# Copyright The Royal Society of Chemistry, 1999
# CCDC Number: 440/096

data_/tintin3/people/zoe/liz/j
#=================================================================
# SUBMISSION DETAILS
_publ_contact_author
;
	Dr. Michael Ward
	School of Chemistry
	University of Bristol
	Cantock's Close
	BS8 1TS Bristol
	UK
;
_publ_contact_author_phone        '0117 9287655'
_publ_contact_author_fax          '0117 9290509'
_publ_contact_author_email        mike.ward@bristol.ac.uk

_publ_contact_letter
;
This CIF file contains details of the three crystal structures in the paper
'Copper(II) complexes of new potentially hexadentate N3S3 or N6-donor podand
ligands based on the tris(pyrazolyl)borate or tris(pyrazolyl)methane core'
by E. R. Humphrey, K. L. V. Mann, Z. R. Reeves, A. Behrendt, J. C. Jeffery,
J. A. McCleverty and M. D. Ward
submitted for publication to Dalton Transactions.
;
#=================================================================

_audit_creation_method            SHELXL
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_formula_moiety          ?
_chemical_formula_structural      ?
_chemical_formula_analytical      ?
_chemical_formula_sum             'C30 H30 B Cu F6 N6 O P S3'
_chemical_formula_weight          806.10
_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'
 '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'
 'S'  'S'   0.1246   0.1234
 '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'
 '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'
 'O'  'O'   0.0106   0.0060
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting            Cubic
_symmetry_space_group_name_H-M    Pa-3

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'
 'z, x, y'
 'z+1/2, -x+1/2, -y'
 '-z+1/2, -x, y+1/2'
 '-z, x+1/2, -y+1/2'
 'y, z, x'
 '-y, z+1/2, -x+1/2'
 'y+1/2, -z+1/2, -x'
 '-y+1/2, -z, x+1/2'
 '-x, -y, -z'
 'x-1/2, y, -z-1/2'
 'x, -y-1/2, z-1/2'
 '-x-1/2, y-1/2, z'
 '-z, -x, -y'
 '-z-1/2, x-1/2, y'
 'z-1/2, x, -y-1/2'
 'z, -x-1/2, y-1/2'
 '-y, -z, -x'
 'y, -z-1/2, x-1/2'
 '-y-1/2, z-1/2, x'
 'y-1/2, z, -x-1/2'

_cell_length_a                    27.283(3)
_cell_length_b                    27.283(4)
_cell_length_c                    27.283(3)
_cell_angle_alpha                 90.000(10)
_cell_angle_beta                  90.000(7)
_cell_angle_gamma                 90.000(8)
_cell_volume                      20308.4(41)
_cell_formula_units_Z             24
_cell_measurement_temperature     173(2)
_cell_measurement_reflns_used     ?
_cell_measurement_theta_min       ?
_cell_measurement_theta_max       ?

_exptl_crystal_description        block
_exptl_crystal_colour             green
_exptl_crystal_size_max           0.4
_exptl_crystal_size_mid           0.36
_exptl_crystal_size_min           0.14
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.582
_exptl_crystal_density_method     ?
_exptl_crystal_F_000              9864
_exptl_absorpt_coefficient_mu     0.947
_exptl_absorpt_correction_type
'Empirical, pseudo-azimuthal scan (SADABS)'
_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        'Siemens SMART Area Detector'
_diffrn_measurement_method        
'\w rotation with narrow frames (0.3 degrees)'
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             81102
_diffrn_reflns_av_R_equivalents   0.1297
_diffrn_reflns_av_sigmaI/netI     0.0408
_diffrn_reflns_limit_h_min        -35
_diffrn_reflns_limit_h_max        33
_diffrn_reflns_limit_k_min        -33
_diffrn_reflns_limit_k_max        35
_diffrn_reflns_limit_l_min        -35
_diffrn_reflns_limit_l_max        25
_diffrn_reflns_theta_min          1.49
_diffrn_reflns_theta_max          22.48
_reflns_number_total              4431
_reflns_number_observed           3522
_reflns_observed_criterion        >2sigma(I)

_computing_data_collection        ?
_computing_cell_refinement        ?
_computing_data_reduction         ?
_computing_structure_solution     'SHELXS-86 (Sheldrick, 1990)'
_computing_structure_refinement   'SHELXL-93 (Sheldrick, 1993)'
_computing_molecular_graphics     ?
_computing_publication_material   ?

_refine_special_details
;
 Refinement on F^2^ for ALL reflections except for 4 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^)+(0.0369P)^2^+86.3345P] 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_number_reflns          4427
_refine_ls_number_parameters      472
_refine_ls_number_restraints      15
_refine_ls_R_factor_all           0.0833
_refine_ls_R_factor_obs           0.0601
_refine_ls_wR_factor_all          0.1279
_refine_ls_wR_factor_obs          0.1167
_refine_ls_goodness_of_fit_all    1.102
_refine_ls_goodness_of_fit_obs    1.146
_refine_ls_restrained_S_all       1.103
_refine_ls_restrained_S_obs       1.144
_refine_ls_shift/esd_max          0.045
_refine_ls_shift/esd_mean         0.001

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 0.86054(2) 0.98637(3) 0.22456(3) 0.0287(2) Uani 1 d . .
S27 S 0.85313(6) 0.90328(5) 0.23954(6) 0.0334(4) Uani 1 d . .
S47 S 0.84710(6) 1.00788(6) 0.33353(6) 0.0427(5) Uani 1 d . .
S67 S 0.78240(5) 0.99174(5) 0.18682(6) 0.0310(4) Uani 1 d . .
N11 N 0.9605(2) 1.0175(2) 0.2213(2) 0.0295(12) Uani 1 d . .
N12 N 0.9306(2) 0.9830(2) 0.2414(2) 0.0306(12) Uani 1 d . .
N31 N 0.8993(2) 1.0853(2) 0.2156(2) 0.0292(12) Uani 1 d . .
N32 N 0.8631(2) 1.0600(2) 0.2390(2) 0.0299(12) Uani 1 d . .
N51 N 0.9161(2) 1.0335(2) 0.1418(2) 0.0270(11) Uani 1 d . .
N52 N 0.8787(2) 1.0014(2) 0.1497(2) 0.0300(12) Uani 1 d . .
C13 C 0.9576(2) 0.9550(2) 0.2713(2) 0.0290(14) Uani 1 d . .
C14 C 1.0056(2) 0.9725(2) 0.2704(2) 0.038(2) Uani 1 d . .
H16A H 1.0327(2) 0.9598(2) 0.2883(2) 0.046 Uiso 1 calc R .
C15 C 1.0062(2) 1.0113(2) 0.2390(2) 0.037(2) Uani 1 d . .
H19A H 1.0340(2) 1.0307(2) 0.2309(2) 0.044 Uiso 1 calc R .
C21 C 0.9368(2) 0.9137(2) 0.2999(2) 0.035(2) Uani 1 d . .
C22 C 0.8931(2) 0.8890(2) 0.2895(2) 0.036(2) Uani 1 d . .
C23 C 0.8782(2) 0.8492(2) 0.3175(2) 0.043(2) Uani 1 d . .
H12A H 0.8490(2) 0.8321(2) 0.3094(2) 0.051 Uiso 1 calc R .
C24 C 0.9058(3) 0.8343(3) 0.3573(3) 0.062(2) Uani 1 d . .
H4A H 0.8953(3) 0.8075(3) 0.3769(3) 0.074 Uiso 1 calc R .
C25 C 0.9484(3) 0.8584(3) 0.3683(3) 0.068(2) Uani 1 d . .
H1A H 0.9677(3) 0.8480(3) 0.3953(3) 0.082 Uiso 1 calc R .
C26 C 0.9633(3) 0.8978(3) 0.3402(3) 0.054(2) Uani 1 d . .
H2A H 0.9927(3) 0.9144(3) 0.3487(3) 0.065 Uiso 1 calc R .
C28 C 0.8860(3) 0.8760(2) 0.1887(2) 0.048(2) Uani 1 d . .
H6A H 0.8676(3) 0.8814(2) 0.1583(2) 0.072 Uiso 1 calc R .
H6B H 0.8898(3) 0.8408(2) 0.1943(2) 0.072 Uiso 1 calc R .
H6C H 0.9184(3) 0.8912(2) 0.1859(2) 0.072 Uiso 1 calc R .
C33 C 0.8335(2) 1.0934(2) 0.2602(2) 0.0303(14) Uani 1 d . .
C34 C 0.8500(2) 1.1402(2) 0.2497(2) 0.036(2) Uani 1 d . .
H23A H 0.8356(2) 1.1704(2) 0.2596(2) 0.044 Uiso 1 calc R .
C35 C 0.8916(2) 1.1339(2) 0.2219(2) 0.034(2) Uani 1 d . .
H13A H 0.9116(2) 1.1595(2) 0.2093(2) 0.041 Uiso 1 calc R .
C41 C 0.7904(2) 1.0783(2) 0.2894(2) 0.033(2) Uani 1 d . .
C42 C 0.7911(2) 1.0398(2) 0.3238(2) 0.035(2) Uani 1 d . .
C43 C 0.7489(2) 1.0294(2) 0.3496(2) 0.040(2) Uani 1 d . .
H27A H 0.7492(2) 1.0035(2) 0.3729(2) 0.048 Uiso 1 calc R .
C44 C 0.7067(3) 1.0553(3) 0.3427(3) 0.048(2) Uani 1 d . .
H11A H 0.6782(3) 1.0471(3) 0.3609(3) 0.058 Uiso 1 calc R .
C45 C 0.7052(3) 1.0932(3) 0.3095(3) 0.051(2) Uani 1 d . .
H8A H 0.6759(3) 1.1114(3) 0.3050(3) 0.062 Uiso 1 calc R .
C46 C 0.7469(2) 1.1046(2) 0.2829(2) 0.043(2) Uani 1 d . .
H10A H 0.7459(2) 1.1307(2) 0.2598(2) 0.052 Uiso 1 calc R .
C48 C 0.8340(3) 0.9684(3) 0.3852(3) 0.059(2) Uani 1 d . .
H3A H 0.8632(3) 0.9491(3) 0.3933(3) 0.088 Uiso 1 calc R .
H3B H 0.8070(3) 0.9462(3) 0.3768(3) 0.088 Uiso 1 calc R .
H3C H 0.8246(3) 0.9884(3) 0.4135(3) 0.088 Uiso 1 calc R .
C53 C 0.8620(2) 0.9872(2) 0.1056(2) 0.0258(13) Uani 1 d . .
C54 C 0.8891(2) 1.0105(2) 0.0689(2) 0.0288(14) Uani 1 d . .
H29A H 0.8852(2) 1.0070(2) 0.0345(2) 0.035 Uiso 1 calc R .
C55 C 0.9223(2) 1.0393(2) 0.0929(2) 0.0281(14) Uani 1 d . .
H17A H 0.9459(2) 1.0600(2) 0.0778(2) 0.034 Uiso 1 calc R .
C61 C 0.8229(2) 0.9504(2) 0.1031(2) 0.0275(14) Uani 1 d . .
C62 C 0.7865(2) 0.9456(2) 0.1400(2) 0.0304(14) Uani 1 d . .
C63 C 0.7535(2) 0.9071(2) 0.1382(2) 0.036(2) Uani 1 d . .
H20A H 0.7302(2) 0.9031(2) 0.1638(2) 0.043 Uiso 1 calc R .
C64 C 0.7544(2) 0.8744(2) 0.0994(2) 0.043(2) Uani 1 d . .
H9A H 0.7317(2) 0.8481(2) 0.0984(2) 0.052 Uiso 1 calc R .
C65 C 0.7881(2) 0.8800(2) 0.0624(2) 0.038(2) Uani 1 d . .
H26A H 0.7878(2) 0.8583(2) 0.0352(2) 0.046 Uiso 1 calc R .
C66 C 0.8226(2) 0.9172(2) 0.0647(2) 0.033(2) Uani 1 d . .
H15A H 0.8464(2) 0.9200(2) 0.0394(2) 0.040 Uiso 1 calc R .
C68 C 0.7335(2) 0.9709(2) 0.2253(2) 0.044(2) Uani 1 d . .
H5A H 0.7286(2) 0.9942(2) 0.2522(2) 0.065 Uiso 1 calc R .
H5B H 0.7417(2) 0.9386(2) 0.2387(2) 0.065 Uiso 1 calc R .
H5C H 0.7033(2) 0.9684(2) 0.2059(2) 0.065 Uiso 1 calc R .
B1 B 0.9394(3) 1.0576(3) 0.1869(3) 0.032(2) Uani 1 d . .
H1 H 0.9660(3) 1.0807(3) 0.1766(3) 0.038 Uiso 1 calc R .
P1 P 0.77057(7) 1.27057(7) 0.22943(7) 0.0461(8) Uani 1 d S .
F11 F 0.8241(2) 1.2567(2) 0.2133(2) 0.091(2) Uani 1 d . .
F12 F 0.7522(2) 1.2166(2) 0.2164(2) 0.0776(14) Uani 1 d . .
P2 P 0.57529(6) 1.07529(6) 0.42471(6) 0.0299(7) Uani 1 d SD .
F21 F 0.54156(13) 1.04156(13) 0.45844(13) 0.066(2) Uani 1 d SD .
F22 F 0.5594(25) 1.0452(14) 0.3773(8) 0.079(15) Uani 0.33 d PD .
F23 F 0.5668(20) 1.1169(13) 0.4638(17) 0.064(10) Uani 0.33 d PD .
F24 F 0.5942(17) 1.1052(14) 0.4711(8) 0.049(9) Uani 0.33 d PD .
F25 F 0.5829(15) 1.0307(13) 0.3892(19) 0.076(15) Uani 0.33 d PD .
F26 F 0.60889(12) 1.10889(12) 0.39111(12) 0.048(2) Uani 1 d SD .
P3 P 1.10105(8) 0.89895(8) 0.39895(8) 0.0568(10) Uani 1 d S .
F31 F 1.0697(2) 0.9439(2) 0.3807(2) 0.104(2) Uani 1 d . .
F32 F 1.0787(3) 0.8688(2) 0.3556(2) 0.129(2) Uani 1 d . .
O1 O 0.9615(4) 1.0090(4) 0.4210(5) 0.179(4) Uani 1 d . .
H11 H 0.9716(22) 0.9685(24) 0.4538(24) 0.050 Uiso 1 d . .
H12 H 0.9315(25) 1.0111(25) 0.4603(25) 0.050 Uiso 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 0.0246(4) 0.0278(4) 0.0337(4) 0.0007(3) 0.0021(3) -0.0022(3)
S27 0.0291(9) 0.0300(9) 0.0411(10) 0.0037(7) -0.0004(7) -0.0016(7)
S47 0.0410(10) 0.0480(11) 0.0391(10) 0.0077(8) 0.0084(8) 0.0074(8)
S67 0.0263(8) 0.0312(9) 0.0354(9) -0.0007(7) 0.0041(7) -0.0018(7)
N11 0.029(3) 0.032(3) 0.028(3) -0.002(2) 0.003(2) -0.007(2)
N12 0.026(3) 0.031(3) 0.034(3) -0.001(2) 0.002(2) -0.003(2)
N31 0.029(3) 0.029(3) 0.030(3) -0.003(2) 0.003(2) -0.008(2)
N32 0.025(3) 0.033(3) 0.032(3) -0.002(2) 0.004(2) -0.001(2)
N51 0.023(3) 0.029(3) 0.029(3) 0.002(2) 0.005(2) -0.003(2)
N52 0.024(3) 0.034(3) 0.032(3) -0.001(2) 0.008(2) -0.005(2)
C13 0.027(4) 0.032(4) 0.028(3) -0.004(3) 0.000(3) 0.003(3)
C14 0.029(4) 0.044(4) 0.041(4) -0.002(3) -0.008(3) 0.011(3)
C15 0.025(4) 0.040(4) 0.045(4) -0.010(3) -0.001(3) -0.001(3)
C21 0.031(4) 0.043(4) 0.031(4) 0.003(3) 0.001(3) 0.006(3)
C22 0.032(4) 0.040(4) 0.036(4) 0.005(3) 0.006(3) 0.006(3)
C23 0.034(4) 0.044(4) 0.049(4) 0.012(4) 0.008(3) 0.006(3)
C24 0.052(5) 0.078(6) 0.056(5) 0.036(4) 0.006(4) 0.004(4)
C25 0.047(5) 0.096(7) 0.062(5) 0.033(5) -0.012(4) -0.003(5)
C26 0.042(4) 0.073(5) 0.048(5) 0.017(4) -0.011(4) -0.005(4)
C28 0.068(5) 0.039(4) 0.037(4) -0.007(3) -0.004(4) 0.015(4)
C33 0.028(3) 0.036(4) 0.027(3) -0.001(3) 0.004(3) 0.001(3)
C34 0.046(4) 0.026(4) 0.037(4) -0.001(3) 0.009(3) 0.002(3)
C35 0.044(4) 0.025(4) 0.034(4) 0.000(3) -0.002(3) -0.006(3)
C41 0.035(4) 0.031(4) 0.033(4) -0.007(3) 0.004(3) 0.004(3)
C42 0.035(4) 0.033(4) 0.036(4) -0.007(3) 0.005(3) -0.002(3)
C43 0.051(4) 0.029(4) 0.041(4) 0.003(3) 0.015(3) 0.001(3)
C44 0.045(4) 0.046(4) 0.053(5) 0.002(4) 0.020(4) 0.005(4)
C45 0.040(4) 0.059(5) 0.056(5) -0.001(4) 0.014(4) 0.016(4)
C46 0.049(4) 0.038(4) 0.042(4) 0.000(3) 0.013(4) 0.008(3)
C48 0.052(5) 0.066(5) 0.058(5) 0.020(4) 0.012(4) 0.011(4)
C53 0.023(3) 0.024(3) 0.030(3) -0.002(3) 0.003(3) 0.003(3)
C54 0.031(3) 0.030(3) 0.026(3) 0.005(3) 0.001(3) 0.002(3)
C55 0.029(3) 0.023(3) 0.032(4) 0.007(3) 0.005(3) 0.002(3)
C61 0.028(3) 0.027(3) 0.027(3) 0.005(3) -0.002(3) 0.002(3)
C62 0.028(3) 0.029(3) 0.035(4) 0.003(3) -0.004(3) 0.001(3)
C63 0.030(4) 0.036(4) 0.040(4) -0.003(3) 0.001(3) -0.011(3)
C64 0.043(4) 0.037(4) 0.050(4) -0.002(3) -0.003(4) -0.014(3)
C65 0.040(4) 0.034(4) 0.042(4) -0.005(3) -0.010(3) 0.001(3)
C66 0.033(4) 0.036(4) 0.030(4) 0.001(3) 0.003(3) 0.007(3)
C68 0.030(4) 0.052(4) 0.049(4) -0.008(3) 0.009(3) -0.011(3)
B1 0.034(4) 0.026(4) 0.035(4) -0.005(3) 0.008(3) -0.010(3)
P1 0.0461(8) 0.0461(8) 0.0461(8) 0.0016(9) 0.0016(9) -0.0016(9)
F11 0.062(3) 0.123(4) 0.088(4) -0.002(3) 0.028(3) 0.013(3)
F12 0.104(4) 0.050(3) 0.079(3) -0.009(2) -0.017(3) -0.004(3)
P2 0.0299(7) 0.0299(7) 0.0299(7) -0.0016(8) -0.0016(8) 0.0016(8)
F21 0.066(2) 0.066(2) 0.066(2) 0.015(2) 0.015(2) -0.015(2)
F22 0.184(50) 0.014(17) 0.040(11) -0.021(14) -0.006(24) 0.011(14)
F23 0.029(19) 0.084(23) 0.078(24) -0.059(18) 0.028(16) -0.022(17)
F24 0.049(20) 0.070(21) 0.028(9) -0.001(12) -0.006(14) -0.041(17)
F25 0.089(27) 0.020(14) 0.121(38) -0.017(16) 0.023(23) 0.017(15)
F26 0.048(2) 0.048(2) 0.048(2) 0.007(2) 0.007(2) -0.007(2)
P3 0.0568(10) 0.0568(10) 0.0568(10) 0.0053(11) -0.0053(11) -0.0053(11)
F31 0.082(4) 0.086(4) 0.146(5) 0.047(3) -0.052(3) -0.020(3)
F32 0.174(6) 0.126(5) 0.087(4) -0.054(4) -0.006(4) -0.005(5)
O1 0.174(10) 0.133(8) 0.229(12) 0.028(9) -0.054(9) -0.014(8)

_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 N12 1.968(5) . ?
Cu1 N32 2.048(5) . ?
Cu1 N52 2.141(5) . ?
Cu1 S27 2.313(2) . ?
Cu1 S67 2.372(2) . ?
S27 C22 1.790(6) . ?
S27 C28 1.812(6) . ?
S47 C42 1.778(6) . ?
S47 C48 1.811(7) . ?
S67 C68 1.790(6) . ?
S67 C62 1.798(6) . ?
N11 C15 1.347(7) . ?
N11 N12 1.361(6) . ?
N11 B1 1.552(8) . ?
N12 C13 1.338(7) . ?
N31 C35 1.354(7) . ?
N31 N32 1.366(6) . ?
N31 B1 1.544(8) . ?
N32 C33 1.348(7) . ?
N51 C55 1.354(7) . ?
N51 N52 1.361(6) . ?
N51 B1 1.533(8) . ?
N52 C53 1.342(7) . ?
C13 C14 1.395(8) . ?
C13 C21 1.484(8) . ?
C14 C15 1.365(8) . ?
C21 C26 1.386(9) . ?
C21 C22 1.399(9) . ?
C22 C23 1.389(8) . ?
C23 C24 1.380(9) . ?
C24 C25 1.368(10) . ?
C25 C26 1.381(10) . ?
C33 C34 1.386(8) . ?
C33 C41 1.477(8) . ?
C34 C35 1.375(8) . ?
C41 C46 1.399(9) . ?
C41 C42 1.410(8) . ?
C42 C43 1.380(8) . ?
C43 C44 1.363(9) . ?
C44 C45 1.375(9) . ?
C45 C46 1.386(9) . ?
C53 C54 1.397(8) . ?
C53 C61 1.468(8) . ?
C54 C55 1.367(8) . ?
C61 C66 1.387(8) . ?
C61 C62 1.418(8) . ?
C62 C63 1.385(8) . ?
C63 C64 1.384(9) . ?
C64 C65 1.375(9) . ?
C65 C66 1.384(8) . ?
P1 F11 1.572(5) 11_466 ?
P1 F11 1.572(5) . ?
P1 F11 1.572(5) 8_656 ?
P1 F12 1.595(5) 11_466 ?
P1 F12 1.595(5) 8_656 ?
P1 F12 1.595(5) . ?
P2 F25 1.57(2) 11_466 ?
P2 F25 1.57(2) . ?
P2 F25 1.57(2) 8_656 ?
P2 F23 1.58(2) 8_656 ?
P2 F23 1.58(2) . ?
P2 F23 1.58(2) 11_466 ?
P2 F26 1.588(6) . ?
P2 F22 1.59(2) 11_466 ?
P2 F22 1.59(2) . ?
P2 F22 1.59(2) 8_656 ?
P2 F24 1.59(2) 8_656 ?
P2 F24 1.59(2) . ?
F22 F25 0.82(3) . ?
F22 F23 0.88(2) 8_656 ?
F22 F24 1.54(4) 11_466 ?
F22 F24 1.64(3) 8_656 ?
F23 F24 0.84(3) . ?
F23 F22 0.88(2) 11_466 ?
F23 F25 1.53(3) 8_656 ?
F23 F25 1.62(3) 11_466 ?
F24 F25 0.76(3) 8_656 ?
F24 F22 1.54(4) 8_656 ?
F24 F22 1.64(3) 11_466 ?
F25 F24 0.76(3) 11_466 ?
F25 F23 1.53(3) 11_466 ?
F25 F23 1.62(3) 8_656 ?
P3 F32 1.564(6) . ?
P3 F32 1.564(6) 7_674 ?
P3 F32 1.564(6) 10_756 ?
P3 F31 1.576(5) . ?
P3 F31 1.576(5) 10_756 ?
P3 F31 1.576(5) 7_674 ?

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
N12 Cu1 N32 88.1(2) . . ?
N12 Cu1 N52 90.4(2) . . ?
N32 Cu1 N52 89.3(2) . . ?
N12 Cu1 S27 89.92(15) . . ?
N32 Cu1 S27 158.48(14) . . ?
N52 Cu1 S27 112.13(13) . . ?
N12 Cu1 S67 167.72(15) . . ?
N32 Cu1 S67 93.06(14) . . ?
N52 Cu1 S67 77.39(13) . . ?
S27 Cu1 S67 93.36(6) . . ?
C22 S27 C28 101.1(3) . . ?
C22 S27 Cu1 107.2(2) . . ?
C28 S27 Cu1 102.9(2) . . ?
C42 S47 C48 103.7(3) . . ?
C68 S67 C62 103.9(3) . . ?
C68 S67 Cu1 113.3(2) . . ?
C62 S67 Cu1 102.1(2) . . ?
C15 N11 N12 108.9(5) . . ?
C15 N11 B1 130.4(5) . . ?
N12 N11 B1 120.6(5) . . ?
C13 N12 N11 108.1(5) . . ?
C13 N12 Cu1 134.7(4) . . ?
N11 N12 Cu1 117.2(4) . . ?
C35 N31 N32 108.9(5) . . ?
C35 N31 B1 130.9(5) . . ?
N32 N31 B1 120.2(5) . . ?
C33 N32 N31 107.0(4) . . ?
C33 N32 Cu1 136.5(4) . . ?
N31 N32 Cu1 115.5(3) . . ?
C55 N51 N52 109.0(5) . . ?
C55 N51 B1 133.3(5) . . ?
N52 N51 B1 117.5(5) . . ?
C53 N52 N51 107.3(4) . . ?
C53 N52 Cu1 136.1(4) . . ?
N51 N52 Cu1 116.5(3) . . ?
N12 C13 C14 108.2(5) . . ?
N12 C13 C21 123.0(5) . . ?
C14 C13 C21 128.8(6) . . ?
C15 C14 C13 106.7(5) . . ?
N11 C15 C14 108.2(5) . . ?
C26 C21 C22 117.0(6) . . ?
C26 C21 C13 117.2(6) . . ?
C22 C21 C13 125.8(5) . . ?
C23 C22 C21 121.0(6) . . ?
C23 C22 S27 114.3(5) . . ?
C21 C22 S27 124.7(5) . . ?
C24 C23 C22 120.2(7) . . ?
C25 C24 C23 119.5(7) . . ?
C24 C25 C26 120.2(7) . . ?
C25 C26 C21 122.0(7) . . ?
N32 C33 C34 109.8(5) . . ?
N32 C33 C41 121.2(5) . . ?
C34 C33 C41 128.9(5) . . ?
C35 C34 C33 105.5(5) . . ?
N31 C35 C34 108.7(5) . . ?
C46 C41 C42 118.6(6) . . ?
C46 C41 C33 117.6(6) . . ?
C42 C41 C33 123.8(5) . . ?
C43 C42 C41 118.8(6) . . ?
C43 C42 S47 122.8(5) . . ?
C41 C42 S47 118.4(5) . . ?
C44 C43 C42 121.9(6) . . ?
C43 C44 C45 120.4(6) . . ?
C44 C45 C46 119.3(6) . . ?
C45 C46 C41 120.9(6) . . ?
N52 C53 C54 109.4(5) . . ?
N52 C53 C61 119.0(5) . . ?
C54 C53 C61 131.5(5) . . ?
C55 C54 C53 105.6(5) . . ?
N51 C55 C54 108.6(5) . . ?
C66 C61 C62 118.2(5) . . ?
C66 C61 C53 119.1(5) . . ?
C62 C61 C53 122.7(5) . . ?
C63 C62 C61 120.1(5) . . ?
C63 C62 S67 121.0(5) . . ?
C61 C62 S67 118.9(4) . . ?
C64 C63 C62 120.2(6) . . ?
C65 C64 C63 120.1(6) . . ?
C64 C65 C66 120.2(6) . . ?
C65 C66 C61 121.1(6) . . ?
N51 B1 N31 108.8(5) . . ?
N51 B1 N11 109.7(5) . . ?
N31 B1 N11 107.5(5) . . ?
F11 P1 F11 91.8(3) 11_466 . ?
F11 P1 F11 91.8(3) 11_466 8_656 ?
F11 P1 F11 91.8(3) . 8_656 ?
F11 P1 F12 90.4(3) 11_466 11_466 ?
F11 P1 F12 177.7(3) . 11_466 ?
F11 P1 F12 88.6(2) 8_656 11_466 ?
F11 P1 F12 177.7(3) 11_466 8_656 ?
F11 P1 F12 88.6(2) . 8_656 ?
F11 P1 F12 90.4(3) 8_656 8_656 ?
F12 P1 F12 89.1(3) 11_466 8_656 ?
F11 P1 F12 88.6(2) 11_466 . ?
F11 P1 F12 90.4(3) . . ?
F11 P1 F12 177.7(3) 8_656 . ?
F12 P1 F12 89.1(3) 11_466 . ?
F12 P1 F12 89.1(3) 8_656 . ?
F25 P2 F25 119.98(8) 11_466 . ?
F25 P2 F25 119.98(7) 11_466 8_656 ?
F25 P2 F25 119.97(9) . 8_656 ?
F25 P2 F23 58.0(13) 11_466 8_656 ?
F25 P2 F23 62.0(13) . 8_656 ?
F25 P2 F23 175.2(13) 8_656 8_656 ?
F25 P2 F23 62.0(13) 11_466 . ?
F25 P2 F23 175.2(13) . . ?
F25 P2 F23 58.0(13) 8_656 . ?
F23 P2 F23 119.6(2) 8_656 . ?
F25 P2 F23 175.2(14) 11_466 11_466 ?
F25 P2 F23 58.0(13) . 11_466 ?
F25 P2 F23 62.0(13) 8_656 11_466 ?
F23 P2 F23 119.6(2) 8_656 11_466 ?
F23 P2 F23 119.6(2) . 11_466 ?
F25 P2 F26 90.9(16) 11_466 . ?
F25 P2 F26 90.9(15) . . ?
F25 P2 F26 90.9(15) 8_656 . ?
F23 P2 F26 93.4(9) 8_656 . ?
F23 P2 F26 93.4(9) . . ?
F23 P2 F26 93.4(9) 11_466 . ?
F25 P2 F22 30.1(10) 11_466 11_466 ?
F25 P2 F22 150.1(11) . 11_466 ?
F25 P2 F22 90.0(11) 8_656 11_466 ?
F23 P2 F22 88.1(8) 8_656 11_466 ?
F23 P2 F22 32.2(9) . 11_466 ?
F23 P2 F22 151.8(8) 11_466 11_466 ?
F26 P2 F22 89.2(10) . 11_466 ?
F25 P2 F22 90.0(11) 11_466 . ?
F25 P2 F22 30.1(10) . . ?
F25 P2 F22 150.1(11) 8_656 . ?
F23 P2 F22 32.2(9) 8_656 . ?
F23 P2 F22 151.8(8) . . ?
F23 P2 F22 88.1(8) 11_466 . ?
F26 P2 F22 89.2(10) . . ?
F22 P2 F22 119.98(4) 11_466 . ?
F25 P2 F22 150.1(11) 11_466 8_656 ?
F25 P2 F22 90.0(11) . 8_656 ?
F25 P2 F22 30.1(10) 8_656 8_656 ?
F23 P2 F22 151.8(8) 8_656 8_656 ?
F23 P2 F22 88.1(8) . 8_656 ?
F23 P2 F22 32.2(9) 11_466 8_656 ?
F26 P2 F22 89.2(10) . 8_656 ?
F22 P2 F22 119.98(6) 11_466 8_656 ?
F22 P2 F22 119.98(6) . 8_656 ?
F25 P2 F24 27.8(11) 11_466 8_656 ?
F25 P2 F24 92.3(12) . 8_656 ?
F25 P2 F24 147.7(11) 8_656 8_656 ?
F23 P2 F24 30.7(12) 8_656 8_656 ?
F23 P2 F24 89.8(13) . 8_656 ?
F23 P2 F24 150.3(13) 11_466 8_656 ?
F26 P2 F24 88.6(9) . 8_656 ?
F22 P2 F24 57.8(14) 11_466 8_656 ?
F22 P2 F24 62.2(14) . 8_656 ?
F22 P2 F24 176.9(15) 8_656 8_656 ?
F25 P2 F24 92.3(12) 11_466 . ?
F25 P2 F24 147.7(11) . . ?
F25 P2 F24 27.8(11) 8_656 . ?
F23 P2 F24 150.3(13) 8_656 . ?
F23 P2 F24 30.7(12) . . ?
F23 P2 F24 89.8(13) 11_466 . ?
F26 P2 F24 88.6(9) . . ?
F22 P2 F24 62.2(14) 11_466 . ?
F22 P2 F24 176.9(15) . . ?
F22 P2 F24 57.8(14) 8_656 . ?
F24 P2 F24 119.94(7) 8_656 . ?
F25 F22 F23 144.7(30) . 8_656 ?
F25 F22 F24 12.9(20) . 11_466 ?
F23 F22 F24 133.6(23) 8_656 11_466 ?
F25 F22 P2 73.5(20) . . ?
F23 F22 P2 72.9(15) 8_656 . ?
F24 F22 P2 61.2(12) 11_466 . ?
F25 F22 F24 132.4(22) . 8_656 ?
F23 F22 F24 16.1(14) 8_656 8_656 ?
F24 F22 F24 120.0(17) 11_466 8_656 ?
P2 F22 F24 58.9(9) . 8_656 ?
F24 F23 F22 146.9(28) . 11_466 ?
F24 F23 F25 16.5(17) . 8_656 ?
F22 F23 F25 135.0(21) 11_466 8_656 ?
F24 F23 P2 75.8(17) . . ?
F22 F23 P2 74.9(16) 11_466 . ?
F25 F23 P2 60.8(10) 8_656 . ?
F24 F23 F25 133.7(20) . 11_466 ?
F22 F23 F25 17.1(15) 11_466 11_466 ?
F25 F23 F25 119.6(16) 8_656 11_466 ?
P2 F23 F25 58.8(10) . 11_466 ?
F25 F24 F23 145.3(35) 8_656 . ?
F25 F24 F22 14.0(21) 8_656 8_656 ?
F23 F24 F22 133.8(21) . 8_656 ?
F25 F24 P2 74.4(21) 8_656 . ?
F23 F24 P2 73.5(16) . . ?
F22 F24 P2 61.1(10) 8_656 . ?
F25 F24 F22 133.1(26) 8_656 11_466 ?
F23 F24 F22 16.9(16) . 11_466 ?
F22 F24 F22 119.9(16) 8_656 11_466 ?
P2 F24 F22 58.9(12) . 11_466 ?
F24 F25 F22 153.1(40) 11_466 . ?
F24 F25 F23 18.2(20) 11_466 11_466 ?
F22 F25 F23 137.6(23) . 11_466 ?
F24 F25 P2 77.8(22) 11_466 . ?
F22 F25 P2 76.4(18) . . ?
F23 F25 P2 61.2(10) 11_466 . ?
F24 F25 F23 137.0(27) 11_466 8_656 ?
F22 F25 F23 18.3(16) . 8_656 ?
F23 F25 F23 120.0(16) 11_466 8_656 ?
P2 F25 F23 59.2(10) . 8_656 ?
F32 P3 F32 95.8(4) . 7_674 ?
F32 P3 F32 95.8(4) . 10_756 ?
F32 P3 F32 95.8(4) 7_674 10_756 ?
F32 P3 F31 87.7(3) . . ?
F32 P3 F31 86.7(3) 7_674 . ?
F32 P3 F31 175.5(4) 10_756 . ?
F32 P3 F31 86.7(3) . 10_756 ?
F32 P3 F31 175.5(4) 7_674 10_756 ?
F32 P3 F31 87.7(3) 10_756 10_756 ?
F31 P3 F31 89.7(4) . 10_756 ?
F32 P3 F31 175.5(4) . 7_674 ?
F32 P3 F31 87.7(3) 7_674 7_674 ?
F32 P3 F31 86.7(3) 10_756 7_674 ?
F31 P3 F31 89.7(4) . 7_674 ?
F31 P3 F31 89.7(4) 10_756 7_674 ?

_refine_diff_density_max    1.689
_refine_diff_density_min   -0.443
_refine_diff_density_rms    0.067
#=END

 data_dati

_audit_creation_method            SHELXL

_chemical_name_systematic

;

 ?

;

_chemical_name_common             ?

_chemical_formula_moiety          ?

_chemical_formula_structural      ?

_chemical_formula_analytical      ?

_chemical_formula_sum             'C34 H36 Cu F12 N9 O4 P2'

_chemical_formula_weight          988.20

_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'

 '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    P21/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                    19.585(3)

_cell_length_b                    9.9751(9)

_cell_length_c                    20.884(2)

_cell_angle_alpha                 90.00

_cell_angle_beta                  92.845(11)

_cell_angle_gamma                 90.00

_cell_volume                      4075.0(8)

_cell_formula_units_Z             4

_cell_measurement_temperature     173(2)

_cell_measurement_reflns_used     ?

_cell_measurement_theta_min       ?

_cell_measurement_theta_max       ?



_exptl_crystal_description        needle

_exptl_crystal_colour             green

_exptl_crystal_size_max           0.50

_exptl_crystal_size_mid           0.40

_exptl_crystal_size_min           0.12

_exptl_crystal_density_meas       ?

_exptl_crystal_density_diffrn     1.611

_exptl_crystal_density_method     ?

_exptl_crystal_F_000              2008

_exptl_absorpt_coefficient_mu     0.720

_exptl_absorpt_correction_type

'Empirical, pseudo-azimuthal scan (SADABS)'

_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        'Siemens SMART Area Detector'

_diffrn_measurement_method        
'\w rotation with narrow frames (0.3 degrees)'

_diffrn_standards_number          ?

_diffrn_standards_interval_count  ?

_diffrn_standards_interval_time   ?

_diffrn_standards_decay_%         ?

_diffrn_reflns_number             25058

_diffrn_reflns_av_R_equivalents   0.0429

_diffrn_reflns_av_sigmaI/netI     0.0624

_diffrn_reflns_limit_h_min        -14

_diffrn_reflns_limit_h_max        25

_diffrn_reflns_limit_k_min        -12

_diffrn_reflns_limit_k_max        12

_diffrn_reflns_limit_l_min        -27

_diffrn_reflns_limit_l_max        25

_diffrn_reflns_theta_min          1.95

_diffrn_reflns_theta_max          27.48

_reflns_number_total              9265

_reflns_number_observed           5974

_reflns_observed_criterion        >2sigma(I)



_computing_data_collection        ?

_computing_cell_refinement        ?

_computing_data_reduction         ?

_computing_structure_solution     'SHELXS-86 (Sheldrick, 1990)'

_computing_structure_refinement   'SHELXL-93 (Sheldrick, 1993)'

_computing_molecular_graphics     ?

_computing_publication_material   ?



_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^)+(0.1061P)^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     ?

_refine_ls_extinction_method      none

_refine_ls_extinction_coef        ?

_refine_ls_number_reflns          9265

_refine_ls_number_parameters      617

_refine_ls_number_restraints      0

_refine_ls_R_factor_all           0.0923

_refine_ls_R_factor_obs           0.0577

_refine_ls_wR_factor_all          0.1692

_refine_ls_wR_factor_obs          0.1515

_refine_ls_goodness_of_fit_all    0.954

_refine_ls_goodness_of_fit_obs    1.080

_refine_ls_restrained_S_all       0.954

_refine_ls_restrained_S_obs       1.080

_refine_ls_shift/esd_max          0.001

_refine_ls_shift/esd_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_thermal_displace_type

 _atom_site_occupancy

 _atom_site_calc_flag

 _atom_site_refinement_flags

 _atom_site_disorder_group

Cu1 Cu 0.34333(2) 0.09598(4) 0.45269(2) 0.02683(13) Uani 1 d . .

C1 C 0.2495(2) 0.3088(3) 0.35005(15) 0.0288(7) Uani 1 d . .

C11 C 0.2387(2) 0.4202(3) 0.2994(2) 0.0335(8) Uani 1 d . .

C12 C 0.1736(2) 0.4686(4) 0.2847(2) 0.0492(10) Uani 1 d . .

H12 H 0.1352(2) 0.4340(4) 0.3054(2) 0.059 Uiso 1 calc R .

C13 C 0.1655(3) 0.5700(5) 0.2384(2) 0.0674(14) Uani 1 d . .

H13 H 0.1212(3) 0.6049(5) 0.2279(2) 0.081 Uiso 1 calc R .

C14 C 0.2205(3) 0.6192(4) 0.2083(2) 0.0623(14) Uani 1 d . .

H14 H 0.2140(3) 0.6871(4) 0.1767(2) 0.075 Uiso 1 calc R .

C15 C 0.2852(3) 0.5712(4) 0.2232(2) 0.0481(11) Uani 1 d . .

H15 H 0.3234(3) 0.6061(4) 0.2022(2) 0.058 Uiso 1 calc R .

C16 C 0.2943(2) 0.4710(4) 0.2693(2) 0.0381(9) Uani 1 d . .

H16 H 0.3388(2) 0.4376(4) 0.2801(2) 0.046 Uiso 1 calc R .

N21 N 0.31927(14) 0.1059(3) 0.36139(12) 0.0273(6) Uani 1 d . .

N22 N 0.28842(14) 0.1990(3) 0.32266(12) 0.0267(6) Uani 1 d . .

C23 C 0.2857(2) 0.1541(4) 0.2608(2) 0.0333(8) Uani 1 d . .

H23 H 0.2647(2) 0.1988(4) 0.2249(2) 0.040 Uiso 1 calc R .

C24 C 0.3188(2) 0.0331(4) 0.2598(2) 0.0340(8) Uani 1 d . .

H24 H 0.3261(2) -0.0215(4) 0.2236(2) 0.041 Uiso 1 calc R .

C25 C 0.3394(2) 0.0072(3) 0.32401(15) 0.0292(7) Uani 1 d . .

N31 N 0.38749(15) -0.0777(3) 0.42242(12) 0.0285(6) Uani 1 d . .

C32 C 0.3763(2) -0.1003(3) 0.35830(15) 0.0276(7) Uani 1 d . .

C33 C 0.3971(2) -0.2181(3) 0.3295(2) 0.0341(8) Uani 1 d . .

H33 H 0.3895(2) -0.2308(3) 0.2847(2) 0.041 Uiso 1 calc R .

C34 C 0.4288(2) -0.3161(3) 0.3665(2) 0.0378(9) Uani 1 d . .

H34 H 0.4420(2) -0.3984(3) 0.3478(2) 0.045 Uiso 1 calc R .

C35 C 0.4412(2) -0.2930(3) 0.4319(2) 0.0369(8) Uani 1 d . .

H35 H 0.4641(2) -0.3580(3) 0.4584(2) 0.044 Uiso 1 calc R .

C36 C 0.4195(2) -0.1737(3) 0.4573(2) 0.0334(8) Uani 1 d . .

H36 H 0.4277(2) -0.1588(3) 0.5020(2) 0.040 Uiso 1 calc R .

N41 N 0.31263(15) 0.2819(3) 0.45361(12) 0.0275(6) Uani 1 d . .

N42 N 0.28762(14) 0.3639(3) 0.40659(12) 0.0275(6) Uani 1 d . .

C43 C 0.2921(2) 0.4947(3) 0.4271(2) 0.0326(8) Uani 1 d . .

H43 H 0.2767(2) 0.5716(3) 0.4037(2) 0.039 Uiso 1 calc R .

C44 C 0.3230(2) 0.4936(3) 0.4876(2) 0.0321(8) Uani 1 d . .

H44 H 0.3333(2) 0.5689(3) 0.5142(2) 0.038 Uiso 1 calc R .

C45 C 0.3362(2) 0.3585(3) 0.50200(15) 0.0264(7) Uani 1 d . .

N51 N 0.37957(15) 0.1525(3) 0.54292(12) 0.0280(6) Uani 1 d . .

C52 C 0.3694(2) 0.2834(3) 0.55547(14) 0.0265(7) Uani 1 d . .

C53 C 0.3874(2) 0.3401(4) 0.6145(2) 0.0309(7) Uani 1 d . .

H53 H 0.3802(2) 0.4328(4) 0.6219(2) 0.037 Uiso 1 calc R .

C54 C 0.4160(2) 0.2589(4) 0.6623(2) 0.0354(8) Uani 1 d . .

H54 H 0.4294(2) 0.2958(4) 0.7029(2) 0.042 Uiso 1 calc R .

C55 C 0.4251(2) 0.1240(4) 0.6506(2) 0.0355(8) Uani 1 d . .

H55 H 0.4439(2) 0.0665(4) 0.6832(2) 0.043 Uiso 1 calc R .

C56 C 0.4062(2) 0.0747(4) 0.5908(2) 0.0346(8) Uani 1 d . .

H56 H 0.4122(2) -0.0183(4) 0.5828(2) 0.042 Uiso 1 calc R .

N62 N 0.18589(15) 0.2525(3) 0.37173(13) 0.0312(6) Uani 1 d . .

C63 C 0.1484(2) 0.2905(4) 0.4212(2) 0.0435(9) Uani 1 d . .

H63 H 0.1606(2) 0.3554(4) 0.4531(2) 0.052 Uiso 1 calc R .

C64 C 0.0899(2) 0.2177(4) 0.4165(2) 0.0484(10) Uani 1 d . .

H64 H 0.0530(2) 0.2208(4) 0.4443(2) 0.058 Uiso 1 calc R .

C65 C 0.0954(2) 0.1368(4) 0.3622(2) 0.0351(8) Uani 1 d . .

N61 N 0.1534(2) 0.1591(3) 0.33412(13) 0.0338(7) Uani 1 d . .

C72 C 0.0481(2) 0.0320(4) 0.3359(2) 0.0372(8) Uani 1 d . .

N71 N -0.0008(2) -0.0081(4) 0.3745(2) 0.0478(9) Uani 1 d . .

C76 C -0.0417(2) -0.1092(5) 0.3526(2) 0.0561(12) Uani 1 d . .

H76 H -0.0766(2) -0.1394(5) 0.3791(2) 0.067 Uiso 1 calc R .

C75 C -0.0361(2) -0.1703(5) 0.2946(2) 0.0554(12) Uani 1 d . .

H75 H -0.0661(2) -0.2412(5) 0.2816(2) 0.067 Uiso 1 calc R .

C74 C 0.0137(2) -0.1276(5) 0.2557(2) 0.0525(11) Uani 1 d . .

H74 H 0.0189(2) -0.1688(5) 0.2152(2) 0.063 Uiso 1 calc R .

C73 C 0.0559(2) -0.0246(4) 0.2757(2) 0.0443(10) Uani 1 d . .

H73 H 0.0901(2) 0.0078(4) 0.2489(2) 0.053 Uiso 1 calc R .

C2 C 0.2142(3) 0.0188(7) 0.5369(3) 0.084(2) Uani 1 d . .

H2A H 0.2130(17) -0.0503(22) 0.5701(12) 0.126 Uiso 1 calc R .

H2B H 0.1684(6) 0.0295(44) 0.5163(5) 0.126 Uiso 1 calc R .

H2C H 0.2290(13) 0.1041(24) 0.5563(15) 0.126 Uiso 1 calc R .

O3 O 0.2613(2) -0.0206(3) 0.48965(14) 0.0540(8) Uani 1 d . .

C4 C 0.0497(4) -0.3847(9) 0.4355(5) 0.138(3) Uani 1 d . .

H4A H 0.0502(19) -0.4048(52) 0.3896(8) 0.208 Uiso 1 calc R .

H4B H 0.0066(5) -0.3405(27) 0.4447(29) 0.208 Uiso 1 calc R .

H4C H 0.0541(18) -0.4682(28) 0.4601(23) 0.208 Uiso 1 calc R .

O5 O 0.1011(5) -0.3049(12) 0.4518(4) 0.266(6) Uani 1 d . .

H5 H 0.0971(5) -0.2328(12) 0.4312(4) 0.400 Uiso 1 calc R .

C6 C 0.1974(3) -0.1836(6) 0.3554(4) 0.094(2) Uani 1 d . .

H6A H 0.1515(10) -0.2174(39) 0.3435(9) 0.141 Uiso 1 calc R .

H6B H 0.2300(14) -0.2190(39) 0.3255(5) 0.141 Uiso 1 calc R .

H6C H 0.1973(23) -0.0854(6) 0.3534(6) 0.141 Uiso 1 calc R .

O7 O 0.2160(2) -0.2239(4) 0.4160(2) 0.0910(13) Uani 1 d . .

H7 H 0.1808(2) -0.2373(4) 0.4365(2) 0.136 Uiso 1 calc R .

O8 O -0.0429(4) 0.0707(8) 0.4933(4) 0.192(3) Uani 1 d . .

P1 P 0.17152(7) 0.0039(2) 0.11140(6) 0.0656(4) Uani 0.616(7) d P 1

F1 F 0.1599(5) 0.0581(13) 0.0471(3) 0.138(4) Uani 0.616(7) d P 1

F2 F 0.1847(3) -0.0691(5) 0.1835(2) 0.072(2) Uani 0.616(7) d P 1

F3 F 0.1981(6) -0.1344(8) 0.0809(4) 0.140(4) Uani 0.616(7) d P 1

F4 F 0.2456(4) 0.0536(14) 0.1206(3) 0.127(4) Uani 0.616(7) d P 1

F5 F 0.1454(7) 0.1173(8) 0.1493(5) 0.158(6) Uani 0.616(7) d P 1

F6 F 0.0982(4) -0.0578(13) 0.1139(4) 0.122(4) Uani 0.616(7) d P 1

P1' P 0.17152(7) 0.0039(2) 0.11140(6) 0.0656(4) Uani 0.384(7) d P 2

F1' F 0.1799(5) -0.0417(13) 0.0380(4) 0.074(3) Uani 0.384(7) d P 2

F2' F 0.1585(5) 0.1038(15) 0.1686(5) 0.097(6) Uani 0.384(7) d P 2

F3' F 0.2372(5) -0.0573(11) 0.1296(6) 0.105(5) Uani 0.384(7) d P 2

F4' F 0.2156(6) 0.1424(11) 0.0834(7) 0.102(4) Uani 0.384(7) d P 2

F5' F 0.1043(6) 0.0936(16) 0.0777(6) 0.130(6) Uani 0.384(7) d P 2

F6' F 0.1324(7) -0.1143(15) 0.1236(8) 0.120(6) Uani 0.384(7) d P 2

P2 P 0.50906(5) 0.29308(8) 0.35798(4) 0.0311(2) Uani 1 d . .

F7 F 0.48394(12) 0.1786(2) 0.40541(11) 0.0500(6) Uani 1 d . .

F8 F 0.53405(14) 0.4072(2) 0.31095(11) 0.0528(6) Uani 1 d . .

F9 F 0.5030(2) 0.4012(2) 0.41273(12) 0.0776(10) Uani 1 d . .

F10 F 0.5175(2) 0.1838(2) 0.30329(12) 0.0772(9) Uani 1 d . .

F11 F 0.58562(13) 0.2652(3) 0.38321(14) 0.0700(8) Uani 1 d . .

F12 F 0.43277(14) 0.3205(3) 0.3325(2) 0.0831(10) 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 0.0369(3) 0.0234(2) 0.0192(2) -0.0006(2) -0.0080(2) 0.0001(2)

C1 0.034(2) 0.029(2) 0.022(2) 0.0004(13) -0.0091(14) -0.0003(14)

C11 0.044(2) 0.031(2) 0.024(2) 0.0015(13) -0.011(2) 0.003(2)

C12 0.047(3) 0.049(2) 0.051(2) 0.011(2) -0.016(2) 0.008(2)

C13 0.068(3) 0.068(3) 0.063(3) 0.015(2) -0.027(3) 0.023(3)

C14 0.100(4) 0.045(2) 0.041(2) 0.019(2) -0.015(3) 0.007(3)

C15 0.075(3) 0.043(2) 0.026(2) 0.006(2) -0.003(2) 0.002(2)

C16 0.047(2) 0.036(2) 0.031(2) 0.0062(15) -0.006(2) 0.001(2)

N21 0.032(2) 0.0261(13) 0.0235(13) 0.0008(11) -0.0043(12) 0.0004(12)

N22 0.031(2) 0.0284(14) 0.0201(13) 0.0018(10) -0.0074(11) 0.0004(12)

C23 0.040(2) 0.040(2) 0.019(2) 0.0000(14) -0.0066(14) 0.000(2)

C24 0.048(2) 0.034(2) 0.019(2) -0.0038(13) -0.006(2) 0.000(2)

C25 0.037(2) 0.028(2) 0.022(2) -0.0021(13) -0.0044(14) -0.0034(14)

N31 0.035(2) 0.0271(14) 0.0227(13) 0.0009(11) -0.0028(12) -0.0025(12)

C32 0.033(2) 0.027(2) 0.023(2) -0.0008(13) -0.0002(13) -0.0056(14)

C33 0.043(2) 0.031(2) 0.028(2) -0.0032(14) 0.000(2) -0.003(2)

C34 0.046(2) 0.027(2) 0.041(2) -0.0070(15) 0.005(2) 0.000(2)

C35 0.044(2) 0.029(2) 0.038(2) 0.0064(15) 0.001(2) 0.003(2)

C36 0.042(2) 0.032(2) 0.026(2) 0.0044(14) -0.003(2) 0.000(2)

N41 0.036(2) 0.0240(13) 0.0218(13) -0.0007(10) -0.0094(11) 0.0012(12)

N42 0.033(2) 0.0256(13) 0.0231(13) 0.0015(10) -0.0108(12) 0.0005(12)

C43 0.041(2) 0.026(2) 0.030(2) 0.0028(14) -0.004(2) 0.0003(15)

C44 0.043(2) 0.029(2) 0.024(2) -0.0033(13) -0.0030(15) -0.002(2)

C45 0.030(2) 0.028(2) 0.0202(15) -0.0019(12) -0.0029(13) -0.0012(14)

N51 0.036(2) 0.0267(14) 0.0206(13) -0.0001(11) -0.0060(12) 0.0003(12)

C52 0.027(2) 0.032(2) 0.0203(15) -0.0008(13) -0.0041(13) -0.0031(14)

C53 0.032(2) 0.033(2) 0.028(2) -0.0043(14) -0.0050(14) -0.0016(15)

C54 0.038(2) 0.046(2) 0.022(2) -0.0050(15) -0.0079(15) 0.000(2)

C55 0.037(2) 0.043(2) 0.025(2) 0.0054(14) -0.0096(15) 0.001(2)

C56 0.042(2) 0.032(2) 0.028(2) 0.0023(14) -0.008(2) 0.001(2)

N62 0.033(2) 0.036(2) 0.0247(14) -0.0019(12) -0.0052(12) -0.0031(13)

C63 0.047(2) 0.049(2) 0.034(2) -0.012(2) 0.004(2) -0.005(2)

C64 0.045(2) 0.060(3) 0.041(2) -0.010(2) 0.011(2) -0.009(2)

C65 0.036(2) 0.041(2) 0.028(2) 0.0024(15) -0.005(2) -0.004(2)

N61 0.035(2) 0.039(2) 0.0262(14) -0.0040(12) -0.0084(13) -0.0050(14)

C72 0.029(2) 0.049(2) 0.033(2) 0.002(2) -0.005(2) -0.001(2)

N71 0.041(2) 0.059(2) 0.043(2) -0.001(2) -0.003(2) -0.011(2)

C76 0.048(3) 0.067(3) 0.053(3) 0.001(2) -0.001(2) -0.019(2)

C75 0.053(3) 0.060(3) 0.051(3) -0.002(2) -0.016(2) -0.016(2)

C74 0.050(3) 0.064(3) 0.042(2) -0.009(2) -0.014(2) -0.008(2)

C73 0.043(2) 0.057(2) 0.033(2) -0.004(2) -0.006(2) -0.009(2)

C2 0.074(4) 0.120(5) 0.059(3) 0.007(3) 0.009(3) -0.021(4)

O3 0.056(2) 0.060(2) 0.047(2) -0.0041(14) 0.0108(15) -0.019(2)

C4 0.100(6) 0.119(7) 0.195(10) 0.042(6) -0.006(7) -0.003(5)

O5 0.182(7) 0.389(15) 0.225(9) 0.030(9) -0.024(6) -0.184(10)

C6 0.083(4) 0.064(4) 0.132(6) 0.002(4) -0.026(4) 0.004(3)

O7 0.070(3) 0.072(3) 0.128(4) -0.026(3) -0.019(3) 0.000(2)

O8 0.223(9) 0.202(8) 0.153(6) -0.035(5) 0.029(6) -0.008(6)

P1 0.0487(8) 0.1052(11) 0.0427(6) -0.0115(7) -0.0008(6) -0.0006(7)

F1 0.167(10) 0.201(10) 0.041(4) 0.065(5) -0.034(5) -0.040(9)

F2 0.082(4) 0.083(4) 0.050(3) 0.020(2) -0.001(3) 0.014(3)

F3 0.236(11) 0.096(5) 0.091(5) -0.027(4) 0.027(6) 0.023(6)

F4 0.076(4) 0.263(12) 0.042(3) -0.027(5) 0.006(3) -0.078(7)

F5 0.263(13) 0.083(5) 0.133(9) 0.049(6) 0.073(8) 0.108(7)

F6 0.068(5) 0.216(12) 0.079(4) 0.013(6) -0.007(4) -0.044(6)

P1' 0.0487(8) 0.1052(11) 0.0427(6) -0.0115(7) -0.0008(6) -0.0006(7)

F1' 0.072(6) 0.107(8) 0.044(5) -0.020(5) 0.002(4) 0.005(6)

F2' 0.062(6) 0.193(15) 0.038(5) -0.057(7) 0.021(4) -0.057(8)

F3' 0.076(7) 0.093(7) 0.137(10) 0.059(7) -0.072(7) -0.014(5)

F4' 0.101(8) 0.092(7) 0.116(10) -0.003(7) 0.037(7) -0.009(6)

F5' 0.070(7) 0.226(16) 0.091(8) -0.042(9) -0.023(6) 0.080(8)

F6' 0.060(8) 0.137(11) 0.163(14) 0.060(9) 0.018(9) -0.034(8)

P2 0.0385(5) 0.0245(4) 0.0291(4) 0.0042(3) -0.0092(4) -0.0002(4)

F7 0.0537(15) 0.0423(13) 0.0529(14) 0.0226(10) -0.0073(11) -0.0050(11)

F8 0.076(2) 0.0405(13) 0.0412(13) 0.0113(10) -0.0014(12) -0.0089(12)

F9 0.148(3) 0.0430(14) 0.0425(14) -0.0067(11) 0.009(2) 0.010(2)

F10 0.145(3) 0.0380(14) 0.0480(15) -0.0099(11) -0.005(2) 0.001(2)

F11 0.0436(15) 0.078(2) 0.086(2) 0.029(2) -0.0197(14) -0.0027(14)

F12 0.050(2) 0.084(2) 0.112(2) 0.052(2) -0.031(2) -0.0015(15)



_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 N21 1.944(3) . ?

Cu1 N41 1.950(3) . ?

Cu1 N31 2.051(3) . ?

Cu1 N51 2.059(3) . ?

Cu1 O3 2.156(3) . ?

C1 N62 1.459(4) . ?

C1 N22 1.467(4) . ?

C1 N42 1.472(4) . ?

C1 C11 1.541(4) . ?

C11 C16 1.380(5) . ?

C11 C12 1.385(5) . ?

C12 C13 1.402(6) . ?

C13 C14 1.365(8) . ?

C14 C15 1.376(7) . ?

C15 C16 1.394(5) . ?

N21 C25 1.328(4) . ?

N21 N22 1.354(3) . ?

N22 C23 1.365(4) . ?

C23 C24 1.370(5) . ?

C24 C25 1.404(4) . ?

C25 C32 1.460(5) . ?

N31 C36 1.340(4) . ?

N31 C32 1.365(4) . ?

C32 C33 1.391(5) . ?

C33 C34 1.374(5) . ?

C34 C35 1.395(5) . ?

C35 C36 1.378(5) . ?

N41 C45 1.331(4) . ?

N41 N42 1.351(3) . ?

N42 C43 1.375(4) . ?

C43 C44 1.373(5) . ?

C44 C45 1.402(5) . ?

C45 C52 1.470(4) . ?

N51 C52 1.349(4) . ?

N51 C56 1.350(4) . ?

C52 C53 1.385(4) . ?

C53 C54 1.382(5) . ?

C54 C55 1.380(5) . ?

C55 C56 1.376(5) . ?

N62 C63 1.352(5) . ?

N62 N61 1.357(4) . ?

C63 C64 1.355(6) . ?

C64 C65 1.400(5) . ?

C65 N61 1.322(5) . ?

C65 C72 1.485(5) . ?

C72 N71 1.343(5) . ?

C72 C73 1.393(5) . ?

N71 C76 1.353(5) . ?

C76 C75 1.364(6) . ?

C75 C74 1.368(6) . ?

C74 C73 1.372(6) . ?

C2 O3 1.439(6) . ?

C4 O5 1.315(10) . ?

C6 O7 1.361(7) . ?

P1 F1 1.456(5) . ?

P1 F5 1.486(9) . ?

P1 F4 1.536(6) . ?

P1 F6 1.566(8) . ?

P1 F3 1.617(7) . ?

P1 F2 1.681(4) . ?

P1' F6' 1.436(12) . ?

P1' F3' 1.456(9) . ?

P1' F2' 1.586(11) . ?

P1' F1' 1.615(8) . ?

P1' F5' 1.714(10) . ?

P1' F4' 1.746(10) . ?

P2 F9 1.580(3) . ?

P2 F12 1.584(3) . ?

P2 F11 1.589(3) . ?

P2 F10 1.593(3) . ?

P2 F8 1.596(2) . ?

P2 F7 1.605(2) . ?



loop_

 _geom_angle_atom_site_label_1

 _geom_angle_atom_site_label_2

 _geom_angle_atom_site_label_3

 _geom_angle

 _geom_angle_site_symmetry_1

 _geom_angle_site_symmetry_3

 _geom_angle_publ_flag

N21 Cu1 N41 84.34(11) . . ?

N21 Cu1 N31 79.98(11) . . ?

N41 Cu1 N31 160.34(11) . . ?

N21 Cu1 N51 159.98(11) . . ?

N41 Cu1 N51 79.80(11) . . ?

N31 Cu1 N51 112.47(11) . . ?

N21 Cu1 O3 103.29(11) . . ?

N41 Cu1 O3 105.89(12) . . ?

N31 Cu1 O3 89.30(11) . . ?

N51 Cu1 O3 92.81(11) . . ?

N62 C1 N22 107.6(3) . . ?

N62 C1 N42 107.6(3) . . ?

N22 C1 N42 109.8(3) . . ?

N62 C1 C11 113.6(3) . . ?

N22 C1 C11 109.1(3) . . ?

N42 C1 C11 109.2(3) . . ?

C16 C11 C12 120.7(3) . . ?

C16 C11 C1 119.5(3) . . ?

C12 C11 C1 119.8(3) . . ?

C11 C12 C13 118.4(4) . . ?

C14 C13 C12 120.8(5) . . ?

C13 C14 C15 120.7(4) . . ?

C14 C15 C16 119.3(4) . . ?

C11 C16 C15 120.1(4) . . ?

C25 N21 N22 107.1(3) . . ?

C25 N21 Cu1 118.3(2) . . ?

N22 N21 Cu1 134.4(2) . . ?

N21 N22 C23 109.6(3) . . ?

N21 N22 C1 120.3(2) . . ?

C23 N22 C1 128.1(3) . . ?

N22 C23 C24 107.9(3) . . ?

C23 C24 C25 105.1(3) . . ?

N21 C25 C24 110.2(3) . . ?

N21 C25 C32 114.2(3) . . ?

C24 C25 C32 135.6(3) . . ?

C36 N31 C32 117.7(3) . . ?

C36 N31 Cu1 129.0(2) . . ?

C32 N31 Cu1 113.1(2) . . ?

N31 C32 C33 121.8(3) . . ?

N31 C32 C25 114.3(3) . . ?

C33 C32 C25 123.9(3) . . ?

C34 C33 C32 119.5(3) . . ?

C33 C34 C35 119.0(3) . . ?

C36 C35 C34 118.6(3) . . ?

N31 C36 C35 123.5(3) . . ?

C45 N41 N42 107.7(3) . . ?

C45 N41 Cu1 117.3(2) . . ?

N42 N41 Cu1 132.0(2) . . ?

N41 N42 C43 109.5(2) . . ?

N41 N42 C1 120.6(2) . . ?

C43 N42 C1 128.8(3) . . ?

C44 C43 N42 107.3(3) . . ?

C43 C44 C45 105.9(3) . . ?

N41 C45 C44 109.6(3) . . ?

N41 C45 C52 114.1(3) . . ?

C44 C45 C52 136.3(3) . . ?

C52 N51 C56 117.9(3) . . ?

C52 N51 Cu1 113.3(2) . . ?

C56 N51 Cu1 128.5(2) . . ?

N51 C52 C53 122.3(3) . . ?

N51 C52 C45 114.2(3) . . ?

C53 C52 C45 123.5(3) . . ?

C54 C53 C52 118.7(3) . . ?

C55 C54 C53 119.6(3) . . ?

C56 C55 C54 118.5(3) . . ?

N51 C56 C55 122.9(3) . . ?

C63 N62 N61 112.2(3) . . ?

C63 N62 C1 129.4(3) . . ?

N61 N62 C1 117.9(3) . . ?

N62 C63 C64 106.4(3) . . ?

C63 C64 C65 105.6(4) . . ?

N61 C65 C64 111.4(3) . . ?

N61 C65 C72 119.2(3) . . ?

C64 C65 C72 129.3(4) . . ?

C65 N61 N62 104.3(3) . . ?

N71 C72 C73 122.3(4) . . ?

N71 C72 C65 116.0(3) . . ?

C73 C72 C65 121.6(4) . . ?

C72 N71 C76 116.5(4) . . ?

N71 C76 C75 124.1(4) . . ?

C76 C75 C74 118.7(4) . . ?

C75 C74 C73 119.2(4) . . ?

C74 C73 C72 119.1(4) . . ?

C2 O3 Cu1 127.8(3) . . ?

F1 P1 F5 99.6(7) . . ?

F1 P1 F4 95.6(5) . . ?

F5 P1 F4 92.1(7) . . ?

F1 P1 F6 94.3(5) . . ?

F5 P1 F6 86.6(7) . . ?

F4 P1 F6 170.0(5) . . ?

F1 P1 F3 89.5(6) . . ?

F5 P1 F3 170.4(5) . . ?

F4 P1 F3 90.2(6) . . ?

F6 P1 F3 89.5(6) . . ?

F1 P1 F2 176.2(6) . . ?

F5 P1 F2 83.9(4) . . ?

F4 P1 F2 85.8(4) . . ?

F6 P1 F2 84.3(4) . . ?

F3 P1 F2 86.9(4) . . ?

F6' P1' F3' 94.7(7) . . ?

F6' P1' F2' 106.0(8) . . ?

F3' P1' F2' 103.9(7) . . ?

F6' P1' F1' 91.0(8) . . ?

F3' P1' F1' 90.0(7) . . ?

F2' P1' F1' 156.8(7) . . ?

F6' P1' F5' 95.5(7) . . ?

F3' P1' F5' 167.4(7) . . ?

F2' P1' F5' 80.3(6) . . ?

F1' P1' F5' 82.5(5) . . ?

F6' P1' F4' 170.6(8) . . ?

F3' P1' F4' 88.5(6) . . ?

F2' P1' F4' 81.7(6) . . ?

F1' P1' F4' 80.2(6) . . ?

F5' P1' F4' 80.3(7) . . ?

F9 P2 F12 91.2(2) . . ?

F9 P2 F11 89.0(2) . . ?

F12 P2 F11 179.7(2) . . ?

F9 P2 F10 178.3(2) . . ?

F12 P2 F10 90.4(2) . . ?

F11 P2 F10 89.3(2) . . ?

F9 P2 F8 89.70(14) . . ?

F12 P2 F8 89.06(15) . . ?

F11 P2 F8 90.90(15) . . ?

F10 P2 F8 90.04(14) . . ?

F9 P2 F7 90.16(14) . . ?

F12 P2 F7 90.96(14) . . ?

F11 P2 F7 89.08(14) . . ?

F10 P2 F7 90.10(14) . . ?

F8 P2 F7 179.86(14) . . ?



_refine_diff_density_max    1.079

_refine_diff_density_min   -0.813

_refine_diff_density_rms    0.096

#=END
data_mdw

_audit_creation_method            SHELXL
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_formula_moiety          ?
_chemical_formula_structural      ?
_chemical_formula_analytical      ?
_chemical_formula_sum             'C33 H41 B Cl2 Cu F6 N9 O P'
_chemical_formula_weight          869.97
_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'
 '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'
 'O'  'O'   0.0106   0.0060
 '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'

_symmetry_cell_setting            triclinic
_symmetry_space_group_name_H-M    P-1

loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x, -y, -z'

_cell_length_a                    10.020(2)
_cell_length_b                    13.254(2)
_cell_length_c                    15.142(3)
_cell_angle_alpha                 105.878(13)
_cell_angle_beta                  106.30(2)
_cell_angle_gamma                 92.291(14)
_cell_volume                      1841.5(6)
_cell_formula_units_Z             2
_cell_measurement_temperature     173(2)
_cell_measurement_reflns_used     ?
_cell_measurement_theta_min       ?
_cell_measurement_theta_max       ?

_exptl_crystal_description        plate
_exptl_crystal_colour             green
_exptl_crystal_size_max           0.26
_exptl_crystal_size_mid           0.20
_exptl_crystal_size_min           0.04
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.569
_exptl_crystal_density_method     ?
_exptl_crystal_F_000              894
_exptl_absorpt_coefficient_mu     0.855
_exptl_absorpt_correction_type
'Empirical, pseudo-azimuthal scan (SADABS)'
_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        'Siemens SMART Area Detector'
 _diffrn_measurement_method        
 '\w rotation with narrow frames (0.3 degrees)'
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             15701
_diffrn_reflns_av_R_equivalents   0.0583
_diffrn_reflns_av_sigmaI/netI     0.0903
_diffrn_reflns_limit_h_min        -12
_diffrn_reflns_limit_h_max        13
_diffrn_reflns_limit_k_min        -17
_diffrn_reflns_limit_k_max        17
_diffrn_reflns_limit_l_min        -19
_diffrn_reflns_limit_l_max        19
_diffrn_reflns_theta_min          1.47
_diffrn_reflns_theta_max          25.00
_reflns_number_total              6449
_reflns_number_observed           4190
_reflns_observed_criterion        >2sigma(I)

_computing_data_collection        ?
_computing_cell_refinement        ?
_computing_data_reduction         ?
_computing_structure_solution     'SHELXS-86 (Sheldrick, 1990)'
_computing_structure_refinement   'SHELXL-93 (Sheldrick, 1993)'
_computing_molecular_graphics     ?
_computing_publication_material   ?

_refine_special_details
;
 Refinement on F^2^ for ALL reflections except for 23 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^)+(0.0870P)^2^+1.8400P] 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_number_reflns          6426
_refine_ls_number_parameters      516
_refine_ls_number_restraints      74
_refine_ls_R_factor_all           0.1106
_refine_ls_R_factor_obs           0.0627
_refine_ls_wR_factor_all          0.1811
_refine_ls_wR_factor_obs          0.1510
_refine_ls_goodness_of_fit_all    1.027
_refine_ls_goodness_of_fit_obs    1.106
_refine_ls_restrained_S_all       1.056
_refine_ls_restrained_S_obs       1.113
_refine_ls_shift/esd_max          -0.011
_refine_ls_shift/esd_mean         0.001

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 0.68513(7) -0.16526(5) 0.68549(5) 0.0230(2) Uani 1 d . .
O1 O 0.5489(4) -0.0731(3) 0.6584(3) 0.0250(9) Uani 1 d . .
H1B H 0.5756(56) -0.0191(41) 0.6792(39) 0.012(16) Uiso 1 d . .
H1A H 0.4972(104) -0.0818(74) 0.5818(77) 0.131(37) Uiso 1 d . .
N11 N 0.9706(4) -0.0827(3) 0.6876(3) 0.0221(10) Uani 1 d . .
N12 N 0.8639(4) -0.0428(3) 0.7202(3) 0.0230(10) Uani 1 d . .
N22 N 0.6814(4) 0.1088(3) 0.7832(3) 0.0234(10) Uani 1 d . .
N31 N 0.8365(4) -0.2294(3) 0.5384(3) 0.0243(10) Uani 1 d . .
N32 N 0.7033(4) -0.2126(3) 0.5407(3) 0.0236(10) Uani 1 d . .
N42 N 0.4186(5) -0.1602(3) 0.4695(3) 0.0265(10) Uani 1 d . .
N51 N 0.9382(5) -0.2680(3) 0.6946(3) 0.0255(10) Uani 1 d . .
N52 N 0.8197(5) -0.2563(3) 0.7185(3) 0.0257(10) Uani 1 d . .
N62 N 0.5982(4) -0.2436(3) 0.7725(3) 0.0232(10) Uani 1 d . .
C13 C 0.9080(5) 0.0611(4) 0.7671(4) 0.0209(11) Uani 1 d . .
C14 C 1.0419(6) 0.0865(4) 0.7634(4) 0.0293(13) Uani 1 d . .
H14 H 1.0972(6) 0.1537(4) 0.7903(4) 0.035 Uiso 1 calc R .
C15 C 1.0777(6) -0.0055(4) 0.7128(4) 0.0264(12) Uani 1 d . .
H15 H 1.1635(6) -0.0134(4) 0.6980(4) 0.032 Uiso 1 calc R .
C21 C 0.8233(6) 0.1331(4) 0.8133(4) 0.0240(12) Uani 1 d . .
C23 C 0.6045(6) 0.1764(4) 0.8238(4) 0.0274(13) Uani 1 d . .
C24 C 0.6653(6) 0.2706(4) 0.8954(4) 0.0337(14) Uani 1 d . .
H24 H 0.6084(6) 0.3175(4) 0.9227(4) 0.040 Uiso 1 calc R .
C25 C 0.8081(6) 0.2951(4) 0.9260(4) 0.0365(14) Uani 1 d . .
H25 H 0.8512(6) 0.3591(4) 0.9749(4) 0.044 Uiso 1 calc R .
C26 C 0.8889(6) 0.2257(4) 0.8850(4) 0.0290(13) Uani 1 d . .
H26 H 0.9881(6) 0.2414(4) 0.9057(4) 0.035 Uiso 1 calc R .
C27 C 0.4478(6) 0.1442(5) 0.7893(5) 0.041(2) Uani 1 d . .
H27A H 0.4015(7) 0.2033(11) 0.8168(23) 0.062 Uiso 1 calc R .
H27B H 0.4262(7) 0.0832(20) 0.8100(24) 0.062 Uiso 1 calc R .
H27C H 0.4140(8) 0.1253(29) 0.7188(5) 0.062 Uiso 1 calc R .
C33 C 0.6196(6) -0.2496(4) 0.4491(4) 0.0288(13) Uani 1 d . .
C34 C 0.6999(6) -0.2914(5) 0.3881(4) 0.0362(14) Uani 1 d . .
H34 H 0.6676(6) -0.3233(5) 0.3203(4) 0.043 Uiso 1 calc R .
C35 C 0.8354(7) -0.2759(4) 0.4481(4) 0.0337(14) Uani 1 d . .
H35 H 0.9151(7) -0.2952(4) 0.4284(4) 0.040 Uiso 1 calc R .
C41 C 0.4670(6) -0.2443(4) 0.4204(4) 0.0283(13) Uani 1 d . .
C43 C 0.2802(6) -0.1544(5) 0.4423(4) 0.0323(14) Uani 1 d . .
C44 C 0.1875(7) -0.2313(5) 0.3670(4) 0.0386(15) Uani 1 d . .
H44 H 0.0900(7) -0.2255(5) 0.3500(4) 0.046 Uiso 1 calc R .
C45 C 0.2363(7) -0.3155(5) 0.3173(5) 0.043(2) Uani 1 d . .
H45 H 0.1733(7) -0.3692(5) 0.2654(5) 0.051 Uiso 1 calc R .
C46 C 0.3790(7) -0.3223(5) 0.3427(4) 0.0372(15) Uani 1 d . .
H46 H 0.4156(7) -0.3795(5) 0.3076(4) 0.045 Uiso 1 calc R .
C47 C 0.2328(7) -0.0567(5) 0.4974(4) 0.043(2) Uani 1 d . .
H47A H 0.1307(8) -0.0672(13) 0.4829(23) 0.065 Uiso 1 calc R .
H47B H 0.2597(38) 0.0042(8) 0.4783(22) 0.065 Uiso 1 calc R .
H47C H 0.2771(34) -0.0436(19) 0.5667(5) 0.065 Uiso 1 calc R .
C53 C 0.8117(6) -0.3159(4) 0.7754(4) 0.0267(12) Uani 1 d . .
C54 C 0.9291(6) -0.3690(4) 0.7885(4) 0.0317(14) Uani 1 d . .
H54 H 0.9516(6) -0.4168(4) 0.8255(4) 0.038 Uiso 1 calc R .
C55 C 1.0063(6) -0.3370(4) 0.7360(4) 0.0316(14) Uani 1 d . .
H55 H 1.0929(6) -0.3598(4) 0.7301(4) 0.038 Uiso 1 calc R .
C61 C 0.6850(6) -0.3110(4) 0.8062(4) 0.0259(12) Uani 1 d . .
C63 C 0.4777(6) -0.2361(4) 0.7959(4) 0.0298(13) Uani 1 d . .
C64 C 0.4435(6) -0.2930(5) 0.8526(4) 0.0373(15) Uani 1 d . .
H64 H 0.3580(6) -0.2860(5) 0.8680(4) 0.045 Uiso 1 calc R .
C65 C 0.5330(6) -0.3599(5) 0.8870(5) 0.0391(15) Uani 1 d . .
H65 H 0.5104(6) -0.3989(5) 0.9260(5) 0.047 Uiso 1 calc R .
C66 C 0.6565(6) -0.3685(5) 0.8628(4) 0.0353(14) Uani 1 d . .
H66 H 0.7205(6) -0.4137(5) 0.8851(4) 0.042 Uiso 1 calc R .
C67 C 0.3782(6) -0.1650(5) 0.7584(5) 0.0374(15) Uani 1 d . .
H67A H 0.4245(15) -0.0919(6) 0.7832(22) 0.056 Uiso 1 calc R .
H67B H 0.2950(19) -0.1691(23) 0.7799(23) 0.056 Uiso 1 calc R .
H67C H 0.3500(31) -0.1874(19) 0.6879(5) 0.056 Uiso 1 calc R .
B1 B 0.9622(6) -0.2012(5) 0.6305(5) 0.0255(14) Uani 1 d . .
H1 H 1.0510(6) -0.2150(5) 0.6141(5) 0.031 Uiso 1 calc R .
P1 P 0.78292(15) 0.57629(11) 1.12936(10) 0.0261(3) Uani 1 d . .
F1 F 0.7902(4) 0.4743(3) 1.1659(3) 0.0515(10) Uani 1 d . .
F2 F 0.8737(4) 0.6495(3) 1.2343(2) 0.0514(10) Uani 1 d . .
F3 F 0.6412(3) 0.5978(3) 1.1566(2) 0.0406(9) Uani 1 d . .
F4 F 0.6918(4) 0.5049(2) 1.0243(2) 0.0392(8) Uani 1 d . .
F5 F 0.9245(3) 0.5551(3) 1.1019(3) 0.0442(9) Uani 1 d . .
F6 F 0.7757(4) 0.6781(2) 1.0917(3) 0.0425(9) Uani 1 d . .
C1 C 1.2924(8) -0.4947(6) 0.4823(6) 0.062(2) Uani 1 d D .
Cl1 Cl 1.4643(17) -0.4762(11) 0.5207(11) 0.187(7) Uani 0.30 d PDU 1
Cl2 Cl 1.2377(21) -0.4220(30) 0.5734(16) 0.416(21) Uani 0.30 d PDU 1
Cl1' Cl 1.4254(9) -0.4195(6) 0.5785(6) 0.213(3) Uani 0.70 d PDU 2
Cl2' Cl 1.1418(10) -0.4450(6) 0.5010(6) 0.209(3) Uani 0.70 d PDU 2
C2 C 0.9119(15) -0.0269(9) 0.9863(8) 0.125(4) Uani 1 d U .
C3 C 0.8383(17) 0.0551(14) 1.0387(12) 0.130(6) Uani 1 d U .
C4 C 0.6680(15) 0.0029(8) 0.9942(8) 0.094(4) Uani 1 d U .
C5 C 0.9099(13) 0.1041(7) 1.0774(7) 0.079(4) Uani 1 d U .
C6 C 0.6939(19) -0.0720(16) 1.0145(8) 0.197(10) Uani 1 d U .

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 0.0228(4) 0.0240(4) 0.0265(4) 0.0110(3) 0.0100(3) 0.0087(3)
O1 0.025(2) 0.018(2) 0.034(2) 0.008(2) 0.011(2) 0.008(2)
N11 0.021(2) 0.021(2) 0.024(2) 0.002(2) 0.011(2) 0.004(2)
N12 0.020(2) 0.025(2) 0.023(2) 0.005(2) 0.007(2) 0.007(2)
N22 0.025(3) 0.020(2) 0.026(2) 0.005(2) 0.009(2) 0.006(2)
N31 0.021(2) 0.025(2) 0.030(3) 0.008(2) 0.012(2) 0.006(2)
N32 0.024(3) 0.019(2) 0.026(3) 0.005(2) 0.007(2) 0.005(2)
N42 0.025(3) 0.031(3) 0.021(2) 0.010(2) 0.004(2) -0.001(2)
N51 0.025(3) 0.024(2) 0.028(3) 0.007(2) 0.009(2) 0.009(2)
N52 0.027(3) 0.028(2) 0.028(3) 0.011(2) 0.012(2) 0.011(2)
N62 0.024(2) 0.021(2) 0.025(2) 0.008(2) 0.008(2) 0.002(2)
C13 0.023(3) 0.017(3) 0.019(3) 0.004(2) 0.002(2) 0.002(2)
C14 0.025(3) 0.025(3) 0.036(3) 0.008(3) 0.008(3) 0.002(2)
C15 0.022(3) 0.026(3) 0.035(3) 0.010(2) 0.013(3) 0.001(2)
C21 0.030(3) 0.023(3) 0.021(3) 0.009(2) 0.009(3) 0.001(2)
C23 0.029(3) 0.021(3) 0.036(3) 0.008(2) 0.018(3) 0.007(2)
C24 0.035(4) 0.024(3) 0.040(4) 0.000(3) 0.016(3) 0.007(3)
C25 0.044(4) 0.026(3) 0.032(3) 0.000(3) 0.008(3) 0.000(3)
C26 0.027(3) 0.024(3) 0.031(3) 0.003(2) 0.006(3) -0.001(2)
C27 0.028(3) 0.032(3) 0.065(5) 0.007(3) 0.022(3) 0.007(3)
C33 0.035(3) 0.027(3) 0.023(3) 0.007(2) 0.007(3) 0.001(2)
C34 0.040(4) 0.043(4) 0.023(3) 0.004(3) 0.010(3) 0.004(3)
C35 0.043(4) 0.032(3) 0.031(3) 0.004(3) 0.022(3) 0.010(3)
C41 0.035(3) 0.031(3) 0.019(3) 0.011(2) 0.005(3) 0.001(3)
C43 0.025(3) 0.041(3) 0.036(3) 0.023(3) 0.008(3) 0.002(3)
C44 0.033(4) 0.043(4) 0.042(4) 0.025(3) 0.002(3) 0.002(3)
C45 0.039(4) 0.039(4) 0.037(4) 0.015(3) -0.011(3) -0.013(3)
C46 0.047(4) 0.030(3) 0.027(3) 0.007(3) 0.003(3) 0.001(3)
C47 0.037(4) 0.058(4) 0.036(4) 0.018(3) 0.009(3) 0.013(3)
C53 0.030(3) 0.022(3) 0.027(3) 0.008(2) 0.004(3) 0.003(2)
C54 0.031(3) 0.030(3) 0.038(3) 0.019(3) 0.006(3) 0.011(3)
C55 0.027(3) 0.027(3) 0.042(4) 0.012(3) 0.010(3) 0.015(2)
C61 0.023(3) 0.024(3) 0.030(3) 0.010(2) 0.004(3) 0.007(2)
C63 0.025(3) 0.030(3) 0.034(3) 0.011(3) 0.008(3) 0.001(2)
C64 0.025(3) 0.046(4) 0.044(4) 0.017(3) 0.012(3) 0.002(3)
C65 0.035(4) 0.045(4) 0.045(4) 0.026(3) 0.012(3) 0.002(3)
C66 0.030(3) 0.043(4) 0.037(4) 0.023(3) 0.005(3) 0.008(3)
C67 0.027(3) 0.044(4) 0.052(4) 0.024(3) 0.020(3) 0.010(3)
B1 0.020(3) 0.022(3) 0.034(4) 0.001(3) 0.013(3) 0.005(3)
P1 0.0239(8) 0.0243(7) 0.0286(8) 0.0057(6) 0.0075(7) 0.0057(6)
F1 0.035(2) 0.056(2) 0.079(3) 0.047(2) 0.014(2) 0.009(2)
F2 0.033(2) 0.074(3) 0.030(2) 0.003(2) -0.003(2) -0.006(2)
F3 0.029(2) 0.045(2) 0.042(2) 0.000(2) 0.013(2) 0.008(2)
F4 0.045(2) 0.028(2) 0.032(2) -0.0045(14) 0.006(2) -0.001(2)
F5 0.034(2) 0.040(2) 0.068(3) 0.015(2) 0.029(2) 0.008(2)
F6 0.045(2) 0.025(2) 0.053(2) 0.011(2) 0.008(2) 0.002(2)
C1 0.049(5) 0.054(5) 0.072(6) 0.006(4) 0.017(4) 0.001(4)
Cl1 0.291(20) 0.133(11) 0.154(13) -0.002(9) 0.134(12) 0.064(11)
Cl2 0.171(20) 0.488(35) 0.381(33) -0.017(29) -0.095(21) 0.040(23)
Cl1' 0.212(8) 0.186(7) 0.191(8) 0.010(6) 0.033(6) -0.031(6)
Cl2' 0.286(10) 0.181(6) 0.216(8) 0.074(6) 0.139(8) 0.109(7)
C2 0.182(14) 0.104(9) 0.080(8) 0.016(7) 0.038(9) 0.014(9)
C3 0.136(14) 0.208(17) 0.149(14) 0.137(13) 0.112(12) 0.101(12)
C4 0.136(11) 0.073(7) 0.087(8) 0.033(6) 0.047(8) 0.020(7)
C5 0.121(10) 0.048(5) 0.030(4) 0.011(4) -0.026(5) -0.048(5)
C6 0.197(17) 0.270(20) 0.047(7) -0.027(10) 0.017(9) -0.174(16)

_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 N52 1.898(4) . ?
Cu1 O1 1.901(4) . ?
Cu1 N32 2.171(4) . ?
Cu1 N12 2.212(4) . ?
Cu1 N62 2.212(4) . ?
N11 C15 1.347(6) . ?
N11 N12 1.365(5) . ?
N11 B1 1.558(7) . ?
N12 C13 1.354(6) . ?
N22 C23 1.339(6) . ?
N22 C21 1.361(7) . ?
N31 C35 1.333(7) . ?
N31 N32 1.371(6) . ?
N31 B1 1.537(8) . ?
N32 C33 1.346(7) . ?
N42 C43 1.343(7) . ?
N42 C41 1.350(7) . ?
N51 N52 1.338(6) . ?
N51 C55 1.348(6) . ?
N51 B1 1.539(7) . ?
N52 C53 1.333(7) . ?
N62 C63 1.350(7) . ?
N62 C61 1.370(6) . ?
C13 C14 1.391(7) . ?
C13 C21 1.467(7) . ?
C14 C15 1.371(7) . ?
C21 C26 1.387(7) . ?
C23 C24 1.390(8) . ?
C23 C27 1.511(8) . ?
C24 C25 1.370(8) . ?
C25 C26 1.384(8) . ?
C33 C34 1.406(8) . ?
C33 C41 1.478(8) . ?
C34 C35 1.376(8) . ?
C41 C46 1.382(8) . ?
C43 C44 1.376(8) . ?
C43 C47 1.510(8) . ?
C44 C45 1.357(9) . ?
C45 C46 1.386(9) . ?
C53 C54 1.390(7) . ?
C53 C61 1.468(7) . ?
C54 C55 1.384(8) . ?
C61 C66 1.369(8) . ?
C63 C64 1.387(8) . ?
C63 C67 1.502(7) . ?
C64 C65 1.384(8) . ?
C65 C66 1.386(8) . ?
P1 F1 1.592(3) . ?
P1 F4 1.598(3) . ?
P1 F6 1.599(3) . ?
P1 F5 1.601(3) . ?
P1 F3 1.601(3) . ?
P1 F2 1.602(4) . ?
C1 Cl1 1.64(2) . ?
C1 Cl2 1.69(2) . ?
C1 Cl1' 1.703(10) . ?
C1 Cl2' 1.734(10) . ?
Cl1 Cl1 1.17(2) 2_846 ?
C2 C3 1.51(2) . ?
C2 C2 1.77(3) 2_757 ?
C2 C5 1.90(2) . ?
C3 C5 0.89(2) . ?
C3 C4 1.69(2) . ?
C4 C6 1.14(2) . ?

loop_
 _geom_angle_atom_site_label_1
 _geom_angle_atom_site_label_2
 _geom_angle_atom_site_label_3
 _geom_angle
 _geom_angle_site_symmetry_1
 _geom_angle_site_symmetry_3
 _geom_angle_publ_flag
N52 Cu1 O1 177.2(2) . . ?
N52 Cu1 N32 88.4(2) . . ?
O1 Cu1 N32 94.4(2) . . ?
N52 Cu1 N12 87.0(2) . . ?
O1 Cu1 N12 93.6(2) . . ?
N32 Cu1 N12 86.1(2) . . ?
N52 Cu1 N62 76.9(2) . . ?
O1 Cu1 N62 100.8(2) . . ?
N32 Cu1 N62 135.2(2) . . ?
N12 Cu1 N62 133.9(2) . . ?
C15 N11 N12 109.9(4) . . ?
C15 N11 B1 127.6(4) . . ?
N12 N11 B1 122.5(4) . . ?
C13 N12 N11 106.3(4) . . ?
C13 N12 Cu1 141.2(3) . . ?
N11 N12 Cu1 112.4(3) . . ?
C23 N22 C21 118.9(5) . . ?
C35 N31 N32 110.0(4) . . ?
C35 N31 B1 127.9(5) . . ?
N32 N31 B1 122.0(4) . . ?
C33 N32 N31 106.3(4) . . ?
C33 N32 Cu1 138.9(4) . . ?
N31 N32 Cu1 113.3(3) . . ?
C43 N42 C41 118.3(5) . . ?
N52 N51 C55 108.4(4) . . ?
N52 N51 B1 114.5(4) . . ?
C55 N51 B1 137.1(5) . . ?
C53 N52 N51 109.1(4) . . ?
C53 N52 Cu1 123.4(4) . . ?
N51 N52 Cu1 127.4(3) . . ?
C63 N62 C61 117.2(4) . . ?
C63 N62 Cu1 131.2(3) . . ?
C61 N62 Cu1 111.6(3) . . ?
N12 C13 C14 109.6(4) . . ?
N12 C13 C21 123.6(5) . . ?
C14 C13 C21 126.8(5) . . ?
C15 C14 C13 105.8(5) . . ?
N11 C15 C14 108.4(5) . . ?
N22 C21 C26 121.3(5) . . ?
N22 C21 C13 119.2(4) . . ?
C26 C21 C13 119.5(5) . . ?
N22 C23 C24 122.0(5) . . ?
N22 C23 C27 116.6(5) . . ?
C24 C23 C27 121.4(5) . . ?
C25 C24 C23 119.3(5) . . ?
C24 C25 C26 119.4(5) . . ?
C25 C26 C21 119.2(5) . . ?
N32 C33 C34 109.7(5) . . ?
N32 C33 C41 123.3(5) . . ?
C34 C33 C41 127.0(5) . . ?
C35 C34 C33 105.0(5) . . ?
N31 C35 C34 109.0(5) . . ?
N42 C41 C46 122.0(5) . . ?
N42 C41 C33 118.2(5) . . ?
C46 C41 C33 119.7(5) . . ?
N42 C43 C44 122.2(6) . . ?
N42 C43 C47 115.9(5) . . ?
C44 C43 C47 121.9(5) . . ?
C45 C44 C43 119.6(6) . . ?
C44 C45 C46 119.4(6) . . ?
C41 C46 C45 118.6(6) . . ?
N52 C53 C54 108.8(5) . . ?
N52 C53 C61 114.6(4) . . ?
C54 C53 C61 136.6(5) . . ?
C55 C54 C53 105.0(5) . . ?
N51 C55 C54 108.6(5) . . ?
C66 C61 N62 123.5(5) . . ?
C66 C61 C53 123.2(5) . . ?
N62 C61 C53 113.4(4) . . ?
N62 C63 C64 121.7(5) . . ?
N62 C63 C67 118.8(5) . . ?
C64 C63 C67 119.5(5) . . ?
C65 C64 C63 120.4(5) . . ?
C64 C65 C66 118.2(5) . . ?
C61 C66 C65 119.0(5) . . ?
N31 B1 N51 108.7(4) . . ?
N31 B1 N11 109.3(4) . . ?
N51 B1 N11 107.6(4) . . ?
F1 P1 F4 89.7(2) . . ?
F1 P1 F6 179.5(2) . . ?
F4 P1 F6 89.9(2) . . ?
F1 P1 F5 89.9(2) . . ?
F4 P1 F5 90.6(2) . . ?
F6 P1 F5 89.8(2) . . ?
F1 P1 F3 90.3(2) . . ?
F4 P1 F3 89.3(2) . . ?
F6 P1 F3 90.0(2) . . ?
F5 P1 F3 179.8(2) . . ?
F1 P1 F2 91.2(2) . . ?
F4 P1 F2 179.1(2) . . ?
F6 P1 F2 89.2(2) . . ?
F5 P1 F2 89.6(2) . . ?
F3 P1 F2 90.5(2) . . ?
Cl1 C1 Cl2 106.5(9) . . ?
Cl1' C1 Cl2' 104.6(6) . . ?
Cl1 Cl1 C1 124.1(20) 2_846 . ?
C3 C2 C2 108.4(12) . 2_757 ?
C3 C2 C5 27.4(8) . . ?
C2 C2 C5 81.4(8) 2_757 . ?
C5 C3 C2 101.8(17) . . ?
C5 C3 C4 154.2(20) . . ?
C2 C3 C4 104.0(14) . . ?
C6 C4 C3 91.5(14) . . ?
C3 C5 C2 50.9(13) . . ?

_refine_diff_density_max    0.639
_refine_diff_density_min   -0.899
_refine_diff_density_rms    0.100
#=END