Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Halcrow, Malcolm A.' 'Collison, D.' 'Davies, John E.' 'Kilner, Colin A.' 'McInnes, E.' 'Solanki, Nayan K.' _publ_contact_author_name 'Dr Malcolm A Halcrow' _publ_contact_author_address ; Department of Chemistry University of Leeds Woodhouse Lane LEEDS LS2 9JT ; _publ_contact_author_email 'M.A.HALCROW@CHEM.LEEDS.AC.UK' _publ_section_title ; Copper(II) complexes of 2,6-Bis-(3-tert-butylpyrazol-1-yl)pyridine. ; data_nks130lt _database_code_CSD 175839 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Dichlorobis[2,6-bis(3-tert-butylpyrazolyl)pyridine]dicopper(II) ditetrafluoroborate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H50 Cl2 Cu2 N10, 2[B F4]' _chemical_formula_sum 'C38 H50 B2 Cl2 Cu2 F8 N10' _chemical_formula_weight 1018.48 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' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.1630(1) _cell_length_b 12.9098(2) _cell_length_c 19.5616(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.4727(6) _cell_angle_gamma 90.00 _cell_volume 2313.91(6) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 41554 _cell_measurement_theta_min 2.61 _cell_measurement_theta_max 27.50 _exptl_crystal_description Prism _exptl_crystal_colour Green _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.462 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1044 _exptl_absorpt_coefficient_mu 1.107 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6914 _exptl_absorpt_correction_T_max 0.8428 _exptl_absorpt_process_details ; Using multiple and symmetry-related data measurements via the program SORTAV See R.H. Blessing, Acta Cryst (1995), A51, 33-38 ; _exptl_special_details ; Detector set at 30mm from sample with different 2theta offsets 1 degree phi exposures for chi=0 degree settings 1 degree omega exposures for chi=90 degree settings ; _diffrn_ambient_temperature 100(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 'Nonius KappaCCD diffractometer' _diffrn_measurement_method 'Area detector scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 41554 _diffrn_reflns_av_R_equivalents 0.0591 _diffrn_reflns_av_sigmaI/netI 0.0345 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.61 _diffrn_reflns_theta_max 27.50 _reflns_number_total 5300 _reflns_number_gt 4438 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1999)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (McArdle, 1995)' _computing_publication_material 'local program' _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. The asymmetric unit contains half a dimeric molecule, lying across the crystallographic inversion centre 0.5, 0.5, 0.5. The tert-butyl group centred on C22 is disordered over two equally occupied orientations, C22A and C22B. All disordered C-C bonds were restrained to 1.53(2)/%A, and non-bonded 1,3-C...C contacts within a given disorder orientation to 2.50(2)\%A. The BF~4~^-^ anion is also disordered over two equally occupied orientations, B27A-F31A and B27B-B31B. All B-F bonds were restrained to 1.38(2)/%A, and non-bonded F...F contacts within a given disorder orientation to 2.25(2)\%A. All non-H atoms were refined anisotropically. All H atoms were placed in calculated positions and refined using a riding model. ; _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^)+(0.0647P)^2^+1.0277P] 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 5300 _refine_ls_number_parameters 363 _refine_ls_number_restraints 40 _refine_ls_R_factor_all 0.0490 _refine_ls_R_factor_gt 0.0367 _refine_ls_wR_factor_ref 0.1080 _refine_ls_wR_factor_gt 0.0998 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.002 _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 0.57509(3) 0.475206(18) 0.405502(12) 0.02484(10) Uani 1 1 d . . . N2 N 0.4296(2) 0.52226(13) 0.33973(9) 0.0252(4) Uani 1 1 d . . . C3 C 0.3246(2) 0.45769(17) 0.31894(11) 0.0274(4) Uani 1 1 d . . . C4 C 0.2025(3) 0.4909(2) 0.28316(11) 0.0329(5) Uani 1 1 d . . . H4 H 0.1306 0.4449 0.2685 0.039 Uiso 1 1 calc R . . C5 C 0.1925(2) 0.5963(2) 0.27020(11) 0.0330(5) Uani 1 1 d . . . H5 H 0.1116 0.6216 0.2466 0.040 Uiso 1 1 calc R B . C6 C 0.3002(2) 0.66512(18) 0.29155(11) 0.0294(5) Uani 1 1 d . . . H6 H 0.2935 0.7357 0.2827 0.035 Uiso 1 1 calc R . . C7 C 0.4176(2) 0.62314(16) 0.32662(10) 0.0241(4) Uani 1 1 d . . . N8 N 0.3524(2) 0.35511(14) 0.33816(9) 0.0305(4) Uani 1 1 d . B . N9 N 0.4748(2) 0.33395(13) 0.37723(9) 0.0284(4) Uani 1 1 d . B . C10 C 0.4812(3) 0.23014(17) 0.38100(12) 0.0338(5) Uani 1 1 d . . . C11 C 0.3624(3) 0.18623(19) 0.34443(12) 0.0422(6) Uani 1 1 d . . . H11 H 0.3418 0.1161 0.3393 0.051 Uiso 1 1 calc R . . C12 C 0.2846(3) 0.2664(2) 0.31832(12) 0.0401(6) Uani 1 1 d . . . H12 H 0.2004 0.2615 0.2917 0.048 Uiso 1 1 calc R B . C13 C 0.5976(3) 0.17154(17) 0.42039(12) 0.0375(5) Uani 1 1 d . . . C14 C 0.5603(3) 0.17468(19) 0.49665(12) 0.0409(6) Uani 1 1 d . . . H14A H 0.6335 0.1378 0.5222 0.049 Uiso 1 1 calc R B . H14B H 0.4669 0.1428 0.5036 0.049 Uiso 1 1 calc R . . H14C H 0.5571 0.2454 0.5118 0.049 Uiso 1 1 calc R . . C15 C 0.7495(3) 0.21583(18) 0.40716(13) 0.0392(6) Uani 1 1 d . . . H15A H 0.8208 0.1771 0.4328 0.047 Uiso 1 1 calc R B . H15B H 0.7525 0.2871 0.4211 0.047 Uiso 1 1 calc R . . H15C H 0.7708 0.2111 0.3593 0.047 Uiso 1 1 calc R . . C16 C 0.5959(4) 0.0572(2) 0.39700(15) 0.0501(7) Uani 1 1 d . . . H16A H 0.6696 0.0193 0.4216 0.060 Uiso 1 1 calc R B . H16B H 0.6151 0.0537 0.3489 0.060 Uiso 1 1 calc R . . H16C H 0.5019 0.0276 0.4060 0.060 Uiso 1 1 calc R . . N17 N 0.53584(18) 0.68003(13) 0.35232(9) 0.0239(4) Uani 1 1 d . A . N18 N 0.64325(18) 0.62853(13) 0.38909(9) 0.0241(4) Uani 1 1 d . A . C19 C 0.7491(2) 0.69847(17) 0.39896(10) 0.0259(4) Uani 1 1 d D . . C20 C 0.7084(2) 0.79404(17) 0.36869(11) 0.0291(4) Uani 1 1 d . A . H20 H 0.7630 0.8548 0.3685 0.035 Uiso 1 1 calc R . . C21 C 0.5743(2) 0.77974(16) 0.34003(11) 0.0282(4) Uani 1 1 d . . . H21 H 0.5193 0.8289 0.3165 0.034 Uiso 1 1 calc R A . C22A C 0.8907(15) 0.6826(13) 0.4401(8) 0.027(3) Uani 0.50 1 d PD A 1 C23A C 0.855(2) 0.6922(15) 0.5165(6) 0.028(3) Uani 0.50 1 d PD A 1 H23A H 0.9429 0.6832 0.5431 0.034 Uiso 0.50 1 calc PR A 1 H23B H 0.7856 0.6400 0.5288 0.034 Uiso 0.50 1 calc PR A 1 H23C H 0.8150 0.7595 0.5254 0.034 Uiso 0.50 1 calc PR A 1 C24A C 0.9591(17) 0.5789(11) 0.4217(9) 0.028(3) Uani 0.50 1 d PD A 1 H24A H 1.0479 0.5698 0.4474 0.033 Uiso 0.50 1 calc PR A 1 H24B H 0.9801 0.5776 0.3737 0.033 Uiso 0.50 1 calc PR A 1 H24C H 0.8925 0.5240 0.4324 0.033 Uiso 0.50 1 calc PR A 1 C25A C 0.9980(16) 0.7700(14) 0.4206(13) 0.038(3) Uani 0.50 1 d PD A 1 H25A H 1.0875 0.7617 0.4459 0.046 Uiso 0.50 1 calc PR A 1 H25B H 0.9555 0.8360 0.4312 0.046 Uiso 0.50 1 calc PR A 1 H25C H 1.0177 0.7666 0.3725 0.046 Uiso 0.50 1 calc PR A 1 C22B C 0.8911(15) 0.6692(12) 0.4340(8) 0.031(4) Uani 0.50 1 d PD A 2 C23B C 0.868(2) 0.6718(15) 0.5125(6) 0.031(3) Uani 0.50 1 d PD A 2 H23D H 0.9565 0.6523 0.5355 0.037 Uiso 0.50 1 calc PR A 2 H23E H 0.7915 0.6243 0.5245 0.037 Uiso 0.50 1 calc PR A 2 H23F H 0.8405 0.7406 0.5262 0.037 Uiso 0.50 1 calc PR A 2 C24B C 0.9428(16) 0.5621(11) 0.4124(9) 0.029(3) Uani 0.50 1 d PD A 2 H24D H 1.0329 0.5461 0.4354 0.035 Uiso 0.50 1 calc PR A 2 H24E H 0.9577 0.5611 0.3638 0.035 Uiso 0.50 1 calc PR A 2 H24F H 0.8705 0.5115 0.4242 0.035 Uiso 0.50 1 calc PR A 2 C25B C 1.0087(16) 0.7504(14) 0.4162(12) 0.039(3) Uani 0.50 1 d PD A 2 H25D H 1.0995 0.7315 0.4377 0.047 Uiso 0.50 1 calc PR A 2 H25E H 0.9787 0.8172 0.4324 0.047 Uiso 0.50 1 calc PR A 2 H25F H 1.0210 0.7528 0.3676 0.047 Uiso 0.50 1 calc PR A 2 Cl26 Cl 0.66901(5) 0.43846(4) 0.50636(2) 0.02726(13) Uani 1 1 d . . . B27A B 0.7959(15) 0.4486(12) 0.2561(7) 0.030(3) Uani 0.50 1 d PD B 1 F28A F 0.7588(9) 0.4314(8) 0.3237(4) 0.0380(12) Uani 0.50 1 d PD B 1 F29A F 0.8462(17) 0.5479(9) 0.2463(8) 0.033(2) Uani 0.50 1 d PD B 1 F30A F 0.9022(17) 0.3776(12) 0.2375(9) 0.041(3) Uani 0.50 1 d PD B 1 F31A F 0.6716(8) 0.4307(7) 0.2158(3) 0.0516(15) Uani 0.50 1 d PD B 1 B27B B 0.8015(15) 0.4364(11) 0.2447(7) 0.032(3) Uani 0.50 1 d PD B 2 F28B F 0.7230(10) 0.4329(9) 0.3054(4) 0.076(3) Uani 0.50 1 d PD B 2 F29B F 0.7072(9) 0.4224(7) 0.1892(4) 0.073(2) Uani 0.50 1 d PD B 2 F30B F 0.8674(18) 0.5331(10) 0.2384(9) 0.039(3) Uani 0.50 1 d PD B 2 F31B F 0.9063(16) 0.3597(12) 0.2471(9) 0.0322(19) Uani 0.50 1 d PD B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.02790(16) 0.02173(15) 0.02485(15) 0.00203(9) -0.00223(10) 0.00115(9) N2 0.0263(9) 0.0264(9) 0.0230(9) -0.0006(7) 0.0004(7) -0.0011(7) C3 0.0293(11) 0.0316(11) 0.0213(10) -0.0012(8) 0.0040(8) -0.0034(8) C4 0.0270(12) 0.0467(13) 0.0250(11) -0.0027(9) 0.0017(9) -0.0067(9) C5 0.0239(11) 0.0477(14) 0.0275(11) 0.0023(9) -0.0008(8) 0.0026(9) C6 0.0252(11) 0.0358(12) 0.0271(11) 0.0035(9) 0.0003(8) 0.0051(9) C7 0.0228(10) 0.0272(10) 0.0221(10) -0.0006(8) 0.0014(7) 0.0019(8) N8 0.0374(11) 0.0301(9) 0.0241(9) -0.0007(7) 0.0003(7) -0.0091(8) N9 0.0329(10) 0.0250(9) 0.0273(9) 0.0008(7) 0.0037(7) -0.0010(7) C10 0.0479(14) 0.0250(11) 0.0287(11) -0.0016(9) 0.0117(10) -0.0062(10) C11 0.0657(17) 0.0286(12) 0.0323(12) -0.0032(9) 0.0076(11) -0.0178(11) C12 0.0498(15) 0.0405(14) 0.0301(12) -0.0050(10) 0.0016(10) -0.0195(11) C13 0.0562(16) 0.0213(11) 0.0354(12) 0.0022(9) 0.0149(11) 0.0033(10) C14 0.0565(16) 0.0317(12) 0.0345(13) 0.0075(10) 0.0120(11) 0.0062(11) C15 0.0509(15) 0.0273(11) 0.0395(13) 0.0022(9) 0.0120(11) 0.0081(10) C16 0.075(2) 0.0237(12) 0.0526(17) -0.0005(11) 0.0221(15) 0.0031(12) N17 0.0240(9) 0.0229(8) 0.0247(9) 0.0017(6) -0.0017(7) 0.0037(6) N18 0.0228(9) 0.0264(9) 0.0230(8) 0.0023(7) -0.0010(7) 0.0035(7) C19 0.0244(10) 0.0310(11) 0.0224(10) -0.0011(8) 0.0035(8) -0.0002(8) C20 0.0317(11) 0.0260(10) 0.0296(11) -0.0006(8) 0.0024(9) -0.0009(8) C21 0.0324(12) 0.0232(10) 0.0290(11) 0.0007(8) 0.0024(8) 0.0040(8) C22A 0.020(5) 0.030(4) 0.032(6) -0.005(3) -0.002(3) 0.000(3) C23A 0.031(5) 0.030(6) 0.024(4) -0.001(3) -0.003(3) -0.001(3) C24A 0.022(4) 0.039(5) 0.021(5) 0.001(3) -0.006(3) -0.004(3) C25A 0.024(5) 0.044(6) 0.047(5) 0.004(4) 0.000(4) -0.011(4) C22B 0.026(5) 0.047(8) 0.021(4) 0.009(4) 0.000(3) -0.010(4) C23B 0.025(4) 0.035(7) 0.032(4) -0.005(3) -0.001(3) -0.001(4) C24B 0.014(4) 0.046(6) 0.029(5) -0.003(3) -0.003(3) 0.004(4) C25B 0.030(5) 0.047(7) 0.040(6) 0.013(5) -0.002(4) -0.003(4) Cl26 0.0262(3) 0.0296(3) 0.0259(3) 0.00438(19) 0.00039(19) 0.00516(19) B27A 0.025(5) 0.025(5) 0.041(5) -0.012(4) -0.007(4) 0.005(3) F28A 0.040(3) 0.033(2) 0.041(2) 0.0023(16) 0.0119(17) 0.0062(18) F29A 0.037(4) 0.025(3) 0.038(4) 0.004(3) -0.009(3) -0.008(3) F30A 0.035(3) 0.038(6) 0.051(6) -0.013(4) 0.007(3) 0.001(3) F31A 0.037(3) 0.046(2) 0.071(4) -0.009(3) -0.022(2) -0.0108(19) B27B 0.028(5) 0.022(5) 0.045(6) -0.008(4) 0.007(3) -0.012(4) F28B 0.073(6) 0.044(3) 0.112(7) 0.011(5) 0.066(5) 0.005(4) F29B 0.069(5) 0.042(3) 0.106(6) 0.006(4) -0.058(4) -0.015(3) F30B 0.037(4) 0.032(4) 0.047(4) 0.001(3) -0.003(3) -0.008(3) F31B 0.028(3) 0.028(4) 0.040(3) -0.006(3) -0.002(2) 0.002(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 N2 1.9425(18) . ? Cu1 N18 2.1011(17) . ? Cu1 N9 2.1134(18) . ? Cu1 Cl26 2.1978(5) . ? Cu1 F28A 2.400(9) . ? Cu1 F28B 2.453(10) . ? Cu1 Cl26 3.0465(6) 3_666 ? N2 C7 1.332(3) . ? N2 C3 1.334(3) . ? C3 C4 1.383(3) . ? C3 N8 1.399(3) . ? C4 C5 1.387(4) . ? C5 C6 1.389(3) . ? C6 C7 1.382(3) . ? C7 N17 1.399(3) . ? N8 C12 1.358(3) . ? N8 N9 1.380(3) . ? N9 C10 1.343(3) . ? C10 C11 1.416(4) . ? C10 C13 1.513(4) . ? C11 C12 1.354(4) . ? C13 C15 1.529(4) . ? C13 C14 1.534(3) . ? C13 C16 1.546(3) . ? N17 C21 1.357(3) . ? N17 N18 1.384(2) . ? N18 C19 1.338(3) . ? C19 C20 1.417(3) . ? C19 C22B 1.513(13) . ? C19 C22A 1.535(13) . ? C20 C21 1.360(3) . ? C22A C24A 1.522(13) . ? C22A C23A 1.537(14) . ? C22A C25A 1.547(14) . ? C22B C24B 1.523(14) . ? C22B C25B 1.544(13) . ? C22B C23B 1.554(13) . ? B27A F29A 1.377(13) . ? B27A F28A 1.386(14) . ? B27A F30A 1.387(13) . ? B27A F31A 1.399(12) . ? B27B F31B 1.379(14) . ? B27B F30B 1.393(12) . ? B27B F29B 1.393(13) . ? B27B F28B 1.394(13) . ? 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 N2 Cu1 N18 78.90(7) . . ? N2 Cu1 N9 78.59(7) . . ? N18 Cu1 N9 154.42(7) . . ? N2 Cu1 Cl26 157.46(6) . . ? N18 Cu1 Cl26 103.05(5) . . ? N9 Cu1 Cl26 102.40(5) . . ? N2 Cu1 F28A 96.50(16) . . ? N18 Cu1 F28A 84.8(3) . . ? N9 Cu1 F28A 85.9(2) . . ? Cl26 Cu1 F28A 106.03(15) . . ? N2 Cu1 F28B 85.5(2) . . ? N18 Cu1 F28B 85.5(3) . . ? N9 Cu1 F28B 80.8(3) . . ? Cl26 Cu1 F28B 117.0(2) . . ? F28A Cu1 F28B 11.4(3) . . ? N2 Cu1 Cl26 75.96(5) . 3_666 ? N18 Cu1 Cl26 87.84(5) . 3_666 ? N9 Cu1 Cl26 98.29(5) . 3_666 ? Cl26 Cu1 Cl26 81.652(18) . 3_666 ? F28A Cu1 Cl26 170.4(2) . 3_666 ? F28B Cu1 Cl26 161.2(2) . 3_666 ? C7 N2 C3 119.63(19) . . ? C7 N2 Cu1 119.23(14) . . ? C3 N2 Cu1 119.73(14) . . ? N2 C3 C4 122.6(2) . . ? N2 C3 N8 112.33(19) . . ? C4 C3 N8 125.1(2) . . ? C3 C4 C5 116.6(2) . . ? C4 C5 C6 121.8(2) . . ? C7 C6 C5 116.5(2) . . ? N2 C7 C6 122.8(2) . . ? N2 C7 N17 112.46(18) . . ? C6 C7 N17 124.76(19) . . ? C12 N8 N9 111.04(19) . . ? C12 N8 C3 129.8(2) . . ? N9 N8 C3 118.80(17) . . ? C10 N9 N8 105.24(18) . . ? C10 N9 Cu1 145.86(17) . . ? N8 N9 Cu1 108.89(12) . . ? N9 C10 C11 109.8(2) . . ? N9 C10 C13 123.8(2) . . ? C11 C10 C13 126.4(2) . . ? C12 C11 C10 106.5(2) . . ? C11 C12 N8 107.4(2) . . ? C10 C13 C15 111.45(19) . . ? C10 C13 C14 108.7(2) . . ? C15 C13 C14 111.4(2) . . ? C10 C13 C16 108.7(2) . . ? C15 C13 C16 108.3(2) . . ? C14 C13 C16 108.1(2) . . ? C21 N17 N18 111.30(17) . . ? C21 N17 C7 129.49(18) . . ? N18 N17 C7 118.67(16) . . ? C19 N18 N17 105.21(16) . . ? C19 N18 Cu1 146.07(14) . . ? N17 N18 Cu1 108.71(12) . . ? N18 C19 C20 109.83(18) . . ? N18 C19 C22B 121.1(6) . . ? C20 C19 C22B 129.0(6) . . ? N18 C19 C22A 126.4(7) . . ? C20 C19 C22A 123.6(7) . . ? C22B C19 C22A 7.9(12) . . ? C21 C20 C19 106.74(19) . . ? N17 C21 C20 106.91(19) . . ? C24A C22A C19 110.0(11) . . ? C24A C22A C23A 113.1(11) . . ? C19 C22A C23A 108.3(10) . . ? C24A C22A C25A 108.6(11) . . ? C19 C22A C25A 108.0(11) . . ? C23A C22A C25A 108.7(11) . . ? C19 C22B C24B 111.7(11) . . ? C19 C22B C25B 109.1(10) . . ? C24B C22B C25B 109.5(11) . . ? C19 C22B C23B 108.5(10) . . ? C24B C22B C23B 109.9(10) . . ? C25B C22B C23B 108.1(11) . . ? Cu1 Cl26 Cu1 98.348(15) . 3_666 ? F29A B27A F28A 111.5(12) . . ? F29A B27A F30A 110.0(12) . . ? F28A B27A F30A 108.8(10) . . ? F29A B27A F31A 110.3(10) . . ? F28A B27A F31A 107.8(10) . . ? F30A B27A F31A 108.3(12) . . ? B27A F28A Cu1 141.1(7) . . ? F31B B27B F30B 110.1(11) . . ? F31B B27B F29B 111.1(12) . . ? F30B B27B F29B 108.3(11) . . ? F31B B27B F28B 108.2(11) . . ? F30B B27B F28B 109.3(12) . . ? F29B B27B F28B 109.8(10) . . ? B27B F28B Cu1 164.9(9) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.950 _refine_diff_density_min -0.669 _refine_diff_density_rms 0.110 #=END data_mh9711 _database_code_CSD 175840 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Dichlorodiaquabis[2,6-bis(3-tert-butylpyrazolyl)pyridine]dicopper(II) ditetrafluoroborate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H54 Cl2 Cu2 N10 O2, 2[B F4]' _chemical_formula_sum 'C38 H54 B2 Cl2 Cu2 F8 N10 O2' _chemical_formula_weight 1054.51 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' 'O' 'O' 0.0106 0.0060 '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' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 '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 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.347(15) _cell_length_b 11.521(7) _cell_length_c 19.455(17) _cell_angle_alpha 90.00 _cell_angle_beta 96.36(9) _cell_angle_gamma 90.00 _cell_volume 2305.0(41) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Amber _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.519 _exptl_crystal_density_method ? _exptl_crystal_F_000 1084 _exptl_absorpt_coefficient_mu 1.117 _exptl_absorpt_correction_type Semi-empirical _exptl_absorpt_correction_T_min 0.974 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Rigaku AFC7-R' _diffrn_measurement_method 'omega-2theta' _diffrn_standards_number 3 _diffrn_standards_interval_count 200 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4291 _diffrn_reflns_av_R_equivalents 0.0226 _diffrn_reflns_av_sigmaI/netI 0.0405 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.65 _diffrn_reflns_theta_max 24.99 _reflns_number_total 4054 _reflns_number_gt 3468 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Rigaku control software' _computing_cell_refinement 'Rigaku control software' _computing_data_reduction 'TEXSAN (Molecular Structure Corporation, 1995)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL (Sheldrick, 1987)' _computing_publication_material 'Siemens SHELXTL (Sheldrick, 1987)' _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. The asymmetric unit contains half a dimeric molecule, lying across the crystallographic inversion centre 0.5, 0.5, 0.5. The BF4- anion was modelled over two disorder orientations: B28A-F32A, occupancy 0.75 B28B-F32B, occupancy 0.25 All B-F and F...F distances were restrained to 1.36(2) and 2.22(2)\%A, respectively. All non-H atoms with occupancy >0.5 were refined anisotropically. The H atoms for the water ligand, H27A and H27B, were located in the difference map and allowed to refine freely. All other H atoms were placed in calculated positions and refined using a riding model. ; _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^)+(0.0473P)^2^+1.9267P] 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 4054 _refine_ls_number_parameters 318 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.0484 _refine_ls_R_factor_gt 0.0386 _refine_ls_wR_factor_ref 0.1040 _refine_ls_wR_factor_gt 0.0981 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.061 _refine_ls_shift/su_max 0.001 _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 0.68070(3) 0.51275(3) 0.575409(18) 0.02310(12) Uani 1 1 d . . . N2 N 0.7890(2) 0.3950(2) 0.53693(12) 0.0244(5) Uani 1 1 d . . . C3 C 0.7991(3) 0.2894(3) 0.56496(16) 0.0263(6) Uani 1 1 d . . . C4 C 0.8584(3) 0.1985(3) 0.53429(18) 0.0345(7) Uani 1 1 d . . . H4 H 0.8671 0.1257 0.5550 0.041 Uiso 1 1 calc R . . C5 C 0.9044(3) 0.2208(3) 0.47113(18) 0.0382(8) Uani 1 1 d . . . H5 H 0.9429 0.1612 0.4484 0.046 Uiso 1 1 calc R . . C6 C 0.8941(3) 0.3296(3) 0.44143(18) 0.0357(8) Uani 1 1 d . . . H6 H 0.9257 0.3448 0.3994 0.043 Uiso 1 1 calc R . . C7 C 0.8349(3) 0.4151(3) 0.47675(16) 0.0280(7) Uani 1 1 d . . . N8 N 0.7450(2) 0.2819(2) 0.62719(13) 0.0267(5) Uani 1 1 d . . . N9 N 0.6786(2) 0.3768(2) 0.64930(13) 0.0246(5) Uani 1 1 d . . . C10 C 0.6442(3) 0.3451(3) 0.71099(15) 0.0273(6) Uani 1 1 d . . . C11 C 0.6879(3) 0.2312(3) 0.72696(17) 0.0336(7) Uani 1 1 d . . . H11 H 0.6756 0.1894 0.7666 0.040 Uiso 1 1 calc R . . C12 C 0.7506(3) 0.1945(3) 0.67386(17) 0.0340(7) Uani 1 1 d . . . H12 H 0.7903 0.1227 0.6700 0.041 Uiso 1 1 calc R . . C13 C 0.5680(3) 0.4210(3) 0.75547(16) 0.0315(7) Uani 1 1 d . . . C14 C 0.5862(4) 0.3739(3) 0.83002(18) 0.0465(9) Uani 1 1 d . . . H14A H 0.5383 0.4213 0.8589 0.056 Uiso 1 1 calc R . . H14B H 0.6768 0.3754 0.8472 0.056 Uiso 1 1 calc R . . H14C H 0.5548 0.2955 0.8304 0.056 Uiso 1 1 calc R . . C15 C 0.4236(3) 0.4140(3) 0.7278(2) 0.0454(9) Uani 1 1 d . . . H15A H 0.3739 0.4618 0.7556 0.054 Uiso 1 1 calc R . . H15B H 0.3946 0.3350 0.7297 0.054 Uiso 1 1 calc R . . H15C H 0.4118 0.4407 0.6808 0.054 Uiso 1 1 calc R . . C16 C 0.6153(3) 0.5472(3) 0.75683(16) 0.0316(7) Uani 1 1 d . . . H16A H 0.5648 0.5926 0.7855 0.038 Uiso 1 1 calc R . . H16B H 0.6054 0.5780 0.7107 0.038 Uiso 1 1 calc R . . H16C H 0.7053 0.5501 0.7752 0.038 Uiso 1 1 calc R . . N17 N 0.8170(2) 0.5299(2) 0.45447(13) 0.0272(5) Uani 1 1 d . . . N18 N 0.7499(2) 0.6051(2) 0.49264(12) 0.0249(5) Uani 1 1 d . . . C19 C 0.7535(3) 0.7080(3) 0.46080(15) 0.0275(7) Uani 1 1 d . . . C20 C 0.8223(3) 0.6962(3) 0.40222(17) 0.0371(8) Uani 1 1 d . . . H20 H 0.8383 0.7546 0.3712 0.045 Uiso 1 1 calc R . . C21 C 0.8603(3) 0.5842(3) 0.39985(16) 0.0352(7) Uani 1 1 d . . . H21 H 0.9073 0.5508 0.3669 0.042 Uiso 1 1 calc R . . C22 C 0.6899(3) 0.8174(3) 0.48404(16) 0.0293(7) Uani 1 1 d . . . C23 C 0.5449(3) 0.8147(3) 0.45537(18) 0.0389(8) Uani 1 1 d . . . H23A H 0.5028 0.8835 0.4696 0.047 Uiso 1 1 calc R . . H23B H 0.5044 0.7475 0.4729 0.047 Uiso 1 1 calc R . . H23C H 0.5372 0.8113 0.4058 0.047 Uiso 1 1 calc R . . C24 C 0.7546(4) 0.9225(3) 0.45401(19) 0.0413(8) Uani 1 1 d . . . H24A H 0.7150 0.9924 0.4685 0.050 Uiso 1 1 calc R . . H24B H 0.7438 0.9180 0.4044 0.050 Uiso 1 1 calc R . . H24C H 0.8457 0.9230 0.4703 0.050 Uiso 1 1 calc R . . C25 C 0.7059(3) 0.8283(3) 0.56304(16) 0.0343(7) Uani 1 1 d . . . H25A H 0.6648 0.8984 0.5761 0.041 Uiso 1 1 calc R . . H25B H 0.7968 0.8307 0.5797 0.041 Uiso 1 1 calc R . . H25C H 0.6663 0.7628 0.5828 0.041 Uiso 1 1 calc R . . Cl26 Cl 0.48788(7) 0.59087(7) 0.57970(4) 0.02992(18) Uani 1 1 d . . . O27 O 0.8468(2) 0.5901(2) 0.64686(12) 0.0327(5) Uani 1 1 d . . . H27A H 0.858(4) 0.647(4) 0.661(2) 0.057(15) Uiso 1 1 d . . . H27B H 0.869(4) 0.551(3) 0.682(2) 0.039(11) Uiso 1 1 d . . . B28A B 0.9779(5) 0.9168(7) 0.7015(4) 0.0302(14) Uani 0.75 1 d PD A 1 F29A F 0.9754(3) 0.7995(2) 0.68444(16) 0.0527(8) Uani 0.75 1 d PD A 1 F30A F 1.0847(4) 0.9370(4) 0.7470(3) 0.0953(18) Uani 0.75 1 d PD A 1 F31A F 0.8682(3) 0.9519(3) 0.7277(2) 0.0805(12) Uani 0.75 1 d PD A 1 F32A F 0.9830(4) 0.9806(3) 0.64279(18) 0.0711(11) Uani 0.75 1 d PD A 1 B28B B 0.9725(19) 0.8877(16) 0.7112(10) 0.049(10) Uiso 0.25 1 d PD B 2 F29B F 0.8780(12) 0.8098(10) 0.7188(6) 0.091(4) Uiso 0.25 1 d PD B 2 F30B F 1.0594(14) 0.8357(14) 0.6741(7) 0.116(5) Uiso 0.25 1 d PD B 2 F31B F 0.9210(19) 0.9784(14) 0.6745(10) 0.154(8) Uiso 0.25 1 d PD B 2 F32B F 1.0352(10) 0.9188(10) 0.7729(5) 0.046(3) Uiso 0.25 1 d PD B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0239(2) 0.01938(19) 0.0267(2) -0.00215(14) 0.00586(14) 0.00143(14) N2 0.0231(12) 0.0238(13) 0.0266(13) -0.0055(10) 0.0037(10) -0.0008(10) C3 0.0204(14) 0.0239(15) 0.0335(16) -0.0070(12) -0.0018(12) -0.0001(12) C4 0.0311(17) 0.0249(16) 0.047(2) -0.0105(14) 0.0029(14) 0.0043(13) C5 0.0332(17) 0.0337(18) 0.049(2) -0.0150(16) 0.0098(15) 0.0051(14) C6 0.0321(17) 0.0389(19) 0.0376(18) -0.0131(15) 0.0112(14) 0.0009(14) C7 0.0227(14) 0.0294(16) 0.0320(16) -0.0074(13) 0.0033(12) -0.0020(12) N8 0.0250(12) 0.0207(12) 0.0343(14) -0.0029(11) 0.0030(11) 0.0031(10) N9 0.0229(12) 0.0194(12) 0.0316(13) -0.0042(10) 0.0043(10) -0.0007(10) C10 0.0267(15) 0.0252(15) 0.0293(16) -0.0001(12) 0.0000(12) -0.0066(12) C11 0.0389(18) 0.0254(16) 0.0356(17) 0.0054(13) 0.0005(14) -0.0028(14) C12 0.0392(18) 0.0188(15) 0.0423(19) 0.0019(14) -0.0035(15) 0.0019(13) C13 0.0389(18) 0.0265(16) 0.0307(16) -0.0004(13) 0.0104(14) -0.0057(13) C14 0.070(3) 0.0355(19) 0.0375(19) 0.0038(16) 0.0228(18) -0.0067(18) C15 0.0345(19) 0.040(2) 0.064(2) -0.0099(18) 0.0177(17) -0.0064(16) C16 0.0427(19) 0.0274(16) 0.0264(16) -0.0045(13) 0.0116(14) -0.0033(14) N17 0.0282(13) 0.0290(13) 0.0250(13) -0.0061(11) 0.0058(10) 0.0001(11) N18 0.0248(12) 0.0255(13) 0.0246(12) -0.0046(10) 0.0032(10) -0.0017(10) C19 0.0280(15) 0.0319(16) 0.0212(14) 0.0007(12) -0.0042(12) -0.0045(13) C20 0.044(2) 0.0422(19) 0.0258(16) 0.0042(14) 0.0053(14) -0.0057(16) C21 0.0368(18) 0.045(2) 0.0252(16) -0.0037(14) 0.0085(13) -0.0061(15) C22 0.0341(17) 0.0244(15) 0.0279(16) 0.0014(12) -0.0032(13) -0.0027(13) C23 0.0376(19) 0.0354(18) 0.0410(19) -0.0009(15) -0.0073(15) 0.0017(15) C24 0.052(2) 0.0301(18) 0.0397(19) 0.0052(15) -0.0035(16) -0.0066(16) C25 0.0452(19) 0.0261(16) 0.0304(17) -0.0061(13) -0.0015(14) -0.0017(14) Cl26 0.0246(4) 0.0320(4) 0.0333(4) -0.0046(3) 0.0036(3) 0.0050(3) O27 0.0393(13) 0.0294(13) 0.0279(12) 0.0023(11) -0.0028(10) -0.0063(11) B28A 0.025(3) 0.026(3) 0.037(3) -0.005(3) -0.009(2) 0.005(2) F29A 0.068(2) 0.0272(14) 0.0571(18) -0.0120(13) -0.0172(16) -0.0042(14) F30A 0.068(3) 0.068(3) 0.133(4) -0.053(3) -0.060(3) 0.015(2) F31A 0.058(2) 0.084(2) 0.108(3) 0.040(2) 0.049(2) 0.0394(19) F32A 0.120(3) 0.0430(18) 0.058(2) 0.0057(15) 0.044(2) 0.0026(18) _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 N2 1.961(3) . ? Cu1 N18 2.120(3) . ? Cu1 N9 2.127(3) . ? Cu1 Cl26 2.199(3) . ? Cu1 O27 2.269(3) . ? Cu1 Cl26 3.523(3) 3_666 ? N2 C7 1.332(4) . ? N2 C3 1.333(4) . ? C3 C4 1.382(4) . ? C3 N8 1.392(4) . ? C4 C5 1.390(5) . ? C5 C6 1.379(5) . ? C6 C7 1.382(4) . ? C7 N17 1.398(4) . ? N8 C12 1.353(4) . ? N8 N9 1.385(3) . ? N9 C10 1.340(4) . ? C10 C11 1.411(4) . ? C10 C13 1.513(4) . ? C11 C12 1.348(5) . ? C13 C15 1.533(5) . ? C13 C16 1.534(4) . ? C13 C14 1.541(5) . ? N17 C21 1.352(4) . ? N17 N18 1.378(3) . ? N18 C19 1.340(4) . ? C19 C20 1.416(5) . ? C19 C22 1.514(4) . ? C20 C21 1.351(5) . ? C22 C24 1.531(4) . ? C22 C25 1.533(4) . ? C22 C23 1.542(5) . ? O27 H27A 0.72(5) . ? O27 H27B 0.83(4) . ? B28A F31A 1.357(6) . ? B28A F30A 1.357(6) . ? B28A F32A 1.364(9) . ? B28A F29A 1.391(7) . ? B28B F31B 1.343(17) . ? B28B F29B 1.347(17) . ? B28B F32B 1.349(17) . ? B28B F30B 1.354(18) . ? 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 N2 Cu1 N18 78.57(12) . . ? N2 Cu1 N9 78.31(11) . . ? N18 Cu1 N9 155.81(10) . . ? N2 Cu1 Cl26 149.02(8) . . ? N18 Cu1 Cl26 102.00(10) . . ? N9 Cu1 Cl26 101.45(9) . . ? N2 Cu1 O27 94.57(13) . . ? N18 Cu1 O27 88.36(12) . . ? N9 Cu1 O27 86.49(11) . . ? Cl26 Cu1 O27 116.40(11) . . ? N2 Cu1 Cl26 71.82(10) . 3_666 ? N18 Cu1 Cl26 72.39(9) . 3_666 ? N9 Cu1 Cl26 106.76(8) . 3_666 ? Cl26 Cu1 Cl26 78.81(9) . 3_666 ? O27 Cu1 Cl26 158.03(7) . 3_666 ? C7 N2 C3 120.0(3) . . ? C7 N2 Cu1 119.3(2) . . ? C3 N2 Cu1 119.9(2) . . ? N2 C3 C4 122.3(3) . . ? N2 C3 N8 113.1(2) . . ? C4 C3 N8 124.7(3) . . ? C3 C4 C5 116.9(3) . . ? C6 C5 C4 121.4(3) . . ? C5 C6 C7 117.2(3) . . ? N2 C7 C6 122.3(3) . . ? N2 C7 N17 112.9(3) . . ? C6 C7 N17 124.8(3) . . ? C12 N8 N9 111.4(3) . . ? C12 N8 C3 129.7(3) . . ? N9 N8 C3 118.8(2) . . ? C10 N9 N8 104.6(2) . . ? C10 N9 Cu1 146.1(2) . . ? N8 N9 Cu1 109.22(18) . . ? N9 C10 C11 109.9(3) . . ? N9 C10 C13 124.2(3) . . ? C11 C10 C13 125.9(3) . . ? C12 C11 C10 107.0(3) . . ? C11 C12 N8 107.0(3) . . ? C10 C13 C15 108.6(3) . . ? C10 C13 C16 111.9(3) . . ? C15 C13 C16 110.7(3) . . ? C10 C13 C14 108.5(3) . . ? C15 C13 C14 109.0(3) . . ? C16 C13 C14 108.2(3) . . ? C21 N17 N18 111.3(3) . . ? C21 N17 C7 129.6(3) . . ? N18 N17 C7 119.0(2) . . ? C19 N18 N17 105.4(2) . . ? C19 N18 Cu1 145.5(2) . . ? N17 N18 Cu1 109.05(19) . . ? N18 C19 C20 109.2(3) . . ? N18 C19 C22 124.3(3) . . ? C20 C19 C22 126.4(3) . . ? C21 C20 C19 107.0(3) . . ? C20 C21 N17 107.0(3) . . ? C19 C22 C24 108.8(3) . . ? C19 C22 C25 111.5(3) . . ? C24 C22 C25 108.3(3) . . ? C19 C22 C23 108.2(3) . . ? C24 C22 C23 109.1(3) . . ? C25 C22 C23 110.9(3) . . ? Cu1 Cl26 Cu1 101.19(9) . 3_666 ? H27A O27 H27B 100(4) . . ? H27A O27 Cu1 133(4) . . ? H27B O27 Cu1 114(3) . . ? F31A B28A F30A 111.0(5) . . ? F31A B28A F32A 105.4(5) . . ? F30A B28A F32A 110.5(7) . . ? F31A B28A F29A 112.6(6) . . ? F30A B28A F29A 108.4(5) . . ? F32A B28A F29A 108.9(4) . . ? F31B B28B F29B 109.1(15) . . ? F31B B28B F32B 113.0(16) . . ? F29B B28B F32B 111.3(14) . . ? F31B B28B F30B 108.0(15) . . ? F29B B28B F30B 107.3(15) . . ? F32B B28B F30B 108.0(14) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O27 H27A F29A 0.72(5) 2.15(5) 2.813(4) 153(5) . O27 H27A F29B 0.72(5) 2.18(5) 2.893(13) 171(5) . O27 H27B F30A 0.83(4) 1.92(4) 2.748(5) 170(4) 2_746 O27 H27B F32B 0.83(4) 1.97(4) 2.720(11) 150(4) 2_746 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.591 _refine_diff_density_min -0.370 _refine_diff_density_rms 0.070 #=END data_nks91 _database_code_CSD 175841 _audit_creation_method SHELXL-97 _chemical_name_systematic ; [2,6-Bis(3-tert-butylpyrazol-1-yl)pyridine]-bis-acetonitrilecopper(II) ditetrafluoroborate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[C23 H31 Cu N7] 2[B F4]' _chemical_formula_sum 'C23 H31 B2 Cu F8 N7' _chemical_formula_weight 642.71 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' 'Cu' 'Cu' 0.3201 1.2651 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.794(3) _cell_length_b 22.584(8) _cell_length_c 13.690(5) _cell_angle_alpha 90.00 _cell_angle_beta 110.09(2) _cell_angle_gamma 90.00 _cell_volume 2843.7(16) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour mauve _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.501 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1316 _exptl_absorpt_coefficient_mu 0.848 _exptl_absorpt_correction_type 'semi-empirical (psi-scans)' _exptl_absorpt_correction_T_min 0.958 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku AFC7-R' _diffrn_measurement_method 'omega/2theta scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 200 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 3% _diffrn_reflns_number 6971 _diffrn_reflns_av_R_equivalents 0.0424 _diffrn_reflns_av_sigmaI/netI 0.0970 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.86 _diffrn_reflns_theta_max 24.99 _reflns_number_total 5007 _reflns_number_gt 3133 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Rigaku control software' _computing_cell_refinement 'Rigaku control software' _computing_data_reduction 'TEXSAN (Molecular Structure Corporation, 1995)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL (Sheldrick, 1987)' _computing_publication_material 'Siemens SHELXTL (Sheldrick, 1987)' _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. The BF4- anion centred on B37 is disordered over two orientations: B37A-F41A: occupancy 0.8 B37B-F41B: occupancy 0.2 All B-F distances within this disordered anion were restrained to 1.36(2)\%A and non-bonded F...F distances within a given disorder orientation to 2.22(2)\%A. All non-H atoms except the minor anion disorder orientation were modelled anisotropically. All H atoms were placed in calculated positions and refined using a riding model. ; _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^)+(0.0487P)^2^+2.8040P] 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 5007 _refine_ls_number_parameters 399 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.1146 _refine_ls_R_factor_gt 0.0567 _refine_ls_wR_factor_ref 0.1380 _refine_ls_wR_factor_gt 0.1150 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.011 _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 0.71091(6) -0.37701(3) 0.79617(4) 0.02829(18) Uani 1 1 d . . . N2 N 0.7209(4) -0.44460(16) 0.8849(3) 0.0275(9) Uani 1 1 d . . . C3 C 0.6635(5) -0.4408(2) 0.9595(4) 0.0335(12) Uani 1 1 d . . . C4 C 0.6852(6) -0.4837(2) 1.0343(4) 0.0425(14) Uani 1 1 d . . . H4 H 0.6454 -0.4802 1.0867 0.051 Uiso 1 1 calc R . . C5 C 0.7685(6) -0.5321(2) 1.0288(4) 0.0431(14) Uani 1 1 d . . . H5 H 0.7847 -0.5620 1.0783 0.052 Uiso 1 1 calc R A . C6 C 0.8272(5) -0.5370(2) 0.9523(4) 0.0375(13) Uani 1 1 d . . . H6 H 0.8825 -0.5698 0.9480 0.045 Uiso 1 1 calc R . . C7 C 0.8011(5) -0.4914(2) 0.8816(4) 0.0322(12) Uani 1 1 d . . . N8 N 0.5856(4) -0.38891(17) 0.9550(3) 0.0334(10) Uani 1 1 d . A . N9 N 0.5749(4) -0.34892(17) 0.8772(3) 0.0279(9) Uani 1 1 d . A . C10 C 0.4857(5) -0.3068(2) 0.8896(4) 0.0335(12) Uani 1 1 d . . . C11 C 0.4397(6) -0.3212(2) 0.9729(4) 0.0430(13) Uani 1 1 d . . . H11 H 0.3761 -0.2996 0.9962 0.052 Uiso 1 1 calc R . . C12 C 0.5060(6) -0.3727(3) 1.0128(4) 0.0438(13) Uani 1 1 d . . . H12 H 0.4977 -0.3931 1.0696 0.053 Uiso 1 1 calc R A . C13 C 0.4448(5) -0.2511(2) 0.8250(4) 0.0321(12) Uani 1 1 d . . . C14 C 0.4177(5) -0.2620(2) 0.7107(4) 0.0394(13) Uani 1 1 d . . . H14A H 0.3837 -0.2261 0.6723 0.059 Uiso 1 1 calc R A . H14B H 0.3458 -0.2924 0.6855 0.059 Uiso 1 1 calc R . . H14C H 0.5066 -0.2742 0.7018 0.059 Uiso 1 1 calc R . . C15 C 0.5664(6) -0.2057(2) 0.8715(5) 0.0447(14) Uani 1 1 d . . . H15A H 0.5448 -0.1702 0.8306 0.067 Uiso 1 1 calc R A . H15B H 0.6570 -0.2218 0.8714 0.067 Uiso 1 1 calc R . . H15C H 0.5733 -0.1968 0.9416 0.067 Uiso 1 1 calc R . . C16 C 0.3054(5) -0.2249(2) 0.8359(4) 0.0417(13) Uani 1 1 d . . . H16A H 0.2278 -0.2531 0.8115 0.062 Uiso 1 1 calc R A . H16B H 0.2794 -0.1893 0.7953 0.062 Uiso 1 1 calc R . . H16C H 0.3223 -0.2159 0.9076 0.062 Uiso 1 1 calc R . . N17 N 0.8624(4) -0.48770(17) 0.8040(3) 0.0321(10) Uani 1 1 d . A . N18 N 0.8579(4) -0.43430(16) 0.7548(3) 0.0281(9) Uani 1 1 d . A . C19 C 0.9371(5) -0.4422(2) 0.6947(3) 0.0303(11) Uani 1 1 d . . . C20 C 0.9915(5) -0.5005(2) 0.7060(4) 0.0364(12) Uani 1 1 d . . . H20 H 1.0500 -0.5173 0.6723 0.044 Uiso 1 1 calc R . . C21 C 0.9418(5) -0.5270(2) 0.7751(4) 0.0395(13) Uani 1 1 d . . . H21 H 0.9599 -0.5659 0.7984 0.047 Uiso 1 1 calc R A . C22 C 0.9708(5) -0.3930(2) 0.6321(4) 0.0338(12) Uani 1 1 d . . . C23 C 0.8311(5) -0.3632(2) 0.5629(4) 0.0405(13) Uani 1 1 d . . . H23A H 0.7722 -0.3915 0.5142 0.061 Uiso 1 1 calc R A . H23B H 0.8549 -0.3311 0.5257 0.061 Uiso 1 1 calc R . . H23C H 0.7784 -0.3482 0.6052 0.061 Uiso 1 1 calc R . . C24 C 1.0711(5) -0.3488(2) 0.7072(4) 0.0390(13) Uani 1 1 d . . . H24A H 1.1623 -0.3676 0.7440 0.059 Uiso 1 1 calc R A . H24B H 1.0269 -0.3356 0.7559 0.059 Uiso 1 1 calc R . . H24C H 1.0872 -0.3155 0.6689 0.059 Uiso 1 1 calc R . . C25 C 1.0487(7) -0.4176(3) 0.5617(5) 0.0554(16) Uani 1 1 d . . . H25A H 0.9854 -0.4444 0.5122 0.083 Uiso 1 1 calc R A . H25B H 1.1348 -0.4383 0.6031 0.083 Uiso 1 1 calc R . . H25C H 1.0750 -0.3856 0.5255 0.083 Uiso 1 1 calc R . . N26 N 0.7732(4) -0.29936(17) 0.7659(3) 0.0319(10) Uani 1 1 d . . . C27 C 0.8233(5) -0.2543(2) 0.7674(4) 0.0352(12) Uani 1 1 d . . . C28 C 0.8904(7) -0.1961(2) 0.7721(6) 0.0631(19) Uani 1 1 d . . . H28A H 0.8232 -0.1660 0.7758 0.095 Uiso 1 1 calc R . . H28B H 0.9156 -0.1901 0.7109 0.095 Uiso 1 1 calc R . . H28C H 0.9766 -0.1939 0.8327 0.095 Uiso 1 1 calc R . . N29 N 0.5424(4) -0.39555(18) 0.6466(3) 0.0342(10) Uani 1 1 d . . . C30 C 0.4653(5) -0.4109(2) 0.5689(4) 0.0321(11) Uani 1 1 d . . . C31 C 0.3664(5) -0.4300(2) 0.4689(4) 0.0419(13) Uani 1 1 d . . . H31A H 0.3265 -0.4679 0.4762 0.063 Uiso 1 1 calc R . . H31B H 0.4178 -0.4332 0.4208 0.063 Uiso 1 1 calc R . . H31C H 0.2891 -0.4017 0.4434 0.063 Uiso 1 1 calc R . . B32 B 0.6058(6) -0.0363(3) 0.7820(5) 0.0352(14) Uani 1 1 d . . . F33 F 0.6156(4) 0.01692(14) 0.7349(3) 0.0630(10) Uani 1 1 d . . . F34 F 0.6449(5) -0.03006(16) 0.8841(3) 0.0817(13) Uani 1 1 d . . . F35 F 0.6951(4) -0.07739(15) 0.7587(3) 0.0715(11) Uani 1 1 d . . . F36 F 0.4692(4) -0.05702(19) 0.7411(4) 0.1057(17) Uani 1 1 d . . . B37A B 0.9958(12) -0.3122(4) 1.0231(8) 0.048(5) Uani 0.80 1 d PD A 1 F38A F 1.0743(10) -0.3357(5) 1.1186(6) 0.075(4) Uani 0.80 1 d PD A 1 F39A F 1.0691(7) -0.2694(3) 0.9957(4) 0.099(2) Uani 0.80 1 d PD A 1 F40A F 0.8687(6) -0.2892(3) 1.0276(4) 0.0871(17) Uani 0.80 1 d PD A 1 F41A F 0.9616(6) -0.35749(18) 0.9506(4) 0.0611(15) Uani 0.80 1 d PD A 1 B37B B 1.017(2) -0.3187(10) 1.0262(17) 0.021(13) Uiso 0.20 1 d PD A 2 F38B F 1.086(2) -0.3342(11) 1.1267(14) 0.017(6) Uiso 0.20 1 d PD A 2 F39B F 1.108(2) -0.3183(10) 0.9707(15) 0.088(6) Uiso 0.20 1 d PD A 2 F40B F 0.954(3) -0.2645(8) 1.0176(16) 0.077(6) Uiso 0.20 1 d PD A 2 F41B F 0.911(2) -0.3594(9) 0.9825(16) 0.062(7) Uiso 0.20 1 d PD A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0271(3) 0.0248(3) 0.0319(3) 0.0009(3) 0.0088(2) 0.0006(3) N2 0.030(2) 0.024(2) 0.025(2) 0.0018(17) 0.0049(17) 0.0013(17) C3 0.036(3) 0.031(3) 0.031(3) -0.002(2) 0.008(2) -0.001(2) C4 0.045(3) 0.045(3) 0.036(3) 0.007(3) 0.013(3) -0.001(3) C5 0.050(3) 0.032(3) 0.038(3) 0.010(3) 0.003(3) -0.003(3) C6 0.034(3) 0.033(3) 0.039(3) 0.005(2) 0.004(2) 0.004(2) C7 0.023(2) 0.030(3) 0.036(3) -0.002(2) 0.001(2) 0.000(2) N8 0.044(2) 0.031(2) 0.028(2) 0.0019(18) 0.0154(19) 0.0035(19) N9 0.030(2) 0.029(2) 0.027(2) -0.0013(18) 0.0118(17) 0.0003(18) C10 0.025(3) 0.035(3) 0.036(3) -0.007(2) 0.005(2) -0.006(2) C11 0.054(3) 0.045(3) 0.041(3) -0.005(3) 0.028(3) 0.004(3) C12 0.059(3) 0.041(3) 0.038(3) 0.005(3) 0.027(3) 0.006(3) C13 0.023(2) 0.030(3) 0.041(3) -0.001(2) 0.008(2) -0.001(2) C14 0.030(3) 0.046(3) 0.041(3) 0.010(3) 0.011(2) 0.007(2) C15 0.035(3) 0.038(3) 0.064(4) -0.006(3) 0.020(3) -0.004(2) C16 0.032(3) 0.041(3) 0.053(3) -0.009(3) 0.016(3) 0.007(2) N17 0.030(2) 0.022(2) 0.038(2) 0.0004(19) 0.0046(19) 0.0031(18) N18 0.028(2) 0.024(2) 0.031(2) -0.0025(17) 0.0073(18) -0.0014(17) C19 0.031(3) 0.030(3) 0.025(3) -0.005(2) 0.003(2) 0.001(2) C20 0.035(3) 0.039(3) 0.036(3) -0.005(2) 0.013(2) 0.008(2) C21 0.039(3) 0.030(3) 0.042(3) -0.004(2) 0.005(3) 0.006(2) C22 0.033(3) 0.035(3) 0.035(3) -0.004(2) 0.013(2) 0.004(2) C23 0.039(3) 0.042(3) 0.037(3) -0.002(2) 0.008(2) -0.005(2) C24 0.026(3) 0.034(3) 0.054(3) 0.006(3) 0.010(2) -0.004(2) C25 0.071(4) 0.055(4) 0.054(4) 0.007(3) 0.039(3) 0.017(3) N26 0.028(2) 0.023(2) 0.045(3) 0.0021(19) 0.0123(19) 0.0002(18) C27 0.032(3) 0.033(3) 0.048(3) 0.005(2) 0.022(2) 0.008(2) C28 0.069(4) 0.026(3) 0.115(6) 0.001(3) 0.058(4) -0.007(3) N29 0.032(2) 0.036(2) 0.036(2) 0.000(2) 0.014(2) -0.0049(19) C30 0.030(3) 0.033(3) 0.036(3) 0.001(2) 0.015(2) -0.002(2) C31 0.038(3) 0.046(3) 0.037(3) -0.001(3) 0.007(2) -0.005(3) B32 0.035(3) 0.032(3) 0.039(4) -0.001(3) 0.014(3) 0.005(3) F33 0.092(3) 0.0403(19) 0.073(2) 0.0126(17) 0.050(2) 0.0171(18) F34 0.135(4) 0.061(2) 0.0358(19) -0.0006(18) 0.013(2) 0.034(2) F35 0.096(3) 0.042(2) 0.103(3) 0.0073(19) 0.068(2) 0.0234(19) F36 0.043(2) 0.093(3) 0.147(4) 0.021(3) -0.011(2) -0.006(2) B37A 0.049(6) 0.028(5) 0.051(7) -0.004(4) -0.003(4) 0.012(5) F38A 0.075(5) 0.071(4) 0.056(4) -0.012(3) -0.006(3) 0.019(3) F39A 0.115(5) 0.076(4) 0.095(4) 0.005(3) 0.022(4) -0.054(4) F40A 0.063(3) 0.092(4) 0.093(4) 0.000(3) 0.010(3) 0.037(3) F41A 0.074(3) 0.039(3) 0.045(3) -0.011(2) -0.012(3) 0.008(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 N2 1.933(4) . ? Cu1 N26 1.947(4) . ? Cu1 N9 2.103(4) . ? Cu1 N18 2.151(4) . ? Cu1 N29 2.184(4) . ? Cu1 F41B 2.66(2) . ? Cu1 F41A 2.669(4) . ? N2 C3 1.327(6) . ? N2 C7 1.327(6) . ? C3 C4 1.370(7) . ? C3 N8 1.389(6) . ? C4 C5 1.383(8) . ? C5 C6 1.362(7) . ? C6 C7 1.377(7) . ? C7 N17 1.391(6) . ? N8 C12 1.340(6) . ? N8 N9 1.372(5) . ? N9 C10 1.342(6) . ? C10 C11 1.400(7) . ? C10 C13 1.510(7) . ? C11 C12 1.353(7) . ? C13 C14 1.515(7) . ? C13 C15 1.533(7) . ? C13 C16 1.541(7) . ? N17 C21 1.327(6) . ? N17 N18 1.375(5) . ? N18 C19 1.321(6) . ? C19 C20 1.409(7) . ? C19 C22 1.508(7) . ? C20 C21 1.343(7) . ? C22 C24 1.524(7) . ? C22 C25 1.525(7) . ? C22 C23 1.527(7) . ? N26 C27 1.128(6) . ? C27 C28 1.461(7) . ? N29 C30 1.127(6) . ? C30 C31 1.445(7) . ? B32 F34 1.324(7) . ? B32 F36 1.344(7) . ? B32 F33 1.384(7) . ? B32 F35 1.385(6) . ? B37A F39A 1.334(10) . ? B37A F40A 1.370(12) . ? B37A F38A 1.375(10) . ? B37A F41A 1.383(9) . ? B37B F40B 1.354(18) . ? B37B F38B 1.356(18) . ? B37B F41B 1.361(18) . ? B37B F39B 1.361(18) . ? 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 N2 Cu1 N26 153.26(16) . . ? N2 Cu1 N9 79.10(16) . . ? N26 Cu1 N9 98.16(16) . . ? N2 Cu1 N18 78.27(16) . . ? N26 Cu1 N18 101.47(16) . . ? N9 Cu1 N18 157.33(15) . . ? N2 Cu1 N29 107.25(15) . . ? N26 Cu1 N29 99.48(16) . . ? N9 Cu1 N29 98.09(15) . . ? N18 Cu1 N29 89.80(14) . . ? N2 Cu1 F41B 69.7(4) . . ? N26 Cu1 F41B 83.5(4) . . ? N9 Cu1 F41B 80.8(4) . . ? N18 Cu1 F41B 90.2(4) . . ? N29 Cu1 F41B 176.9(4) . . ? N2 Cu1 F41A 78.36(16) . . ? N26 Cu1 F41A 75.50(16) . . ? N9 Cu1 F41A 96.26(17) . . ? N18 Cu1 F41A 77.96(15) . . ? N29 Cu1 F41A 165.35(17) . . ? C3 N2 C7 119.4(4) . . ? C3 N2 Cu1 119.3(3) . . ? C7 N2 Cu1 120.7(4) . . ? N2 C3 C4 122.1(5) . . ? N2 C3 N8 113.0(4) . . ? C4 C3 N8 124.8(5) . . ? C3 C4 C5 117.5(5) . . ? C6 C5 C4 121.2(5) . . ? C5 C6 C7 117.1(5) . . ? N2 C7 C6 122.7(5) . . ? N2 C7 N17 113.3(4) . . ? C6 C7 N17 123.9(5) . . ? C12 N8 N9 112.0(4) . . ? C12 N8 C3 128.8(5) . . ? N9 N8 C3 119.0(4) . . ? C10 N9 N8 104.4(4) . . ? C10 N9 Cu1 147.0(3) . . ? N8 N9 Cu1 108.5(3) . . ? N9 C10 C11 110.1(5) . . ? N9 C10 C13 124.8(5) . . ? C11 C10 C13 125.1(5) . . ? C12 C11 C10 106.6(5) . . ? N8 C12 C11 106.9(5) . . ? C10 C13 C14 112.8(4) . . ? C10 C13 C15 107.5(4) . . ? C14 C13 C15 111.8(4) . . ? C10 C13 C16 109.2(4) . . ? C14 C13 C16 108.4(4) . . ? C15 C13 C16 106.9(4) . . ? C21 N17 N18 111.4(4) . . ? C21 N17 C7 129.7(4) . . ? N18 N17 C7 118.5(4) . . ? C19 N18 N17 105.0(4) . . ? C19 N18 Cu1 146.5(3) . . ? N17 N18 Cu1 108.1(3) . . ? N18 C19 C20 109.8(5) . . ? N18 C19 C22 123.0(4) . . ? C20 C19 C22 127.0(5) . . ? C21 C20 C19 106.2(5) . . ? N17 C21 C20 107.6(5) . . ? C19 C22 C24 108.4(4) . . ? C19 C22 C25 110.3(4) . . ? C24 C22 C25 108.5(4) . . ? C19 C22 C23 110.7(4) . . ? C24 C22 C23 111.2(4) . . ? C25 C22 C23 107.7(4) . . ? C27 N26 Cu1 167.4(4) . . ? N26 C27 C28 178.5(6) . . ? C30 N29 Cu1 171.6(4) . . ? N29 C30 C31 179.6(6) . . ? F34 B32 F36 111.3(6) . . ? F34 B32 F33 110.9(5) . . ? F36 B32 F33 109.0(5) . . ? F34 B32 F35 109.8(5) . . ? F36 B32 F35 106.8(5) . . ? F33 B32 F35 108.9(5) . . ? F39A B37A F40A 108.8(8) . . ? F39A B37A F38A 111.6(8) . . ? F40A B37A F38A 108.9(8) . . ? F39A B37A F41A 110.8(8) . . ? F40A B37A F41A 108.3(8) . . ? F38A B37A F41A 108.4(8) . . ? B37A F41A Cu1 128.3(6) . . ? F40B B37B F38B 112.1(17) . . ? F40B B37B F41B 108.7(17) . . ? F38B B37B F41B 108.2(16) . . ? F40B B37B F39B 108.1(16) . . ? F38B B37B F39B 111.7(17) . . ? F41B B37B F39B 108.0(16) . . ? B37B F41B Cu1 136.2(14) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.451 _refine_diff_density_min -0.601 _refine_diff_density_rms 0.078