# Electronic Supplementary Material for CrystEngComm
# This journal is (c) The Royal Society of Chemistry 2009

data_paper
_journal_name_full               CrystEngComm
_journal_coden_cambridge         1350

_publ_contact_author             
; Prof Mir Wais Hosseini
Laboratoire de Chimie de Coordination Organique,
UMR CNRS 7140, Université de Strasbourg,
F-67000 Strasbourg, France
;
_publ_contact_author_email       hosseini@chimie.u-strasbg.fr
_publ_contact_author_fax         '33 3 90 24 13 23'
_publ_contact_author_phone       '33 3 90 24 13 25'
_publ_requested_category         FM

loop_
_publ_author_name
_publ_author_address

S.A.Baudron
; Laboratoire de Chimie de Coordination Organique,
UMR CNRS 7140, Université Louis Pasteur,
F-67000 Strasbourg, France
;
D.Salazar-Mendoza
; Laboratoire de Chimie de Coordination Organique,
UMR CNRS 7140, Université Louis Pasteur,
F-67000 Strasbourg, France
;
M.W.Hosseini
; Laboratoire de Chimie de Coordination Organique,
UMR CNRS 7140, Université Louis Pasteur,
F-67000 Strasbourg, France
;

_publ_section_title              
; Combination of primary amide and dipyrrin for the
elaboration of extended architectures built upon
both coordination and hydrogen bonding
;
_publ_contact_author_name        'Prof Mir Wais Hosseini'

###Material relevant to compound 1 at 173K ##

data_compound1
_database_code_depnum_ccdc_archive 'CCDC 716997'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C16 H13 N3 O'
_chemical_formula_sum            'C16 H13 N3 O'
_chemical_formula_weight         263.29

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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'C2/c '
_symmetry_space_group_name_Hall  '-C 2yc'

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                   36.3670(16)
_cell_length_b                   9.2645(3)
_cell_length_c                   16.8012(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 109.829(2)
_cell_angle_gamma                90.00
_cell_volume                     5325.1(4)
_cell_formula_units_Z            16
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    3778
_cell_measurement_theta_min      2.38
_cell_measurement_theta_max      24.26

_exptl_crystal_description       platelet
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.314
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2208
_exptl_absorpt_coefficient_mu    0.085
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9667
_exptl_absorpt_correction_T_max  0.9899
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            21337
_diffrn_reflns_av_R_equivalents  0.0412
_diffrn_reflns_av_sigmaI/netI    0.0502
_diffrn_reflns_limit_h_min       -47
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.19
_diffrn_reflns_theta_max         27.54
_reflns_number_total             6119
_reflns_number_gt                3926
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² 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/[σ²(Fo²)+(0.0526P)²+5.2363P] where P=(Fo²+2Fc²)/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     SHELXL
_refine_ls_extinction_coef       0.00074(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         6119
_refine_ls_number_parameters     362
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0958
_refine_ls_R_factor_gt           0.0555
_refine_ls_wR_factor_ref         0.1534
_refine_ls_wR_factor_gt          0.1234
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_restrained_S_all      1.028
_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
C1 C 0.02985(8) 0.6214(3) 0.56504(16) 0.0547(7) Uani 1 1 d . . .
H1A H 0.0127 0.5486 0.5676 0.066 Uiso 1 1 calc R . .
C2 C 0.06302(8) 0.6015(3) 0.54361(15) 0.0485(6) Uani 1 1 d . . .
H2 H 0.0718 0.5149 0.5285 0.058 Uiso 1 1 calc R . .
C3 C 0.08051(7) 0.7354(2) 0.54909(14) 0.0398(5) Uani 1 1 d . . .
H3 H 0.1035 0.7552 0.5387 0.048 Uiso 1 1 calc R . .
C4 C 0.05743(6) 0.8358(2) 0.57307(13) 0.0353(5) Uani 1 1 d . . .
C5 C 0.06318(6) 0.9862(2) 0.59025(13) 0.0322(5) Uani 1 1 d . . .
C6 C 0.03814(6) 1.0736(2) 0.61462(14) 0.0378(5) Uani 1 1 d . . .
C7 C 0.04242(8) 1.2226(3) 0.63726(16) 0.0481(6) Uani 1 1 d . . .
H7 H 0.0631 1.2825 0.6385 0.058 Uiso 1 1 calc R . .
C8 C 0.01021(9) 1.2601(3) 0.65674(19) 0.0601(8) Uani 1 1 d . . .
H8 H 0.0046 1.3506 0.6736 0.072 Uiso 1 1 calc R . .
C9 C -0.01292(8) 1.1341(3) 0.64615(16) 0.0588(8) Uani 1 1 d . . .
H9 H -0.0367 1.1305 0.6553 0.071 Uiso 1 1 calc R . .
C10 C 0.09881(6) 1.0489(2) 0.57934(13) 0.0315(5) Uani 1 1 d . . .
C11 C 0.13582(6) 1.0053(2) 0.63076(14) 0.0385(5) Uani 1 1 d . . .
H11 H 0.1384 0.9425 0.6755 0.046 Uiso 1 1 calc R . .
C12 C 0.16882(6) 1.0541(2) 0.61609(14) 0.0369(5) Uani 1 1 d . . .
H12 H 0.1934 1.0235 0.6508 0.044 Uiso 1 1 calc R . .
C13 C 0.16561(6) 1.1485(2) 0.54984(13) 0.0297(4) Uani 1 1 d . . .
C14 C 0.12891(6) 1.1970(2) 0.50062(13) 0.0326(5) Uani 1 1 d . . .
H14 H 0.1265 1.2630 0.4574 0.039 Uiso 1 1 calc R . .
C15 C 0.09572(6) 1.1483(2) 0.51504(13) 0.0336(5) Uani 1 1 d . . .
H15 H 0.0713 1.1819 0.4817 0.040 Uiso 1 1 calc R . .
C16 C 0.20049(6) 1.1963(2) 0.52903(13) 0.0308(5) Uani 1 1 d . . .
N1 N 0.02608(6) 0.7612(2) 0.58159(12) 0.0453(5) Uani 1 1 d . . .
H1 H 0.0073 0.7981 0.5952 0.054 Uiso 1 1 calc R . .
N2 N 0.00307(6) 1.0223(2) 0.62188(12) 0.0487(5) Uani 1 1 d . . .
N3 N 0.23231(5) 1.1163(2) 0.55757(13) 0.0427(5) Uani 1 1 d . . .
H3A H 0.2529 1.1400 0.5466 0.051 Uiso 1 1 calc R . .
H3B H 0.2324 1.0405 0.5872 0.051 Uiso 1 1 calc R . .
O1 O 0.19906(4) 1.30699(15) 0.48593(10) 0.0371(4) Uani 1 1 d . . .
C17 C 0.13276(10) 0.1393(3) 0.89269(19) 0.0642(8) Uani 1 1 d . . .
H17 H 0.1233 0.0735 0.9229 0.077 Uiso 1 1 calc R . .
C18 C 0.16430(9) 0.1128(3) 0.86431(18) 0.0620(8) Uani 1 1 d . . .
H18 H 0.1790 0.0286 0.8718 0.074 Uiso 1 1 calc R . .
C19 C 0.16911(8) 0.2351(3) 0.82353(16) 0.0490(6) Uani 1 1 d . . .
H19 H 0.1879 0.2504 0.7981 0.059 Uiso 1 1 calc R . .
C20 C 0.14004(7) 0.3347(2) 0.82726(14) 0.0400(5) Uani 1 1 d . . .
C21 C 0.13293(6) 0.4756(2) 0.79577(13) 0.0373(5) Uani 1 1 d . . .
C22 C 0.10335(6) 0.5658(3) 0.80463(13) 0.0375(5) Uani 1 1 d . . .
C23 C 0.09193(7) 0.7037(3) 0.77236(14) 0.0452(6) Uani 1 1 d . . .
H23 H 0.1040 0.7596 0.7424 0.054 Uiso 1 1 calc R . .
C24 C 0.05964(8) 0.7426(3) 0.79256(15) 0.0526(7) Uani 1 1 d . . .
H24 H 0.0458 0.8288 0.7790 0.063 Uiso 1 1 calc R . .
C25 C 0.05188(7) 0.6269(3) 0.83743(16) 0.0511(7) Uani 1 1 d . . .
H25 H 0.0314 0.6238 0.8586 0.061 Uiso 1 1 calc R . .
C26 C 0.15639(6) 0.5311(2) 0.74454(13) 0.0349(5) Uani 1 1 d . . .
C27 C 0.15257(7) 0.4640(2) 0.66812(15) 0.0399(5) Uani 1 1 d . . .
H27 H 0.1367 0.3829 0.6516 0.048 Uiso 1 1 calc R . .
C28 C 0.17217(7) 0.5169(2) 0.61629(15) 0.0398(5) Uani 1 1 d . . .
H28 H 0.1686 0.4727 0.5645 0.048 Uiso 1 1 calc R . .
C29 C 0.19691(6) 0.6347(2) 0.64077(14) 0.0343(5) Uani 1 1 d . . .
C30 C 0.20139(7) 0.6996(2) 0.71810(14) 0.0388(5) Uani 1 1 d . . .
H30 H 0.2183 0.7775 0.7360 0.047 Uiso 1 1 calc R . .
C31 C 0.18102(7) 0.6498(2) 0.76885(14) 0.0387(5) Uani 1 1 d . . .
H31 H 0.1839 0.6962 0.8197 0.046 Uiso 1 1 calc R . .
C32 C 0.21859(7) 0.6943(2) 0.58598(15) 0.0372(5) Uani 1 1 d . . .
N4 N 0.11826(7) 0.2698(2) 0.87092(13) 0.0523(6) Uani 1 1 d . . .
H4 H 0.0989 0.3076 0.8818 0.063 Uiso 1 1 calc R . .
N5 N 0.07791(6) 0.5206(2) 0.84594(13) 0.0462(5) Uani 1 1 d . . .
N6 N 0.21900(7) 0.6132(2) 0.52127(14) 0.0520(6) Uani 1 1 d . . .
H6A H 0.2313 0.6422 0.4885 0.062 Uiso 1 1 calc R . .
H6B H 0.2070 0.5316 0.5120 0.062 Uiso 1 1 calc R . .
O2 O 0.23540(5) 0.81211(16) 0.60163(11) 0.0439(4) Uani 1 1 d . . .


_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
C1 N1 1.341(3) . ?
C1 C2 1.383(4) . ?
C1 H1A 0.9300 . ?
C2 C3 1.383(3) . ?
C2 H2 0.9300 . ?
C3 C4 1.401(3) . ?
C3 H3 0.9300 . ?
C4 N1 1.382(3) . ?
C4 C5 1.424(3) . ?
C5 C6 1.380(3) . ?
C5 C10 1.487(3) . ?
C6 N2 1.405(3) . ?
C6 C7 1.426(3) . ?
C7 C8 1.363(3) . ?
C7 H7 0.9300 . ?
C8 C9 1.414(4) . ?
C8 H8 0.9300 . ?
C9 N2 1.319(3) . ?
C9 H9 0.9300 . ?
C10 C11 1.390(3) . ?
C10 C15 1.394(3) . ?
C11 C12 1.381(3) . ?
C11 H11 0.9300 . ?
C12 C13 1.389(3) . ?
C12 H12 0.9300 . ?
C13 C14 1.385(3) . ?
C13 C16 1.492(3) . ?
C14 C15 1.385(3) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 O1 1.247(2) . ?
C16 N3 1.320(3) . ?
N1 H1 0.8600 . ?
N3 H3A 0.8600 . ?
N3 H3B 0.8600 . ?
C17 N4 1.320(3) . ?
C17 C18 1.405(4) . ?
C17 H17 0.9300 . ?
C18 C19 1.366(3) . ?
C18 H18 0.9300 . ?
C19 C20 1.420(3) . ?
C19 H19 0.9300 . ?
C20 N4 1.386(3) . ?
C20 C21 1.399(3) . ?
C21 C22 1.410(3) . ?
C21 C26 1.494(3) . ?
C22 C23 1.395(3) . ?
C22 N5 1.396(3) . ?
C23 C24 1.376(3) . ?
C23 H23 0.9300 . ?
C24 C25 1.394(4) . ?
C24 H24 0.9300 . ?
C25 N5 1.339(3) . ?
C25 H25 0.9300 . ?
C26 C31 1.390(3) . ?
C26 C27 1.390(3) . ?
C27 C28 1.388(3) . ?
C27 H27 0.9300 . ?
C28 C29 1.385(3) . ?
C28 H28 0.9300 . ?
C29 C30 1.390(3) . ?
C29 C32 1.505(3) . ?
C30 C31 1.384(3) . ?
C30 H30 0.9300 . ?
C31 H31 0.9300 . ?
C32 O2 1.235(3) . ?
C32 N6 1.326(3) . ?
N4 H4 0.8600 . ?
N6 H6A 0.8600 . ?
N6 H6B 0.8600 . ?

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 C1 C2 110.0(2) . . ?
N1 C1 H1A 125.0 . . ?
C2 C1 H1A 125.0 . . ?
C3 C2 C1 106.5(2) . . ?
C3 C2 H2 126.7 . . ?
C1 C2 H2 126.7 . . ?
C2 C3 C4 107.9(2) . . ?
C2 C3 H3 126.0 . . ?
C4 C3 H3 126.0 . . ?
N1 C4 C3 107.07(19) . . ?
N1 C4 C5 122.6(2) . . ?
C3 C4 C5 130.3(2) . . ?
C6 C5 C4 124.6(2) . . ?
C6 C5 C10 119.85(19) . . ?
C4 C5 C10 115.55(18) . . ?
C5 C6 N2 122.5(2) . . ?
C5 C6 C7 128.6(2) . . ?
N2 C6 C7 108.9(2) . . ?
C8 C7 C6 106.6(2) . . ?
C8 C7 H7 126.7 . . ?
C6 C7 H7 126.7 . . ?
C7 C8 C9 106.4(2) . . ?
C7 C8 H8 126.8 . . ?
C9 C8 H8 126.8 . . ?
N2 C9 C8 112.4(2) . . ?
N2 C9 H9 123.8 . . ?
C8 C9 H9 123.8 . . ?
C11 C10 C15 118.70(19) . . ?
C11 C10 C5 120.67(18) . . ?
C15 C10 C5 120.58(19) . . ?
C12 C11 C10 120.71(19) . . ?
C12 C11 H11 119.6 . . ?
C10 C11 H11 119.6 . . ?
C11 C12 C13 120.5(2) . . ?
C11 C12 H12 119.8 . . ?
C13 C12 H12 119.8 . . ?
C14 C13 C12 118.99(18) . . ?
C14 C13 C16 119.18(18) . . ?
C12 C13 C16 121.82(19) . . ?
C15 C14 C13 120.69(19) . . ?
C15 C14 H14 119.7 . . ?
C13 C14 H14 119.7 . . ?
C14 C15 C10 120.3(2) . . ?
C14 C15 H15 119.8 . . ?
C10 C15 H15 119.8 . . ?
O1 C16 N3 122.11(19) . . ?
O1 C16 C13 120.57(19) . . ?
N3 C16 C13 117.31(18) . . ?
C1 N1 C4 108.4(2) . . ?
C1 N1 H1 125.8 . . ?
C4 N1 H1 125.8 . . ?
C9 N2 C6 105.6(2) . . ?
C16 N3 H3A 120.0 . . ?
C16 N3 H3B 120.0 . . ?
H3A N3 H3B 120.0 . . ?
N4 C17 C18 111.2(2) . . ?
N4 C17 H17 124.4 . . ?
C18 C17 H17 124.4 . . ?
C19 C18 C17 106.4(2) . . ?
C19 C18 H18 126.8 . . ?
C17 C18 H18 126.8 . . ?
C18 C19 C20 107.0(2) . . ?
C18 C19 H19 126.5 . . ?
C20 C19 H19 126.5 . . ?
N4 C20 C21 122.6(2) . . ?
N4 C20 C19 108.0(2) . . ?
C21 C20 C19 129.4(2) . . ?
C20 C21 C22 124.3(2) . . ?
C20 C21 C26 118.1(2) . . ?
C22 C21 C26 117.5(2) . . ?
C23 C22 N5 107.9(2) . . ?
C23 C22 C21 129.7(2) . . ?
N5 C22 C21 122.2(2) . . ?
C24 C23 C22 108.1(2) . . ?
C24 C23 H23 126.0 . . ?
C22 C23 H23 126.0 . . ?
C23 C24 C25 106.2(2) . . ?
C23 C24 H24 126.9 . . ?
C25 C24 H24 126.9 . . ?
N5 C25 C24 111.0(2) . . ?
N5 C25 H25 124.5 . . ?
C24 C25 H25 124.5 . . ?
C31 C26 C27 118.52(19) . . ?
C31 C26 C21 122.7(2) . . ?
C27 C26 C21 118.7(2) . . ?
C28 C27 C26 120.7(2) . . ?
C28 C27 H27 119.7 . . ?
C26 C27 H27 119.7 . . ?
C29 C28 C27 120.8(2) . . ?
C29 C28 H28 119.6 . . ?
C27 C28 H28 119.6 . . ?
C28 C29 C30 118.45(19) . . ?
C28 C29 C32 122.0(2) . . ?
C30 C29 C32 119.6(2) . . ?
C31 C30 C29 120.9(2) . . ?
C31 C30 H30 119.5 . . ?
C29 C30 H30 119.5 . . ?
C30 C31 C26 120.6(2) . . ?
C30 C31 H31 119.7 . . ?
C26 C31 H31 119.7 . . ?
O2 C32 N6 122.2(2) . . ?
O2 C32 C29 121.2(2) . . ?
N6 C32 C29 116.6(2) . . ?
C17 N4 C20 107.3(2) . . ?
C17 N4 H4 126.3 . . ?
C20 N4 H4 126.3 . . ?
C25 N5 C22 106.9(2) . . ?
C32 N6 H6A 120.0 . . ?
C32 N6 H6B 120.0 . . ?
H6A N6 H6B 120.0 . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        27.54
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.244
_refine_diff_density_min         -0.334
_refine_diff_density_rms         0.051

#===END

###Material relevant to compound 2 at 173K ########

data_compound2
_database_code_depnum_ccdc_archive 'CCDC 716998'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C16 H15 N3 O'
_chemical_formula_sum            'C16 H15 N3 O'
_chemical_formula_weight         265.31

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'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P-1 '
_symmetry_space_group_name_Hall  '-P 1'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.3130(3)
_cell_length_b                   9.5783(3)
_cell_length_c                   9.8020(3)
_cell_angle_alpha                80.064(2)
_cell_angle_beta                 65.596(2)
_cell_angle_gamma                74.133(2)
_cell_volume                     682.08(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    2747
_cell_measurement_theta_min      2.29
_cell_measurement_theta_max      27.52

_exptl_crystal_description       platelet
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.17
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.292
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             280
_exptl_absorpt_coefficient_mu    0.083
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9698
_exptl_absorpt_correction_T_max  0.9860
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            7482
_diffrn_reflns_av_R_equivalents  0.0224
_diffrn_reflns_av_sigmaI/netI    0.0314
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.22
_diffrn_reflns_theta_max         26.93
_reflns_number_total             2865
_reflns_number_gt                2277
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² 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/[σ²(Fo²)+(0.0689P)²+0.2063P] where P=(Fo²+2Fc²)/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_number_reflns         2865
_refine_ls_number_parameters     181
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0604
_refine_ls_R_factor_gt           0.0444
_refine_ls_wR_factor_ref         0.1456
_refine_ls_wR_factor_gt          0.1167
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_restrained_S_all      1.110
_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
C1 C -0.0388(3) 0.78913(19) 0.30586(19) 0.0309(4) Uani 1 1 d . . .
H1A H -0.1560 0.8409 0.3193 0.037 Uiso 1 1 calc R . .
C2 C 0.0089(3) 0.64926(19) 0.3590(2) 0.0324(4) Uani 1 1 d . . .
H2A H -0.0693 0.5886 0.4153 0.039 Uiso 1 1 calc R . .
C3 C 0.2001(2) 0.61385(17) 0.31228(18) 0.0269(4) Uani 1 1 d . . .
H3 H 0.2705 0.5252 0.3318 0.032 Uiso 1 1 calc R . .
C4 C 0.2626(2) 0.73396(16) 0.23310(17) 0.0228(4) Uani 1 1 d . . .
C5 C 0.4522(2) 0.75857(16) 0.15494(17) 0.0224(4) Uani 1 1 d . . .
H5 H 0.4752 0.7813 0.0480 0.027 Uiso 1 1 calc R . .
C6 C 0.4725(2) 0.88685(16) 0.21271(17) 0.0234(4) Uani 1 1 d . . .
C7 C 0.3753(2) 0.95596(18) 0.34331(18) 0.0282(4) Uani 1 1 d . . .
H7 H 0.2718 0.9342 0.4208 0.034 Uiso 1 1 calc R . .
C8 C 0.4615(3) 1.06711(19) 0.3389(2) 0.0332(4) Uani 1 1 d . . .
H8 H 0.4242 1.1319 0.4125 0.040 Uiso 1 1 calc R . .
C9 C 0.6092(3) 1.06103(18) 0.2067(2) 0.0334(4) Uani 1 1 d . . .
H9 H 0.6913 1.1208 0.1740 0.040 Uiso 1 1 calc R . .
C10 C 0.5906(2) 0.62043(16) 0.16864(17) 0.0227(4) Uani 1 1 d . . .
C11 C 0.6935(2) 0.53358(17) 0.04876(18) 0.0275(4) Uani 1 1 d . . .
H11 H 0.6782 0.5599 -0.0417 0.033 Uiso 1 1 calc R . .
C12 C 0.8192(3) 0.40768(17) 0.06211(19) 0.0283(4) Uani 1 1 d . . .
H12 H 0.8881 0.3508 -0.0194 0.034 Uiso 1 1 calc R . .
C13 C 0.8420(2) 0.36679(16) 0.19743(18) 0.0253(4) Uani 1 1 d . . .
C14 C 0.7364(3) 0.45186(18) 0.31855(19) 0.0287(4) Uani 1 1 d . . .
H14 H 0.7484 0.4238 0.4102 0.034 Uiso 1 1 calc R . .
C15 C 0.6133(2) 0.57799(18) 0.30408(18) 0.0277(4) Uani 1 1 d . . .
H15 H 0.5451 0.6351 0.3855 0.033 Uiso 1 1 calc R . .
C16 C 0.9847(3) 0.23535(18) 0.2062(2) 0.0307(4) Uani 1 1 d . . .
N1 N 0.1148(2) 0.83967(14) 0.22987(15) 0.0273(3) Uani 1 1 d . . .
H1 H 0.1186 0.9253 0.1862 0.033 Uiso 1 1 calc R . .
N2 N 0.6149(2) 0.95132(15) 0.13087(16) 0.0289(3) Uani 1 1 d . . .
H2 H 0.6961 0.9265 0.0444 0.035 Uiso 1 1 calc R . .
N3 N 1.0396(3) 0.22106(19) 0.3185(2) 0.0564(6) Uani 1 1 d . . .
H3A H 1.1216 0.1466 0.3268 0.068 Uiso 1 1 calc R . .
H3B H 0.9932 0.2863 0.3828 0.068 Uiso 1 1 calc R . .
O1 O 1.04958(18) 0.14298(12) 0.11243(14) 0.0342(3) Uani 1 1 d . . .


_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
C1 N1 1.359(2) . ?
C1 C2 1.365(2) . ?
C1 H1A 0.9300 . ?
C2 C3 1.417(3) . ?
C2 H2A 0.9300 . ?
C3 C4 1.372(2) . ?
C3 H3 0.9300 . ?
C4 N1 1.370(2) . ?
C4 C5 1.507(2) . ?
C5 C6 1.514(2) . ?
C5 C10 1.525(2) . ?
C5 H5 0.9800 . ?
C6 N2 1.367(2) . ?
C6 C7 1.369(2) . ?
C7 C8 1.423(2) . ?
C7 H7 0.9300 . ?
C8 C9 1.365(3) . ?
C8 H8 0.9300 . ?
C9 N2 1.368(2) . ?
C9 H9 0.9300 . ?
C10 C11 1.386(2) . ?
C10 C15 1.394(2) . ?
C11 C12 1.390(2) . ?
C11 H11 0.9300 . ?
C12 C13 1.392(2) . ?
C12 H12 0.9300 . ?
C13 C14 1.388(2) . ?
C13 C16 1.493(2) . ?
C14 C15 1.382(2) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 O1 1.237(2) . ?
C16 N3 1.330(2) . ?
N1 H1 0.8600 . ?
N2 H2 0.8600 . ?
N3 H3A 0.8600 . ?
N3 H3B 0.8600 . ?

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 C1 C2 108.13(16) . . ?
N1 C1 H1A 125.9 . . ?
C2 C1 H1A 125.9 . . ?
C1 C2 C3 107.13(16) . . ?
C1 C2 H2A 126.4 . . ?
C3 C2 H2A 126.4 . . ?
C4 C3 C2 107.65(14) . . ?
C4 C3 H3 126.2 . . ?
C2 C3 H3 126.2 . . ?
N1 C4 C3 107.13(15) . . ?
N1 C4 C5 121.67(13) . . ?
C3 C4 C5 131.17(15) . . ?
C4 C5 C6 111.57(13) . . ?
C4 C5 C10 110.54(12) . . ?
C6 C5 C10 111.67(13) . . ?
C4 C5 H5 107.6 . . ?
C6 C5 H5 107.6 . . ?
C10 C5 H5 107.6 . . ?
N2 C6 C7 107.35(15) . . ?
N2 C6 C5 120.22(14) . . ?
C7 C6 C5 132.38(15) . . ?
C6 C7 C8 107.58(16) . . ?
C6 C7 H7 126.2 . . ?
C8 C7 H7 126.2 . . ?
C9 C8 C7 107.27(16) . . ?
C9 C8 H8 126.4 . . ?
C7 C8 H8 126.4 . . ?
C8 C9 N2 107.74(16) . . ?
C8 C9 H9 126.1 . . ?
N2 C9 H9 126.1 . . ?
C11 C10 C15 118.74(15) . . ?
C11 C10 C5 121.15(13) . . ?
C15 C10 C5 120.11(14) . . ?
C10 C11 C12 120.84(14) . . ?
C10 C11 H11 119.6 . . ?
C12 C11 H11 119.6 . . ?
C11 C12 C13 120.01(15) . . ?
C11 C12 H12 120.0 . . ?
C13 C12 H12 120.0 . . ?
C14 C13 C12 119.24(15) . . ?
C14 C13 C16 121.87(15) . . ?
C12 C13 C16 118.85(15) . . ?
C15 C14 C13 120.50(15) . . ?
C15 C14 H14 119.7 . . ?
C13 C14 H14 119.7 . . ?
C14 C15 C10 120.65(15) . . ?
C14 C15 H15 119.7 . . ?
C10 C15 H15 119.7 . . ?
O1 C16 N3 121.12(17) . . ?
O1 C16 C13 121.22(16) . . ?
N3 C16 C13 117.66(16) . . ?
C1 N1 C4 109.96(14) . . ?
C1 N1 H1 125.0 . . ?
C4 N1 H1 125.0 . . ?
C6 N2 C9 110.06(15) . . ?
C6 N2 H2 125.0 . . ?
C9 N2 H2 125.0 . . ?
C16 N3 H3A 120.0 . . ?
C16 N3 H3B 120.0 . . ?
H3A N3 H3B 120.0 . . ?

_diffrn_measured_fraction_theta_max 0.968
_diffrn_reflns_theta_full        26.93
_diffrn_measured_fraction_theta_full 0.968
_refine_diff_density_max         0.207
_refine_diff_density_min         -0.254
_refine_diff_density_rms         0.067

#===END

###Material relevant to compound 4THF at 173K ##

data_compound4THF
_database_code_depnum_ccdc_archive 'CCDC 716999'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H24 Cu N6 O2, 2(C4 H8 O)'
_chemical_formula_sum            'C40 H40 Cu N6 O4'
_chemical_formula_weight         732.34

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 0.0020 '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 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3200 1.2650 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'C2/c '
_symmetry_space_group_name_Hall  '-C 2yc'

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                   22.9322(12)
_cell_length_b                   15.8716(8)
_cell_length_c                   10.2807(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 105.4940(10)
_cell_angle_gamma                90.00
_cell_volume                     3605.9(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    3052
_cell_measurement_theta_min      2.39
_cell_measurement_theta_max      27.03

_exptl_crystal_description       rod
_exptl_crystal_colour            dark-red
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.17
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.349
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1532
_exptl_absorpt_coefficient_mu    0.656
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7981
_exptl_absorpt_correction_T_max  0.8967
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10737
_diffrn_reflns_av_R_equivalents  0.0303
_diffrn_reflns_av_sigmaI/netI    0.0391
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         1.58
_diffrn_reflns_theta_max         27.51
_reflns_number_total             4095
_reflns_number_gt                3423
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² 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/[σ²(Fo²)+(0.0827P)²+8.7717P] where P=(Fo²+2Fc²)/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_number_reflns         4095
_refine_ls_number_parameters     208
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0661
_refine_ls_R_factor_gt           0.0521
_refine_ls_wR_factor_ref         0.1628
_refine_ls_wR_factor_gt          0.1398
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_restrained_S_all      1.103
_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
C1 C 0.06073(13) 0.73801(17) 0.1854(3) 0.0232(6) Uani 1 1 d . . .
H1 H 0.0243 0.7099 0.1509 0.028 Uiso 1 1 calc R . .
C2 C 0.11711(13) 0.70862(18) 0.1747(3) 0.0246(6) Uani 1 1 d . . .
H2 H 0.1244 0.6592 0.1331 0.030 Uiso 1 1 calc R . .
C3 C 0.15935(12) 0.76750(18) 0.2379(3) 0.0228(6) Uani 1 1 d . . .
H3 H 0.2008 0.7652 0.2473 0.027 Uiso 1 1 calc R . .
C4 C 0.12781(11) 0.83220(17) 0.2859(3) 0.0192(5) Uani 1 1 d . . .
C5 C 0.15177(12) 0.90837(18) 0.3472(3) 0.0200(5) Uani 1 1 d . . .
C6 C 0.11840(12) 0.97406(17) 0.3817(3) 0.0216(6) Uani 1 1 d . . .
C7 C 0.14044(13) 1.04902(18) 0.4549(3) 0.0262(6) Uani 1 1 d . . .
H7 H 0.1808 1.0649 0.4872 0.031 Uiso 1 1 calc R . .
C8 C 0.09115(14) 1.09338(19) 0.4690(3) 0.0281(6) Uani 1 1 d . . .
H8 H 0.0914 1.1445 0.5132 0.034 Uiso 1 1 calc R . .
C9 C 0.03987(13) 1.04552(18) 0.4026(3) 0.0251(6) Uani 1 1 d . . .
H9 H 0.0001 1.0616 0.3955 0.030 Uiso 1 1 calc R . .
C10 C 0.21827(12) 0.92262(18) 0.3757(3) 0.0210(5) Uani 1 1 d . . .
C11 C 0.23945(13) 0.98313(19) 0.3005(3) 0.0268(6) Uani 1 1 d . . .
H11 H 0.2122 1.0124 0.2322 0.032 Uiso 1 1 calc R . .
C12 C 0.30070(13) 0.99948(19) 0.3272(3) 0.0257(6) Uani 1 1 d . . .
H12 H 0.3145 1.0384 0.2747 0.031 Uiso 1 1 calc R . .
C13 C 0.34174(12) 0.95844(18) 0.4318(3) 0.0209(5) Uani 1 1 d . . .
C14 C 0.32077(12) 0.89813(18) 0.5069(3) 0.0240(6) Uani 1 1 d . . .
H14 H 0.3480 0.8699 0.5766 0.029 Uiso 1 1 calc R . .
C15 C 0.25950(13) 0.88002(19) 0.4781(3) 0.0245(6) Uani 1 1 d . . .
H15 H 0.2459 0.8391 0.5278 0.029 Uiso 1 1 calc R . .
C16 C 0.40772(12) 0.97869(18) 0.4589(3) 0.0220(6) Uani 1 1 d . . .
N1 N 0.06612(10) 0.81162(14) 0.2518(2) 0.0196(5) Uani 1 1 d . . .
N2 N 0.05556(10) 0.97428(15) 0.3513(2) 0.0219(5) Uani 1 1 d . . .
N3 N 0.44148(11) 0.97134(19) 0.5852(3) 0.0324(6) Uani 1 1 d . . .
H3A H 0.4795 0.9828 0.6047 0.039 Uiso 1 1 calc R . .
H3B H 0.4253 0.9551 0.6474 0.039 Uiso 1 1 calc R . .
O1 O 0.42877(9) 1.00185(14) 0.3654(2) 0.0263(5) Uani 1 1 d . . .
Cu1 Cu 0.0000 0.89034(3) 0.2500 0.01997(17) Uani 1 2 d S . .
C17 C 0.1733(3) 0.2736(4) 0.3222(7) 0.0885(8) Uani 1 1 d . . .
H17A H 0.1982 0.3231 0.3225 0.106 Uiso 1 1 calc R . .
H17B H 0.1864 0.2472 0.4103 0.106 Uiso 1 1 calc R . .
C18 C 0.1087(3) 0.2986(4) 0.2943(7) 0.0885(8) Uani 1 1 d . . .
H18A H 0.1043 0.3593 0.2849 0.106 Uiso 1 1 calc R . .
H18B H 0.0916 0.2801 0.3662 0.106 Uiso 1 1 calc R . .
C19 C 0.0783(3) 0.2548(4) 0.1631(7) 0.0885(8) Uani 1 1 d . . .
H19A H 0.0404 0.2292 0.1671 0.106 Uiso 1 1 calc R . .
H19B H 0.0706 0.2938 0.0878 0.106 Uiso 1 1 calc R . .
C20 C 0.1235(3) 0.1894(4) 0.1514(7) 0.0885(8) Uani 1 1 d . . .
H20A H 0.1143 0.1362 0.1878 0.106 Uiso 1 1 calc R . .
H20B H 0.1228 0.1811 0.0575 0.106 Uiso 1 1 calc R . .
O2 O 0.1799(2) 0.2182(3) 0.2242(4) 0.0885(8) Uani 1 1 d . . .


_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
C1 N1 1.342(4) . ?
C1 C2 1.406(4) . ?
C1 H1 0.9300 . ?
C2 C3 1.378(4) . ?
C2 H2 0.9300 . ?
C3 C4 1.418(4) . ?
C3 H3 0.9300 . ?
C4 N1 1.402(3) . ?
C4 C5 1.406(4) . ?
C5 C6 1.394(4) . ?
C5 C10 1.491(4) . ?
C6 N2 1.390(3) . ?
C6 C7 1.427(4) . ?
C7 C8 1.372(4) . ?
C7 H7 0.9300 . ?
C8 C9 1.413(4) . ?
C8 H8 0.9300 . ?
C9 N2 1.337(4) . ?
C9 H9 0.9300 . ?
C10 C15 1.388(4) . ?
C10 C11 1.399(4) . ?
C11 C12 1.382(4) . ?
C11 H11 0.9300 . ?
C12 C13 1.387(4) . ?
C12 H12 0.9300 . ?
C13 C14 1.394(4) . ?
C13 C16 1.499(4) . ?
C14 C15 1.386(4) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 O1 1.241(3) . ?
C16 N3 1.327(4) . ?
N1 Cu1 1.961(2) . ?
N2 Cu1 1.943(2) . ?
N3 H3A 0.8600 . ?
N3 H3B 0.8600 . ?
Cu1 N2 1.943(2) 2 ?
Cu1 N1 1.961(2) 2 ?
C17 O2 1.377(7) . ?
C17 C18 1.485(8) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C18 C19 1.512(9) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C19 C20 1.495(8) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 O2 1.388(8) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?

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 C1 C2 111.5(2) . . ?
N1 C1 H1 124.2 . . ?
C2 C1 H1 124.2 . . ?
C3 C2 C1 106.5(2) . . ?
C3 C2 H2 126.8 . . ?
C1 C2 H2 126.8 . . ?
C2 C3 C4 107.2(2) . . ?
C2 C3 H3 126.4 . . ?
C4 C3 H3 126.4 . . ?
N1 C4 C5 124.1(2) . . ?
N1 C4 C3 108.6(2) . . ?
C5 C4 C3 127.2(2) . . ?
C6 C5 C4 125.6(2) . . ?
C6 C5 C10 116.0(2) . . ?
C4 C5 C10 118.4(2) . . ?
N2 C6 C5 123.5(2) . . ?
N2 C6 C7 108.4(2) . . ?
C5 C6 C7 128.1(3) . . ?
C8 C7 C6 107.3(3) . . ?
C8 C7 H7 126.3 . . ?
C6 C7 H7 126.3 . . ?
C7 C8 C9 106.0(3) . . ?
C7 C8 H8 127.0 . . ?
C9 C8 H8 127.0 . . ?
N2 C9 C8 111.6(3) . . ?
N2 C9 H9 124.2 . . ?
C8 C9 H9 124.2 . . ?
C15 C10 C11 119.1(2) . . ?
C15 C10 C5 121.9(2) . . ?
C11 C10 C5 118.9(3) . . ?
C12 C11 C10 120.2(3) . . ?
C12 C11 H11 119.9 . . ?
C10 C11 H11 119.9 . . ?
C11 C12 C13 120.6(3) . . ?
C11 C12 H12 119.7 . . ?
C13 C12 H12 119.7 . . ?
C12 C13 C14 119.2(3) . . ?
C12 C13 C16 119.1(2) . . ?
C14 C13 C16 121.7(3) . . ?
C15 C14 C13 120.3(3) . . ?
C15 C14 H14 119.9 . . ?
C13 C14 H14 119.9 . . ?
C14 C15 C10 120.4(3) . . ?
C14 C15 H15 119.8 . . ?
C10 C15 H15 119.8 . . ?
O1 C16 N3 122.5(3) . . ?
O1 C16 C13 120.1(3) . . ?
N3 C16 C13 117.3(2) . . ?
C1 N1 C4 106.3(2) . . ?
C1 N1 Cu1 125.73(19) . . ?
C4 N1 Cu1 125.44(18) . . ?
C9 N2 C6 106.6(2) . . ?
C9 N2 Cu1 125.8(2) . . ?
C6 N2 Cu1 127.62(19) . . ?
C16 N3 H3A 120.0 . . ?
C16 N3 H3B 120.0 . . ?
H3A N3 H3B 120.0 . . ?
N2 Cu1 N2 93.42(14) . 2 ?
N2 Cu1 N1 146.79(10) . 2 ?
N2 Cu1 N1 92.13(9) 2 2 ?
N2 Cu1 N1 92.13(9) . . ?
N2 Cu1 N1 146.79(10) 2 . ?
N1 Cu1 N1 100.85(13) 2 . ?
O2 C17 C18 109.2(6) . . ?
O2 C17 H17A 109.8 . . ?
C18 C17 H17A 109.8 . . ?
O2 C17 H17B 109.8 . . ?
C18 C17 H17B 109.8 . . ?
H17A C17 H17B 108.3 . . ?
C17 C18 C19 104.4(5) . . ?
C17 C18 H18A 110.9 . . ?
C19 C18 H18A 110.9 . . ?
C17 C18 H18B 110.9 . . ?
C19 C18 H18B 110.9 . . ?
H18A C18 H18B 108.9 . . ?
C20 C19 C18 103.1(6) . . ?
C20 C19 H19A 111.1 . . ?
C18 C19 H19A 111.1 . . ?
C20 C19 H19B 111.1 . . ?
C18 C19 H19B 111.1 . . ?
H19A C19 H19B 109.1 . . ?
O2 C20 C19 107.2(6) . . ?
O2 C20 H20A 110.3 . . ?
C19 C20 H20A 110.3 . . ?
O2 C20 H20B 110.3 . . ?
C19 C20 H20B 110.3 . . ?
H20A C20 H20B 108.5 . . ?
C17 O2 C20 109.6(5) . . ?

_diffrn_measured_fraction_theta_max 0.988
_diffrn_reflns_theta_full        27.51
_diffrn_measured_fraction_theta_full 0.988
_refine_diff_density_max         1.214
_refine_diff_density_min         -1.079
_refine_diff_density_rms         0.116

#===END

###Material relevant to compound 4CHCl3 at 173K ##

data_compound4CHCl3
_database_code_depnum_ccdc_archive 'CCDC 717000'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H24 Cu N6 O2, C2 H2 Cl6'
_chemical_formula_sum            'C34 H26 Cl6 Cu N6 O2'
_chemical_formula_weight         826.89

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 0.0020 '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 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1480 0.1590 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3200 1.2650 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'C2/c '
_symmetry_space_group_name_Hall  '-C 2yc'

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                   22.9849(16)
_cell_length_b                   16.1578(13)
_cell_length_c                   10.2185(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 106.103(3)
_cell_angle_gamma                90.00
_cell_volume                     3646.1(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    1156
_cell_measurement_theta_min      2.38
_cell_measurement_theta_max      21.02

_exptl_crystal_description       rod
_exptl_crystal_colour            dark-red
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.506
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1676
_exptl_absorpt_coefficient_mu    1.079
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7378
_exptl_absorpt_correction_T_max  0.9683
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
The chloroform solvate molecule is disordered over
two positions which have been modeled accordingly
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13056
_diffrn_reflns_av_R_equivalents  0.0730
_diffrn_reflns_av_sigmaI/netI    0.1071
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         1.56
_diffrn_reflns_theta_max         27.51
_reflns_number_total             4151
_reflns_number_gt                2249
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² 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/[σ²(Fo²)+(0.1073P)²+0.0000P] where P=(Fo²+2Fc²)/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     SHELXL
_refine_ls_extinction_coef       0.0031(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         4151
_refine_ls_number_parameters     251
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1315
_refine_ls_R_factor_gt           0.0615
_refine_ls_wR_factor_ref         0.2011
_refine_ls_wR_factor_gt          0.1498
_refine_ls_goodness_of_fit_ref   0.980
_refine_ls_restrained_S_all      0.980
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.06144(19) 0.7413(3) 0.1865(4) 0.0305(10) Uani 1 1 d . . .
H1 H 0.0253 0.7130 0.1511 0.037 Uiso 1 1 calc R . .
C2 C 0.1178(2) 0.7144(3) 0.1758(5) 0.0354(11) Uani 1 1 d . . .
H2 H 0.1255 0.6664 0.1332 0.042 Uiso 1 1 calc R . .
C3 C 0.15909(19) 0.7719(3) 0.2395(4) 0.0322(10) Uani 1 1 d . . .
H3 H 0.2004 0.7707 0.2482 0.039 Uiso 1 1 calc R . .
C4 C 0.12787(18) 0.8338(3) 0.2900(4) 0.0265(9) Uani 1 1 d . . .
C5 C 0.15168(19) 0.9080(3) 0.3532(4) 0.0301(10) Uani 1 1 d . . .
C6 C 0.11810(19) 0.9725(3) 0.3885(4) 0.0293(10) Uani 1 1 d . . .
C7 C 0.1396(2) 1.0459(3) 0.4636(4) 0.0352(11) Uani 1 1 d . . .
H7 H 0.1799 1.0614 0.4986 0.042 Uiso 1 1 calc R . .
C8 C 0.0900(2) 1.0895(3) 0.4748(5) 0.0379(11) Uani 1 1 d . . .
H8 H 0.0901 1.1395 0.5200 0.045 Uiso 1 1 calc R . .
C9 C 0.0387(2) 1.0432(3) 0.4040(4) 0.0336(11) Uani 1 1 d . . .
H9 H -0.0011 1.0594 0.3936 0.040 Uiso 1 1 calc R . .
C10 C 0.21825(18) 0.9247(3) 0.3815(4) 0.0280(10) Uani 1 1 d . . .
C11 C 0.2381(2) 0.9865(3) 0.3098(5) 0.0347(11) Uani 1 1 d . . .
H11 H 0.2100 1.0164 0.2437 0.042 Uiso 1 1 calc R . .
C12 C 0.2987(2) 1.0043(3) 0.3353(5) 0.0340(11) Uani 1 1 d . . .
H12 H 0.3113 1.0448 0.2846 0.041 Uiso 1 1 calc R . .
C13 C 0.34122(18) 0.9618(3) 0.4364(4) 0.0284(10) Uani 1 1 d . . .
C14 C 0.32174(19) 0.8988(3) 0.5079(4) 0.0338(11) Uani 1 1 d . . .
H14 H 0.3498 0.8690 0.5743 0.041 Uiso 1 1 calc R . .
C15 C 0.26078(19) 0.8810(3) 0.4797(5) 0.0347(11) Uani 1 1 d . . .
H15 H 0.2481 0.8389 0.5275 0.042 Uiso 1 1 calc R . .
C16 C 0.40718(18) 0.9832(3) 0.4625(4) 0.0295(10) Uani 1 1 d . . .
N1 N 0.06632(15) 0.8135(2) 0.2548(3) 0.0273(8) Uani 1 1 d . . .
N2 N 0.05503(15) 0.9724(2) 0.3533(4) 0.0295(8) Uani 1 1 d . . .
N3 N 0.44262(16) 0.9713(3) 0.5882(4) 0.0448(11) Uani 1 1 d . . .
H3A H 0.4807 0.9820 0.6071 0.054 Uiso 1 1 calc R . .
H3B H 0.4274 0.9529 0.6506 0.054 Uiso 1 1 calc R . .
O1 O 0.42660(13) 1.0096(2) 0.3686(3) 0.0355(8) Uani 1 1 d . . .
Cu1 Cu 0.0000 0.89011(5) 0.2500 0.0300(3) Uani 1 2 d S . .
C17 C 0.1189(4) 0.7582(5) 0.7693(9) 0.106(3) Uani 1 1 d . . .
H17 H 0.1188 0.8018 0.8358 0.127 Uiso 1 1 calc R A 1
Cl1A Cl 0.1309(8) 0.7996(6) 0.6359(14) 0.208(7) Uani 0.502(7) 1 d P B 1
Cl2A Cl 0.1722(3) 0.6901(5) 0.8397(5) 0.153(4) Uani 0.502(7) 1 d P B 1
Cl3A Cl 0.0484(4) 0.7053(4) 0.7307(11) 0.213(4) Uani 0.502(7) 1 d P . 1
Cl1B Cl 0.1035(6) 0.7983(9) 0.6094(12) 0.197(6) Uani 0.498(7) 1 d P B 2
Cl2B Cl 0.2006(3) 0.7699(5) 0.8577(8) 0.167(3) Uani 0.498(7) 1 d P B 2
Cl3B Cl 0.1034(3) 0.6605(3) 0.7867(5) 0.111(3) Uani 0.498(7) 1 d P B 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.349(5) . ?
C1 C2 1.398(6) . ?
C1 H1 0.9300 . ?
C2 C3 1.359(6) . ?
C2 H2 0.9300 . ?
C3 C4 1.409(6) . ?
C3 H3 0.9300 . ?
C4 N1 1.398(5) . ?
C4 C5 1.399(6) . ?
C5 C6 1.402(6) . ?
C5 C10 1.501(6) . ?
C6 N2 1.393(5) . ?
C6 C7 1.424(6) . ?
C7 C8 1.371(6) . ?
C7 H7 0.9300 . ?
C8 C9 1.415(6) . ?
C8 H8 0.9300 . ?
C9 N2 1.350(5) . ?
C9 H9 0.9300 . ?
C10 C15 1.384(6) . ?
C10 C11 1.389(6) . ?
C11 C12 1.375(6) . ?
C11 H11 0.9300 . ?
C12 C13 1.391(6) . ?
C12 H12 0.9300 . ?
C13 C14 1.397(6) . ?
C13 C16 1.505(6) . ?
C14 C15 1.380(6) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 O1 1.240(5) . ?
C16 N3 1.331(5) . ?
N1 Cu1 1.953(3) . ?
N2 Cu1 1.934(4) . ?
N3 H3A 0.8600 . ?
N3 H3B 0.8600 . ?
Cu1 N2 1.934(4) 2 ?
Cu1 N1 1.953(3) 2 ?
C17 Cl1A 1.609(12) . ?
C17 Cl3B 1.638(9) . ?
C17 Cl2A 1.655(10) . ?
C17 Cl1B 1.701(13) . ?
C17 Cl3A 1.776(10) . ?
C17 Cl2B 1.854(12) . ?
C17 H17 0.9800 . ?
Cl3A Cl3A 2.365(16) 2_556 ?

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 C1 C2 111.3(4) . . ?
N1 C1 H1 124.3 . . ?
C2 C1 H1 124.3 . . ?
C3 C2 C1 106.8(4) . . ?
C3 C2 H2 126.6 . . ?
C1 C2 H2 126.6 . . ?
C2 C3 C4 107.5(4) . . ?
C2 C3 H3 126.2 . . ?
C4 C3 H3 126.2 . . ?
N1 C4 C5 123.9(4) . . ?
N1 C4 C3 108.8(4) . . ?
C5 C4 C3 127.1(4) . . ?
C4 C5 C6 125.7(4) . . ?
C4 C5 C10 119.4(4) . . ?
C6 C5 C10 114.9(4) . . ?
N2 C6 C5 122.7(4) . . ?
N2 C6 C7 108.7(4) . . ?
C5 C6 C7 128.6(4) . . ?
C8 C7 C6 107.5(4) . . ?
C8 C7 H7 126.3 . . ?
C6 C7 H7 126.3 . . ?
C7 C8 C9 106.2(4) . . ?
C7 C8 H8 126.9 . . ?
C9 C8 H8 126.9 . . ?
N2 C9 C8 111.3(4) . . ?
N2 C9 H9 124.3 . . ?
C8 C9 H9 124.3 . . ?
C15 C10 C11 118.7(4) . . ?
C15 C10 C5 121.7(4) . . ?
C11 C10 C5 119.6(4) . . ?
C12 C11 C10 120.9(4) . . ?
C12 C11 H11 119.5 . . ?
C10 C11 H11 119.5 . . ?
C11 C12 C13 120.3(4) . . ?
C11 C12 H12 119.9 . . ?
C13 C12 H12 119.9 . . ?
C12 C13 C14 119.2(4) . . ?
C12 C13 C16 118.9(4) . . ?
C14 C13 C16 121.9(4) . . ?
C15 C14 C13 119.8(4) . . ?
C15 C14 H14 120.1 . . ?
C13 C14 H14 120.1 . . ?
C14 C15 C10 121.1(4) . . ?
C14 C15 H15 119.4 . . ?
C10 C15 H15 119.4 . . ?
O1 C16 N3 122.8(4) . . ?
O1 C16 C13 120.2(4) . . ?
N3 C16 C13 117.0(4) . . ?
C1 N1 C4 105.6(3) . . ?
C1 N1 Cu1 125.6(3) . . ?
C4 N1 Cu1 125.8(3) . . ?
C9 N2 C6 106.2(4) . . ?
C9 N2 Cu1 125.6(3) . . ?
C6 N2 Cu1 128.1(3) . . ?
C16 N3 H3A 120.0 . . ?
C16 N3 H3B 120.0 . . ?
H3A N3 H3B 120.0 . . ?
N2 Cu1 N2 93.1(2) . 2 ?
N2 Cu1 N1 146.79(14) . 2 ?
N2 Cu1 N1 91.95(14) 2 2 ?
N2 Cu1 N1 91.95(14) . . ?
N2 Cu1 N1 146.79(14) 2 . ?
N1 Cu1 N1 101.4(2) 2 . ?
Cl1A C17 Cl3B 125.9(7) . . ?
Cl1A C17 Cl2A 111.4(7) . . ?
Cl3B C17 Cl2A 58.0(5) . . ?
Cl1A C17 Cl1B 21.1(9) . . ?
Cl3B C17 Cl1B 118.5(8) . . ?
Cl2A C17 Cl1B 127.1(6) . . ?
Cl1A C17 Cl3A 111.8(9) . . ?
Cl3B C17 Cl3A 49.3(4) . . ?
Cl2A C17 Cl3A 107.2(6) . . ?
Cl1B C17 Cl3A 92.1(8) . . ?
Cl1A C17 Cl2B 89.0(8) . . ?
Cl3B C17 Cl2B 105.5(7) . . ?
Cl2A C17 Cl2B 47.8(4) . . ?
Cl1B C17 Cl2B 110.0(7) . . ?
Cl3A C17 Cl2B 153.6(7) . . ?
Cl1A C17 H17 108.8 . . ?
Cl3B C17 H17 125.1 . . ?
Cl2A C17 H17 108.8 . . ?
Cl1B C17 H17 110.6 . . ?
Cl3A C17 H17 108.8 . . ?
Cl2B C17 H17 77.6 . . ?
C17 Cl3A Cl3A 143.7(6) . 2_556 ?

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        27.51
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         0.673
_refine_diff_density_min         -0.779
_refine_diff_density_rms         0.131

#===END

###Material relevant to compound 5 at 173K ##

data_compound5
_database_code_depnum_ccdc_archive 'CCDC 717001'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H24 N6 O2 Zn, 2(C4 H8 O2)'
_chemical_formula_sum            'C40 H40 N6 O6 Zn'
_chemical_formula_weight         766.19

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 0.0020 '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 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2840 1.4300 '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 '
_symmetry_space_group_name_Hall  '-P 1'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.9609(3)
_cell_length_b                   13.6458(3)
_cell_length_c                   14.1783(3)
_cell_angle_alpha                103.3150(10)
_cell_angle_beta                 97.276(2)
_cell_angle_gamma                95.440(2)
_cell_volume                     1844.86(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    4338
_cell_measurement_theta_min      2.37
_cell_measurement_theta_max      27.46

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.379
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             800
_exptl_absorpt_coefficient_mu    0.722
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8632
_exptl_absorpt_correction_T_max  0.9580
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            19542
_diffrn_reflns_av_R_equivalents  0.0353
_diffrn_reflns_av_sigmaI/netI    0.0609
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.49
_diffrn_reflns_theta_max         27.56
_reflns_number_total             8216
_reflns_number_gt                6104
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² 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/[σ²(Fo²)+(0.0656P)²+3.5041P] where P=(Fo²+2Fc²)/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_number_reflns         8216
_refine_ls_number_parameters     460
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0920
_refine_ls_R_factor_gt           0.0642
_refine_ls_wR_factor_ref         0.1781
_refine_ls_wR_factor_gt          0.1489
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_restrained_S_all      1.033
_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
C1 C 0.5008(4) 0.1719(3) 0.2269(3) 0.0444(10) Uani 1 1 d . . .
H1 H 0.5424 0.2254 0.2060 0.053 Uiso 1 1 calc R . .
C2 C 0.5633(4) 0.0861(4) 0.2387(3) 0.0454(10) Uani 1 1 d . . .
H2 H 0.6497 0.0725 0.2257 0.055 Uiso 1 1 calc R . .
C3 C 0.4719(4) 0.0271(3) 0.2727(3) 0.0362(9) Uani 1 1 d . . .
H3 H 0.4847 -0.0342 0.2885 0.043 Uiso 1 1 calc R . .
C4 C 0.3534(4) 0.0772(3) 0.2797(2) 0.0273(7) Uani 1 1 d . . .
C5 C 0.2322(4) 0.0438(2) 0.3097(2) 0.0252(7) Uani 1 1 d . . .
C6 C 0.1116(4) 0.0891(3) 0.3093(2) 0.0278(7) Uani 1 1 d . . .
C7 C -0.0038(4) 0.0643(3) 0.3525(3) 0.0350(8) Uani 1 1 d . . .
H7 H -0.0172 0.0106 0.3819 0.042 Uiso 1 1 calc R . .
C8 C -0.0919(5) 0.1341(4) 0.3429(3) 0.0452(10) Uani 1 1 d . . .
H8 H -0.1759 0.1373 0.3649 0.054 Uiso 1 1 calc R . .
C9 C -0.0304(5) 0.1993(3) 0.2937(3) 0.0445(10) Uani 1 1 d . . .
H9 H -0.0691 0.2537 0.2773 0.053 Uiso 1 1 calc R . .
C10 C 0.2342(4) -0.0476(2) 0.3507(2) 0.0255(7) Uani 1 1 d . . .
C11 C 0.3190(4) -0.0422(3) 0.4379(2) 0.0275(7) Uani 1 1 d . . .
H11 H 0.3743 0.0181 0.4698 0.033 Uiso 1 1 calc R . .
C12 C 0.3222(4) -0.1255(3) 0.4777(2) 0.0279(7) Uani 1 1 d . . .
H12 H 0.3804 -0.1212 0.5357 0.034 Uiso 1 1 calc R . .
C13 C 0.2382(4) -0.2162(2) 0.4311(2) 0.0248(7) Uani 1 1 d . . .
C14 C 0.1523(4) -0.2211(3) 0.3451(3) 0.0316(8) Uani 1 1 d . . .
H14 H 0.0949 -0.2807 0.3140 0.038 Uiso 1 1 calc R . .
C15 C 0.1509(4) -0.1380(3) 0.3049(3) 0.0331(8) Uani 1 1 d . . .
H15 H 0.0937 -0.1426 0.2464 0.040 Uiso 1 1 calc R . .
C16 C 0.2370(4) -0.3056(3) 0.4759(2) 0.0296(8) Uani 1 1 d . . .
C17 C 0.2796(5) 0.4588(3) 0.2775(3) 0.0406(9) Uani 1 1 d . . .
H17 H 0.2895 0.4562 0.3429 0.049 Uiso 1 1 calc R . .
C18 C 0.2978(5) 0.5484(3) 0.2460(3) 0.0416(10) Uani 1 1 d . . .
H18 H 0.3205 0.6140 0.2855 0.050 Uiso 1 1 calc R . .
C19 C 0.2754(4) 0.5207(3) 0.1456(3) 0.0365(9) Uani 1 1 d . . .
H19 H 0.2809 0.5640 0.1039 0.044 Uiso 1 1 calc R . .
C20 C 0.2422(4) 0.4137(2) 0.1171(2) 0.0291(8) Uani 1 1 d . . .
C21 C 0.2098(4) 0.3528(3) 0.0212(3) 0.0293(7) Uani 1 1 d . . .
C22 C 0.1789(4) 0.2476(3) -0.0084(2) 0.0286(7) Uani 1 1 d . . .
C23 C 0.1483(4) 0.1853(3) -0.1055(3) 0.0347(8) Uani 1 1 d . . .
H23 H 0.1415 0.2076 -0.1630 0.042 Uiso 1 1 calc R . .
C24 C 0.1306(5) 0.0862(3) -0.0991(3) 0.0407(9) Uani 1 1 d . . .
H24 H 0.1097 0.0284 -0.1508 0.049 Uiso 1 1 calc R . .
C25 C 0.1507(5) 0.0899(3) 0.0016(3) 0.0394(9) Uani 1 1 d . . .
H25 H 0.1452 0.0328 0.0269 0.047 Uiso 1 1 calc R . .
C26 C 0.2106(4) 0.4060(3) -0.0609(2) 0.0294(8) Uani 1 1 d . . .
C27 C 0.3326(4) 0.4342(3) -0.0909(3) 0.0359(9) Uani 1 1 d . . .
H27 H 0.4147 0.4235 -0.0581 0.043 Uiso 1 1 calc R . .
C28 C 0.3323(4) 0.4784(3) -0.1698(3) 0.0361(9) Uani 1 1 d . . .
H28 H 0.4145 0.4973 -0.1894 0.043 Uiso 1 1 calc R . .
C29 C 0.2107(4) 0.4947(3) -0.2195(2) 0.0296(8) Uani 1 1 d . . .
C30 C 0.0895(4) 0.4683(3) -0.1886(3) 0.0354(9) Uani 1 1 d . . .
H30 H 0.0076 0.4798 -0.2211 0.042 Uiso 1 1 calc R . .
C31 C 0.0890(4) 0.4249(3) -0.1092(3) 0.0368(9) Uani 1 1 d . . .
H31 H 0.0069 0.4082 -0.0883 0.044 Uiso 1 1 calc R . .
N1 N 0.3757(3) 0.1672(2) 0.2494(2) 0.0334(7) Uani 1 1 d . . .
N2 N 0.0909(3) 0.1741(2) 0.2729(2) 0.0333(7) Uani 1 1 d . . .
N3 N 0.3518(3) -0.3139(3) 0.5300(2) 0.0403(8) Uani 1 1 d . . .
H3A H 0.3557 -0.3630 0.5585 0.048 Uiso 1 1 calc R . .
H3B H 0.4226 -0.2701 0.5367 0.048 Uiso 1 1 calc R . .
N4 N 0.2466(4) 0.3775(2) 0.2021(2) 0.0352(7) Uani 1 1 d . . .
N5 N 0.1783(3) 0.1844(2) 0.0564(2) 0.0329(7) Uani 1 1 d . . .
N6 N 0.1066(4) 0.5258(3) -0.3730(2) 0.0407(8) Uani 1 1 d . . .
H6A H 0.1077 0.5510 -0.4232 0.049 Uiso 1 1 calc R . .
H6B H 0.0333 0.4915 -0.3656 0.049 Uiso 1 1 calc R . .
O1 O 0.1317(3) -0.36662(19) 0.46357(19) 0.0361(6) Uani 1 1 d . . .
O2 O 0.3257(3) 0.5883(3) -0.3137(2) 0.0556(9) Uani 1 1 d . . .
Zn1 Zn 0.22148(5) 0.23329(3) 0.20131(3) 0.03549(15) Uani 1 1 d . . .
C32 C 0.2185(4) 0.5399(3) -0.3064(3) 0.0351(9) Uani 1 1 d . . .
C33 C 0.6853(5) 0.8185(5) 0.3136(4) 0.0605(14) Uani 1 1 d . . .
H33A H 0.6615 0.8162 0.2446 0.073 Uiso 1 1 calc R . .
H33B H 0.7032 0.8892 0.3497 0.073 Uiso 1 1 calc R . .
C34 C 0.5691(5) 0.7665(4) 0.3480(4) 0.0571(13) Uani 1 1 d . . .
H34A H 0.4881 0.7989 0.3364 0.069 Uiso 1 1 calc R . .
H34B H 0.5501 0.6961 0.3110 0.069 Uiso 1 1 calc R . .
C35 C 0.7203(6) 0.7242(4) 0.4665(4) 0.0604(13) Uani 1 1 d . . .
H35A H 0.7024 0.6525 0.4337 0.072 Uiso 1 1 calc R . .
H35B H 0.7447 0.7302 0.5362 0.072 Uiso 1 1 calc R . .
C36 C 0.8371(5) 0.7727(5) 0.4289(4) 0.0601(13) Uani 1 1 d . . .
H36A H 0.8609 0.8426 0.4664 0.072 Uiso 1 1 calc R . .
H36B H 0.9158 0.7374 0.4384 0.072 Uiso 1 1 calc R . .
O3 O 0.6001(3) 0.7707(2) 0.4499(2) 0.0487(7) Uani 1 1 d . . .
O4 O 0.8048(3) 0.7705(3) 0.3278(2) 0.0571(9) Uani 1 1 d . . .
C37 C 0.7575(9) 0.2773(8) -0.0283(8) 0.1313(18) Uani 1 1 d . . .
H37A H 0.7503 0.3337 0.0260 0.158 Uiso 1 1 calc R . .
H37B H 0.8211 0.3009 -0.0672 0.158 Uiso 1 1 calc R . .
C38 C 0.8090(9) 0.1940(8) 0.0100(8) 0.1313(18) Uani 1 1 d . . .
H38A H 0.8440 0.1486 -0.0419 0.158 Uiso 1 1 calc R . .
H38B H 0.8844 0.2222 0.0626 0.158 Uiso 1 1 calc R . .
C39 C 0.5888(9) 0.1191(9) -0.0084(8) 0.1313(18) Uani 1 1 d . . .
H39A H 0.5217 0.0921 0.0261 0.158 Uiso 1 1 calc R . .
H39B H 0.5925 0.0674 -0.0675 0.158 Uiso 1 1 calc R . .
C40 C 0.5456(9) 0.2014(8) -0.0348(8) 0.1313(18) Uani 1 1 d . . .
H40A H 0.5342 0.2512 0.0237 0.158 Uiso 1 1 calc R . .
H40B H 0.4572 0.1814 -0.0759 0.158 Uiso 1 1 calc R . .
O5 O 0.7068(8) 0.1355(5) 0.0465(4) 0.122(2) Uani 1 1 d . . .
O6 O 0.6335(8) 0.2452(6) -0.0842(5) 0.153(3) Uani 1 1 d . . .


_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
C1 N1 1.324(5) . ?
C1 C2 1.410(6) . ?
C1 H1 0.9300 . ?
C2 C3 1.365(6) . ?
C2 H2 0.9300 . ?
C3 C4 1.421(5) . ?
C3 H3 0.9300 . ?
C4 N1 1.399(4) . ?
C4 C5 1.400(5) . ?
C5 C6 1.402(5) . ?
C5 C10 1.494(4) . ?
C6 N2 1.396(4) . ?
C6 C7 1.418(5) . ?
C7 C8 1.373(6) . ?
C7 H7 0.9300 . ?
C8 C9 1.395(6) . ?
C8 H8 0.9300 . ?
C9 N2 1.337(5) . ?
C9 H9 0.9300 . ?
C10 C11 1.389(4) . ?
C10 C15 1.390(5) . ?
C11 C12 1.381(4) . ?
C11 H11 0.9300 . ?
C12 C13 1.399(5) . ?
C12 H12 0.9300 . ?
C13 C14 1.382(5) . ?
C13 C16 1.500(4) . ?
C14 C15 1.381(5) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 O1 1.243(4) . ?
C16 N3 1.323(5) . ?
C17 N4 1.333(5) . ?
C17 C18 1.400(5) . ?
C17 H17 0.9300 . ?
C18 C19 1.368(6) . ?
C18 H18 0.9300 . ?
C19 C20 1.417(5) . ?
C19 H19 0.9300 . ?
C20 C21 1.401(5) . ?
C20 N4 1.401(4) . ?
C21 C22 1.393(5) . ?
C21 C26 1.508(4) . ?
C22 N5 1.397(4) . ?
C22 C23 1.420(5) . ?
C23 C24 1.373(5) . ?
C23 H23 0.9300 . ?
C24 C25 1.405(5) . ?
C24 H24 0.9300 . ?
C25 N5 1.326(5) . ?
C25 H25 0.9300 . ?
C26 C27 1.387(5) . ?
C26 C31 1.390(5) . ?
C27 C28 1.387(5) . ?
C27 H27 0.9300 . ?
C28 C29 1.386(5) . ?
C28 H28 0.9300 . ?
C29 C30 1.380(5) . ?
C29 C32 1.506(4) . ?
C30 C31 1.388(5) . ?
C30 H30 0.9300 . ?
C31 H31 0.9300 . ?
N1 Zn1 1.979(3) . ?
N2 Zn1 1.972(3) . ?
N3 H3A 0.8600 . ?
N3 H3B 0.8600 . ?
N4 Zn1 1.957(3) . ?
N5 Zn1 1.985(3) . ?
N6 C32 1.334(5) . ?
N6 H6A 0.8600 . ?
N6 H6B 0.8600 . ?
O2 C32 1.231(5) . ?
C33 O4 1.426(6) . ?
C33 C34 1.492(7) . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C34 O3 1.425(6) . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
C35 O3 1.426(6) . ?
C35 C36 1.499(7) . ?
C35 H35A 0.9700 . ?
C35 H35B 0.9700 . ?
C36 O4 1.421(6) . ?
C36 H36A 0.9700 . ?
C36 H36B 0.9700 . ?
C37 O6 1.355(10) . ?
C37 C38 1.475(12) . ?
C37 H37A 0.9700 . ?
C37 H37B 0.9700 . ?
C38 O5 1.453(9) . ?
C38 H38A 0.9700 . ?
C38 H38B 0.9700 . ?
C39 O5 1.295(10) . ?
C39 C40 1.353(12) . ?
C39 H39A 0.9700 . ?
C39 H39B 0.9700 . ?
C40 O6 1.366(10) . ?
C40 H40A 0.9700 . ?
C40 H40B 0.9700 . ?

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 C1 C2 111.8(4) . . ?
N1 C1 H1 124.1 . . ?
C2 C1 H1 124.1 . . ?
C3 C2 C1 106.5(4) . . ?
C3 C2 H2 126.8 . . ?
C1 C2 H2 126.8 . . ?
C2 C3 C4 107.0(4) . . ?
C2 C3 H3 126.5 . . ?
C4 C3 H3 126.5 . . ?
N1 C4 C5 124.3(3) . . ?
N1 C4 C3 108.5(3) . . ?
C5 C4 C3 127.2(3) . . ?
C4 C5 C6 127.2(3) . . ?
C4 C5 C10 116.1(3) . . ?
C6 C5 C10 116.6(3) . . ?
N2 C6 C5 124.5(3) . . ?
N2 C6 C7 108.1(3) . . ?
C5 C6 C7 127.2(3) . . ?
C8 C7 C6 107.4(4) . . ?
C8 C7 H7 126.3 . . ?
C6 C7 H7 126.3 . . ?
C7 C8 C9 106.3(4) . . ?
C7 C8 H8 126.9 . . ?
C9 C8 H8 126.9 . . ?
N2 C9 C8 111.8(4) . . ?
N2 C9 H9 124.1 . . ?
C8 C9 H9 124.1 . . ?
C11 C10 C15 118.8(3) . . ?
C11 C10 C5 119.6(3) . . ?
C15 C10 C5 121.7(3) . . ?
C12 C11 C10 120.7(3) . . ?
C12 C11 H11 119.6 . . ?
C10 C11 H11 119.6 . . ?
C11 C12 C13 120.2(3) . . ?
C11 C12 H12 119.9 . . ?
C13 C12 H12 119.9 . . ?
C14 C13 C12 119.1(3) . . ?
C14 C13 C16 120.4(3) . . ?
C12 C13 C16 120.5(3) . . ?
C15 C14 C13 120.5(3) . . ?
C15 C14 H14 119.8 . . ?
C13 C14 H14 119.8 . . ?
C14 C15 C10 120.8(3) . . ?
C14 C15 H15 119.6 . . ?
C10 C15 H15 119.6 . . ?
O1 C16 N3 122.8(3) . . ?
O1 C16 C13 120.7(3) . . ?
N3 C16 C13 116.5(3) . . ?
N4 C17 C18 111.7(3) . . ?
N4 C17 H17 124.1 . . ?
C18 C17 H17 124.1 . . ?
C19 C18 C17 106.6(3) . . ?
C19 C18 H18 126.7 . . ?
C17 C18 H18 126.7 . . ?
C18 C19 C20 107.2(3) . . ?
C18 C19 H19 126.4 . . ?
C20 C19 H19 126.4 . . ?
C21 C20 N4 124.8(3) . . ?
C21 C20 C19 126.9(3) . . ?
N4 C20 C19 108.3(3) . . ?
C22 C21 C20 127.8(3) . . ?
C22 C21 C26 115.2(3) . . ?
C20 C21 C26 117.0(3) . . ?
C21 C22 N5 123.9(3) . . ?
C21 C22 C23 128.0(3) . . ?
N5 C22 C23 108.1(3) . . ?
C24 C23 C22 107.5(3) . . ?
C24 C23 H23 126.2 . . ?
C22 C23 H23 126.2 . . ?
C23 C24 C25 105.8(3) . . ?
C23 C24 H24 127.1 . . ?
C25 C24 H24 127.1 . . ?
N5 C25 C24 112.2(3) . . ?
N5 C25 H25 123.9 . . ?
C24 C25 H25 123.9 . . ?
C27 C26 C31 119.2(3) . . ?
C27 C26 C21 120.3(3) . . ?
C31 C26 C21 120.5(3) . . ?
C26 C27 C28 120.1(4) . . ?
C26 C27 H27 119.9 . . ?
C28 C27 H27 119.9 . . ?
C29 C28 C27 120.6(4) . . ?
C29 C28 H28 119.7 . . ?
C27 C28 H28 119.7 . . ?
C30 C29 C28 119.3(3) . . ?
C30 C29 C32 123.2(3) . . ?
C28 C29 C32 117.5(3) . . ?
C29 C30 C31 120.4(4) . . ?
C29 C30 H30 119.8 . . ?
C31 C30 H30 119.8 . . ?
C30 C31 C26 120.3(4) . . ?
C30 C31 H31 119.8 . . ?
C26 C31 H31 119.9 . . ?
C1 N1 C4 106.3(3) . . ?
C1 N1 Zn1 128.0(2) . . ?
C4 N1 Zn1 121.2(3) . . ?
C9 N2 C6 106.4(3) . . ?
C9 N2 Zn1 130.8(3) . . ?
C6 N2 Zn1 122.8(3) . . ?
C16 N3 H3A 120.0 . . ?
C16 N3 H3B 120.0 . . ?
H3A N3 H3B 120.0 . . ?
C17 N4 C20 106.2(3) . . ?
C17 N4 Zn1 129.8(3) . . ?
C20 N4 Zn1 123.9(2) . . ?
C25 N5 C22 106.5(3) . . ?
C25 N5 Zn1 129.1(2) . . ?
C22 N5 Zn1 124.3(2) . . ?
C32 N6 H6A 120.0 . . ?
C32 N6 H6B 120.0 . . ?
H6A N6 H6B 120.0 . . ?
N4 Zn1 N2 123.50(14) . . ?
N4 Zn1 N1 120.70(14) . . ?
N2 Zn1 N1 94.70(12) . . ?
N4 Zn1 N5 95.15(12) . . ?
N2 Zn1 N5 114.30(13) . . ?
N1 Zn1 N5 109.08(13) . . ?
O2 C32 N6 122.4(3) . . ?
O2 C32 C29 119.8(3) . . ?
N6 C32 C29 117.9(3) . . ?
O4 C33 C34 110.5(4) . . ?
O4 C33 H33A 109.6 . . ?
C34 C33 H33A 109.6 . . ?
O4 C33 H33B 109.6 . . ?
C34 C33 H33B 109.6 . . ?
H33A C33 H33B 108.1 . . ?
O3 C34 C33 110.8(4) . . ?
O3 C34 H34A 109.5 . . ?
C33 C34 H34A 109.5 . . ?
O3 C34 H34B 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 108.1 . . ?
O3 C35 C36 111.2(4) . . ?
O3 C35 H35A 109.4 . . ?
C36 C35 H35A 109.4 . . ?
O3 C35 H35B 109.4 . . ?
C36 C35 H35B 109.4 . . ?
H35A C35 H35B 108.0 . . ?
O4 C36 C35 112.0(4) . . ?
O4 C36 H36A 109.2 . . ?
C35 C36 H36A 109.2 . . ?
O4 C36 H36B 109.2 . . ?
C35 C36 H36B 109.2 . . ?
H36A C36 H36B 107.9 . . ?
C34 O3 C35 109.1(4) . . ?
C36 O4 C33 109.0(4) . . ?
O6 C37 C38 110.3(8) . . ?
O6 C37 H37A 109.6 . . ?
C38 C37 H37A 109.6 . . ?
O6 C37 H37B 109.6 . . ?
C38 C37 H37B 109.6 . . ?
H37A C37 H37B 108.1 . . ?
O5 C38 C37 113.8(7) . . ?
O5 C38 H38A 108.8 . . ?
C37 C38 H38A 108.8 . . ?
O5 C38 H38B 108.8 . . ?
C37 C38 H38B 108.8 . . ?
H38A C38 H38B 107.7 . . ?
O5 C39 C40 115.2(10) . . ?
O5 C39 H39A 108.5 . . ?
C40 C39 H39A 108.5 . . ?
O5 C39 H39B 108.5 . . ?
C40 C39 H39B 108.5 . . ?
H39A C39 H39B 107.5 . . ?
C39 C40 O6 113.0(9) . . ?
C39 C40 H40A 109.0 . . ?
O6 C40 H40A 109.0 . . ?
C39 C40 H40B 109.0 . . ?
O6 C40 H40B 109.0 . . ?
H40A C40 H40B 107.8 . . ?
C39 O5 C38 112.6(7) . . ?
C37 O6 C40 111.0(8) . . ?

_diffrn_measured_fraction_theta_max 0.966
_diffrn_reflns_theta_full        27.56
_diffrn_measured_fraction_theta_full 0.966
_refine_diff_density_max         0.786
_refine_diff_density_min         -0.731
_refine_diff_density_rms         0.087

#===END

###Material relevant to compound 6 at 173K ##

data_compound6
_database_code_depnum_ccdc_archive 'CCDC 717002'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C42 H38 Cu2 N6 O6, 1.5(C4 H8 O2)'
_chemical_formula_sum            'C48 H50 Cu2 N6 O9'
_chemical_formula_weight         982.05

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 0.0020 '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 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3200 1.2650 '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 '
_symmetry_space_group_name_Hall  '-P 1'

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

_cell_length_a                   13.5360(8)
_cell_length_b                   13.8314(4)
_cell_length_c                   14.2718(4)
_cell_angle_alpha                111.8430(10)
_cell_angle_beta                 102.397(2)
_cell_angle_gamma                104.374(2)
_cell_volume                     2258.09(16)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    8214
_cell_measurement_theta_min      2.51
_cell_measurement_theta_max      27.53

_exptl_crystal_description       platelet
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.444
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1020
_exptl_absorpt_coefficient_mu    1.006
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7326
_exptl_absorpt_correction_T_max  0.9239
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            36519
_diffrn_reflns_av_R_equivalents  0.0369
_diffrn_reflns_av_sigmaI/netI    0.0470
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.64
_diffrn_reflns_theta_max         27.53
_reflns_number_total             10304
_reflns_number_gt                7866
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² 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/[σ²(Fo²)+(0.0653P)²+1.0032P] where P=(Fo²+2Fc²)/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_number_reflns         10304
_refine_ls_number_parameters     590
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0698
_refine_ls_R_factor_gt           0.0459
_refine_ls_wR_factor_ref         0.1431
_refine_ls_wR_factor_gt          0.1163
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_restrained_S_all      1.116
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.2578(2) 0.3602(3) 0.6815(2) 0.0318(7) Uani 1 1 d . . .
H1 H 0.2666 0.4353 0.7060 0.038 Uiso 1 1 calc R . .
C2 C 0.1604(3) 0.2719(3) 0.6112(3) 0.0384(8) Uani 1 1 d . . .
H2 H 0.0952 0.2776 0.5814 0.046 Uiso 1 1 calc R . .
C3 C 0.1798(2) 0.1755(3) 0.5950(2) 0.0320(7) Uani 1 1 d . . .
H3 H 0.1301 0.1029 0.5523 0.038 Uiso 1 1 calc R . .
C4 C 0.2904(2) 0.2074(2) 0.6559(2) 0.0243(6) Uani 1 1 d . . .
C5 C 0.3492(2) 0.1369(2) 0.6581(2) 0.0230(6) Uani 1 1 d . . .
C6 C 0.4614(2) 0.1732(2) 0.7090(2) 0.0223(6) Uani 1 1 d . . .
C7 C 0.5273(2) 0.1081(2) 0.7068(2) 0.0265(6) Uani 1 1 d . . .
H7 H 0.5033 0.0304 0.6755 0.032 Uiso 1 1 calc R . .
C8 C 0.6335(2) 0.1804(3) 0.7594(2) 0.0291(6) Uani 1 1 d . . .
H8 H 0.6950 0.1616 0.7694 0.035 Uiso 1 1 calc R . .
C9 C 0.6300(2) 0.2879(2) 0.7949(2) 0.0273(6) Uani 1 1 d . . .
H9 H 0.6910 0.3531 0.8338 0.033 Uiso 1 1 calc R . .
C10 C 0.2887(2) 0.0141(2) 0.5981(2) 0.0237(6) Uani 1 1 d . . .
C11 C 0.3136(2) -0.0521(2) 0.5121(2) 0.0271(6) Uani 1 1 d . . .
H11 H 0.3681 -0.0191 0.4915 0.033 Uiso 1 1 calc R . .
C12 C 0.2578(2) -0.1663(2) 0.4574(2) 0.0285(6) Uani 1 1 d . . .
H12 H 0.2750 -0.2095 0.4001 0.034 Uiso 1 1 calc R . .
C13 C 0.1767(2) -0.2170(2) 0.4870(2) 0.0260(6) Uani 1 1 d . . .
C14 C 0.1501(2) -0.1521(2) 0.5711(2) 0.0279(6) Uani 1 1 d . . .
H14 H 0.0952 -0.1856 0.5910 0.033 Uiso 1 1 calc R . .
C15 C 0.2052(2) -0.0368(2) 0.6259(2) 0.0269(6) Uani 1 1 d . . .
H15 H 0.1861 0.0063 0.6815 0.032 Uiso 1 1 calc R . .
C16 C 0.1177(2) -0.3407(2) 0.4230(2) 0.0301(7) Uani 1 1 d . . .
C17 C 0.4197(3) 0.7067(3) 0.9664(3) 0.0490(9) Uani 1 1 d . . .
H17A H 0.4062 0.7297 0.9107 0.074 Uiso 1 1 calc R . .
H17B H 0.4599 0.7714 1.0343 0.074 Uiso 1 1 calc R . .
H17C H 0.3519 0.6669 0.9687 0.074 Uiso 1 1 calc R . .
C18 C 0.4843(3) 0.6319(3) 0.9439(3) 0.0360(7) Uani 1 1 d . . .
C19 C 0.5837(3) 0.6601(3) 1.0190(3) 0.0381(8) Uani 1 1 d . . .
H19 H 0.6076 0.7247 1.0834 0.046 Uiso 1 1 calc R . .
C20 C 0.6500(3) 0.5968(3) 1.0035(2) 0.0339(7) Uani 1 1 d . . .
C21 C 0.7615(3) 0.6405(3) 1.0855(3) 0.0471(9) Uani 1 1 d . . .
H21A H 0.7707 0.5839 1.1062 0.071 Uiso 1 1 calc R . .
H21B H 0.7693 0.7055 1.1474 0.071 Uiso 1 1 calc R . .
H21C H 0.8154 0.6600 1.0549 0.071 Uiso 1 1 calc R . .
C22 C 0.3907(2) 0.7543(3) 0.7197(2) 0.0341(7) Uani 1 1 d . . .
H22 H 0.3292 0.6971 0.6648 0.041 Uiso 1 1 calc R . .
C23 C 0.3952(3) 0.8628(3) 0.7807(3) 0.0387(8) Uani 1 1 d . . .
H23 H 0.3389 0.8896 0.7731 0.046 Uiso 1 1 calc R . .
C24 C 0.4980(2) 0.9213(3) 0.8531(3) 0.0341(7) Uani 1 1 d . . .
H24 H 0.5247 0.9953 0.9051 0.041 Uiso 1 1 calc R . .
C25 C 0.5567(2) 0.8478(2) 0.8344(2) 0.0265(6) Uani 1 1 d . . .
C26 C 0.6650(2) 0.8707(2) 0.8894(2) 0.0258(6) Uani 1 1 d . . .
C27 C 0.7171(2) 0.7927(2) 0.8715(2) 0.0264(6) Uani 1 1 d . . .
C28 C 0.8274(2) 0.8125(3) 0.9192(2) 0.0312(7) Uani 1 1 d . . .
H28 H 0.8807 0.8811 0.9691 0.037 Uiso 1 1 calc R . .
C29 C 0.8414(3) 0.7127(3) 0.8790(3) 0.0366(7) Uani 1 1 d . . .
H29 H 0.9056 0.6999 0.8965 0.044 Uiso 1 1 calc R . .
C30 C 0.7403(2) 0.6335(3) 0.8064(2) 0.0323(7) Uani 1 1 d . . .
H30 H 0.7271 0.5580 0.7675 0.039 Uiso 1 1 calc R . .
C31 C 0.7309(2) 0.9871(2) 0.9748(2) 0.0270(6) Uani 1 1 d . . .
C32 C 0.7411(2) 1.0772(2) 0.9510(2) 0.0313(7) Uani 1 1 d . . .
H32 H 0.7070 1.0646 0.8814 0.038 Uiso 1 1 calc R . .
C33 C 0.8011(2) 1.1846(2) 1.0293(2) 0.0315(7) Uani 1 1 d . . .
H33 H 0.8069 1.2438 1.0118 0.038 Uiso 1 1 calc R . .
C34 C 0.8529(2) 1.2062(2) 1.1338(2) 0.0265(6) Uani 1 1 d . . .
C35 C 0.8444(2) 1.1163(2) 1.1574(2) 0.0306(7) Uani 1 1 d . . .
H35 H 0.8796 1.1290 1.2267 0.037 Uiso 1 1 calc R . .
C36 C 0.7844(2) 1.0085(2) 1.0794(2) 0.0306(7) Uani 1 1 d . . .
H36 H 0.7796 0.9494 1.0967 0.037 Uiso 1 1 calc R . .
C37 C 0.9179(2) 1.3223(2) 1.2219(2) 0.0310(7) Uani 1 1 d . . .
C38 C 0.2231(3) 0.4106(3) 0.4338(3) 0.0473(9) Uani 1 1 d . . .
H38A H 0.1721 0.4031 0.4705 0.071 Uiso 1 1 calc R . .
H38B H 0.2035 0.3413 0.3712 0.071 Uiso 1 1 calc R . .
H38C H 0.2223 0.4688 0.4127 0.071 Uiso 1 1 calc R . .
C39 C 0.3345(3) 0.4394(3) 0.5072(2) 0.0338(7) Uani 1 1 d . . .
C40 C 0.3884(3) 0.3647(3) 0.4847(2) 0.0359(7) Uani 1 1 d . . .
H40 H 0.3577 0.3016 0.4185 0.043 Uiso 1 1 calc R . .
C41 C 0.4851(3) 0.3783(3) 0.5550(2) 0.0332(7) Uani 1 1 d . . .
C42 C 0.5333(3) 0.2892(3) 0.5263(3) 0.0431(8) Uani 1 1 d . . .
H42A H 0.6087 0.3225 0.5372 0.065 Uiso 1 1 calc R . .
H42B H 0.4957 0.2357 0.4523 0.065 Uiso 1 1 calc R . .
H42C H 0.5265 0.2522 0.5710 0.065 Uiso 1 1 calc R . .
N1 N 0.33625(19) 0.3236(2) 0.70882(19) 0.0257(5) Uani 1 1 d . . .
N2 N 0.52833(18) 0.28587(19) 0.76628(17) 0.0230(5) Uani 1 1 d . . .
N3 N 0.0666(2) -0.3953(2) 0.4683(2) 0.0371(6) Uani 1 1 d . . .
H3A H 0.0313 -0.4662 0.4328 0.045 Uiso 1 1 calc R . .
H3B H 0.0687 -0.3599 0.5330 0.045 Uiso 1 1 calc R . .
N4 N 0.48679(19) 0.7438(2) 0.75116(19) 0.0271(5) Uani 1 1 d . . .
N5 N 0.66459(19) 0.67944(19) 0.79974(18) 0.0253(5) Uani 1 1 d . . .
N6 N 0.9490(2) 1.4012(2) 1.1910(2) 0.0440(7) Uani 1 1 d . . .
H6A H 0.9871 1.4690 1.2382 0.053 Uiso 1 1 calc R . .
H6B H 0.9311 1.3844 1.1237 0.053 Uiso 1 1 calc R . .
O1 O 0.44033(18) 0.54375(18) 0.85348(18) 0.0377(5) Uani 1 1 d . . .
O2 O 0.62441(16) 0.50191(17) 0.92388(16) 0.0330(5) Uani 1 1 d . . .
O3 O 0.1166(2) -0.38826(18) 0.33077(17) 0.0491(7) Uani 1 1 d . . .
O4 O 0.37310(17) 0.53446(17) 0.58910(17) 0.0345(5) Uani 1 1 d . . .
O5 O 0.53859(17) 0.46390(17) 0.64665(16) 0.0331(5) Uani 1 1 d . . .
O6 O 0.94178(19) 1.34272(18) 1.31758(16) 0.0416(6) Uani 1 1 d . . .
Cu1 Cu 0.48389(3) 0.41513(3) 0.81153(3) 0.02626(11) Uani 1 1 d . . .
Cu2 Cu 0.51557(3) 0.60465(3) 0.69748(3) 0.02675(11) Uani 1 1 d . . .
C43 C -0.0161(3) -0.0951(4) 0.2429(4) 0.0624(11) Uani 1 1 d . . .
H43A H -0.0354 -0.1322 0.1655 0.075 Uiso 1 1 calc R . .
H43B H -0.0768 -0.1275 0.2612 0.075 Uiso 1 1 calc R . .
C44 C 0.0801(4) -0.1129(4) 0.2936(4) 0.0628(11) Uani 1 1 d . . .
H44A H 0.0985 -0.0776 0.3710 0.075 Uiso 1 1 calc R . .
H44B H 0.0644 -0.1923 0.2695 0.075 Uiso 1 1 calc R . .
C45 C 0.1894(3) 0.0470(4) 0.2984(4) 0.0720(14) Uani 1 1 d . . .
H45A H 0.2477 0.0780 0.2766 0.086 Uiso 1 1 calc R . .
H45B H 0.2120 0.0861 0.3761 0.086 Uiso 1 1 calc R . .
C46 C 0.0922(4) 0.0640(4) 0.2509(5) 0.0938(19) Uani 1 1 d . . .
H46A H 0.1076 0.1434 0.2760 0.113 Uiso 1 1 calc R . .
H46B H 0.0733 0.0299 0.1735 0.113 Uiso 1 1 calc R . .
O7 O 0.0040(2) 0.0182(3) 0.2771(3) 0.0757(10) Uani 1 1 d . . .
O8 O 0.1697(2) -0.0668(3) 0.2660(2) 0.0679(8) Uani 1 1 d . . .
C47 C -0.0522(3) 0.3993(3) -0.0920(2) 0.0390(8) Uani 1 1 d . . .
H47A H -0.1124 0.3284 -0.1347 0.047 Uiso 1 1 calc R . .
H47B H -0.0047 0.4058 -0.1332 0.047 Uiso 1 1 calc R . .
C48 C 0.0939(3) 0.5086(3) 0.0692(3) 0.0414(8) Uani 1 1 d . . .
H48A H 0.1442 0.5172 0.0311 0.050 Uiso 1 1 calc R . .
H48B H 0.1329 0.5114 0.1363 0.050 Uiso 1 1 calc R . .
O9 O 0.00587(18) 0.40159(19) 0.00510(18) 0.0433(6) Uani 1 1 d . . .


_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
C1 N1 1.331(4) . ?
C1 C2 1.399(4) . ?
C1 H1 0.9300 . ?
C2 C3 1.368(4) . ?
C2 H2 0.9300 . ?
C3 C4 1.421(4) . ?
C3 H3 0.9300 . ?
C4 N1 1.393(4) . ?
C4 C5 1.407(4) . ?
C5 C6 1.400(4) . ?
C5 C10 1.489(4) . ?
C6 N2 1.397(3) . ?
C6 C7 1.415(4) . ?
C7 C8 1.376(4) . ?
C7 H7 0.9300 . ?
C8 C9 1.399(4) . ?
C8 H8 0.9300 . ?
C9 N2 1.338(3) . ?
C9 H9 0.9300 . ?
C10 C15 1.391(4) . ?
C10 C11 1.399(4) . ?
C11 C12 1.383(4) . ?
C11 H11 0.9300 . ?
C12 C13 1.384(4) . ?
C12 H12 0.9300 . ?
C13 C14 1.386(4) . ?
C13 C16 1.498(4) . ?
C14 C15 1.393(4) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 O3 1.228(3) . ?
C16 N3 1.328(4) . ?
C17 C18 1.504(5) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 O1 1.282(4) . ?
C18 C19 1.387(5) . ?
C19 C20 1.397(5) . ?
C19 H19 0.9300 . ?
C20 O2 1.276(3) . ?
C20 C21 1.508(5) . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 N4 1.344(4) . ?
C22 C23 1.405(4) . ?
C22 H22 0.9300 . ?
C23 C24 1.364(4) . ?
C23 H23 0.9300 . ?
C24 C25 1.423(4) . ?
C24 H24 0.9300 . ?
C25 N4 1.395(4) . ?
C25 C26 1.399(4) . ?
C26 C27 1.406(4) . ?
C26 C31 1.494(4) . ?
C27 N5 1.395(4) . ?
C27 C28 1.410(4) . ?
C28 C29 1.364(4) . ?
C28 H28 0.9300 . ?
C29 C30 1.396(4) . ?
C29 H29 0.9300 . ?
C30 N5 1.337(4) . ?
C30 H30 0.9300 . ?
C31 C32 1.392(4) . ?
C31 C36 1.393(4) . ?
C32 C33 1.376(4) . ?
C32 H32 0.9300 . ?
C33 C34 1.387(4) . ?
C33 H33 0.9300 . ?
C34 C35 1.389(4) . ?
C34 C37 1.502(4) . ?
C35 C36 1.377(4) . ?
C35 H35 0.9300 . ?
C36 H36 0.9300 . ?
C37 O6 1.236(3) . ?
C37 N6 1.332(4) . ?
C38 C39 1.498(4) . ?
C38 H38A 0.9600 . ?
C38 H38B 0.9600 . ?
C38 H38C 0.9600 . ?
C39 O4 1.273(4) . ?
C39 C40 1.390(5) . ?
C40 C41 1.388(4) . ?
C40 H40 0.9300 . ?
C41 O5 1.286(4) . ?
C41 C42 1.501(4) . ?
C42 H42A 0.9600 . ?
C42 H42B 0.9600 . ?
C42 H42C 0.9600 . ?
N1 Cu1 1.962(2) . ?
N2 Cu1 1.954(2) . ?
N3 H3A 0.8600 . ?
N3 H3B 0.8600 . ?
N4 Cu2 1.962(2) . ?
N5 Cu2 1.961(2) . ?
N6 H6A 0.8600 . ?
N6 H6B 0.8600 . ?
O1 Cu1 1.937(2) . ?
O2 Cu1 1.938(2) . ?
O4 Cu2 1.930(2) . ?
O5 Cu2 1.939(2) . ?
C43 O7 1.390(5) . ?
C43 C44 1.473(6) . ?
C43 H43A 0.9700 . ?
C43 H43B 0.9700 . ?
C44 O8 1.428(5) . ?
C44 H44A 0.9700 . ?
C44 H44B 0.9700 . ?
C45 O8 1.401(5) . ?
C45 C46 1.460(6) . ?
C45 H45A 0.9700 . ?
C45 H45B 0.9700 . ?
C46 O7 1.400(5) . ?
C46 H46A 0.9700 . ?
C46 H46B 0.9700 . ?
C47 O9 1.423(4) . ?
C47 C48 1.475(5) 2_565 ?
C47 H47A 0.9700 . ?
C47 H47B 0.9700 . ?
C48 O9 1.447(4) . ?
C48 C47 1.475(5) 2_565 ?
C48 H48A 0.9700 . ?
C48 H48B 0.9700 . ?

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 C1 C2 111.7(3) . . ?
N1 C1 H1 124.1 . . ?
C2 C1 H1 124.1 . . ?
C3 C2 C1 106.6(3) . . ?
C3 C2 H2 126.7 . . ?
C1 C2 H2 126.7 . . ?
C2 C3 C4 106.9(3) . . ?
C2 C3 H3 126.5 . . ?
C4 C3 H3 126.5 . . ?
N1 C4 C5 124.0(2) . . ?
N1 C4 C3 108.4(2) . . ?
C5 C4 C3 127.4(3) . . ?
C6 C5 C4 125.1(3) . . ?
C6 C5 C10 117.1(2) . . ?
C4 C5 C10 117.7(2) . . ?
N2 C6 C5 123.2(2) . . ?
N2 C6 C7 108.3(2) . . ?
C5 C6 C7 128.3(3) . . ?
C8 C7 C6 107.5(3) . . ?
C8 C7 H7 126.2 . . ?
C6 C7 H7 126.2 . . ?
C7 C8 C9 106.0(2) . . ?
C7 C8 H8 127.0 . . ?
C9 C8 H8 127.0 . . ?
N2 C9 C8 112.0(3) . . ?
N2 C9 H9 124.0 . . ?
C8 C9 H9 124.0 . . ?
C15 C10 C11 118.7(3) . . ?
C15 C10 C5 120.5(2) . . ?
C11 C10 C5 120.7(2) . . ?
C12 C11 C10 120.5(3) . . ?
C12 C11 H11 119.8 . . ?
C10 C11 H11 119.8 . . ?
C11 C12 C13 120.6(3) . . ?
C11 C12 H12 119.7 . . ?
C13 C12 H12 119.7 . . ?
C12 C13 C14 119.5(3) . . ?
C12 C13 C16 118.0(3) . . ?
C14 C13 C16 122.5(3) . . ?
C13 C14 C15 120.2(3) . . ?
C13 C14 H14 119.9 . . ?
C15 C14 H14 119.9 . . ?
C10 C15 C14 120.5(3) . . ?
C10 C15 H15 119.8 . . ?
C14 C15 H15 119.8 . . ?
O3 C16 N3 122.0(3) . . ?
O3 C16 C13 119.7(3) . . ?
N3 C16 C13 118.2(3) . . ?
C18 C17 H17A 109.5 . . ?
C18 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C18 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
O1 C18 C19 124.7(3) . . ?
O1 C18 C17 115.4(3) . . ?
C19 C18 C17 119.9(3) . . ?
C18 C19 C20 123.6(3) . . ?
C18 C19 H19 118.2 . . ?
C20 C19 H19 118.2 . . ?
O2 C20 C19 125.3(3) . . ?
O2 C20 C21 115.2(3) . . ?
C19 C20 C21 119.4(3) . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N4 C22 C23 111.2(3) . . ?
N4 C22 H22 124.4 . . ?
C23 C22 H22 124.4 . . ?
C24 C23 C22 106.9(3) . . ?
C24 C23 H23 126.6 . . ?
C22 C23 H23 126.6 . . ?
C23 C24 C25 107.2(3) . . ?
C23 C24 H24 126.4 . . ?
C25 C24 H24 126.4 . . ?
N4 C25 C26 123.7(3) . . ?
N4 C25 C24 108.4(2) . . ?
C26 C25 C24 127.8(3) . . ?
C25 C26 C27 125.3(3) . . ?
C25 C26 C31 117.6(3) . . ?
C27 C26 C31 117.1(2) . . ?
N5 C27 C26 123.8(3) . . ?
N5 C27 C28 108.5(3) . . ?
C26 C27 C28 127.7(3) . . ?
C29 C28 C27 107.5(3) . . ?
C29 C28 H28 126.3 . . ?
C27 C28 H28 126.3 . . ?
C28 C29 C30 106.3(3) . . ?
C28 C29 H29 126.8 . . ?
C30 C29 H29 126.8 . . ?
N5 C30 C29 111.8(3) . . ?
N5 C30 H30 124.1 . . ?
C29 C30 H30 124.1 . . ?
C32 C31 C36 118.3(3) . . ?
C32 C31 C26 120.4(2) . . ?
C36 C31 C26 121.3(3) . . ?
C33 C32 C31 120.8(3) . . ?
C33 C32 H32 119.6 . . ?
C31 C32 H32 119.6 . . ?
C32 C33 C34 121.0(3) . . ?
C32 C33 H33 119.5 . . ?
C34 C33 H33 119.5 . . ?
C33 C34 C35 118.3(3) . . ?
C33 C34 C37 122.7(3) . . ?
C35 C34 C37 119.0(3) . . ?
C36 C35 C34 120.9(3) . . ?
C36 C35 H35 119.5 . . ?
C34 C35 H35 119.5 . . ?
C35 C36 C31 120.7(3) . . ?
C35 C36 H36 119.7 . . ?
C31 C36 H36 119.7 . . ?
O6 C37 N6 122.2(3) . . ?
O6 C37 C34 121.5(3) . . ?
N6 C37 C34 116.2(3) . . ?
C39 C38 H38A 109.5 . . ?
C39 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C39 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
O4 C39 C40 124.3(3) . . ?
O4 C39 C38 115.2(3) . . ?
C40 C39 C38 120.5(3) . . ?
C41 C40 C39 124.1(3) . . ?
C41 C40 H40 118.0 . . ?
C39 C40 H40 118.0 . . ?
O5 C41 C40 124.4(3) . . ?
O5 C41 C42 115.5(3) . . ?
C40 C41 C42 120.1(3) . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C1 N1 C4 106.3(2) . . ?
C1 N1 Cu1 126.7(2) . . ?
C4 N1 Cu1 126.78(18) . . ?
C9 N2 C6 106.2(2) . . ?
C9 N2 Cu1 125.97(19) . . ?
C6 N2 Cu1 127.47(18) . . ?
C16 N3 H3A 120.0 . . ?
C16 N3 H3B 120.0 . . ?
H3A N3 H3B 120.0 . . ?
C22 N4 C25 106.3(2) . . ?
C22 N4 Cu2 125.6(2) . . ?
C25 N4 Cu2 127.87(19) . . ?
C30 N5 C27 105.8(2) . . ?
C30 N5 Cu2 126.2(2) . . ?
C27 N5 Cu2 127.62(19) . . ?
C37 N6 H6A 120.0 . . ?
C37 N6 H6B 120.0 . . ?
H6A N6 H6B 120.0 . . ?
C18 O1 Cu1 126.2(2) . . ?
C20 O2 Cu1 126.2(2) . . ?
C39 O4 Cu2 127.6(2) . . ?
C41 O5 Cu2 126.3(2) . . ?
O1 Cu1 O2 90.93(9) . . ?
O1 Cu1 N2 178.64(9) . . ?
O2 Cu1 N2 89.40(9) . . ?
O1 Cu1 N1 88.94(10) . . ?
O2 Cu1 N1 174.04(9) . . ?
N2 Cu1 N1 90.87(10) . . ?
O4 Cu2 O5 90.38(9) . . ?
O4 Cu2 N5 175.50(9) . . ?
O5 Cu2 N5 89.94(9) . . ?
O4 Cu2 N4 88.52(9) . . ?
O5 Cu2 N4 177.23(9) . . ?
N5 Cu2 N4 91.35(10) . . ?
O7 C43 C44 110.8(3) . . ?
O7 C43 H43A 109.5 . . ?
C44 C43 H43A 109.5 . . ?
O7 C43 H43B 109.5 . . ?
C44 C43 H43B 109.5 . . ?
H43A C43 H43B 108.1 . . ?
O8 C44 C43 110.0(3) . . ?
O8 C44 H44A 109.7 . . ?
C43 C44 H44A 109.7 . . ?
O8 C44 H44B 109.7 . . ?
C43 C44 H44B 109.7 . . ?
H44A C44 H44B 108.2 . . ?
O8 C45 C46 110.9(4) . . ?
O8 C45 H45A 109.5 . . ?
C46 C45 H45A 109.5 . . ?
O8 C45 H45B 109.5 . . ?
C46 C45 H45B 109.5 . . ?
H45A C45 H45B 108.0 . . ?
O7 C46 C45 112.2(4) . . ?
O7 C46 H46A 109.2 . . ?
C45 C46 H46A 109.2 . . ?
O7 C46 H46B 109.2 . . ?
C45 C46 H46B 109.2 . . ?
H46A C46 H46B 107.9 . . ?
C43 O7 C46 108.8(4) . . ?
C45 O8 C44 109.0(3) . . ?
O9 C47 C48 110.8(3) . 2_565 ?
O9 C47 H47A 109.5 . . ?
C48 C47 H47A 109.5 2_565 . ?
O9 C47 H47B 109.5 . . ?
C48 C47 H47B 109.5 2_565 . ?
H47A C47 H47B 108.1 . . ?
O9 C48 C47 110.8(3) . 2_565 ?
O9 C48 H48A 109.5 . . ?
C47 C48 H48A 109.5 2_565 . ?
O9 C48 H48B 109.5 . . ?
C47 C48 H48B 109.5 2_565 . ?
H48A C48 H48B 108.1 . . ?
C47 O9 C48 109.0(2) . . ?

_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full        27.53
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max         0.894
_refine_diff_density_min         -0.706
_refine_diff_density_rms         0.164

#===END

###Material relevant to compound 7(CHCl3) at 173K ##

data_compound7CHCl3
_database_code_depnum_ccdc_archive 'CCDC 717003'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ' C32 H26 Co N5 O3, C H Cl3'
_chemical_formula_sum            'C33 H27 Cl3 Co N5 O3'
_chemical_formula_weight         706.88

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'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P2(1)/c '
_symmetry_space_group_name_Hall  '-P 2ybc'

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

_cell_length_a                   13.4382(5)
_cell_length_b                   21.1339(8)
_cell_length_c                   12.3217(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 114.3580(10)
_cell_angle_gamma                90.00
_cell_volume                     3187.9(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    6566
_cell_measurement_theta_min      2.55
_cell_measurement_theta_max      25.25

_exptl_crystal_description       prism
_exptl_crystal_colour            dark-red
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.14
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.473
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1448
_exptl_absorpt_coefficient_mu    0.833
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7650
_exptl_absorpt_correction_T_max  0.8923
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            30856
_diffrn_reflns_av_R_equivalents  0.0541
_diffrn_reflns_av_sigmaI/netI    0.0597
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.66
_diffrn_reflns_theta_max         27.53
_reflns_number_total             7325
_reflns_number_gt                4826
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² 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/[σ²(Fo²)+(0.1751P)²+6.2311P] where P=(Fo²+2Fc²)/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     SHELXL
_refine_ls_extinction_coef       0.027(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         7325
_refine_ls_number_parameters     407
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1305
_refine_ls_R_factor_gt           0.0881
_refine_ls_wR_factor_ref         0.2930
_refine_ls_wR_factor_gt          0.2598
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_restrained_S_all      1.060
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.6808(5) 0.2897(2) 0.2424(5) 0.0350(11) Uani 1 1 d . . .
H1 H 0.6284 0.3119 0.1797 0.042 Uiso 1 1 calc R . .
C2 C 0.7884(5) 0.3109(3) 0.3088(5) 0.0393(12) Uani 1 1 d . . .
H2 H 0.8189 0.3488 0.2991 0.047 Uiso 1 1 calc R . .
C3 C 0.8389(4) 0.2644(3) 0.3902(5) 0.0373(12) Uani 1 1 d . . .
H3 H 0.9115 0.2647 0.4450 0.045 Uiso 1 1 calc R . .
C4 C 0.7631(4) 0.2162(2) 0.3776(4) 0.0310(11) Uani 1 1 d . . .
C5 C 0.7698(4) 0.1648(2) 0.4518(5) 0.0314(11) Uani 1 1 d . . .
C6 C 0.6789(4) 0.1289(2) 0.4428(4) 0.0309(11) Uani 1 1 d . . .
C7 C 0.6676(5) 0.0901(3) 0.5327(5) 0.0383(12) Uani 1 1 d . . .
H7 H 0.7235 0.0756 0.6025 0.046 Uiso 1 1 calc R . .
C8 C 0.5592(5) 0.0787(3) 0.4958(5) 0.0389(12) Uani 1 1 d . . .
H8 H 0.5264 0.0561 0.5369 0.047 Uiso 1 1 calc R . .
C9 C 0.5050(5) 0.1079(2) 0.3825(5) 0.0352(11) Uani 1 1 d . . .
H9 H 0.4300 0.1066 0.3369 0.042 Uiso 1 1 calc R . .
C10 C 0.8760(4) 0.1504(3) 0.5532(5) 0.0349(11) Uani 1 1 d . . .
C11 C 0.9298(4) 0.1941(3) 0.6406(5) 0.0341(11) Uani 1 1 d . . .
H11 H 0.9018 0.2348 0.6342 0.041 Uiso 1 1 calc R . .
C12 C 1.0256(4) 0.1784(3) 0.7387(5) 0.0362(12) Uani 1 1 d . . .
H12 H 1.0613 0.2086 0.7968 0.043 Uiso 1 1 calc R . .
C13 C 1.0674(4) 0.1177(3) 0.7490(5) 0.0371(12) Uani 1 1 d . . .
C14 C 1.0150(5) 0.0735(3) 0.6612(5) 0.0457(14) Uani 1 1 d . . .
H14 H 1.0442 0.0331 0.6671 0.055 Uiso 1 1 calc R . .
C15 C 0.9191(5) 0.0891(3) 0.5642(5) 0.0447(14) Uani 1 1 d . . .
H15 H 0.8834 0.0589 0.5064 0.054 Uiso 1 1 calc R . .
C16 C 1.1700(4) 0.0963(3) 0.8544(5) 0.0419(13) Uani 1 1 d . . .
C17 C 0.3683(5) 0.2584(3) 0.1280(5) 0.0394(12) Uani 1 1 d . . .
C18 C 0.2792(5) 0.2848(4) 0.1466(6) 0.0556(17) Uani 1 1 d . . .
H18 H 0.2756 0.2790 0.2197 0.067 Uiso 1 1 calc R . .
C19 C 0.1980(7) 0.3187(5) 0.0589(8) 0.081(3) Uani 1 1 d . . .
H19 H 0.1392 0.3336 0.0728 0.097 Uiso 1 1 calc R . .
C20 C 0.2021(7) 0.3312(5) -0.0499(8) 0.084(3) Uani 1 1 d . . .
H20 H 0.1480 0.3553 -0.1074 0.100 Uiso 1 1 calc R . .
C21 C 0.2884(6) 0.3069(4) -0.0708(6) 0.0583(18) Uani 1 1 d . . .
H21 H 0.2915 0.3147 -0.1436 0.070 Uiso 1 1 calc R . .
C22 C 0.3725(5) 0.2703(3) 0.0168(5) 0.0403(13) Uani 1 1 d . . .
C23 C 0.4565(5) 0.2472(3) -0.0139(5) 0.0374(12) Uani 1 1 d . . .
H23 H 0.4567 0.2607 -0.0857 0.045 Uiso 1 1 calc R . .
C24 C 0.6145(5) 0.1898(3) 0.0064(6) 0.0455(14) Uani 1 1 d . . .
H24A H 0.6430 0.2266 -0.0182 0.055 Uiso 1 1 calc R . .
H24B H 0.5818 0.1618 -0.0616 0.055 Uiso 1 1 calc R . .
C25 C 0.7062(5) 0.1557(3) 0.1075(6) 0.0438(14) Uani 1 1 d . . .
H25A H 0.7449 0.1271 0.0767 0.053 Uiso 1 1 calc R . .
H25B H 0.7578 0.1857 0.1610 0.053 Uiso 1 1 calc R . .
C26 C 0.6475(5) 0.0597(3) 0.1669(5) 0.0423(13) Uani 1 1 d . . .
H26 H 0.7013 0.0380 0.1530 0.051 Uiso 1 1 calc R . .
C27 C 0.5653(5) 0.0238(3) 0.1861(5) 0.0408(13) Uani 1 1 d . . .
C28 C 0.5853(6) -0.0394(3) 0.2242(6) 0.0515(15) Uani 1 1 d . . .
H28 H 0.6548 -0.0564 0.2462 0.062 Uiso 1 1 calc R . .
C29 C 0.5031(7) -0.0764(3) 0.2294(6) 0.0591(19) Uani 1 1 d . . .
H29 H 0.5174 -0.1175 0.2588 0.071 Uiso 1 1 calc R . .
C30 C 0.3988(6) -0.0514(3) 0.1900(6) 0.0507(16) Uani 1 1 d . . .
H30 H 0.3422 -0.0769 0.1896 0.061 Uiso 1 1 calc R . .
C31 C 0.3768(5) 0.0105(3) 0.1512(5) 0.0459(14) Uani 1 1 d . . .
H31 H 0.3057 0.0258 0.1243 0.055 Uiso 1 1 calc R . .
C32 C 0.4606(4) 0.0508(3) 0.1519(5) 0.0355(12) Uani 1 1 d . . .
N1 N 0.6637(3) 0.23306(19) 0.2814(4) 0.0291(9) Uani 1 1 d . . .
N2 N 0.5757(3) 0.13718(19) 0.3507(4) 0.0293(9) Uani 1 1 d . . .
N3 N 1.2335(4) 0.1394(3) 0.9252(5) 0.0623(17) Uani 1 1 d . . .
H3A H 1.2911 0.1283 0.9863 0.075 Uiso 1 1 calc R . .
H3B H 1.2177 0.1788 0.9109 0.075 Uiso 1 1 calc R . .
N4 N 0.5322(4) 0.2091(2) 0.0498(4) 0.0347(10) Uani 1 1 d . . .
N5 N 0.6496(3) 0.1207(2) 0.1681(4) 0.0349(10) Uani 1 1 d . . .
O1 O 1.1889(4) 0.0391(2) 0.8708(5) 0.0656(14) Uani 1 1 d . . .
O2 O 0.4399(3) 0.22553(17) 0.2143(3) 0.0329(8) Uani 1 1 d . . .
O3 O 0.4389(3) 0.11081(17) 0.1217(3) 0.0342(8) Uani 1 1 d . . .
Co1 Co 0.54894(5) 0.17357(3) 0.19834(6) 0.0276(3) Uani 1 1 d . . .
C33 C 1.0044(18) 0.4478(9) 0.642(2) 0.226(12) Uani 1 1 d . . .
H33 H 0.9599 0.4862 0.6175 0.272 Uiso 1 1 calc R . .
Cl1 Cl 1.1385(4) 0.4701(3) 0.7333(6) 0.201(2) Uani 1 1 d . . .
Cl2 Cl 0.9609(5) 0.4016(4) 0.7501(10) 0.316(6) Uani 1 1 d . . .
Cl3 Cl 0.9857(10) 0.4104(7) 0.5311(12) 0.406(8) Uani 1 1 d . . .


_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
C1 N1 1.344(7) . ?
C1 C2 1.410(8) . ?
C1 H1 0.9300 . ?
C2 C3 1.368(8) . ?
C2 H2 0.9300 . ?
C3 C4 1.404(7) . ?
C3 H3 0.9300 . ?
C4 C5 1.397(7) . ?
C4 N1 1.418(6) . ?
C5 C6 1.403(7) . ?
C5 C10 1.491(7) . ?
C6 N2 1.394(6) . ?
C6 C7 1.436(7) . ?
C7 C8 1.356(8) . ?
C7 H7 0.9300 . ?
C8 C9 1.422(8) . ?
C8 H8 0.9300 . ?
C9 N2 1.321(7) . ?
C9 H9 0.9300 . ?
C10 C11 1.375(8) . ?
C10 C15 1.402(8) . ?
C11 C12 1.394(7) . ?
C11 H11 0.9300 . ?
C12 C13 1.386(8) . ?
C12 H12 0.9300 . ?
C13 C14 1.382(8) . ?
C13 C16 1.522(7) . ?
C14 C15 1.388(8) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 O1 1.235(8) . ?
C16 N3 1.306(8) . ?
C17 O2 1.301(7) . ?
C17 C22 1.417(8) . ?
C17 C18 1.423(9) . ?
C18 C19 1.379(10) . ?
C18 H18 0.9300 . ?
C19 C20 1.388(12) . ?
C19 H19 0.9300 . ?
C20 C21 1.386(11) . ?
C20 H20 0.9300 . ?
C21 C22 1.427(8) . ?
C21 H21 0.9300 . ?
C22 C23 1.417(8) . ?
C23 N4 1.281(7) . ?
C23 H23 0.9300 . ?
C24 N4 1.471(7) . ?
C24 C25 1.524(9) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C25 N5 1.467(7) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C26 N5 1.290(7) . ?
C26 C27 1.438(8) . ?
C26 H26 0.9300 . ?
C27 C28 1.405(8) . ?
C27 C32 1.411(8) . ?
C28 C29 1.377(10) . ?
C28 H28 0.9300 . ?
C29 C30 1.385(10) . ?
C29 H29 0.9300 . ?
C30 C31 1.384(9) . ?
C30 H30 0.9300 . ?
C31 C32 1.409(8) . ?
C31 H31 0.9300 . ?
C32 O3 1.320(6) . ?
N1 Co1 1.925(4) . ?
N2 Co1 1.921(4) . ?
N3 H3A 0.8600 . ?
N3 H3B 0.8600 . ?
N4 Co1 1.903(4) . ?
N5 Co1 1.906(4) . ?
O2 Co1 1.904(4) . ?
O3 Co1 1.920(4) . ?
C33 Cl3 1.50(2) . ?
C33 Cl1 1.752(19) . ?
C33 Cl2 1.93(3) . ?
C33 H33 0.9800 . ?

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 C1 C2 111.2(5) . . ?
N1 C1 H1 124.4 . . ?
C2 C1 H1 124.4 . . ?
C3 C2 C1 106.1(5) . . ?
C3 C2 H2 127.0 . . ?
C1 C2 H2 127.0 . . ?
C2 C3 C4 108.8(5) . . ?
C2 C3 H3 125.6 . . ?
C4 C3 H3 125.6 . . ?
C5 C4 C3 130.0(5) . . ?
C5 C4 N1 121.8(4) . . ?
C3 C4 N1 107.5(4) . . ?
C4 C5 C6 123.3(5) . . ?
C4 C5 C10 119.2(5) . . ?
C6 C5 C10 117.2(5) . . ?
N2 C6 C5 122.5(4) . . ?
N2 C6 C7 108.2(4) . . ?
C5 C6 C7 127.9(5) . . ?
C8 C7 C6 106.4(5) . . ?
C8 C7 H7 126.8 . . ?
C6 C7 H7 126.8 . . ?
C7 C8 C9 107.3(5) . . ?
C7 C8 H8 126.3 . . ?
C9 C8 H8 126.3 . . ?
N2 C9 C8 110.7(5) . . ?
N2 C9 H9 124.6 . . ?
C8 C9 H9 124.6 . . ?
C11 C10 C15 118.8(5) . . ?
C11 C10 C5 122.1(5) . . ?
C15 C10 C5 119.0(5) . . ?
C10 C11 C12 121.3(5) . . ?
C10 C11 H11 119.4 . . ?
C12 C11 H11 119.4 . . ?
C13 C12 C11 119.5(5) . . ?
C13 C12 H12 120.2 . . ?
C11 C12 H12 120.2 . . ?
C14 C13 C12 119.9(5) . . ?
C14 C13 C16 117.2(5) . . ?
C12 C13 C16 122.9(5) . . ?
C13 C14 C15 120.3(5) . . ?
C13 C14 H14 119.9 . . ?
C15 C14 H14 119.9 . . ?
C14 C15 C10 120.2(5) . . ?
C14 C15 H15 119.9 . . ?
C10 C15 H15 119.9 . . ?
O1 C16 N3 122.7(5) . . ?
O1 C16 C13 118.9(5) . . ?
N3 C16 C13 118.4(5) . . ?
O2 C17 C22 125.0(5) . . ?
O2 C17 C18 117.8(5) . . ?
C22 C17 C18 117.3(5) . . ?
C19 C18 C17 121.6(6) . . ?
C19 C18 H18 119.2 . . ?
C17 C18 H18 119.2 . . ?
C18 C19 C20 121.5(7) . . ?
C18 C19 H19 119.3 . . ?
C20 C19 H19 119.3 . . ?
C21 C20 C19 118.6(7) . . ?
C21 C20 H20 120.7 . . ?
C19 C20 H20 120.7 . . ?
C20 C21 C22 121.5(6) . . ?
C20 C21 H21 119.2 . . ?
C22 C21 H21 119.2 . . ?
C23 C22 C17 123.5(5) . . ?
C23 C22 C21 117.1(5) . . ?
C17 C22 C21 119.5(6) . . ?
N4 C23 C22 124.8(5) . . ?
N4 C23 H23 117.6 . . ?
C22 C23 H23 117.6 . . ?
N4 C24 C25 108.1(5) . . ?
N4 C24 H24A 110.1 . . ?
C25 C24 H24A 110.1 . . ?
N4 C24 H24B 110.1 . . ?
C25 C24 H24B 110.1 . . ?
H24A C24 H24B 108.4 . . ?
N5 C25 C24 103.8(5) . . ?
N5 C25 H25A 111.0 . . ?
C24 C25 H25A 111.0 . . ?
N5 C25 H25B 111.0 . . ?
C24 C25 H25B 111.0 . . ?
H25A C25 H25B 109.0 . . ?
N5 C26 C27 122.7(5) . . ?
N5 C26 H26 118.6 . . ?
C27 C26 H26 118.6 . . ?
C28 C27 C32 120.9(6) . . ?
C28 C27 C26 120.1(6) . . ?
C32 C27 C26 118.5(5) . . ?
C29 C28 C27 120.6(7) . . ?
C29 C28 H28 119.7 . . ?
C27 C28 H28 119.7 . . ?
C28 C29 C30 118.9(6) . . ?
C28 C29 H29 120.5 . . ?
C30 C29 H29 120.5 . . ?
C29 C30 C31 121.5(6) . . ?
C29 C30 H30 119.2 . . ?
C31 C30 H30 119.2 . . ?
C30 C31 C32 120.9(6) . . ?
C30 C31 H31 119.6 . . ?
C32 C31 H31 119.6 . . ?
O3 C32 C31 119.7(5) . . ?
O3 C32 C27 123.3(5) . . ?
C31 C32 C27 117.0(5) . . ?
C1 N1 C4 106.4(4) . . ?
C1 N1 Co1 127.5(4) . . ?
C4 N1 Co1 123.5(3) . . ?
C9 N2 C6 107.2(4) . . ?
C9 N2 Co1 127.5(4) . . ?
C6 N2 Co1 124.6(3) . . ?
C16 N3 H3A 120.0 . . ?
C16 N3 H3B 120.0 . . ?
H3A N3 H3B 120.0 . . ?
C23 N4 C24 118.5(5) . . ?
C23 N4 Co1 126.0(4) . . ?
C24 N4 Co1 115.5(4) . . ?
C26 N5 C25 120.8(5) . . ?
C26 N5 Co1 125.0(4) . . ?
C25 N5 Co1 111.3(3) . . ?
C17 O2 Co1 124.4(3) . . ?
C32 O3 Co1 119.3(3) . . ?
N4 Co1 O2 94.60(17) . . ?
N4 Co1 N5 81.7(2) . . ?
O2 Co1 N5 174.99(17) . . ?
N4 Co1 O3 92.16(17) . . ?
O2 Co1 O3 88.87(16) . . ?
N5 Co1 O3 87.91(17) . . ?
N4 Co1 N2 176.33(18) . . ?
O2 Co1 N2 88.40(16) . . ?
N5 Co1 N2 95.44(19) . . ?
O3 Co1 N2 90.01(16) . . ?
N4 Co1 N1 90.28(18) . . ?
O2 Co1 N1 92.87(17) . . ?
N5 Co1 N1 90.52(18) . . ?
O3 Co1 N1 176.88(16) . . ?
N2 Co1 N1 87.45(17) . . ?
Cl3 C33 Cl1 118.0(18) . . ?
Cl3 C33 Cl2 112.2(12) . . ?
Cl1 C33 Cl2 102.4(13) . . ?
Cl3 C33 H33 108.0 . . ?
Cl1 C33 H33 108.0 . . ?
Cl2 C33 H33 108.0 . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        27.53
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         1.393
_refine_diff_density_min         -1.086
_refine_diff_density_rms         0.248

#===END

###Material relevant to compound 7(acetone) at 173K ##

data_7(acetone)
_database_code_depnum_ccdc_archive 'CCDC 717004'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C32 H26 Co N5 O3), 3(C3 H6 O)'
_chemical_formula_sum            'C73 H70 Co2 N10 O9'
_chemical_formula_weight         1349.25

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'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   'Pbcn '
_symmetry_space_group_name_Hall  '-P 2n 2ab '

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

_cell_length_a                   23.4552(4)
_cell_length_b                   17.1577(3)
_cell_length_c                   17.1153(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     6887.8(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    9428
_cell_measurement_theta_min      2.37
_cell_measurement_theta_max      26.21

_exptl_crystal_description       rod
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.301
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2816
_exptl_absorpt_coefficient_mu    0.545
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9424
_exptl_absorpt_correction_T_max  0.9785
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            70305
_diffrn_reflns_av_R_equivalents  0.0622
_diffrn_reflns_av_sigmaI/netI    0.0404
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.47
_diffrn_reflns_theta_max         27.55
_reflns_number_total             7937
_reflns_number_gt                5846
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'

_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² 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/[σ²(Fo²)+(0.1066P)²+7.7569P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7937
_refine_ls_number_parameters     403
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0895
_refine_ls_R_factor_gt           0.0611
_refine_ls_wR_factor_ref         0.1986
_refine_ls_wR_factor_gt          0.1743
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_restrained_S_all      1.096
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.20176(15) 0.0645(2) 0.8259(2) 0.0327(8) Uani 1 1 d . . .
H1 H 0.1777 0.0230 0.8143 0.039 Uiso 1 1 calc R . .
C2 C 0.24659(16) 0.0613(2) 0.8801(2) 0.0396(9) Uani 1 1 d . . .
H2 H 0.2576 0.0184 0.9098 0.047 Uiso 1 1 calc R . .
C3 C 0.27105(16) 0.1341(2) 0.8805(2) 0.0373(8) Uani 1 1 d . . .
H3 H 0.3014 0.1501 0.9116 0.045 Uiso 1 1 calc R . .
C4 C 0.24178(14) 0.1801(2) 0.82531(18) 0.0289(7) Uani 1 1 d . . .
C5 C 0.25772(15) 0.2534(2) 0.79634(19) 0.0297(7) Uani 1 1 d . . .
C6 C 0.23608(15) 0.2852(2) 0.72746(19) 0.0312(8) Uani 1 1 d . . .
C7 C 0.25579(17) 0.3511(2) 0.6845(2) 0.0400(9) Uani 1 1 d . . .
H7 H 0.2820 0.3880 0.7015 0.048 Uiso 1 1 calc R . .
C8 C 0.22885(18) 0.3497(2) 0.6136(2) 0.0434(10) Uani 1 1 d . . .
H8 H 0.2337 0.3850 0.5728 0.052 Uiso 1 1 calc R . .
C9 C 0.19234(15) 0.2845(2) 0.6143(2) 0.0334(8) Uani 1 1 d . . .
H9 H 0.1691 0.2701 0.5727 0.040 Uiso 1 1 calc R . .
C10 C 0.30483(15) 0.2945(2) 0.83777(19) 0.0303(7) Uani 1 1 d . . .
C11 C 0.29983(15) 0.3127(2) 0.9170(2) 0.0326(8) Uani 1 1 d . . .
H11 H 0.2668 0.2995 0.9439 0.039 Uiso 1 1 calc R . .
C12 C 0.34402(14) 0.3506(2) 0.95617(19) 0.0288(7) Uani 1 1 d . . .
H12 H 0.3406 0.3615 1.0092 0.035 Uiso 1 1 calc R . .
C13 C 0.39298(14) 0.37214(18) 0.91633(18) 0.0251(6) Uani 1 1 d . . .
C14 C 0.39811(15) 0.3524(2) 0.83792(19) 0.0314(7) Uani 1 1 d . . .
H14 H 0.4312 0.3658 0.8111 0.038 Uiso 1 1 calc R . .
C15 C 0.35512(16) 0.3132(2) 0.7988(2) 0.0337(8) Uani 1 1 d . . .
H15 H 0.3598 0.2995 0.7466 0.040 Uiso 1 1 calc R . .
C16 C 0.43927(13) 0.42095(18) 0.95206(18) 0.0226(6) Uani 1 1 d . . .
C17 C 0.14579(13) 0.02902(19) 0.63257(18) 0.0238(6) Uani 1 1 d . . .
C18 C 0.16769(15) -0.0151(2) 0.56998(19) 0.0304(7) Uani 1 1 d . . .
H18 H 0.1989 0.0038 0.5423 0.037 Uiso 1 1 calc R . .
C19 C 0.14428(16) -0.0851(2) 0.5488(2) 0.0381(9) Uani 1 1 d . . .
H19 H 0.1591 -0.1120 0.5062 0.046 Uiso 1 1 calc R . .
C20 C 0.09833(17) -0.1166(2) 0.5903(2) 0.0388(9) Uani 1 1 d . . .
H20 H 0.0822 -0.1639 0.5753 0.047 Uiso 1 1 calc R . .
C21 C 0.07772(15) -0.0770(2) 0.6528(2) 0.0317(8) Uani 1 1 d . . .
H21 H 0.0480 -0.0985 0.6815 0.038 Uiso 1 1 calc R . .
C22 C 0.10004(13) -0.00401(19) 0.67572(18) 0.0249(6) Uani 1 1 d . . .
C23 C 0.07557(13) 0.03379(19) 0.74292(19) 0.0257(7) Uani 1 1 d . . .
H23 H 0.0481 0.0063 0.7708 0.031 Uiso 1 1 calc R . .
C24 C 0.06162(16) 0.1321(2) 0.8402(2) 0.0331(8) Uani 1 1 d . . .
H24A H 0.0621 0.0925 0.8806 0.040 Uiso 1 1 calc R . .
H24B H 0.0224 0.1468 0.8303 0.040 Uiso 1 1 calc R . .
C25 C 0.09617(17) 0.2032(2) 0.8662(2) 0.0344(8) Uani 1 1 d . . .
H25A H 0.0740 0.2366 0.9005 0.041 Uiso 1 1 calc R . .
H25B H 0.1309 0.1877 0.8927 0.041 Uiso 1 1 calc R . .
C26 C 0.08280(17) 0.3060(2) 0.7749(2) 0.0367(8) Uani 1 1 d . . .
H26 H 0.0704 0.3374 0.8157 0.044 Uiso 1 1 calc R . .
C27 C 0.07173(18) 0.3318(2) 0.6959(2) 0.0399(9) Uani 1 1 d . . .
C28 C 0.0548(2) 0.4086(3) 0.6819(3) 0.0616(13) Uani 1 1 d . . .
H28 H 0.0572 0.4450 0.7221 0.074 Uiso 1 1 calc R . .
C29 C 0.0347(3) 0.4315(3) 0.6100(3) 0.0757(17) Uani 1 1 d . . .
H29 H 0.0242 0.4830 0.6009 0.091 Uiso 1 1 calc R . .
C30 C 0.0305(3) 0.3759(3) 0.5513(3) 0.0693(15) Uani 1 1 d . . .
H30 H 0.0164 0.3906 0.5027 0.083 Uiso 1 1 calc R . .
C31 C 0.04666(19) 0.2997(3) 0.5628(3) 0.0484(10) Uani 1 1 d . . .
H31 H 0.0427 0.2638 0.5224 0.058 Uiso 1 1 calc R . .
C32 C 0.06910(15) 0.2756(2) 0.6352(2) 0.0330(8) Uani 1 1 d . . .
N1 N 0.19817(12) 0.13525(17) 0.79285(15) 0.0261(6) Uani 1 1 d . . .
N2 N 0.19517(12) 0.24624(17) 0.68157(16) 0.0285(6) Uani 1 1 d . . .
N3 N 0.45259(11) 0.41087(16) 1.02640(15) 0.0255(6) Uani 1 1 d . . .
H3A H 0.4790 0.4386 1.0474 0.031 Uiso 1 1 calc R . .
H3B H 0.4348 0.3766 1.0538 0.031 Uiso 1 1 calc R . .
N4 N 0.08841(11) 0.10169(16) 0.76743(15) 0.0246(6) Uani 1 1 d . . .
N5 N 0.10872(12) 0.24231(17) 0.79198(16) 0.0297(6) Uani 1 1 d . . .
O1 O 0.46383(10) 0.46972(13) 0.91056(13) 0.0278(5) Uani 1 1 d . . .
O2 O 0.16831(9) 0.09778(13) 0.64545(12) 0.0264(5) Uani 1 1 d . . .
O3 O 0.08589(9) 0.20287(13) 0.64385(13) 0.0275(5) Uani 1 1 d . . .
Co1 Co 0.141627(18) 0.17058(2) 0.71998(2) 0.02277(15) Uani 1 1 d . . .
C33 C 0.6770(6) 0.0725(10) 0.8230(8) 0.215(4) Uani 1 1 d . . .
H33A H 0.6577 0.0644 0.7742 0.322 Uiso 1 1 calc R . .
H33B H 0.6787 0.0242 0.8512 0.322 Uiso 1 1 calc R . .
H33C H 0.7150 0.0909 0.8132 0.322 Uiso 1 1 calc R . .
C34 C 0.6465(8) 0.1293(12) 0.8684(9) 0.215(4) Uani 1 1 d D . .
C35 C 0.6719(6) 0.1475(10) 0.9402(8) 0.215(4) Uani 1 1 d D . .
H35A H 0.6493 0.1859 0.9668 0.322 Uiso 1 1 calc R . .
H35B H 0.7095 0.1678 0.9314 0.322 Uiso 1 1 calc R . .
H35C H 0.6743 0.1013 0.9717 0.322 Uiso 1 1 calc R . .
O4 O 0.5972(7) 0.1465(12) 0.8746(16) 0.481(16) Uani 1 1 d . . .
C36 C 0.5000 0.1774(16) 0.7500 0.405(11) Uani 1 2 d SD . .
C37 C 0.4651(9) 0.1291(13) 0.8044(13) 0.405(11) Uani 1 1 d D . .
H37A H 0.4437 0.1626 0.8384 0.607 Uiso 1 1 calc R . .
H37B H 0.4898 0.0966 0.8350 0.607 Uiso 1 1 calc R . .
H37C H 0.4394 0.0971 0.7748 0.607 Uiso 1 1 calc R . .
O5 O 0.5000 0.2517(15) 0.7500 0.405(11) Uani 1 2 d SD . .


_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
C1 N1 1.342(4) . ?
C1 C2 1.404(5) . ?
C1 H1 0.9300 . ?
C2 C3 1.375(5) . ?
C2 H2 0.9300 . ?
C3 C4 1.410(5) . ?
C3 H3 0.9300 . ?
C4 N1 1.396(4) . ?
C4 C5 1.402(5) . ?
C5 C6 1.395(5) . ?
C5 C10 1.490(4) . ?
C6 N2 1.409(4) . ?
C6 C7 1.426(5) . ?
C7 C8 1.369(5) . ?
C7 H7 0.9300 . ?
C8 C9 1.409(5) . ?
C8 H8 0.9300 . ?
C9 N2 1.327(4) . ?
C9 H9 0.9300 . ?
C10 C15 1.393(5) . ?
C10 C11 1.396(5) . ?
C11 C12 1.396(5) . ?
C11 H11 0.9300 . ?
C12 C13 1.386(5) . ?
C12 H12 0.9300 . ?
C13 C14 1.389(4) . ?
C13 C16 1.501(4) . ?
C14 C15 1.384(5) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 O1 1.240(4) . ?
C16 N3 1.321(4) . ?
C17 O2 1.311(4) . ?
C17 C18 1.409(5) . ?
C17 C22 1.421(4) . ?
C18 C19 1.369(5) . ?
C18 H18 0.9300 . ?
C19 C20 1.400(6) . ?
C19 H19 0.9300 . ?
C20 C21 1.357(5) . ?
C20 H20 0.9300 . ?
C21 C22 1.412(5) . ?
C21 H21 0.9300 . ?
C22 C23 1.440(5) . ?
C23 N4 1.274(4) . ?
C23 H23 0.9300 . ?
C24 N4 1.490(4) . ?
C24 C25 1.531(5) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C25 N5 1.467(4) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C26 N5 1.284(5) . ?
C26 C27 1.445(6) . ?
C26 H26 0.9300 . ?
C27 C28 1.397(6) . ?
C27 C32 1.419(5) . ?
C28 C29 1.376(7) . ?
C28 H28 0.9300 . ?
C29 C30 1.390(8) . ?
C29 H29 0.9300 . ?
C30 C31 1.375(7) . ?
C30 H30 0.9300 . ?
C31 C32 1.409(5) . ?
C31 H31 0.9300 . ?
C32 O3 1.317(4) . ?
N1 Co1 1.919(3) . ?
N2 Co1 1.922(3) . ?
N3 H3A 0.8600 . ?
N3 H3B 0.8600 . ?
N4 Co1 1.901(3) . ?
N5 Co1 1.905(3) . ?
O2 Co1 1.892(2) . ?
O3 Co1 1.927(2) . ?
C33 C34 1.44(2) . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
C34 O4 1.20(2) . ?
C34 C35 1.402(9) . ?
C35 H35A 0.9600 . ?
C35 H35B 0.9600 . ?
C35 H35C 0.9600 . ?
C36 O5 1.275(10) . ?
C36 C37 1.491(9) . ?
C36 C37 1.491(9) 3_656 ?
C37 H37A 0.9600 . ?
C37 H37B 0.9600 . ?
C37 H37C 0.9600 . ?

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 C1 C2 111.2(3) . . ?
N1 C1 H1 124.4 . . ?
C2 C1 H1 124.4 . . ?
C3 C2 C1 106.3(3) . . ?
C3 C2 H2 126.9 . . ?
C1 C2 H2 126.9 . . ?
C2 C3 C4 107.6(3) . . ?
C2 C3 H3 126.2 . . ?
C4 C3 H3 126.2 . . ?
N1 C4 C5 123.3(3) . . ?
N1 C4 C3 108.3(3) . . ?
C5 C4 C3 127.5(3) . . ?
C6 C5 C4 123.6(3) . . ?
C6 C5 C10 119.1(3) . . ?
C4 C5 C10 117.0(3) . . ?
C5 C6 N2 122.2(3) . . ?
C5 C6 C7 128.9(3) . . ?
N2 C6 C7 108.0(3) . . ?
C8 C7 C6 107.1(3) . . ?
C8 C7 H7 126.4 . . ?
C6 C7 H7 126.4 . . ?
C7 C8 C9 106.6(3) . . ?
C7 C8 H8 126.7 . . ?
C9 C8 H8 126.7 . . ?
N2 C9 C8 111.7(3) . . ?
N2 C9 H9 124.1 . . ?
C8 C9 H9 124.1 . . ?
C15 C10 C11 119.0(3) . . ?
C15 C10 C5 120.6(3) . . ?
C11 C10 C5 120.4(3) . . ?
C12 C11 C10 120.6(3) . . ?
C12 C11 H11 119.7 . . ?
C10 C11 H11 119.7 . . ?
C13 C12 C11 120.2(3) . . ?
C13 C12 H12 119.9 . . ?
C11 C12 H12 119.9 . . ?
C12 C13 C14 118.8(3) . . ?
C12 C13 C16 123.2(3) . . ?
C14 C13 C16 117.8(3) . . ?
C15 C14 C13 121.5(3) . . ?
C15 C14 H14 119.3 . . ?
C13 C14 H14 119.3 . . ?
C14 C15 C10 119.8(3) . . ?
C14 C15 H15 120.1 . . ?
C10 C15 H15 120.1 . . ?
O1 C16 N3 122.0(3) . . ?
O1 C16 C13 118.6(3) . . ?
N3 C16 C13 119.4(3) . . ?
O2 C17 C18 117.7(3) . . ?
O2 C17 C22 125.2(3) . . ?
C18 C17 C22 117.2(3) . . ?
C19 C18 C17 121.8(3) . . ?
C19 C18 H18 119.1 . . ?
C17 C18 H18 119.1 . . ?
C18 C19 C20 120.9(4) . . ?
C18 C19 H19 119.5 . . ?
C20 C19 H19 119.5 . . ?
C21 C20 C19 118.7(3) . . ?
C21 C20 H20 120.7 . . ?
C19 C20 H20 120.7 . . ?
C20 C21 C22 122.1(4) . . ?
C20 C21 H21 119.0 . . ?
C22 C21 H21 119.0 . . ?
C21 C22 C17 119.3(3) . . ?
C21 C22 C23 118.2(3) . . ?
C17 C22 C23 122.5(3) . . ?
N4 C23 C22 125.5(3) . . ?
N4 C23 H23 117.3 . . ?
C22 C23 H23 117.3 . . ?
N4 C24 C25 107.4(3) . . ?
N4 C24 H24A 110.2 . . ?
C25 C24 H24A 110.2 . . ?
N4 C24 H24B 110.2 . . ?
C25 C24 H24B 110.2 . . ?
H24A C24 H24B 108.5 . . ?
N5 C25 C24 102.6(3) . . ?
N5 C25 H25A 111.2 . . ?
C24 C25 H25A 111.2 . . ?
N5 C25 H25B 111.2 . . ?
C24 C25 H25B 111.2 . . ?
H25A C25 H25B 109.2 . . ?
N5 C26 C27 124.0(3) . . ?
N5 C26 H26 118.0 . . ?
C27 C26 H26 118.0 . . ?
C28 C27 C32 120.2(4) . . ?
C28 C27 C26 120.0(4) . . ?
C32 C27 C26 119.0(3) . . ?
C29 C28 C27 121.3(5) . . ?
C29 C28 H28 119.3 . . ?
C27 C28 H28 119.3 . . ?
C28 C29 C30 118.4(4) . . ?
C28 C29 H29 120.8 . . ?
C30 C29 H29 120.8 . . ?
C31 C30 C29 122.0(5) . . ?
C31 C30 H30 119.0 . . ?
C29 C30 H30 119.0 . . ?
C30 C31 C32 120.5(4) . . ?
C30 C31 H31 119.7 . . ?
C32 C31 H31 119.7 . . ?
O3 C32 C31 119.3(4) . . ?
O3 C32 C27 123.2(3) . . ?
C31 C32 C27 117.5(4) . . ?
C1 N1 C4 106.6(3) . . ?
C1 N1 Co1 127.1(2) . . ?
C4 N1 Co1 126.2(2) . . ?
C9 N2 C6 106.4(3) . . ?
C9 N2 Co1 126.7(2) . . ?
C6 N2 Co1 125.1(2) . . ?
C16 N3 H3A 120.0 . . ?
C16 N3 H3B 120.0 . . ?
H3A N3 H3B 120.0 . . ?
C23 N4 C24 119.7(3) . . ?
C23 N4 Co1 125.7(2) . . ?
C24 N4 Co1 114.6(2) . . ?
C26 N5 C25 119.4(3) . . ?
C26 N5 Co1 126.4(3) . . ?
C25 N5 Co1 110.3(2) . . ?
C17 O2 Co1 125.0(2) . . ?
C32 O3 Co1 123.5(2) . . ?
O2 Co1 N4 95.44(11) . . ?
O2 Co1 N5 175.39(11) . . ?
N4 Co1 N5 81.91(12) . . ?
O2 Co1 N1 90.06(11) . . ?
N4 Co1 N1 88.84(12) . . ?
N5 Co1 N1 93.65(12) . . ?
O2 Co1 N2 89.95(11) . . ?
N4 Co1 N2 174.22(12) . . ?
N5 Co1 N2 92.84(12) . . ?
N1 Co1 N2 89.09(12) . . ?
O2 Co1 O3 87.61(10) . . ?
N4 Co1 O3 91.27(11) . . ?
N5 Co1 O3 88.67(11) . . ?
N1 Co1 O3 177.67(11) . . ?
N2 Co1 O3 91.02(11) . . ?
C34 C33 H33A 109.5 . . ?
C34 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C34 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
O4 C34 C35 106(2) . . ?
O4 C34 C33 134.1(19) . . ?
C35 C34 C33 114.4(18) . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
O5 C36 C37 123.8(11) . . ?
O5 C36 C37 123.8(11) . 3_656 ?
C37 C36 C37 112(2) . 3_656 ?
C36 C37 H37A 109.5 . . ?
C36 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C36 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        27.55
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         1.381
_refine_diff_density_min         -0.556
_refine_diff_density_rms         0.174

#===END


