.91(10) . . ? O2 Cu2 O6 92.91(10) 4_565 . ? O4 Cu2 Cu1 87.73(8) 4_565 . ? O4 Cu2 Cu1 87.73(8) . . ? O2 Cu2 Cu1 81.36(7) . . ? O2 Cu2 Cu1 81.36(7) 4_565 . ? O6 Cu2 Cu1 171.94(10) . . ? O5 C31 C32 103.1(5) . . ? O5 C31 C32 103.1(5) . 4_565 ? C32 C31 C32 36.0(7) . 4_565 ? O5 C31 H31A 111.2 . . ? C32 C31 H31A 111.2 . . ? C32 C31 H31A 78.2 4_565 . ? O5 C31 H31B 111.2 . . ? C32 C31 H31B 111.2 . . ? C32 C31 H31B 138.5 4_565 . ? H31A C31 H31B 109.1 . . ? C33 C32 C31 104.2(6) . . ? C33 C32 H32A 110.9 . . ? C31 C32 H32A 110.9 . . ? C33 C32 H32B 110.9 . . ? C31 C32 H32B 110.9 . . ? H32A C32 H32B 108.9 . . ? C32 C33 C32 39.7(9) 4_565 . ? C32 C33 C34 107.1(6) 4_565 . ? C32 C33 C34 107.1(6) . . ? C32 C33 H33A 73.7 4_565 . ? C32 C33 H33A 110.3 . . ? C34 C33 H33A 110.3 . . ? C32 C33 H33B 138.5 4_565 . ? C32 C33 H33B 110.3 . . ? C34 C33 H33B 110.3 . . ? H33A C33 H33B 108.6 . . ? O5 C34 C33 104.2(5) . . ? O5 C34 H34A 110.9 . . ? C33 C34 H34A 110.9 . . ? O5 C34 H34B 110.9 . . ? C33 C34 H34B 110.9 . . ? H34A C34 H34B 108.9 . . ? C34 O5 C31 110.9(4) . . ? C34 O5 Cu1 124.8(3) . . ? C31 O5 Cu1 124.3(3) . . ? O6 C35 C36 102.4(5) . . ? O6 C35 C36 102.4(5) . 4_565 ? C36 C35 C36 39.5(7) . 4_565 ? O6 C35 H35A 111.3 . . ? C36 C35 H35A 111.3 . . ? C36 C35 H35A 74.9 4_565 . ? O6 C35 H35B 111.3 . . ? C36 C35 H35B 111.3 . . ? C36 C35 H35B 140.8 4_565 . ? H35A C35 H35B 109.2 . . ? C37 C36 C35 102.5(6) . . ? C37 C36 H36A 111.3 . . ? C35 C36 H36A 111.3 . . ? C37 C36 H36B 111.3 . . ? C35 C36 H36B 111.3 . . ? H36A C36 H36B 109.2 . . ? C36 C37 C36 45.8(9) 4_565 . ? C36 C37 C38 107.2(6) 4_565 . ? C36 C37 C38 107.2(6) . . ? C36 C37 H37A 67.7 4_565 . ? C36 C37 H37A 110.3 . . ? C38 C37 H37A 110.3 . . ? C36 C37 H37B 140.7 4_565 . ? C36 C37 H37B 110.3 . . ? C38 C37 H37B 110.3 . . ? H37A C37 H37B 108.5 . . ? O6 C38 C37 104.4(5) . . ? O6 C38 H38A 110.9 . . ? C37 C38 H38A 110.9 . . ? O6 C38 H38B 110.9 . . ? C37 C38 H38B 110.9 . . ? H38A C38 H38B 108.9 . . ? C35 O6 C38 109.9(4) . . ? C35 O6 Cu2 125.5(3) . . ? C38 O6 Cu2 124.5(3) . . ? # SQUEEZE RESULTS (APPEND TO CIF) 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 0.004 0.250 0.755 769.2 24.1 2 -0.105 0.750 0.245 769.1 23.9 _platon_squeeze_details ; ; # The following lines are used to test the character set of files sent by # network email or other means. They are not part of the CIF data set # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];'`,./ # END of CIF _database_code_depnum_ccdc_archive 'CCDC 936778'