# Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2004


data_global
_journal_name_full               Chem.Commun.

_journal_coden_Cambridge         0182

_publ_contact_author_name        'Prof Gabor Speier'
_publ_contact_author_address     
;
Department of Organic Chemistry
University of Veszprem
Wartha V. u. 1
Veszprem
8200
HUNGARY
;

_publ_contact_author_email       SPEIER@ALMOS.VEIN.HU

_publ_section_title              
;
Facile copper-mediated activation of the N?H bond
and the oxidative cleavage of the C2?C3 bond in
1H-2-phenyl-3-hydroxy-4-oxoquinoline
;
loop_
_publ_author_name
'Gabor Speier'
'Miklos Czaun'
'Laszlo Parkanyi'

data_cm316
_database_code_depnum_ccdc_archive 'CCDC 222925'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C104 H92 Cu3 N4 O6 P4'
_chemical_formula_weight         1856.36

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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'

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

_cell_length_a                   40.058(4)
_cell_length_b                   10.251(2)
_cell_length_c                   27.769(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 125.64(1)
_cell_angle_gamma                90.00
_cell_volume                     9267(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    25
_cell_measurement_theta_min      14.96
_cell_measurement_theta_max      15.94

_exptl_crystal_description       prism
_exptl_crystal_colour            ?
_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    1.331
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3852
_exptl_absorpt_coefficient_mu    0.809
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_correction_T_min  0.9720
_exptl_absorpt_correction_T_max  0.9822
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71070
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Enraf-Nonius CAD4'
_diffrn_measurement_method       \w--2\q
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         3
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  60
_diffrn_standards_decay_%        6
_diffrn_reflns_number            13945
_diffrn_reflns_av_R_equivalents  0.0136
_diffrn_reflns_av_sigmaI/netI    0.0850
_diffrn_reflns_limit_h_min       -56
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_theta_min         2.41
_diffrn_reflns_theta_max         29.95
_reflns_number_total             13366
_reflns_number_gt                6940
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CAD4 Express'
_computing_cell_refinement       'CAD4 Express'
_computing_data_reduction        'XCAD4 (Harms 1996)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F^2^ against ALL reflections.  The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement.  R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0531P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         13366
_refine_ls_number_parameters     587
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.1095
_refine_ls_R_factor_gt           0.0379
_refine_ls_wR_factor_ref         0.0935
_refine_ls_wR_factor_gt          0.0834
_refine_ls_goodness_of_fit_ref   0.859
_refine_ls_restrained_S_all      0.860
_refine_ls_shift/su_max          0.139
_refine_ls_shift/su_mean         0.005

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 0.125646(7) 0.41387(2) 0.238925(9) 0.03515(7) Uani 1 1 d . . .
Cu2 Cu 0.2500 0.7500 0.5000 0.04524(10) Uani 1 2 d S . .
P1 P 0.150786(15) 0.20796(5) 0.26950(2) 0.03689(12) Uani 1 1 d . . .
P2 P 0.073268(15) 0.44749(5) 0.14318(2) 0.03715(12) Uani 1 1 d . . .
O1 O 0.20430(4) 0.63753(14) 0.44836(6) 0.0486(4) Uani 1 1 d . . .
O2 O 0.25163(4) 0.78223(14) 0.43297(6) 0.0511(4) Uani 1 1 d . . .
N1 N 0.15961(4) 0.56327(15) 0.29300(6) 0.0349(3) Uani 1 1 d . . .
C1 C 0.19735(5) 0.63598(19) 0.39532(8) 0.0379(4) Uani 1 1 d . . .
C2 C 0.22294(6) 0.71293(19) 0.38779(8) 0.0400(4) Uani 1 1 d . . .
C3 C 0.21648(5) 0.71663(18) 0.33196(8) 0.0385(4) Uani 1 1 d . . .
C4 C 0.18493(5) 0.63585(18) 0.28612(8) 0.0368(4) Uani 1 1 d . . .
C5 C 0.16479(5) 0.56764(18) 0.34603(7) 0.0363(4) Uani 1 1 d . . .
C6 C 0.23967(6) 0.7963(2) 0.32030(10) 0.0503(5) Uani 1 1 d . . .
H6 H 0.2598 0.8506 0.3499 0.065 Uiso 1 1 calc R . .
C7 C 0.23307(7) 0.7950(2) 0.26647(11) 0.0598(6) Uani 1 1 d . . .
H7 H 0.2482 0.8494 0.2592 0.078 Uiso 1 1 calc R . .
C8 C 0.20336(7) 0.7114(3) 0.22200(10) 0.0641(7) Uani 1 1 d . . .
H8 H 0.1995 0.7091 0.1856 0.083 Uiso 1 1 calc R . .
C9 C 0.18018(7) 0.6339(2) 0.23132(9) 0.0519(5) Uani 1 1 d . . .
H9 H 0.1609 0.5785 0.2013 0.067 Uiso 1 1 calc R . .
C10 C 0.13197(6) 0.50645(19) 0.34747(8) 0.0395(4) Uani 1 1 d . . .
C11 C 0.09125(6) 0.5204(2) 0.29845(10) 0.0508(5) Uani 1 1 d . . .
H11 H 0.0857 0.5632 0.2650 0.066 Uiso 1 1 calc R . .
C12 C 0.05927(8) 0.4728(3) 0.29832(15) 0.0755(8) Uani 1 1 d . . .
H12 H 0.0324 0.4834 0.2650 0.098 Uiso 1 1 calc R . .
C13 C 0.06654(10) 0.4100(3) 0.34671(16) 0.0868(10) Uani 1 1 d . . .
H13 H 0.0447 0.3793 0.3468 0.113 Uiso 1 1 calc R . .
C14 C 0.10628(10) 0.3922(3) 0.39546(13) 0.0851(10) Uani 1 1 d . . .
H14 H 0.1113 0.3475 0.4282 0.111 Uiso 1 1 calc R . .
C15 C 0.13901(8) 0.4402(2) 0.39632(10) 0.0643(7) Uani 1 1 d . . .
H15 H 0.1658 0.4281 0.4297 0.084 Uiso 1 1 calc R . .
C16 C 0.20381(6) 0.20446(19) 0.33584(8) 0.0403(4) Uani 1 1 d . . .
C17 C 0.22772(6) 0.3143(2) 0.34772(10) 0.0548(6) Uani 1 1 d . . .
H17 H 0.2167 0.3849 0.3219 0.071 Uiso 1 1 calc R . .
C18 C 0.26769(7) 0.3193(3) 0.39759(11) 0.0694(7) Uani 1 1 d . . .
H18 H 0.2835 0.3932 0.4051 0.090 Uiso 1 1 calc R . .
C19 C 0.28420(7) 0.2160(3) 0.43610(11) 0.0741(8) Uani 1 1 d . . .
H19 H 0.3110 0.2206 0.4700 0.096 Uiso 1 1 calc R . .
C20 C 0.26138(7) 0.1063(3) 0.42484(11) 0.0748(8) Uani 1 1 d . . .
H20 H 0.2727 0.0360 0.4509 0.097 Uiso 1 1 calc R . .
C21 C 0.22133(7) 0.1001(2) 0.37452(10) 0.0583(6) Uani 1 1 d . . .
H21 H 0.2060 0.0248 0.3666 0.076 Uiso 1 1 calc R . .
C22 C 0.12219(6) 0.09709(19) 0.28438(8) 0.0421(5) Uani 1 1 d . . .
C23 C 0.12778(7) -0.0383(2) 0.28758(10) 0.0555(6) Uani 1 1 d . . .
H23 H 0.1463 -0.0742 0.2814 0.072 Uiso 1 1 calc R . .
C24 C 0.10611(9) -0.1182(3) 0.29970(12) 0.0767(8) Uani 1 1 d . . .
H24 H 0.1107 -0.2077 0.3030 0.100 Uiso 1 1 calc R . .
C25 C 0.07769(10) -0.0666(3) 0.30699(13) 0.0850(9) Uani 1 1 d . . .
H25 H 0.0626 -0.1214 0.3143 0.111 Uiso 1 1 calc R . .
C26 C 0.07146(9) 0.0667(3) 0.30346(13) 0.0790(8) Uani 1 1 d . . .
H26 H 0.0522 0.1021 0.3083 0.103 Uiso 1 1 calc R . .
C27 C 0.09425(7) 0.1474(2) 0.29258(10) 0.0563(6) Uani 1 1 d . . .
H27 H 0.0904 0.2372 0.2908 0.073 Uiso 1 1 calc R . .
C28 C 0.15185(6) 0.11838(19) 0.21337(8) 0.0445(5) Uani 1 1 d . . .
C29 C 0.11543(7) 0.0644(2) 0.16543(10) 0.0592(6) Uani 1 1 d . . .
H29 H 0.0916 0.0687 0.1638 0.077 Uiso 1 1 calc R . .
C30 C 0.11480(9) 0.0043(3) 0.12020(11) 0.0768(8) Uani 1 1 d . . .
H30 H 0.0906 -0.0331 0.0886 0.100 Uiso 1 1 calc R . .
C31 C 0.14929(10) -0.0003(3) 0.12169(12) 0.0840(9) Uani 1 1 d . . .
H31 H 0.1486 -0.0413 0.0913 0.109 Uiso 1 1 calc R . .
C32 C 0.18520(9) 0.0554(3) 0.16796(13) 0.0807(8) Uani 1 1 d . . .
H32 H 0.2085 0.0542 0.1682 0.105 Uiso 1 1 calc R . .
C33 C 0.18652(7) 0.1132(2) 0.21406(11) 0.0601(6) Uani 1 1 d . . .
H33 H 0.2110 0.1488 0.2458 0.078 Uiso 1 1 calc R . .
C34 C 0.03792(5) 0.31211(19) 0.10527(8) 0.0375(4) Uani 1 1 d . . .
C35 C 0.02168(6) 0.2525(2) 0.13227(9) 0.0480(5) Uani 1 1 d . . .
H35 H 0.0301 0.2796 0.1697 0.062 Uiso 1 1 calc R . .
C36 C -0.00677(7) 0.1537(2) 0.10416(11) 0.0593(6) Uani 1 1 d . . .
H36 H -0.0178 0.1154 0.1224 0.077 Uiso 1 1 calc R . .
C37 C -0.01884(7) 0.1118(2) 0.04931(11) 0.0590(6) Uani 1 1 d . . .
H37 H -0.0381 0.0453 0.0303 0.077 Uiso 1 1 calc R . .
C38 C -0.00269(7) 0.1674(2) 0.02259(9) 0.0540(6) Uani 1 1 d . . .
H38 H -0.0105 0.1369 -0.0142 0.070 Uiso 1 1 calc R . .
C39 C 0.02532(6) 0.2689(2) 0.04963(8) 0.0462(5) Uani 1 1 d . . .
H39 H 0.0356 0.3080 0.0306 0.060 Uiso 1 1 calc R . .
C40 C 0.03911(6) 0.58392(19) 0.12784(8) 0.0409(4) Uani 1 1 d . . .
C41 C 0.05586(7) 0.7025(2) 0.15542(10) 0.0583(6) Uani 1 1 d . . .
H41 H 0.0842 0.7129 0.1795 0.076 Uiso 1 1 calc R . .
C42 C 0.03094(9) 0.8056(2) 0.14765(11) 0.0697(7) Uani 1 1 d . . .
H42 H 0.0426 0.8849 0.1663 0.091 Uiso 1 1 calc R . .
C43 C -0.01133(9) 0.7916(3) 0.11230(12) 0.0717(7) Uani 1 1 d . . .
H43 H -0.0281 0.8606 0.1073 0.093 Uiso 1 1 calc R . .
C44 C -0.02811(8) 0.6740(3) 0.08469(13) 0.0722(7) Uani 1 1 d . . .
H44 H -0.0565 0.6640 0.0607 0.094 Uiso 1 1 calc R . .
C45 C -0.00341(7) 0.5708(2) 0.09217(10) 0.0570(6) Uani 1 1 d . . .
H45 H -0.0153 0.4919 0.0732 0.074 Uiso 1 1 calc R . .
C46 C 0.09370(6) 0.4781(2) 0.10033(8) 0.0432(5) Uani 1 1 d . . .
C47 C 0.08384(7) 0.5857(2) 0.06445(10) 0.0586(6) Uani 1 1 d . . .
H47 H 0.0646 0.6457 0.0595 0.076 Uiso 1 1 calc R . .
C48 C 0.10257(9) 0.6043(3) 0.03588(13) 0.0808(8) Uani 1 1 d . . .
H48 H 0.0958 0.6768 0.0117 0.105 Uiso 1 1 calc R . .
C49 C 0.13076(9) 0.5174(4) 0.04283(12) 0.0820(9) Uani 1 1 d . . .
H49 H 0.1433 0.5311 0.0237 0.107 Uiso 1 1 calc R . .
C50 C 0.14077(8) 0.4091(3) 0.07814(11) 0.0696(7) Uani 1 1 d . . .
H50 H 0.1598 0.3491 0.0825 0.090 Uiso 1 1 calc R . .
C51 C 0.12251(7) 0.3898(2) 0.10697(10) 0.0559(6) Uani 1 1 d . . .
H51 H 0.1295 0.3170 0.1311 0.073 Uiso 1 1 calc R . .
N1S N 0.35071(9) 0.5511(3) 0.53309(11) 0.1044(10) Uani 1 1 d D . .
C1S C 0.35279(14) 0.6872(4) 0.5218(2) 0.186(3) Uani 1 1 d D A .
H1S1 H 0.3598 0.7379 0.5556 0.260 Uiso 1 1 calc R . .
H1S2 H 0.3266 0.7150 0.4877 0.260 Uiso 1 1 calc R . .
H1S3 H 0.3734 0.6992 0.5148 0.260 Uiso 1 1 calc R . .
C2S C 0.32003(12) 0.5155(4) 0.54266(17) 0.1187(12) Uani 1 1 d D A .
H2S1 H 0.2932 0.5215 0.5059 0.166 Uiso 1 1 calc R . .
H2S2 H 0.3217 0.5736 0.5711 0.166 Uiso 1 1 calc R . .
H2S3 H 0.3248 0.4276 0.5573 0.166 Uiso 1 1 calc R . .
C3S C 0.3747(2) 0.4416(7) 0.5452(3) 0.107(3) Uani 0.656(12) 1 d PD A .
H3S H 0.3688 0.3630 0.5554 0.139 Uiso 0.656(12) 1 calc PR . .
O1S O 0.4012(2) 0.4498(13) 0.5425(5) 0.214(5) Uani 0.656(12) 1 d PD . .
C3SX C 0.3804(3) 0.5077(9) 0.5256(4) 0.070(4) Uani 0.344(12) 1 d PD A 1
H3SX H 0.3976 0.5672 0.5248 0.090 Uiso 0.344(12) 1 calc PR A 1
O1SX O 0.3834(6) 0.4023(9) 0.5205(6) 0.125(5) Uani 0.344(12) 1 d PD A 1

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 0.03580(12) 0.03265(12) 0.02521(10) -0.00369(9) 0.01109(9) -0.00462(10)
Cu2 0.04038(19) 0.0463(2) 0.03228(17) -0.01569(15) 0.01164(15) -0.01300(16)
P1 0.0375(3) 0.0316(3) 0.0309(2) -0.00112(19) 0.0138(2) -0.0008(2)
P2 0.0370(3) 0.0355(3) 0.0246(2) -0.00104(19) 0.0098(2) -0.0035(2)
O1 0.0496(8) 0.0553(9) 0.0318(7) -0.0173(6) 0.0185(6) -0.0192(7)
O2 0.0476(8) 0.0532(9) 0.0368(7) -0.0181(7) 0.0157(6) -0.0233(7)
N1 0.0343(8) 0.0339(8) 0.0269(7) -0.0054(6) 0.0124(6) -0.0056(6)
C1 0.0347(9) 0.0381(10) 0.0297(9) -0.0078(8) 0.0125(8) -0.0049(8)
C2 0.0332(9) 0.0358(10) 0.0354(9) -0.0080(8) 0.0111(8) -0.0056(8)
C3 0.0324(9) 0.0349(10) 0.0380(10) -0.0038(8) 0.0147(8) -0.0031(8)
C4 0.0356(10) 0.0360(10) 0.0320(9) -0.0029(8) 0.0159(8) -0.0039(8)
C5 0.0335(9) 0.0333(10) 0.0284(8) -0.0057(7) 0.0103(8) -0.0037(8)
C6 0.0452(12) 0.0469(12) 0.0530(12) -0.0072(10) 0.0252(10) -0.0126(10)
C7 0.0603(14) 0.0618(15) 0.0636(14) -0.0003(12) 0.0396(13) -0.0151(12)
C8 0.0654(15) 0.0822(18) 0.0467(12) -0.0031(12) 0.0339(12) -0.0184(14)
C9 0.0513(12) 0.0580(14) 0.0369(10) -0.0078(10) 0.0204(10) -0.0155(11)
C10 0.0416(10) 0.0376(10) 0.0343(10) -0.0125(8) 0.0192(9) -0.0097(9)
C11 0.0386(11) 0.0489(13) 0.0598(13) -0.0052(11) 0.0258(11) -0.0031(10)
C12 0.0531(15) 0.0762(19) 0.104(2) -0.0103(17) 0.0494(16) -0.0069(13)
C13 0.086(2) 0.094(2) 0.119(3) -0.039(2) 0.082(2) -0.0399(18)
C14 0.120(3) 0.094(2) 0.0674(17) -0.0305(16) 0.0694(19) -0.054(2)
C15 0.0721(16) 0.0721(17) 0.0379(11) -0.0134(11) 0.0259(12) -0.0318(13)
C16 0.0402(10) 0.0363(10) 0.0345(9) -0.0015(8) 0.0161(8) 0.0013(9)
C17 0.0441(12) 0.0453(13) 0.0554(13) 0.0059(10) 0.0179(10) -0.0030(10)
C18 0.0438(13) 0.0552(15) 0.0763(17) -0.0003(13) 0.0164(12) -0.0105(11)
C19 0.0430(13) 0.0657(17) 0.0619(15) 0.0009(13) 0.0012(11) 0.0012(12)
C20 0.0558(14) 0.0575(16) 0.0574(15) 0.0144(12) 0.0026(12) 0.0043(12)
C21 0.0497(12) 0.0441(13) 0.0500(12) 0.0068(10) 0.0115(10) -0.0047(10)
C22 0.0440(11) 0.0364(11) 0.0340(9) -0.0016(8) 0.0160(9) -0.0044(9)
C23 0.0553(13) 0.0412(12) 0.0545(13) 0.0012(10) 0.0232(11) -0.0036(10)
C24 0.089(2) 0.0467(15) 0.0721(18) 0.0013(12) 0.0344(16) -0.0226(14)
C25 0.097(2) 0.076(2) 0.083(2) 0.0008(16) 0.0533(19) -0.0357(18)
C26 0.0839(19) 0.088(2) 0.087(2) -0.0014(17) 0.0624(18) -0.0136(16)
C27 0.0629(14) 0.0532(14) 0.0549(13) -0.0005(11) 0.0356(12) -0.0028(12)
C28 0.0532(12) 0.0358(11) 0.0350(10) -0.0010(8) 0.0202(9) 0.0020(9)
C29 0.0589(14) 0.0572(15) 0.0428(12) -0.0102(11) 0.0190(11) -0.0014(11)
C30 0.0816(19) 0.0789(19) 0.0496(14) -0.0229(13) 0.0268(14) -0.0037(16)
C31 0.109(2) 0.086(2) 0.0613(17) -0.0178(15) 0.0520(18) 0.0103(19)
C32 0.087(2) 0.097(2) 0.0761(18) -0.0103(17) 0.0580(17) 0.0070(17)
C33 0.0588(14) 0.0668(16) 0.0527(13) -0.0066(11) 0.0313(12) 0.0033(12)
C34 0.0359(10) 0.0352(10) 0.0290(9) -0.0019(8) 0.0117(8) -0.0012(8)
C35 0.0533(12) 0.0453(12) 0.0409(10) -0.0047(9) 0.0249(10) -0.0052(10)
C36 0.0639(15) 0.0510(14) 0.0662(15) -0.0037(12) 0.0397(13) -0.0128(12)
C37 0.0536(13) 0.0444(13) 0.0584(14) -0.0133(11) 0.0209(12) -0.0153(10)
C38 0.0557(13) 0.0507(13) 0.0386(11) -0.0142(10) 0.0178(10) -0.0100(11)
C39 0.0481(12) 0.0438(12) 0.0313(9) -0.0027(9) 0.0144(9) -0.0053(9)
C40 0.0456(11) 0.0380(10) 0.0302(9) 0.0024(8) 0.0170(8) 0.0013(9)
C41 0.0567(13) 0.0445(13) 0.0492(12) -0.0034(10) 0.0169(11) -0.0027(11)
C42 0.0830(19) 0.0409(13) 0.0642(15) -0.0070(12) 0.0310(15) 0.0023(13)
C43 0.084(2) 0.0502(15) 0.0805(18) 0.0092(14) 0.0479(16) 0.0171(14)
C44 0.0563(15) 0.0624(17) 0.0841(18) -0.0006(15) 0.0331(14) 0.0061(13)
C45 0.0518(12) 0.0453(13) 0.0574(13) -0.0032(11) 0.0225(11) 0.0010(10)
C46 0.0388(10) 0.0486(12) 0.0275(9) -0.0025(8) 0.0111(8) -0.0080(9)
C47 0.0593(14) 0.0635(15) 0.0469(12) 0.0111(11) 0.0275(11) 0.0016(12)
C48 0.088(2) 0.087(2) 0.0754(18) 0.0273(16) 0.0521(17) -0.0013(17)
C49 0.0704(18) 0.115(3) 0.0724(18) 0.0140(18) 0.0485(16) -0.0096(18)
C50 0.0556(14) 0.096(2) 0.0596(14) 0.0059(15) 0.0347(13) 0.0080(14)
C51 0.0549(13) 0.0625(15) 0.0454(12) 0.0101(11) 0.0264(11) 0.0077(11)
N1S 0.102(2) 0.138(3) 0.0649(15) 0.0087(16) 0.0441(15) 0.057(2)
C1S 0.151(4) 0.204(6) 0.255(6) 0.144(5) 0.148(5) 0.082(4)
C2S 0.150(3) 0.091(3) 0.104(3) -0.002(2) 0.068(3) 0.000(3)
C3S 0.082(4) 0.146(7) 0.067(4) 0.033(4) 0.029(3) 0.053(4)
O1S 0.120(5) 0.382(13) 0.144(8) 0.076(7) 0.080(6) 0.138(6)
C3SX 0.078(7) 0.062(6) 0.052(5) 0.004(4) 0.029(5) 0.017(5)
O1SX 0.173(13) 0.148(9) 0.108(9) 0.025(6) 0.112(10) 0.081(7)

_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 N1 2.0176(14) . ?
Cu1 P2 2.2559(6) . ?
Cu1 P1 2.2791(7) . ?
Cu2 O1 1.9177(13) . ?
Cu2 O1 1.9177(13) 7_566 ?
Cu2 O2 1.9286(14) . ?
Cu2 O2 1.9286(14) 7_566 ?
P1 C22 1.824(2) . ?
P1 C16 1.8295(19) . ?
P1 C28 1.831(2) . ?
P2 C34 1.8172(19) . ?
P2 C46 1.822(2) . ?
P2 C40 1.825(2) . ?
O1 C1 1.330(2) . ?
O2 C2 1.311(2) . ?
N1 C4 1.358(2) . ?
N1 C5 1.363(2) . ?
C1 C2 1.402(3) . ?
C1 C5 1.409(2) . ?
C2 C3 1.416(3) . ?
C3 C6 1.409(3) . ?
C3 C4 1.424(2) . ?
C4 C9 1.419(3) . ?
C5 C10 1.478(3) . ?
C6 C7 1.358(3) . ?
C7 C8 1.401(3) . ?
C8 C9 1.357(3) . ?
C10 C15 1.391(3) . ?
C10 C11 1.395(3) . ?
C11 C12 1.369(3) . ?
C12 C13 1.360(4) . ?
C13 C14 1.374(4) . ?
C14 C15 1.388(4) . ?
C16 C21 1.383(3) . ?
C16 C17 1.387(3) . ?
C17 C18 1.378(3) . ?
C18 C19 1.371(3) . ?
C19 C20 1.365(3) . ?
C20 C21 1.385(3) . ?
C22 C27 1.366(3) . ?
C22 C23 1.400(3) . ?
C23 C24 1.371(3) . ?
C24 C25 1.373(4) . ?
C25 C26 1.382(4) . ?
C26 C27 1.389(3) . ?
C28 C33 1.379(3) . ?
C28 C29 1.394(3) . ?
C29 C30 1.386(3) . ?
C30 C31 1.359(4) . ?
C31 C32 1.376(4) . ?
C32 C33 1.383(3) . ?
C34 C35 1.388(3) . ?
C34 C39 1.389(2) . ?
C35 C36 1.377(3) . ?
C36 C37 1.371(3) . ?
C37 C38 1.361(3) . ?
C38 C39 1.387(3) . ?
C40 C41 1.384(3) . ?
C40 C45 1.391(3) . ?
C41 C42 1.382(3) . ?
C42 C43 1.384(4) . ?
C43 C44 1.376(4) . ?
C44 C45 1.379(3) . ?
C46 C47 1.381(3) . ?
C46 C51 1.392(3) . ?
C47 C48 1.387(3) . ?
C48 C49 1.361(4) . ?
C49 C50 1.377(4) . ?
C50 C51 1.377(3) . ?
N1S C3S 1.386(5) . ?
N1S C3SX 1.395(5) . ?
N1S C1S 1.443(3) . ?
N1S C2S 1.447(3) . ?
C3S O1S 1.108(3) . ?
O1S O1SX 0.782(17) . ?
C3SX O1SX 1.105(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Cu1 P2 121.46(5) . . ?
N1 Cu1 P1 117.76(5) . . ?
P2 Cu1 P1 119.09(2) . . ?
O1 Cu2 O1 179.995(1) . 7_566 ?
O1 Cu2 O2 86.31(6) . . ?
O1 Cu2 O2 93.68(6) 7_566 . ?
O1 Cu2 O2 93.69(6) . 7_566 ?
O1 Cu2 O2 86.31(6) 7_566 7_566 ?
O2 Cu2 O2 180.00(8) . 7_566 ?
C22 P1 C16 105.88(9) . . ?
C22 P1 C28 102.11(10) . . ?
C16 P1 C28 104.96(9) . . ?
C22 P1 Cu1 117.51(7) . . ?
C16 P1 Cu1 113.27(7) . . ?
C28 P1 Cu1 111.83(7) . . ?
C34 P2 C46 104.36(9) . . ?
C34 P2 C40 103.00(9) . . ?
C46 P2 C40 106.07(9) . . ?
C34 P2 Cu1 116.22(6) . . ?
C46 P2 Cu1 109.44(6) . . ?
C40 P2 Cu1 116.63(6) . . ?
C1 O1 Cu2 109.14(12) . . ?
C2 O2 Cu2 109.09(13) . . ?
C4 N1 C5 118.56(15) . . ?
C4 N1 Cu1 123.10(12) . . ?
C5 N1 Cu1 116.18(12) . . ?
O1 C1 C2 117.31(16) . . ?
O1 C1 C5 124.04(17) . . ?
C2 C1 C5 118.56(17) . . ?
O2 C2 C1 118.12(17) . . ?
O2 C2 C3 122.16(18) . . ?
C1 C2 C3 119.70(16) . . ?
C6 C3 C2 122.88(17) . . ?
C6 C3 C4 119.49(17) . . ?
C2 C3 C4 117.64(17) . . ?
N1 C4 C9 119.90(16) . . ?
N1 C4 C3 122.63(16) . . ?
C9 C4 C3 117.47(17) . . ?
N1 C5 C1 122.54(17) . . ?
N1 C5 C10 115.94(15) . . ?
C1 C5 C10 121.28(16) . . ?
C7 C6 C3 121.04(19) . . ?
C6 C7 C8 119.8(2) . . ?
C9 C8 C7 121.0(2) . . ?
C8 C9 C4 121.1(2) . . ?
C15 C10 C11 117.3(2) . . ?
C15 C10 C5 123.74(18) . . ?
C11 C10 C5 118.86(18) . . ?
C12 C11 C10 121.7(2) . . ?
C13 C12 C11 120.3(3) . . ?
C12 C13 C14 119.6(2) . . ?
C13 C14 C15 120.7(3) . . ?
C14 C15 C10 120.3(2) . . ?
C21 C16 C17 118.39(18) . . ?
C21 C16 P1 124.28(16) . . ?
C17 C16 P1 117.33(15) . . ?
C18 C17 C16 120.4(2) . . ?
C19 C18 C17 120.3(2) . . ?
C20 C19 C18 120.2(2) . . ?
C19 C20 C21 119.8(2) . . ?
C16 C21 C20 120.9(2) . . ?
C27 C22 C23 118.7(2) . . ?
C27 C22 P1 119.09(16) . . ?
C23 C22 P1 122.23(18) . . ?
C24 C23 C22 120.5(2) . . ?
C23 C24 C25 120.3(3) . . ?
C24 C25 C26 120.1(3) . . ?
C25 C26 C27 119.3(3) . . ?
C22 C27 C26 121.2(2) . . ?
C33 C28 C29 118.9(2) . . ?
C33 C28 P1 122.05(16) . . ?
C29 C28 P1 118.78(17) . . ?
C30 C29 C28 119.9(2) . . ?
C31 C30 C29 120.4(3) . . ?
C30 C31 C32 120.4(2) . . ?
C31 C32 C33 119.8(3) . . ?
C28 C33 C32 120.6(2) . . ?
C35 C34 C39 118.66(18) . . ?
C35 C34 P2 118.38(14) . . ?
C39 C34 P2 122.91(15) . . ?
C36 C35 C34 120.7(2) . . ?
C37 C36 C35 120.0(2) . . ?
C38 C37 C36 120.2(2) . . ?
C37 C38 C39 120.7(2) . . ?
C38 C39 C34 119.8(2) . . ?
C41 C40 C45 118.5(2) . . ?
C41 C40 P2 119.22(16) . . ?
C45 C40 P2 122.19(16) . . ?
C42 C41 C40 120.8(2) . . ?
C41 C42 C43 120.3(2) . . ?
C44 C43 C42 119.0(2) . . ?
C43 C44 C45 120.9(2) . . ?
C44 C45 C40 120.4(2) . . ?
C47 C46 C51 118.8(2) . . ?
C47 C46 P2 124.06(18) . . ?
C51 C46 P2 117.08(16) . . ?
C46 C47 C48 120.0(2) . . ?
C49 C48 C47 120.7(3) . . ?
C48 C49 C50 120.1(3) . . ?
C51 C50 C49 119.8(3) . . ?
C50 C51 C46 120.7(2) . . ?
C3S N1S C3SX 41.1(4) . . ?
C3S N1S C1S 135.7(5) . . ?
C3SX N1S C1S 96.5(5) . . ?
C3S N1S C2S 107.1(4) . . ?
C3SX N1S C2S 146.8(5) . . ?
C1S N1S C2S 116.5(3) . . ?
O1S C3S N1S 118.6(10) . . ?
O1SX O1S C3S 62.2(11) . . ?
O1SX C3SX N1S 119.7(12) . . ?
O1S O1SX C3SX 53.7(11) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 Cu1 P1 C22 114.81(9) . . . . ?
P2 Cu1 P1 C22 -79.74(7) . . . . ?
N1 Cu1 P1 C16 -9.23(9) . . . . ?
P2 Cu1 P1 C16 156.21(7) . . . . ?
N1 Cu1 P1 C28 -127.58(9) . . . . ?
P2 Cu1 P1 C28 37.86(8) . . . . ?
N1 Cu1 P2 C34 -165.31(8) . . . . ?
P1 Cu1 P2 C34 29.80(8) . . . . ?
N1 Cu1 P2 C46 76.86(9) . . . . ?
P1 Cu1 P2 C46 -88.03(8) . . . . ?
N1 Cu1 P2 C40 -43.49(9) . . . . ?
P1 Cu1 P2 C40 151.62(7) . . . . ?
O1 Cu2 O1 C1 -12(4) 7_566 . . . ?
O2 Cu2 O1 C1 1.07(13) . . . . ?
O2 Cu2 O1 C1 -178.93(13) 7_566 . . . ?
O1 Cu2 O2 C2 -1.44(13) . . . . ?
O1 Cu2 O2 C2 178.56(13) 7_566 . . . ?
O2 Cu2 O2 C2 125(8) 7_566 . . . ?
P2 Cu1 N1 C4 -67.23(15) . . . . ?
P1 Cu1 N1 C4 97.85(14) . . . . ?
P2 Cu1 N1 C5 129.76(12) . . . . ?
P1 Cu1 N1 C5 -65.16(14) . . . . ?
Cu2 O1 C1 C2 -0.5(2) . . . . ?
Cu2 O1 C1 C5 -177.08(16) . . . . ?
Cu2 O2 C2 C1 1.5(2) . . . . ?
Cu2 O2 C2 C3 179.73(15) . . . . ?
O1 C1 C2 O2 -0.7(3) . . . . ?
C5 C1 C2 O2 176.02(18) . . . . ?
O1 C1 C2 C3 -178.96(17) . . . . ?
C5 C1 C2 C3 -2.2(3) . . . . ?
O2 C2 C3 C6 -1.2(3) . . . . ?
C1 C2 C3 C6 176.92(19) . . . . ?
O2 C2 C3 C4 178.97(18) . . . . ?
C1 C2 C3 C4 -2.9(3) . . . . ?
C5 N1 C4 C9 -179.69(18) . . . . ?
Cu1 N1 C4 C9 17.7(3) . . . . ?
C5 N1 C4 C3 -0.3(3) . . . . ?
Cu1 N1 C4 C3 -162.94(14) . . . . ?
C6 C3 C4 N1 -175.51(18) . . . . ?
C2 C3 C4 N1 4.3(3) . . . . ?
C6 C3 C4 C9 3.9(3) . . . . ?
C2 C3 C4 C9 -176.31(19) . . . . ?
C4 N1 C5 C1 -5.2(3) . . . . ?
Cu1 N1 C5 C1 158.58(15) . . . . ?
C4 N1 C5 C10 169.29(16) . . . . ?
Cu1 N1 C5 C10 -26.9(2) . . . . ?
O1 C1 C5 N1 -176.97(17) . . . . ?
C2 C1 C5 N1 6.5(3) . . . . ?
O1 C1 C5 C10 8.8(3) . . . . ?
C2 C1 C5 C10 -167.73(18) . . . . ?
C2 C3 C6 C7 178.6(2) . . . . ?
C4 C3 C6 C7 -1.6(3) . . . . ?
C3 C6 C7 C8 -1.3(4) . . . . ?
C6 C7 C8 C9 1.8(4) . . . . ?
C7 C8 C9 C4 0.7(4) . . . . ?
N1 C4 C9 C8 175.9(2) . . . . ?
C3 C4 C9 C8 -3.5(3) . . . . ?
N1 C5 C10 C15 144.9(2) . . . . ?
C1 C5 C10 C15 -40.5(3) . . . . ?
N1 C5 C10 C11 -38.4(3) . . . . ?
C1 C5 C10 C11 136.2(2) . . . . ?
C15 C10 C11 C12 0.9(3) . . . . ?
C5 C10 C11 C12 -176.1(2) . . . . ?
C10 C11 C12 C13 0.1(4) . . . . ?
C11 C12 C13 C14 -1.3(5) . . . . ?
C12 C13 C14 C15 1.5(5) . . . . ?
C13 C14 C15 C10 -0.5(4) . . . . ?
C11 C10 C15 C14 -0.7(3) . . . . ?
C5 C10 C15 C14 176.1(2) . . . . ?
C22 P1 C16 C21 26.6(2) . . . . ?
C28 P1 C16 C21 -81.0(2) . . . . ?
Cu1 P1 C16 C21 156.75(18) . . . . ?
C22 P1 C16 C17 -153.36(17) . . . . ?
C28 P1 C16 C17 99.08(18) . . . . ?
Cu1 P1 C16 C17 -23.18(19) . . . . ?
C21 C16 C17 C18 -1.2(4) . . . . ?
P1 C16 C17 C18 178.71(19) . . . . ?
C16 C17 C18 C19 -0.2(4) . . . . ?
C17 C18 C19 C20 1.1(5) . . . . ?
C18 C19 C20 C21 -0.5(5) . . . . ?
C17 C16 C21 C20 1.8(4) . . . . ?
P1 C16 C21 C20 -178.1(2) . . . . ?
C19 C20 C21 C16 -1.0(4) . . . . ?
C16 P1 C22 C27 110.16(17) . . . . ?
C28 P1 C22 C27 -140.24(17) . . . . ?
Cu1 P1 C22 C27 -17.52(19) . . . . ?
C16 P1 C22 C23 -70.00(19) . . . . ?
C28 P1 C22 C23 39.60(19) . . . . ?
Cu1 P1 C22 C23 162.32(15) . . . . ?
C27 C22 C23 C24 -1.1(3) . . . . ?
P1 C22 C23 C24 179.07(18) . . . . ?
C22 C23 C24 C25 2.1(4) . . . . ?
C23 C24 C25 C26 -1.5(5) . . . . ?
C24 C25 C26 C27 -0.1(5) . . . . ?
C23 C22 C27 C26 -0.5(3) . . . . ?
P1 C22 C27 C26 179.38(19) . . . . ?
C25 C26 C27 C22 1.1(4) . . . . ?
C22 P1 C28 C33 -138.65(19) . . . . ?
C16 P1 C28 C33 -28.3(2) . . . . ?
Cu1 P1 C28 C33 94.85(18) . . . . ?
C22 P1 C28 C29 47.59(19) . . . . ?
C16 P1 C28 C29 157.89(17) . . . . ?
Cu1 P1 C28 C29 -78.92(18) . . . . ?
C33 C28 C29 C30 1.4(4) . . . . ?
P1 C28 C29 C30 175.3(2) . . . . ?
C28 C29 C30 C31 -1.2(4) . . . . ?
C29 C30 C31 C32 -0.4(5) . . . . ?
C30 C31 C32 C33 1.9(5) . . . . ?
C29 C28 C33 C32 0.0(4) . . . . ?
P1 C28 C33 C32 -173.7(2) . . . . ?
C31 C32 C33 C28 -1.6(4) . . . . ?
C46 P2 C34 C35 170.62(16) . . . . ?
C40 P2 C34 C35 -78.75(17) . . . . ?
Cu1 P2 C34 C35 50.03(18) . . . . ?
C46 P2 C34 C39 -11.82(19) . . . . ?
C40 P2 C34 C39 98.81(18) . . . . ?
Cu1 P2 C34 C39 -132.41(15) . . . . ?
C39 C34 C35 C36 -0.8(3) . . . . ?
P2 C34 C35 C36 176.83(17) . . . . ?
C34 C35 C36 C37 1.0(4) . . . . ?
C35 C36 C37 C38 0.2(4) . . . . ?
C36 C37 C38 C39 -1.6(4) . . . . ?
C37 C38 C39 C34 1.8(3) . . . . ?
C35 C34 C39 C38 -0.6(3) . . . . ?
P2 C34 C39 C38 -178.12(16) . . . . ?
C34 P2 C40 C41 173.19(17) . . . . ?
C46 P2 C40 C41 -77.47(18) . . . . ?
Cu1 P2 C40 C41 44.66(19) . . . . ?
C34 P2 C40 C45 -2.6(2) . . . . ?
C46 P2 C40 C45 106.73(18) . . . . ?
Cu1 P2 C40 C45 -131.15(16) . . . . ?
C45 C40 C41 C42 -0.1(3) . . . . ?
P2 C40 C41 C42 -176.11(19) . . . . ?
C40 C41 C42 C43 0.4(4) . . . . ?
C41 C42 C43 C44 -0.6(4) . . . . ?
C42 C43 C44 C45 0.4(4) . . . . ?
C43 C44 C45 C40 -0.1(4) . . . . ?
C41 C40 C45 C44 0.0(3) . . . . ?
P2 C40 C45 C44 175.8(2) . . . . ?
C34 P2 C46 C47 108.49(19) . . . . ?
C40 P2 C46 C47 0.1(2) . . . . ?
Cu1 P2 C46 C47 -126.49(17) . . . . ?
C34 P2 C46 C51 -74.77(17) . . . . ?
C40 P2 C46 C51 176.86(16) . . . . ?
Cu1 P2 C46 C51 50.26(17) . . . . ?
C51 C46 C47 C48 -0.1(3) . . . . ?
P2 C46 C47 C48 176.6(2) . . . . ?
C46 C47 C48 C49 -0.1(4) . . . . ?
C47 C48 C49 C50 0.5(5) . . . . ?
C48 C49 C50 C51 -0.8(4) . . . . ?
C49 C50 C51 C46 0.6(4) . . . . ?
C47 C46 C51 C50 -0.2(3) . . . . ?
P2 C46 C51 C50 -177.15(18) . . . . ?
C3SX N1S C3S O1S 14.8(10) . . . . ?
C1S N1S C3S O1S -7.1(12) . . . . ?
C2S N1S C3S O1S -177.2(9) . . . . ?
N1S C3S O1S O1SX -116.7(16) . . . . ?
C3S N1S C3SX O1SX 29.2(10) . . . . ?
C1S N1S C3SX O1SX -166.0(11) . . . . ?
C2S N1S C3SX O1SX 7.9(17) . . . . ?
C3S O1S O1SX C3SX 57.0(8) . . . . ?
N1S C3SX O1SX O1S -129.5(14) . . . . ?

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        29.95
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         0.348
_refine_diff_density_min         -0.344
_refine_diff_density_rms         0.057

# =========================== Compound 3 cm395===========================

data_cm395
_database_code_depnum_ccdc_archive 'CCDC 222926'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H34 Cu N4 O6'
_chemical_formula_weight         682.21

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu -1.9646 0.5888 '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                   9.340(2)
_cell_length_b                   9.626(3)
_cell_length_c                   10.522(1)
_cell_angle_alpha                101.86(1)
_cell_angle_beta                 108.49(2)
_cell_angle_gamma                107.73(2)
_cell_volume                     805.3(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    25
_cell_measurement_theta_min      24.95
_cell_measurement_theta_max      29.39

_exptl_crystal_description       block
_exptl_crystal_colour            red-brown
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.407
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             355
_exptl_absorpt_coefficient_mu    1.396
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_correction_T_min  0.8425
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   
;
North A.C., Philips, D.C. and Mathews, F. (1968) Acta Cryst.
A24 350-359.
;
_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           'CU k\a'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Enraf-Nonius CAD4'
_diffrn_measurement_method       \w--2\q
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         3
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  60
_diffrn_standards_decay_%        6
_diffrn_reflns_number            6981
_diffrn_reflns_av_R_equivalents  0.0293
_diffrn_reflns_av_sigmaI/netI    0.0390
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         4.70
_diffrn_reflns_theta_max         75.16
_reflns_number_total             2904
_reflns_number_gt                2697
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CAD4 Express'
_computing_cell_refinement       'CAD4 Express'
_computing_data_reduction        'XCAD4 (Harms 1996)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'PLATON (Spek, 1990)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections.  The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement.  R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0787P)^2^+0.0874P] 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         2904
_refine_ls_number_parameters     212
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0445
_refine_ls_R_factor_gt           0.0425
_refine_ls_wR_factor_ref         0.1169
_refine_ls_wR_factor_gt          0.1148
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_restrained_S_all      1.086
_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 0.5000 0.5000 0.5000 0.03684(15) Uani 1 2 d S . .
O1 O 0.41564(17) 0.61456(15) 0.39069(13) 0.0452(3) Uani 1 1 d . . .
O2 O 0.46730(16) 0.36343(15) 0.32144(14) 0.0438(3) Uani 1 1 d . . .
C1 C 0.3767(2) 0.5472(2) 0.25496(18) 0.0370(3) Uani 1 1 d . . .
C2 C 0.3087(2) 0.6010(2) 0.14714(18) 0.0372(3) Uani 1 1 d . . .
N3 N 0.27614(17) 0.52385(18) 0.01099(15) 0.0404(3) Uani 1 1 d . . .
H3 H 0.2315 0.5613 -0.0464 0.052 Uiso 1 1 d R . .
C4 C 0.3019(2) 0.3931(2) -0.02867(19) 0.0405(4) Uani 1 1 d . . .
C5 C 0.2652(3) 0.3202(3) -0.1722(2) 0.0525(5) Uani 1 1 d . . .
H5 H 0.2256 0.3628 -0.2404 0.068 Uiso 1 1 calc R . .
C6 C 0.2879(3) 0.1868(3) -0.2112(2) 0.0607(6) Uani 1 1 d . . .
H6 H 0.2631 0.1386 -0.3062 0.079 Uiso 1 1 calc R . .
C7 C 0.3485(3) 0.1216(3) -0.1088(3) 0.0591(5) Uani 1 1 d . . .
H7 H 0.3616 0.0298 -0.1367 0.077 Uiso 1 1 calc R . .
C8 C 0.3881(2) 0.1930(2) 0.0315(2) 0.0466(4) Uani 1 1 d . . .
H8 H 0.4302 0.1505 0.0988 0.061 Uiso 1 1 calc R . .
C9 C 0.3654(2) 0.33111(19) 0.07499(18) 0.0384(4) Uani 1 1 d . . .
C10 C 0.40520(19) 0.41000(19) 0.21870(18) 0.0363(3) Uani 1 1 d . . .
C11 C 0.2678(2) 0.7378(2) 0.17086(19) 0.0391(4) Uani 1 1 d . . .
C12 C 0.1261(2) 0.7380(2) 0.0729(2) 0.0506(5) Uani 1 1 d . . .
H12 H 0.0564 0.6509 -0.0070 0.066 Uiso 1 1 calc R . .
C13 C 0.0891(3) 0.8672(3) 0.0943(3) 0.0602(6) Uani 1 1 d . . .
H13 H -0.0063 0.8660 0.0294 0.078 Uiso 1 1 calc R . .
C14 C 0.1937(3) 0.9985(3) 0.2120(3) 0.0584(5) Uani 1 1 d . . .
H14 H 0.1688 1.0854 0.2257 0.076 Uiso 1 1 calc R . .
C15 C 0.3344(3) 1.0001(2) 0.3085(2) 0.0558(5) Uani 1 1 d . . .
H15 H 0.4053 1.0888 0.3867 0.073 Uiso 1 1 calc R . .
C16 C 0.3710(2) 0.8702(2) 0.2895(2) 0.0465(4) Uani 1 1 d . . .
H16 H 0.4649 0.8712 0.3564 0.060 Uiso 1 1 calc R . .
N1S N 0.0992(2) 0.7101(2) -0.40288(19) 0.0556(4) Uani 1 1 d . . .
O1S O 0.1411(3) 0.6053(3) -0.2307(2) 0.0943(7) Uani 1 1 d . . .
C1S C -0.0502(4) 0.7175(5) -0.4018(3) 0.0959(11) Uani 1 1 d . . .
H1AS H -0.0860 0.6588 -0.3459 0.134 Uiso 1 1 calc R . .
H1BS H -0.1329 0.6752 -0.4974 0.134 Uiso 1 1 calc R . .
H1CS H -0.0324 0.8233 -0.3613 0.134 Uiso 1 1 calc R . .
C2S C 0.1574(3) 0.7649(4) -0.5041(3) 0.0788(8) Uani 1 1 d R . .
H2AS H 0.2555 0.7482 -0.4971 0.110 Uiso 1 1 calc R . .
H2BS H 0.1812 0.8734 -0.4830 0.110 Uiso 1 1 calc R . .
H2CS H 0.0739 0.7091 -0.5989 0.110 Uiso 1 1 calc R . .
C3S C 0.1832(3) 0.6558(3) -0.3167(3) 0.0683(6) Uani 1 1 d . . .
H3S H 0.2924 0.6541 -0.3216 0.089 Uiso 1 1 d R . .

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 0.0496(2) 0.0372(2) 0.0326(2) 0.01984(15) 0.01535(15) 0.02466(15)
O1 0.0682(8) 0.0449(7) 0.0350(6) 0.0209(5) 0.0193(5) 0.0353(6)
O2 0.0608(7) 0.0414(6) 0.0389(6) 0.0214(5) 0.0170(5) 0.0308(5)
C1 0.0440(8) 0.0368(8) 0.0366(8) 0.0195(6) 0.0153(6) 0.0206(6)
C2 0.0421(8) 0.0376(8) 0.0363(8) 0.0194(6) 0.0142(6) 0.0188(6)
N3 0.0473(7) 0.0435(8) 0.0343(7) 0.0215(6) 0.0137(6) 0.0206(6)
C4 0.0416(8) 0.0416(9) 0.0368(8) 0.0153(7) 0.0151(6) 0.0143(6)
C5 0.0589(10) 0.0571(12) 0.0391(9) 0.0167(8) 0.0192(8) 0.0202(9)
C6 0.0744(13) 0.0626(13) 0.0423(10) 0.0089(9) 0.0265(10) 0.0263(11)
C7 0.0749(13) 0.0506(11) 0.0559(12) 0.0116(9) 0.0321(10) 0.0289(10)
C8 0.0547(9) 0.0413(9) 0.0487(10) 0.0170(8) 0.0238(8) 0.0214(8)
C9 0.0408(8) 0.0361(8) 0.0392(8) 0.0148(7) 0.0169(6) 0.0145(6)
C10 0.0404(7) 0.0340(8) 0.0396(8) 0.0186(6) 0.0162(6) 0.0173(6)
C11 0.0475(8) 0.0414(9) 0.0439(9) 0.0279(7) 0.0231(7) 0.0240(7)
C12 0.0451(9) 0.0466(10) 0.0636(12) 0.0297(9) 0.0177(8) 0.0201(8)
C13 0.0493(10) 0.0603(12) 0.0904(17) 0.0483(12) 0.0276(10) 0.0324(9)
C14 0.0759(13) 0.0527(11) 0.0814(15) 0.0415(11) 0.0469(12) 0.0421(10)
C15 0.0825(14) 0.0458(10) 0.0537(11) 0.0253(9) 0.0333(10) 0.0329(10)
C16 0.0627(10) 0.0453(10) 0.0410(9) 0.0244(8) 0.0194(8) 0.0289(8)
N1S 0.0633(10) 0.0662(11) 0.0479(9) 0.0269(8) 0.0228(8) 0.0341(8)
O1S 0.1154(16) 0.1196(18) 0.0681(12) 0.0608(13) 0.0284(11) 0.0628(14)
C1S 0.106(2) 0.154(3) 0.092(2) 0.071(2) 0.0628(19) 0.092(2)
C2S 0.0930(18) 0.0870(19) 0.0704(16) 0.0392(14) 0.0445(14) 0.0336(15)
C3S 0.0713(14) 0.0820(17) 0.0571(13) 0.0286(12) 0.0179(11) 0.0428(12)

_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 O1 1.9067(13) . ?
Cu1 O1 1.9067(13) 2_666 ?
Cu1 O2 1.9307(13) . ?
Cu1 O2 1.9307(13) 2_666 ?
O1 C1 1.319(2) . ?
O2 C10 1.291(2) . ?
C1 C2 1.394(2) . ?
C1 C10 1.425(2) . ?
C2 N3 1.358(2) . ?
C2 C11 1.475(2) . ?
N3 C4 1.359(2) . ?
C4 C9 1.404(3) . ?
C4 C5 1.407(3) . ?
C5 C6 1.366(3) . ?
C6 C7 1.408(4) . ?
C7 C8 1.368(3) . ?
C8 C9 1.416(3) . ?
C9 C10 1.414(2) . ?
C11 C16 1.395(3) . ?
C11 C12 1.396(3) . ?
C12 C13 1.383(3) . ?
C13 C14 1.387(4) . ?
C14 C15 1.375(3) . ?
C15 C16 1.386(3) . ?
N1S C3S 1.305(3) . ?
N1S C1S 1.422(3) . ?
N1S C2S 1.461(3) . ?
O1S C3S 1.225(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
O1 Cu1 O1 180.00(5) . 2_666 ?
O1 Cu1 O2 85.74(6) . . ?
O1 Cu1 O2 94.26(6) 2_666 . ?
O1 Cu1 O2 94.26(6) . 2_666 ?
O1 Cu1 O2 85.74(6) 2_666 2_666 ?
O2 Cu1 O2 180.0 . 2_666 ?
C1 O1 Cu1 110.04(10) . . ?
C10 O2 Cu1 110.17(11) . . ?
O1 C1 C2 124.06(16) . . ?
O1 C1 C10 116.85(15) . . ?
C2 C1 C10 119.09(16) . . ?
N3 C2 C1 119.04(16) . . ?
N3 C2 C11 116.95(14) . . ?
C1 C2 C11 124.01(16) . . ?
C2 N3 C4 123.98(15) . . ?
N3 C4 C9 119.37(16) . . ?
N3 C4 C5 120.49(17) . . ?
C9 C4 C5 120.14(18) . . ?
C6 C5 C4 119.9(2) . . ?
C5 C6 C7 120.55(19) . . ?
C8 C7 C6 120.2(2) . . ?
C7 C8 C9 120.51(19) . . ?
C4 C9 C10 118.55(16) . . ?
C4 C9 C8 118.66(17) . . ?
C10 C9 C8 122.79(16) . . ?
O2 C10 C9 122.90(15) . . ?
O2 C10 C1 117.19(16) . . ?
C9 C10 C1 119.91(15) . . ?
C16 C11 C12 118.83(18) . . ?
C16 C11 C2 120.82(16) . . ?
C12 C11 C2 120.34(17) . . ?
C13 C12 C11 120.3(2) . . ?
C12 C13 C14 120.27(19) . . ?
C15 C14 C13 119.9(2) . . ?
C14 C15 C16 120.2(2) . . ?
C15 C16 C11 120.43(19) . . ?
C3S N1S C1S 121.6(2) . . ?
C3S N1S C2S 120.2(2) . . ?
C1S N1S C2S 118.2(2) . . ?
O1S C3S N1S 124.1(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 Cu1 O1 C1 -6(21) 2_666 . . . ?
O2 Cu1 O1 C1 0.82(11) . . . . ?
O2 Cu1 O1 C1 -179.18(11) 2_666 . . . ?
O1 Cu1 O2 C10 -0.98(11) . . . . ?
O1 Cu1 O2 C10 179.02(11) 2_666 . . . ?
O2 Cu1 O2 C10 59(14) 2_666 . . . ?
Cu1 O1 C1 C2 178.74(13) . . . . ?
Cu1 O1 C1 C10 -0.55(19) . . . . ?
O1 C1 C2 N3 178.81(15) . . . . ?
C10 C1 C2 N3 -1.9(2) . . . . ?
O1 C1 C2 C11 -1.7(3) . . . . ?
C10 C1 C2 C11 177.54(15) . . . . ?
C1 C2 N3 C4 1.7(2) . . . . ?
C11 C2 N3 C4 -177.80(15) . . . . ?
C2 N3 C4 C9 0.3(2) . . . . ?
C2 N3 C4 C5 -179.83(16) . . . . ?
N3 C4 C5 C6 -178.41(18) . . . . ?
C9 C4 C5 C6 1.5(3) . . . . ?
C4 C5 C6 C7 -0.3(3) . . . . ?
C5 C6 C7 C8 -1.1(3) . . . . ?
C6 C7 C8 C9 1.3(3) . . . . ?
N3 C4 C9 C10 -1.9(2) . . . . ?
C5 C4 C9 C10 178.21(16) . . . . ?
N3 C4 C9 C8 178.62(15) . . . . ?
C5 C4 C9 C8 -1.3(3) . . . . ?
C7 C8 C9 C4 -0.1(3) . . . . ?
C7 C8 C9 C10 -179.62(18) . . . . ?
Cu1 O2 C10 C9 -178.97(12) . . . . ?
Cu1 O2 C10 C1 0.93(18) . . . . ?
C4 C9 C10 O2 -178.52(15) . . . . ?
C8 C9 C10 O2 1.0(3) . . . . ?
C4 C9 C10 C1 1.6(2) . . . . ?
C8 C9 C10 C1 -178.93(15) . . . . ?
O1 C1 C10 O2 -0.3(2) . . . . ?
C2 C1 C10 O2 -179.60(14) . . . . ?
O1 C1 C10 C9 179.63(14) . . . . ?
C2 C1 C10 C9 0.3(2) . . . . ?
N3 C2 C11 C16 -141.07(17) . . . . ?
C1 C2 C11 C16 39.5(2) . . . . ?
N3 C2 C11 C12 37.6(2) . . . . ?
C1 C2 C11 C12 -141.87(18) . . . . ?
C16 C11 C12 C13 -0.4(3) . . . . ?
C2 C11 C12 C13 -179.07(18) . . . . ?
C11 C12 C13 C14 1.0(3) . . . . ?
C12 C13 C14 C15 -0.4(3) . . . . ?
C13 C14 C15 C16 -0.9(3) . . . . ?
C14 C15 C16 C11 1.6(3) . . . . ?
C12 C11 C16 C15 -0.9(3) . . . . ?
C2 C11 C16 C15 177.77(17) . . . . ?
C1S N1S C3S O1S 1.2(5) . . . . ?
C2S N1S C3S O1S -178.7(3) . . . . ?

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
N3 H3 O1S 0.83 2.04 2.839(2) 160.7 .

_diffrn_measured_fraction_theta_max 0.874
_diffrn_reflns_theta_full        75.16
_diffrn_measured_fraction_theta_full 0.874
_refine_diff_density_max         0.505
_refine_diff_density_min         -0.767
_refine_diff_density_rms         0.064
# ===================================================================
data_cm452
_database_code_depnum_ccdc_archive 'CCDC 222927'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C41 H50 Cu N6 O7'
_chemical_formula_weight         802.41

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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 c'

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

_cell_length_a                   10.033(3)
_cell_length_b                   12.778(11)
_cell_length_c                   17.681(15)
_cell_angle_alpha                90.00
_cell_angle_beta                 117.36(6)
_cell_angle_gamma                90.00
_cell_volume                     2013(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    25
_cell_measurement_theta_min      25.46
_cell_measurement_theta_max      29.83

_exptl_crystal_description       prism
_exptl_crystal_colour            'grayish green'
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.324
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             846
_exptl_absorpt_coefficient_mu    1.227
_exptl_absorpt_correction_type   'not applied'
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           'CU k\a'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Enraf-Nonius CAD4'
_diffrn_measurement_method       \w--2\q
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         3
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  60
_diffrn_standards_decay_%        27
_diffrn_reflns_number            5677
_diffrn_reflns_av_R_equivalents  0.0095
_diffrn_reflns_av_sigmaI/netI    0.0170
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.46
_diffrn_reflns_theta_max         58.27
_reflns_number_total             5190
_reflns_number_gt                4991
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CAD4 Express'
_computing_cell_refinement       'CAD4 Express'
_computing_data_reduction        'XCAD4 (Harms 1996)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F^2^ against ALL reflections.  The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement.  R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0536P)^2^+0.2737P] 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    riding
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.024(19)
_refine_ls_number_reflns         5190
_refine_ls_number_parameters     504
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0318
_refine_ls_R_factor_gt           0.0297
_refine_ls_wR_factor_ref         0.0781
_refine_ls_wR_factor_gt          0.0770
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_restrained_S_all      1.044
_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 0.74114(3) 0.80163(3) 0.67040(2) 0.04372(12) Uani 1 1 d . . .
O1 O 0.55276(18) 0.87477(14) 0.62804(12) 0.0439(4) Uani 1 1 d . . .
O2 O 0.6186(2) 0.67480(15) 0.63632(14) 0.0540(5) Uani 1 1 d . . .
O3 O 0.7881(2) 0.83802(18) 0.54608(13) 0.0609(5) Uani 1 1 d . . .
O4 O 0.8691(2) 0.78320(19) 0.45660(14) 0.0604(6) Uani 1 1 d . . .
O5 O 0.5574(3) 0.7332(3) 0.15338(15) 0.0933(9) Uani 1 1 d . . .
N1 N 0.8624(2) 0.93224(18) 0.73013(15) 0.0475(6) Uani 1 1 d . . .
N2 N 0.9353(3) 0.7194(2) 0.73186(16) 0.0498(6) Uani 1 1 d . . .
N3 N 0.1816(2) 0.76059(17) 0.53869(13) 0.0400(5) Uani 1 1 d . . .
H3N H 0.0714 0.7800 0.5180 0.052 Uiso 1 1 d R . .
N4 N 0.6820(3) 0.7665(2) 0.29510(15) 0.0537(6) Uani 1 1 d . . .
H4N H 0.7707 0.7652 0.3374 0.070 Uiso 1 1 d R . .
C1 C 1.0200(4) 0.8981(3) 0.7644(3) 0.0885(13) Uani 1 1 d . . .
H1A H 1.0526 0.9089 0.7212 0.115 Uiso 1 1 calc R . .
H1B H 1.0817 0.9421 0.8127 0.115 Uiso 1 1 calc R . .
C2 C 1.0448(5) 0.7935(4) 0.7903(4) 0.113(2) Uani 1 1 d . . .
H2A H 1.0453 0.7879 0.8452 0.146 Uiso 1 1 calc R . .
H2B H 1.1436 0.7734 0.7982 0.146 Uiso 1 1 calc R . .
C3 C 0.8324(4) 1.0200(3) 0.6708(2) 0.0697(9) Uani 1 1 d . . .
H3A H 0.8966 1.0777 0.7001 0.098 Uiso 1 1 calc R . .
H3B H 0.7294 1.0411 0.6487 0.098 Uiso 1 1 calc R . .
H3C H 0.8515 0.9985 0.6246 0.098 Uiso 1 1 calc R . .
C4 C 0.8272(5) 0.9662(3) 0.7976(2) 0.0809(10) Uani 1 1 d . . .
H4A H 0.8409 0.9088 0.8356 0.113 Uiso 1 1 calc R . .
H4B H 0.7248 0.9895 0.7731 0.113 Uiso 1 1 calc R . .
H4C H 0.8925 1.0227 0.8287 0.113 Uiso 1 1 calc R . .
C5 C 0.9820(5) 0.6708(3) 0.6734(2) 0.0815(11) Uani 1 1 d . . .
H5A H 0.9831 0.7224 0.6342 0.114 Uiso 1 1 calc R . .
H5B H 0.9130 0.6160 0.6424 0.114 Uiso 1 1 calc R . .
H5C H 1.0808 0.6419 0.7050 0.114 Uiso 1 1 calc R . .
C6 C 0.9246(5) 0.6337(4) 0.7850(3) 0.1060(16) Uani 1 1 d . . .
H6A H 1.0171 0.5953 0.8100 0.148 Uiso 1 1 calc R . .
H6B H 0.8440 0.5876 0.7502 0.148 Uiso 1 1 calc R . .
H6C H 0.9056 0.6626 0.8293 0.148 Uiso 1 1 calc R . .
C7 C 0.4405(3) 0.80707(19) 0.59961(16) 0.0336(6) Uani 1 1 d . . .
C8 C 0.4786(3) 0.6995(2) 0.60489(18) 0.0405(7) Uani 1 1 d . . .
C9 C 0.3632(3) 0.6223(2) 0.57824(17) 0.0408(6) Uani 1 1 d . . .
C10 C 0.3931(3) 0.5137(2) 0.5848(2) 0.0541(7) Uani 1 1 d . . .
H10 H 0.4918 0.4903 0.6077 0.070 Uiso 1 1 calc R . .
C11 C 0.2781(4) 0.4425(2) 0.5578(2) 0.0614(8) Uani 1 1 d . . .
H11 H 0.2987 0.3711 0.5631 0.080 Uiso 1 1 calc R . .
C12 C 0.1277(4) 0.4783(2) 0.5218(2) 0.0574(8) Uani 1 1 d . . .
H12 H 0.0497 0.4300 0.5011 0.075 Uiso 1 1 calc R . .
C13 C 0.0956(3) 0.5821(2) 0.51705(18) 0.0476(7) Uani 1 1 d . . .
H13 H -0.0035 0.6041 0.4954 0.062 Uiso 1 1 calc R . .
C14 C 0.2116(3) 0.6560(2) 0.54467(16) 0.0406(6) Uani 1 1 d . . .
C15 C 0.2890(3) 0.8375(2) 0.56377(16) 0.0360(6) Uani 1 1 d . . .
C16 C 0.2365(3) 0.9463(2) 0.55195(15) 0.0397(6) Uani 1 1 d . . .
C17 C 0.3155(3) 1.0252(2) 0.53545(18) 0.0468(6) Uani 1 1 d . . .
H17 H 0.4053 1.0093 0.5347 0.061 Uiso 1 1 calc R . .
C18 C 0.2622(3) 1.1266(2) 0.52024(19) 0.0520(7) Uani 1 1 d . . .
H18 H 0.3153 1.1777 0.5079 0.068 Uiso 1 1 calc R . .
C19 C 0.1323(3) 1.1532(2) 0.5230(2) 0.0537(7) Uani 1 1 d . . .
H19 H 0.0976 1.2218 0.5131 0.070 Uiso 1 1 calc R . .
C20 C 0.0533(3) 1.0765(2) 0.5407(2) 0.0566(8) Uani 1 1 d . . .
H20 H -0.0343 1.0938 0.5436 0.074 Uiso 1 1 calc R . .
C21 C 0.1042(3) 0.9740(2) 0.55433(18) 0.0479(7) Uani 1 1 d . . .
H21 H 0.0492 0.9229 0.5652 0.062 Uiso 1 1 calc R . .
C22 C 0.7679(3) 0.8136(2) 0.47340(18) 0.0427(7) Uani 1 1 d . . .
C23 C 0.6084(3) 0.8232(2) 0.40018(18) 0.0434(6) Uani 1 1 d . . .
C24 C 0.4959(3) 0.8530(3) 0.41993(19) 0.0534(7) Uani 1 1 d . . .
H24 H 0.5194 0.8651 0.4766 0.069 Uiso 1 1 calc R . .
C25 C 0.3496(4) 0.8655(3) 0.3581(2) 0.0721(10) Uani 1 1 d . . .
H25 H 0.2754 0.8858 0.3727 0.094 Uiso 1 1 calc R . .
C26 C 0.3152(4) 0.8473(3) 0.2747(2) 0.0743(10) Uani 1 1 d . . .
H26 H 0.2240 0.8545 0.2359 0.097 Uiso 1 1 d R . .
C27 C 0.4207(4) 0.8170(3) 0.2525(2) 0.0640(8) Uani 1 1 d . . .
H27 H 0.3947 0.8057 0.1954 0.083 Uiso 1 1 calc R . .
C28 C 0.5695(3) 0.8023(2) 0.31456(18) 0.0474(7) Uani 1 1 d . . .
C29 C 0.6733(4) 0.7338(3) 0.2207(2) 0.0584(8) Uani 1 1 d . . .
C30 C 0.8163(4) 0.6951(2) 0.2234(2) 0.0593(8) Uani 1 1 d . . .
C31 C 0.8175(7) 0.6770(4) 0.1469(3) 0.0941(14) Uani 1 1 d . . .
H31 H 0.7304 0.6873 0.0961 0.122 Uiso 1 1 calc R . .
C32 C 0.9445(8) 0.6443(5) 0.1448(4) 0.1145(17) Uani 1 1 d . . .
H32 H 0.9436 0.6333 0.0926 0.149 Uiso 1 1 calc R . .
C33 C 1.0730(7) 0.6273(4) 0.2180(4) 0.1054(16) Uani 1 1 d . . .
H33 H 1.1595 0.6050 0.2158 0.137 Uiso 1 1 calc R . .
C34 C 1.0741(5) 0.6433(4) 0.2941(3) 0.1006(14) Uani 1 1 d . . .
H34 H 1.1613 0.6306 0.3443 0.131 Uiso 1 1 calc R . .
C35 C 0.9476(4) 0.6781(3) 0.2979(3) 0.0817(11) Uani 1 1 d . . .
H35 H 0.9501 0.6901 0.3504 0.106 Uiso 1 1 calc R . .
O1S O 0.7828(4) 0.7149(3) 0.9246(3) 0.1175(12) Uani 1 1 d . . .
N1S N 0.5844(4) 0.8262(3) 0.8747(2) 0.0781(9) Uani 1 1 d . . .
C1S C 0.6717(6) 0.7546(4) 0.8675(3) 0.0946(13) Uani 1 1 d . . .
H1S H 0.6459 0.7316 0.8126 0.123 Uiso 1 1 calc R . .
C2S C 0.6147(7) 0.8671(5) 0.9556(3) 0.1250(19) Uani 1 1 d . . .
H2S1 H 0.7042 0.8353 0.9987 0.175 Uiso 1 1 calc R . .
H2S2 H 0.5319 0.8521 0.9670 0.175 Uiso 1 1 calc R . .
H2S3 H 0.6286 0.9414 0.9560 0.175 Uiso 1 1 calc R . .
C3S C 0.4542(6) 0.8664(6) 0.7997(3) 0.129(2) Uani 1 1 d . . .
H3S1 H 0.4231 0.8161 0.7545 0.181 Uiso 1 1 calc R . .
H3S2 H 0.4805 0.9308 0.7819 0.181 Uiso 1 1 calc R . .
H3S3 H 0.3736 0.8788 0.8135 0.181 Uiso 1 1 calc R . .
O1R O 0.3367(4) 0.3639(4) 0.3509(4) 0.180(2) Uani 1 1 d . . .
N1R N 0.5214(4) 0.4834(3) 0.3876(3) 0.1022(12) Uani 1 1 d . . .
C1R C 0.4364(6) 0.4133(5) 0.4027(5) 0.128(2) Uani 1 1 d . . .
H1R H 0.4583 0.4027 0.4593 0.167 Uiso 1 1 calc R . .
C2R C 0.5018(11) 0.5046(7) 0.3039(5) 0.202(4) Uani 1 1 d . . .
H2R1 H 0.4518 0.4465 0.2673 0.283 Uiso 1 1 calc R . .
H2R2 H 0.5980 0.5148 0.3057 0.283 Uiso 1 1 calc R . .
H2R3 H 0.4422 0.5666 0.2822 0.283 Uiso 1 1 calc R . .
C3R C 0.6393(8) 0.5344(5) 0.4585(4) 0.166(3) Uani 1 1 d . . .
H3R1 H 0.6259 0.6089 0.4520 0.232 Uiso 1 1 calc R . .
H3R2 H 0.7341 0.5157 0.4614 0.232 Uiso 1 1 calc R . .
H3R3 H 0.6371 0.5131 0.5100 0.232 Uiso 1 1 calc R . .

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 0.02848(18) 0.0447(2) 0.0501(2) -0.00227(19) 0.01134(15) 0.00223(17)
O1 0.0289(10) 0.0396(10) 0.0580(11) -0.0034(8) 0.0156(9) 0.0000(7)
O2 0.0321(11) 0.0448(10) 0.0734(14) -0.0064(10) 0.0142(10) 0.0017(8)
O3 0.0440(11) 0.0862(14) 0.0428(12) -0.0041(10) 0.0115(9) 0.0035(10)
O4 0.0343(11) 0.0797(14) 0.0560(12) -0.0178(11) 0.0113(10) 0.0012(10)
O5 0.0826(19) 0.127(2) 0.0482(14) -0.0133(14) 0.0113(13) 0.0184(17)
N1 0.0353(12) 0.0492(13) 0.0512(13) -0.0005(11) 0.0140(10) -0.0006(10)
N2 0.0379(14) 0.0559(14) 0.0480(14) -0.0030(12) 0.0133(12) 0.0062(12)
N3 0.0297(11) 0.0442(12) 0.0425(11) 0.0016(10) 0.0135(9) -0.0023(9)
N4 0.0481(13) 0.0669(15) 0.0405(14) -0.0087(11) 0.0156(11) -0.0017(11)
C1 0.0352(18) 0.067(2) 0.126(3) -0.005(2) 0.0056(19) -0.0024(16)
C2 0.046(2) 0.092(3) 0.138(4) -0.034(3) -0.011(2) 0.0140(19)
C3 0.088(2) 0.0481(17) 0.071(2) 0.0043(16) 0.0349(19) -0.0069(16)
C4 0.103(3) 0.076(2) 0.072(2) -0.0235(19) 0.047(2) -0.019(2)
C5 0.077(2) 0.108(3) 0.065(2) 0.015(2) 0.0371(19) 0.047(2)
C6 0.090(3) 0.141(4) 0.100(3) 0.067(3) 0.055(3) 0.060(3)
C7 0.0281(14) 0.0385(14) 0.0323(13) -0.0017(10) 0.0124(11) -0.0023(10)
C8 0.0345(15) 0.0426(17) 0.0437(15) -0.0005(11) 0.0173(13) 0.0026(11)
C9 0.0398(14) 0.0377(14) 0.0449(14) -0.0035(11) 0.0193(12) -0.0025(11)
C10 0.0475(16) 0.0454(16) 0.0645(18) -0.0025(14) 0.0214(14) 0.0016(13)
C11 0.074(2) 0.0370(15) 0.078(2) -0.0062(14) 0.0389(18) -0.0063(15)
C12 0.0582(19) 0.0518(18) 0.0670(19) -0.0051(15) 0.0329(16) -0.0172(14)
C13 0.0402(15) 0.0513(17) 0.0502(16) -0.0030(13) 0.0198(13) -0.0096(12)
C14 0.0399(15) 0.0414(14) 0.0411(14) -0.0007(12) 0.0192(12) -0.0062(11)
C15 0.0316(13) 0.0379(13) 0.0357(13) 0.0006(11) 0.0129(10) -0.0028(11)
C16 0.0308(12) 0.0458(14) 0.0378(13) -0.0010(11) 0.0117(11) 0.0018(11)
C17 0.0398(14) 0.0458(16) 0.0538(16) 0.0007(13) 0.0205(12) 0.0011(12)
C18 0.0509(16) 0.0410(15) 0.0584(17) 0.0023(13) 0.0202(13) -0.0003(13)
C19 0.0528(17) 0.0403(15) 0.0572(18) -0.0001(14) 0.0158(14) 0.0083(13)
C20 0.0446(15) 0.0560(18) 0.0694(19) 0.0007(15) 0.0264(15) 0.0126(13)
C21 0.0383(14) 0.0500(16) 0.0576(16) 0.0031(13) 0.0238(13) 0.0019(12)
C22 0.0362(15) 0.0439(15) 0.0420(18) -0.0010(12) 0.0128(12) 0.0027(11)
C23 0.0393(14) 0.0450(14) 0.0416(15) -0.0008(12) 0.0149(12) -0.0005(11)
C24 0.0425(16) 0.0703(19) 0.0448(16) 0.0066(14) 0.0179(13) 0.0112(14)
C25 0.0451(17) 0.098(3) 0.069(2) 0.005(2) 0.0226(16) 0.0151(18)
C26 0.0413(18) 0.103(3) 0.059(2) 0.007(2) 0.0056(15) 0.0140(18)
C27 0.0515(18) 0.082(2) 0.0457(17) 0.0010(15) 0.0113(15) 0.0063(15)
C28 0.0417(15) 0.0506(16) 0.0433(16) -0.0001(12) 0.0140(13) -0.0021(12)
C29 0.065(2) 0.0536(17) 0.051(2) -0.0003(15) 0.0222(17) -0.0025(15)
C30 0.074(2) 0.0470(17) 0.063(2) -0.0052(14) 0.0375(18) -0.0044(14)
C31 0.124(4) 0.096(3) 0.076(3) -0.015(2) 0.057(3) 0.003(3)
C32 0.136(5) 0.137(4) 0.110(4) -0.026(3) 0.090(4) -0.001(4)
C33 0.119(4) 0.087(3) 0.158(5) -0.028(3) 0.104(4) -0.009(3)
C34 0.080(3) 0.121(4) 0.115(4) -0.018(3) 0.057(3) 0.004(3)
C35 0.071(2) 0.106(3) 0.078(2) -0.005(2) 0.042(2) 0.010(2)
O1S 0.088(2) 0.120(3) 0.142(3) -0.001(2) 0.050(2) 0.008(2)
N1S 0.071(2) 0.089(2) 0.084(2) -0.0095(19) 0.044(2) -0.0023(18)
C1S 0.108(4) 0.096(3) 0.101(3) -0.010(3) 0.066(3) -0.017(3)
C2S 0.136(5) 0.132(4) 0.088(3) -0.023(3) 0.036(3) 0.023(4)
C3S 0.106(4) 0.188(6) 0.089(3) 0.011(4) 0.040(3) 0.010(4)
O1R 0.081(2) 0.173(4) 0.254(6) -0.098(4) 0.050(3) -0.063(3)
N1R 0.075(2) 0.073(2) 0.128(3) -0.011(2) 0.021(2) -0.0081(19)
C1R 0.097(4) 0.112(4) 0.188(6) -0.048(4) 0.077(4) -0.024(3)
C2R 0.268(11) 0.156(7) 0.132(6) 0.047(5) 0.048(7) -0.010(7)
C3R 0.168(6) 0.125(5) 0.150(5) -0.024(4) 0.026(5) -0.072(5)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix.  The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry.  An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 O1 1.9250(19) . ?
Cu1 O2 1.955(2) . ?
Cu1 N2 2.033(3) . ?
Cu1 N1 2.049(3) . ?
O1 C7 1.323(3) . ?
O2 C8 1.290(4) . ?
O3 C22 1.245(4) . ?
O4 C22 1.244(4) . ?
O5 C29 1.223(4) . ?
N1 C4 1.458(4) . ?
N1 C3 1.469(4) . ?
N1 C1 1.476(4) . ?
N2 C5 1.456(5) . ?
N2 C2 1.459(5) . ?
N2 C6 1.479(5) . ?
N3 C14 1.363(4) . ?
N3 C15 1.373(3) . ?
N4 C29 1.344(4) . ?
N4 C28 1.400(4) . ?
C1 C2 1.397(7) . ?
C7 C15 1.406(4) . ?
C7 C8 1.418(4) . ?
C8 C9 1.426(4) . ?
C9 C10 1.413(4) . ?
C9 C14 1.421(4) . ?
C10 C11 1.371(5) . ?
C11 C12 1.418(5) . ?
C12 C13 1.358(5) . ?
C13 C14 1.402(4) . ?
C15 C16 1.467(4) . ?
C16 C17 1.393(4) . ?
C16 C21 1.393(4) . ?
C17 C18 1.380(4) . ?
C18 C19 1.369(4) . ?
C19 C20 1.384(5) . ?
C20 C21 1.386(4) . ?
C22 C23 1.532(4) . ?
C23 C24 1.380(4) . ?
C23 C28 1.405(4) . ?
C24 C25 1.378(5) . ?
C25 C26 1.370(6) . ?
C26 C27 1.346(5) . ?
C27 C28 1.401(4) . ?
C29 C30 1.498(5) . ?
C30 C31 1.378(6) . ?
C30 C35 1.388(6) . ?
C31 C32 1.358(8) . ?
C32 C33 1.360(8) . ?
C33 C34 1.357(7) . ?
C34 C35 1.375(6) . ?
O1S C1S 1.218(6) . ?
N1S C1S 1.312(6) . ?
N1S C2S 1.419(6) . ?
N1S C3S 1.461(6) . ?
O1R C1R 1.181(7) . ?
N1R C1R 1.346(7) . ?
N1R C3R 1.426(6) . ?
N1R C2R 1.427(8) . ?

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
O1 Cu1 O2 85.21(9) . . ?
O1 Cu1 N2 170.78(10) . . ?
O2 Cu1 N2 92.81(12) . . ?
O1 Cu1 N1 92.82(10) . . ?
O2 Cu1 N1 167.02(10) . . ?
N2 Cu1 N1 87.09(11) . . ?
C7 O1 Cu1 110.04(16) . . ?
C8 O2 Cu1 109.66(18) . . ?
C4 N1 C3 108.1(3) . . ?
C4 N1 C1 111.6(3) . . ?
C3 N1 C1 110.4(3) . . ?
C4 N1 Cu1 110.8(2) . . ?
C3 N1 Cu1 112.02(19) . . ?
C1 N1 Cu1 104.0(2) . . ?
C5 N2 C2 113.4(4) . . ?
C5 N2 C6 106.0(3) . . ?
C2 N2 C6 106.4(4) . . ?
C5 N2 Cu1 112.5(2) . . ?
C2 N2 Cu1 105.5(2) . . ?
C6 N2 Cu1 113.0(2) . . ?
C14 N3 C15 124.3(2) . . ?
C29 N4 C28 130.2(3) . . ?
C2 C1 N1 114.4(3) . . ?
C1 C2 N2 115.2(4) . . ?
O1 C7 C15 123.1(2) . . ?
O1 C7 C8 116.9(2) . . ?
C15 C7 C8 120.0(2) . . ?
O2 C8 C7 118.2(2) . . ?
O2 C8 C9 122.1(2) . . ?
C7 C8 C9 119.7(2) . . ?
C10 C9 C14 118.5(2) . . ?
C10 C9 C8 122.8(3) . . ?
C14 C9 C8 118.6(2) . . ?
C11 C10 C9 120.7(3) . . ?
C10 C11 C12 119.6(3) . . ?
C13 C12 C11 121.1(3) . . ?
C12 C13 C14 120.1(3) . . ?
N3 C14 C13 121.0(2) . . ?
N3 C14 C9 119.0(2) . . ?
C13 C14 C9 120.0(3) . . ?
N3 C15 C7 118.2(2) . . ?
N3 C15 C16 117.1(2) . . ?
C7 C15 C16 124.7(2) . . ?
C17 C16 C21 117.7(2) . . ?
C17 C16 C15 121.0(2) . . ?
C21 C16 C15 121.3(2) . . ?
C18 C17 C16 120.9(3) . . ?
C19 C18 C17 121.0(3) . . ?
C18 C19 C20 119.1(3) . . ?
C19 C20 C21 120.3(3) . . ?
C20 C21 C16 120.9(3) . . ?
O4 C22 O3 124.1(3) . . ?
O4 C22 C23 118.3(3) . . ?
O3 C22 C23 117.6(3) . . ?
C24 C23 C28 118.1(3) . . ?
C24 C23 C22 117.8(2) . . ?
C28 C23 C22 124.1(3) . . ?
C25 C24 C23 121.9(3) . . ?
C26 C25 C24 118.9(3) . . ?
C27 C26 C25 121.4(3) . . ?
C26 C27 C28 120.5(3) . . ?
N4 C28 C27 122.7(3) . . ?
N4 C28 C23 118.1(3) . . ?
C27 C28 C23 119.2(3) . . ?
O5 C29 N4 124.0(3) . . ?
O5 C29 C30 119.8(3) . . ?
N4 C29 C30 116.2(3) . . ?
C31 C30 C35 118.2(4) . . ?
C31 C30 C29 117.7(4) . . ?
C35 C30 C29 124.0(3) . . ?
C32 C31 C30 120.7(5) . . ?
C31 C32 C33 121.0(5) . . ?
C34 C33 C32 119.5(4) . . ?
C33 C34 C35 120.7(5) . . ?
C34 C35 C30 120.0(4) . . ?
C1S N1S C2S 120.7(4) . . ?
C1S N1S C3S 121.0(4) . . ?
C2S N1S C3S 118.3(4) . . ?
O1S C1S N1S 127.4(5) . . ?
C1R N1R C3R 118.3(5) . . ?
C1R N1R C2R 122.3(5) . . ?
C3R N1R C2R 119.3(6) . . ?
O1R C1R N1R 126.2(7) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2 Cu1 O1 C7 0.80(17) . . . . ?
N2 Cu1 O1 C7 -77.1(7) . . . . ?
N1 Cu1 O1 C7 -166.34(17) . . . . ?
O1 Cu1 O2 C8 -1.0(2) . . . . ?
N2 Cu1 O2 C8 170.0(2) . . . . ?
N1 Cu1 O2 C8 80.8(5) . . . . ?
O1 Cu1 N1 C4 64.1(2) . . . . ?
O2 Cu1 N1 C4 -16.8(5) . . . . ?
N2 Cu1 N1 C4 -106.7(2) . . . . ?
O1 Cu1 N1 C3 -56.6(2) . . . . ?
O2 Cu1 N1 C3 -137.5(4) . . . . ?
N2 Cu1 N1 C3 132.6(2) . . . . ?
O1 Cu1 N1 C1 -175.8(2) . . . . ?
O2 Cu1 N1 C1 103.3(5) . . . . ?
N2 Cu1 N1 C1 13.4(3) . . . . ?
O1 Cu1 N2 C5 152.9(6) . . . . ?
O2 Cu1 N2 C5 75.6(3) . . . . ?
N1 Cu1 N2 C5 -117.4(3) . . . . ?
O1 Cu1 N2 C2 -83.0(7) . . . . ?
O2 Cu1 N2 C2 -160.3(3) . . . . ?
N1 Cu1 N2 C2 6.7(3) . . . . ?
O1 Cu1 N2 C6 32.9(8) . . . . ?
O2 Cu1 N2 C6 -44.4(3) . . . . ?
N1 Cu1 N2 C6 122.6(3) . . . . ?
C4 N1 C1 C2 85.8(5) . . . . ?
C3 N1 C1 C2 -154.0(4) . . . . ?
Cu1 N1 C1 C2 -33.7(5) . . . . ?
N1 C1 C2 N2 44.2(7) . . . . ?
C5 N2 C2 C1 95.1(5) . . . . ?
C6 N2 C2 C1 -148.8(5) . . . . ?
Cu1 N2 C2 C1 -28.5(6) . . . . ?
Cu1 O1 C7 C15 -179.2(2) . . . . ?
Cu1 O1 C7 C8 -0.5(3) . . . . ?
Cu1 O2 C8 C7 1.0(3) . . . . ?
Cu1 O2 C8 C9 -177.0(2) . . . . ?
O1 C7 C8 O2 -0.3(4) . . . . ?
C15 C7 C8 O2 178.4(3) . . . . ?
O1 C7 C8 C9 177.7(2) . . . . ?
C15 C7 C8 C9 -3.6(4) . . . . ?
O2 C8 C9 C10 0.6(4) . . . . ?
C7 C8 C9 C10 -177.4(3) . . . . ?
O2 C8 C9 C14 179.7(3) . . . . ?
C7 C8 C9 C14 1.7(4) . . . . ?
C14 C9 C10 C11 1.3(4) . . . . ?
C8 C9 C10 C11 -179.6(3) . . . . ?
C9 C10 C11 C12 0.9(5) . . . . ?
C10 C11 C12 C13 -3.0(5) . . . . ?
C11 C12 C13 C14 2.7(5) . . . . ?
C15 N3 C14 C13 -179.5(2) . . . . ?
C15 N3 C14 C9 -0.5(4) . . . . ?
C12 C13 C14 N3 178.5(3) . . . . ?
C12 C13 C14 C9 -0.4(4) . . . . ?
C10 C9 C14 N3 179.4(3) . . . . ?
C8 C9 C14 N3 0.3(4) . . . . ?
C10 C9 C14 C13 -1.6(4) . . . . ?
C8 C9 C14 C13 179.3(2) . . . . ?
C14 N3 C15 C7 -1.3(4) . . . . ?
C14 N3 C15 C16 179.4(2) . . . . ?
O1 C7 C15 N3 -178.0(2) . . . . ?
C8 C7 C15 N3 3.4(4) . . . . ?
O1 C7 C15 C16 1.2(4) . . . . ?
C8 C7 C15 C16 -177.4(2) . . . . ?
N3 C15 C16 C17 -148.9(2) . . . . ?
C7 C15 C16 C17 31.9(4) . . . . ?
N3 C15 C16 C21 29.2(4) . . . . ?
C7 C15 C16 C21 -150.0(3) . . . . ?
C21 C16 C17 C18 -1.3(4) . . . . ?
C15 C16 C17 C18 176.8(3) . . . . ?
C16 C17 C18 C19 1.6(4) . . . . ?
C17 C18 C19 C20 -0.5(5) . . . . ?
C18 C19 C20 C21 -0.9(5) . . . . ?
C19 C20 C21 C16 1.1(5) . . . . ?
C17 C16 C21 C20 0.0(4) . . . . ?
C15 C16 C21 C20 -178.2(3) . . . . ?
O4 C22 C23 C24 177.5(3) . . . . ?
O3 C22 C23 C24 -3.3(4) . . . . ?
O4 C22 C23 C28 -1.7(4) . . . . ?
O3 C22 C23 C28 177.5(3) . . . . ?
C28 C23 C24 C25 -1.9(5) . . . . ?
C22 C23 C24 C25 178.8(3) . . . . ?
C23 C24 C25 C26 0.2(6) . . . . ?
C24 C25 C26 C27 0.5(6) . . . . ?
C25 C26 C27 C28 0.5(6) . . . . ?
C29 N4 C28 C27 -4.9(5) . . . . ?
C29 N4 C28 C23 174.5(3) . . . . ?
C26 C27 C28 N4 177.1(3) . . . . ?
C26 C27 C28 C23 -2.2(5) . . . . ?
C24 C23 C28 N4 -176.5(3) . . . . ?
C22 C23 C28 N4 2.7(4) . . . . ?
C24 C23 C28 C27 2.9(4) . . . . ?
C22 C23 C28 C27 -177.9(3) . . . . ?
C28 N4 C29 O5 2.2(6) . . . . ?
C28 N4 C29 C30 -177.0(3) . . . . ?
O5 C29 C30 C31 11.0(5) . . . . ?
N4 C29 C30 C31 -169.8(3) . . . . ?
O5 C29 C30 C35 -170.0(4) . . . . ?
N4 C29 C30 C35 9.2(5) . . . . ?
C35 C30 C31 C32 -0.6(7) . . . . ?
C29 C30 C31 C32 178.4(4) . . . . ?
C30 C31 C32 C33 0.8(8) . . . . ?
C31 C32 C33 C34 0.1(9) . . . . ?
C32 C33 C34 C35 -1.1(8) . . . . ?
C33 C34 C35 C30 1.3(7) . . . . ?
C31 C30 C35 C34 -0.4(6) . . . . ?
C29 C30 C35 C34 -179.4(4) . . . . ?
C2S N1S C1S O1S 0.5(8) . . . . ?
C3S N1S C1S O1S -179.9(5) . . . . ?
C3R N1R C1R O1R -178.8(6) . . . . ?
C2R N1R C1R O1R -1.8(10) . . . . ?

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
N3 H3N O4 1.02 1.81 2.799(3) 161.9 1_455
N4 H4N O4 0.86 1.89 2.607(4) 140.4 .

_diffrn_measured_fraction_theta_max 0.930
_diffrn_reflns_theta_full        58.27
_diffrn_measured_fraction_theta_full 0.930
_refine_diff_density_max         0.256
_refine_diff_density_min         -0.206
_refine_diff_density_rms         0.038