# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 186/1299 data_sy348 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis[2,6-bis-(3-{2,4,6-trimethylphenyl}pyrazol-1-yl)pyridine]dicopper(I) ditetrafluoroborate diacetone solvate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H70 B2 Cu2 F8 N10 O2' _chemical_formula_weight 1312.00 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' 'B' 'B' 0.0013 0.0007 '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' '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' 'O' 'O' 0.0106 0.0060 '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 20.430(3) _cell_length_b 21.288(3) _cell_length_c 14.4499(19) _cell_angle_alpha 90.00 _cell_angle_beta 92.371(12) _cell_angle_gamma 90.00 _cell_volume 6279.1(15) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 44 _cell_measurement_theta_min 3.49 _cell_measurement_theta_max 10.92 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.43 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.388 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2720 _exptl_absorpt_coefficient_mu 0.753 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.44317 _exptl_absorpt_correction_T_max 0.94587 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens P4' _diffrn_measurement_method 'Theta/2theta' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 1 _diffrn_reflns_number 3914 _diffrn_reflns_av_R_equivalents 0.0437 _diffrn_reflns_av_sigmaI/netI 0.0788 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 20.99 _reflns_number_total 3371 _reflns_number_gt 2108 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _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^)+(0.1178P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3371 _refine_ls_number_parameters 405 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1018 _refine_ls_R_factor_gt 0.0608 _refine_ls_wR_factor_ref 0.1916 _refine_ls_wR_factor_gt 0.1559 _refine_ls_goodness_of_fit_ref 0.969 _refine_ls_restrained_S_all 0.970 _refine_ls_shift/su_max 0.707 _refine_ls_shift/su_mean 0.031 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 0.0000 0.18072(6) 0.2500 0.0430(5) Uani 1 2 d S . . Cu2 Cu 0.0000 0.30211(6) 0.2500 0.0410(5) Uani 1 2 d S . . N1 N 0.0838(3) 0.2137(3) 0.1698(4) 0.0377(15) Uani 1 1 d . . . N2 N -0.0069(3) 0.3081(3) 0.1213(4) 0.0393(16) Uani 1 1 d . . . N21 N 0.0325(3) 0.2795(3) 0.0597(4) 0.0407(16) Uani 1 1 d . . . N3 N -0.0732(3) 0.1475(3) 0.1733(4) 0.0372(15) Uani 1 1 d . . . N31 N -0.1317(3) 0.1506(3) 0.2158(4) 0.0380(15) Uani 1 1 d . . . C1 C -0.1813(5) 0.2883(4) 0.0970(7) 0.075(3) Uani 1 1 d . . . H1A H -0.2166 0.2735 0.1343 0.113 Uiso 1 1 calc R . . H1B H -0.1432 0.2616 0.1073 0.113 Uiso 1 1 calc R . . H1C H -0.1953 0.2869 0.0320 0.113 Uiso 1 1 calc R . . C2 C -0.2553(5) 0.5003(4) 0.1997(6) 0.073(3) Uani 1 1 d . . . H2A H -0.2877 0.5032 0.1490 0.110 Uiso 1 1 calc R . . H2B H -0.2376 0.5418 0.2133 0.110 Uiso 1 1 calc R . . H2C H -0.2756 0.4838 0.2541 0.110 Uiso 1 1 calc R . . C3 C -0.0201(4) 0.4698(4) 0.1259(6) 0.071(3) Uani 1 1 d . . . H3A H -0.0196 0.5130 0.1474 0.107 Uiso 1 1 calc R . . H3B H -0.0098 0.4687 0.0610 0.107 Uiso 1 1 calc R . . H3C H 0.0123 0.4457 0.1618 0.107 Uiso 1 1 calc R . . C4 C 0.0325(4) 0.0358(4) 0.1348(5) 0.053(2) Uani 1 1 d . . . H4A H 0.0597 -0.0004 0.1227 0.079 Uiso 1 1 calc R . . H4B H -0.0103 0.0218 0.1529 0.079 Uiso 1 1 calc R . . H4C H 0.0529 0.0606 0.1843 0.079 Uiso 1 1 calc R . . C5 C 0.1245(5) 0.1061(5) -0.1635(6) 0.080(3) Uani 1 1 d . . . H5A H 0.1108 0.0812 -0.2171 0.119 Uiso 1 1 calc R . . H5B H 0.1635 0.0877 -0.1342 0.119 Uiso 1 1 calc R . . H5C H 0.1339 0.1487 -0.1830 0.119 Uiso 1 1 calc R . . C6 C -0.0982(4) 0.1799(4) -0.0849(6) 0.061(2) Uani 1 1 d . . . H6A H -0.0883 0.2084 -0.1349 0.091 Uiso 1 1 calc R . . H6B H -0.1124 0.2039 -0.0323 0.091 Uiso 1 1 calc R . . H6C H -0.1329 0.1514 -0.1057 0.091 Uiso 1 1 calc R . . C11 C 0.1358(3) 0.1786(3) 0.1968(5) 0.0356(18) Uani 1 1 d . . . C12 C 0.1898(4) 0.1690(4) 0.1446(5) 0.045(2) Uani 1 1 d . . . H12 H 0.2251 0.1439 0.1664 0.054 Uiso 1 1 calc R . . C13 C 0.1900(4) 0.1977(4) 0.0593(6) 0.056(2) Uani 1 1 d . . . H13 H 0.2258 0.1918 0.0215 0.067 Uiso 1 1 calc R . . C14 C 0.1384(4) 0.2351(4) 0.0284(5) 0.048(2) Uani 1 1 d . . . H14 H 0.1382 0.2553 -0.0295 0.058 Uiso 1 1 calc R . . C15 C 0.0868(4) 0.2414(3) 0.0870(5) 0.0359(18) Uani 1 1 d . . . C21 C 0.0140(4) 0.2964(4) -0.0285(5) 0.048(2) Uani 1 1 d . . . H21 H 0.0342 0.2838 -0.0828 0.058 Uiso 1 1 calc R . . C22 C -0.0390(4) 0.3349(4) -0.0240(5) 0.047(2) Uani 1 1 d . . . H22 H -0.0628 0.3533 -0.0740 0.057 Uiso 1 1 calc R . . C23 C -0.0508(4) 0.3417(3) 0.0705(5) 0.0422(19) Uani 1 1 d . . . C24 C -0.1014(4) 0.3795(3) 0.1138(5) 0.0409(19) Uani 1 1 d . . . C25 C -0.1641(4) 0.3549(4) 0.1238(6) 0.051(2) Uani 1 1 d . . . C26 C -0.2122(4) 0.3945(4) 0.1546(6) 0.055(2) Uani 1 1 d . . . H26 H -0.2542 0.3779 0.1633 0.066 Uiso 1 1 calc R . . C27 C -0.2014(4) 0.4578(4) 0.1733(5) 0.048(2) Uani 1 1 d . . . C28 C -0.1370(4) 0.4796(4) 0.1671(5) 0.054(2) Uani 1 1 d . . . H28 H -0.1277 0.5214 0.1837 0.065 Uiso 1 1 calc R . . C29 C -0.0866(4) 0.4421(4) 0.1376(5) 0.046(2) Uani 1 1 d . . . C31 C -0.1797(4) 0.1218(4) 0.1620(6) 0.050(2) Uani 1 1 d . . . H31 H -0.2240 0.1178 0.1759 0.060 Uiso 1 1 calc R . . C32 C -0.1516(4) 0.1004(4) 0.0856(6) 0.053(2) Uani 1 1 d . . . H32 H -0.1723 0.0782 0.0363 0.064 Uiso 1 1 calc R . . C33 C -0.0842(4) 0.1178(3) 0.0940(5) 0.0401(19) Uani 1 1 d . . . C34 C -0.0310(4) 0.1113(3) 0.0266(5) 0.0391(19) Uani 1 1 d . . . C35 C 0.0250(4) 0.0752(3) 0.0487(5) 0.044(2) Uani 1 1 d . . . C36 C 0.0746(4) 0.0739(4) -0.0146(5) 0.049(2) Uani 1 1 d . . . H36 H 0.1121 0.0494 -0.0011 0.059 Uiso 1 1 calc R . . C37 C 0.0709(4) 0.1073(4) -0.0962(6) 0.053(2) Uani 1 1 d . . . C38 C 0.0142(4) 0.1414(4) -0.1159(5) 0.055(2) Uani 1 1 d . . . H38 H 0.0111 0.1644 -0.1714 0.066 Uiso 1 1 calc R . . C39 C -0.0386(4) 0.1432(3) -0.0573(5) 0.0425(19) Uani 1 1 d . . . C1S C 0.1959(5) 0.5360(5) -0.4397(6) 0.070(3) Uani 1 1 d . . . C2S C 0.1587(5) 0.4774(4) -0.4200(6) 0.075(3) Uani 1 1 d . . . H2S1 H 0.1857 0.4411 -0.4320 0.113 Uiso 1 1 calc R . . H2S2 H 0.1191 0.4758 -0.4595 0.113 Uiso 1 1 calc R . . H2S3 H 0.1470 0.4772 -0.3556 0.113 Uiso 1 1 calc R . . C3S C 0.1609(6) 0.5966(5) -0.4237(8) 0.104(4) Uani 1 1 d . . . H3S1 H 0.1893 0.6314 -0.4383 0.156 Uiso 1 1 calc R . . H3S2 H 0.1495 0.5992 -0.3594 0.156 Uiso 1 1 calc R . . H3S3 H 0.1214 0.5983 -0.4632 0.156 Uiso 1 1 calc R . . O1S O 0.2500(4) 0.5346(4) -0.4688(5) 0.104(3) Uani 1 1 d . . . B1 B 0.3588(7) 0.1825(7) 0.2260(9) 0.088(4) Uani 1 1 d U . . F1 F 0.4187(6) 0.2135(6) 0.2375(8) 0.071(3) Uiso 0.50 1 d P . . F2 F 0.3969(7) 0.2305(6) 0.2107(9) 0.086(4) Uiso 0.50 1 d P . . F3 F 0.3441(3) 0.1554(3) 0.1422(4) 0.104(2) Uani 1 1 d . . . F4 F 0.3392(10) 0.1421(10) 0.2863(13) 0.053(6) Uiso 0.25 1 d P . . F5 F 0.3257(6) 0.1725(7) 0.2966(7) 0.066(3) Uiso 0.50 1 d P . . F6 F 0.3094(14) 0.2164(16) 0.269(2) 0.114(9) Uiso 0.25 1 d P . . F7 F 0.3142(10) 0.2441(10) 0.2066(15) 0.070(5) Uiso 0.25 1 d P . . F8 F 0.4151(8) 0.1295(8) 0.2552(10) 0.213(6) Uiso 0.75 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 Cu1 0.0363(8) 0.0456(9) 0.0469(9) 0.000 -0.0013(6) 0.000 Cu2 0.0453(8) 0.0414(8) 0.0362(8) 0.000 0.0018(6) 0.000 N1 0.039(4) 0.034(4) 0.040(4) -0.001(3) 0.002(3) 0.004(3) N2 0.044(4) 0.036(4) 0.038(4) -0.004(3) 0.007(3) 0.004(3) N21 0.048(4) 0.035(4) 0.040(4) 0.004(3) 0.005(3) 0.005(3) N3 0.040(4) 0.030(3) 0.041(4) -0.006(3) 0.001(3) -0.003(3) N31 0.038(4) 0.034(4) 0.042(4) 0.001(3) 0.003(3) -0.002(3) C1 0.063(6) 0.052(6) 0.112(8) -0.007(6) 0.013(6) 0.004(5) C2 0.083(7) 0.070(6) 0.068(6) -0.003(5) 0.016(5) 0.028(6) C3 0.080(7) 0.060(6) 0.076(6) 0.005(5) 0.027(5) -0.017(5) C4 0.062(5) 0.046(5) 0.050(5) 0.001(4) 0.000(4) 0.015(4) C5 0.074(7) 0.099(8) 0.068(6) 0.001(6) 0.032(5) 0.012(6) C6 0.067(6) 0.064(6) 0.051(5) 0.005(4) -0.001(4) 0.006(5) C11 0.040(5) 0.029(4) 0.038(5) 0.001(4) 0.006(4) 0.000(4) C12 0.039(5) 0.042(5) 0.056(5) 0.011(4) 0.013(4) 0.010(4) C13 0.048(5) 0.048(5) 0.074(6) 0.007(5) 0.022(5) 0.012(4) C14 0.053(5) 0.045(5) 0.048(5) 0.006(4) 0.021(4) 0.005(4) C15 0.045(5) 0.028(4) 0.035(4) -0.001(4) 0.004(4) 0.003(4) C21 0.061(6) 0.047(5) 0.038(5) 0.002(4) 0.004(4) -0.001(5) C22 0.050(5) 0.053(5) 0.039(5) -0.001(4) 0.004(4) 0.007(4) C23 0.039(5) 0.034(4) 0.053(5) 0.004(4) 0.000(4) 0.002(4) C24 0.046(5) 0.035(5) 0.042(5) 0.005(4) 0.002(4) 0.010(4) C25 0.052(6) 0.043(5) 0.059(5) 0.007(4) -0.001(4) 0.003(5) C26 0.046(5) 0.049(6) 0.070(6) 0.010(4) 0.008(4) 0.014(5) C27 0.058(6) 0.045(6) 0.042(5) 0.004(4) 0.006(4) 0.027(5) C28 0.070(6) 0.037(5) 0.055(5) -0.002(4) 0.009(5) -0.006(5) C29 0.056(5) 0.048(5) 0.033(4) 0.002(4) 0.004(4) 0.008(5) C31 0.052(5) 0.043(5) 0.055(5) -0.004(4) 0.005(4) -0.017(4) C32 0.052(6) 0.054(5) 0.053(6) -0.013(4) -0.011(4) -0.010(4) C33 0.048(5) 0.035(4) 0.037(5) -0.005(4) -0.005(4) 0.003(4) C34 0.044(5) 0.034(4) 0.039(5) -0.004(4) -0.006(4) -0.009(4) C35 0.067(6) 0.035(4) 0.030(4) -0.006(4) -0.005(4) 0.003(4) C36 0.062(6) 0.035(5) 0.049(5) -0.008(4) 0.006(4) 0.002(4) C37 0.056(6) 0.045(5) 0.057(6) -0.006(4) 0.003(5) 0.001(5) C38 0.073(6) 0.059(6) 0.033(5) 0.003(4) 0.011(5) -0.004(5) C39 0.054(5) 0.036(4) 0.037(5) 0.000(4) -0.001(4) -0.006(4) C1S 0.069(7) 0.091(8) 0.049(6) 0.003(5) -0.005(5) 0.002(7) C2S 0.088(7) 0.067(7) 0.070(6) -0.012(5) -0.011(5) -0.001(6) C3S 0.111(10) 0.078(8) 0.124(10) 0.032(7) 0.012(8) 0.012(7) O1S 0.061(5) 0.139(7) 0.112(6) -0.016(5) 0.004(4) -0.005(5) B1 0.077(7) 0.109(8) 0.077(7) -0.010(7) 0.003(6) -0.020(7) F3 0.096(5) 0.136(5) 0.080(4) -0.018(4) -0.009(3) -0.014(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 N3 1.956(6) . ? Cu1 N3 1.956(6) 6_556 ? Cu1 N1 2.221(6) 6_556 ? Cu1 N1 2.221(6) . ? Cu1 Cu2 2.5840(19) . ? Cu2 N2 1.863(6) . ? Cu2 N2 1.863(6) 6_556 ? N1 C11 1.343(9) . ? N1 C15 1.337(9) . ? N2 C23 1.343(9) . ? N2 N21 1.367(8) . ? N21 C21 1.362(9) . ? N21 C15 1.418(9) . ? N3 C33 1.320(8) . ? N3 N31 1.366(8) . ? N31 C31 1.369(9) . ? N31 C11 1.403(9) 6_556 ? C1 C25 1.509(11) . ? C2 C27 1.488(10) . ? C3 C29 1.497(11) . ? C4 C35 1.503(10) . ? C5 C37 1.495(11) . ? C6 C39 1.488(11) . ? C11 C12 1.378(10) . ? C11 N31 1.403(9) 6_556 ? C12 C13 1.376(11) . ? C13 C14 1.381(11) . ? C14 C15 1.386(10) . ? C21 C22 1.361(10) . ? C22 C23 1.404(10) . ? C23 C24 1.468(10) . ? C24 C25 1.397(11) . ? C24 C29 1.408(11) . ? C25 C26 1.383(11) . ? C26 C27 1.388(11) . ? C27 C28 1.401(11) . ? C28 C29 1.384(11) . ? C31 C32 1.346(10) . ? C32 C33 1.426(10) . ? C33 C34 1.496(10) . ? C34 C39 1.393(10) . ? C34 C35 1.405(10) . ? C35 C36 1.393(10) . ? C36 C37 1.376(10) . ? C37 C38 1.386(11) . ? C38 C39 1.398(10) . ? C1S O1S 1.200(10) . ? C1S C2S 1.494(13) . ? C1S C3S 1.497(14) . ? B1 F5 1.265(16) . ? B1 F2 1.310(17) . ? B1 F4 1.30(2) . ? B1 F6 1.41(3) . ? B1 F1 1.396(17) . ? B1 F3 1.363(13) . ? B1 F7 1.62(2) . ? B1 F8 1.65(2) . ? F1 F2 0.681(15) . ? F4 F5 0.72(2) . ? F4 F6 1.71(4) . ? F4 F8 1.65(2) . ? F5 F6 1.06(3) . ? F6 F7 1.09(3) . ? 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 N3 Cu1 N3 137.7(3) . 6_556 ? N3 Cu1 N1 79.7(2) . 6_556 ? N3 Cu1 N1 114.0(2) 6_556 6_556 ? N3 Cu1 N1 114.0(2) . . ? N3 Cu1 N1 79.7(2) 6_556 . ? N1 Cu1 N1 143.2(3) 6_556 . ? N2 Cu2 N2 172.1(4) . 6_556 ? C11 N1 C15 116.2(6) . . ? C11 N1 Cu1 106.9(4) . . ? C15 N1 Cu1 132.1(5) . . ? C23 N2 N21 106.2(6) . . ? C23 N2 Cu2 127.1(5) . . ? N21 N2 Cu2 126.7(5) . . ? N2 N21 C21 110.2(6) . . ? N2 N21 C15 123.2(6) . . ? C21 N21 C15 126.6(6) . . ? C33 N3 N31 107.0(6) . . ? C33 N3 Cu1 139.7(5) . . ? N31 N3 Cu1 113.0(4) . . ? N3 N31 C31 110.1(6) . . ? N3 N31 C11 120.7(6) . 6_556 ? C31 N31 C11 129.3(6) . 6_556 ? N1 C11 C12 124.4(6) . . ? N1 C11 N31 115.0(6) . 6_556 ? C12 C11 N31 120.6(7) . 6_556 ? C11 C12 C13 117.1(7) . . ? C12 C13 C14 121.1(7) . . ? C13 C14 C15 116.6(7) . . ? N1 C15 C14 124.6(7) . . ? N1 C15 N21 116.0(6) . . ? C14 C15 N21 119.4(7) . . ? C22 C21 N21 107.7(7) . . ? C21 C22 C23 106.2(7) . . ? N2 C23 C22 109.8(6) . . ? N2 C23 C24 121.7(7) . . ? C22 C23 C24 128.5(7) . . ? C25 C24 C29 121.2(7) . . ? C25 C24 C23 120.2(7) . . ? C29 C24 C23 118.4(7) . . ? C26 C25 C24 118.2(7) . . ? C26 C25 C1 119.6(8) . . ? C24 C25 C1 122.1(7) . . ? C27 C26 C25 122.9(8) . . ? C26 C27 C28 116.8(7) . . ? C26 C27 C2 121.8(8) . . ? C28 C27 C2 121.4(8) . . ? C29 C28 C27 122.8(8) . . ? C28 C29 C24 117.8(7) . . ? C28 C29 C3 119.9(7) . . ? C24 C29 C3 122.2(7) . . ? C32 C31 N31 107.3(7) . . ? C31 C32 C33 106.5(7) . . ? N3 C33 C32 109.1(7) . . ? N3 C33 C34 120.6(7) . . ? C32 C33 C34 130.1(7) . . ? C39 C34 C35 121.6(7) . . ? C39 C34 C33 117.7(7) . . ? C35 C34 C33 120.7(6) . . ? C36 C35 C34 118.0(7) . . ? C36 C35 C4 118.7(7) . . ? C34 C35 C4 123.1(7) . . ? C37 C36 C35 122.4(8) . . ? C36 C37 C38 117.5(8) . . ? C36 C37 C5 122.2(8) . . ? C38 C37 C5 120.2(8) . . ? C37 C38 C39 123.3(7) . . ? C34 C39 C38 117.0(7) . . ? C34 C39 C6 123.3(7) . . ? C38 C39 C6 119.7(7) . . ? O1S C1S C2S 122.0(10) . . ? O1S C1S C3S 121.9(11) . . ? C2S C1S C3S 116.1(9) . . ? F5 B1 F2 127.4(14) . . ? F5 B1 F4 32.7(9) . . ? F2 B1 F4 146.3(15) . . ? F5 B1 F6 46.5(13) . . ? F2 B1 F6 96.7(18) . . ? F4 B1 F6 78.2(17) . . ? F5 B1 F1 118.6(12) . . ? F2 B1 F1 29.0(7) . . ? F4 B1 F1 121.9(14) . . ? F6 B1 F1 110.2(16) . . ? F5 B1 F3 122.7(12) . . ? F2 B1 F3 106.9(12) . . ? F4 B1 F3 104.6(14) . . ? F6 B1 F3 118.4(16) . . ? F1 B1 F3 117.8(11) . . ? F5 B1 F7 87.7(12) . . ? F2 B1 F7 70.8(12) . . ? F4 B1 F7 117.8(16) . . ? F6 B1 F7 41.5(14) . . ? F1 B1 F7 96.9(13) . . ? F3 B1 F7 95.0(11) . . ? F5 B1 F8 94.0(12) . . ? F2 B1 F8 99.4(12) . . ? F4 B1 F8 66.9(13) . . ? F6 B1 F8 137.8(19) . . ? F1 B1 F8 72.2(10) . . ? F3 B1 F8 93.6(10) . . ? F7 B1 F8 168.5(13) . . ? F2 F1 B1 68.5(17) . . ? F1 F2 B1 82.5(19) . . ? F5 F4 B1 71(2) . . ? F5 F4 F6 20.5(18) . . ? B1 F4 F6 53.7(13) . . ? F5 F4 F8 125(2) . . ? B1 F4 F8 66.8(12) . . ? F6 F4 F8 116.3(16) . . ? F4 F5 F6 146(3) . . ? F4 F5 B1 76(2) . . ? F6 F5 B1 73.8(18) . . ? F5 F6 F7 139(3) . . ? F5 F6 B1 59.7(18) . . ? F7 F6 B1 80(2) . . ? F5 F6 F4 13.7(12) . . ? F7 F6 F4 125(3) . . ? B1 F6 F4 48.1(13) . . ? F6 F7 B1 59.0(19) . . ? F4 F8 B1 46.3(9) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 20.99 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.577 _refine_diff_density_min -0.449 _refine_diff_density_rms 0.078 #=END data_nks149/sy327/3(PF6)2 _audit_creation_method SHELXL _chemical_name_systematic ; Bis[2,6-bis-(3-tert-butylpyrazol-1-yl)pyridine]dicopper(I) dihexafluorophosphate ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C38 H50 Cu2 F12 N10 P2' _chemical_formula_weight 1063.90 _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' '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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 20.732(5) _cell_length_b 12.235(2) _cell_length_c 9.238(5) _cell_angle_alpha 90.00 _cell_angle_beta 95.35(2) _cell_angle_gamma 90.00 _cell_volume 2333.2(14) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 39 _cell_measurement_theta_min 5.10 _cell_measurement_theta_max 12.58 _exptl_crystal_description block _exptl_crystal_colour yellow-green _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.55 _exptl_crystal_size_min 0.48 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.514 _exptl_crystal_density_method ? _exptl_crystal_F_000 1088 _exptl_absorpt_coefficient_mu 1.068 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.18211 _exptl_absorpt_correction_T_max 0.92340 _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method theta/2theta _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 1 _diffrn_reflns_number 2580 _diffrn_reflns_av_R_equivalents 0.0414 _diffrn_reflns_av_sigmaI/netI 0.0373 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 1 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2373 _reflns_number_observed 1968 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _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^)+(0.0747P)^2^+3.4010P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.01(3) _refine_ls_number_reflns 2373 _refine_ls_number_parameters 289 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0653 _refine_ls_R_factor_obs 0.0498 _refine_ls_wR_factor_all 0.1321 _refine_ls_wR_factor_obs 0.1217 _refine_ls_goodness_of_fit_all 1.055 _refine_ls_goodness_of_fit_obs 1.081 _refine_ls_restrained_S_all 1.055 _refine_ls_restrained_S_obs 1.080 _refine_ls_shift/esd_max -0.040 _refine_ls_shift/esd_mean 0.006 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 Cu1 Cu 0.55320(4) 0.16109(8) -0.09260(8) 0.0491(3) Uani 1 d . . N1 N 0.4490(2) 0.1472(6) -0.1985(5) 0.0370(12) Uani 1 d . . N2 N 0.4985(3) -0.0141(5) -0.2549(6) 0.0425(14) Uani 1 d . . N3 N 0.4018(3) 0.3090(5) -0.1279(6) 0.0434(14) Uani 1 d . . N21 N 0.5543(3) 0.0161(5) -0.1743(6) 0.0408(13) Uani 1 d . . N31 N 0.4153(3) 0.2978(5) 0.0179(6) 0.0404(13) Uani 1 d . . C11 C 0.4011(3) 0.2199(6) -0.2239(7) 0.041(2) Uani 1 d . . C12 C 0.3525(4) 0.2100(9) -0.3350(8) 0.065(2) Uani 1 d . . H12 H 0.3194(4) 0.2624(9) -0.3499(8) 0.077 Uiso 1 calc R . C13 C 0.3546(4) 0.1203(9) -0.4229(9) 0.071(3) Uani 1 d . . H13 H 0.3219(4) 0.1104(9) -0.4995(9) 0.085 Uiso 1 calc R . C14 C 0.4027(4) 0.0452(9) -0.4019(8) 0.062(2) Uani 1 d . . H14 H 0.4051(4) -0.0149(9) -0.4646(8) 0.074 Uiso 1 calc R . C15 C 0.4480(3) 0.0612(7) -0.2842(7) 0.042(2) Uani 1 d . . C21 C 0.5044(5) -0.1184(7) -0.3019(10) 0.066(2) Uani 1 d . . H21 H 0.4727(5) -0.1582(7) -0.3591(10) 0.079 Uiso 1 calc R . C22 C 0.5641(5) -0.1552(8) -0.2519(11) 0.071(3) Uani 1 d . . H22 H 0.5816(5) -0.2246(8) -0.2673(11) 0.086 Uiso 1 calc R . C23 C 0.5941(4) -0.0700(7) -0.1736(9) 0.048(2) Uani 1 d . . C24 C 0.6625(4) -0.0667(8) -0.1008(9) 0.056(2) Uani 1 d . . C25 C 0.7017(5) 0.0017(18) -0.1926(19) 0.181(10) Uani 1 d . . H25A H 0.6994(5) -0.0284(18) -0.2901(19) 0.272 Uiso 1 calc R . H25B H 0.7465(5) 0.0023(18) -0.1511(19) 0.272 Uiso 1 calc R . H25C H 0.6849(5) 0.0757(18) -0.1964(19) 0.272 Uiso 1 calc R . C26 C 0.6632(6) -0.0266(14) 0.0503(13) 0.131(6) Uani 1 d . . H26A H 0.6367(6) -0.0741(14) 0.1046(13) 0.196 Uiso 1 calc R . H26B H 0.6460(6) 0.0471(14) 0.0498(13) 0.196 Uiso 1 calc R . H26C H 0.7073(6) -0.0265(14) 0.0955(13) 0.196 Uiso 1 calc R . C27 C 0.6909(7) -0.1826(11) -0.0930(14) 0.112(5) Uani 1 d . . H27A H 0.6657(7) -0.2282(11) -0.0334(14) 0.168 Uiso 1 calc R . H27B H 0.7355(7) -0.1798(11) -0.0504(14) 0.168 Uiso 1 calc R . H27C H 0.6896(7) -0.2131(11) -0.1901(14) 0.168 Uiso 1 calc R . C31 C 0.3848(4) 0.4145(8) -0.1615(11) 0.066(3) Uani 1 d . . H31 H 0.3751(4) 0.4431(8) -0.2554(11) 0.079 Uiso 1 calc R . C32 C 0.3844(4) 0.4696(7) -0.0366(10) 0.062(2) Uani 1 d . . H32 H 0.3732(4) 0.5435(7) -0.0260(10) 0.075 Uiso 1 calc R . C33 C 0.4040(4) 0.3953(6) 0.0765(9) 0.048(2) Uani 1 d . . C34 C 0.4076(4) 0.4183(7) 0.2353(10) 0.057(2) Uani 1 d . . C35 C 0.3399(5) 0.4439(14) 0.2740(13) 0.114(5) Uani 1 d . . H35A H 0.3411(5) 0.4592(14) 0.3772(13) 0.171 Uiso 1 calc R . H35B H 0.3119(5) 0.3816(14) 0.2503(13) 0.171 Uiso 1 calc R . H35C H 0.3233(5) 0.5072(14) 0.2193(13) 0.171 Uiso 1 calc R . C36 C 0.4348(7) 0.3244(10) 0.3279(10) 0.104(4) Uani 1 d . . H36A H 0.4359(7) 0.3441(10) 0.4298(10) 0.156 Uiso 1 calc R . H36B H 0.4784(7) 0.3082(10) 0.3042(10) 0.156 Uiso 1 calc R . H36C H 0.4077(7) 0.2604(10) 0.3093(10) 0.156 Uiso 1 calc R . C37 C 0.4499(7) 0.5158(12) 0.2733(15) 0.111(5) Uani 1 d . . H37A H 0.4515(7) 0.5294(12) 0.3770(15) 0.167 Uiso 1 calc R . H37B H 0.4323(7) 0.5793(12) 0.2207(15) 0.167 Uiso 1 calc R . H37C H 0.4933(7) 0.5015(12) 0.2468(15) 0.167 Uiso 1 calc R . P1 P 0.66793(11) -0.2989(2) -0.6011(3) 0.0573(6) Uani 1 d . . F1 F 0.6016(3) -0.3062(11) -0.5420(8) 0.167(5) Uani 1 d . . F2 F 0.6373(5) -0.3040(11) -0.7565(7) 0.171(5) Uani 1 d . . F3 F 0.6794(6) -0.4263(6) -0.6002(9) 0.153(4) Uani 1 d . . F4 F 0.6558(5) -0.1761(7) -0.6054(13) 0.163(4) Uani 1 d . . F5 F 0.6974(3) -0.3045(7) -0.4422(7) 0.125(3) Uani 1 d . . F6 F 0.7355(4) -0.2834(8) -0.6538(11) 0.150(4) Uani 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 0.0571(5) 0.0413(4) 0.0475(4) -0.0030(4) -0.0028(3) -0.0055(5) N1 0.028(2) 0.048(3) 0.035(2) 0.004(3) 0.006(2) -0.001(3) N2 0.031(3) 0.046(3) 0.046(3) -0.002(3) 0.012(2) 0.003(3) N3 0.029(3) 0.048(3) 0.044(3) -0.002(3) 0.005(2) 0.008(3) N21 0.035(3) 0.051(3) 0.042(3) -0.010(3) 0.011(3) -0.007(3) N31 0.034(3) 0.049(3) 0.048(3) 0.004(3) 0.007(3) 0.008(3) C11 0.027(3) 0.063(5) 0.035(3) 0.004(3) 0.009(3) 0.002(3) C12 0.039(4) 0.105(7) 0.049(4) -0.006(5) -0.001(3) 0.012(4) C13 0.042(4) 0.117(9) 0.053(4) -0.015(5) -0.004(4) 0.007(5) C14 0.044(4) 0.097(7) 0.045(4) -0.019(4) 0.003(3) -0.003(5) C15 0.030(3) 0.061(4) 0.037(3) -0.009(3) 0.018(3) -0.010(3) C21 0.071(6) 0.050(5) 0.077(6) -0.024(4) 0.010(5) -0.013(5) C22 0.081(7) 0.051(5) 0.085(7) -0.013(5) 0.023(6) 0.005(5) C23 0.045(4) 0.050(4) 0.050(4) -0.010(4) 0.014(4) 0.003(4) C24 0.041(4) 0.075(5) 0.056(5) 0.005(4) 0.023(4) 0.021(4) C25 0.050(6) 0.265(24) 0.227(17) 0.162(18) -0.003(8) -0.026(10) C26 0.089(8) 0.182(14) 0.111(9) -0.070(10) -0.045(7) 0.077(9) C27 0.111(9) 0.108(10) 0.112(9) -0.026(8) -0.010(8) 0.057(8) C31 0.047(5) 0.069(6) 0.084(6) 0.029(5) 0.018(4) 0.019(4) C32 0.061(5) 0.048(4) 0.080(6) 0.000(4) 0.017(5) 0.014(4) C33 0.042(4) 0.042(4) 0.061(5) -0.006(4) 0.010(4) 0.009(3) C34 0.053(5) 0.053(5) 0.065(5) -0.016(4) 0.007(4) 0.013(4) C35 0.072(7) 0.188(15) 0.086(7) -0.044(9) 0.026(6) 0.015(9) C36 0.175(13) 0.093(8) 0.045(5) -0.012(5) 0.010(6) 0.041(9) C37 0.100(9) 0.118(12) 0.115(10) -0.052(9) 0.006(7) -0.014(8) P1 0.0520(12) 0.0648(13) 0.0572(12) -0.0039(10) 0.0159(10) 0.0085(10) F1 0.065(4) 0.301(16) 0.142(6) 0.097(8) 0.045(4) 0.039(6) F2 0.208(8) 0.230(14) 0.070(4) 0.020(6) -0.025(4) -0.029(8) F3 0.283(12) 0.068(4) 0.108(6) -0.013(4) 0.033(7) -0.034(7) F4 0.169(8) 0.079(5) 0.240(11) 0.004(6) 0.020(8) 0.044(5) F5 0.123(5) 0.143(7) 0.103(4) -0.022(5) -0.032(4) 0.009(5) F6 0.091(5) 0.155(8) 0.219(9) 0.066(7) 0.086(5) 0.040(5) _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 N3 1.902(6) 2_655 ? Cu1 N2 1.929(6) . ? Cu1 N1 2.293(4) . ? Cu1 Cu1 2.915(2) 2_655 ? N1 C15 1.317(9) . ? N1 C11 1.337(9) . ? N21 C21 1.357(10) . ? N21 N2 1.368(8) . ? N21 C15 1.402(9) . ? N31 N3 1.357(8) . ? N31 C31 1.366(11) . ? N31 C11 1.404(9) . ? N2 C23 1.336(10) . ? N3 C33 1.339(9) . ? C11 C12 1.376(9) . ? C12 C13 1.368(13) . ? C13 C14 1.356(13) . ? C14 C15 1.383(10) . ? C21 C22 1.356(14) . ? C22 C23 1.383(13) . ? C23 C24 1.513(11) . ? C24 C25 1.486(15) . ? C24 C26 1.479(14) . ? C24 C27 1.535(14) . ? C31 C32 1.337(13) . ? C32 C33 1.416(11) . ? C33 C34 1.489(11) . ? C34 C37 1.502(15) . ? C34 C35 1.512(13) . ? C34 C36 1.511(14) . ? P1 F2 1.516(7) . ? P1 F4 1.523(8) . ? P1 F1 1.528(6) . ? P1 F6 1.537(7) . ? P1 F5 1.538(6) . ? P1 F3 1.576(9) . ? 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 N3 Cu1 N2 159.2(2) 2_655 . ? N3 Cu1 N1 119.8(2) 2_655 . ? N2 Cu1 N1 79.1(2) . . ? C15 N1 C11 117.2(5) . . ? C15 N1 Cu1 106.1(4) . . ? C11 N1 Cu1 132.9(5) . . ? C21 N21 N2 109.3(7) . . ? C21 N21 C15 130.1(7) . . ? N2 N21 C15 120.5(6) . . ? N3 N31 C31 110.2(7) . . ? N3 N31 C11 122.5(6) . . ? C31 N3 C11 127.1(7) . . ? C23 N2 N21 106.3(6) . . ? C23 N2 Cu1 138.8(5) . . ? N21 N2 Cu1 114.9(4) . . ? C33 N3 N31 106.5(6) . . ? C33 N3 Cu1 134.8(5) . 2_655 ? N31 N3 Cu1 118.7(4) . 2_655 ? N1 C11 C12 123.6(7) . . ? N1 C11 N31 116.2(5) . . ? C12 C11 N31 120.2(7) . . ? C13 C12 C11 116.8(8) . . ? C14 C13 C12 121.5(7) . . ? C13 C14 C15 116.9(8) . . ? N1 C15 C14 123.9(7) . . ? N1 C15 N21 116.1(6) . . ? C14 C15 N21 120.0(7) . . ? C22 C21 N21 108.1(8) . . ? C21 C22 C23 106.2(8) . . ? N2 C23 C22 110.2(7) . . ? N2 C23 C24 122.3(7) . . ? C22 C23 C24 127.5(8) . . ? C25 C24 C26 113.2(13) . . ? C25 C24 C23 107.6(7) . . ? C26 C24 C23 110.8(7) . . ? C25 C24 C27 108.6(11) . . ? C26 C24 C27 107.0(9) . . ? C23 C24 C27 109.7(8) . . ? C32 C31 N31 107.6(8) . . ? C31 C32 C33 106.7(8) . . ? N3 C33 C32 108.9(7) . . ? N3 C33 C34 124.9(7) . . ? C32 C33 C34 126.2(7) . . ? C33 C34 C37 110.8(9) . . ? C33 C34 C35 108.1(7) . . ? C37 C34 C35 108.4(10) . . ? C33 C34 C36 113.3(7) . . ? C37 C34 C36 107.0(10) . . ? C35 C34 C36 109.2(10) . . ? F2 P1 F4 87.8(7) . . ? F2 P1 F1 91.4(5) . . ? F4 P1 F1 85.1(6) . . ? F2 P1 F6 91.1(6) . . ? F4 P1 F6 91.4(5) . . ? F1 P1 F6 175.6(6) . . ? F2 P1 F5 174.9(6) . . ? F4 P1 F5 96.9(6) . . ? F1 P1 F5 87.0(4) . . ? F6 P1 F5 90.9(5) . . ? F2 P1 F3 90.8(6) . . ? F4 P1 F3 178.6(6) . . ? F1 P1 F3 94.6(6) . . ? F6 P1 F3 89.0(6) . . ? F5 P1 F3 84.5(5) . . ? _refine_diff_density_max 0.490 _refine_diff_density_min -0.327 _refine_diff_density_rms 0.069