# Copyright The Royal Society of Chemistry, 1998 

data_k11 
 
_audit_creation_method            SHELXL 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_formula_moiety          ? 
_chemical_formula_structural      ? 
_chemical_formula_analytical      ? 
_chemical_formula_sum             'C52 H40 B Cu F4 N4 P2' 
_chemical_formula_weight          933.17 
_chemical_melting_point           ? 
_chemical_compound_source         
'diffusion of diethylether into dichloromethane' 
 
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' 
 '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            orthorombic 
_symmetry_space_group_name_H-M    Pbca 
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x+1/2, -y, z+1/2' 
 '-x, y+1/2, -z+1/2' 
 'x+1/2, -y+1/2, -z' 
 '-x, -y, -z' 
 'x-1/2, y, -z-1/2' 
 'x, -y-1/2, z-1/2' 
 '-x-1/2, y-1/2, z' 
 
_cell_length_a                    18.849(11) 
_cell_length_b                    20.303(9) 
_cell_length_c                    23.301(9) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.00 
_cell_angle_gamma                 90.00 
_cell_volume                      8917.1(74) 
_cell_formula_units_Z             8 
_cell_measurement_temperature     173(2) 
_cell_measurement_reflns_used     25 
_cell_measurement_theta_min       9 
_cell_measurement_theta_max       19 
 
_exptl_crystal_description        rod 
_exptl_crystal_colour             red 
_exptl_crystal_size_max           0.80 
_exptl_crystal_size_mid           0.50 
_exptl_crystal_size_min           0.40 
_exptl_crystal_density_meas       'not measured' 
_exptl_crystal_density_diffrn     1.390 
_exptl_crystal_density_method     ? 
_exptl_crystal_F_000              3840 
_exptl_absorpt_coefficient_mu     0.620 
_exptl_absorpt_correction_type    none 
_exptl_absorpt_correction_T_min   ? 
_exptl_absorpt_correction_T_max   ? 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       173(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        'Enraf-Nonius CAD4' 
_diffrn_measurement_method        theta-2theta 
_diffrn_standards_number          3 
_diffrn_standards_interval_count  100 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         <2% 
_diffrn_reflns_number             30415 
_diffrn_reflns_av_R_equivalents   0.0736 
_diffrn_reflns_av_sigmaI/netI     0.0617 
_diffrn_reflns_limit_h_min        0 
_diffrn_reflns_limit_h_max        22 
_diffrn_reflns_limit_k_min        -24 
_diffrn_reflns_limit_k_max        24 
_diffrn_reflns_limit_l_min        -27 
_diffrn_reflns_limit_l_max        27 
_diffrn_reflns_theta_min          1.71 
_diffrn_reflns_theta_max          25.07 
_reflns_number_total              7884 
_reflns_number_observed           4819 
_reflns_observed_criterion        >2sigma(I) 
 
_computing_data_collection        'NONIUS CAD4/PC' 
_computing_cell_refinement        'NONIUS CAD4/PC'
_computing_data_reduction         'XCAD-4B (Harms, 1994)'      
_computing_structure_solution     'SHELXS-95 (Sheldrick, 1995)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     'XPMA (Zsolnai, 1994)'
_computing_publication_material   'SHELXL-97 (Sheldrick, 1997)'
 
_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^)+(0.0536P)^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     constr 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          7884 
_refine_ls_number_parameters      614 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0904 
_refine_ls_R_factor_obs           0.0369 
_refine_ls_wR_factor_all          0.0941 
_refine_ls_wR_factor_obs          0.0812 
_refine_ls_goodness_of_fit_all    0.959 
_refine_ls_goodness_of_fit_obs    1.085 
_refine_ls_restrained_S_all       0.959 
_refine_ls_restrained_S_obs       1.085 
_refine_ls_shift/esd_max          2.003 
_refine_ls_shift/esd_mean         0.094 
 
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 0.76036(2) 0.241003(14) 0.508704(12) 0.03551(10) Uani 1 d . . 
P1 P 0.81894(3) 0.19589(3) 0.43262(3) 0.0348(2) Uani 1 d . . 
P2 P 0.69168(3) 0.18574(3) 0.57296(3) 0.0347(2) Uani 1 d . . 
N1 N 0.87026(12) 0.23329(11) 0.61577(9) 0.0479(6) Uani 1 d . . 
N2 N 0.81329(10) 0.31110(10) 0.56122(8) 0.0375(5) Uani 1 d . . 
N3 N 0.72084(11) 0.33071(10) 0.47784(8) 0.0377(5) Uani 1 d . . 
N4 N 0.65064(12) 0.28061(11) 0.41019(10) 0.0503(6) Uani 1 d . . 
C1 C 0.9080(2) 0.2181(2) 0.66126(13) 0.0594(8) Uani 1 d . . 
H1B H 0.9208(2) 0.1726(2) 0.66575(13) 0.071 Uiso 1 d R . 
C2 C 0.9333(2) 0.2637(2) 0.70124(13) 0.0645(8) Uani 1 d . . 
H2A H 0.9598(2) 0.2496(2) 0.73420(13) 0.077 Uiso 1 d R . 
C3 C 0.9178(2) 0.3277(2) 0.69405(13) 0.0639(9) Uani 1 d . . 
H3A H 0.9351(2) 0.3605(2) 0.72024(13) 0.077 Uiso 1 d R . 
C4 C 0.87600(14) 0.34764(14) 0.64646(11) 0.0482(7) Uani 1 d . . 
C5 C 0.8554(2) 0.41211(15) 0.63506(13) 0.0614(8) Uani 1 d . . 
H5A H 0.8698(2) 0.44700(15) 0.66032(13) 0.074 Uiso 1 d R . 
C6 C 0.8149(2) 0.42506(13) 0.58830(13) 0.0566(8) Uani 1 d . . 
H6A H 0.7993(2) 0.46913(13) 0.58038(13) 0.068 Uiso 1 d R . 
C7 C 0.79461(14) 0.37328(13) 0.55193(11) 0.0423(6) Uani 1 d . . 
C8 C 0.75036(13) 0.38420(13) 0.50019(10) 0.0431(7) Uani 1 d . . 
C9 C 0.7415(2) 0.44674(14) 0.47527(14) 0.0597(8) Uani 1 d . . 
H9A H 0.7632(2) 0.48456(14) 0.49274(14) 0.072 Uiso 1 d R . 
C10 C 0.7029(2) 0.45340(15) 0.42687(14) 0.0669(9) Uani 1 d . . 
H10A H 0.6984(2) 0.49576(15) 0.40894(14) 0.080 Uiso 1 d R . 
C11 C 0.6706(2) 0.39833(14) 0.40261(12) 0.0529(8) Uani 1 d . . 
C12 C 0.6306(2) 0.3993(2) 0.35175(14) 0.0708(10) Uani 1 d . . 
H12A H 0.6244(2) 0.4398(2) 0.33098(14) 0.085 Uiso 1 d R . 
C13 C 0.6023(2) 0.3432(2) 0.33189(14) 0.0751(10) Uani 1 d . . 
H13A H 0.5746(2) 0.3433(2) 0.29729(14) 0.090 Uiso 1 d R . 
C14 C 0.6128(2) 0.2847(2) 0.36268(13) 0.0629(8) Uani 1 d . . 
H14A H 0.5920(2) 0.2450(2) 0.34797(13) 0.076 Uiso 1 d R . 
C15 C 0.68016(14) 0.33708(13) 0.42956(11) 0.0435(6) Uani 1 d . . 
C16 C 0.85367(13) 0.29780(13) 0.60847(10) 0.0408(6) Uani 1 d . . 
C111 C 0.90090(13) 0.15058(13) 0.44878(10) 0.0401(6) Uani 1 d . . 
C112 C 0.9276(2) 0.10039(14) 0.41535(13) 0.0620(8) Uani 1 d . . 
H11A H 0.9035(2) 0.08865(14) 0.38053(13) 0.074 Uiso 1 d R . 
C113 C 0.9891(2) 0.0682(2) 0.4311(2) 0.0860(12) Uani 1 d . . 
H11B H 1.0077(2) 0.0338(2) 0.4072(2) 0.103 Uiso 1 d R . 
C114 C 1.0243(2) 0.0858(2) 0.4795(2) 0.0862(12) Uani 1 d . . 
H11C H 1.0662(2) 0.0621(2) 0.4906(2) 0.103 Uiso 1 d R . 
C115 C 0.9991(2) 0.1350(2) 0.5131(2) 0.0801(11) Uani 1 d . . 
H11D H 1.0252(2) 0.1473(2) 0.5468(2) 0.096 Uiso 1 d R . 
C116 C 0.93716(15) 0.1677(2) 0.49798(12) 0.0616(9) Uani 1 d . . 
H11E H 0.91957(15) 0.2028(2) 0.52173(12) 0.074 Uiso 1 d R . 
C121 C 0.84736(14) 0.25717(12) 0.37969(10) 0.0398(6) Uani 1 d . . 
C122 C 0.8001(2) 0.27913(14) 0.33825(12) 0.0564(8) Uani 1 d . . 
H12B H 0.7538(2) 0.25954(14) 0.33565(12) 0.068 Uiso 1 d R . 
C123 C 0.8183(2) 0.3294(2) 0.30136(13) 0.0714(10) Uani 1 d . . 
H12C H 0.7846(2) 0.3442(2) 0.27326(13) 0.086 Uiso 1 d R . 
C124 C 0.8824(2) 0.3581(2) 0.30460(14) 0.0792(11) Uani 1 d . . 
H12D H 0.8945(2) 0.3930(2) 0.27859(14) 0.095 Uiso 1 d R . 
C125 C 0.9301(2) 0.3368(2) 0.3442(2) 0.0940(13) Uani 1 d . . 
H12E H 0.9760(2) 0.3571(2) 0.3463(2) 0.113 Uiso 1 d R . 
C126 C 0.9123(2) 0.2869(2) 0.38220(13) 0.0724(10) Uani 1 d . . 
H12F H 0.9463(2) 0.2717(2) 0.40990(13) 0.087 Uiso 1 d R . 
C131 C 0.76670(14) 0.13876(12) 0.38966(11) 0.0399(6) Uani 1 d . . 
C132 C 0.7864(2) 0.11928(14) 0.33463(12) 0.0543(8) Uani 1 d . . 
H13B H 0.8297(2) 0.13622(14) 0.31862(12) 0.065 Uiso 1 d R . 
C133 C 0.7452(2) 0.0761(2) 0.30392(14) 0.0706(10) Uani 1 d . . 
H13C H 0.7594(2) 0.0631(2) 0.26599(14) 0.085 Uiso 1 d R . 
C134 C 0.6841(2) 0.0515(2) 0.3267(2) 0.0763(11) Uani 1 d . . 
H13D H 0.6556(2) 0.0218(2) 0.3045(2) 0.092 Uiso 1 d R . 
C135 C 0.6633(2) 0.0697(2) 0.3808(2) 0.0742(10) Uani 1 d . . 
H13E H 0.6202(2) 0.0519(2) 0.3963(2) 0.089 Uiso 1 d R . 
C136 C 0.70532(15) 0.11329(13) 0.41229(13) 0.0542(8) Uani 1 d . . 
H13F H 0.69098(15) 0.12624(13) 0.45018(13) 0.065 Uiso 1 d R . 
C211 C 0.60920(13) 0.14748(13) 0.54849(11) 0.0416(6) Uani 1 d . . 
C212 C 0.5740(2) 0.1762(2) 0.50232(12) 0.0602(8) Uani 1 d . . 
H21A H 0.5936(2) 0.2141(2) 0.48333(12) 0.072 Uiso 1 d R . 
C213 C 0.5112(2) 0.1493(2) 0.4826(2) 0.0840(12) Uani 1 d . . 
H21B H 0.4860(2) 0.1692(2) 0.4512(2) 0.101 Uiso 1 d R . 
C214 C 0.4832(2) 0.0946(2) 0.5078(2) 0.0959(14) Uani 1 d . . 
H21C H 0.4403(2) 0.0760(2) 0.4927(2) 0.115 Uiso 1 d R . 
C215 C 0.5169(2) 0.0659(2) 0.5538(2) 0.0871(12) Uani 1 d . . 
H21D H 0.4951(2) 0.0287(2) 0.5720(2) 0.104 Uiso 1 d R . 
C216 C 0.5798(2) 0.09220(14) 0.57357(13) 0.0595(8) Uani 1 d . . 
H21E H 0.6037(2) 0.07117(14) 0.60503(13) 0.071 Uiso 1 d R . 
C221 C 0.73801(14) 0.11953(12) 0.61042(11) 0.0402(6) Uani 1 d . . 
C222 C 0.7181(2) 0.09684(13) 0.66446(12) 0.0549(8) Uani 1 d . . 
H22A H 0.6763(2) 0.11457(13) 0.68220(12) 0.066 Uiso 1 d R . 
C223 C 0.7575(2) 0.0495(2) 0.69159(15) 0.0756(11) Uani 1 d . . 
H22B H 0.7436(2) 0.0347(2) 0.72907(15) 0.091 Uiso 1 d R . 
C224 C 0.8159(2) 0.0229(2) 0.6666(2) 0.0845(12) Uani 1 d . . 
H22C H 0.8431(2) -0.0100(2) 0.6863(2) 0.101 Uiso 1 d R . 
C225 C 0.8363(2) 0.0439(2) 0.6126(2) 0.0783(11) Uani 1 d . . 
H22D H 0.8774(2) 0.0250(2) 0.5948(2) 0.094 Uiso 1 d R . 
C226 C 0.79706(15) 0.09284(13) 0.58462(13) 0.0544(8) Uani 1 d . . 
H22E H 0.81050(15) 0.10770(13) 0.54705(13) 0.065 Uiso 1 d R . 
C231 C 0.66069(13) 0.24003(12) 0.63050(10) 0.0385(6) Uani 1 d . . 
C232 C 0.7023(2) 0.25317(14) 0.67788(12) 0.0570(8) Uani 1 d . . 
H23A H 0.7473(2) 0.23155(14) 0.68201(12) 0.068 Uiso 1 d R . 
C233 C 0.6797(2) 0.2970(2) 0.71934(14) 0.0746(10) Uani 1 d . . 
H23B H 0.7085(2) 0.3043(2) 0.75272(14) 0.090 Uiso 1 d R . 
C234 C 0.6170(2) 0.3291(2) 0.71396(15) 0.0783(11) Uani 1 d . . 
H23C H 0.6023(2) 0.3597(2) 0.74304(15) 0.094 Uiso 1 d R . 
C235 C 0.5763(2) 0.3173(2) 0.6675(2) 0.0986(14) Uani 1 d . . 
H23D H 0.5320(2) 0.3402(2) 0.6632(2) 0.118 Uiso 1 d R . 
C236 C 0.5980(2) 0.2737(2) 0.62544(14) 0.0757(10) Uani 1 d . . 
H23E H 0.5684(2) 0.2651(2) 0.59279(14) 0.091 Uiso 1 d R . 
B B 0.9773(2) 0.5031(2) 0.7491(2) 0.0653(11) Uani 1 d . . 
F1 F 0.9330(6) 0.4628(4) 0.7775(3) 0.138(4) Uani 0.694(10) d P . 
F2 F 1.0168(6) 0.4696(5) 0.7131(5) 0.161(5) Uani 0.694(10) d P . 
F3 F 0.9388(4) 0.5468(4) 0.7214(2) 0.135(3) Uani 0.694(10) d P . 
F4 F 1.0142(3) 0.5368(4) 0.7877(3) 0.131(3) Uani 0.694(10) d P . 
F5 F 1.0166(15) 0.4661(17) 0.7745(10) 0.272(14) Uani 0.306(10) d P . 
F6 F 0.9943(17) 0.5623(8) 0.7643(15) 0.264(18) Uani 0.306(10) d P . 
F7 F 0.9956(12) 0.4882(13) 0.6943(8) 0.170(12) Uani 0.306(10) d P . 
F8 F 0.9116(7) 0.4887(12) 0.7545(9) 0.151(11) Uani 0.306(10) 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 
Cu 0.0402(2) 0.0317(2) 0.0347(2) 0.00030(13) -0.00034(14) 0.00061(13) 
P1 0.0363(4) 0.0349(3) 0.0332(3) -0.0022(3) -0.0014(3) 0.0007(3) 
P2 0.0342(4) 0.0360(3) 0.0340(3) 0.0014(3) -0.0017(3) -0.0002(3) 
N1 0.0531(15) 0.0454(14) 0.0451(13) 0.0008(11) -0.0069(11) 0.0002(11) 
N2 0.0409(12) 0.0352(12) 0.0364(12) -0.0028(9) 0.0016(10) -0.0030(10) 
N3 0.0393(13) 0.0365(12) 0.0375(12) 0.0043(9) 0.0017(9) 0.0039(9) 
N4 0.0532(15) 0.0523(14) 0.0454(13) 0.0024(11) -0.0086(12) 0.0020(12) 
C1 0.063(2) 0.061(2) 0.054(2) 0.007(2) -0.011(2) 0.003(2) 
C2 0.069(2) 0.077(2) 0.048(2) 0.003(2) -0.016(2) -0.003(2) 
C3 0.069(2) 0.074(2) 0.048(2) -0.012(2) -0.011(2) -0.009(2) 
C4 0.048(2) 0.054(2) 0.043(2) -0.0114(13) 0.0026(14) -0.0068(14) 
C5 0.072(2) 0.052(2) 0.060(2) -0.022(2) -0.008(2) -0.006(2) 
C6 0.069(2) 0.035(2) 0.066(2) -0.0089(14) -0.001(2) 0.0027(14) 
C7 0.043(2) 0.039(2) 0.045(2) -0.0034(12) 0.0034(13) -0.0040(12) 
C8 0.047(2) 0.0349(14) 0.048(2) 0.0010(11) 0.0059(13) 0.0022(12) 
C9 0.072(2) 0.036(2) 0.071(2) 0.0055(14) -0.005(2) -0.0036(15) 
C10 0.077(2) 0.042(2) 0.081(2) 0.025(2) -0.003(2) 0.005(2) 
C11 0.048(2) 0.057(2) 0.054(2) 0.0178(15) 0.0009(14) 0.0083(14) 
C12 0.065(2) 0.076(2) 0.072(2) 0.031(2) -0.010(2) 0.000(2) 
C13 0.068(2) 0.103(3) 0.055(2) 0.019(2) -0.020(2) 0.007(2) 
C14 0.057(2) 0.073(2) 0.059(2) 0.001(2) -0.013(2) -0.001(2) 
C15 0.041(2) 0.046(2) 0.044(2) 0.0088(13) 0.0042(13) 0.0088(13) 
C16 0.041(2) 0.045(2) 0.0356(14) -0.0032(12) 0.0048(12) -0.0031(13) 
C111 0.0343(14) 0.045(2) 0.0408(15) 0.0035(12) 0.0025(12) -0.0002(12) 
C112 0.058(2) 0.063(2) 0.066(2) -0.014(2) -0.008(2) 0.019(2) 
C113 0.066(2) 0.085(3) 0.107(3) -0.026(2) -0.012(2) 0.035(2) 
C114 0.056(2) 0.099(3) 0.104(3) 0.002(2) -0.014(2) 0.028(2) 
C115 0.052(2) 0.122(3) 0.067(2) -0.009(2) -0.017(2) 0.019(2) 
C116 0.047(2) 0.080(2) 0.058(2) -0.018(2) -0.009(2) 0.014(2) 
C121 0.046(2) 0.0388(14) 0.0345(13) -0.0026(11) 0.0012(12) -0.0025(13) 
C122 0.056(2) 0.064(2) 0.049(2) 0.0128(15) 0.004(2) 0.001(2) 
C123 0.081(3) 0.074(2) 0.059(2) 0.023(2) 0.002(2) 0.010(2) 
C124 0.124(4) 0.059(2) 0.055(2) 0.010(2) 0.007(2) -0.016(2) 
C125 0.101(3) 0.100(3) 0.081(3) 0.022(2) -0.011(2) -0.061(2) 
C126 0.074(2) 0.084(2) 0.059(2) 0.020(2) -0.022(2) -0.032(2) 
C131 0.043(2) 0.0331(14) 0.0441(15) -0.0027(11) -0.0054(13) 0.0029(12) 
C132 0.067(2) 0.052(2) 0.044(2) -0.0082(14) -0.0056(15) -0.0025(15) 
C133 0.101(3) 0.057(2) 0.054(2) -0.019(2) -0.017(2) -0.003(2) 
C134 0.088(3) 0.052(2) 0.089(3) -0.021(2) -0.032(2) -0.008(2) 
C135 0.050(2) 0.060(2) 0.113(3) -0.015(2) -0.004(2) -0.013(2) 
C136 0.048(2) 0.048(2) 0.066(2) -0.0167(15) 0.003(2) -0.0029(14) 
C211 0.037(2) 0.046(2) 0.0424(15) -0.0120(12) 0.0001(12) -0.0006(13) 
C212 0.048(2) 0.079(2) 0.054(2) 0.000(2) -0.0099(15) 0.001(2) 
C213 0.052(2) 0.117(3) 0.083(3) -0.019(2) -0.026(2) 0.008(2) 
C214 0.049(2) 0.105(3) 0.134(4) -0.047(3) -0.024(2) -0.014(2) 
C215 0.057(2) 0.072(3) 0.132(4) -0.017(2) -0.009(2) -0.023(2) 
C216 0.049(2) 0.050(2) 0.079(2) -0.004(2) -0.005(2) -0.0104(15) 
C221 0.042(2) 0.0332(14) 0.0449(15) 0.0027(11) -0.0079(13) -0.0042(12) 
C222 0.075(2) 0.043(2) 0.047(2) 0.0085(14) -0.003(2) -0.0037(15) 
C223 0.113(3) 0.052(2) 0.062(2) 0.020(2) -0.023(2) -0.002(2) 
C224 0.099(3) 0.050(2) 0.105(3) 0.021(2) -0.042(3) 0.007(2) 
C225 0.054(2) 0.054(2) 0.126(3) 0.009(2) -0.012(2) 0.015(2) 
C226 0.048(2) 0.043(2) 0.072(2) 0.0128(15) 0.000(2) 0.0024(14) 
C231 0.0409(15) 0.0385(14) 0.0361(13) 0.0010(11) 0.0009(11) -0.0023(12) 
C232 0.057(2) 0.062(2) 0.052(2) -0.0106(15) -0.0067(15) 0.009(2) 
C233 0.089(3) 0.083(2) 0.052(2) -0.023(2) -0.013(2) 0.009(2) 
C234 0.092(3) 0.078(3) 0.064(2) -0.028(2) 0.005(2) 0.018(2) 
C235 0.084(3) 0.113(3) 0.100(3) -0.048(3) -0.018(2) 0.054(2) 
C236 0.069(2) 0.091(3) 0.067(2) -0.028(2) -0.024(2) 0.032(2) 
B 0.058(3) 0.062(3) 0.076(3) -0.005(2) 0.004(3) 0.006(2) 
F1 0.197(10) 0.101(4) 0.115(5) -0.008(3) 0.069(5) -0.074(5) 
F2 0.118(6) 0.133(5) 0.232(13) -0.058(7) 0.094(8) 0.019(4) 
F3 0.151(6) 0.149(5) 0.105(4) 0.018(3) -0.030(4) 0.051(4) 
F4 0.089(3) 0.156(7) 0.147(4) -0.032(4) -0.052(3) -0.033(3) 
F5 0.288(25) 0.317(32) 0.210(19) 0.006(21) -0.116(19) 0.167(22) 
F6 0.290(27) 0.085(10) 0.417(35) -0.108(15) 0.304(27) -0.086(13) 
F7 0.159(19) 0.279(29) 0.071(8) -0.045(11) 0.062(9) -0.104(17) 
F8 0.043(5) 0.258(24) 0.153(15) -0.156(16) 0.048(8) -0.052(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 N3 2.095(2) . ? 
Cu N2 2.126(2) . ? 
Cu P2 2.2753(9) . ? 
Cu P1 2.2806(9) . ? 
P1 C131 1.821(3) . ? 
P1 C121 1.832(3) . ? 
P1 C111 1.837(3) . ? 
P2 C221 1.825(3) . ? 
P2 C211 1.829(3) . ? 
P2 C231 1.831(3) . ? 
N1 C1 1.313(3) . ? 
N1 C16 1.357(3) . ? 
N2 C7 1.328(3) . ? 
N2 C16 1.366(3) . ? 
N3 C8 1.327(3) . ? 
N3 C15 1.368(3) . ? 
N4 C14 1.319(3) . ? 
N4 C15 1.352(3) . ? 
C1 C2 1.397(4) . ? 
C2 C3 1.343(4) . ? 
C3 C4 1.419(4) . ? 
C4 C5 1.391(4) . ? 
C4 C16 1.409(3) . ? 
C5 C6 1.356(4) . ? 
C6 C7 1.403(4) . ? 
C7 C8 1.483(3) . ? 
C8 C9 1.406(4) . ? 
C9 C10 1.349(4) . ? 
C10 C11 1.393(4) . ? 
C11 C15 1.405(4) . ? 
C11 C12 1.405(4) . ? 
C12 C13 1.340(4) . ? 
C13 C14 1.403(4) . ? 
C111 C112 1.378(4) . ? 
C111 C116 1.379(4) . ? 
C112 C113 1.380(4) . ? 
C113 C114 1.358(5) . ? 
C114 C115 1.355(5) . ? 
C115 C116 1.389(4) . ? 
C121 C126 1.366(4) . ? 
C121 C122 1.388(4) . ? 
C122 C123 1.379(4) . ? 
C123 C124 1.343(5) . ? 
C124 C125 1.360(5) . ? 
C125 C126 1.386(4) . ? 
C131 C136 1.373(4) . ? 
C131 C132 1.392(4) . ? 
C132 C133 1.373(4) . ? 
C133 C134 1.362(5) . ? 
C134 C135 1.371(5) . ? 
C135 C136 1.396(4) . ? 
C211 C216 1.381(4) . ? 
C211 C212 1.392(4) . ? 
C212 C213 1.384(4) . ? 
C213 C214 1.361(5) . ? 
C214 C215 1.374(5) . ? 
C215 C216 1.380(4) . ? 
C221 C226 1.376(4) . ? 
C221 C222 1.393(4) . ? 
C222 C223 1.370(4) . ? 
C223 C224 1.358(5) . ? 
C224 C225 1.382(5) . ? 
C225 C226 1.399(4) . ? 
C231 C236 1.370(4) . ? 
C231 C232 1.380(4) . ? 
C232 C233 1.381(4) . ? 
C233 C234 1.356(4) . ? 
C234 C235 1.348(5) . ? 
C235 C236 1.384(4) . ? 
B F5 1.21(2) . ? 
B F2 1.312(9) . ? 
B F8 1.277(12) . ? 
B F3 1.316(6) . ? 
B F6 1.295(15) . ? 
B F1 1.342(7) . ? 
B F4 1.328(7) . ? 
B F7 1.36(2) . ? 
F1 F8 0.85(3) . ? 
F1 F5 1.58(3) . ? 
F2 F7 0.70(3) . ? 
F2 F5 1.43(2) . ? 
F3 F6 1.48(4) . ? 
F3 F8 1.50(2) . ? 
F3 F7 1.72(2) . ? 
F4 F5 1.47(3) . ? 
F4 F6 0.84(4) . ? 
 
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 Cu N2 77.43(8) . . ? 
N3 Cu P2 116.89(6) . . ? 
N2 Cu P2 102.61(6) . . ? 
N3 Cu P1 104.74(6) . . ? 
N2 Cu P1 119.29(6) . . ? 
P2 Cu P1 126.08(4) . . ? 
C131 P1 C121 102.74(12) . . ? 
C131 P1 C111 104.38(12) . . ? 
C121 P1 C111 103.43(12) . . ? 
C131 P1 Cu 114.91(9) . . ? 
C121 P1 Cu 113.09(9) . . ? 
C111 P1 Cu 116.68(9) . . ? 
C221 P2 C211 104.07(12) . . ? 
C221 P2 C231 104.23(12) . . ? 
C211 P2 C231 102.28(12) . . ? 
C221 P2 Cu 113.93(9) . . ? 
C211 P2 Cu 119.20(9) . . ? 
C231 P2 Cu 111.49(9) . . ? 
C1 N1 C16 116.9(2) . . ? 
C7 N2 C16 117.8(2) . . ? 
C7 N2 Cu 114.7(2) . . ? 
C16 N2 Cu 126.4(2) . . ? 
C8 N3 C15 118.7(2) . . ? 
C8 N3 Cu 115.3(2) . . ? 
C15 N3 Cu 124.3(2) . . ? 
C14 N4 C15 116.7(2) . . ? 
N1 C1 C2 124.6(3) . . ? 
C3 C2 C1 119.0(3) . . ? 
C2 C3 C4 119.6(3) . . ? 
C5 C4 C16 118.2(3) . . ? 
C5 C4 C3 124.9(3) . . ? 
C16 C4 C3 116.9(3) . . ? 
C6 C5 C4 119.5(3) . . ? 
C5 C6 C7 119.6(3) . . ? 
N2 C7 C6 122.8(3) . . ? 
N2 C7 C8 115.1(2) . . ? 
C6 C7 C8 122.2(2) . . ? 
N3 C8 C9 121.8(2) . . ? 
N3 C8 C7 115.6(2) . . ? 
C9 C8 C7 122.5(2) . . ? 
C10 C9 C8 120.0(3) . . ? 
C9 C10 C11 119.7(3) . . ? 
C10 C11 C15 118.2(3) . . ? 
C10 C11 C12 124.4(3) . . ? 
C15 C11 C12 117.3(3) . . ? 
C13 C12 C11 119.5(3) . . ? 
C12 C13 C14 119.1(3) . . ? 
N4 C14 C13 124.0(3) . . ? 
N4 C15 N3 115.2(2) . . ? 
N4 C15 C11 123.3(3) . . ? 
N3 C15 C11 121.6(3) . . ? 
N1 C16 N2 114.9(2) . . ? 
N1 C16 C4 123.1(2) . . ? 
N2 C16 C4 122.1(2) . . ? 
C112 C111 C116 118.4(3) . . ? 
C112 C111 P1 124.2(2) . . ? 
C116 C111 P1 117.4(2) . . ? 
C111 C112 C113 120.5(3) . . ? 
C114 C113 C112 120.4(3) . . ? 
C115 C114 C113 120.2(3) . . ? 
C114 C115 C116 120.1(3) . . ? 
C111 C116 C115 120.4(3) . . ? 
C126 C121 C122 117.6(3) . . ? 
C126 C121 P1 122.2(2) . . ? 
C122 C121 P1 119.9(2) . . ? 
C123 C122 C121 120.8(3) . . ? 
C124 C123 C122 120.7(3) . . ? 
C123 C124 C125 119.6(3) . . ? 
C124 C125 C126 120.4(3) . . ? 
C121 C126 C125 120.8(3) . . ? 
C136 C131 C132 118.2(3) . . ? 
C136 C131 P1 119.0(2) . . ? 
C132 C131 P1 122.9(2) . . ? 
C133 C132 C131 120.7(3) . . ? 
C134 C133 C132 120.6(3) . . ? 
C133 C134 C135 120.1(3) . . ? 
C134 C135 C136 119.5(3) . . ? 
C131 C136 C135 121.0(3) . . ? 
C216 C211 C212 118.5(3) . . ? 
C216 C211 P2 123.6(2) . . ? 
C212 C211 P2 117.9(2) . . ? 
C213 C212 C211 119.9(3) . . ? 
C214 C213 C212 120.7(4) . . ? 
C213 C214 C215 120.2(3) . . ? 
C214 C215 C216 119.5(4) . . ? 
C215 C216 C211 121.1(3) . . ? 
C226 C221 C222 118.9(3) . . ? 
C226 C221 P2 117.9(2) . . ? 
C222 C221 P2 123.2(2) . . ? 
C223 C222 C221 120.2(3) . . ? 
C224 C223 C222 121.4(3) . . ? 
C223 C224 C225 119.5(3) . . ? 
C224 C225 C226 119.8(3) . . ? 
C221 C226 C225 120.2(3) . . ? 
C236 C231 C232 117.6(3) . . ? 
C236 C231 P2 120.8(2) . . ? 
C232 C231 P2 121.4(2) . . ? 
C233 C232 C231 120.6(3) . . ? 
C234 C233 C232 121.0(3) . . ? 
C235 C234 C233 119.0(3) . . ? 
C234 C235 C236 120.9(3) . . ? 
C231 C236 C235 120.9(3) . . ? 
F5 B F2 69.1(11) . . ? 
F5 B F8 113.8(15) . . ? 
F2 B F8 119.7(9) . . ? 
F5 B F3 175.3(18) . . ? 
F2 B F3 110.5(8) . . ? 
F8 B F3 70.6(12) . . ? 
F5 B F6 106.8(17) . . ? 
F2 B F6 121.1(8) . . ? 
F8 B F6 115.1(12) . . ? 
F3 B F6 69.1(18) . . ? 
F5 B F1 76.2(16) . . ? 
F2 B F1 110.6(7) . . ? 
F8 B F1 37.9(11) . . ? 
F3 B F1 108.1(6) . . ? 
F6 B F1 125.8(9) . . ? 
F5 B F4 70.5(15) . . ? 
F2 B F4 113.7(7) . . ? 
F8 B F4 124.0(7) . . ? 
F3 B F4 105.9(5) . . ? 
F6 B F4 37.4(19) . . ? 
F1 B F4 107.8(6) . . ? 
F5 B F7 99.6(14) . . ? 
F2 B F7 30.6(13) . . ? 
F8 B F7 106.8(13) . . ? 
F3 B F7 80.1(12) . . ? 
F6 B F7 113.7(15) . . ? 
F1 B F7 119.1(11) . . ? 
F4 B F7 128.2(11) . . ? 
F8 F1 B 66.9(10) . . ? 
F8 F1 F5 114.7(14) . . ? 
B F1 F5 48.1(9) . . ? 
F7 F2 B 78.3(18) . . ? 
F7 F2 F5 130.3(21) . . ? 
B F2 F5 52.1(8) . . ? 
F6 F3 B 54.8(9) . . ? 
F6 F3 F8 93.5(9) . . ? 
B F3 F8 53.5(7) . . ? 
F6 F3 F7 87.5(10) . . ? 
B F3 F7 51.0(8) . . ? 
F8 F3 F7 81.8(9) . . ? 
F5 F4 B 51.0(6) . . ? 
F5 F4 F6 118.8(18) . . ? 
B F4 F6 69.2(17) . . ? 
F4 F5 B 58.5(12) . . ? 
F4 F5 F2 99.3(18) . . ? 
B F5 F2 58.8(8) . . ? 
F4 F5 F1 90.2(12) . . ? 
B F5 F1 55.7(9) . . ? 
F2 F5 F1 92.8(11) . . ? 
F3 F6 B 56.1(12) . . ? 
F3 F6 F4 128.4(16) . . ? 
B F6 F4 73.4(12) . . ? 
F2 F7 B 71.2(19) . . ? 
F2 F7 F3 119.8(23) . . ? 
B F7 F3 48.9(7) . . ? 
F1 F8 B 75.2(13) . . ? 
F1 F8 F3 130.4(15) . . ? 
B F8 F3 55.9(7) . . ? 
 
_refine_diff_density_max    0.225 
_refine_diff_density_min   -0.560 
_refine_diff_density_rms    0.058