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

data_global
_journal_name_full               CrystEngComm

_journal_coden_Cambridge         1350
#=================================================

# 1. SUBMISSION DETAILS

_publ_contact_author             
# Name and address of author for correspondence
;
Professor Ming-Liang Tong
School of Chemistry and Chemical Engineering
Sun Yat-Sen University
Guangzhou 510275
PR China
;
_publ_contact_author_phone       86-20-8411-0966
_publ_contact_author_fax         81-20-8411-2245
_publ_contact_author_email       tongml@mail.sysu.edu.cn
_publ_requested_coeditor_name    ?
_publ_contact_letter             
;
Dear Sir or Madam:
Please consider this CIF as supplmentary data for a manuscript
submitted to rystEngComm.

Ming-Liang Tong
;
#=================================================================

# 2. PROCESSING SUMMARY (IUCr Office Use Only)

_journal_coden_ASTM              ?
_journal_year                    ?
_journal_volume                  ?
_journal_issue                   ?
_journal_page_first              ?
_journal_page_last               ?

#=======================================================

# 3. TITLE AND AUTHOR LIST

_publ_section_title              
;
Spontaneous Resolution of Chiral
Metal Mandelates by Stereochemical Control
;

loop_
_publ_author_name
_publ_author_address
'Ming-Liang Tong'
; School of Chemistry and Chemical Engineering
Sun Yat-Sen University
Guangzhou 510275
P. R. China
;
'Hong-Qing Hao'
; School of Chemistry and Chemical Engineering
Sun Yat-Sen University
Guangzhou 510275
P. R. China
;
'Zhuojia Lin'
; School of Chemistry and Chemical Engineering
Sun Yat-Sen University
Guangzhou 510275
P. R. China
;
'Wen-Ting Liu'
; School of Chemistry and Chemical Engineering
Sun Yat-Sen University
Guangzhou 510275
P. R. China
;
'Wei Tan'
; School of Chemistry and Chemical Engineering
Sun Yat-Sen University
Guangzhou 510275
P. R. China
;
_publ_contact_author_name        'Professor Ming-Liang Tong'

#============================================================

data_complex1R
_database_code_depnum_ccdc_archive 'CCDC 704861'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C29 H28 Cu N2 O6'
_chemical_formula_sum            'C29 H28 Cu N2 O6'
_chemical_formula_weight         564.07

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_H-M   P6(5)22
_chemical_absolute_configuration R

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z+2/3'
'-x+y, -x, z+1/3'
'-x, -y, z+1/2'
'y, -x+y, z+1/6'
'x-y, x, z+5/6'
'y, x, -z+2/3'
'x-y, -y, -z'
'-x, -x+y, -z+1/3'
'-y, -x, -z+1/6'
'-x+y, y, -z+1/2'
'x, x-y, -z+5/6'

_cell_length_a                   11.5450(1)
_cell_length_b                   11.5450(1)
_cell_length_c                   32.9386(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     3802.10(8)
_cell_formula_units_Z            6
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    1881
_cell_measurement_theta_min      4.42
_cell_measurement_theta_max      59.96

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.17
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.478
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1758
_exptl_absorpt_coefficient_mu    1.620
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6336
_exptl_absorpt_correction_T_max  0.7703
_exptl_absorpt_process_details   
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET)
(compiled Jun 10 2008,16:49:55)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'Ultra (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'Gemini S Ultra'
_diffrn_measurement_method       'ω and π scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13500
_diffrn_reflns_av_R_equivalents  0.0382
_diffrn_reflns_av_sigmaI/netI    0.0266
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_theta_min         4.42
_diffrn_reflns_theta_max         59.96
_reflns_number_total             1881
_reflns_number_gt                1642
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
(compiled Oct 18 2006,16:28:17)
;
_computing_cell_refinement       
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
(compiled Oct 18 2006,16:28:17)
;
_computing_data_reduction        
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
(compiled Oct 18 2006,16:28:17)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement of 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)+(0.0599P)²+40.6781P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.04(18)
_refine_ls_number_reflns         1881
_refine_ls_number_parameters     175
_refine_ls_number_restraints     100
_refine_ls_R_factor_all          0.1088
_refine_ls_R_factor_gt           0.0972
_refine_ls_wR_factor_ref         0.2267
_refine_ls_wR_factor_gt          0.2189
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_restrained_S_all      1.177
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.87294(10) 0.12706(10) 0.0833 0.0414(7) Uani 1 2 d S . .
O1 O 0.8133(6) -0.0800(6) 0.08238(19) 0.0343(15) Uani 1 1 d D . .
H1O H 0.823(9) -0.121(8) 0.0626(19) 0.02(3) Uiso 1 1 d D . .
O2 O 0.8469(7) 0.0827(6) 0.14201(17) 0.0355(17) Uani 1 1 d . . .
O3 O 0.8227(7) -0.0648(7) 0.18939(18) 0.0406(18) Uani 1 1 d . . .
N1 N 0.6663(10) 0.0663(12) 0.0735(3) 0.078(4) Uani 1 1 d DU . .
C1 C 0.6923(10) -0.2661(10) 0.1278(2) 0.033(2) Uani 1 1 d . . .
C2 C 0.7003(13) -0.3804(11) 0.1307(4) 0.057(3) Uani 1 1 d . . .
H2 H 0.7858 -0.3735 0.1295 0.068 Uiso 1 1 calc R . .
C3 C 0.5861(16) -0.5079(13) 0.1356(4) 0.070(4) Uani 1 1 d U . .
H3 H 0.5949 -0.5851 0.1382 0.084 Uiso 1 1 calc R . .
C4 C 0.4691(16) -0.5181(16) 0.1364(4) 0.075(5) Uani 1 1 d U . .
H4 H 0.3923 -0.6045 0.1387 0.090 Uiso 1 1 calc R . .
C5 C 0.4519(14) -0.4102(17) 0.1341(4) 0.074(4) Uani 1 1 d U . .
H5 H 0.3651 -0.4207 0.1359 0.089 Uiso 1 1 calc R . .
C6 C 0.5660(11) -0.2815(14) 0.1288(3) 0.056(4) Uani 1 1 d . . .
H6 H 0.5552 -0.2056 0.1260 0.067 Uiso 1 1 calc R . .
C7 C 0.8143(9) -0.1330(10) 0.1218(2) 0.028(2) Uani 1 1 d . . .
H7 H 0.8944 -0.1446 0.1235 0.033 Uiso 1 1 calc R . .
C8 C 0.8291(9) -0.0294(10) 0.1537(3) 0.029(2) Uani 1 1 d . . .
C9 C 0.1248(19) -0.1248(19) 0.0833 0.107(5) Uani 0.50 2 d SPDU A 1
H9 H 0.0393 -0.1689 0.0712 0.129 Uiso 0.50 1 d PR A 1
C10 C 0.248(2) -0.095(3) 0.0613(10) 0.107(5) Uani 0.50 1 d PDU A 1
H10A H 0.2420 -0.0466 0.0373 0.129 Uiso 0.50 1 calc PR A 1
H10B H 0.2240 -0.1846 0.0509 0.129 Uiso 0.50 1 calc PR A 1
C11 C 0.3958(10) -0.0328(14) 0.0656(4) 0.097(5) Uani 0.50 1 d PDU A 1
C9' C 0.210(2) -0.210(2) 0.0833 0.107(5) Uani 0.50 2 d SPD A 2
H9' H 0.2639 -0.1963 0.1049 0.129 Uiso 0.50 1 d PR A 2
C10' C 0.241(2) -0.087(3) 0.0572(9) 0.107(5) Uani 0.50 1 d PDU A 2
H10C H 0.2072 -0.0308 0.0687 0.129 Uiso 0.50 1 calc PR A 2
H10D H 0.2150 -0.1087 0.0283 0.129 Uiso 0.50 1 calc PR A 2
C11' C 0.3958(10) -0.0328(14) 0.0656(4) 0.097(5) Uani 0.50 1 d PD A 2
C12 C 0.4675(13) 0.0652(15) 0.0920(4) 0.103(6) Uani 1 1 d DU . .
H12 H 0.4239 0.1007 0.1079 0.124 Uiso 1 1 calc R A 1
C13 C 0.6029(13) 0.1161(15) 0.0966(4) 0.093(5) Uani 1 1 d DU A .
H13 H 0.6519 0.1853 0.1158 0.111 Uiso 1 1 calc R . .
C14 C 0.5949(13) -0.0333(15) 0.0472(4) 0.073(4) Uani 1 1 d DU A .
H14 H 0.6392 -0.0681 0.0313 0.087 Uiso 1 1 calc R . .
C15 C 0.4595(13) -0.0860(15) 0.0426(4) 0.088(4) Uani 1 1 d DU . .
H15 H 0.4102 -0.1572 0.0241 0.105 Uiso 1 1 calc R A 1


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 O2 1.984(6) 10_665 ?
Cu1 O2 1.984(6) . ?
Cu1 O1 2.131(7) . ?
Cu1 O1 2.131(7) 10_665 ?
Cu1 N1 2.149(10) . ?
Cu1 N1 2.149(10) 10_665 ?
O1 C7 1.437(10) . ?
O1 H1O 0.85(2) . ?
O2 C8 1.265(11) . ?
O3 C8 1.236(11) . ?
N1 C14 1.344(13) . ?
N1 C13 1.366(13) . ?
C1 C2 1.372(16) . ?
C1 C6 1.378(17) . ?
C1 C7 1.490(13) . ?
C2 C3 1.410(17) . ?
C2 H2 0.9500 . ?
C3 C4 1.30(2) . ?
C3 H3 0.9500 . ?
C4 C5 1.36(2) . ?
C4 H4 0.9500 . ?
C5 C6 1.419(19) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C8 1.536(12) . ?
C7 H7 1.0000 . ?
C9 C10 1.48(2) . ?
C9 C10 1.48(2) 10 ?
C9 H9 0.9440 . ?
C10 C11 1.49(2) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.336(12) . ?
C11 C15 1.395(12) . ?
C9' C10' 1.54(2) . ?
C9' C10' 1.54(2) 10 ?
C9' H9' 0.9030 . ?
C10' H10C 0.9900 . ?
C10' H10D 0.9900 . ?
C12 C13 1.377(13) . ?
C12 H12 0.9500 . ?
C13 H13 0.9500 . ?
C14 C15 1.373(13) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Cu1 O2 169.4(4) 10_665 . ?
O2 Cu1 O1 94.0(3) 10_665 . ?
O2 Cu1 O1 78.6(2) . . ?
O2 Cu1 O1 78.6(2) 10_665 10_665 ?
O2 Cu1 O1 94.0(3) . 10_665 ?
O1 Cu1 O1 92.5(4) . 10_665 ?
O2 Cu1 N1 93.6(3) 10_665 . ?
O2 Cu1 N1 93.6(4) . . ?
O1 Cu1 N1 87.0(4) . . ?
O1 Cu1 N1 172.2(3) 10_665 . ?
O2 Cu1 N1 93.6(4) 10_665 10_665 ?
O2 Cu1 N1 93.6(3) . 10_665 ?
O1 Cu1 N1 172.2(3) . 10_665 ?
O1 Cu1 N1 87.0(4) 10_665 10_665 ?
N1 Cu1 N1 94.5(6) . 10_665 ?
C7 O1 Cu1 113.4(5) . . ?
C7 O1 H1O 115(6) . . ?
Cu1 O1 H1O 126(6) . . ?
C8 O2 Cu1 119.1(5) . . ?
C14 N1 C13 119.5(9) . . ?
C14 N1 Cu1 118.9(7) . . ?
C13 N1 Cu1 121.3(8) . . ?
C2 C1 C6 116.7(11) . . ?
C2 C1 C7 121.2(10) . . ?
C6 C1 C7 122.0(11) . . ?
C1 C2 C3 122.3(14) . . ?
C1 C2 H2 118.8 . . ?
C3 C2 H2 118.8 . . ?
C4 C3 C2 119.0(15) . . ?
C4 C3 H3 120.5 . . ?
C2 C3 H3 120.5 . . ?
C3 C4 C5 122.6(15) . . ?
C3 C4 H4 118.7 . . ?
C5 C4 H4 118.7 . . ?
C4 C5 C6 118.9(15) . . ?
C4 C5 H5 120.6 . . ?
C6 C5 H5 120.6 . . ?
C1 C6 C5 120.4(15) . . ?
C1 C6 H6 119.8 . . ?
C5 C6 H6 119.8 . . ?
O1 C7 C1 110.7(7) . . ?
O1 C7 C8 107.9(8) . . ?
C1 C7 C8 113.1(7) . . ?
O1 C7 H7 108.3 . . ?
C1 C7 H7 108.3 . . ?
C8 C7 H7 108.3 . . ?
O3 C8 O2 125.4(8) . . ?
O3 C8 C7 115.4(9) . . ?
O2 C8 C7 119.1(8) . . ?
C10 C9 C10 102(4) . 10 ?
C10 C9 H9 123.0 . . ?
C10 C9 H9 90.6 10 . ?
C9 C10 C11 144(2) . . ?
C9 C10 H10A 101.0 . . ?
C11 C10 H10A 101.0 . . ?
C9 C10 H10B 101.0 . . ?
C11 C10 H10B 101.0 . . ?
H10A C10 H10B 104.5 . . ?
C12 C11 C15 119.2(9) . . ?
C12 C11 C10 123.0(12) . . ?
C15 C11 C10 117.7(11) . . ?
C10' C9' C10' 107(3) . 10 ?
C10' C9' H9' 117.0 . . ?
C9' C10' H10C 114.0 . . ?
C9' C10' H10D 114.0 . . ?
H10C C10' H10D 111.2 . . ?
C11 C12 C13 121.6(10) . . ?
C11 C12 H12 119.2 . . ?
C13 C12 H12 119.2 . . ?
N1 C13 C12 119.4(10) . . ?
N1 C13 H13 120.3 . . ?
C12 C13 H13 120.3 . . ?
N1 C14 C15 121.7(9) . . ?
N1 C14 H14 119.1 . . ?
C15 C14 H14 119.1 . . ?
C14 C15 C11 118.6(9) . . ?
C14 C15 H15 120.7 . . ?
C11 C15 H15 120.7 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1O O3 0.85(2) 1.78(3) 2.611(9) 166(9) 6_544

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        59.96
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         1.024
_refine_diff_density_min         -0.959
_refine_diff_density_rms         0.115

#=================================================END

data_complex1S
_database_code_depnum_ccdc_archive 'CCDC 704862'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C29 H28 Cu N2 O6'
_chemical_formula_weight         564.07

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_H-M   P6(1)22
_chemical_absolute_configuration S

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z+1/3'
'-x+y, -x, z+2/3'
'-x, -y, z+1/2'
'y, -x+y, z+5/6'
'x-y, x, z+1/6'
'y, x, -z+1/3'
'x-y, -y, -z'
'-x, -x+y, -z+2/3'
'-y, -x, -z+5/6'
'-x+y, y, -z+1/2'
'x, x-y, -z+1/6'

_cell_length_a                   11.5503(2)
_cell_length_b                   11.5503(2)
_cell_length_c                   32.9751(17)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     3809.8(2)
_cell_formula_units_Z            6
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    1637
_cell_measurement_theta_min      4.42
_cell_measurement_theta_max      59.98

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.07
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.475
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1758
_exptl_absorpt_coefficient_mu    1.617
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6976
_exptl_absorpt_correction_T_max  0.8952
_exptl_absorpt_process_details   
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET)
(compiled Jun 10 2008,16:49:55)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'Ultra (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'Gemini S Ultra'
_diffrn_measurement_method       'ω and π scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            12977
_diffrn_reflns_av_R_equivalents  0.0312
_diffrn_reflns_av_sigmaI/netI    0.0218
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_theta_min         4.42
_diffrn_reflns_theta_max         59.98
_reflns_number_total             1727
_reflns_number_gt                1547
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
(compiled Oct 18 2006,16:28:17)
;
_computing_cell_refinement       
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
(compiled Oct 18 2006,16:28:17)
;
_computing_data_reduction        
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
(compiled Oct 18 2006,16:28:17)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement of 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)+(0.0637P)²+0.1548P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.02(6)
_refine_ls_number_reflns         1727
_refine_ls_number_parameters     245
_refine_ls_number_restraints     122
_refine_ls_R_factor_all          0.0377
_refine_ls_R_factor_gt           0.0320
_refine_ls_wR_factor_ref         0.0891
_refine_ls_wR_factor_gt          0.0864
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_restrained_S_all      1.368
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.25399(7) 0.12700(3) 0.0833 0.0430(3) Uani 1 2 d SD . .
O1 O 0.1068(2) -0.0802(2) 0.08232(9) 0.0354(6) Uani 1 1 d D . .
H1O H 0.047(4) -0.111(4) 0.0642(11) 0.059(15) Uiso 1 1 d D . .
O2 O 0.2353(2) 0.0825(2) 0.14186(8) 0.0364(7) Uani 1 1 d . . .
O3 O 0.1129(3) -0.0649(3) 0.18960(10) 0.0413(7) Uani 1 1 d . . .
C1 C 0.0404(4) -0.2680(4) 0.12771(12) 0.0353(10) Uani 1 1 d D . .
C2 C -0.0835(5) -0.3813(4) 0.13080(16) 0.0553(14) Uani 1 1 d DU . .
H2 H -0.1622 -0.3748 0.1297 0.066 Uiso 1 1 calc R . .
C3 C -0.0928(7) -0.5066(4) 0.13560(17) 0.0784(19) Uani 1 1 d DU . .
H3 H -0.1785 -0.5840 0.1381 0.094 Uiso 1 1 calc R . .
C4 C 0.0137(9) -0.5193(6) 0.13668(18) 0.087(2) Uani 1 1 d DU . .
H4 H 0.0048 -0.6053 0.1395 0.104 Uiso 1 1 calc R . .
C5 C 0.1377(7) -0.4081(7) 0.13369(19) 0.090(2) Uani 1 1 d DU . .
H5 H 0.2149 -0.4171 0.1349 0.108 Uiso 1 1 calc R . .
C6 C 0.1521(5) -0.2806(5) 0.12880(16) 0.0576(14) Uani 1 1 d DU . .
H6 H 0.2385 -0.2039 0.1263 0.069 Uiso 1 1 calc R . .
C7 C 0.0526(3) -0.1320(3) 0.12142(12) 0.0273(9) Uani 1 1 d . . .
H7 H -0.0389 -0.1431 0.1230 0.033 Uiso 1 1 calc R . .
C8 C 0.1412(3) -0.0299(3) 0.15392(14) 0.0296(10) Uani 1 1 d . . .
N1 N 0.3972(7) 0.0367(9) 0.0711(4) 0.032(3) Uani 0.50 1 d PDU . 1
C9 C 0.3660(9) -0.0670(10) 0.0454(3) 0.035(3) Uani 0.50 1 d PDU . 1
H9 H 0.2837 -0.1038 0.0311 0.042 Uiso 0.50 1 calc PR . 1
C10 C 0.4449(9) -0.1210(9) 0.0388(3) 0.041(2) Uani 0.50 1 d PD . 1
H10 H 0.4171 -0.1939 0.0206 0.049 Uiso 0.50 1 calc PR . 1
C11 C 0.5665(7) -0.0697(8) 0.0589(3) 0.0278(19) Uani 0.50 1 d PDU . 1
C12 C 0.5996(11) 0.0309(13) 0.0862(4) 0.033(3) Uani 0.50 1 d PDU . 1
H12 H 0.6799 0.0652 0.1015 0.040 Uiso 0.50 1 calc PR . 1
C13 C 0.5158(10) 0.0820(9) 0.0915(3) 0.038(2) Uani 0.50 1 d PD . 1
H13 H 0.5413 0.1528 0.1104 0.046 Uiso 0.50 1 calc PR . 1
C14 C 0.6589(7) -0.1258(8) 0.0487(3) 0.035(2) Uani 0.50 1 d P . 1
H14A H 0.6033 -0.2180 0.0383 0.041 Uiso 0.50 1 calc PR . 1
H14B H 0.7197 -0.0714 0.0266 0.041 Uiso 0.50 1 calc PR . 1
C15 C 0.7421(9) -0.1289(5) 0.0833 0.038(3) Uani 0.50 2 d SP . 1
H15 H 0.8040 -0.0388 0.0942 0.045 Uiso 0.50 1 d PR . 1
N1' N 0.4049(8) 0.0987(7) 0.0761(3) 0.034(2) Uani 0.50 1 d PD . 2
C9' C 0.3809(9) 0.0000(12) 0.0498(4) 0.028(3) Uani 0.50 1 d PDU . 2
H9' H 0.3032 -0.0368 0.0332 0.034 Uiso 0.50 1 calc PR . 2
C10' C 0.4688(10) -0.0479(9) 0.0468(3) 0.039(2) Uani 0.50 1 d PD . 2
H10' H 0.4537 -0.1150 0.0275 0.047 Uiso 0.50 1 calc PR . 2
C11' C 0.5796(11) 0.0028(13) 0.0723(4) 0.032(3) Uani 0.50 1 d PDU . 2
C12' C 0.5991(9) 0.1017(9) 0.0995(3) 0.039(2) Uani 0.50 1 d PD . 2
H12' H 0.6745 0.1391 0.1170 0.047 Uiso 0.50 1 calc PR . 2
C13' C 0.5076(8) 0.1461(8) 0.1009(3) 0.038(2) Uani 0.50 1 d PD . 2
H13' H 0.5194 0.2121 0.1203 0.045 Uiso 0.50 1 calc PR . 2
C14' C 0.6665(8) -0.0608(8) 0.0727(3) 0.043(2) Uani 0.50 1 d P . 2
H14C H 0.7392 -0.0147 0.0927 0.051 Uiso 0.50 1 calc PR . 2
H14D H 0.7077 -0.0508 0.0456 0.051 Uiso 0.50 1 calc PR . 2
C15' C 0.5843(11) -0.2078(5) 0.0833 0.041(3) Uani 0.50 2 d SP . 2
H15' H 0.5258 -0.2558 0.0600 0.049 Uiso 0.50 1 d PR . 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
Cu1 N1' 1.942(7) . ?
Cu1 N1' 1.942(7) 12 ?
Cu1 O2 1.981(3) 12 ?
Cu1 O2 1.981(3) . ?
Cu1 O1 2.133(3) . ?
Cu1 O1 2.133(3) 12 ?
Cu1 N1 2.390(8) . ?
Cu1 N1 2.390(8) 12 ?
O1 C7 1.428(5) . ?
O1 H1O 0.849(13) . ?
O2 C8 1.270(5) . ?
O3 C8 1.234(5) . ?
C1 C6 1.368(6) . ?
C1 C2 1.378(6) . ?
C1 C7 1.520(5) . ?
C2 C3 1.405(6) . ?
C2 H2 0.9500 . ?
C3 C4 1.310(8) . ?
C3 H3 0.9500 . ?
C4 C5 1.368(9) . ?
C4 H4 0.9500 . ?
C5 C6 1.407(7) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C8 1.543(5) . ?
C7 H7 1.0000 . ?
N1 C9 1.361(11) . ?
N1 C13 1.373(13) . ?
C9 C10 1.355(14) . ?
C9 H9 0.9500 . ?
C10 C11 1.389(12) . ?
C10 H10 0.9500 . ?
C11 C12 1.365(15) . ?
C11 C14 1.537(11) . ?
C12 C13 1.374(16) . ?
C12 H12 0.9500 . ?
C13 H13 0.9500 . ?
C14 C15 1.504(10) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C14 1.504(10) 12_545 ?
C15 H15 0.9893 . ?
N1' C13' 1.314(12) . ?
N1' C9' 1.347(13) . ?
C9' C10' 1.381(13) . ?
C9' H9' 0.9500 . ?
C10' C11' 1.393(16) . ?
C10' H10' 0.9500 . ?
C11' C12' 1.378(15) . ?
C11' C14' 1.511(14) . ?
C12' C13' 1.387(13) . ?
C12' H12' 0.9500 . ?
C13' H13' 0.9500 . ?
C14' C15' 1.516(10) . ?
C14' H14C 0.9900 . ?
C14' H14D 0.9900 . ?
C15' C14' 1.516(10) 12_545 ?
C15' H15' 0.9898 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1' Cu1 N1' 77.9(4) . 12 ?
N1' Cu1 O2 94.6(3) . 12 ?
N1' Cu1 O2 93.8(3) 12 12 ?
N1' Cu1 O2 93.8(3) . . ?
N1' Cu1 O2 94.6(3) 12 . ?
O2 Cu1 O2 169.17(14) 12 . ?
N1' Cu1 O1 95.1(2) . . ?
N1' Cu1 O1 170.0(3) 12 . ?
O2 Cu1 O1 93.89(11) 12 . ?
O2 Cu1 O1 78.58(11) . . ?
N1' Cu1 O1 170.0(3) . 12 ?
N1' Cu1 O1 95.1(2) 12 12 ?
O2 Cu1 O1 78.58(11) 12 12 ?
O2 Cu1 O1 93.89(11) . 12 ?
O1 Cu1 O1 92.71(13) . 12 ?
N1' Cu1 N1 14.2(2) . . ?
N1' Cu1 N1 92.1(3) 12 . ?
O2 Cu1 N1 93.0(3) 12 . ?
O2 Cu1 N1 93.5(3) . . ?
O1 Cu1 N1 81.1(2) . . ?
O1 Cu1 N1 169.2(3) 12 . ?
N1' Cu1 N1 92.1(3) . 12 ?
N1' Cu1 N1 14.2(2) 12 12 ?
O2 Cu1 N1 93.5(3) 12 12 ?
O2 Cu1 N1 93.0(3) . 12 ?
O1 Cu1 N1 169.2(3) . 12 ?
O1 Cu1 N1 81.1(2) 12 12 ?
N1 Cu1 N1 106.3(4) . 12 ?
C7 O1 Cu1 113.1(2) . . ?
C7 O1 H1O 111(3) . . ?
Cu1 O1 H1O 120(3) . . ?
C8 O2 Cu1 119.8(3) . . ?
C6 C1 C2 119.0(4) . . ?
C6 C1 C7 120.5(4) . . ?
C2 C1 C7 120.4(3) . . ?
C1 C2 C3 119.6(4) . . ?
C1 C2 H2 120.2 . . ?
C3 C2 H2 120.2 . . ?
C4 C3 C2 121.8(5) . . ?
C4 C3 H3 119.1 . . ?
C2 C3 H3 119.1 . . ?
C3 C4 C5 119.5(5) . . ?
C3 C4 H4 120.2 . . ?
C5 C4 H4 120.2 . . ?
C4 C5 C6 120.8(5) . . ?
C4 C5 H5 119.6 . . ?
C6 C5 H5 119.6 . . ?
C1 C6 C5 119.3(5) . . ?
C1 C6 H6 120.4 . . ?
C5 C6 H6 120.4 . . ?
O1 C7 C1 110.5(3) . . ?
O1 C7 C8 108.8(3) . . ?
C1 C7 C8 112.2(3) . . ?
O1 C7 H7 108.4 . . ?
C1 C7 H7 108.4 . . ?
C8 C7 H7 108.4 . . ?
O3 C8 O2 125.7(4) . . ?
O3 C8 C7 116.5(3) . . ?
O2 C8 C7 117.8(4) . . ?
C9 N1 C13 114.5(8) . . ?
C9 N1 Cu1 123.5(7) . . ?
C13 N1 Cu1 121.8(6) . . ?
C10 C9 N1 124.2(8) . . ?
C10 C9 H9 117.9 . . ?
N1 C9 H9 117.9 . . ?
C9 C10 C11 119.8(7) . . ?
C9 C10 H10 120.1 . . ?
C11 C10 H10 120.1 . . ?
C12 C11 C10 118.1(8) . . ?
C12 C11 C14 123.0(8) . . ?
C10 C11 C14 118.9(8) . . ?
C11 C12 C13 119.4(8) . . ?
C11 C12 H12 120.3 . . ?
C13 C12 H12 120.3 . . ?
N1 C13 C12 123.9(8) . . ?
N1 C13 H13 118.1 . . ?
C12 C13 H13 118.1 . . ?
C15 C14 C11 115.5(7) . . ?
C15 C14 H14A 108.4 . . ?
C11 C14 H14A 108.4 . . ?
C15 C14 H14B 108.4 . . ?
C11 C14 H14B 108.4 . . ?
H14A C14 H14B 107.5 . . ?
C14 C15 C14 112.8(8) . 12_545 ?
C14 C15 H15 112.6 . . ?
C14 C15 H15 108.0 12_545 . ?
C13' N1' C9' 120.9(7) . . ?
C13' N1' Cu1 123.6(7) . . ?
C9' N1' Cu1 113.5(6) . . ?
N1' C9' C10' 120.2(8) . . ?
N1' C9' H9' 119.9 . . ?
C10' C9' H9' 119.9 . . ?
C9' C10' C11' 119.6(8) . . ?
C9' C10' H10' 120.2 . . ?
C11' C10' H10' 120.2 . . ?
C12' C11' C10' 118.4(8) . . ?
C12' C11' C14' 121.7(11) . . ?
C10' C11' C14' 119.6(10) . . ?
C11' C12' C13' 119.3(8) . . ?
C11' C12' H12' 120.3 . . ?
C13' C12' H12' 120.3 . . ?
N1' C13' C12' 121.4(8) . . ?
N1' C13' H13' 119.3 . . ?
C12' C13' H13' 119.3 . . ?
C11' C14' C15' 110.5(8) . . ?
C11' C14' H14C 109.5 . . ?
C15' C14' H14C 109.5 . . ?
C11' C14' H14D 109.5 . . ?
C15' C14' H14D 109.5 . . ?
H14C C14' H14D 108.1 . . ?
C14' C15' C14' 114.4(10) 12_545 . ?
C14' C15' H15' 109.0 12_545 . ?
C14' C15' H15' 108.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1' Cu1 O1 C7 105.7(4) . . . . ?
N1' Cu1 O1 C7 60.5(17) 12 . . . ?
O2 Cu1 O1 C7 -159.3(2) 12 . . . ?
O2 Cu1 O1 C7 12.8(2) . . . . ?
O1 Cu1 O1 C7 -80.6(2) 12 . . . ?
N1 Cu1 O1 C7 108.3(4) . . . . ?
N1 Cu1 O1 C7 -26.2(15) 12 . . . ?
N1' Cu1 O2 C8 -104.4(3) . . . . ?
N1' Cu1 O2 C8 177.4(3) 12 . . . ?
O2 Cu1 O2 C8 36.6(2) 12 . . . ?
O1 Cu1 O2 C8 -9.9(2) . . . . ?
O1 Cu1 O2 C8 82.0(2) 12 . . . ?
N1 Cu1 O2 C8 -90.1(3) . . . . ?
N1 Cu1 O2 C8 163.3(3) 12 . . . ?
C6 C1 C2 C3 1.0(7) . . . . ?
C7 C1 C2 C3 178.4(4) . . . . ?
C1 C2 C3 C4 -1.0(9) . . . . ?
C2 C3 C4 C5 1.0(10) . . . . ?
C3 C4 C5 C6 -1.1(10) . . . . ?
C2 C1 C6 C5 -1.0(7) . . . . ?
C7 C1 C6 C5 -178.5(5) . . . . ?
C4 C5 C6 C1 1.1(9) . . . . ?
Cu1 O1 C7 C1 -137.0(2) . . . . ?
Cu1 O1 C7 C8 -13.3(3) . . . . ?
C6 C1 C7 O1 64.3(5) . . . . ?
C2 C1 C7 O1 -113.1(4) . . . . ?
C6 C1 C7 C8 -57.4(5) . . . . ?
C2 C1 C7 C8 125.2(4) . . . . ?
Cu1 O2 C8 O3 -173.9(3) . . . . ?
Cu1 O2 C8 C7 5.2(4) . . . . ?
O1 C7 C8 O3 -174.7(3) . . . . ?
C1 C7 C8 O3 -52.0(4) . . . . ?
O1 C7 C8 O2 6.1(4) . . . . ?
C1 C7 C8 O2 128.7(3) . . . . ?
N1' Cu1 N1 C9 -150(3) . . . . ?
N1' Cu1 N1 C9 -146.6(8) 12 . . . ?
O2 Cu1 N1 C9 -52.7(9) 12 . . . ?
O2 Cu1 N1 C9 118.7(9) . . . . ?
O1 Cu1 N1 C9 40.8(9) . . . . ?
O1 Cu1 N1 C9 -14(2) 12 . . . ?
N1 Cu1 N1 C9 -147.2(11) 12 . . . ?
N1' Cu1 N1 C13 34.0(16) . . . . ?
N1' Cu1 N1 C13 37.0(11) 12 . . . ?
O2 Cu1 N1 C13 130.9(9) 12 . . . ?
O2 Cu1 N1 C13 -57.8(9) . . . . ?
O1 Cu1 N1 C13 -135.6(9) . . . . ?
O1 Cu1 N1 C13 169.1(9) 12 . . . ?
N1 Cu1 N1 C13 36.4(7) 12 . . . ?
C13 N1 C9 C10 -1.8(16) . . . . ?
Cu1 N1 C9 C10 -178.5(8) . . . . ?
N1 C9 C10 C11 -0.4(16) . . . . ?
C9 C10 C11 C12 2.9(14) . . . . ?
C9 C10 C11 C14 -175.6(8) . . . . ?
C10 C11 C12 C13 -3.1(16) . . . . ?
C14 C11 C12 C13 175.3(9) . . . . ?
C9 N1 C13 C12 1.6(16) . . . . ?
Cu1 N1 C13 C12 178.3(9) . . . . ?
C11 C12 C13 N1 0.9(17) . . . . ?
C12 C11 C14 C15 34.2(12) . . . . ?
C10 C11 C14 C15 -147.3(7) . . . . ?
C11 C14 C15 C14 61.2(5) . . . 12_545 ?
N1' Cu1 N1' C13' 47.8(6) 12 . . . ?
O2 Cu1 N1' C13' 140.8(8) 12 . . . ?
O2 Cu1 N1' C13' -46.1(8) . . . . ?
O1 Cu1 N1' C13' -124.9(8) . . . . ?
O1 Cu1 N1' C13' 94(2) 12 . . . ?
N1 Cu1 N1' C13' -135(3) . . . . ?
N1 Cu1 N1' C13' 47.1(9) 12 . . . ?
N1' Cu1 N1' C9' -147.9(9) 12 . . . ?
O2 Cu1 N1' C9' -55.0(7) 12 . . . ?
O2 Cu1 N1' C9' 118.2(7) . . . . ?
O1 Cu1 N1' C9' 39.3(7) . . . . ?
O1 Cu1 N1' C9' -101.6(18) 12 . . . ?
N1 Cu1 N1' C9' 29(2) . . . . ?
N1 Cu1 N1' C9' -148.7(8) 12 . . . ?
C13' N1' C9' C10' -3.8(16) . . . . ?
Cu1 N1' C9' C10' -168.5(9) . . . . ?
N1' C9' C10' C11' 2.5(17) . . . . ?
C9' C10' C11' C12' -1.1(16) . . . . ?
C9' C10' C11' C14' 172.6(10) . . . . ?
C10' C11' C12' C13' 0.9(15) . . . . ?
C14' C11' C12' C13' -172.7(9) . . . . ?
C9' N1' C13' C12' 3.6(15) . . . . ?
Cu1 N1' C13' C12' 166.8(7) . . . . ?
C11' C12' C13' N1' -2.1(14) . . . . ?
C12' C11' C14' C15' 115.7(11) . . . . ?
C10' C11' C14' C15' -57.9(13) . . . . ?
C11' C14' C15' C14' -166.5(10) . . . 12_545 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1O O3 0.849(13) 1.763(15) 2.608(4) 173(5) 5_554

_diffrn_measured_fraction_theta_max 0.904
_diffrn_reflns_theta_full        59.98
_diffrn_measured_fraction_theta_full 0.904
_refine_diff_density_max         0.140
_refine_diff_density_min         -0.435
_refine_diff_density_rms         0.054

#=================================================END

data_complex3
_database_code_depnum_ccdc_archive 'CCDC 704863'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C29 H28 Cu N2 O6'
_chemical_formula_weight         564.07

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   Pna2(1)

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

_cell_length_a                   11.1531(4)
_cell_length_b                   9.9944(3)
_cell_length_c                   24.0449(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2680.25(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    2750
_cell_measurement_theta_min      6.22
_cell_measurement_theta_max      62.38

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.17
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.398
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1172
_exptl_absorpt_coefficient_mu    1.532
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6650
_exptl_absorpt_correction_T_max  0.7807
_exptl_absorpt_process_details   
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET)
(compiled Jun 10 2008,16:49:55)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'Ultra (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'Gemini S Ultra'
_diffrn_measurement_method       'ω and π scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            4556
_diffrn_reflns_av_R_equivalents  0.0433
_diffrn_reflns_av_sigmaI/netI    0.0649
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         6.22
_diffrn_reflns_theta_max         62.38
_reflns_number_total             2750
_reflns_number_gt                2054
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
(compiled Oct 18 2006,16:28:17)
;
_computing_cell_refinement       
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
(compiled Oct 18 2006,16:28:17)
;
_computing_data_reduction        
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
(compiled Oct 18 2006,16:28:17)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement of 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)+(0.0828P)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    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.18(7)
_refine_ls_number_reflns         2750
_refine_ls_number_parameters     343
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0738
_refine_ls_R_factor_gt           0.0537
_refine_ls_wR_factor_ref         0.1369
_refine_ls_wR_factor_gt          0.1290
_refine_ls_goodness_of_fit_ref   0.991
_refine_ls_restrained_S_all      0.990
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu -0.68284(8) -0.50085(10) -0.21244(6) 0.0285(3) Uani 1 1 d . . .
O1 O -0.5449(4) -0.6466(4) -0.1736(2) 0.0305(11) Uani 1 1 d D . .
H1O H -0.5464 -0.7219 -0.1900 0.037 Uiso 1 1 d RD . .
O2 O -0.5384(4) -0.3916(4) -0.2066(2) 0.0284(10) Uani 1 1 d . . .
O3 O -0.3386(4) -0.3843(4) -0.2013(2) 0.0378(14) Uani 1 1 d . . .
O4 O -0.8215(4) -0.3523(4) -0.2485(2) 0.0321(11) Uani 1 1 d D . .
H4O H -0.8174 -0.2781 -0.2314 0.038 Uiso 1 1 d RD . .
O5 O -0.8289(4) -0.6106(4) -0.2177(3) 0.0321(11) Uani 1 1 d . . .
O6 O -1.0270(4) -0.6102(4) -0.2133(3) 0.0368(11) Uani 1 1 d . . .
N1 N -0.7341(6) -0.4447(5) -0.1348(3) 0.0316(14) Uani 1 1 d . . .
N2 N -0.8696(6) -0.0614(6) 0.2109(3) 0.0332(15) Uani 1 1 d . . .
C1 C -0.3658(7) -0.5959(6) -0.1197(3) 0.0335(18) Uani 1 1 d . . .
C2 C -0.4322(7) -0.6156(8) -0.0709(3) 0.039(2) Uani 1 1 d . . .
H2 H -0.5169 -0.6248 -0.0729 0.047 Uiso 1 1 calc R . .
C3 C -0.3757(9) -0.6217(9) -0.0205(4) 0.057(2) Uani 1 1 d . . .
H3 H -0.4218 -0.6332 0.0124 0.068 Uiso 1 1 calc R . .
C4 C -0.2502(10) -0.6111(9) -0.0168(4) 0.061(3) Uani 1 1 d . . .
H4 H -0.2112 -0.6145 0.0183 0.074 Uiso 1 1 calc R . .
C5 C -0.1849(8) -0.5955(9) -0.0649(5) 0.055(3) Uani 1 1 d . . .
H5 H -0.1000 -0.5897 -0.0631 0.066 Uiso 1 1 calc R . .
C6 C -0.2417(7) -0.5884(7) -0.1155(4) 0.043(2) Uani 1 1 d . . .
H6 H -0.1951 -0.5782 -0.1483 0.051 Uiso 1 1 calc R . .
C7 C -0.4277(6) -0.5901(7) -0.1757(3) 0.0310(17) Uani 1 1 d . . .
H7 H -0.3789 -0.6420 -0.2031 0.037 Uiso 1 1 calc R . .
C8 C -0.4358(6) -0.4432(7) -0.1958(3) 0.0279(17) Uani 1 1 d . . .
C9 C -1.0077(6) -0.3953(6) -0.2963(3) 0.0292(16) Uani 1 1 d . . .
C10 C -1.1327(6) -0.4057(6) -0.2955(3) 0.0329(17) Uani 1 1 d . . .
H10 H -1.1726 -0.4229 -0.2613 0.039 Uiso 1 1 calc R . .
C11 C -1.1979(8) -0.3917(8) -0.3428(4) 0.043(2) Uani 1 1 d . . .
H11 H -1.2829 -0.3982 -0.3416 0.051 Uiso 1 1 calc R . .
C12 C -1.1410(9) -0.3682(8) -0.3921(4) 0.052(2) Uani 1 1 d . . .
H12 H -1.1870 -0.3564 -0.4250 0.062 Uiso 1 1 calc R . .
C13 C -1.0191(7) -0.3612(8) -0.3948(3) 0.042(2) Uani 1 1 d . . .
H13 H -0.9802 -0.3473 -0.4295 0.050 Uiso 1 1 calc R . .
C14 C -0.9524(7) -0.3748(7) -0.3465(4) 0.0378(18) Uani 1 1 d . . .
H14 H -0.8675 -0.3698 -0.3482 0.045 Uiso 1 1 calc R . .
C15 C -0.9377(6) -0.4068(6) -0.2430(3) 0.0276(16) Uani 1 1 d . . .
H15 H -0.9809 -0.3542 -0.2139 0.033 Uiso 1 1 calc R . .
C16 C -0.9305(6) -0.5581(6) -0.2225(3) 0.0311(18) Uani 1 1 d . . .
C17 C -0.7303(7) -0.3160(7) -0.1181(3) 0.0347(18) Uani 1 1 d . . .
H17 H -0.6920 -0.2522 -0.1415 0.042 Uiso 1 1 calc R . .
C18 C -0.7796(7) -0.2731(7) -0.0690(3) 0.0402(19) Uani 1 1 d . . .
H18 H -0.7761 -0.1809 -0.0596 0.048 Uiso 1 1 calc R . .
C19 C -0.8344(7) -0.3623(7) -0.0326(3) 0.0353(18) Uani 1 1 d . . .
C20 C -0.8330(7) -0.4975(8) -0.0493(4) 0.0429(19) Uani 1 1 d . . .
H20 H -0.8659 -0.5644 -0.0257 0.052 Uiso 1 1 calc R . .
C21 C -0.7847(7) -0.5318(8) -0.0989(3) 0.0377(19) Uani 1 1 d . . .
H21 H -0.7865 -0.6236 -0.1092 0.045 Uiso 1 1 calc R . .
C22 C -0.8919(8) -0.3203(9) 0.0208(4) 0.050(2) Uani 1 1 d . . .
H22A H -0.9202 -0.4013 0.0405 0.060 Uiso 1 1 calc R . .
H22B H -0.8303 -0.2773 0.0444 0.060 Uiso 1 1 calc R . .
C23 C -0.9941(9) -0.2269(10) 0.0146(4) 0.055(2) Uani 1 1 d . . .
H23A H -1.0487 -0.2616 -0.0145 0.066 Uiso 1 1 calc R . .
H23B H -0.9635 -0.1391 0.0019 0.066 Uiso 1 1 calc R . .
C24 C -1.0650(8) -0.2069(11) 0.0681(4) 0.056(2) Uani 1 1 d . . .
H24A H -1.1307 -0.1427 0.0606 0.068 Uiso 1 1 calc R . .
H24B H -1.1022 -0.2933 0.0785 0.068 Uiso 1 1 calc R . .
C25 C -0.9928(7) -0.1560(8) 0.1174(3) 0.0404(19) Uani 1 1 d . . .
C26 C -0.9806(7) -0.0199(8) 0.1281(3) 0.041(2) Uani 1 1 d . . .
H26 H -1.0128 0.0431 0.1026 0.049 Uiso 1 1 calc R . .
C27 C -0.9231(7) 0.0244(7) 0.1747(3) 0.0345(17) Uani 1 1 d . . .
H27 H -0.9204 0.1178 0.1820 0.041 Uiso 1 1 calc R . .
C28 C -0.8756(7) -0.1933(7) 0.1986(3) 0.0352(18) Uani 1 1 d . . .
H28 H -0.8364 -0.2548 0.2227 0.042 Uiso 1 1 calc R . .
C29 C -0.9351(7) -0.2424(8) 0.1534(3) 0.0424(19) Uani 1 1 d . . .
H29 H -0.9368 -0.3361 0.1467 0.051 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 O2 1.951(4) . ?
Cu1 O5 1.968(4) . ?
Cu1 N2 2.027(6) 3_344 ?
Cu1 N1 2.033(6) . ?
Cu1 O4 2.312(5) . ?
Cu1 O1 2.315(5) . ?
O1 C7 1.425(8) . ?
O1 H1O 0.8500 . ?
O2 C8 1.281(8) . ?
O3 C8 1.241(8) . ?
O4 C15 1.411(8) . ?
O4 H4O 0.8500 . ?
O5 C16 1.254(8) . ?
O6 C16 1.215(8) . ?
N1 C17 1.348(10) . ?
N1 C21 1.348(10) . ?
N2 C28 1.353(9) . ?
N2 C27 1.360(9) . ?
N2 Cu1 2.027(6) 3_355 ?
C1 C6 1.390(11) . ?
C1 C2 1.401(11) . ?
C1 C7 1.513(11) . ?
C2 C3 1.367(12) . ?
C2 H2 0.9500 . ?
C3 C4 1.407(14) . ?
C3 H3 0.9500 . ?
C4 C5 1.375(14) . ?
C4 H4 0.9500 . ?
C5 C6 1.374(13) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C8 1.549(10) . ?
C7 H7 1.0000 . ?
C9 C14 1.371(11) . ?
C9 C10 1.398(10) . ?
C9 C15 1.505(10) . ?
C10 C11 1.358(12) . ?
C10 H10 0.9500 . ?
C11 C12 1.365(14) . ?
C11 H11 0.9500 . ?
C12 C13 1.363(13) . ?
C12 H12 0.9500 . ?
C13 C14 1.386(11) . ?
C13 H13 0.9500 . ?
C14 H14 0.9500 . ?
C15 C16 1.593(9) . ?
C15 H15 1.0000 . ?
C17 C18 1.372(11) . ?
C17 H17 0.9500 . ?
C18 C19 1.390(11) . ?
C18 H18 0.9500 . ?
C19 C20 1.410(11) . ?
C19 C22 1.496(12) . ?
C20 C21 1.354(12) . ?
C20 H20 0.9500 . ?
C21 H21 0.9500 . ?
C22 C23 1.480(12) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 C24 1.522(13) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 C25 1.521(12) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 C29 1.381(11) . ?
C25 C26 1.391(11) . ?
C26 C27 1.364(11) . ?
C26 H26 0.9500 . ?
C27 H27 0.9500 . ?
C28 C29 1.365(11) . ?
C28 H28 0.9500 . ?
C29 H29 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Cu1 O5 179.5(3) . . ?
O2 Cu1 N2 89.7(2) . 3_344 ?
O5 Cu1 N2 90.8(3) . 3_344 ?
O2 Cu1 N1 90.7(2) . . ?
O5 Cu1 N1 88.9(3) . . ?
N2 Cu1 N1 178.6(3) 3_344 . ?
O2 Cu1 O4 102.71(17) . . ?
O5 Cu1 O4 77.29(17) . . ?
N2 Cu1 O4 92.5(2) 3_344 . ?
N1 Cu1 O4 88.8(2) . . ?
O2 Cu1 O1 76.96(17) . . ?
O5 Cu1 O1 103.03(17) . . ?
N2 Cu1 O1 89.3(2) 3_344 . ?
N1 Cu1 O1 89.4(2) . . ?
O4 Cu1 O1 178.2(2) . . ?
C7 O1 Cu1 110.3(4) . . ?
C7 O1 H1O 110.6 . . ?
Cu1 O1 H1O 110.9 . . ?
C8 O2 Cu1 121.8(4) . . ?
C15 O4 Cu1 109.4(4) . . ?
C15 O4 H4O 109.9 . . ?
Cu1 O4 H4O 110.1 . . ?
C16 O5 Cu1 121.4(4) . . ?
C17 N1 C21 116.1(7) . . ?
C17 N1 Cu1 121.8(5) . . ?
C21 N1 Cu1 121.8(5) . . ?
C28 N2 C27 117.0(7) . . ?
C28 N2 Cu1 120.2(5) . 3_355 ?
C27 N2 Cu1 121.4(5) . 3_355 ?
C6 C1 C2 118.2(8) . . ?
C6 C1 C7 121.1(7) . . ?
C2 C1 C7 120.6(7) . . ?
C3 C2 C1 120.3(8) . . ?
C3 C2 H2 119.8 . . ?
C1 C2 H2 119.8 . . ?
C2 C3 C4 120.7(9) . . ?
C2 C3 H3 119.6 . . ?
C4 C3 H3 119.6 . . ?
C5 C4 C3 118.8(9) . . ?
C5 C4 H4 120.6 . . ?
C3 C4 H4 120.6 . . ?
C6 C5 C4 120.5(9) . . ?
C6 C5 H5 119.8 . . ?
C4 C5 H5 119.8 . . ?
C5 C6 C1 121.4(9) . . ?
C5 C6 H6 119.3 . . ?
C1 C6 H6 119.3 . . ?
O1 C7 C1 111.9(6) . . ?
O1 C7 C8 109.4(5) . . ?
C1 C7 C8 109.9(5) . . ?
O1 C7 H7 108.5 . . ?
C1 C7 H7 108.5 . . ?
C8 C7 H7 108.5 . . ?
O3 C8 O2 124.6(6) . . ?
O3 C8 C7 115.6(6) . . ?
O2 C8 C7 119.8(5) . . ?
C14 C9 C10 118.2(7) . . ?
C14 C9 C15 121.8(7) . . ?
C10 C9 C15 120.0(7) . . ?
C11 C10 C9 121.0(8) . . ?
C11 C10 H10 119.5 . . ?
C9 C10 H10 119.5 . . ?
C10 C11 C12 119.8(8) . . ?
C10 C11 H11 120.1 . . ?
C12 C11 H11 120.1 . . ?
C13 C12 C11 120.9(8) . . ?
C13 C12 H12 119.5 . . ?
C11 C12 H12 119.5 . . ?
C12 C13 C14 119.4(8) . . ?
C12 C13 H13 120.3 . . ?
C14 C13 H13 120.3 . . ?
C9 C14 C13 120.7(7) . . ?
C9 C14 H14 119.6 . . ?
C13 C14 H14 119.6 . . ?
O4 C15 C9 111.6(6) . . ?
O4 C15 C16 110.4(5) . . ?
C9 C15 C16 111.2(5) . . ?
O4 C15 H15 107.8 . . ?
C9 C15 H15 107.8 . . ?
C16 C15 H15 107.8 . . ?
O6 C16 O5 127.2(6) . . ?
O6 C16 C15 114.7(6) . . ?
O5 C16 C15 118.1(6) . . ?
N1 C17 C18 122.7(7) . . ?
N1 C17 H17 118.6 . . ?
C18 C17 H17 118.6 . . ?
C17 C18 C19 121.2(7) . . ?
C17 C18 H18 119.4 . . ?
C19 C18 H18 119.4 . . ?
C18 C19 C20 115.5(7) . . ?
C18 C19 C22 123.3(7) . . ?
C20 C19 C22 121.2(7) . . ?
C21 C20 C19 119.8(7) . . ?
C21 C20 H20 120.1 . . ?
C19 C20 H20 120.1 . . ?
N1 C21 C20 124.5(7) . . ?
N1 C21 H21 117.8 . . ?
C20 C21 H21 117.8 . . ?
C23 C22 C19 114.9(7) . . ?
C23 C22 H22A 108.5 . . ?
C19 C22 H22A 108.5 . . ?
C23 C22 H22B 108.5 . . ?
C19 C22 H22B 108.5 . . ?
H22A C22 H22B 107.5 . . ?
C22 C23 C24 113.5(8) . . ?
C22 C23 H23A 108.9 . . ?
C24 C23 H23A 108.9 . . ?
C22 C23 H23B 108.9 . . ?
C24 C23 H23B 108.9 . . ?
H23A C23 H23B 107.7 . . ?
C25 C24 C23 115.3(8) . . ?
C25 C24 H24A 108.5 . . ?
C23 C24 H24A 108.5 . . ?
C25 C24 H24B 108.5 . . ?
C23 C24 H24B 108.5 . . ?
H24A C24 H24B 107.5 . . ?
C29 C25 C26 116.7(8) . . ?
C29 C25 C24 121.7(7) . . ?
C26 C25 C24 121.5(8) . . ?
C27 C26 C25 121.1(7) . . ?
C27 C26 H26 119.5 . . ?
C25 C26 H26 119.5 . . ?
N2 C27 C26 121.8(7) . . ?
N2 C27 H27 119.1 . . ?
C26 C27 H27 119.1 . . ?
N2 C28 C29 123.2(7) . . ?
N2 C28 H28 118.4 . . ?
C29 C28 H28 118.4 . . ?
C28 C29 C25 120.0(7) . . ?
C28 C29 H29 120.0 . . ?
C25 C29 H29 120.0 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2 Cu1 O1 C7 -10.5(5) . . . . ?
O5 Cu1 O1 C7 170.0(5) . . . . ?
N2 Cu1 O1 C7 79.3(5) 3_344 . . . ?
N1 Cu1 O1 C7 -101.3(5) . . . . ?
O4 Cu1 O1 C7 -90(6) . . . . ?
O5 Cu1 O2 C8 102(33) . . . . ?
N2 Cu1 O2 C8 -77.1(6) 3_344 . . . ?
N1 Cu1 O2 C8 101.5(6) . . . . ?
O4 Cu1 O2 C8 -169.6(5) . . . . ?
O1 Cu1 O2 C8 12.3(5) . . . . ?
O2 Cu1 O4 C15 -166.3(4) . . . . ?
O5 Cu1 O4 C15 13.2(5) . . . . ?
N2 Cu1 O4 C15 103.5(5) 3_344 . . . ?
N1 Cu1 O4 C15 -75.9(5) . . . . ?
O1 Cu1 O4 C15 -87(6) . . . . ?
O2 Cu1 O5 C16 71(33) . . . . ?
N2 Cu1 O5 C16 -110.2(6) 3_344 . . . ?
N1 Cu1 O5 C16 71.2(6) . . . . ?
O4 Cu1 O5 C16 -17.8(6) . . . . ?
O1 Cu1 O5 C16 160.3(6) . . . . ?
O2 Cu1 N1 C17 46.2(6) . . . . ?
O5 Cu1 N1 C17 -133.8(6) . . . . ?
N2 Cu1 N1 C17 150(11) 3_344 . . . ?
O4 Cu1 N1 C17 -56.5(6) . . . . ?
O1 Cu1 N1 C17 123.2(6) . . . . ?
O2 Cu1 N1 C21 -140.3(6) . . . . ?
O5 Cu1 N1 C21 39.7(6) . . . . ?
N2 Cu1 N1 C21 -36(12) 3_344 . . . ?
O4 Cu1 N1 C21 117.0(6) . . . . ?
O1 Cu1 N1 C21 -63.4(6) . . . . ?
C6 C1 C2 C3 2.6(10) . . . . ?
C7 C1 C2 C3 179.5(7) . . . . ?
C1 C2 C3 C4 -1.3(12) . . . . ?
C2 C3 C4 C5 -0.6(13) . . . . ?
C3 C4 C5 C6 1.0(14) . . . . ?
C4 C5 C6 C1 0.4(13) . . . . ?
C2 C1 C6 C5 -2.2(10) . . . . ?
C7 C1 C6 C5 -179.0(7) . . . . ?
Cu1 O1 C7 C1 129.7(4) . . . . ?
Cu1 O1 C7 C8 7.7(7) . . . . ?
C6 C1 C7 O1 158.7(6) . . . . ?
C2 C1 C7 O1 -18.1(8) . . . . ?
C6 C1 C7 C8 -79.6(8) . . . . ?
C2 C1 C7 C8 103.6(7) . . . . ?
Cu1 O2 C8 O3 166.4(6) . . . . ?
Cu1 O2 C8 C7 -12.0(9) . . . . ?
O1 C7 C8 O3 -177.5(6) . . . . ?
C1 C7 C8 O3 59.3(8) . . . . ?
O1 C7 C8 O2 1.1(9) . . . . ?
C1 C7 C8 O2 -122.1(7) . . . . ?
C14 C9 C10 C11 -2.1(10) . . . . ?
C15 C9 C10 C11 178.0(6) . . . . ?
C9 C10 C11 C12 0.5(12) . . . . ?
C10 C11 C12 C13 1.4(13) . . . . ?
C11 C12 C13 C14 -1.7(12) . . . . ?
C10 C9 C14 C13 1.7(10) . . . . ?
C15 C9 C14 C13 -178.4(6) . . . . ?
C12 C13 C14 C9 0.1(11) . . . . ?
Cu1 O4 C15 C9 -132.6(4) . . . . ?
Cu1 O4 C15 C16 -8.3(7) . . . . ?
C14 C9 C15 O4 19.1(8) . . . . ?
C10 C9 C15 O4 -161.0(6) . . . . ?
C14 C9 C15 C16 -104.7(7) . . . . ?
C10 C9 C15 C16 75.2(8) . . . . ?
Cu1 O5 C16 O6 -161.5(7) . . . . ?
Cu1 O5 C16 C15 18.8(10) . . . . ?
O4 C15 C16 O6 175.6(7) . . . . ?
C9 C15 C16 O6 -59.9(9) . . . . ?
O4 C15 C16 O5 -4.7(10) . . . . ?
C9 C15 C16 O5 119.8(8) . . . . ?
C21 N1 C17 C18 -3.0(11) . . . . ?
Cu1 N1 C17 C18 170.8(6) . . . . ?
N1 C17 C18 C19 1.5(12) . . . . ?
C17 C18 C19 C20 1.4(11) . . . . ?
C17 C18 C19 C22 -178.5(8) . . . . ?
C18 C19 C20 C21 -2.6(11) . . . . ?
C22 C19 C20 C21 177.3(8) . . . . ?
C17 N1 C21 C20 1.7(12) . . . . ?
Cu1 N1 C21 C20 -172.1(7) . . . . ?
C19 C20 C21 N1 1.1(13) . . . . ?
C18 C19 C22 C23 61.7(11) . . . . ?
C20 C19 C22 C23 -118.2(9) . . . . ?
C19 C22 C23 C24 169.1(8) . . . . ?
C22 C23 C24 C25 57.5(12) . . . . ?
C23 C24 C25 C29 -88.5(11) . . . . ?
C23 C24 C25 C26 90.8(10) . . . . ?
C29 C25 C26 C27 -5.5(11) . . . . ?
C24 C25 C26 C27 175.1(7) . . . . ?
C28 N2 C27 C26 0.1(11) . . . . ?
Cu1 N2 C27 C26 -166.3(6) 3_355 . . . ?
C25 C26 C27 N2 3.8(11) . . . . ?
C27 N2 C28 C29 -2.1(11) . . . . ?
Cu1 N2 C28 C29 164.5(6) 3_355 . . . ?
N2 C28 C29 C25 0.2(12) . . . . ?
C26 C25 C29 C28 3.6(11) . . . . ?
C24 C25 C29 C28 -177.1(8) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1O O6 0.85 1.78 2.620(6) 167.7 4_535
O4 H4O O3 0.85 1.79 2.629(6) 168.2 4_445
C6 H6 O6 0.95 2.46 3.364(11) 158.4 1_655
C7 H7 O5 1.00 2.56 3.344(8) 135.3 4_535
C10 H10 O3 0.95 2.38 3.232(9) 149.3 1_455
C15 H15 O2 1.00 2.55 3.305(8) 132.6 4_445

_diffrn_measured_fraction_theta_max 0.938
_diffrn_reflns_theta_full        62.38
_diffrn_measured_fraction_theta_full 0.938
_refine_diff_density_max         0.714
_refine_diff_density_min         -0.619
_refine_diff_density_rms         0.076

#=================================================END

data_complex2
_database_code_depnum_ccdc_archive 'CCDC 704864'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C42 H40 Cu2 N4 O6'
_chemical_formula_weight         823.86

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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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

_cell_length_a                   9.0498(17)
_cell_length_b                   13.270(2)
_cell_length_c                   16.353(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 103.053(4)
_cell_angle_gamma                90.00
_cell_volume                     1913.2(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3505
_cell_measurement_theta_min      2.00
_cell_measurement_theta_max      26.00

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.07
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.430
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             852
_exptl_absorpt_coefficient_mu    1.165
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8729
_exptl_absorpt_correction_T_max  0.9229
_exptl_absorpt_process_details   'SADABS (Bruker, 2002)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(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 SMART CCD area detector'
_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            5697
_diffrn_reflns_av_R_equivalents  0.0281
_diffrn_reflns_av_sigmaI/netI    0.0574
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.00
_diffrn_reflns_theta_max         26.00
_reflns_number_total             3505
_reflns_number_gt                2957
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART (Bruker, 1998)'
_computing_cell_refinement       'Bruker SMART (Bruker, 1998)'
_computing_data_reduction        'Bruker SAINT + & SHELXTL (Bruker, 1998)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_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)+(0.0484P)²+2.3205P] 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         3505
_refine_ls_number_parameters     244
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0713
_refine_ls_R_factor_gt           0.0590
_refine_ls_wR_factor_ref         0.1402
_refine_ls_wR_factor_gt          0.1335
_refine_ls_goodness_of_fit_ref   1.152
_refine_ls_restrained_S_all      1.152
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.34280(6) 0.03621(3) -0.00421(3) 0.03263(19) Uani 1 1 d . . .
O1 O 0.4846(3) -0.0623(2) 0.05362(19) 0.0380(7) Uani 1 1 d . . .
O2 O 0.2384(3) 0.0098(2) 0.0850(2) 0.0429(8) Uani 1 1 d . . .
N1 N 0.2295(4) 0.1633(2) -0.0426(2) 0.0356(8) Uani 1 1 d . . .
O3 O 0.2565(4) -0.0780(2) 0.2019(2) 0.0565(10) Uani 1 1 d . . .
C18 C 0.2293(5) 0.7565(3) -0.1606(3) 0.0421(11) Uani 1 1 d . . .
H18A H 0.2856 0.7131 -0.1863 0.051 Uiso 1 1 calc R . .
N2 N 0.2115(4) 0.9165(3) -0.0964(2) 0.0375(8) Uani 1 1 d . . .
C15 C 0.0980(6) 0.5380(3) -0.1192(3) 0.0457(12) Uani 1 1 d . . .
H15A H 0.2045 0.5351 -0.1206 0.055 Uiso 1 1 calc R . .
H15B H 0.0916 0.5500 -0.0616 0.055 Uiso 1 1 calc R . .
C19 C 0.0143(5) 0.7949(3) -0.1082(3) 0.0419(11) Uani 1 1 d . . .
H19A H -0.0796 0.7785 -0.0977 0.050 Uiso 1 1 calc R . .
C17 C 0.0892(5) 0.7267(3) -0.1475(3) 0.0378(10) Uani 1 1 d . . .
C8 C 0.3047(6) -0.0530(3) 0.1410(3) 0.0410(11) Uani 1 1 d . . .
C1 C 0.4761(5) -0.2032(3) 0.1474(3) 0.0390(11) Uani 1 1 d . . .
C10 C 0.0920(5) 0.1658(3) -0.0935(3) 0.0391(10) Uani 1 1 d . . .
H10A H 0.0413 0.1053 -0.1086 0.047 Uiso 1 1 calc R . .
C12 C 0.0230(5) 0.2531(3) -0.1245(3) 0.0415(11) Uani 1 1 d . . .
H12A H -0.0735 0.2511 -0.1594 0.050 Uiso 1 1 calc R . .
C13 C 0.0946(5) 0.3449(3) -0.1047(3) 0.0413(11) Uani 1 1 d . . .
C16 C 0.0234(6) 0.6243(3) -0.1736(3) 0.0479(12) Uani 1 1 d . . .
H16A H 0.0314 0.6118 -0.2309 0.057 Uiso 1 1 calc R . .
H16B H -0.0836 0.6251 -0.1732 0.057 Uiso 1 1 calc R . .
C21 C 0.0778(5) 0.8873(3) -0.0846(3) 0.0436(11) Uani 1 1 d . . .
H21A H 0.0238 0.9321 -0.0587 0.052 Uiso 1 1 calc R . .
C14 C 0.0244(6) 0.4393(3) -0.1481(4) 0.0555(14) Uani 1 1 d . . .
H14A H 0.0219 0.4325 -0.2075 0.067 Uiso 1 1 calc R . .
H14B H -0.0799 0.4424 -0.1425 0.067 Uiso 1 1 calc R . .
C7 C 0.4626(5) -0.0917(3) 0.1323(3) 0.0427(11) Uani 1 1 d . . .
H7A H 0.5400 -0.0584 0.1754 0.051 Uiso 1 1 calc R . .
C11 C 0.2343(5) 0.3423(3) -0.0483(3) 0.0443(11) Uani 1 1 d . . .
H11A H 0.2853 0.4019 -0.0303 0.053 Uiso 1 1 calc R . .
C20 C 0.2835(5) 0.8504(3) -0.1354(3) 0.0412(11) Uani 1 1 d . . .
H20A H 0.3764 0.8694 -0.1460 0.049 Uiso 1 1 calc R . .
C9 C 0.2970(5) 0.2512(3) -0.0194(3) 0.0426(11) Uani 1 1 d . . .
H9A H 0.3909 0.2510 0.0182 0.051 Uiso 1 1 calc R . .
C2 C 0.5818(7) -0.2446(4) 0.2122(4) 0.0642(15) Uani 1 1 d . . .
H2A H 0.6469 -0.2023 0.2491 0.077 Uiso 1 1 calc R . .
C3 C 0.5937(8) -0.3483(4) 0.2239(4) 0.0709(17) Uani 1 1 d . . .
H3A H 0.6648 -0.3747 0.2689 0.085 Uiso 1 1 calc R . .
C6 C 0.3800(6) -0.2689(4) 0.0926(4) 0.0588(14) Uani 1 1 d . . .
H6A H 0.3066 -0.2429 0.0485 0.071 Uiso 1 1 calc R . .
C5 C 0.3936(8) -0.3713(4) 0.1037(4) 0.0731(18) Uani 1 1 d . . .
H5A H 0.3297 -0.4141 0.0666 0.088 Uiso 1 1 calc R . .
C4 C 0.5010(8) -0.4114(5) 0.1692(5) 0.0759(19) Uani 1 1 d . . .
H4A H 0.5103 -0.4808 0.1760 0.091 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 O1 1.924(3) . ?
Cu1 O2 1.941(3) . ?
Cu1 O1 1.945(3) 3_655 ?
Cu1 N1 1.999(3) . ?
Cu1 N2 2.323(4) 1_545 ?
Cu1 Cu1 2.9768(11) 3_655 ?
O1 C7 1.402(5) . ?
O1 Cu1 1.945(3) 3_655 ?
O2 C8 1.282(5) . ?
N1 C10 1.332(6) . ?
N1 C9 1.332(6) . ?
O3 C8 1.220(5) . ?
C18 C20 1.368(6) . ?
C18 C17 1.390(6) . ?
N2 C21 1.326(6) . ?
N2 C20 1.338(5) . ?
N2 Cu1 2.323(4) 1_565 ?
C15 C14 1.497(6) . ?
C15 C16 1.512(6) . ?
C19 C17 1.374(6) . ?
C19 C21 1.372(6) . ?
C17 C16 1.507(6) . ?
C8 C7 1.555(6) . ?
C1 C2 1.371(7) . ?
C1 C6 1.402(7) . ?
C1 C7 1.501(6) . ?
C10 C12 1.358(6) . ?
C12 C13 1.384(6) . ?
C13 C11 1.386(7) . ?
C13 C14 1.508(6) . ?
C11 C9 1.373(6) . ?
C2 C3 1.390(8) . ?
C3 C4 1.366(9) . ?
C6 C5 1.373(7) . ?
C5 C4 1.380(9) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Cu1 O2 83.80(12) . . ?
O1 Cu1 O1 79.40(12) . 3_655 ?
O2 Cu1 O1 156.57(14) . 3_655 ?
O1 Cu1 N1 164.81(15) . . ?
O2 Cu1 N1 94.91(13) . . ?
O1 Cu1 N1 97.04(13) 3_655 . ?
O1 Cu1 N2 92.36(13) . 1_545 ?
O2 Cu1 N2 95.74(13) . 1_545 ?
O1 Cu1 N2 101.13(13) 3_655 1_545 ?
N1 Cu1 N2 102.83(14) . 1_545 ?
O1 Cu1 Cu1 39.95(8) . 3_655 ?
O2 Cu1 Cu1 121.98(10) . 3_655 ?
O1 Cu1 Cu1 39.45(8) 3_655 3_655 ?
N1 Cu1 Cu1 134.74(10) . 3_655 ?
N2 Cu1 Cu1 98.78(9) 1_545 3_655 ?
C7 O1 Cu1 115.0(2) . . ?
C7 O1 Cu1 136.5(3) . 3_655 ?
Cu1 O1 Cu1 100.60(12) . 3_655 ?
C8 O2 Cu1 115.1(3) . . ?
C10 N1 C9 117.3(4) . . ?
C10 N1 Cu1 123.9(3) . . ?
C9 N1 Cu1 118.7(3) . . ?
C20 C18 C17 119.3(4) . . ?
C21 N2 C20 115.9(4) . . ?
C21 N2 Cu1 117.1(3) . 1_565 ?
C20 N2 Cu1 121.7(3) . 1_565 ?
C14 C15 C16 111.6(4) . . ?
C17 C19 C21 120.1(4) . . ?
C19 C17 C18 116.6(4) . . ?
C19 C17 C16 121.5(4) . . ?
C18 C17 C16 121.9(4) . . ?
O3 C8 O2 124.3(4) . . ?
O3 C8 C7 119.3(4) . . ?
O2 C8 C7 116.2(4) . . ?
C2 C1 C6 117.9(5) . . ?
C2 C1 C7 122.6(5) . . ?
C6 C1 C7 119.5(4) . . ?
N1 C10 C12 122.7(4) . . ?
C10 C12 C13 120.8(5) . . ?
C11 C13 C12 116.2(4) . . ?
C11 C13 C14 123.9(4) . . ?
C12 C13 C14 119.7(4) . . ?
C17 C16 C15 114.8(4) . . ?
N2 C21 C19 123.9(4) . . ?
C15 C14 C13 117.9(4) . . ?
O1 C7 C1 113.7(4) . . ?
O1 C7 C8 108.4(4) . . ?
C1 C7 C8 110.7(4) . . ?
C9 C11 C13 119.7(4) . . ?
N2 C20 C18 124.1(4) . . ?
N1 C9 C11 123.1(5) . . ?
C1 C2 C3 121.4(6) . . ?
C4 C3 C2 120.0(6) . . ?
C5 C6 C1 120.5(6) . . ?
C4 C5 C6 120.6(6) . . ?
C3 C4 C5 119.5(6) . . ?

_diffrn_measured_fraction_theta_max 0.932
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.932
_refine_diff_density_max         0.581
_refine_diff_density_min         -0.451
_refine_diff_density_rms         0.084

#=================================================END

data_complex4R
_database_code_depnum_ccdc_archive 'CCDC 704865'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C29 H28 Fe N2 O6'
_chemical_formula_sum            'C29 H28 Fe N2 O6'
_chemical_formula_weight         556.38

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'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_H-M   P6522
_chemical_absolute_configuration R

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z+2/3'
'-x+y, -x, z+1/3'
'-x, -y, z+1/2'
'y, -x+y, z+1/6'
'x-y, x, z+5/6'
'y, x, -z+2/3'
'x-y, -y, -z'
'-x, -x+y, -z+1/3'
'-y, -x, -z+1/6'
'-x+y, y, -z+1/2'
'x, x-y, -z+5/6'

_cell_length_a                   11.6431(12)
_cell_length_b                   11.6431(12)
_cell_length_c                   32.956(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     3869.0(9)
_cell_formula_units_Z            6
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2746
_cell_measurement_theta_min      2.37
_cell_measurement_theta_max      27.82

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.19
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.433
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1740
_exptl_absorpt_coefficient_mu    0.632
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8138
_exptl_absorpt_correction_T_max  0.8894
_exptl_absorpt_process_details   'SADABS (Bruker, 2002)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(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 SMART CCD area detector'
_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            7089
_diffrn_reflns_av_R_equivalents  0.0281
_diffrn_reflns_av_sigmaI/netI    0.0454
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_theta_min         2.37
_diffrn_reflns_theta_max         27.82
_reflns_number_total             2746
_reflns_number_gt                2191
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART (Bruker, 1998)'
_computing_cell_refinement       'Bruker SMART (Bruker, 1998)'
_computing_data_reduction        'Bruker SAINT + & SHELXTL (Bruker, 1998)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_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)+(0.0723P)²+4.5353P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.02(6)
_refine_ls_number_reflns         2746
_refine_ls_number_parameters     175
_refine_ls_number_restraints     100
_refine_ls_R_factor_all          0.0875
_refine_ls_R_factor_gt           0.0713
_refine_ls_wR_factor_ref         0.1793
_refine_ls_wR_factor_gt          0.1676
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_restrained_S_all      1.259
_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
Fe1 Fe 0.87092(3) 0.12908(3) 0.0833 0.05686(14) Uani 1 2 d S . .
O1 O 0.81379(19) -0.07871(19) 0.08411(6) 0.0553(6) Uani 1 1 d D . .
H1O H 0.8308(19) -0.1174(18) 0.0655(6) 0.061(10) Uiso 1 1 d D . .
O2 O 0.84562(19) 0.07886(18) 0.14395(6) 0.0546(6) Uani 1 1 d . . .
O3 O 0.8259(2) -0.0654(2) 0.19120(6) 0.0702(8) Uani 1 1 d . . .
N1 N 0.6637(2) 0.0674(3) 0.07284(9) 0.0880(10) Uani 1 1 d DU . .
C1 C 0.6928(3) -0.2652(3) 0.12892(8) 0.0589(11) Uani 1 1 d . . .
C2 C 0.6987(5) -0.3786(4) 0.13083(13) 0.0890(17) Uani 1 1 d . . .
H2 H 0.7810 -0.3732 0.1291 0.107 Uiso 1 1 calc R . .
C3 C 0.5850(6) -0.5038(5) 0.13534(14) 0.114(2) Uani 1 1 d U . .
H3 H 0.5911 -0.5802 0.1377 0.137 Uiso 1 1 calc R . .
C4 C 0.4719(6) -0.5091(6) 0.13615(13) 0.122(2) Uani 1 1 d U . .
H4 H 0.3965 -0.5926 0.1379 0.147 Uiso 1 1 calc R . .
C5 C 0.4539(5) -0.4026(6) 0.13462(15) 0.122(2) Uani 1 1 d U . .
H5 H 0.3699 -0.4119 0.1362 0.146 Uiso 1 1 calc R . .
C6 C 0.5698(4) -0.2762(5) 0.13049(12) 0.0957(18) Uani 1 1 d . . .
H6 H 0.5622 -0.2005 0.1288 0.115 Uiso 1 1 calc R . .
C7 C 0.8142(3) -0.1319(3) 0.12266(8) 0.0479(8) Uani 1 1 d . . .
H7 H 0.8920 -0.1433 0.1241 0.058 Uiso 1 1 calc R . .
C8 C 0.8291(3) -0.0309(3) 0.15556(8) 0.0488(8) Uani 1 1 d . . .
C9 C 0.1374(6) -0.1374(6) 0.0833 0.0998(16) Uani 0.50 2 d SPDU A 1
H9 H 0.0519 -0.1689 0.0712 0.120 Uiso 0.50 1 d PR A 1
C10 C 0.2358(7) -0.1296(8) 0.0530(3) 0.0998(16) Uani 0.50 1 d PDU A 1
H10A H 0.2207 -0.0956 0.0279 0.120 Uiso 0.50 1 calc PR A 1
H10B H 0.2172 -0.2192 0.0476 0.120 Uiso 0.50 1 calc PR A 1
C11 C 0.3917(3) -0.0406(4) 0.06408(12) 0.1168(16) Uani 0.50 1 d PDU A 1
C9' C 0.1994(6) -0.1994(6) 0.0833 0.0998(16) Uani 0.50 2 d SPD A 2
H9' H 0.2532 -0.1963 0.1049 0.120 Uiso 0.50 1 d PR A 2
C10' C 0.2494(7) -0.0712(7) 0.0626(3) 0.0998(16) Uani 0.50 1 d PDU A 2
H10C H 0.2346 -0.0086 0.0779 0.120 Uiso 0.50 1 calc PR A 2
H10D H 0.2158 -0.0800 0.0352 0.120 Uiso 0.50 1 calc PR A 2
C11' C 0.3917(3) -0.0406(4) 0.06408(12) 0.1168(16) Uani 0.50 1 d PD A 2
C12 C 0.4606(4) 0.0591(4) 0.09025(14) 0.1172(16) Uani 1 1 d DU . .
H12 H 0.4171 0.0930 0.1055 0.141 Uiso 1 1 calc R A 1
C13 C 0.5972(3) 0.1124(4) 0.09469(12) 0.1021(14) Uani 1 1 d DU A .
H13 H 0.6432 0.1806 0.1132 0.123 Uiso 1 1 calc R . .
C14 C 0.5948(4) -0.0320(5) 0.04732(12) 0.0997(15) Uani 1 1 d DU A .
H14 H 0.6394 -0.0649 0.0322 0.120 Uiso 1 1 calc R . .
C15 C 0.4603(4) -0.0880(5) 0.04243(14) 0.1173(18) Uani 1 1 d DU . .
H15 H 0.4155 -0.1581 0.0244 0.141 Uiso 1 1 calc R A 1


_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
Fe1 O2 2.0610(19) 10_665 ?
Fe1 O2 2.0610(19) . ?
Fe1 O1 2.165(2) 10_665 ?
Fe1 O1 2.165(2) . ?
Fe1 N1 2.174(3) . ?
Fe1 N1 2.174(3) 10_665 ?
O1 C7 1.415(3) . ?
O1 H1O 0.841(17) . ?
O2 C8 1.253(4) . ?
O3 C8 1.236(3) . ?
N1 C14 1.327(5) . ?
N1 C13 1.340(6) . ?
C1 C2 1.358(6) . ?
C1 C6 1.374(6) . ?
C1 C7 1.502(4) . ?
C2 C3 1.404(6) . ?
C2 H2 0.9300 . ?
C3 C4 1.287(9) . ?
C3 H3 0.9300 . ?
C4 C5 1.358(10) . ?
C4 H4 0.9300 . ?
C5 C6 1.421(6) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C7 C8 1.544(4) . ?
C7 H7 0.9800 . ?
C9 C10 1.490(10) . ?
C9 C10 1.490(10) 10 ?
C9 H9 0.9595 . ?
C10 C11 1.618(7) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 C12 1.344(6) . ?
C11 C15 1.376(7) . ?
C9' C10' 1.471(10) . ?
C9' C10' 1.471(10) 10 ?
C9' H9' 0.9354 . ?
C10' H10C 0.9700 . ?
C10' H10D 0.9700 . ?
C12 C13 1.396(5) . ?
C12 H12 0.9300 . ?
C13 H13 0.9300 . ?
C14 C15 1.372(5) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?

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
O2 Fe1 O2 165.99(14) 10_665 . ?
O2 Fe1 O1 75.59(8) 10_665 10_665 ?
O2 Fe1 O1 94.46(8) . 10_665 ?
O2 Fe1 O1 94.46(8) 10_665 . ?
O2 Fe1 O1 75.58(8) . . ?
O1 Fe1 O1 90.88(11) 10_665 . ?
O2 Fe1 N1 94.69(10) 10_665 . ?
O2 Fe1 N1 94.75(10) . . ?
O1 Fe1 N1 170.07(9) 10_665 . ?
O1 Fe1 N1 87.85(11) . . ?
O2 Fe1 N1 94.75(10) 10_665 10_665 ?
O2 Fe1 N1 94.69(10) . 10_665 ?
O1 Fe1 N1 87.85(11) 10_665 10_665 ?
O1 Fe1 N1 170.07(9) . 10_665 ?
N1 Fe1 N1 95.06(19) . 10_665 ?
C7 O1 Fe1 115.70(16) . . ?
C7 O1 H1O 111.5(17) . . ?
Fe1 O1 H1O 124.5(14) . . ?
C8 O2 Fe1 120.82(18) . . ?
C14 N1 C13 117.8(3) . . ?
C14 N1 Fe1 118.4(3) . . ?
C13 N1 Fe1 123.2(2) . . ?
C2 C1 C6 117.7(4) . . ?
C2 C1 C7 122.1(4) . . ?
C6 C1 C7 120.1(4) . . ?
C1 C2 C3 122.3(5) . . ?
C1 C2 H2 118.8 . . ?
C3 C2 H2 118.8 . . ?
C4 C3 C2 117.6(6) . . ?
C4 C3 H3 121.2 . . ?
C2 C3 H3 121.2 . . ?
C3 C4 C5 125.2(5) . . ?
C3 C4 H4 117.4 . . ?
C5 C4 H4 117.4 . . ?
C4 C5 C6 116.7(6) . . ?
C4 C5 H5 121.7 . . ?
C6 C5 H5 121.7 . . ?
C1 C6 C5 120.4(6) . . ?
C1 C6 H6 119.8 . . ?
C5 C6 H6 119.8 . . ?
O1 C7 C1 111.6(2) . . ?
O1 C7 C8 108.7(3) . . ?
C1 C7 C8 112.3(2) . . ?
O1 C7 H7 108.0 . . ?
C1 C7 H7 108.0 . . ?
C8 C7 H7 108.0 . . ?
O3 C8 O2 125.9(3) . . ?
O3 C8 C7 116.5(3) . . ?
O2 C8 C7 117.6(2) . . ?
C10 C9 C10 104.3(10) . 10 ?
C10 C9 H9 111.3 . . ?
C10 C9 H9 109.5 10 . ?
C9 C10 C11 118.0(6) . . ?
C9 C10 H10A 107.8 . . ?
C11 C10 H10A 107.8 . . ?
C9 C10 H10B 107.8 . . ?
C11 C10 H10B 107.8 . . ?
H10A C10 H10B 107.1 . . ?
C12 C11 C15 117.6(3) . . ?
C12 C11 C10 133.8(5) . . ?
C15 C11 C10 108.5(4) . . ?
C10' C9' C10' 115.3(10) . 10 ?
C10' C9' H9' 113.3 . . ?
C10' C9' H9' 101.0 10 . ?
C9' C10' H10C 113.1 . . ?
C9' C10' H10D 113.1 . . ?
H10C C10' H10D 110.5 . . ?
C11 C12 C13 120.5(4) . . ?
C11 C12 H12 119.8 . . ?
C13 C12 H12 119.8 . . ?
N1 C13 C12 121.5(4) . . ?
N1 C13 H13 119.3 . . ?
C12 C13 H13 119.3 . . ?
N1 C14 C15 122.5(4) . . ?
N1 C14 H14 118.7 . . ?
C15 C14 H14 118.7 . . ?
C14 C15 C11 120.2(4) . . ?
C14 C15 H15 119.9 . . ?
C11 C15 H15 119.9 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1O O3 0.841(17) 1.795(18) 2.628(3) 170.6(18) 6_544

_diffrn_measured_fraction_theta_max 0.912
_diffrn_reflns_theta_full        27.82
_diffrn_measured_fraction_theta_full 0.912
_refine_diff_density_max         0.509
_refine_diff_density_min         -0.480
_refine_diff_density_rms         0.065

#=================================================END

data_complex4S
_database_code_depnum_ccdc_archive 'CCDC 704866'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C29 H28 Fe N2 O6'
_chemical_formula_weight         556.38

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'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_H-M   P6122
_chemical_absolute_configuration S

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z+1/3'
'-x+y, -x, z+2/3'
'-x, -y, z+1/2'
'y, -x+y, z+5/6'
'x-y, x, z+1/6'
'y, x, -z+1/3'
'x-y, -y, -z'
'-x, -x+y, -z+2/3'
'-y, -x, -z+5/6'
'-x+y, y, -z+1/2'
'x, x-y, -z+1/6'

_cell_length_a                   11.5654(8)
_cell_length_b                   11.5654(8)
_cell_length_c                   32.789(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     3798.2(5)
_cell_formula_units_Z            6
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    3235
_cell_measurement_theta_min      2.76
_cell_measurement_theta_max      29.00

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.17
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.459
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1740
_exptl_absorpt_coefficient_mu    0.644
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8556
_exptl_absorpt_correction_T_max  0.8984
_exptl_absorpt_process_details   'SADABS (Bruker, 2002)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(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 SMART CCD area detector'
_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            9634
_diffrn_reflns_av_R_equivalents  0.0341
_diffrn_reflns_av_sigmaI/netI    0.0595
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_theta_min         2.76
_diffrn_reflns_theta_max         29.00
_reflns_number_total             3235
_reflns_number_gt                2125
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART (Bruker, 1998)'
_computing_cell_refinement       'Bruker SMART (Bruker, 1998)'
_computing_data_reduction        'Bruker SAINT + & SHELXTL (Bruker, 1998)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_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)+(0.0579P)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    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(3)
_refine_ls_number_reflns         3235
_refine_ls_number_parameters     245
_refine_ls_number_restraints     49
_refine_ls_R_factor_all          0.0725
_refine_ls_R_factor_gt           0.0422
_refine_ls_wR_factor_ref         0.1107
_refine_ls_wR_factor_gt          0.1006
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_restrained_S_all      1.089
_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
Fe1 Fe 0.25739(6) 0.12870(3) 0.0833 0.0495(2) Uani 1 2 d S . .
O1 O 0.1071(2) -0.06782(19) 0.19147(5) 0.0503(5) Uani 1 1 d . . .
O2 O 0.23187(18) 0.0781(2) 0.14409(5) 0.0432(5) Uani 1 1 d . . .
O3 O 0.10761(19) -0.08001(19) 0.08392(5) 0.0411(4) Uani 1 1 d D . .
H3O H 0.048(2) -0.117(3) 0.0662(7) 0.040(8) Uiso 1 1 d D . .
C1 C 0.1377(3) -0.0324(3) 0.15562(7) 0.0378(6) Uani 1 1 d . . .
C2 C 0.0512(3) -0.1336(3) 0.12259(7) 0.0377(6) Uani 1 1 d . . .
H2 H -0.0402 -0.1446 0.1237 0.045 Uiso 1 1 calc R . .
C3 C 0.0386(3) -0.2695(3) 0.12888(7) 0.0474(8) Uani 1 1 d D . .
C4 C -0.0839(4) -0.3818(3) 0.13130(12) 0.0731(11) Uani 1 1 d DU . .
H4 H -0.1623 -0.3749 0.1301 0.088 Uiso 1 1 calc R . .
C5 C -0.0944(6) -0.5067(4) 0.13560(12) 0.0970(17) Uani 1 1 d DU . .
H5 H -0.1803 -0.5840 0.1376 0.116 Uiso 1 1 calc R . .
C6 C 0.0118(9) -0.5192(5) 0.13696(12) 0.117(2) Uani 1 1 d DU . .
H6 H 0.0027 -0.6050 0.1401 0.141 Uiso 1 1 calc R . .
C7 C 0.1360(7) -0.4090(7) 0.13383(12) 0.113(2) Uani 1 1 d DU . .
H7 H 0.2129 -0.4186 0.1344 0.135 Uiso 1 1 calc R . .
C8 C 0.1505(5) -0.2813(4) 0.12983(10) 0.0757(12) Uani 1 1 d DU . .
H8 H 0.2367 -0.2044 0.1278 0.091 Uiso 1 1 calc R . .
N1 N 0.3947(7) 0.0369(7) 0.0723(2) 0.0340(16) Uani 0.50 1 d P . 1
C9 C 0.3584(11) -0.0669(9) 0.0473(3) 0.051(2) Uani 0.50 1 d P . 1
H9 H 0.2748 -0.1025 0.0338 0.061 Uiso 0.50 1 calc PR . 1
C10 C 0.4344(7) -0.1248(7) 0.0400(2) 0.0482(17) Uani 0.50 1 d P . 1
H10 H 0.4035 -0.1987 0.0219 0.058 Uiso 0.50 1 calc PR . 1
C11 C 0.5543(7) -0.0761(7) 0.0587(2) 0.0354(17) Uani 0.50 1 d P . 1
C12 C 0.5905(12) 0.0249(11) 0.0858(3) 0.036(2) Uani 0.50 1 d P . 1
H12 H 0.6716 0.0589 0.1006 0.044 Uiso 0.50 1 calc PR . 1
C13 C 0.5068(8) 0.0781(8) 0.0915(2) 0.0437(18) Uani 0.50 1 d P . 1
H13 H 0.5334 0.1488 0.1106 0.052 Uiso 0.50 1 calc PR . 1
C14 C 0.6438(6) -0.1325(6) 0.04855(15) 0.0413(13) Uani 0.50 1 d P . 1
H14A H 0.7041 -0.0791 0.0261 0.050 Uiso 0.50 1 calc PR . 1
H14B H 0.5874 -0.2247 0.0383 0.050 Uiso 0.50 1 calc PR . 1
C15 C 0.7283(7) -0.1359(4) 0.0833 0.0427(16) Uani 0.50 2 d SP . 1
H15 H 0.7848 -0.0467 0.0933 0.051 Uiso 0.50 1 d PR . 1
N1' N 0.4126(8) 0.1029(7) 0.0737(3) 0.0435(18) Uani 0.50 1 d P . 2
C9' C 0.3902(10) 0.0031(11) 0.0483(3) 0.046(2) Uani 0.50 1 d P . 2
H9' H 0.3125 -0.0342 0.0317 0.055 Uiso 0.50 1 calc PR . 2
C10' C 0.4763(8) -0.0485(8) 0.0452(2) 0.0499(17) Uani 0.50 1 d P . 2
H10' H 0.4576 -0.1172 0.0260 0.060 Uiso 0.50 1 calc PR . 2
C11' C 0.5889(11) -0.0008(15) 0.0697(3) 0.045(3) Uani 0.50 1 d P . 2
C12' C 0.6092(8) 0.0987(9) 0.0964(2) 0.0466(16) Uani 0.50 1 d P . 2
H12' H 0.6844 0.1350 0.1141 0.056 Uiso 0.50 1 calc PR . 2
C13' C 0.5224(7) 0.1460(8) 0.0978(2) 0.0431(17) Uani 0.50 1 d P . 2
H13' H 0.5399 0.2141 0.1171 0.052 Uiso 0.50 1 calc PR . 2
C14' C 0.6776(7) -0.0587(7) 0.0711(2) 0.0593(16) Uani 0.50 1 d P . 2
H14C H 0.7504 -0.0098 0.0910 0.071 Uiso 0.50 1 calc PR . 2
H14D H 0.7181 -0.0519 0.0439 0.071 Uiso 0.50 1 calc PR . 2
C15' C 0.5951(9) -0.2024(5) 0.0833 0.056(2) Uani 0.50 2 d SP . 2
H15' H 0.5388 -0.2540 0.0609 0.068 Uiso 0.50 1 d PR . 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
Fe1 N1' 1.986(7) 12 ?
Fe1 N1' 1.986(7) . ?
Fe1 O2 2.0555(17) 12 ?
Fe1 O2 2.0555(17) . ?
Fe1 O3 2.156(2) 12 ?
Fe1 O3 2.156(2) . ?
Fe1 N1 2.338(7) 12 ?
Fe1 N1 2.338(7) . ?
O1 C1 1.237(3) . ?
O2 C1 1.254(3) . ?
O3 C2 1.419(3) . ?
O3 H3O 0.839(18) . ?
C1 C2 1.540(4) . ?
C2 C3 1.518(4) . ?
C2 H2 1.0000 . ?
C3 C4 1.364(5) . ?
C3 C8 1.368(5) . ?
C4 C5 1.395(5) . ?
C4 H4 0.9500 . ?
C5 C6 1.308(7) . ?
C5 H5 0.9500 . ?
C6 C7 1.366(8) . ?
C6 H6 0.9500 . ?
C7 C8 1.407(6) . ?
C7 H7 0.9500 . ?
C8 H8 0.9500 . ?
N1 C13 1.298(11) . ?
N1 C9 1.337(10) . ?
C9 C10 1.368(14) . ?
C9 H9 0.9500 . ?
C10 C11 1.354(11) . ?
C10 H10 0.9500 . ?
C11 C12 1.356(11) . ?
C11 C14 1.512(10) . ?
C12 C13 1.395(13) . ?
C12 H12 0.9500 . ?
C13 H13 0.9500 . ?
C14 C15 1.514(7) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C14 1.514(7) 12_545 ?
C15 H15 0.9606 . ?
N1' C9' 1.339(12) . ?
N1' C13' 1.363(11) . ?
C9' C10' 1.397(13) . ?
C9' H9' 0.9500 . ?
C10' C11' 1.389(14) . ?
C10' H10' 0.9500 . ?
C11' C12' 1.370(12) . ?
C11' C14' 1.481(13) . ?
C12' C13' 1.363(12) . ?
C12' H12' 0.9500 . ?
C13' H13' 0.9500 . ?
C14' C15' 1.500(9) . ?
C14' H14C 0.9900 . ?
C14' H14D 0.9900 . ?
C15' C14' 1.500(9) 12_545 ?
C15' H15' 0.9651 . ?

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' Fe1 N1' 77.0(4) 12 . ?
N1' Fe1 O2 97.1(2) 12 12 ?
N1' Fe1 O2 94.1(2) . 12 ?
N1' Fe1 O2 94.1(2) 12 . ?
N1' Fe1 O2 97.1(2) . . ?
O2 Fe1 O2 165.71(11) 12 . ?
N1' Fe1 O3 96.5(2) 12 12 ?
N1' Fe1 O3 167.3(2) . 12 ?
O2 Fe1 O3 75.64(7) 12 12 ?
O2 Fe1 O3 94.29(7) . 12 ?
N1' Fe1 O3 167.3(2) 12 . ?
N1' Fe1 O3 96.5(2) . . ?
O2 Fe1 O3 94.29(7) 12 . ?
O2 Fe1 O3 75.64(7) . . ?
O3 Fe1 O3 91.79(10) 12 . ?
N1' Fe1 N1 15.7(3) 12 12 ?
N1' Fe1 N1 92.4(3) . 12 ?
O2 Fe1 N1 93.1(2) 12 12 ?
O2 Fe1 N1 95.3(2) . 12 ?
O3 Fe1 N1 80.85(18) 12 12 ?
O3 Fe1 N1 168.0(2) . 12 ?
N1' Fe1 N1 92.4(3) 12 . ?
N1' Fe1 N1 15.7(3) . . ?
O2 Fe1 N1 95.3(2) 12 . ?
O2 Fe1 N1 93.1(2) . . ?
O3 Fe1 N1 168.0(2) 12 . ?
O3 Fe1 N1 80.85(18) . . ?
N1 Fe1 N1 107.9(4) 12 . ?
C1 O2 Fe1 120.69(15) . . ?
C2 O3 Fe1 115.71(15) . . ?
C2 O3 H3O 108.2(19) . . ?
Fe1 O3 H3O 124.3(19) . . ?
O1 C1 O2 125.7(2) . . ?
O1 C1 C2 116.6(3) . . ?
O2 C1 C2 117.8(2) . . ?
O3 C2 C3 111.0(2) . . ?
O3 C2 C1 108.3(2) . . ?
C3 C2 C1 112.4(2) . . ?
O3 C2 H2 108.3 . . ?
C3 C2 H2 108.3 . . ?
C1 C2 H2 108.3 . . ?
C4 C3 C8 119.1(3) . . ?
C4 C3 C2 120.7(3) . . ?
C8 C3 C2 120.0(3) . . ?
C3 C4 C5 120.3(4) . . ?
C3 C4 H4 119.9 . . ?
C5 C4 H4 119.9 . . ?
C6 C5 C4 121.2(5) . . ?
C6 C5 H5 119.4 . . ?
C4 C5 H5 119.4 . . ?
C5 C6 C7 120.1(4) . . ?
C5 C6 H6 119.9 . . ?
C7 C6 H6 119.9 . . ?
C6 C7 C8 120.2(5) . . ?
C6 C7 H7 119.9 . . ?
C8 C7 H7 119.9 . . ?
C3 C8 C7 119.0(4) . . ?
C3 C8 H8 120.5 . . ?
C7 C8 H8 120.5 . . ?
C13 N1 C9 115.8(8) . . ?
C13 N1 Fe1 122.6(6) . . ?
C9 N1 Fe1 121.5(7) . . ?
N1 C9 C10 123.9(9) . . ?
N1 C9 H9 118.0 . . ?
C10 C9 H9 118.0 . . ?
C11 C10 C9 119.4(7) . . ?
C11 C10 H10 120.3 . . ?
C9 C10 H10 120.3 . . ?
C10 C11 C12 117.8(9) . . ?
C10 C11 C14 120.0(6) . . ?
C12 C11 C14 122.2(8) . . ?
C11 C12 C13 119.0(10) . . ?
C11 C12 H12 120.5 . . ?
C13 C12 H12 120.5 . . ?
N1 C13 C12 124.0(7) . . ?
N1 C13 H13 118.0 . . ?
C12 C13 H13 118.0 . . ?
C11 C14 C15 115.8(4) . . ?
C11 C14 H14A 108.3 . . ?
C15 C14 H14A 108.3 . . ?
C11 C14 H14B 108.3 . . ?
C15 C14 H14B 108.3 . . ?
H14A C14 H14B 107.4 . . ?
C14 C15 C14 112.1(6) . 12_545 ?
C14 C15 H15 109.2 . . ?
C14 C15 H15 109.2 12_545 . ?
C9' N1' C13' 114.7(8) . . ?
C9' N1' Fe1 115.4(7) . . ?
C13' N1' Fe1 126.9(6) . . ?
N1' C9' C10' 122.9(9) . . ?
N1' C9' H9' 118.6 . . ?
C10' C9' H9' 118.6 . . ?
C11' C10' C9' 120.9(9) . . ?
C11' C10' H10' 119.5 . . ?
C9' C10' H10' 119.5 . . ?
C12' C11' C10' 115.9(10) . . ?
C12' C11' C14' 119.7(9) . . ?
C10' C11' C14' 124.2(11) . . ?
C13' C12' C11' 120.5(9) . . ?
C13' C12' H12' 119.8 . . ?
C11' C12' H12' 119.8 . . ?
C12' C13' N1' 125.0(8) . . ?
C12' C13' H13' 117.5 . . ?
N1' C13' H13' 117.5 . . ?
C11' C14' C15' 108.0(8) . . ?
C11' C14' H15 139.4 . . ?
C15' C14' H15 90.7 . . ?
C11' C14' H14C 110.1 . . ?
C15' C14' H14C 110.1 . . ?
H15 C14' H14C 29.8 . . ?
C11' C14' H14D 110.1 . . ?
C15' C14' H14D 110.1 . . ?
H15 C14' H14D 95.8 . . ?
H14C C14' H14D 108.4 . . ?
C14' C15' C14' 113.1(8) 12_545 . ?
C14' C15' H15' 107.8 12_545 . ?
C14' C15' H15' 109.8 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O3 H3O O1 0.839(18) 1.784(18) 2.618(2) 172(3) 5_554

_diffrn_measured_fraction_theta_max 0.968
_diffrn_reflns_theta_full        29.00
_diffrn_measured_fraction_theta_full 0.968
_refine_diff_density_max         0.171
_refine_diff_density_min         -0.435
_refine_diff_density_rms         0.044

#=================================================END

data_complex5R
_database_code_depnum_ccdc_archive 'CCDC 704867'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C29 H28 Co N2 O6'
_chemical_formula_weight         559.46

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           hexagonal
_symmetry_space_group_name_H-M   P6522
_chemical_absolute_configuration R

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z+2/3'
'-x+y, -x, z+1/3'
'-x, -y, z+1/2'
'y, -x+y, z+1/6'
'x-y, x, z+5/6'
'y, x, -z+2/3'
'x-y, -y, -z'
'-x, -x+y, -z+1/3'
'-y, -x, -z+1/6'
'-x+y, y, -z+1/2'
'x, x-y, -z+5/6'

_cell_length_a                   11.5947(16)
_cell_length_b                   11.5947(16)
_cell_length_c                   33.068(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     3849.9(13)
_cell_formula_units_Z            6
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2563
_cell_measurement_theta_min      2.03
_cell_measurement_theta_max      27.49

_exptl_crystal_description       block
_exptl_crystal_colour            purple
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.448
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1746
_exptl_absorpt_coefficient_mu    0.716
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7980
_exptl_absorpt_correction_T_max  0.9002
_exptl_absorpt_process_details   'SADABS (Bruker, 2002)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(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 SMART CCD area detector'
_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            7061
_diffrn_reflns_av_R_equivalents  0.0655
_diffrn_reflns_av_sigmaI/netI    0.0879
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         2.03
_diffrn_reflns_theta_max         27.49
_reflns_number_total             2563
_reflns_number_gt                1746
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART (Bruker, 1998)'
_computing_cell_refinement       'Bruker SMART (Bruker, 1998)'
_computing_data_reduction        'Bruker SAINT + & SHELXTL (Bruker, 1998)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_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)+(0.1012P)²+15.3704P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.11(8)
_refine_ls_number_reflns         2563
_refine_ls_number_parameters     174
_refine_ls_number_restraints     100
_refine_ls_R_factor_all          0.1389
_refine_ls_R_factor_gt           0.1025
_refine_ls_wR_factor_ref         0.2551
_refine_ls_wR_factor_gt          0.2294
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_restrained_S_all      1.073
_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
Co1 Co 0.87211(5) 0.12789(5) 0.0833 0.0462(2) Uani 1 2 d S . .
O1 O 0.8163(3) -0.0757(3) 0.08368(8) 0.0482(10) Uani 1 1 d D . .
H1O H 0.831(2) -0.1201(18) 0.0661(7) 0.058 Uiso 1 1 d D . .
O2 O 0.8499(3) 0.0827(3) 0.14376(8) 0.0467(9) Uani 1 1 d . . .
O3 O 0.8286(4) -0.0645(3) 0.19052(8) 0.0568(12) Uani 1 1 d . . .
N1 N 0.6678(3) 0.0658(5) 0.07371(13) 0.0726(15) Uani 1 1 d DU . .
C1 C 0.6967(5) -0.2643(5) 0.12847(12) 0.0477(17) Uani 1 1 d . . .
C2 C 0.7039(7) -0.3778(6) 0.13076(19) 0.082(3) Uani 1 1 d . . .
H2 H 0.7865 -0.3729 0.1295 0.098 Uiso 1 1 calc R . .
C3 C 0.5863(8) -0.5039(7) 0.1351(2) 0.094(3) Uani 1 1 d U . .
H3 H 0.5921 -0.5808 0.1371 0.113 Uiso 1 1 calc R . .
C4 C 0.4737(8) -0.5112(8) 0.13612(19) 0.098(3) Uani 1 1 d U . .
H4 H 0.3991 -0.5955 0.1385 0.117 Uiso 1 1 calc R . .
C5 C 0.4534(8) -0.4070(9) 0.1340(2) 0.100(3) Uani 1 1 d U . .
H5 H 0.3683 -0.4179 0.1354 0.120 Uiso 1 1 calc R . .
C6 C 0.5726(7) -0.2747(8) 0.12951(18) 0.091(3) Uani 1 1 d . . .
H6 H 0.5645 -0.1990 0.1274 0.109 Uiso 1 1 calc R . .
C7 C 0.8162(4) -0.1301(4) 0.12233(12) 0.0356(12) Uani 1 1 d . . .
H7 H 0.8948 -0.1407 0.1236 0.043 Uiso 1 1 calc R . .
C8 C 0.8329(4) -0.0268(5) 0.15494(12) 0.0355(12) Uani 1 1 d . . .
C9 C 0.2010(11) -0.2010(11) 0.0833 0.137(3) Uani 0.50 2 d SPDU A 1
H9 H 0.2757 -0.1894 0.1001 0.164 Uiso 0.50 1 d PR A 1
C10 C 0.2518(10) -0.0897(10) 0.0553(4) 0.137(3) Uani 0.50 1 d PDU A 1
H10A H 0.2248 -0.0254 0.0623 0.164 Uiso 0.50 1 calc PR A 1
H10B H 0.2286 -0.1179 0.0274 0.164 Uiso 0.50 1 calc PR A 1
C11 C 0.3980(4) -0.0399(5) 0.06450(16) 0.098(2) Uani 0.50 1 d PDU A 1
C9' C 0.1254(8) -0.1254(8) 0.0833 0.137(3) Uani 0.50 2 d SPD A 2
H9' H 0.0489 -0.1449 0.0669 0.164 Uiso 0.50 1 d PR A 2
C10' C 0.2424(8) -0.1124(12) 0.0585(4) 0.137(3) Uani 0.50 1 d PDU A 2
H10C H 0.2324 -0.0784 0.0327 0.164 Uiso 0.50 1 calc PR A 2
H10D H 0.2183 -0.2041 0.0533 0.164 Uiso 0.50 1 calc PR A 2
C11' C 0.3980(4) -0.0399(5) 0.06450(16) 0.098(2) Uani 0.50 1 d PD A 2
C12 C 0.4643(5) 0.0578(6) 0.09140(18) 0.106(3) Uani 1 1 d DU . .
H12 H 0.4190 0.0896 0.1068 0.127 Uiso 1 1 calc R A 1
C13 C 0.6018(5) 0.1121(6) 0.09637(16) 0.087(2) Uani 1 1 d DU A .
H13 H 0.6478 0.1796 0.1151 0.105 Uiso 1 1 calc R . .
C14 C 0.5999(4) -0.0317(6) 0.04703(16) 0.081(2) Uani 1 1 d DU A .
H14 H 0.6457 -0.0623 0.0314 0.097 Uiso 1 1 calc R . .
C15 C 0.4658(5) -0.0877(6) 0.04205(18) 0.100(3) Uani 1 1 d DU . .
H15 H 0.4205 -0.1571 0.0238 0.120 Uiso 1 1 calc R A 1


_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
Co1 O2 2.049(3) 10_665 ?
Co1 O2 2.049(3) . ?
Co1 O1 2.113(3) 10_665 ?
Co1 O1 2.113(3) . ?
Co1 N1 2.128(4) . ?
Co1 N1 2.128(4) 10_665 ?
O1 C7 1.425(5) . ?
O1 H1O 0.849(17) . ?
O2 C8 1.240(6) . ?
O3 C8 1.247(5) . ?
N1 C14 1.336(6) . ?
N1 C13 1.359(7) . ?
C1 C2 1.363(10) . ?
C1 C6 1.383(10) . ?
C1 C7 1.492(6) . ?
C2 C3 1.422(8) . ?
C2 H2 0.9300 . ?
C3 C4 1.266(12) . ?
C3 H3 0.9300 . ?
C4 C5 1.344(14) . ?
C4 H4 0.9300 . ?
C5 C6 1.471(10) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C7 C8 1.550(6) . ?
C7 H7 0.9800 . ?
C9 C10 1.454(13) . ?
C9 C10 1.454(13) 10 ?
C9 H9 0.9786 . ?
C10 C11 1.524(11) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 C12 1.340(7) . ?
C11 C15 1.384(8) . ?
C9' C10' 1.528(13) . ?
C9' C10' 1.528(13) 10 ?
C9' H9' 0.9658 . ?
C10' H10C 0.9700 . ?
C10' H10D 0.9700 . ?
C12 C13 1.401(7) . ?
C12 H12 0.9300 . ?
C13 H13 0.9300 . ?
C14 C15 1.363(6) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?

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
O2 Co1 O2 167.1(2) 10_665 . ?
O2 Co1 O1 77.28(12) 10_665 10_665 ?
O2 Co1 O1 93.55(12) . 10_665 ?
O2 Co1 O1 93.55(12) 10_665 . ?
O2 Co1 O1 77.28(12) . . ?
O1 Co1 O1 90.79(18) 10_665 . ?
O2 Co1 N1 93.91(14) 10_665 . ?
O2 Co1 N1 94.77(15) . . ?
O1 Co1 N1 170.89(14) 10_665 . ?
O1 Co1 N1 87.45(16) . . ?
O2 Co1 N1 94.77(15) 10_665 10_665 ?
O2 Co1 N1 93.91(14) . 10_665 ?
O1 Co1 N1 87.45(16) 10_665 10_665 ?
O1 Co1 N1 170.90(14) . 10_665 ?
N1 Co1 N1 95.7(3) . 10_665 ?
C7 O1 Co1 115.6(2) . . ?
C7 O1 H1O 107.6(19) . . ?
Co1 O1 H1O 129.2(15) . . ?
C8 O2 Co1 119.2(3) . . ?
C14 N1 C13 119.3(4) . . ?
C14 N1 Co1 118.0(4) . . ?
C13 N1 Co1 122.4(3) . . ?
C2 C1 C6 118.6(6) . . ?
C2 C1 C7 122.8(5) . . ?
C6 C1 C7 118.5(6) . . ?
C1 C2 C3 120.5(8) . . ?
C1 C2 H2 119.7 . . ?
C3 C2 H2 119.7 . . ?
C4 C3 C2 119.9(9) . . ?
C4 C3 H3 120.1 . . ?
C2 C3 H3 120.1 . . ?
C3 C4 C5 125.3(7) . . ?
C3 C4 H4 117.4 . . ?
C5 C4 H4 117.4 . . ?
C4 C5 C6 116.5(8) . . ?
C4 C5 H5 121.7 . . ?
C6 C5 H5 121.7 . . ?
C1 C6 C5 119.2(9) . . ?
C1 C6 H6 120.4 . . ?
C5 C6 H6 120.4 . . ?
O1 C7 C1 112.2(3) . . ?
O1 C7 C8 108.1(4) . . ?
C1 C7 C8 113.8(4) . . ?
O1 C7 H7 107.5 . . ?
C1 C7 H7 107.5 . . ?
C8 C7 H7 107.5 . . ?
O2 C8 O3 126.7(4) . . ?
O2 C8 C7 118.6(4) . . ?
O3 C8 C7 114.7(4) . . ?
C10 C9 C10 130.6(18) . 10 ?
C10 C9 H9 107.5 . . ?
C10 C9 H9 103.8 10 . ?
C9 C10 C11 95.0(9) . . ?
C9 C10 H10A 112.7 . . ?
C11 C10 H10A 112.7 . . ?
C9 C10 H10B 112.7 . . ?
C11 C10 H10B 112.7 . . ?
H10A C10 H10B 110.2 . . ?
C12 C11 C15 119.6(4) . . ?
C12 C11 C10 120.9(6) . . ?
C15 C11 C10 119.2(6) . . ?
C10' C9' C10' 93.7(14) . 10 ?
C10' C9' H9' 112.8 . . ?
C10' C9' H9' 115.1 10 . ?
C9' C10' H10C 103.4 . . ?
C9' C10' H10D 103.4 . . ?
H10C C10' H10D 105.2 . . ?
C11 C12 C13 120.1(5) . . ?
C11 C12 H12 120.0 . . ?
C13 C12 H12 120.0 . . ?
N1 C13 C12 119.8(5) . . ?
N1 C13 H13 120.1 . . ?
C12 C13 H13 120.1 . . ?
N1 C14 C15 122.1(5) . . ?
N1 C14 H14 118.9 . . ?
C15 C14 H14 118.9 . . ?
C14 C15 C11 119.1(5) . . ?
C14 C15 H15 120.5 . . ?
C11 C15 H15 120.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1O O3 0.849(17) 1.803(18) 2.632(4) 165(2) 6_544

_diffrn_measured_fraction_theta_max 0.913
_diffrn_reflns_theta_full        27.49
_diffrn_measured_fraction_theta_full 0.913
_refine_diff_density_max         0.938
_refine_diff_density_min         -0.478
_refine_diff_density_rms         0.094

#=================================================END

data_complex5S
_database_code_depnum_ccdc_archive 'CCDC 704868'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C29 H28 Co N2 O6'
_chemical_formula_weight         559.46

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           hexagonal
_symmetry_space_group_name_H-M   P6122
_chemical_absolute_configuration S

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z+1/3'
'-x+y, -x, z+2/3'
'-x, -y, z+1/2'
'y, -x+y, z+5/6'
'x-y, x, z+1/6'
'y, x, -z+1/3'
'x-y, -y, -z'
'-x, -x+y, -z+2/3'
'-y, -x, -z+5/6'
'-x+y, y, -z+1/2'
'x, x-y, -z+1/6'

_cell_length_a                   11.5834(17)
_cell_length_b                   11.5834(17)
_cell_length_c                   33.052(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     3840.7(14)
_cell_formula_units_Z            6
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2359
_cell_measurement_theta_min      2.03
_cell_measurement_theta_max      25.99

_exptl_crystal_description       block
_exptl_crystal_colour            purple
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.451
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1746
_exptl_absorpt_coefficient_mu    0.718
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7872
_exptl_absorpt_correction_T_max  0.9317
_exptl_absorpt_process_details   'SADABS (Bruker, 2002)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(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 SMART CCD area detector'
_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            6403
_diffrn_reflns_av_R_equivalents  0.0609
_diffrn_reflns_av_sigmaI/netI    0.1124
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       3
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_theta_min         2.03
_diffrn_reflns_theta_max         25.99
_reflns_number_total             2359
_reflns_number_gt                1534
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART (Bruker, 1998)'
_computing_cell_refinement       'Bruker SMART (Bruker, 1998)'
_computing_data_reduction        'Bruker SAINT + & SHELXTL (Bruker, 1998)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_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)+(0.0000P)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    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(4)
_refine_ls_number_reflns         2359
_refine_ls_number_parameters     245
_refine_ls_number_restraints     49
_refine_ls_R_factor_all          0.1003
_refine_ls_R_factor_gt           0.0537
_refine_ls_wR_factor_ref         0.1282
_refine_ls_wR_factor_gt          0.1102
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_restrained_S_all      1.073
_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
Co1 Co 0.25624(8) 0.12812(4) 0.0833 0.0515(3) Uani 1 2 d S . .
O1 O 0.1081(3) -0.0636(3) 0.19050(11) 0.0636(10) Uani 1 1 d . . .
O2 O 0.2331(3) 0.0826(3) 0.14354(10) 0.0523(9) Uani 1 1 d . . .
O3 O 0.1084(3) -0.0762(3) 0.08357(12) 0.0522(8) Uani 1 1 d D . .
H3O H 0.049(4) -0.110(5) 0.0654(12) 0.074(19) Uiso 1 1 d D . .
C1 C 0.1392(5) -0.0287(5) 0.15494(16) 0.0452(11) Uani 1 1 d . . .
C2 C 0.0526(4) -0.1301(4) 0.12227(15) 0.0452(12) Uani 1 1 d . . .
H2 H -0.0372 -0.1417 0.1236 0.054 Uiso 1 1 calc R . .
C3 C 0.0414(5) -0.2650(5) 0.12797(15) 0.0547(14) Uani 1 1 d D . .
C4 C -0.0807(6) -0.3785(5) 0.1307(2) 0.085(2) Uani 1 1 d DU . .
H4 H -0.1580 -0.3728 0.1297 0.102 Uiso 1 1 calc R . .
C5 C -0.0895(9) -0.5023(6) 0.1350(2) 0.118(3) Uani 1 1 d DU . .
H5 H -0.1724 -0.5794 0.1367 0.141 Uiso 1 1 calc R . .
C6 C 0.0213(12) -0.5096(8) 0.1367(3) 0.126(3) Uani 1 1 d DU . .
H6 H 0.0147 -0.5926 0.1396 0.152 Uiso 1 1 calc R . .
C7 C 0.1434(9) -0.3995(9) 0.1343(2) 0.120(3) Uani 1 1 d DU . .
H7 H 0.2197 -0.4068 0.1358 0.144 Uiso 1 1 calc R . .
C8 C 0.1540(6) -0.2751(6) 0.1296(2) 0.087(2) Uani 1 1 d DU . .
H8 H 0.2375 -0.1989 0.1276 0.104 Uiso 1 1 calc R . .
N1 N 0.3955(19) 0.0437(15) 0.0735(7) 0.042(4) Uani 0.50 1 d P . 1
C9 C 0.355(2) -0.056(2) 0.0453(8) 0.056(5) Uani 0.50 1 d P . 1
H9 H 0.2765 -0.0839 0.0308 0.067 Uiso 0.50 1 calc PR . 1
C10 C 0.4300(14) -0.1151(14) 0.0389(5) 0.056(4) Uani 0.50 1 d P . 1
H10 H 0.4025 -0.1830 0.0199 0.068 Uiso 0.50 1 calc PR . 1
C11 C 0.5490(15) -0.0740(13) 0.0606(5) 0.045(4) Uani 0.50 1 d P . 1
C12 C 0.577(2) 0.023(2) 0.0877(7) 0.052(6) Uani 0.50 1 d P . 1
H12 H 0.6516 0.0514 0.1040 0.062 Uiso 0.50 1 calc PR . 1
C13 C 0.507(2) 0.0808(15) 0.0927(5) 0.052(4) Uani 0.50 1 d P . 1
H13 H 0.5368 0.1515 0.1108 0.063 Uiso 0.50 1 calc PR . 1
C14 C 0.6356(12) -0.1359(13) 0.0497(4) 0.060(3) Uani 0.50 1 d P . 1
H14A H 0.5775 -0.2264 0.0404 0.072 Uiso 0.50 1 calc PR . 1
H14B H 0.6930 -0.0861 0.0272 0.072 Uiso 0.50 1 calc PR . 1
C15 C 0.7214(14) -0.1393(7) 0.0833 0.060(4) Uani 0.50 2 d SP . 1
H15 H 0.7779 -0.0467 0.0933 0.072 Uiso 0.50 1 d PR . 1
N1' N 0.4020(19) 0.0964(14) 0.0741(6) 0.046(4) Uani 0.50 1 d P . 2
C9' C 0.390(2) -0.003(2) 0.0528(7) 0.055(5) Uani 0.50 1 d P . 2
H9' H 0.3099 -0.0493 0.0390 0.066 Uiso 0.50 1 calc PR . 2
C10' C 0.4757(17) -0.0508(15) 0.0472(5) 0.063(4) Uani 0.50 1 d P . 2
H10' H 0.4582 -0.1163 0.0280 0.075 Uiso 0.50 1 calc PR . 2
C11' C 0.589(2) 0.001(2) 0.0711(6) 0.042(5) Uani 0.50 1 d P . 2
C12' C 0.6077(15) 0.0976(14) 0.0969(5) 0.055(4) Uani 0.50 1 d P . 2
H12' H 0.6826 0.1363 0.1134 0.066 Uiso 0.50 1 calc PR . 2
C13' C 0.5116(17) 0.1414(15) 0.0990(5) 0.061(5) Uani 0.50 1 d P . 2
H13' H 0.5243 0.2044 0.1186 0.073 Uiso 0.50 1 calc PR . 2
C14' C 0.6772(12) -0.0610(11) 0.0701(5) 0.072(4) Uani 0.50 1 d P . 2
H14C H 0.7106 -0.0571 0.0429 0.086 Uiso 0.50 1 calc PR . 2
H14D H 0.7528 -0.0132 0.0880 0.086 Uiso 0.50 1 calc PR . 2
C15' C 0.5952(18) -0.2024(9) 0.0833 0.100(6) Uani 0.50 2 d SP . 2
H15' H 0.5389 -0.2540 0.0609 0.120 Uiso 0.50 1 d PR . 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
Co1 N1' 1.924(16) 12 ?
Co1 N1' 1.924(16) . ?
Co1 O2 2.042(3) 12 ?
Co1 O2 2.042(3) . ?
Co1 O3 2.117(3) 12 ?
Co1 O3 2.117(3) . ?
Co1 N1 2.290(14) 12 ?
Co1 N1 2.290(14) . ?
O1 C1 1.237(6) . ?
O2 C1 1.260(5) . ?
O3 C2 1.429(5) . ?
O3 H3O 0.85(2) . ?
C1 C2 1.541(6) . ?
C2 C3 1.514(6) . ?
C2 H2 0.9800 . ?
C3 C8 1.368(7) . ?
C3 C4 1.370(7) . ?
C4 C5 1.394(8) . ?
C4 H4 0.9300 . ?
C5 C6 1.329(10) . ?
C5 H5 0.9300 . ?
C6 C7 1.353(11) . ?
C6 H6 0.9300 . ?
C7 C8 1.393(8) . ?
C7 H7 0.9300 . ?
C8 H8 0.9300 . ?
N1 C13 1.30(2) . ?
N1 C9 1.37(2) . ?
C9 C10 1.36(3) . ?
C9 H9 0.9300 . ?
C10 C11 1.41(2) . ?
C10 H10 0.9300 . ?
C11 C12 1.35(2) . ?
C11 C14 1.540(18) . ?
C12 C13 1.29(2) . ?
C12 H12 0.9300 . ?
C13 H13 0.9300 . ?
C14 C15 1.505(14) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 C14 1.505(14) 12_545 ?
C15 H15 0.9924 . ?
N1' C9' 1.29(2) . ?
N1' C13' 1.38(2) . ?
C9' C10' 1.37(3) . ?
C9' H9' 0.9300 . ?
C10' C11' 1.39(3) . ?
C10' H10' 0.9300 . ?
C11' C12' 1.33(2) . ?
C11' C14' 1.51(2) . ?
C12' C13' 1.44(2) . ?
C12' H12' 0.9300 . ?
C13' H13' 0.9300 . ?
C14' C15' 1.490(14) . ?
C14' H14C 0.9700 . ?
C14' H14D 0.9700 . ?
C15' C14' 1.490(14) 12_545 ?
C15' H15' 0.9705 . ?

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' Co1 N1' 81.0(10) 12 . ?
N1' Co1 O2 96.9(6) 12 12 ?
N1' Co1 O2 93.0(6) . 12 ?
N1' Co1 O2 93.0(6) 12 . ?
N1' Co1 O2 96.9(6) . . ?
O2 Co1 O2 166.94(17) 12 . ?
N1' Co1 O3 94.8(5) 12 12 ?
N1' Co1 O3 169.0(5) . 12 ?
O2 Co1 O3 77.26(14) 12 12 ?
O2 Co1 O3 93.51(14) . 12 ?
N1' Co1 O3 169.0(5) 12 . ?
N1' Co1 O3 94.8(5) . . ?
O2 Co1 O3 93.51(14) 12 . ?
O2 Co1 O3 77.26(14) . . ?
O3 Co1 O3 91.05(17) 12 . ?
N1' Co1 N1 12.2(8) 12 12 ?
N1' Co1 N1 92.8(5) . 12 ?
O2 Co1 N1 93.3(5) 12 12 ?
O2 Co1 N1 94.7(6) . 12 ?
O3 Co1 N1 82.6(4) 12 12 ?
O3 Co1 N1 169.5(6) . 12 ?
N1' Co1 N1 92.8(5) 12 . ?
N1' Co1 N1 12.2(8) . . ?
O2 Co1 N1 94.7(6) 12 . ?
O2 Co1 N1 93.3(5) . . ?
O3 Co1 N1 169.5(6) 12 . ?
O3 Co1 N1 82.6(5) . . ?
N1 Co1 N1 104.8(9) 12 . ?
C1 O2 Co1 119.4(3) . . ?
C2 O3 Co1 115.4(3) . . ?
C2 O3 H3O 110(4) . . ?
Co1 O3 H3O 122(3) . . ?
O1 C1 O2 125.5(5) . . ?
O1 C1 C2 116.4(4) . . ?
O2 C1 C2 118.1(5) . . ?
O3 C2 C3 110.4(4) . . ?
O3 C2 C1 108.3(4) . . ?
C3 C2 C1 112.7(4) . . ?
O3 C2 H2 108.4 . . ?
C3 C2 H2 108.4 . . ?
C1 C2 H2 108.4 . . ?
C8 C3 C4 119.1(4) . . ?
C8 C3 C2 120.0(5) . . ?
C4 C3 C2 120.9(5) . . ?
C3 C4 C5 120.2(5) . . ?
C3 C4 H4 119.9 . . ?
C5 C4 H4 119.9 . . ?
C6 C5 C4 119.6(6) . . ?
C6 C5 H5 120.2 . . ?
C4 C5 H5 120.2 . . ?
C5 C6 C7 121.7(6) . . ?
C5 C6 H6 119.2 . . ?
C7 C6 H6 119.2 . . ?
C6 C7 C8 119.4(6) . . ?
C6 C7 H7 120.3 . . ?
C8 C7 H7 120.3 . . ?
C3 C8 C7 119.9(6) . . ?
C3 C8 H8 120.1 . . ?
C7 C8 H8 120.1 . . ?
C13 N1 C9 118.4(16) . . ?
C13 N1 Co1 125.6(13) . . ?
C9 N1 Co1 115.9(16) . . ?
C10 C9 N1 119.4(17) . . ?
C10 C9 H9 120.3 . . ?
N1 C9 H9 120.3 . . ?
C9 C10 C11 120.8(12) . . ?
C9 C10 H10 119.6 . . ?
C11 C10 H10 119.6 . . ?
C12 C11 C10 113.9(16) . . ?
C12 C11 C14 127.5(16) . . ?
C10 C11 C14 118.5(12) . . ?
C13 C12 C11 125(2) . . ?
C13 C12 H12 117.7 . . ?
C11 C12 H12 117.7 . . ?
C12 C13 N1 122.7(16) . . ?
C12 C13 H13 118.6 . . ?
N1 C13 H13 118.6 . . ?
C15 C14 C11 115.5(10) . . ?
C15 C14 H14A 108.4 . . ?
C11 C14 H14A 108.4 . . ?
C15 C14 H14B 108.4 . . ?
C11 C14 H14B 108.4 . . ?
H14A C14 H14B 107.5 . . ?
C14 C15 C14 110.3(13) . 12_545 ?
C14 C15 H15 107.7 . . ?
C14 C15 H15 110.5 12_545 . ?
C9' N1' C13' 109.2(14) . . ?
C9' N1' Co1 122.9(16) . . ?
C13' N1' Co1 124.3(14) . . ?
N1' C9' C10' 131.2(17) . . ?
N1' C9' H9' 114.4 . . ?
C10' C9' H9' 114.4 . . ?
C9' C10' C11' 117.7(14) . . ?
C9' C10' H10' 121.1 . . ?
C11' C10' H10' 121.1 . . ?
C12' C11' C10' 116.6(19) . . ?
C12' C11' C14' 123(2) . . ?
C10' C11' C14' 119.8(18) . . ?
C11' C12' C13' 119.9(16) . . ?
C11' C12' H12' 120.0 . . ?
C13' C12' H12' 120.0 . . ?
N1' C13' C12' 124.5(13) . . ?
N1' C13' H13' 117.8 . . ?
C12' C13' H13' 117.8 . . ?
C15' C14' C11' 107.8(12) . . ?
C15' C14' H14C 110.1 . . ?
C11' C14' H14C 110.1 . . ?
H15 C14' H14C 103.0 . . ?
C15' C14' H14D 110.1 . . ?
C11' C14' H14D 110.1 . . ?
H14C C14' H14D 108.5 . . ?
C14' C15' C14' 113.0(15) 12_545 . ?
C14' C15' H15' 109.1 12_545 . ?
C14' C15' H15' 108.4 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O3 H3O O1 0.85(2) 1.78(2) 2.625(5) 174(5) 5_554

_diffrn_measured_fraction_theta_max 0.921
_diffrn_reflns_theta_full        25.99
_diffrn_measured_fraction_theta_full 0.921
_refine_diff_density_max         0.254
_refine_diff_density_min         -0.302
_refine_diff_density_rms         0.045

#=================================================END

data_complex6R
_database_code_depnum_ccdc_archive 'CCDC 704869'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C29 H28 N2 Ni O6'
_chemical_formula_sum            'C29 H28 N2 Ni O6'
_chemical_formula_weight         559.24

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'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_H-M   P6522
_chemical_absolute_configuration R

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z+2/3'
'-x+y, -x, z+1/3'
'-x, -y, z+1/2'
'y, -x+y, z+1/6'
'x-y, x, z+5/6'
'y, x, -z+2/3'
'x-y, -y, -z'
'-x, -x+y, -z+1/3'
'-y, -x, -z+1/6'
'-x+y, y, -z+1/2'
'x, x-y, -z+5/6'

_cell_length_a                   11.5175(8)
_cell_length_b                   11.5175(8)
_cell_length_c                   33.162(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     3809.6(6)
_cell_formula_units_Z            6
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    2315
_cell_measurement_theta_min      2.04
_cell_measurement_theta_max      26.00

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.13
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.463
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1752
_exptl_absorpt_coefficient_mu    0.812
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8228
_exptl_absorpt_correction_T_max  0.9018
_exptl_absorpt_process_details   'SADABS (Bruker, 2002)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(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 SMART CCD area detector'
_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            9642
_diffrn_reflns_av_R_equivalents  0.0472
_diffrn_reflns_av_sigmaI/netI    0.0525
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.04
_diffrn_reflns_theta_max         26.00
_reflns_number_total             2315
_reflns_number_gt                1999
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART (Bruker, 1998)'
_computing_cell_refinement       'Bruker SMART (Bruker, 1998)'
_computing_data_reduction        'Bruker SAINT + & SHELXTL (Bruker, 1998)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_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)+(0.0750P)²+15.1311P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.04(6)
_refine_ls_number_reflns         2315
_refine_ls_number_parameters     175
_refine_ls_number_restraints     100
_refine_ls_R_factor_all          0.0956
_refine_ls_R_factor_gt           0.0854
_refine_ls_wR_factor_ref         0.2066
_refine_ls_wR_factor_gt          0.1982
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_restrained_S_all      1.189
_refine_ls_shift/su_max          0.003
_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
Ni1 Ni 0.87496(4) 0.12504(4) 0.0833 0.04403(17) Uani 1 2 d S . .
O1 O 0.8203(2) -0.0747(2) 0.08331(9) 0.0417(8) Uani 1 1 d D . .
H1O H 0.831(2) -0.1233(17) 0.0662(7) 0.027(10) Uiso 1 1 d D . .
O2 O 0.8500(3) 0.0827(2) 0.14358(9) 0.0443(8) Uani 1 1 d . . .
O3 O 0.8303(3) -0.0645(3) 0.18982(10) 0.0530(10) Uani 1 1 d . . .
N1 N 0.6737(3) 0.0644(4) 0.07463(14) 0.0744(15) Uani 1 1 d DU . .
C1 C 0.6981(5) -0.2658(4) 0.12762(14) 0.0496(15) Uani 1 1 d . . .
C2 C 0.7066(7) -0.3791(5) 0.1307(2) 0.081(2) Uani 1 1 d . . .
H2 H 0.7921 -0.3726 0.1301 0.098 Uiso 1 1 calc R . .
C3 C 0.5899(8) -0.5067(7) 0.1349(2) 0.102(3) Uani 1 1 d U . .
H3 H 0.5963 -0.5855 0.1372 0.122 Uiso 1 1 calc R . .
C4 C 0.4742(7) -0.5132(7) 0.1354(2) 0.095(3) Uani 1 1 d U . .
H4 H 0.3966 -0.5995 0.1374 0.114 Uiso 1 1 calc R . .
C5 C 0.4559(7) -0.4061(8) 0.1333(2) 0.104(3) Uani 1 1 d U . .
H5 H 0.3692 -0.4156 0.1346 0.125 Uiso 1 1 calc R . .
C6 C 0.5727(5) -0.2793(7) 0.12889(18) 0.081(2) Uani 1 1 d . . .
H6 H 0.5643 -0.2016 0.1268 0.098 Uiso 1 1 calc R . .
C7 C 0.8205(3) -0.1292(4) 0.12197(13) 0.0366(11) Uani 1 1 d . . .
H7 H 0.9013 -0.1401 0.1235 0.044 Uiso 1 1 calc R . .
C8 C 0.8347(3) -0.0285(4) 0.15468(14) 0.0368(12) Uani 1 1 d . . .
C9 C 0.1386(7) -0.1386(7) 0.0833 0.0952(19) Uani 0.50 2 d SPDU A 1
H9 H 0.0531 -0.1689 0.0712 0.114 Uiso 0.50 1 d PR A 1
C10 C 0.2500(8) -0.1179(10) 0.0581(3) 0.0952(19) Uani 0.50 1 d PDU A 1
H10A H 0.2378 -0.0800 0.0327 0.114 Uiso 0.50 1 calc PR A 1
H10B H 0.2313 -0.2093 0.0512 0.114 Uiso 0.50 1 calc PR A 1
C11 C 0.4020(4) -0.0379(5) 0.06614(16) 0.099(2) Uani 0.50 1 d PDU A 1
C9' C 0.2060(7) -0.2060(7) 0.0833 0.0952(19) Uani 0.50 2 d SPD A 2
H9' H 0.2598 -0.1963 0.1049 0.114 Uiso 0.50 1 d PR A 2
C10' C 0.2540(9) -0.0737(9) 0.0611(4) 0.0952(19) Uani 0.50 1 d PDU A 2
H10C H 0.2324 -0.0112 0.0753 0.114 Uiso 0.50 1 calc PR A 2
H10D H 0.2244 -0.0852 0.0326 0.114 Uiso 0.50 1 calc PR A 2
C11' C 0.4020(4) -0.0379(5) 0.06614(16) 0.099(2) Uani 0.50 1 d PD A 2
C12 C 0.4710(4) 0.0591(6) 0.09336(19) 0.107(2) Uani 1 1 d DU . .
H12 H 0.4262 0.0933 0.1093 0.128 Uiso 1 1 calc R A 1
C13 C 0.6085(4) 0.1096(6) 0.09826(18) 0.090(2) Uani 1 1 d DU A .
H13 H 0.6565 0.1758 0.1182 0.108 Uiso 1 1 calc R . .
C14 C 0.6045(4) -0.0319(6) 0.04775(17) 0.0768(19) Uani 1 1 d DU A .
H14 H 0.6496 -0.0663 0.0321 0.092 Uiso 1 1 calc R . .
C15 C 0.4696(4) -0.0824(6) 0.04215(17) 0.096(2) Uani 1 1 d DU . .
H15 H 0.4231 -0.1477 0.0219 0.115 Uiso 1 1 calc R A 1


_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
Ni1 O2 2.043(3) 10_665 ?
Ni1 O2 2.043(3) . ?
Ni1 O1 2.059(3) . ?
Ni1 O1 2.059(3) 10_665 ?
Ni1 N1 2.080(4) . ?
Ni1 N1 2.080(4) 10_665 ?
O1 C7 1.428(5) . ?
O1 H1O 0.849(17) . ?
O2 C8 1.258(5) . ?
O3 C8 1.229(5) . ?
N1 C14 1.332(6) . ?
N1 C13 1.356(7) . ?
C1 C2 1.359(9) . ?
C1 C6 1.374(9) . ?
C1 C7 1.510(5) . ?
C2 C3 1.418(8) . ?
C2 H2 0.9500 . ?
C3 C4 1.297(12) . ?
C3 H3 0.9500 . ?
C4 C5 1.353(13) . ?
C4 H4 0.9500 . ?
C5 C6 1.414(9) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C8 1.536(6) . ?
C7 H7 1.0000 . ?
C9 C10 1.449(12) . ?
C9 C10 1.449(12) 10 ?
C9 H9 0.9540 . ?
C10 C11 1.540(9) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.344(7) . ?
C11 C15 1.379(7) . ?
C9' C10' 1.526(12) . ?
C9' C10' 1.526(12) 10 ?
C9' H9' 0.9152 . ?
C10' H10C 0.9900 . ?
C10' H10D 0.9900 . ?
C12 C13 1.397(6) . ?
C12 H12 0.9500 . ?
C13 H13 0.9500 . ?
C14 C15 1.372(6) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Ni1 O2 170.28(18) 10_665 . ?
O2 Ni1 O1 94.31(12) 10_665 . ?
O2 Ni1 O1 78.80(11) . . ?
O2 Ni1 O1 78.80(11) 10_665 10_665 ?
O2 Ni1 O1 94.31(12) . 10_665 ?
O1 Ni1 O1 90.68(15) . 10_665 ?
O2 Ni1 N1 93.39(15) 10_665 . ?
O2 Ni1 N1 93.16(15) . . ?
O1 Ni1 N1 87.59(15) . . ?
O1 Ni1 N1 171.86(15) 10_665 . ?
O2 Ni1 N1 93.16(15) 10_665 10_665 ?
O2 Ni1 N1 93.39(15) . 10_665 ?
O1 Ni1 N1 171.86(15) . 10_665 ?
O1 Ni1 N1 87.59(15) 10_665 10_665 ?
N1 Ni1 N1 95.2(3) . 10_665 ?
C7 O1 Ni1 115.1(2) . . ?
C7 O1 H1O 105.9(18) . . ?
Ni1 O1 H1O 132.4(14) . . ?
C8 O2 Ni1 117.4(3) . . ?
C14 N1 C13 119.4(4) . . ?
C14 N1 Ni1 118.3(4) . . ?
C13 N1 Ni1 121.9(3) . . ?
C2 C1 C6 117.7(5) . . ?
C2 C1 C7 122.1(5) . . ?
C6 C1 C7 120.2(5) . . ?
C1 C2 C3 121.1(7) . . ?
C1 C2 H2 119.5 . . ?
C3 C2 H2 119.5 . . ?
C4 C3 C2 118.4(8) . . ?
C4 C3 H3 120.8 . . ?
C2 C3 H3 120.8 . . ?
C3 C4 C5 124.7(6) . . ?
C3 C4 H4 117.6 . . ?
C5 C4 H4 117.6 . . ?
C4 C5 C6 116.5(8) . . ?
C4 C5 H5 121.8 . . ?
C6 C5 H5 121.8 . . ?
C1 C6 C5 121.6(8) . . ?
C1 C6 H6 119.2 . . ?
C5 C6 H6 119.2 . . ?
O1 C7 C1 111.3(3) . . ?
O1 C7 C8 108.9(3) . . ?
C1 C7 C8 113.0(3) . . ?
O1 C7 H7 107.8 . . ?
C1 C7 H7 107.8 . . ?
C8 C7 H7 107.8 . . ?
O3 C8 O2 125.6(4) . . ?
O3 C8 C7 116.3(4) . . ?
O2 C8 C7 118.1(4) . . ?
C10 C9 C10 102.7(13) . 10 ?
C10 C9 H9 118.9 . . ?
C10 C9 H9 103.8 10 . ?
C9 C10 C11 130.3(8) . . ?
C9 C10 H10A 104.7 . . ?
C11 C10 H10A 104.7 . . ?
C9 C10 H10B 104.7 . . ?
C11 C10 H10B 104.7 . . ?
H10A C10 H10B 105.7 . . ?
C12 C11 C15 119.2(4) . . ?
C12 C11 C10 129.5(6) . . ?
C15 C11 C10 111.2(5) . . ?
C10' C9' C10' 113.2(12) . 10 ?
C10' C9' H9' 111.7 . . ?
C10' C9' H9' 99.2 10 . ?
C9' C10' H10C 113.5 . . ?
C9' C10' H10D 113.5 . . ?
H10C C10' H10D 110.8 . . ?
C11 C12 C13 120.0(5) . . ?
C11 C12 H12 120.0 . . ?
C13 C12 H12 120.0 . . ?
N1 C13 C12 120.2(5) . . ?
N1 C13 H13 119.9 . . ?
C12 C13 H13 119.9 . . ?
N1 C14 C15 121.5(5) . . ?
N1 C14 H14 119.2 . . ?
C15 C14 H14 119.2 . . ?
C14 C15 C11 119.6(5) . . ?
C14 C15 H15 120.2 . . ?
C11 C15 H15 120.2 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1O O3 0.849(17) 1.804(19) 2.618(4) 160.0(19) 6_544

_diffrn_measured_fraction_theta_max 0.905
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.905
_refine_diff_density_max         0.803
_refine_diff_density_min         -0.704
_refine_diff_density_rms         0.089

#=================================================END

data_complex6S
_database_code_depnum_ccdc_archive 'CCDC 704870'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C29 H28 N2 Ni O6'
_chemical_formula_weight         559.24

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_H-M   P6122
_chemical_absolute_configuration S

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z+1/3'
'-x+y, -x, z+2/3'
'-x, -y, z+1/2'
'y, -x+y, z+5/6'
'x-y, x, z+1/6'
'y, x, -z+1/3'
'x-y, -y, -z'
'-x, -x+y, -z+2/3'
'-y, -x, -z+5/6'
'-x+y, y, -z+1/2'
'x, x-y, -z+1/6'

_cell_length_a                   11.4711(1)
_cell_length_b                   11.4711(1)
_cell_length_c                   33.0791(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     3769.59(7)
_cell_formula_units_Z            6
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.478
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1752
_exptl_absorpt_coefficient_mu    1.521
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8385
_exptl_absorpt_correction_T_max  0.8880
_exptl_absorpt_process_details   
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET)
(compiled Jun 10 2008,16:49:55)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'Ultra (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'Gemini S Ultra'
_diffrn_measurement_method       'ω and π scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            9433
_diffrn_reflns_av_R_equivalents  0.0296
_diffrn_reflns_av_sigmaI/netI    0.0508
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_theta_min         4.45
_diffrn_reflns_theta_max         59.93
_reflns_number_total             1814
_reflns_number_gt                1343
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
(compiled Oct 18 2006,16:28:17)
;
_computing_cell_refinement       
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
(compiled Oct 18 2006,16:28:17)
;
_computing_data_reduction        
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
(compiled Oct 18 2006,16:28:17)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement of 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)+(0.0389P)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    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.01(6)
_refine_ls_number_reflns         1814
_refine_ls_number_parameters     245
_refine_ls_number_restraints     61
_refine_ls_R_factor_all          0.0456
_refine_ls_R_factor_gt           0.0323
_refine_ls_wR_factor_ref         0.0649
_refine_ls_wR_factor_gt          0.0629
_refine_ls_goodness_of_fit_ref   0.926
_refine_ls_restrained_S_all      1.126
_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
Ni1 Ni 0.24867(8) 0.12434(4) 0.0833 0.0359(3) Uani 1 2 d S . .
O1 O 0.1019(2) -0.0674(2) 0.19010(6) 0.0330(6) Uani 1 1 d . . .
O2 O 0.2316(2) 0.0823(2) 0.14344(6) 0.0317(6) Uani 1 1 d . . .
O3 O 0.1045(2) -0.0758(2) 0.08297(6) 0.0298(6) Uani 1 1 d D . .
H3O H 0.046(3) -0.110(3) 0.0644(8) 0.052(13) Uiso 1 1 d D . .
C1 C 0.1358(4) -0.0291(4) 0.15437(10) 0.0258(9) Uani 1 1 d . . .
C2 C 0.0469(3) -0.1315(3) 0.12179(8) 0.0275(9) Uani 1 1 d . . .
H2 H -0.0448 -0.1417 0.1231 0.033 Uiso 1 1 calc R . .
C3 C 0.0327(4) -0.2689(4) 0.12755(9) 0.0344(10) Uani 1 1 d D . .
C4 C -0.0911(5) -0.3810(4) 0.13086(12) 0.0595(13) Uani 1 1 d DU . .
H4 H -0.1696 -0.3730 0.1302 0.071 Uiso 1 1 calc R . .
C5 C -0.1029(6) -0.5089(5) 0.13528(14) 0.0816(16) Uani 1 1 d DU . .
H5 H -0.1893 -0.5869 0.1377 0.098 Uiso 1 1 calc R . .
C6 C 0.0062(7) -0.5200(5) 0.13603(12) 0.0760(16) Uani 1 1 d DU . .
H6 H -0.0028 -0.6065 0.1388 0.091 Uiso 1 1 calc R . .
C7 C 0.1293(6) -0.4118(6) 0.13296(12) 0.0749(15) Uani 1 1 d DU . .
H7 H 0.2064 -0.4222 0.1339 0.090 Uiso 1 1 calc R . .
C8 C 0.1451(5) -0.2828(4) 0.12843(11) 0.0545(12) Uani 1 1 d DU . .
H8 H 0.2324 -0.2061 0.1260 0.065 Uiso 1 1 calc R . .
N1 N 0.3773(16) 0.0359(12) 0.0733(6) 0.025(4) Uani 0.50 1 d P . 1
C9 C 0.3497(13) -0.0626(11) 0.0463(3) 0.025(3) Uani 0.50 1 d P . 1
H9 H 0.2685 -0.0958 0.0314 0.030 Uiso 0.50 1 calc PR . 1
C10 C 0.4264(12) -0.1185(10) 0.0386(3) 0.028(3) Uani 0.50 1 d P . 1
H10 H 0.3994 -0.1867 0.0186 0.033 Uiso 0.50 1 calc PR . 1
C11 C 0.5459(11) -0.0758(10) 0.0601(3) 0.021(2) Uani 0.50 1 d P . 1
C12 C 0.5736(15) 0.0202(17) 0.0887(4) 0.024(4) Uani 0.50 1 d PU . 1
H12 H 0.6520 0.0512 0.1048 0.029 Uiso 0.50 1 calc PR . 1
C13 C 0.4922(14) 0.0729(10) 0.0946(3) 0.027(3) Uani 0.50 1 d P . 1
H13 H 0.5168 0.1397 0.1149 0.033 Uiso 0.50 1 calc PR . 1
C14 C 0.6349(7) -0.1328(9) 0.0489(2) 0.0293(18) Uani 0.50 1 d P . 1
H14A H 0.6957 -0.0774 0.0269 0.035 Uiso 0.50 1 calc PR . 1
H14B H 0.5773 -0.2248 0.0382 0.035 Uiso 0.50 1 calc PR . 1
C15 C 0.7208(10) -0.1396(5) 0.0833 0.032(2) Uani 0.50 2 d SP . 1
H15 H 0.7773 -0.0467 0.0933 0.038 Uiso 0.50 1 d PR . 1
N1' N 0.4019(17) 0.0982(10) 0.0768(6) 0.028(4) Uani 0.50 1 d P . 2
C9' C 0.3835(12) 0.0043(12) 0.0503(4) 0.020(3) Uani 0.50 1 d PU . 2
H9' H 0.3072 -0.0305 0.0330 0.024 Uiso 0.50 1 calc PR . 2
C10' C 0.4728(12) -0.0465(10) 0.0466(3) 0.026(2) Uani 0.50 1 d P . 2
H10' H 0.4562 -0.1145 0.0274 0.031 Uiso 0.50 1 calc PR . 2
C11' C 0.5864(13) 0.0050(16) 0.0719(4) 0.021(3) Uani 0.50 1 d P . 2
C12' C 0.6029(10) 0.1045(10) 0.0990(2) 0.028(2) Uani 0.50 1 d P . 2
H12' H 0.6793 0.1448 0.1162 0.033 Uiso 0.50 1 calc PR . 2
C13' C 0.5075(12) 0.1451(10) 0.1006(3) 0.025(3) Uani 0.50 1 d P . 2
H13' H 0.5192 0.2107 0.1202 0.030 Uiso 0.50 1 calc PR . 2
C14' C 0.6727(7) -0.0571(7) 0.0729(2) 0.0284(18) Uani 0.50 1 d P . 2
H14C H 0.7447 -0.0108 0.0933 0.034 Uiso 0.50 1 calc PR . 2
H14D H 0.7158 -0.0467 0.0462 0.034 Uiso 0.50 1 calc PR . 2
C15' C 0.5896(11) -0.2052(5) 0.0833 0.031(2) Uani 0.50 2 d SP . 2
H15' H 0.5332 -0.2540 0.0609 0.037 Uiso 0.50 1 d PR . 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
Ni1 N1' 1.937(19) . ?
Ni1 N1' 1.937(19) 12 ?
Ni1 O2 2.032(2) 12 ?
Ni1 O2 2.032(2) . ?
Ni1 O3 2.052(2) . ?
Ni1 O3 2.052(2) 12 ?
Ni1 N1 2.194(17) . ?
Ni1 N1 2.194(17) 12 ?
O1 C1 1.253(4) . ?
O2 C1 1.252(4) . ?
O3 C2 1.439(3) . ?
O3 H3O 0.845(12) . ?
C1 C2 1.544(4) . ?
C2 C3 1.514(5) . ?
C2 H2 1.0000 . ?
C3 C4 1.362(5) . ?
C3 C8 1.376(5) . ?
C4 C5 1.412(6) . ?
C4 H4 0.9500 . ?
C5 C6 1.320(6) . ?
C5 H5 0.9500 . ?
C6 C7 1.339(7) . ?
C6 H6 0.9500 . ?
C7 C8 1.405(6) . ?
C7 H7 0.9500 . ?
C8 H8 0.9500 . ?
N1 C9 1.348(16) . ?
N1 C13 1.36(2) . ?
C9 C10 1.348(18) . ?
C9 H9 0.9500 . ?
C10 C11 1.398(16) . ?
C10 H10 0.9500 . ?
C11 C12 1.363(16) . ?
C11 C14 1.507(13) . ?
C12 C13 1.36(2) . ?
C12 H12 0.9500 . ?
C13 H13 0.9500 . ?
C14 C15 1.533(8) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C14 1.533(8) 12_545 ?
C15 H15 0.9865 . ?
N1' C13' 1.31(2) . ?
N1' C9' 1.32(2) . ?
C9' C10' 1.41(2) . ?
C9' H9' 0.9500 . ?
C10' C11' 1.407(17) . ?
C10' H10' 0.9500 . ?
C11' C12' 1.386(16) . ?
C11' C14' 1.482(16) . ?
C12' C13' 1.389(16) . ?
C12' H12' 0.9500 . ?
C13' H13' 0.9500 . ?
C14' C15' 1.514(9) . ?
C14' H14C 0.9900 . ?
C14' H14D 0.9900 . ?
C15' C14' 1.514(9) 12_545 ?
C15' H15' 0.9585 . ?

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' Ni1 N1' 76.4(6) . 12 ?
N1' Ni1 O2 94.1(6) . 12 ?
N1' Ni1 O2 93.4(6) 12 12 ?
N1' Ni1 O2 93.4(6) . . ?
N1' Ni1 O2 94.1(6) 12 . ?
O2 Ni1 O2 170.40(13) 12 . ?
N1' Ni1 O3 96.4(3) . . ?
N1' Ni1 O3 170.0(5) 12 . ?
O2 Ni1 O3 94.08(9) 12 . ?
O2 Ni1 O3 79.16(9) . . ?
N1' Ni1 O3 170.0(5) . 12 ?
N1' Ni1 O3 96.4(3) 12 12 ?
O2 Ni1 O3 79.16(9) 12 12 ?
O2 Ni1 O3 94.08(9) . 12 ?
O3 Ni1 O3 91.45(12) . 12 ?
N1' Ni1 N1 16.2(5) . . ?
N1' Ni1 N1 92.6(4) 12 . ?
O2 Ni1 N1 93.0(5) 12 . ?
O2 Ni1 N1 92.6(5) . . ?
O3 Ni1 N1 80.4(3) . . ?
O3 Ni1 N1 168.3(4) 12 . ?
N1' Ni1 N1 92.6(4) . 12 ?
N1' Ni1 N1 16.2(5) 12 12 ?
O2 Ni1 N1 92.6(5) 12 12 ?
O2 Ni1 N1 93.0(5) . 12 ?
O3 Ni1 N1 168.3(4) . 12 ?
O3 Ni1 N1 80.4(3) 12 12 ?
N1 Ni1 N1 108.8(7) . 12 ?
C1 O2 Ni1 117.1(2) . . ?
C2 O3 Ni1 115.20(18) . . ?
C2 O3 H3O 111(2) . . ?
Ni1 O3 H3O 122(2) . . ?
O2 C1 O1 126.2(3) . . ?
O2 C1 C2 118.9(3) . . ?
O1 C1 C2 114.9(3) . . ?
O3 C2 C3 111.2(3) . . ?
O3 C2 C1 107.6(3) . . ?
C3 C2 C1 113.0(3) . . ?
O3 C2 H2 108.3 . . ?
C3 C2 H2 108.3 . . ?
C1 C2 H2 108.3 . . ?
C4 C3 C8 118.9(4) . . ?
C4 C3 C2 120.7(4) . . ?
C8 C3 C2 120.3(4) . . ?
C3 C4 C5 120.2(4) . . ?
C3 C4 H4 119.9 . . ?
C5 C4 H4 119.9 . . ?
C6 C5 C4 119.9(5) . . ?
C6 C5 H5 120.1 . . ?
C4 C5 H5 120.1 . . ?
C5 C6 C7 121.4(5) . . ?
C5 C6 H6 119.3 . . ?
C7 C6 H6 119.3 . . ?
C6 C7 C8 120.3(5) . . ?
C6 C7 H7 119.8 . . ?
C8 C7 H7 119.8 . . ?
C3 C8 C7 119.3(4) . . ?
C3 C8 H8 120.4 . . ?
C7 C8 H8 120.4 . . ?
C9 N1 C13 112.9(14) . . ?
C9 N1 Ni1 123.9(12) . . ?
C13 N1 Ni1 123.2(10) . . ?
C10 C9 N1 126.1(13) . . ?
C10 C9 H9 116.9 . . ?
N1 C9 H9 116.9 . . ?
C9 C10 C11 119.7(9) . . ?
C9 C10 H10 120.1 . . ?
C11 C10 H10 120.1 . . ?
C12 C11 C10 115.3(12) . . ?
C12 C11 C14 125.9(11) . . ?
C10 C11 C14 118.7(8) . . ?
C13 C12 C11 121.8(14) . . ?
C13 C12 H12 119.1 . . ?
C11 C12 H12 119.1 . . ?
C12 C13 N1 124.1(11) . . ?
C12 C13 H13 118.0 . . ?
N1 C13 H13 118.0 . . ?
C11 C14 C15 115.6(6) . . ?
C11 C14 H14A 108.4 . . ?
C15 C14 H14A 108.4 . . ?
C11 C14 H14B 108.4 . . ?
C15 C14 H14B 108.4 . . ?
H14A C14 H14B 107.4 . . ?
C14 C15 C14 112.3(8) . 12_545 ?
C14 C15 H15 106.5 . . ?
C14 C15 H15 110.5 12_545 . ?
C13' N1' C9' 118.1(16) . . ?
C13' N1' Ni1 126.3(12) . . ?
C9' N1' Ni1 114.4(13) . . ?
N1' C9' C10' 122.6(14) . . ?
N1' C9' H9' 118.7 . . ?
C10' C9' H9' 118.7 . . ?
C11' C10' C9' 119.0(10) . . ?
C11' C10' H10' 120.5 . . ?
C9' C10' H10' 120.5 . . ?
C12' C11' C10' 116.5(12) . . ?
C12' C11' C14' 122.2(11) . . ?
C10' C11' C14' 120.8(12) . . ?
C11' C12' C13' 119.7(10) . . ?
C11' C12' H12' 120.1 . . ?
C13' C12' H12' 120.1 . . ?
N1' C13' C12' 124.0(11) . . ?
N1' C13' H13' 118.0 . . ?
C12' C13' H13' 118.0 . . ?
C11' C14' C15' 110.3(8) . . ?
C11' C14' H14C 109.6 . . ?
C15' C14' H14C 109.6 . . ?
C11' C14' H14D 109.6 . . ?
C15' C14' H14D 109.6 . . ?
H14C C14' H14D 108.1 . . ?
C14' C15' C14' 113.9(9) 12_545 . ?
C14' C15' H15' 107.2 12_545 . ?
C14' C15' H15' 110.0 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O3 H3O O1 0.845(12) 1.765(13) 2.608(3) 175(4) 5_554

_diffrn_measured_fraction_theta_max 0.972
_diffrn_reflns_theta_full        59.93
_diffrn_measured_fraction_theta_full 0.972
_refine_diff_density_max         0.169
_refine_diff_density_min         -0.250
_refine_diff_density_rms         0.040

#=================================================END

data_complex7R
_database_code_depnum_ccdc_archive 'CCDC 704871'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C29 H28 N2 O6 Zn'
_chemical_formula_weight         565.90

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'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_H-M   P6522
_chemical_absolute_configuration R

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z+2/3'
'-x+y, -x, z+1/3'
'-x, -y, z+1/2'
'y, -x+y, z+1/6'
'x-y, x, z+5/6'
'y, x, -z+2/3'
'x-y, -y, -z'
'-x, -x+y, -z+1/3'
'-y, -x, -z+1/6'
'-x+y, y, -z+1/2'
'x, x-y, -z+5/6'

_cell_length_a                   11.5947(16)
_cell_length_b                   11.5947(16)
_cell_length_c                   33.068(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     3849.9(13)
_cell_formula_units_Z            6
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    2949
_cell_measurement_theta_min      2.74
_cell_measurement_theta_max      27.50

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.17
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.464
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1764
_exptl_absorpt_coefficient_mu    1.004
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7459
_exptl_absorpt_correction_T_max  0.8478
_exptl_absorpt_process_details   'SADABS (Bruker, 2002)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      123(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 SMART CCD area detector'
_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            10870
_diffrn_reflns_av_R_equivalents  0.0374
_diffrn_reflns_av_sigmaI/netI    0.0561
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_theta_min         2.74
_diffrn_reflns_theta_max         27.50
_reflns_number_total             2949
_reflns_number_gt                2066
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART (Bruker, 1998)'
_computing_cell_refinement       'Bruker SMART (Bruker, 1998)'
_computing_data_reduction        'Bruker SAINT + & SHELXTL (Bruker, 1998)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_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)+(0.0608P)²+9.2807P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(5)
_refine_ls_number_reflns         2949
_refine_ls_number_parameters     191
_refine_ls_number_restraints     114
_refine_ls_R_factor_all          0.0945
_refine_ls_R_factor_gt           0.0669
_refine_ls_wR_factor_ref         0.1716
_refine_ls_wR_factor_gt          0.1603
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_restrained_S_all      1.352
_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
Zn1 Zn 0.87057(3) 0.12943(3) 0.0833 0.04356(13) Uani 1 2 d S . .
O1 O 0.8149(2) -0.0759(2) 0.08337(7) 0.0331(6) Uani 1 1 d D . .
H1O H 0.830(2) -0.1185(19) 0.0650(6) 0.029(10) Uiso 1 1 d D . .
O2 O 0.8489(2) 0.0834(2) 0.14419(6) 0.0356(6) Uani 1 1 d . . .
O3 O 0.8290(2) -0.0658(2) 0.19082(7) 0.0372(8) Uani 1 1 d . . .
N1 N 0.6652(3) 0.0668(4) 0.07299(11) 0.0779(12) Uani 1 1 d DU . .
C1 C 0.6944(4) -0.2644(4) 0.12839(10) 0.0404(13) Uani 1 1 d . . .
C2 C 0.6997(5) -0.3788(4) 0.13103(16) 0.0655(18) Uani 1 1 d . . .
H2 H 0.7825 -0.3731 0.1297 0.079 Uiso 1 1 calc R . .
C3 C 0.5868(6) -0.5043(5) 0.13562(16) 0.084(2) Uani 1 1 d U . .
H3 H 0.5953 -0.5797 0.1381 0.101 Uiso 1 1 calc R . .
C4 C 0.4686(6) -0.5150(6) 0.13646(14) 0.089(2) Uani 1 1 d U . .
H4 H 0.3930 -0.5985 0.1390 0.107 Uiso 1 1 calc R . .
C5 C 0.4561(6) -0.4069(7) 0.13369(15) 0.087(2) Uani 1 1 d U . .
H5 H 0.3717 -0.4162 0.1347 0.105 Uiso 1 1 calc R . .
C6 C 0.5691(4) -0.2779(6) 0.12919(13) 0.0641(18) Uani 1 1 d . . .
H6 H 0.5589 -0.2035 0.1268 0.077 Uiso 1 1 calc R . .
C7 C 0.8171(3) -0.1298(3) 0.12202(9) 0.0276(9) Uani 1 1 d . . .
H7 H 0.8953 -0.1412 0.1231 0.033 Uiso 1 1 calc R . .
C8 C 0.8327(3) -0.0280(3) 0.15517(10) 0.0278(9) Uani 1 1 d . . .
C9 C 0.1350(5) -0.1350(5) 0.0833 0.034(2) Uani 0.50 2 d SPU A 1
H9 H 0.0495 -0.1689 0.0712 0.041 Uiso 0.50 1 d PR A 1
C10 C 0.2384(7) -0.1252(7) 0.0497(2) 0.041(2) Uani 0.50 1 d PDU A 1
H10A H 0.2261 -0.0861 0.0253 0.050 Uiso 0.50 1 calc PR A 1
H10B H 0.2210 -0.2140 0.0431 0.050 Uiso 0.50 1 calc PR A 1
C11 C 0.3942(3) -0.0339(5) 0.06554(14) 0.1002(17) Uani 0.50 1 d PDU A 1
C9' C 0.2023(6) -0.2023(6) 0.0833 0.045(3) Uani 0.50 2 d SPD A 2
H9' H 0.2561 -0.1963 0.1049 0.054 Uiso 0.50 1 d PR A 2
C10' C 0.2549(6) -0.0581(6) 0.0705(2) 0.040(2) Uani 0.50 1 d PD A 2
H10C H 0.2162 -0.0498 0.0455 0.048 Uiso 0.50 1 calc PR A 2
H10D H 0.2473 -0.0040 0.0916 0.048 Uiso 0.50 1 calc PRD A 2
C11' C 0.3942(3) -0.0339(5) 0.06554(14) 0.1002(17) Uani 0.50 1 d PD A 2
C12 C 0.4692(4) 0.0679(5) 0.09239(15) 0.1004(17) Uani 1 1 d DU . .
H12 H 0.4283 0.1040 0.1080 0.120 Uiso 1 1 calc RD A 1
C13 C 0.6017(4) 0.1154(5) 0.09609(13) 0.0836(15) Uani 1 1 d DU A .
H13 H 0.6504 0.1825 0.1147 0.100 Uiso 1 1 calc R . .
C14 C 0.5948(4) -0.0320(5) 0.04707(12) 0.0750(16) Uani 1 1 d DU A .
H14 H 0.6381 -0.0659 0.0316 0.090 Uiso 1 1 calc R . .
C15 C 0.4597(4) -0.0849(5) 0.04254(14) 0.0959(19) Uani 1 1 d DU . .
H15 H 0.4124 -0.1540 0.0244 0.115 Uiso 1 1 calc R A 1


_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
Zn1 O2 2.065(2) 10_665 ?
Zn1 O2 2.065(2) . ?
Zn1 O1 2.132(3) . ?
Zn1 O1 2.132(3) 10_665 ?
Zn1 N1 2.141(3) . ?
Zn1 N1 2.141(3) 10_665 ?
O1 C7 1.429(4) . ?
O1 H1O 0.853(18) . ?
O2 C8 1.262(5) . ?
O3 C8 1.251(4) . ?
N1 C14 1.333(5) . ?
N1 C13 1.363(6) . ?
C1 C2 1.360(8) . ?
C1 C6 1.382(7) . ?
C1 C7 1.512(4) . ?
C2 C3 1.396(6) . ?
C2 H2 0.9300 . ?
C3 C4 1.314(10) . ?
C3 H3 0.9300 . ?
C4 C5 1.335(11) . ?
C4 H4 0.9300 . ?
C5 C6 1.420(7) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C7 C8 1.553(5) . ?
C7 H7 0.9800 . ?
C9 C10 1.597(10) . ?
C9 C10 1.597(10) 10 ?
C9 H9 0.9534 . ?
C10 C11 1.657(8) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 C12 1.383(6) . ?
C11 C15 1.399(7) . ?
C9' C10' 1.525(9) . ?
C9' C10' 1.525(9) 10 ?
C9' H9' 0.9262 . ?
C10' H10C 0.9700 . ?
C10' H10D 0.9700 . ?
C12 C13 1.354(6) . ?
C12 H12 0.9300 . ?
C13 H13 0.9300 . ?
C14 C15 1.374(6) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?

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
O2 Zn1 O2 166.40(16) 10_665 . ?
O2 Zn1 O1 92.98(9) 10_665 . ?
O2 Zn1 O1 77.36(9) . . ?
O2 Zn1 O1 77.36(9) 10_665 10_665 ?
O2 Zn1 O1 92.98(9) . 10_665 ?
O1 Zn1 O1 90.40(13) . 10_665 ?
O2 Zn1 N1 93.52(11) 10_665 . ?
O2 Zn1 N1 95.57(12) . . ?
O1 Zn1 N1 87.53(13) . . ?
O1 Zn1 N1 170.54(11) 10_665 . ?
O2 Zn1 N1 95.57(12) 10_665 10_665 ?
O2 Zn1 N1 93.52(11) . 10_665 ?
O1 Zn1 N1 170.54(11) . 10_665 ?
O1 Zn1 N1 87.53(13) 10_665 10_665 ?
N1 Zn1 N1 96.0(2) . 10_665 ?
C7 O1 Zn1 115.30(19) . . ?
C7 O1 H1O 109.3(17) . . ?
Zn1 O1 H1O 127.7(14) . . ?
C8 O2 Zn1 118.8(2) . . ?
C14 N1 C13 119.3(3) . . ?
C14 N1 Zn1 119.6(3) . . ?
C13 N1 Zn1 120.6(3) . . ?
C2 C1 C6 116.5(4) . . ?
C2 C1 C7 122.5(4) . . ?
C6 C1 C7 120.8(5) . . ?
C1 C2 C3 123.2(6) . . ?
C1 C2 H2 118.4 . . ?
C3 C2 H2 118.4 . . ?
C4 C3 C2 119.4(7) . . ?
C4 C3 H3 120.3 . . ?
C2 C3 H3 120.3 . . ?
C3 C4 C5 120.5(5) . . ?
C3 C4 H4 119.7 . . ?
C5 C4 H4 119.7 . . ?
C4 C5 C6 121.4(6) . . ?
C4 C5 H5 119.3 . . ?
C6 C5 H5 119.3 . . ?
C1 C6 C5 119.0(6) . . ?
C1 C6 H6 120.5 . . ?
C5 C6 H6 120.5 . . ?
O1 C7 C1 111.3(3) . . ?
O1 C7 C8 108.6(3) . . ?
C1 C7 C8 112.2(3) . . ?
O1 C7 H7 108.2 . . ?
C1 C7 H7 108.2 . . ?
C8 C7 H7 108.2 . . ?
O3 C8 O2 126.2(3) . . ?
O3 C8 C7 115.3(3) . . ?
O2 C8 C7 118.4(3) . . ?
C10 C9 C10 107.8(9) . 10 ?
C10 C9 H9 108.9 . . ?
C10 C9 H9 108.4 10 . ?
C9 C10 C11 111.4(5) . . ?
C9 C10 H10A 109.3 . . ?
C11 C10 H10A 109.3 . . ?
C9 C10 H10B 109.3 . . ?
C11 C10 H10B 109.3 . . ?
H10A C10 H10B 108.0 . . ?
C12 C11 C15 117.9(4) . . ?
C12 C11 C10 140.2(5) . . ?
C15 C11 C10 102.0(4) . . ?
C10' C9' C10' 105.9(9) . 10 ?
C10' C9' H9' 104.2 . . ?
C10' C9' H9' 112.3 10 . ?
C9' C10' H10C 113.2 . . ?
C9' C10' H10D 113.2 . . ?
H10C C10' H10D 110.6 . . ?
C13 C12 C11 120.5(5) . . ?
C13 C12 H12 119.8 . . ?
C11 C12 H12 119.8 . . ?
C12 C13 N1 121.2(4) . . ?
C12 C13 H13 119.4 . . ?
N1 C13 H13 119.4 . . ?
N1 C14 C15 121.7(5) . . ?
N1 C14 H14 119.1 . . ?
C15 C14 H14 119.1 . . ?
C14 C15 C11 119.4(4) . . ?
C14 C15 H15 120.3 . . ?
C11 C15 H15 120.3 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1O O3 0.853(18) 1.796(19) 2.633(3) 166.5(18) 6_544

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.928
_refine_diff_density_min         -0.696
_refine_diff_density_rms         0.087

#=================================================END

data_complex7S
_database_code_depnum_ccdc_archive 'CCDC 704872'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C29 H28 N2 O6 Zn'
_chemical_formula_sum            'C29 H28 N2 O6 Zn'
_chemical_formula_weight         565.90

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'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_H-M   P6122
_chemical_absolute_configuration S

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z+1/3'
'-x+y, -x, z+2/3'
'-x, -y, z+1/2'
'y, -x+y, z+5/6'
'x-y, x, z+1/6'
'y, x, -z+1/3'
'x-y, -y, -z'
'-x, -x+y, -z+2/3'
'-y, -x, -z+5/6'
'-x+y, y, -z+1/2'
'x, x-y, -z+1/6'

_cell_length_a                   11.6056(10)
_cell_length_b                   11.6056(10)
_cell_length_c                   33.043(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     3854.3(8)
_cell_formula_units_Z            6
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2816
_cell_measurement_theta_min      2.03
_cell_measurement_theta_max      27.81

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.19
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.463
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1764
_exptl_absorpt_coefficient_mu    1.003
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7462
_exptl_absorpt_correction_T_max  0.8322
_exptl_absorpt_process_details   'SADABS (Bruker, 2002)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(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 SMART CCD area detector'
_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            10274
_diffrn_reflns_av_R_equivalents  0.0412
_diffrn_reflns_av_sigmaI/netI    0.0518
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_theta_min         2.03
_diffrn_reflns_theta_max         27.81
_reflns_number_total             2816
_reflns_number_gt                2165
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART (Bruker, 1998)'
_computing_cell_refinement       'Bruker SMART (Bruker, 1998)'
_computing_data_reduction        'Bruker SAINT + & SHELXTL (Bruker, 1998)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_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)+(0.0631P)²+0.1703P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.02(2)
_refine_ls_number_reflns         2816
_refine_ls_number_parameters     245
_refine_ls_number_restraints     49
_refine_ls_R_factor_all          0.0697
_refine_ls_R_factor_gt           0.0506
_refine_ls_wR_factor_ref         0.1196
_refine_ls_wR_factor_gt          0.1112
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_restrained_S_all      1.092
_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
Zn1 Zn 0.26104(6) 0.13052(3) 0.0833 0.0537(2) Uani 1 2 d S . .
O1 O 0.1099(3) -0.0621(3) 0.19062(7) 0.0631(8) Uani 1 1 d . . .
O2 O 0.2362(2) 0.0846(3) 0.14385(6) 0.0500(6) Uani 1 1 d . . .
O3 O 0.1102(3) -0.0753(3) 0.08360(7) 0.0511(6) Uani 1 1 d D . .
H3O H 0.057(4) -0.113(4) 0.0643(10) 0.074(14) Uiso 1 1 d D . .
C1 C 0.1426(4) -0.0262(4) 0.15493(9) 0.0450(8) Uani 1 1 d . . .
C2 C 0.0561(4) -0.1274(4) 0.12230(9) 0.0443(8) Uani 1 1 d . . .
H2 H -0.0336 -0.1395 0.1237 0.053 Uiso 1 1 calc R . .
C3 C 0.0459(5) -0.2617(4) 0.12841(9) 0.0549(11) Uani 1 1 d D . .
C4 C -0.0758(5) -0.3759(5) 0.13040(15) 0.0846(16) Uani 1 1 d DU . .
H4 H -0.1530 -0.3706 0.1288 0.102 Uiso 1 1 calc R . .
C5 C -0.0851(8) -0.5001(6) 0.13487(18) 0.113(2) Uani 1 1 d DU . .
H5 H -0.1676 -0.5771 0.1368 0.136 Uiso 1 1 calc R . .
C6 C 0.0265(10) -0.5058(7) 0.13629(16) 0.112(2) Uani 1 1 d DU . .
H6 H 0.0203 -0.5885 0.1387 0.135 Uiso 1 1 calc R . .
C7 C 0.1470(8) -0.3974(8) 0.13438(18) 0.114(2) Uani 1 1 d DU . .
H7 H 0.2229 -0.4050 0.1360 0.137 Uiso 1 1 calc R . .
C8 C 0.1579(6) -0.2712(6) 0.12983(14) 0.0886(17) Uani 1 1 d DU . .
H8 H 0.2413 -0.1951 0.1278 0.106 Uiso 1 1 calc R . .
N1 N 0.3965(15) 0.0431(12) 0.0716(5) 0.043(3) Uani 0.50 1 d P . 1
C9 C 0.3594(18) -0.0579(14) 0.0453(5) 0.056(4) Uani 0.50 1 d P . 1
H9 H 0.2793 -0.0902 0.0315 0.067 Uiso 0.50 1 calc PR . 1
C10 C 0.4349(12) -0.1130(12) 0.0385(3) 0.058(3) Uani 0.50 1 d P . 1
H10 H 0.4083 -0.1790 0.0189 0.069 Uiso 0.50 1 calc PR . 1
C11 C 0.5505(13) -0.0750(10) 0.0596(3) 0.045(3) Uani 0.50 1 d P . 1
C12 C 0.5864(15) 0.0273(16) 0.0861(4) 0.050(4) Uani 0.50 1 d P . 1
H12 H 0.6669 0.0624 0.0998 0.061 Uiso 0.50 1 calc PR . 1
C13 C 0.5032(15) 0.0794(11) 0.0927(4) 0.056(3) Uani 0.50 1 d P . 1
H13 H 0.5249 0.1425 0.1130 0.067 Uiso 0.50 1 calc PR . 1
C14 C 0.6361(10) -0.1347(10) 0.0495(3) 0.064(2) Uani 0.50 1 d P . 1
H14A H 0.6932 -0.0853 0.0270 0.076 Uiso 0.50 1 calc PR . 1
H14B H 0.5784 -0.2252 0.0403 0.076 Uiso 0.50 1 calc PR . 1
C15 C 0.7235(11) -0.1382(6) 0.0833 0.062(3) Uani 0.50 2 d SP . 1
H15 H 0.7800 -0.0467 0.0933 0.075 Uiso 0.50 1 d PR . 1
N1' N 0.4102(17) 0.0976(12) 0.0751(5) 0.054(3) Uani 0.50 1 d P . 2
C9' C 0.3913(17) -0.0006(17) 0.0507(6) 0.058(4) Uani 0.50 1 d P . 2
H9' H 0.3150 -0.0390 0.0348 0.069 Uiso 0.50 1 calc PR . 2
C10' C 0.4780(14) -0.0506(14) 0.0471(3) 0.071(4) Uani 0.50 1 d P . 2
H10' H 0.4582 -0.1187 0.0287 0.086 Uiso 0.50 1 calc PR . 2
C11' C 0.5894(16) -0.0031(18) 0.0695(4) 0.052(4) Uani 0.50 1 d P . 2
C12' C 0.6126(12) 0.0993(12) 0.0965(3) 0.063(3) Uani 0.50 1 d P . 2
H12' H 0.6865 0.1364 0.1134 0.076 Uiso 0.50 1 calc PR . 2
C13' C 0.5222(14) 0.1433(12) 0.0971(4) 0.055(3) Uani 0.50 1 d P . 2
H13' H 0.5407 0.2126 0.1149 0.067 Uiso 0.50 1 calc PR . 2
C14' C 0.6817(10) -0.0584(11) 0.0700(4) 0.080(3) Uani 0.50 1 d P . 2
H14C H 0.7182 -0.0536 0.0433 0.096 Uiso 0.50 1 calc PR . 2
H14D H 0.7546 -0.0086 0.0887 0.096 Uiso 0.50 1 calc PR . 2
C15' C 0.6013(16) -0.1993(8) 0.0833 0.103(5) Uani 0.50 2 d SP . 2
H15' H 0.5450 -0.2540 0.0609 0.124 Uiso 0.50 1 d PR . 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
Zn1 N1' 1.969(15) . ?
Zn1 N1' 1.969(15) 12 ?
Zn1 O2 2.052(2) 12 ?
Zn1 O2 2.052(2) . ?
Zn1 O3 2.142(3) . ?
Zn1 O3 2.142(3) 12 ?
Zn1 N1 2.291(13) . ?
Zn1 N1 2.291(14) 12 ?
O1 C1 1.245(4) . ?
O2 C1 1.253(4) . ?
O3 C2 1.420(4) . ?
O3 H3O 0.84(2) . ?
C1 C2 1.540(5) . ?
C2 C3 1.516(5) . ?
C2 H2 0.9800 . ?
C3 C8 1.359(7) . ?
C3 C4 1.373(6) . ?
C4 C5 1.398(7) . ?
C4 H4 0.9300 . ?
C5 C6 1.330(9) . ?
C5 H5 0.9300 . ?
C6 C7 1.335(9) . ?
C6 H6 0.9300 . ?
C7 C8 1.414(7) . ?
C7 H7 0.9300 . ?
C8 H8 0.9300 . ?
N1 C13 1.29(2) . ?
N1 C9 1.346(13) . ?
C9 C10 1.34(2) . ?
C9 H9 0.9300 . ?
C10 C11 1.375(18) . ?
C10 H10 0.9300 . ?
C11 C12 1.362(15) . ?
C11 C14 1.505(15) . ?
C12 C13 1.39(2) . ?
C12 H12 0.9300 . ?
C13 H13 0.9300 . ?
C14 C15 1.524(11) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 C14 1.524(11) 12_545 ?
C15 H15 0.9847 . ?
N1' C9' 1.323(15) . ?
N1' C13' 1.35(2) . ?
C9' C10' 1.39(2) . ?
C9' H9' 0.9300 . ?
C10' C11' 1.35(2) . ?
C10' H10' 0.9300 . ?
C11' C12' 1.401(16) . ?
C11' C14' 1.499(18) . ?
C12' C13' 1.38(2) . ?
C12' H12' 0.9300 . ?
C13' H13' 0.9300 . ?
C14' C15' 1.487(13) . ?
C14' H14C 0.9700 . ?
C14' H14D 0.9700 . ?
C15' C14' 1.487(13) 12_545 ?
C15' H15' 0.9816 . ?

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' Zn1 N1' 80.8(8) . 12 ?
N1' Zn1 O2 94.5(5) . 12 ?
N1' Zn1 O2 96.2(5) 12 12 ?
N1' Zn1 O2 96.2(5) . . ?
N1' Zn1 O2 94.5(5) 12 . ?
O2 Zn1 O2 166.03(14) 12 . ?
N1' Zn1 O3 95.3(4) . . ?
N1' Zn1 O3 170.3(5) 12 . ?
O2 Zn1 O3 92.97(10) 12 . ?
O2 Zn1 O3 77.06(9) . . ?
N1' Zn1 O3 170.3(5) . 12 ?
N1' Zn1 O3 95.3(4) 12 12 ?
O2 Zn1 O3 77.06(9) 12 12 ?
O2 Zn1 O3 92.97(10) . 12 ?
O3 Zn1 O3 89.90(15) . 12 ?
N1' Zn1 N1 93.9(4) 12 . ?
O2 Zn1 N1 93.2(4) 12 . ?
O2 Zn1 N1 95.1(4) . . ?
O3 Zn1 N1 82.3(3) . . ?
O3 Zn1 N1 167.3(4) 12 . ?
N1' Zn1 N1 93.9(4) . 12 ?
O2 Zn1 N1 95.1(4) 12 12 ?
O2 Zn1 N1 93.2(4) . 12 ?
O3 Zn1 N1 167.3(4) . 12 ?
O3 Zn1 N1 82.3(3) 12 12 ?
N1 Zn1 N1 107.0(7) . 12 ?
C1 O2 Zn1 119.2(2) . . ?
C2 O3 Zn1 114.8(2) . . ?
C2 O3 H3O 114(3) . . ?
Zn1 O3 H3O 124(3) . . ?
O1 C1 O2 125.7(3) . . ?
O1 C1 C2 115.8(3) . . ?
O2 C1 C2 118.6(3) . . ?
O3 C2 C3 110.4(3) . . ?
O3 C2 C1 108.9(3) . . ?
C3 C2 C1 112.1(3) . . ?
O3 C2 H2 108.4 . . ?
C3 C2 H2 108.4 . . ?
C1 C2 H2 108.4 . . ?
C8 C3 C4 119.0(4) . . ?
C8 C3 C2 120.1(4) . . ?
C4 C3 C2 120.8(4) . . ?
C3 C4 C5 120.8(5) . . ?
C3 C4 H4 119.6 . . ?
C5 C4 H4 119.6 . . ?
C6 C5 C4 118.7(6) . . ?
C6 C5 H5 120.7 . . ?
C4 C5 H5 120.7 . . ?
C5 C6 C7 122.6(5) . . ?
C5 C6 H6 118.7 . . ?
C7 C6 H6 118.7 . . ?
C6 C7 C8 119.3(6) . . ?
C6 C7 H7 120.3 . . ?
C8 C7 H7 120.3 . . ?
C3 C8 C7 119.6(5) . . ?
C3 C8 H8 120.2 . . ?
C7 C8 H8 120.2 . . ?
C13 N1 C9 118.0(14) . . ?
C13 N1 Zn1 121.5(9) . . ?
C9 N1 Zn1 120.2(13) . . ?
C10 C9 N1 121.6(15) . . ?
C10 C9 H9 119.2 . . ?
N1 C9 H9 119.2 . . ?
C9 C10 C11 122.0(10) . . ?
C9 C10 H10 119.0 . . ?
C11 C10 H10 119.0 . . ?
C12 C11 C10 115.4(13) . . ?
C12 C11 C14 124.0(13) . . ?
C10 C11 C14 120.2(9) . . ?
C11 C12 C13 120.3(13) . . ?
C11 C12 H12 119.9 . . ?
C13 C12 H12 119.9 . . ?
N1 C13 C12 122.3(10) . . ?
N1 C13 H13 118.8 . . ?
C12 C13 H13 118.8 . . ?
C11 C14 C15 116.8(7) . . ?
C11 C14 H14A 108.1 . . ?
C15 C14 H14A 108.1 . . ?
C11 C14 H14B 108.1 . . ?
C15 C14 H14B 108.1 . . ?
H14A C14 H14B 107.3 . . ?
C11 C14 H15' 93.0 . . ?
C15 C14 H15' 87.5 . . ?
H14A C14 H15' 143.0 . . ?
H14B C14 H15' 35.9 . . ?
C14 C15 C14 109.5(10) . 12_545 ?
C14 C15 H15 108.0 . . ?
C14 C15 H15 110.9 12_545 . ?
C9' N1' C13' 112.4(14) . . ?
C9' N1' Zn1 117.9(14) . . ?
C13' N1' Zn1 128.2(11) . . ?
N1' C9' C10' 124.6(15) . . ?
N1' C9' H9' 117.7 . . ?
C10' C9' H9' 117.7 . . ?
C11' C10' C9' 121.8(12) . . ?
C11' C10' H10' 119.1 . . ?
C9' C10' H10' 119.1 . . ?
C10' C11' C12' 115.8(14) . . ?
C10' C11' C14' 125.3(16) . . ?
C12' C11' C14' 118.7(14) . . ?
C13' C12' C11' 117.7(13) . . ?
C13' C12' H12' 121.1 . . ?
C11' C12' H12' 121.1 . . ?
N1' C13' C12' 127.6(12) . . ?
N1' C13' H13' 116.2 . . ?
C12' C13' H13' 116.2 . . ?
C15' C14' C11' 106.6(10) . . ?
C15' C14' H15 88.6 . . ?
C11' C14' H15 136.6 . . ?
C15' C14' H14C 110.4 . . ?
C11' C14' H14C 110.4 . . ?
H15 C14' H14C 101.2 . . ?
C15' C14' H14D 110.4 . . ?
C11' C14' H14D 110.4 . . ?
H15 C14' H14D 28.5 . . ?
H14C C14' H14D 108.6 . . ?
C14' C15' C14' 114.2(14) 12_545 . ?
C14' C15' H15' 106.9 12_545 . ?
C14' C15' H15' 109.7 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O3 H3O O1 0.84(2) 1.79(2) 2.626(3) 170(4) 5_554

_diffrn_measured_fraction_theta_max 0.948
_diffrn_reflns_theta_full        27.81
_diffrn_measured_fraction_theta_full 0.948
_refine_diff_density_max         0.338
_refine_diff_density_min         -0.200
_refine_diff_density_rms         0.061

#_eof
#End of Crystallographic Information File



