Supplementary Material (ESI) for Journal of Materials Chemistry This journal is © The Royal Society of Chemistry 2003 data_global _publ_contact_author_email Michele.Cesario@icsn.cnrs-gif.fr _publ_contact_author_name 'Michele Cesario' _journal_name_full J.Mater.Chem. _journal_coden_Cambridge 1145 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name L.Douce T.H.Diep R.Ziessel A.Skoulios M.Cesario data_DIEP-LD-001 _database_code_CSD 200811 _audit_creation_method SHELXL #_chemical_absolute_configuration _chemical_name_systematic ; ? ; _chemical_name_common 'copper(i) complex' _chemical_formula_moiety [Cu(I)C28N4O2H280],(BF4) _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C28 H28 B Cu F4 N4 O2' _chemical_formula_weight 602.89 _chemical_melting_point ? _chemical_compound_source ? 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' 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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 28.324(11) _cell_length_b 13.313(5) _cell_length_c 16.721(6) _cell_angle_alpha 90.00 _cell_angle_beta 113.7(4) _cell_angle_gamma 90.00 _cell_volume 5774.6(4) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 12382 _cell_measurement_theta_min 1.97 _cell_measurement_theta_max 27.52 _exptl_crystal_description prism _exptl_crystal_colour 'dark red ' _exptl_crystal_size_max 0.57 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.387 _exptl_crystal_density_method ? _exptl_crystal_F_000 2480 _exptl_absorpt_coefficient_mu 0.814 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Nonius kappaCCD diffractometer' _diffrn_measurement_method 'phi scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21966/10481 _diffrn_reflns_av_R_equivalents 0.0306 _diffrn_reflns_av_sigmaI/netI 0.0464 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 27.52 _reflns_number_total 5577 _reflns_number_gt 3497 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'DENZO (Otwinowski & Minor, 1997) COLLECT (Hooft,1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) COLLECT (Hooft,1998)' _computing_data_reduction 'HKL package (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'R3M (Riche,1983) ORTEP (Johnson,1965)' _computing_publication_material 'SHELXL-93 (Sheldrick,1993)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.1142P)^2^+10.1098P] 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 5577 _refine_ls_number_parameters 379 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.1141 _refine_ls_R_factor_gt 0.0719 _refine_ls_wR_factor_all 0.2248 _refine_ls_wR_factor_ref 0.1921 _refine_ls_goodness_of_fit_all 1.029 _refine_ls_goodness_of_fit_ref 1.125 _refine_ls_restrained_S_all 1.034 _refine_ls_restrained_S_obs 1.133 _refine_ls_shift/su_max 0.044 _refine_ls_shift/esd_mean 0.002 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Cu Cu 0.40100(2) 0.26537(4) 0.37989(4) 0.0679(3) Uani 1 d . . N1A N 0.38803(13) 0.3924(3) 0.3044(2) 0.0549(8) Uani 1 d . . C2A C 0.3651(2) 0.4004(3) 0.2111(3) 0.0599(11) Uani 1 d . . C3A C 0.3600(2) 0.4894(4) 0.1657(3) 0.0759(14) Uani 1 d . . H3A H 0.3725 0.5487 0.1963 0.091 Uiso 1 calc R . C4A C 0.3370(2) 0.4917(5) 0.0758(4) 0.090(2) Uani 1 d . . H4A H 0.3334 0.5525 0.0465 0.108 Uiso 1 calc R . C5A C 0.3195(2) 0.4063(5) 0.0303(3) 0.085(2) Uani 1 d . . C6A C 0.3249(2) 0.3168(5) 0.0734(4) 0.095(2) Uani 1 d . . H6A H 0.3137 0.2576 0.0420 0.114 Uiso 1 calc R . C7A C 0.3468(2) 0.3147(4) 0.1632(4) 0.085(2) Uani 1 d . . H7A H 0.3493 0.2539 0.1920 0.102 Uiso 1 calc R . O8A O 0.2969(2) 0.4168(4) -0.0590(3) 0.124(2) Uani 1 d . . C9A C 0.2837(4) 0.3323(8) -0.1119(5) 0.162(4) Uani 1 d . . H9A1 H 0.2763 0.3513 -0.1710 0.195 Uiso 1 calc R . H9A2 H 0.2537 0.3015 -0.1090 0.195 Uiso 1 calc R . H9A3 H 0.3118 0.2854 -0.0921 0.195 Uiso 1 calc R . C10A C 0.3995(2) 0.4717(3) 0.3507(3) 0.0637(12) Uani 1 d . . H10A H 0.3927 0.5345 0.3241 0.076 Uiso 1 calc R . N1B N 0.42928(13) 0.3691(3) 0.4774(2) 0.0593(9) Uani 1 d . . C2B C 0.4234(2) 0.4638(3) 0.4457(3) 0.0596(11) Uani 1 d . . C3B C 0.4391(2) 0.5473(4) 0.4980(4) 0.0766(14) Uani 1 d . . H3B H 0.4340 0.6114 0.4739 0.092 Uiso 1 calc R . C4B C 0.4626(2) 0.5338(5) 0.5865(4) 0.096(2) Uani 1 d . . H4B H 0.4740 0.5886 0.6239 0.115 Uiso 1 calc R . C5B C 0.4690(3) 0.4373(6) 0.6191(4) 0.098(2) Uani 1 d . . H5B H 0.4853 0.4269 0.6791 0.118 Uiso 1 calc R . C6B C 0.4514(2) 0.3550(4) 0.5631(3) 0.0737(13) Uani 1 d . . C7B C 0.4553(3) 0.2508(5) 0.5960(4) 0.102(2) Uani 1 d . . H7B1 H 0.4289 0.2394 0.6173 0.123 Uiso 1 calc R . H7B2 H 0.4885 0.2409 0.6426 0.123 Uiso 1 calc R . H7B3 H 0.4509 0.2046 0.5495 0.123 Uiso 1 calc R . N1C N 0.4353(2) 0.1320(3) 0.3785(3) 0.0663(10) Uani 1 d . . C2C C 0.4872(2) 0.1130(3) 0.3901(4) 0.0728(13) Uani 1 d . . C3C C 0.5044(2) 0.0312(4) 0.3650(5) 0.097(2) Uani 1 d . . H3C H 0.4812 -0.0199 0.3372 0.116 Uiso 1 calc R . C4C C 0.5560(2) 0.0193(4) 0.3787(4) 0.090(2) Uani 1 d . . H4C H 0.5661 -0.0391 0.3594 0.108 Uiso 1 calc R . C5C C 0.5898(3) 0.0867(4) 0.4172(5) 0.105(2) Uani 1 d . . C6C C 0.5768(3) 0.1658(6) 0.4591(7) 0.147(4) Uani 1 d . . H6C H 0.6020 0.2078 0.4974 0.177 Uiso 1 calc R . C7C C 0.5250(3) 0.1800(5) 0.4420(6) 0.132(3) Uani 1 d . . H7C H 0.5153 0.2355 0.4657 0.158 Uiso 1 calc R . O8C O 0.6424(2) 0.0810(3) 0.4371(4) 0.139(2) Uani 1 d . . C9C C 0.6602(3) 0.0005(5) 0.4062(5) 0.111(2) Uani 1 d . . H9C1 H 0.6571 -0.0594 0.4356 0.134 Uiso 1 calc R . H9C2 H 0.6958 0.0112 0.4169 0.134 Uiso 1 calc R . H9C3 H 0.6403 -0.0064 0.3446 0.134 Uiso 1 calc R . C10C C 0.4043(2) 0.0578(4) 0.3686(3) 0.0742(14) Uani 1 d . . H10C H 0.4153 -0.0076 0.3664 0.089 Uiso 1 calc R . N1D N 0.34058(14) 0.1733(3) 0.3664(2) 0.0615(9) Uani 1 d . . C2D C 0.3523(2) 0.0760(3) 0.3609(3) 0.0641(12) Uani 1 d . . C3D C 0.3176(2) -0.0004(4) 0.3499(4) 0.093(2) Uani 1 d . . H3D H 0.3265 -0.0666 0.3450 0.112 Uiso 1 calc R . C4D C 0.2696(2) 0.0221(5) 0.3462(4) 0.096(2) Uani 1 d . . H4D H 0.2457 -0.0284 0.3396 0.115 Uiso 1 calc R . C5D C 0.2576(2) 0.1203(4) 0.3523(4) 0.084(2) Uani 1 d . . H5D H 0.2251 0.1368 0.3499 0.100 Uiso 1 calc R . C6D C 0.2932(2) 0.1957(4) 0.3621(3) 0.0697(12) Uani 1 d . . C7D C 0.2812(2) 0.3039(5) 0.3674(5) 0.111(2) Uani 1 d . . H7D1 H 0.2943 0.3243 0.4275 0.133 Uiso 1 calc R . H7D2 H 0.2445 0.3135 0.3412 0.133 Uiso 1 calc R . H7D3 H 0.2969 0.3435 0.3369 0.133 Uiso 1 calc R . B B 0.3877(3) 0.2318(5) 0.7644(6) 0.092(2) Uani 1 d D . F11 F 0.4121(4) 0.1474(5) 0.7685(7) 0.135(3) Uani 0.78 d PD 1 F12 F 0.4209(3) 0.3083(4) 0.7908(6) 0.191(5) Uani 0.78 d PD 1 F13 F 0.3565(2) 0.2537(4) 0.6763(4) 0.138(2) Uani 0.78 d PD 1 F14 F 0.3565(5) 0.2378(9) 0.8031(8) 0.241(5) Uani 0.78 d PD 1 F21 F 0.4017(10) 0.2323(19) 0.8578(12) 0.152(5) Uiso 0.22 d PD 2 F22 F 0.3407(8) 0.2084(20) 0.7344(19) 0.152(5) Uiso 0.22 d PD 2 F23 F 0.4145(16) 0.1450(24) 0.7595(29) 0.152(5) Uiso 0.22 d PD 2 F24 F 0.4093(12) 0.3045(20) 0.7461(18) 0.152(5) Uiso 0.22 d PD 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 Cu 0.0691(4) 0.0432(4) 0.0885(5) -0.0047(3) 0.0287(3) -0.0057(2) N1A 0.055(2) 0.048(2) 0.061(2) -0.004(2) 0.023(2) -0.002(2) C2A 0.056(3) 0.055(3) 0.073(3) -0.005(2) 0.030(2) 0.004(2) C3A 0.082(4) 0.063(3) 0.082(3) 0.000(3) 0.032(3) 0.002(2) C4A 0.099(4) 0.092(4) 0.077(4) 0.018(3) 0.034(3) 0.015(3) C5A 0.076(4) 0.112(5) 0.067(3) -0.006(3) 0.027(3) 0.017(3) C6A 0.105(5) 0.087(4) 0.078(4) -0.020(3) 0.021(3) 0.002(3) C7A 0.105(4) 0.060(3) 0.080(4) -0.008(3) 0.026(3) 0.003(3) O8A 0.116(4) 0.172(5) 0.071(3) 0.001(3) 0.024(2) 0.021(3) C9A 0.161(8) 0.222(11) 0.079(5) -0.036(6) 0.022(5) -0.016(8) C10A 0.073(3) 0.043(3) 0.078(3) -0.001(2) 0.034(2) -0.005(2) N1B 0.054(2) 0.057(2) 0.065(2) -0.001(2) 0.022(2) -0.008(2) C2B 0.058(3) 0.052(3) 0.069(3) -0.007(2) 0.027(2) -0.007(2) C3B 0.077(3) 0.064(3) 0.090(4) -0.019(3) 0.036(3) -0.014(3) C4B 0.102(5) 0.096(5) 0.087(4) -0.037(4) 0.037(4) -0.024(4) C5B 0.103(5) 0.121(6) 0.061(3) -0.015(3) 0.023(3) -0.015(4) C6B 0.065(3) 0.084(4) 0.068(3) 0.004(3) 0.023(2) -0.003(3) C7B 0.107(5) 0.101(5) 0.088(4) 0.020(3) 0.028(4) -0.005(4) N1C 0.067(2) 0.046(2) 0.091(3) -0.007(2) 0.037(2) -0.005(2) C2C 0.071(3) 0.048(3) 0.108(4) -0.014(3) 0.046(3) -0.007(2) C3C 0.070(4) 0.064(3) 0.153(6) -0.022(3) 0.041(4) -0.009(3) C4C 0.076(4) 0.058(3) 0.139(5) -0.013(3) 0.046(4) 0.000(3) C5C 0.086(4) 0.063(3) 0.190(7) -0.026(4) 0.080(5) -0.011(3) C6C 0.093(5) 0.106(6) 0.256(10) -0.076(6) 0.084(6) -0.032(4) C7C 0.092(5) 0.079(4) 0.242(9) -0.050(5) 0.086(6) -0.016(4) O8C 0.088(3) 0.089(3) 0.262(7) -0.042(4) 0.091(4) -0.013(2) C9C 0.085(4) 0.105(5) 0.160(6) -0.022(4) 0.065(4) 0.010(4) C10C 0.080(4) 0.045(3) 0.107(4) -0.007(2) 0.047(3) -0.005(2) N1D 0.057(2) 0.052(2) 0.071(2) -0.005(2) 0.021(2) -0.008(2) C2D 0.059(3) 0.052(3) 0.083(3) -0.005(2) 0.029(2) -0.010(2) C3D 0.084(4) 0.056(3) 0.140(5) -0.008(3) 0.047(4) -0.015(3) C4D 0.069(4) 0.077(4) 0.140(5) -0.008(4) 0.041(4) -0.025(3) C5D 0.061(3) 0.082(4) 0.104(4) 0.000(3) 0.029(3) -0.008(3) C6D 0.056(3) 0.068(3) 0.075(3) -0.005(2) 0.015(2) -0.005(2) C7D 0.073(4) 0.078(4) 0.174(7) -0.025(4) 0.042(4) 0.001(3) B 0.086(5) 0.063(4) 0.134(7) 0.002(4) 0.050(5) 0.004(3) F11 0.155(5) 0.055(3) 0.172(6) 0.005(3) 0.040(4) 0.038(3) F12 0.140(5) 0.061(3) 0.261(9) -0.035(4) -0.036(5) 0.005(3) F13 0.122(5) 0.129(5) 0.138(5) 0.017(4) 0.027(4) 0.040(3) F14 0.210(10) 0.356(15) 0.229(10) 0.062(9) 0.161(10) 0.098(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu N1C 2.029(4) . ? Cu N1B 2.039(4) . ? Cu N1D 2.043(4) . ? Cu N1A 2.054(3) . ? N1A C10A 1.272(6) . ? N1A C2A 1.432(5) . ? C2A C7A 1.370(7) . ? C2A C3A 1.384(7) . ? C3A C4A 1.377(8) . ? C4A C5A 1.348(8) . ? C5A C6A 1.369(9) . ? C5A O8A 1.375(7) . ? C6A C7A 1.376(7) . ? O8A C9A 1.386(10) . ? C10A C2B 1.459(7) . ? N1B C6B 1.327(6) . ? N1B C2B 1.351(6) . ? C2B C3B 1.374(6) . ? C3B C4B 1.369(8) . ? C4B C5B 1.379(9) . ? C5B C6B 1.397(8) . ? C6B C7B 1.480(7) . ? N1C C10C 1.289(6) . ? N1C C2C 1.426(6) . ? C2C C3C 1.328(7) . ? C2C C7C 1.396(8) . ? C3C C4C 1.394(8) . ? C4C C5C 1.283(8) . ? C5C O8C 1.390(7) . ? C5C C6C 1.394(9) . ? C6C C7C 1.390(9) . ? O8C C9C 1.371(7) . ? C10C C2D 1.444(6) . ? N1D C6D 1.347(6) . ? N1D C2D 1.351(6) . ? C2D C3D 1.375(7) . ? C3D C4D 1.368(8) . ? C4D C5D 1.365(8) . ? C5D C6D 1.385(7) . ? C6D C7D 1.491(8) . ? B F24 1.25(2) . ? B F22 1.26(2) . ? B F14 1.292(10) . ? B F11 1.306(9) . ? B F12 1.333(9) . ? B F23 1.40(2) . ? B F13 1.412(10) . ? B F21 1.45(2) . ? 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 N1C Cu N1B 124.4(2) . . ? N1C Cu N1D 81.83(15) . . ? N1B Cu N1D 122.49(15) . . ? N1C Cu N1A 133.0(2) . . ? N1B Cu N1A 81.35(14) . . ? N1D Cu N1A 119.43(14) . . ? C10A N1A C2A 119.7(4) . . ? C10A N1A Cu 111.7(3) . . ? C2A N1A Cu 128.4(3) . . ? C7A C2A C3A 117.4(5) . . ? C7A C2A N1A 118.4(4) . . ? C3A C2A N1A 124.3(4) . . ? C4A C3A C2A 121.2(5) . . ? C5A C4A C3A 120.2(6) . . ? C4A C5A C6A 119.9(5) . . ? C4A C5A O8A 115.6(6) . . ? C6A C5A O8A 124.4(6) . . ? C5A C6A C7A 119.9(6) . . ? C2A C7A C6A 121.4(6) . . ? C5A O8A C9A 119.8(6) . . ? N1A C10A C2B 119.8(4) . . ? C6B N1B C2B 119.1(4) . . ? C6B N1B Cu 129.2(3) . . ? C2B N1B Cu 111.8(3) . . ? N1B C2B C3B 123.3(5) . . ? N1B C2B C10A 115.1(4) . . ? C3B C2B C10A 121.6(4) . . ? C4B C3B C2B 118.3(5) . . ? C3B C4B C5B 118.7(5) . . ? C4B C5B C6B 120.7(5) . . ? N1B C6B C5B 120.0(5) . . ? N1B C6B C7B 117.8(5) . . ? C5B C6B C7B 122.2(5) . . ? C10C N1C C2C 119.7(4) . . ? C10C N1C Cu 111.5(3) . . ? C2C N1C Cu 128.8(3) . . ? C3C C2C C7C 115.8(5) . . ? C3C C2C N1C 126.2(5) . . ? C7C C2C N1C 117.6(5) . . ? C2C C3C C4C 122.2(5) . . ? C5C C4C C3C 121.8(5) . . ? C4C C5C O8C 126.5(5) . . ? C4C C5C C6C 119.1(6) . . ? O8C C5C C6C 113.2(6) . . ? C7C C6C C5C 118.0(7) . . ? C6C C7C C2C 121.6(6) . . ? C9C O8C C5C 118.3(5) . . ? N1C C10C C2D 120.1(4) . . ? C6D N1D C2D 118.4(4) . . ? C6D N1D Cu 130.2(3) . . ? C2D N1D Cu 111.4(3) . . ? N1D C2D C3D 122.4(5) . . ? N1D C2D C10C 115.2(4) . . ? C3D C2D C10C 122.5(5) . . ? C4D C3D C2D 119.3(5) . . ? C5D C4D C3D 118.6(5) . . ? C4D C5D C6D 120.7(5) . . ? N1D C6D C5D 120.6(5) . . ? N1D C6D C7D 117.2(4) . . ? C5D C6D C7D 122.2(5) . . ? F24 B F22 129.6(18) . . ? F14 B F11 118.8(9) . . ? F14 B F12 108.6(9) . . ? F11 B F12 110.6(8) . . ? F24 B F23 107.3(19) . . ? F22 B F23 106.4(19) . . ? F14 B F13 103.9(8) . . ? F11 B F13 109.3(8) . . ? F12 B F13 104.5(7) . . ? F24 B F21 108.2(15) . . ? F22 B F21 102.6(16) . . ? F23 B F21 98.5(18) . . ? _refine_diff_density_max 0.742 _refine_diff_density_min -0.309 _refine_diff_density_rms 0.061