# Electronic Supplementary Material (ESI) for CrystEngComm
# This journal is © The Royal Society of Chemistry 2012


data_global
_journal_name_full               CrystEngComm
_journal_coden_cambridge         1350
_journal_year                    ?
_journal_volume                  ?
_journal_page_first              ?
loop_
_publ_author_name
_publ_author_address
T.Bataille
;Science Chimique de Rennes (UMR-CNRS 6226)
Universite' de Rennes 1
Avenue du General Leclerc
35042 Rennes Cedex
France
;
A.Comotti
;Dipartimento di Scienza dei Materiali
Universit\`a di Milano-Bicocca
Via Roberto Cozzi 53
20125 Milano
Italy

;
A.Guerri
;Polo Scientifico - Dipartimento di Chimica
Universit\`a di Firenze
Via della Lastruccia, 3
50019 Sesto Fiorentino - Firenze
Italy
;
A.Ienco
;ICCOM-CNR
Via Madonna del Piano, 10
50019 Sesto Fiorentino - Firenze
Italy
;
F.Marmottini
;Dipartimento di Chimica
Via Elce di Sotto, 8
06123 Perugia
ITALY
;
_publ_contact_author_address     
;Dipartimento di Chimica
Via Elce di Sotto, 8
06123 Perugia
ITALY
;
_publ_contact_author_email       andrea.ienco@iccom.cnr.it
_publ_contact_author_fax         '+39 055 5225203'
_publ_contact_author_phone       '+39 055 5225282'

_publ_contact_author_name        'Costantino Ferdinando'

data_1
_database_code_depnum_ccdc_archive 'CCDC 802886'
#TrackingRef '- sm_tubes_revised.cif'

_audit_update_record             
;
2011-05-18 # Formatted by publCIF
;

_chemical_name_systematic        
;
?
;
_chemical_formula_moiety         'C38 H38 Cu2 N2 O9 P4'
_chemical_formula_sum            'C38 H38 Cu2 N2 O9 P4'
_chemical_formula_weight         917.66
_chemical_absolute_configuration ad

#----------------------------------------------------------------------------#
# UNIT CELL INFORMATION #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   'I -4'
_symmetry_space_group_name_Hall  'I -4'
_symmetry_Int_Tables_number      82

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

_cell_length_a                   29.610(4)
_cell_length_b                   29.610(4)
_cell_length_c                   9.770(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     8566(2)
_cell_formula_units_Z            8
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    1067
_cell_measurement_theta_min      4.2125
_cell_measurement_theta_max      50.7269

#----------------------------------------------------------------------------#
# CRYSTAL INFORMATION #
#----------------------------------------------------------------------------#

_exptl_crystal_density_diffrn    1.423
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3760
_exptl_special_details           
;
The crystal used was weakly diffracting at high theta values
but it was the best diffracting crystal, we can find among numerous
different batches of preparations of the sample.
;

_exptl_crystal_description       needle
_exptl_crystal_colour            'light blue'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02

#----------------------------------------------------------------------------#
# ABSORPTION CORRECTION #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    3.08
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
(compiled May 6 2009,17:20:42)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.66725
_exptl_absorpt_correction_T_max  1

#----------------------------------------------------------------------------#
# DATA COLLECTION #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     1.5418
_diffrn_radiation_type           CuK\a
_diffrn_radiation_monochromator  graphite
_diffrn_detector_area_resol_mean 8.1241
_diffrn_orient_matrix_ub_11      0.031895323
_diffrn_orient_matrix_ub_12      0.0361438844
_diffrn_orient_matrix_ub_13      -0.060883015
_diffrn_orient_matrix_ub_21      -0.0382463338
_diffrn_orient_matrix_ub_22      0.0352844575
_diffrn_orient_matrix_ub_23      0.0084219059
_diffrn_orient_matrix_ub_31      0.0153834875
_diffrn_orient_matrix_ub_32      0.0129036998
_diffrn_orient_matrix_ub_33      0.1457094996
_diffrn_measurement_device_type  'Xcalibur, Onyx'
_diffrn_measurement_method       '\w scans'
_diffrn_reflns_av_R_equivalents  0.081
_diffrn_reflns_av_unetI/netI     0.2148
_diffrn_reflns_number            7721
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         4.22
_diffrn_reflns_theta_max         51.03
_diffrn_reflns_theta_full        51.03
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_reflns_number_total             4301
_reflns_number_gt                2069
_reflns_threshold_expression     >2sigma(I)

#----------------------------------------------------------------------------#
# COMPUTER PROGRAMS USED #
#----------------------------------------------------------------------------#

_computing_data_collection       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
(compiled May 6 2009,17:20:42)
;
_computing_cell_refinement       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
(compiled May 6 2009,17:20:42)
;
_computing_data_reduction        
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
(compiled May 6 2009,17:20:42)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'

#----------------------------------------------------------------------------#
# STRUCTURE SOLUTION
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
# REFINEMENT INFORMATION #
#----------------------------------------------------------------------------#

_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.
ISOR restrain was used to refine the O3 and O8 atoms to avoid a large
ADP max/min Ratio. The N1-C54, N1-C50, N2-C58 and N2-C61 distances was refined
with a restrain of 1.32Ang. The C55-C56, C52-C55, C56-C57 distances was
refined with a restrain of 1.52Ang.
;
_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^)+(0.1074P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         4301
_refine_ls_number_parameters     267
_refine_ls_number_restraints     19
_refine_ls_R_factor_all          0.2049
_refine_ls_R_factor_gt           0.0798
_refine_ls_wR_factor_ref         0.226
_refine_ls_wR_factor_gt          0.1724
_refine_ls_goodness_of_fit_ref   0.991
_refine_ls_restrained_S_all      0.993
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.002
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.09(8)
_refine_diff_density_max         0.411
_refine_diff_density_min         -0.562
_refine_diff_density_rms         0.11

#----------------------------------------------------------------------------#
# ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS #
#----------------------------------------------------------------------------#

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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.018 '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'
P P 0.2955 0.4335 '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'

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 0.54500(9) 0.23503(9) 0.5314(3) 0.0483(9) Uani 1 1 d . . .
Cu2 Cu 0.56531(9) 0.23069(9) 0.0343(3) 0.0497(9) Uani 1 1 d . . .
P4 P 0.62064(17) 0.22875(17) 0.7596(5) 0.0458(15) Uani 1 1 d . . .
P1 P 0.49300(17) 0.25806(18) 0.2596(6) 0.0495(16) Uani 1 1 d . . .
P2 P 0.58415(19) 0.29813(18) 0.2899(6) 0.0499(17) Uani 1 1 d . . .
P3 P 0.55384(19) 0.30291(18) 0.7935(6) 0.0469(16) Uani 1 1 d . . .
O1 O 0.5294(4) 0.2952(4) 0.6638(12) 0.047(4) Uani 1 1 d . . .
O2 O 0.6043(4) 0.2819(4) 0.1573(12) 0.048(4) Uani 1 1 d . . .
O3 O 0.4961(4) 0.2381(4) 0.3985(12) 0.050(4) Uani 1 1 d U . .
O4 O 0.5101(4) 0.2296(4) 0.1410(11) 0.056(4) Uani 1 1 d . . .
O5 O 0.5873(4) 0.2670(4) 0.4128(12) 0.056(4) Uani 1 1 d . . .
O6 O 0.5377(4) 0.2772(4) 0.9186(12) 0.049(4) Uani 1 1 d . . .
O7 O 0.5972(4) 0.2110(4) 0.6317(12) 0.048(4) Uani 1 1 d . . .
O8 O 0.6082(4) 0.2087(4) 0.8962(11) 0.040(4) Uani 1 1 d U . .
N1 N 0.5028(6) 0.2006(6) 0.6564(14) 0.056(5) Uani 1 1 d D . .
N2 N 0.5917(6) 0.1821(5) 0.1588(15) 0.056(5) Uani 1 1 d D . .
C1 C 0.5248(5) 0.3110(5) 0.2654(18) 0.040(5) Uiso 1 1 d . . .
H1A H 0.5206 0.3275 0.1805 0.048 Uiso 1 1 calc R . .
H1B H 0.5139 0.3296 0.3401 0.048 Uiso 1 1 calc R . .
C2 C 0.6127(5) 0.2887(5) 0.7697(18) 0.035(5) Uiso 1 1 d . . .
H2A H 0.6236 0.3027 0.6862 0.041 Uiso 1 1 calc R . .
H2B H 0.6302 0.3006 0.8455 0.041 Uiso 1 1 calc R . .
C10 C 0.4349(3) 0.2704(4) 0.2206(15) 0.048(5) Uiso 1 1 d G . .
C11 C 0.4026(5) 0.2694(4) 0.3236(11) 0.075(7) Uiso 1 1 d G . .
H11 H 0.4113 0.2651 0.4141 0.089 Uiso 1 1 calc R . .
C12 C 0.3572(4) 0.2747(4) 0.2914(13) 0.082(7) Uiso 1 1 d G . .
H12 H 0.3355 0.274 0.3603 0.099 Uiso 1 1 calc R . .
C13 C 0.3441(3) 0.2811(4) 0.1561(15) 0.069(7) Uiso 1 1 d G . .
H13 H 0.3137 0.2846 0.1345 0.083 Uiso 1 1 calc R . .
C14 C 0.3765(5) 0.2821(4) 0.0530(11) 0.088(8) Uiso 1 1 d G . .
H14 H 0.3677 0.2863 -0.0375 0.106 Uiso 1 1 calc R . .
C15 C 0.4219(4) 0.2767(4) 0.0853(13) 0.080(8) Uiso 1 1 d G . .
H15 H 0.4435 0.2774 0.0163 0.096 Uiso 1 1 calc R . .
C20 C 0.6100(4) 0.3509(3) 0.3406(14) 0.053(6) Uiso 1 1 d G . .
C21 C 0.6004(4) 0.3697(4) 0.4676(13) 0.071(6) Uiso 1 1 d G . .
H21 H 0.58 0.3555 0.526 0.086 Uiso 1 1 calc R . .
C22 C 0.6212(4) 0.4097(4) 0.5073(11) 0.086(8) Uiso 1 1 d G . .
H22 H 0.6147 0.4223 0.5923 0.103 Uiso 1 1 calc R . .
C23 C 0.6516(4) 0.4309(3) 0.4201(14) 0.073(7) Uiso 1 1 d G . .
H23 H 0.6655 0.4576 0.4467 0.087 Uiso 1 1 calc R . .
C24 C 0.6613(4) 0.4120(4) 0.2931(13) 0.079(7) Uiso 1 1 d G . .
H24 H 0.6816 0.4262 0.2347 0.095 Uiso 1 1 calc R . .
C25 C 0.6405(4) 0.3720(4) 0.2533(11) 0.057(6) Uiso 1 1 d G . .
H25 H 0.6469 0.3594 0.1683 0.068 Uiso 1 1 calc R . .
C30 C 0.5536(4) 0.3618(3) 0.8340(15) 0.043(5) Uiso 1 1 d G . .
C31 C 0.5789(4) 0.3790(5) 0.9419(13) 0.089(8) Uiso 1 1 d G . .
H31 H 0.5948 0.3596 0.9988 0.107 Uiso 1 1 calc R . .
C32 C 0.5803(5) 0.4253(5) 0.9647(13) 0.109(8) Uiso 1 1 d G . .
H32 H 0.5972 0.4369 1.0369 0.131 Uiso 1 1 calc R . .
C33 C 0.5565(5) 0.4544(3) 0.8796(17) 0.094(8) Uiso 1 1 d G . .
H33 H 0.5574 0.4854 0.8949 0.112 Uiso 1 1 calc R . .
C34 C 0.5312(4) 0.4372(5) 0.7717(14) 0.103(8) Uiso 1 1 d G . .
H34 H 0.5152 0.4567 0.7148 0.123 Uiso 1 1 calc R . .
C35 C 0.5297(4) 0.3909(5) 0.7489(12) 0.070(6) Uiso 1 1 d G . .
H35 H 0.5128 0.3794 0.6768 0.085 Uiso 1 1 calc R . .
C40 C 0.6795(3) 0.2181(4) 0.7355(15) 0.050(5) Uiso 1 1 d G . .
C41 C 0.7053(5) 0.1954(4) 0.8325(12) 0.072(7) Uiso 1 1 d G . .
H41 H 0.6915 0.1827 0.9088 0.086 Uiso 1 1 calc R . .
C42 C 0.7518(5) 0.1918(4) 0.8155(14) 0.093(8) Uiso 1 1 d G . .
H42 H 0.769 0.1766 0.8804 0.111 Uiso 1 1 calc R . .
C43 C 0.7725(3) 0.2108(5) 0.7015(17) 0.092(8) Uiso 1 1 d G . .
H43 H 0.8035 0.2083 0.6901 0.11 Uiso 1 1 calc R . .
C44 C 0.7467(5) 0.2335(4) 0.6045(13) 0.096(9) Uiso 1 1 d G . .
H44 H 0.7605 0.2462 0.5282 0.116 Uiso 1 1 calc R . .
C45 C 0.7002(4) 0.2371(4) 0.6215(13) 0.076(7) Uiso 1 1 d G . .
H45 H 0.683 0.2523 0.5566 0.091 Uiso 1 1 calc R . .
C50 C 0.5168(7) 0.1644(7) 0.721(2) 0.078(7) Uiso 1 1 d D . .
H50 H 0.5462 0.1543 0.7077 0.094 Uiso 1 1 calc R . .
C51 C 0.4864(9) 0.1394(8) 0.813(2) 0.100(9) Uiso 1 1 d . . .
H51 H 0.495 0.112 0.852 0.12 Uiso 1 1 calc R . .
C52 C 0.4432(9) 0.1587(9) 0.842(3) 0.112(10) Uiso 1 1 d D . .
C53 C 0.4322(8) 0.1983(8) 0.770(2) 0.090(8) Uiso 1 1 d . . .
H53 H 0.4044 0.2122 0.7857 0.108 Uiso 1 1 calc R . .
C54 C 0.4626(7) 0.2172(7) 0.676(2) 0.068(7) Uiso 1 1 d D . .
H54 H 0.4538 0.2425 0.6262 0.082 Uiso 1 1 calc R . .
C55 C 0.4066(8) 0.1348(8) 0.925(2) 0.113(9) Uiso 1 1 d D . .
H55A H 0.3769 0.1471 0.9053 0.135 Uiso 1 1 calc R . .
H55B H 0.4064 0.1026 0.9074 0.135 Uiso 1 1 calc R . .
C56 C 0.4207(8) 0.1449(9) 1.068(2) 0.118(10) Uiso 1 1 d D . .
H56A H 0.4243 0.1771 1.0829 0.141 Uiso 1 1 calc R . .
H56B H 0.4486 0.1296 1.0918 0.141 Uiso 1 1 calc R . .
C57 C 0.3808(10) 0.1263(12) 1.150(3) 0.154(13) Uiso 1 1 d D . .
C58 C 0.5640(8) 0.1527(7) 0.213(2) 0.092(8) Uiso 1 1 d D . .
H58 H 0.5335 0.1535 0.1905 0.111 Uiso 1 1 calc R . .
C59 C 0.5802(11) 0.1187(10) 0.309(3) 0.148(12) Uiso 1 1 d . . .
H59 H 0.5606 0.097 0.3437 0.177 Uiso 1 1 calc R . .
C60 C 0.6517(9) 0.1533(9) 0.291(3) 0.127(10) Uiso 1 1 d . . .
H60 H 0.682 0.1556 0.3146 0.152 Uiso 1 1 calc R . .
C61 C 0.6338(7) 0.1852(8) 0.196(2) 0.088(8) Uiso 1 1 d D . .
H61 H 0.652 0.208 0.1614 0.106 Uiso 1 1 calc R . .
O9 O 0.6025(13) 0.1091(11) 0.902(4) 0.160(19) Uani 0.5 1 d P . .
O10 O 0.4549(14) 0.1423(12) 0.398(5) 0.19(2) Uani 0.5 1 d P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cu1 0.0521(19) 0.066(2) 0.0268(18) 0.0027(16) 0.0009(15) -0.0083(17)
Cu2 0.063(2) 0.0556(19) 0.0306(18) 0.0046(16) 0.0033(16) 0.0049(16)
P4 0.048(4) 0.055(4) 0.035(4) 0.002(3) -0.001(3) 0.007(3)
P1 0.041(4) 0.067(4) 0.041(4) 0.005(3) -0.005(3) -0.005(3)
P2 0.057(4) 0.059(4) 0.034(4) -0.004(3) 0.002(3) -0.010(3)
P3 0.058(4) 0.051(4) 0.032(4) -0.002(3) -0.007(3) 0.007(3)
O1 0.060(9) 0.049(9) 0.031(9) 0.015(7) -0.011(7) 0.010(7)
O2 0.059(10) 0.049(9) 0.036(9) 0.001(7) -0.003(7) -0.001(7)
O3 0.058(7) 0.066(7) 0.028(7) 0.010(6) -0.002(6) -0.016(6)
O4 0.075(10) 0.076(11) 0.016(9) -0.018(8) -0.005(7) 0.010(8)
O5 0.050(9) 0.088(11) 0.030(10) 0.018(8) 0.017(7) -0.012(8)
O6 0.072(9) 0.040(8) 0.036(9) 0.026(7) 0.016(7) 0.005(7)
O7 0.038(9) 0.066(10) 0.038(9) 0.008(7) -0.011(7) -0.007(7)
O8 0.048(7) 0.048(7) 0.024(6) 0.011(5) 0.016(5) -0.006(6)
N1 0.070(13) 0.081(14) 0.018(11) 0.027(9) 0.007(9) 0.009(11)
N2 0.077(14) 0.055(13) 0.038(12) 0.036(9) -0.012(10) -0.005(11)
O9 0.19(4) 0.10(3) 0.19(4) 0.08(3) 0.09(3) 0.08(3)
O10 0.17(4) 0.11(3) 0.29(6) -0.02(3) 0.05(4) -0.05(3)

#----------------------------------------------------------------------------#
# MOLECULAR GEOMETRY #
#----------------------------------------------------------------------------#

_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 O3 1.948(12) . ?
Cu1 O5 1.951(11) . ?
Cu1 O7 1.963(11) . ?
Cu1 N1 2.023(15) . ?
Cu1 O1 2.250(12) . ?
Cu2 O4 1.939(12) . ?
Cu2 O6 1.959(11) 1_554 ?
Cu2 O8 1.963(11) 1_554 ?
Cu2 N2 2.040(14) . ?
Cu2 O2 2.254(12) . ?
P4 O8 1.506(11) . ?
P4 O7 1.522(12) . ?
P4 C40 1.788(10) . ?
P4 C2 1.794(15) . ?
P1 O3 1.483(12) . ?
P1 O4 1.519(12) . ?
P1 C10 1.798(10) . ?
P1 C1 1.828(15) . ?
P2 O2 1.506(12) . ?
P2 O5 1.516(12) . ?
P2 C20 1.809(11) . ?
P2 C1 1.815(16) . ?
P3 O1 1.478(12) . ?
P3 O6 1.517(11) . ?
P3 C30 1.788(11) . ?
P3 C2 1.807(16) . ?
O6 Cu2 1.959(11) 1_556 ?
O8 Cu2 1.963(11) 1_556 ?
N1 C54 1.301(15) . ?
N1 C50 1.311(15) . ?
N2 C61 1.301(15) . ?
N2 C58 1.311(15) . ?
C1 H1A 0.97 . ?
C1 H1B 0.97 . ?
C2 H2A 0.97 . ?
C2 H2B 0.97 . ?
C10 C11 1.39 . ?
C10 C15 1.39 . ?
C11 C12 1.39 . ?
C11 H11 0.93 . ?
C12 C13 1.39 . ?
C12 H12 0.93 . ?
C13 C14 1.39 . ?
C13 H13 0.93 . ?
C14 C15 1.39 . ?
C14 H14 0.93 . ?
C15 H15 0.93 . ?
C20 C21 1.39 . ?
C20 C25 1.39 . ?
C21 C22 1.39 . ?
C21 H21 0.93 . ?
C22 C23 1.39 . ?
C22 H22 0.93 . ?
C23 C24 1.39 . ?
C23 H23 0.93 . ?
C24 C25 1.39 . ?
C24 H24 0.93 . ?
C25 H25 0.93 . ?
C30 C31 1.39 . ?
C30 C35 1.39 . ?
C31 C32 1.39 . ?
C31 H31 0.93 . ?
C32 C33 1.39 . ?
C32 H32 0.93 . ?
C33 C34 1.39 . ?
C33 H33 0.93 . ?
C34 C35 1.39 . ?
C34 H34 0.93 . ?
C35 H35 0.93 . ?
C40 C41 1.39 . ?
C40 C45 1.39 . ?
C41 C42 1.39 . ?
C41 H41 0.93 . ?
C42 C43 1.39 . ?
C42 H42 0.93 . ?
C43 C44 1.39 . ?
C43 H43 0.93 . ?
C44 C45 1.39 . ?
C44 H44 0.93 . ?
C45 H45 0.93 . ?
C50 C51 1.48(3) . ?
C50 H50 0.93 . ?
C51 C52 1.43(3) . ?
C51 H51 0.93 . ?
C52 C53 1.40(3) . ?
C52 C55 1.531(10) . ?
C53 C54 1.41(3) . ?
C53 H53 0.93 . ?
C54 H54 0.93 . ?
C55 C56 1.493(10) . ?
C55 H55A 0.97 . ?
C55 H55B 0.97 . ?
C56 C57 1.529(10) . ?
C56 H56A 0.97 . ?
C56 H56B 0.97 . ?
C57 C60 1.39(3) 8_546 ?
C57 C59 1.42(3) 8_546 ?
C58 C59 1.45(3) . ?
C58 H58 0.93 . ?
C59 C57 1.42(3) 7_556 ?
C59 H59 0.93 . ?
C60 C57 1.39(3) 7_556 ?
C60 C61 1.42(3) . ?
C60 H60 0.93 . ?
C61 H61 0.93 . ?

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
O3 Cu1 O5 93.3(5) . . ?
O3 Cu1 O7 159.3(5) . . ?
O5 Cu1 O7 88.1(5) . . ?
O3 Cu1 N1 88.1(6) . . ?
O5 Cu1 N1 178.2(6) . . ?
O7 Cu1 N1 90.2(6) . . ?
O3 Cu1 O1 101.2(5) . . ?
O5 Cu1 O1 95.1(5) . . ?
O7 Cu1 O1 99.3(5) . . ?
N1 Cu1 O1 85.7(6) . . ?
O4 Cu2 O6 88.3(5) . 1_554 ?
O4 Cu2 O8 155.4(5) . 1_554 ?
O6 Cu2 O8 96.1(5) 1_554 1_554 ?
O4 Cu2 N2 89.5(6) . . ?
O6 Cu2 N2 177.8(6) 1_554 . ?
O8 Cu2 N2 85.9(6) 1_554 . ?
O4 Cu2 O2 99.0(5) . . ?
O6 Cu2 O2 92.7(5) 1_554 . ?
O8 Cu2 O2 104.9(5) 1_554 . ?
N2 Cu2 O2 87.7(6) . . ?
O8 P4 O7 118.7(7) . . ?
O8 P4 C40 106.6(7) . . ?
O7 P4 C40 106.1(7) . . ?
O8 P4 C2 108.0(8) . . ?
O7 P4 C2 109.1(8) . . ?
C40 P4 C2 108.0(7) . . ?
O3 P1 O4 117.2(8) . . ?
O3 P1 C10 109.5(7) . . ?
O4 P1 C10 105.6(7) . . ?
O3 P1 C1 106.4(8) . . ?
O4 P1 C1 109.1(8) . . ?
C10 P1 C1 109.0(7) . . ?
O2 P2 O5 117.6(7) . . ?
O2 P2 C20 110.0(7) . . ?
O5 P2 C20 106.4(7) . . ?
O2 P2 C1 109.7(8) . . ?
O5 P2 C1 106.9(8) . . ?
C20 P2 C1 105.4(7) . . ?
O1 P3 O6 117.4(7) . . ?
O1 P3 C30 109.7(7) . . ?
O6 P3 C30 108.1(7) . . ?
O1 P3 C2 109.0(7) . . ?
O6 P3 C2 106.9(8) . . ?
C30 P3 C2 105.0(7) . . ?
P3 O1 Cu1 121.0(7) . . ?
P2 O2 Cu2 118.0(7) . . ?
P1 O3 Cu1 132.4(7) . . ?
P1 O4 Cu2 133.0(8) . . ?
P2 O5 Cu1 136.6(8) . . ?
P3 O6 Cu2 133.4(8) . 1_556 ?
P4 O7 Cu1 130.1(8) . . ?
P4 O8 Cu2 129.6(7) . 1_556 ?
C54 N1 C50 121.9(19) . . ?
C54 N1 Cu1 117.6(14) . . ?
C50 N1 Cu1 120.4(15) . . ?
C61 N2 C58 122(2) . . ?
C61 N2 Cu2 119.0(16) . . ?
C58 N2 Cu2 118.1(16) . . ?
P2 C1 P1 108.8(8) . . ?
P2 C1 H1A 109.9 . . ?
P1 C1 H1A 109.9 . . ?
P2 C1 H1B 109.9 . . ?
P1 C1 H1B 109.9 . . ?
H1A C1 H1B 108.3 . . ?
P4 C2 P3 111.3(8) . . ?
P4 C2 H2A 109.4 . . ?
P3 C2 H2A 109.4 . . ?
P4 C2 H2B 109.4 . . ?
P3 C2 H2B 109.4 . . ?
H2A C2 H2B 108 . . ?
C11 C10 C15 120 . . ?
C11 C10 P1 120.1(9) . . ?
C15 C10 P1 119.7(9) . . ?
C12 C11 C10 120 . . ?
C12 C11 H11 120 . . ?
C10 C11 H11 120 . . ?
C11 C12 C13 120 . . ?
C11 C12 H12 120 . . ?
C13 C12 H12 120 . . ?
C14 C13 C12 120 . . ?
C14 C13 H13 120 . . ?
C12 C13 H13 120 . . ?
C15 C14 C13 120 . . ?
C15 C14 H14 120 . . ?
C13 C14 H14 120 . . ?
C14 C15 C10 120 . . ?
C14 C15 H15 120 . . ?
C10 C15 H15 120 . . ?
C21 C20 C25 120 . . ?
C21 C20 P2 120.2(8) . . ?
C25 C20 P2 119.8(8) . . ?
C22 C21 C20 120 . . ?
C22 C21 H21 120 . . ?
C20 C21 H21 120 . . ?
C21 C22 C23 120 . . ?
C21 C22 H22 120 . . ?
C23 C22 H22 120 . . ?
C22 C23 C24 120 . . ?
C22 C23 H23 120 . . ?
C24 C23 H23 120 . . ?
C25 C24 C23 120 . . ?
C25 C24 H24 120 . . ?
C23 C24 H24 120 . . ?
C24 C25 C20 120 . . ?
C24 C25 H25 120 . . ?
C20 C25 H25 120 . . ?
C31 C30 C35 120 . . ?
C31 C30 P3 121.5(9) . . ?
C35 C30 P3 118.3(9) . . ?
C32 C31 C30 120 . . ?
C32 C31 H31 120 . . ?
C30 C31 H31 120 . . ?
C31 C32 C33 120 . . ?
C31 C32 H32 120 . . ?
C33 C32 H32 120 . . ?
C34 C33 C32 120 . . ?
C34 C33 H33 120 . . ?
C32 C33 H33 120 . . ?
C35 C34 C33 120 . . ?
C35 C34 H34 120 . . ?
C33 C34 H34 120 . . ?
C34 C35 C30 120 . . ?
C34 C35 H35 120 . . ?
C30 C35 H35 120 . . ?
C41 C40 C45 120 . . ?
C41 C40 P4 122.1(9) . . ?
C45 C40 P4 117.6(9) . . ?
C42 C41 C40 120 . . ?
C42 C41 H41 120 . . ?
C40 C41 H41 120 . . ?
C41 C42 C43 120 . . ?
C41 C42 H42 120 . . ?
C43 C42 H42 120 . . ?
C44 C43 C42 120 . . ?
C44 C43 H43 120 . . ?
C42 C43 H43 120 . . ?
C43 C44 C45 120 . . ?
C43 C44 H44 120 . . ?
C45 C44 H44 120 . . ?
C44 C45 C40 120 . . ?
C44 C45 H45 120 . . ?
C40 C45 H45 120 . . ?
N1 C50 C51 121(2) . . ?
N1 C50 H50 119.7 . . ?
C51 C50 H50 119.7 . . ?
C52 C51 C50 118(2) . . ?
C52 C51 H51 121.1 . . ?
C50 C51 H51 121.1 . . ?
C53 C52 C51 117(2) . . ?
C53 C52 C55 119(2) . . ?
C51 C52 C55 124(2) . . ?
C54 C53 C52 121(2) . . ?
C54 C53 H53 119.7 . . ?
C52 C53 H53 119.7 . . ?
N1 C54 C53 122(2) . . ?
N1 C54 H54 118.9 . . ?
C53 C54 H54 118.9 . . ?
C56 C55 C52 102.0(19) . . ?
C56 C55 H55A 111.4 . . ?
C52 C55 H55A 111.4 . . ?
C56 C55 H55B 111.4 . . ?
C52 C55 H55B 111.4 . . ?
H55A C55 H55B 109.2 . . ?
C55 C56 C57 102(2) . . ?
C55 C56 H56A 111.4 . . ?
C57 C56 H56A 111.4 . . ?
C55 C56 H56B 111.4 . . ?
C57 C56 H56B 111.4 . . ?
H56A C56 H56B 109.3 . . ?
C60 C57 C59 114(3) 8_546 8_546 ?
C60 C57 C56 126(3) 8_546 . ?
C59 C57 C56 119(3) 8_546 . ?
N2 C58 C59 121(2) . . ?
N2 C58 H58 119.5 . . ?
C59 C58 H58 119.5 . . ?
C57 C59 C58 119(3) 7_556 . ?
C57 C59 H59 120.4 7_556 . ?
C58 C59 H59 120.4 . . ?
C57 C60 C61 123(3) 7_556 . ?
C57 C60 H60 118.3 7_556 . ?
C61 C60 H60 118.3 . . ?
N2 C61 C60 119(2) . . ?
N2 C61 H61 120.3 . . ?
C60 C61 H61 120.3 . . ?

#===END

data_3
_database_code_depnum_ccdc_archive 'CCDC 802887'
#TrackingRef '- sm_tubes_revised.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?

_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C38 H36 Cu2 N2 O8 P4'
_chemical_formula_sum            'C38 H36 Cu2 N2 O8 P4'
_chemical_formula_weight         899.65

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           tetragonal
_symmetry_space_group_name_H-M   'I -4'
_symmetry_space_group_name_Hall  'I -4'
_symmetry_Int_Tables_number      82

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

_cell_length_a                   29.573(3)
_cell_length_b                   29.573(3)
_cell_length_c                   9.736(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     8515(2)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    3820
_cell_measurement_theta_min      4.2099
_cell_measurement_theta_max      50.8718

_exptl_crystal_description       needle
_exptl_crystal_colour            'pale blue'
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04

_exptl_special_details           
;
The crystal used was weakly diffracting at high theta values
but it was the best diffracting crystal, we can find among numerous
different batches of preparations of the sample.
;

_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.404
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3680
_exptl_absorpt_coefficient_mu    1.199
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6979
_exptl_absorpt_correction_T_max  0.9921
_exptl_absorpt_process_details   
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET)
(compiled Jun 10 2008,16:49:55)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_detector_area_resol_mean 16.4547
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur3'
_diffrn_measurement_method       '\w scans'
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6935
_diffrn_reflns_av_R_equivalents  0.0288
_diffrn_reflns_av_sigmaI/netI    0.0492
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         1.95
_diffrn_reflns_theta_max         21.03
_reflns_number_total             4059
_reflns_number_gt                3410
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET)
(compiled Jun 10 2008,16:49:55)
;
_computing_cell_refinement       
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET)
(compiled Jun 10 2008,16:49:55)
;
_computing_data_reduction        
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET)
(compiled Jun 10 2008,16:49:55)
;
_computing_structure_solution    'Sir97 (Altomare, 1999)'
_computing_structure_refinement  'SHELX (Sheldrick, 2008)'
_computing_molecular_graphics    'SCHAKAL97 (Keller, 1997)'
_computing_publication_material  'PARST (Nardelli, 1995)'

_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.
A racemic twin is present and the twin component was found to be 0.42(2).
The C55-C56, C52-C55, C56-C57 distances was refined with a restrain of
1.52Ang.
;

_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^)+(0.0555P)^2^+32.2128P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.42(2)
_refine_ls_number_reflns         4059
_refine_ls_number_parameters     488
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0631
_refine_ls_R_factor_gt           0.0460
_refine_ls_wR_factor_ref         0.1166
_refine_ls_wR_factor_gt          0.1085
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_restrained_S_all      1.063
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.26898(4) 0.06604(4) 0.03431(12) 0.0503(4) Uani 1 1 d . . .
Cu2 Cu 0.26460(4) 0.04490(4) -0.46915(12) 0.0496(4) Uani 1 1 d . . .
P1 P 0.19687(8) 0.05410(8) -0.2059(2) 0.0313(6) Uani 1 1 d . . .
P2 P 0.27072(8) 0.12083(8) -0.2417(2) 0.0311(6) Uani 1 1 d . . .
P3 P 0.20140(8) 0.08466(8) 0.2898(2) 0.0326(6) Uani 1 1 d . . .
P4 P 0.24127(8) -0.00634(8) -0.7414(2) 0.0337(6) Uani 1 1 d . . .
O1 O 0.2176(2) 0.1047(2) 0.1588(6) 0.0385(16) Uani 1 1 d . . .
O2 O 0.2049(2) 0.0295(2) -0.3374(6) 0.0398(16) Uani 1 1 d . . .
O3 O 0.2905(2) 0.10810(19) -0.1044(5) 0.0390(16) Uani 1 1 d . . .
O4 O 0.28859(18) 0.09684(19) -0.3660(5) 0.0331(15) Uani 1 1 d . . .
O5 O 0.2226(2) 0.03882(19) -0.0819(6) 0.0409(16) Uani 1 1 d . . .
O6 O 0.2328(2) 0.08679(17) 0.4102(6) 0.0390(16) Uani 1 1 d . . .
O7 O 0.27054(19) 0.01063(18) -0.8570(6) 0.0373(16) Uani 1 1 d . . .
O8 O 0.2606(2) -0.00456(18) -0.5997(6) 0.0435(17) Uani 1 1 d . . .
N1 N 0.3177(3) 0.0905(3) 0.1582(8) 0.045(2) Uani 1 1 d . . .
N2 N 0.3013(3) 0.0037(3) -0.3474(7) 0.040(2) Uani 1 1 d . . .
C1 C 0.2112(3) 0.1118(3) -0.2304(10) 0.037(2) Uani 1 1 d . . .
H1A H 0.1990 0.1297 -0.1529 0.045 Uiso 1 1 calc R . .
H1B H 0.1967 0.1228 -0.3157 0.045 Uiso 1 1 calc R . .
C2 C 0.1890(3) 0.0251(3) -0.7401(9) 0.034(2) Uani 1 1 d . . .
H2A H 0.1689 0.0135 -0.6667 0.041 Uiso 1 1 calc R . .
H2B H 0.1733 0.0214 -0.8292 0.041 Uiso 1 1 calc R . .
C10 C 0.2802(3) 0.1805(3) -0.2643(9) 0.036(2) Uani 1 1 d . . .
C11 C 0.2628(3) 0.2019(4) -0.3773(12) 0.063(3) Uani 1 1 d . . .
H11 H 0.2480 0.1848 -0.4467 0.075 Uiso 1 1 calc R . .
C12 C 0.2669(4) 0.2493(4) -0.3910(17) 0.085(5) Uani 1 1 d . . .
H12 H 0.2545 0.2647 -0.4676 0.102 Uiso 1 1 calc R . .
C13 C 0.2898(5) 0.2724(4) -0.2883(19) 0.088(5) Uani 1 1 d . . .
H13 H 0.2915 0.3044 -0.2927 0.106 Uiso 1 1 calc R . .
C14 C 0.3092(5) 0.2514(4) -0.1854(14) 0.080(4) Uani 1 1 d . . .
H14 H 0.3265 0.2681 -0.1208 0.097 Uiso 1 1 calc R . .
C15 C 0.3048(4) 0.2055(4) -0.1699(11) 0.058(3) Uani 1 1 d . . .
H15 H 0.3187 0.1908 -0.0942 0.070 Uiso 1 1 calc R . .
C20 C 0.1371(3) 0.0532(3) -0.1684(10) 0.040(2) Uani 1 1 d . . .
C21 C 0.1204(4) 0.0775(4) -0.0591(12) 0.069(3) Uani 1 1 d . . .
H21 H 0.1405 0.0929 0.0013 0.083 Uiso 1 1 calc R . .
C22 C 0.0738(4) 0.0794(4) -0.0376(15) 0.088(4) Uani 1 1 d . . .
H22 H 0.0621 0.0969 0.0361 0.105 Uiso 1 1 calc R . .
C23 C 0.0449(4) 0.0566(5) -0.1204(15) 0.084(4) Uani 1 1 d . . .
H23 H 0.0132 0.0593 -0.1068 0.101 Uiso 1 1 calc R . .
C24 C 0.0611(4) 0.0300(4) -0.2225(14) 0.079(4) Uani 1 1 d . . .
H24 H 0.0411 0.0119 -0.2757 0.095 Uiso 1 1 calc R . .
C25 C 0.1071(3) 0.0295(3) -0.2483(10) 0.054(3) Uani 1 1 d . . .
H25 H 0.1182 0.0123 -0.3234 0.065 Uiso 1 1 calc R . .
C30 C 0.1493(3) 0.1107(3) 0.3386(10) 0.043(2) Uani 1 1 d . . .
C31 C 0.1269(3) 0.1415(3) 0.2570(10) 0.044(3) Uani 1 1 d . . .
H31 H 0.1396 0.1492 0.1704 0.053 Uiso 1 1 calc R . .
C32 C 0.0874(4) 0.1612(3) 0.2960(11) 0.055(3) Uani 1 1 d . . .
H32 H 0.0723 0.1813 0.2355 0.066 Uiso 1 1 calc R . .
C33 C 0.0699(4) 0.1522(4) 0.4198(12) 0.064(3) Uani 1 1 d . . .
H33 H 0.0430 0.1672 0.4480 0.077 Uiso 1 1 calc R . .
C34 C 0.0903(3) 0.1214(4) 0.5077(11) 0.065(3) Uani 1 1 d . . .
H34 H 0.0774 0.1145 0.5945 0.078 Uiso 1 1 calc R . .
C35 C 0.1298(3) 0.1010(3) 0.4660(11) 0.051(3) Uani 1 1 d . . .
H35 H 0.1441 0.0799 0.5251 0.061 Uiso 1 1 calc R . .
C40 C 0.2299(3) -0.0646(3) -0.7781(10) 0.037(2) Uani 1 1 d . . .
C41 C 0.2302(4) -0.0960(4) -0.6813(12) 0.066(3) Uani 1 1 d . . .
H41 H 0.2345 -0.0877 -0.5879 0.079 Uiso 1 1 calc R . .
C42 C 0.2241(4) -0.1423(4) -0.7176(18) 0.086(4) Uani 1 1 d . . .
H42 H 0.2237 -0.1647 -0.6475 0.103 Uiso 1 1 calc R . .
C43 C 0.2189(4) -0.1548(4) -0.8478(17) 0.071(4) Uani 1 1 d . . .
H43 H 0.2154 -0.1858 -0.8710 0.086 Uiso 1 1 calc R . .
C44 C 0.2186(4) -0.1229(4) -0.9459(15) 0.076(4) Uani 1 1 d . . .
H44 H 0.2145 -0.1314 -1.0392 0.092 Uiso 1 1 calc R . .
C45 C 0.2242(4) -0.0785(4) -0.9132(12) 0.064(3) Uani 1 1 d . . .
H45 H 0.2242 -0.0565 -0.9844 0.077 Uiso 1 1 calc R . .
C50 C 0.3480(4) 0.0647(4) 0.2155(15) 0.089(4) Uani 1 1 d . . .
H50 H 0.3481 0.0334 0.1940 0.106 Uiso 1 1 calc R . .
C51 C 0.3803(5) 0.0811(5) 0.3072(19) 0.146(8) Uani 1 1 d . . .
H51 H 0.4015 0.0609 0.3472 0.175 Uiso 1 1 calc R . .
C52 C 0.3820(5) 0.1258(5) 0.3401(16) 0.111(6) Uani 1 1 d . . .
C53 C 0.3471(5) 0.1516(4) 0.2880(15) 0.103(5) Uani 1 1 d . . .
H53 H 0.3436 0.1822 0.3157 0.124 Uiso 1 1 calc R . .
C54 C 0.3177(4) 0.1327(4) 0.1960(13) 0.080(4) Uani 1 1 d . . .
H54 H 0.2954 0.1519 0.1568 0.095 Uiso 1 1 calc R . .
C55 C 0.3554(5) -0.0790(5) 0.0713(13) 0.121(6) Uani 1 1 d D . .
H55A H 0.3223 -0.0760 0.0837 0.145 Uiso 1 1 calc R . .
H55B H 0.3699 -0.0499 0.0961 0.145 Uiso 1 1 calc R . .
C56 C 0.3663(5) -0.0915(4) -0.0709(12) 0.110(5) Uani 1 1 d D . .
H56A H 0.3552 -0.1224 -0.0908 0.132 Uiso 1 1 calc R . .
H56B H 0.3994 -0.0910 -0.0851 0.132 Uiso 1 1 calc R . .
C57 C 0.3431(5) -0.0571(4) -0.1664(13) 0.086(4) Uani 1 1 d D . .
C58 C 0.3372(4) 0.0156(4) -0.2775(12) 0.069(3) Uani 1 1 d . . .
H58 H 0.3489 0.0453 -0.2887 0.082 Uiso 1 1 calc R . .
C59 C 0.3583(4) -0.0135(5) -0.1882(14) 0.094(5) Uani 1 1 d . . .
H59 H 0.3843 -0.0033 -0.1399 0.113 Uiso 1 1 calc R . .
C60 C 0.3051(5) -0.0679(4) -0.2321(12) 0.084(4) Uani 1 1 d . . .
H60 H 0.2911 -0.0963 -0.2155 0.101 Uiso 1 1 calc R . .
C61 C 0.2857(4) -0.0377(4) -0.3254(12) 0.070(3) Uani 1 1 d . . .
H61 H 0.2599 -0.0473 -0.3758 0.084 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 0.0589(8) 0.0580(8) 0.0342(7) 0.0027(6) -0.0066(7) -0.0070(6)
Cu2 0.0632(8) 0.0536(8) 0.0319(7) -0.0003(6) -0.0057(7) 0.0060(6)
P1 0.0312(13) 0.0402(15) 0.0223(14) 0.0009(12) -0.0030(12) -0.0048(12)
P2 0.0391(14) 0.0324(14) 0.0219(15) 0.0022(11) -0.0036(12) -0.0053(11)
P3 0.0378(14) 0.0364(15) 0.0236(15) 0.0038(11) -0.0022(13) 0.0076(12)
P4 0.0493(15) 0.0310(14) 0.0209(15) 0.0002(11) -0.0044(12) 0.0023(12)
O1 0.046(4) 0.046(4) 0.023(4) -0.002(3) 0.001(3) 0.006(3)
O2 0.041(4) 0.056(4) 0.023(4) -0.010(3) -0.002(3) -0.008(3)
O3 0.045(4) 0.048(4) 0.024(4) 0.008(3) -0.004(3) -0.016(3)
O4 0.038(4) 0.041(4) 0.020(3) 0.003(3) -0.004(3) -0.003(3)
O5 0.046(4) 0.046(4) 0.030(4) 0.010(3) -0.011(3) -0.018(3)
O6 0.059(4) 0.033(3) 0.025(4) -0.003(3) -0.010(3) 0.013(3)
O7 0.044(4) 0.040(4) 0.028(4) 0.009(3) -0.002(3) 0.004(3)
O8 0.075(5) 0.030(3) 0.025(4) 0.000(3) -0.011(3) 0.018(3)
N1 0.050(6) 0.048(6) 0.038(5) 0.001(4) -0.017(4) -0.002(5)
N2 0.062(6) 0.036(5) 0.021(5) -0.001(4) -0.012(4) 0.003(4)
C1 0.040(6) 0.042(6) 0.030(6) -0.002(5) 0.001(5) 0.001(5)
C2 0.035(5) 0.047(6) 0.020(5) -0.002(4) 0.003(4) -0.004(4)
C10 0.036(6) 0.041(6) 0.032(6) -0.003(5) 0.009(5) -0.002(5)
C11 0.036(6) 0.068(8) 0.084(9) 0.022(7) -0.010(6) -0.012(5)
C12 0.055(8) 0.054(9) 0.145(14) 0.061(9) 0.006(8) 0.005(6)
C13 0.082(10) 0.039(8) 0.144(15) -0.014(10) 0.046(10) -0.017(7)
C14 0.112(11) 0.053(9) 0.077(10) 0.017(7) 0.000(9) -0.026(8)
C15 0.075(8) 0.056(8) 0.044(7) 0.006(6) -0.002(6) -0.020(6)
C20 0.036(6) 0.050(7) 0.035(6) 0.011(5) 0.001(5) 0.002(5)
C21 0.053(8) 0.086(8) 0.068(9) -0.011(7) 0.014(7) -0.014(6)
C22 0.064(9) 0.098(9) 0.101(11) -0.033(9) 0.034(9) 0.000(7)
C23 0.054(8) 0.128(12) 0.071(10) 0.026(9) 0.005(8) -0.023(9)
C24 0.038(8) 0.115(11) 0.084(10) -0.009(9) 0.007(7) -0.030(7)
C25 0.054(7) 0.067(7) 0.040(7) -0.005(6) 0.001(6) -0.018(6)
C30 0.048(6) 0.047(6) 0.033(6) 0.004(5) -0.005(5) -0.002(5)
C31 0.055(7) 0.040(6) 0.037(6) 0.008(5) -0.008(6) 0.007(5)
C32 0.067(8) 0.059(7) 0.038(7) 0.006(6) -0.016(6) 0.030(6)
C33 0.061(8) 0.076(8) 0.055(9) -0.016(7) -0.003(7) 0.025(6)
C34 0.061(7) 0.101(9) 0.035(7) 0.005(7) 0.009(6) 0.020(7)
C35 0.055(7) 0.067(7) 0.032(6) 0.001(6) -0.004(6) 0.019(6)
C40 0.046(6) 0.032(5) 0.034(6) 0.004(6) 0.004(5) -0.002(4)
C41 0.101(9) 0.051(8) 0.045(7) -0.002(6) 0.022(6) -0.004(7)
C42 0.102(10) 0.035(8) 0.120(14) 0.015(8) 0.045(10) -0.001(7)
C43 0.063(8) 0.061(9) 0.090(11) -0.025(9) 0.002(7) -0.023(7)
C44 0.106(10) 0.052(8) 0.071(9) -0.022(8) -0.039(8) -0.018(7)
C45 0.074(8) 0.059(8) 0.059(9) 0.002(6) -0.022(6) 0.003(6)
C50 0.087(10) 0.059(8) 0.120(12) -0.039(9) -0.043(9) 0.001(7)
C51 0.137(14) 0.100(13) 0.200(19) -0.028(12) -0.140(14) 0.008(10)
C52 0.147(14) 0.070(10) 0.116(12) -0.006(9) -0.090(11) -0.040(10)
C53 0.146(13) 0.058(8) 0.105(11) -0.013(8) -0.083(11) -0.007(9)
C54 0.100(11) 0.045(8) 0.094(11) 0.004(7) -0.039(9) -0.001(7)
C55 0.130(13) 0.134(14) 0.097(13) 0.037(11) 0.020(10) 0.048(11)
C56 0.140(14) 0.123(12) 0.067(11) 0.007(9) -0.049(10) 0.033(10)
C57 0.103(11) 0.078(10) 0.078(10) 0.035(8) -0.052(9) 0.010(8)
C58 0.075(9) 0.058(7) 0.073(9) 0.020(7) -0.018(8) -0.002(7)
C59 0.101(10) 0.084(10) 0.098(11) 0.035(9) -0.058(9) -0.002(8)
C60 0.130(12) 0.059(8) 0.062(8) 0.036(7) -0.040(9) -0.011(8)
C61 0.088(9) 0.058(8) 0.065(9) -0.001(7) -0.029(7) -0.010(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 O3 1.944(5) . ?
Cu1 O7 1.951(5) 1_556 ?
Cu1 O5 1.952(5) . ?
Cu1 N1 2.014(8) . ?
Cu1 O1 2.255(6) . ?
Cu2 O8 1.941(5) . ?
Cu2 O6 1.950(5) 1_554 ?
Cu2 O4 1.967(5) . ?
Cu2 N2 2.018(7) . ?
Cu2 O2 2.229(6) . ?
P1 O2 1.491(6) . ?
P1 O5 1.497(6) . ?
P1 C1 1.774(9) . ?
P1 C20 1.804(9) . ?
P2 O4 1.500(6) . ?
P2 O3 1.507(6) . ?
P2 C1 1.784(8) . ?
P2 C10 1.800(9) . ?
P3 O1 1.486(6) . ?
P3 O6 1.496(6) . ?
P3 C30 1.787(9) . ?
P3 C2 1.823(8) 1_556 ?
P4 O8 1.494(6) . ?
P4 O7 1.506(6) . ?
P4 C40 1.792(9) . ?
P4 C2 1.804(8) . ?
O6 Cu2 1.950(5) 1_556 ?
O7 Cu1 1.951(5) 1_554 ?
N1 C54 1.300(12) . ?
N1 C50 1.303(13) . ?
N2 C58 1.307(12) . ?
N2 C61 1.324(12) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 P3 1.823(8) 1_554 ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C10 C11 1.369(13) . ?
C10 C15 1.387(12) . ?
C11 C12 1.414(15) . ?
C11 H11 0.9500 . ?
C12 C13 1.388(18) . ?
C12 H12 0.9500 . ?
C13 C14 1.311(18) . ?
C13 H13 0.9500 . ?
C14 C15 1.371(14) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
C20 C21 1.376(13) . ?
C20 C25 1.374(12) . ?
C21 C22 1.396(14) . ?
C21 H21 0.9500 . ?
C22 C23 1.354(16) . ?
C22 H22 0.9500 . ?
C23 C24 1.356(16) . ?
C23 H23 0.9500 . ?
C24 C25 1.383(13) . ?
C24 H24 0.9500 . ?
C25 H25 0.9500 . ?
C30 C31 1.377(12) . ?
C30 C35 1.398(13) . ?
C31 C32 1.361(12) . ?
C31 H31 0.9500 . ?
C32 C33 1.339(14) . ?
C32 H32 0.9500 . ?
C33 C34 1.390(14) . ?
C33 H33 0.9500 . ?
C34 C35 1.374(12) . ?
C34 H34 0.9500 . ?
C35 H35 0.9500 . ?
C40 C41 1.323(13) . ?
C40 C45 1.389(12) . ?
C41 C42 1.426(15) . ?
C41 H41 0.9500 . ?
C42 C43 1.329(17) . ?
C42 H42 0.9500 . ?
C43 C44 1.344(16) . ?
C43 H43 0.9500 . ?
C44 C45 1.360(14) . ?
C44 H44 0.9500 . ?
C45 H45 0.9500 . ?
C50 C51 1.396(16) . ?
C50 H50 0.9500 . ?
C51 C52 1.359(17) . ?
C51 H51 0.9500 . ?
C52 C53 1.381(17) . ?
C52 C55 1.545(9) 7 ?
C53 C54 1.370(15) . ?
C53 H53 0.9500 . ?
C54 H54 0.9500 . ?
C55 C56 1.470(9) . ?
C55 C52 1.545(9) 8_545 ?
C55 H55A 0.9900 . ?
C55 H55B 0.9900 . ?
C56 C57 1.540(9) . ?
C56 H56A 0.9900 . ?
C56 H56B 0.9900 . ?
C57 C60 1.334(15) . ?
C57 C59 1.380(16) . ?
C58 C59 1.374(14) . ?
C58 H58 0.9500 . ?
C59 H59 0.9500 . ?
C60 C61 1.398(14) . ?
C60 H60 0.9500 . ?
C61 H61 0.9500 . ?

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
O3 Cu1 O7 155.0(3) . 1_556 ?
O3 Cu1 O5 95.3(2) . . ?
O7 Cu1 O5 89.1(2) 1_556 . ?
O3 Cu1 N1 87.2(3) . . ?
O7 Cu1 N1 87.7(3) 1_556 . ?
O5 Cu1 N1 176.7(3) . . ?
O3 Cu1 O1 105.6(2) . . ?
O7 Cu1 O1 98.7(2) 1_556 . ?
O5 Cu1 O1 92.7(2) . . ?
N1 Cu1 O1 88.7(3) . . ?
O8 Cu2 O6 93.1(2) . 1_554 ?
O8 Cu2 O4 160.8(3) . . ?
O6 Cu2 O4 89.2(2) 1_554 . ?
O8 Cu2 N2 87.8(3) . . ?
O6 Cu2 N2 176.2(3) 1_554 . ?
O4 Cu2 N2 88.7(3) . . ?
O8 Cu2 O2 100.0(2) . . ?
O6 Cu2 O2 95.4(2) 1_554 . ?
O4 Cu2 O2 98.7(2) . . ?
N2 Cu2 O2 88.0(3) . . ?
O2 P1 O5 117.7(3) . . ?
O2 P1 C1 108.4(4) . . ?
O5 P1 C1 106.1(4) . . ?
O2 P1 C20 108.8(4) . . ?
O5 P1 C20 109.3(4) . . ?
C1 P1 C20 106.0(4) . . ?
O4 P2 O3 117.5(3) . . ?
O4 P2 C1 109.0(4) . . ?
O3 P2 C1 106.9(4) . . ?
O4 P2 C10 108.1(4) . . ?
O3 P2 C10 107.0(4) . . ?
C1 P2 C10 107.9(4) . . ?
O1 P3 O6 117.1(3) . . ?
O1 P3 C30 109.5(4) . . ?
O6 P3 C30 108.0(4) . . ?
O1 P3 C2 108.3(4) . 1_556 ?
O6 P3 C2 106.9(4) . 1_556 ?
C30 P3 C2 106.6(4) . 1_556 ?
O8 P4 O7 117.3(4) . . ?
O8 P4 C40 106.8(4) . . ?
O7 P4 C40 106.2(4) . . ?
O8 P4 C2 107.6(4) . . ?
O7 P4 C2 109.0(4) . . ?
C40 P4 C2 109.7(4) . . ?
P3 O1 Cu1 118.4(3) . . ?
P1 O2 Cu2 121.4(3) . . ?
P2 O3 Cu1 130.4(3) . . ?
P2 O4 Cu2 130.9(3) . . ?
P1 O5 Cu1 134.4(4) . . ?
P3 O6 Cu2 138.1(3) . 1_556 ?
P4 O7 Cu1 132.2(4) . 1_554 ?
P4 O8 Cu2 130.9(3) . . ?
C54 N1 C50 116.2(9) . . ?
C54 N1 Cu1 120.9(8) . . ?
C50 N1 Cu1 122.5(7) . . ?
C58 N2 C61 116.6(9) . . ?
C58 N2 Cu2 125.4(7) . . ?
C61 N2 Cu2 117.7(7) . . ?
P1 C1 P2 112.8(5) . . ?
P1 C1 H1A 109.0 . . ?
P2 C1 H1A 109.0 . . ?
P1 C1 H1B 109.0 . . ?
P2 C1 H1B 109.0 . . ?
H1A C1 H1B 107.8 . . ?
P4 C2 P3 109.1(4) . 1_554 ?
P4 C2 H2A 109.9 . . ?
P3 C2 H2A 109.9 1_554 . ?
P4 C2 H2B 109.9 . . ?
P3 C2 H2B 109.9 1_554 . ?
H2A C2 H2B 108.3 . . ?
C11 C10 C15 118.9(9) . . ?
C11 C10 P2 119.5(8) . . ?
C15 C10 P2 121.6(8) . . ?
C10 C11 C12 120.1(11) . . ?
C10 C11 H11 119.9 . . ?
C12 C11 H11 119.9 . . ?
C13 C12 C11 117.6(12) . . ?
C13 C12 H12 121.2 . . ?
C11 C12 H12 121.2 . . ?
C14 C13 C12 122.0(12) . . ?
C14 C13 H13 119.0 . . ?
C12 C13 H13 119.0 . . ?
C13 C14 C15 120.8(13) . . ?
C13 C14 H14 119.6 . . ?
C15 C14 H14 119.6 . . ?
C14 C15 C10 120.3(11) . . ?
C14 C15 H15 119.8 . . ?
C10 C15 H15 119.8 . . ?
C21 C20 C25 118.2(9) . . ?
C21 C20 P1 120.1(8) . . ?
C25 C20 P1 121.7(8) . . ?
C20 C21 C22 119.4(11) . . ?
C20 C21 H21 120.3 . . ?
C22 C21 H21 120.3 . . ?
C23 C22 C21 121.0(12) . . ?
C23 C22 H22 119.5 . . ?
C21 C22 H22 119.5 . . ?
C24 C23 C22 120.1(12) . . ?
C24 C23 H23 120.0 . . ?
C22 C23 H23 120.0 . . ?
C23 C24 C25 119.2(11) . . ?
C23 C24 H24 120.4 . . ?
C25 C24 H24 120.4 . . ?
C20 C25 C24 121.8(10) . . ?
C20 C25 H25 119.1 . . ?
C24 C25 H25 119.1 . . ?
C31 C30 C35 116.7(9) . . ?
C31 C30 P3 123.0(8) . . ?
C35 C30 P3 120.3(7) . . ?
C32 C31 C30 122.3(10) . . ?
C32 C31 H31 118.9 . . ?
C30 C31 H31 118.9 . . ?
C33 C32 C31 120.0(10) . . ?
C33 C32 H32 120.0 . . ?
C31 C32 H32 120.0 . . ?
C32 C33 C34 121.0(10) . . ?
C32 C33 H33 119.5 . . ?
C34 C33 H33 119.5 . . ?
C35 C34 C33 118.4(10) . . ?
C35 C34 H34 120.8 . . ?
C33 C34 H34 120.8 . . ?
C34 C35 C30 121.6(9) . . ?
C34 C35 H35 119.2 . . ?
C30 C35 H35 119.2 . . ?
C41 C40 C45 117.9(9) . . ?
C41 C40 P4 122.1(8) . . ?
C45 C40 P4 119.8(8) . . ?
C40 C41 C42 119.8(11) . . ?
C40 C41 H41 120.1 . . ?
C42 C41 H41 120.1 . . ?
C43 C42 C41 121.2(13) . . ?
C43 C42 H42 119.4 . . ?
C41 C42 H42 119.4 . . ?
C42 C43 C44 118.9(12) . . ?
C42 C43 H43 120.5 . . ?
C44 C43 H43 120.5 . . ?
C43 C44 C45 120.7(12) . . ?
C43 C44 H44 119.6 . . ?
C45 C44 H44 119.6 . . ?
C44 C45 C40 121.5(11) . . ?
C44 C45 H45 119.3 . . ?
C40 C45 H45 119.3 . . ?
N1 C50 C51 122.7(11) . . ?
N1 C50 H50 118.7 . . ?
C51 C50 H50 118.7 . . ?
C52 C51 C50 121.0(13) . . ?
C52 C51 H51 119.5 . . ?
C50 C51 H51 119.5 . . ?
C51 C52 C53 115.1(10) . . ?
C51 C52 C55 120.7(14) . 7 ?
C53 C52 C55 124.3(13) . 7 ?
C54 C53 C52 119.3(12) . . ?
C54 C53 H53 120.4 . . ?
C52 C53 H53 120.4 . . ?
N1 C54 C53 125.3(11) . . ?
N1 C54 H54 117.4 . . ?
C53 C54 H54 117.4 . . ?
C56 C55 C52 104.9(10) . 8_545 ?
C56 C55 H55A 110.8 . . ?
C52 C55 H55A 110.8 8_545 . ?
C56 C55 H55B 110.8 . . ?
C52 C55 H55B 110.8 8_545 . ?
H55A C55 H55B 108.8 . . ?
C55 C56 C57 107.6(10) . . ?
C55 C56 H56A 110.2 . . ?
C57 C56 H56A 110.2 . . ?
C55 C56 H56B 110.2 . . ?
C57 C56 H56B 110.2 . . ?
H56A C56 H56B 108.5 . . ?
C60 C57 C59 115.1(10) . . ?
C60 C57 C56 120.4(12) . . ?
C59 C57 C56 124.5(12) . . ?
N2 C58 C59 122.0(11) . . ?
N2 C58 H58 119.0 . . ?
C59 C58 H58 119.0 . . ?
C58 C59 C57 122.3(11) . . ?
C58 C59 H59 118.9 . . ?
C57 C59 H59 118.9 . . ?
C57 C60 C61 120.3(11) . . ?
C57 C60 H60 119.9 . . ?
C61 C60 H60 119.9 . . ?
N2 C61 C60 123.5(10) . . ?
N2 C61 H61 118.2 . . ?
C60 C61 H61 118.2 . . ?

_diffrn_measured_fraction_theta_max 0.989
_diffrn_reflns_theta_full        21.03
_diffrn_measured_fraction_theta_full 0.989
_refine_diff_density_max         0.331
_refine_diff_density_min         -0.407
_refine_diff_density_rms         0.066

#===END