# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_21jlead
_audit_block_doi                 10.5517/cc4rg6j
_database_code_depnum_ccdc_archive 'CCDC 141707'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1016/S0277-5387(01)00689-1 2001
_audit_update_record             
;
2000-03-09 deposited with the CCDC.
2016-04-29 downloaded from the CCDC.
;




_audit_creation_method           SHELXL-97

_chemical_name_systematic        
;

?

;

_chemical_name_common            ?

_chemical_melting_point          ?

_chemical_formula_moiety         ?

_chemical_formula_sum            
'C60 H60 B Cl F4 N8 O8 Re2'

_chemical_formula_weight         1515.82



loop_

_atom_type_symbol

_atom_type_description

_atom_type_scat_dispersion_real

_atom_type_scat_dispersion_imag

_atom_type_scat_source
















C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'



_symmetry_cell_setting           ?

_symmetry_space_group_name_H-M   ?



loop_

_symmetry_equiv_pos_as_xyz








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



_cell_length_a                   13.0898(15)

_cell_length_b                   13.0898(15)

_cell_length_c                   16.960(3)

_cell_angle_alpha                90.00

_cell_angle_beta                 90.00

_cell_angle_gamma                90.00

_cell_volume                     2906.0(7)

_cell_formula_units_Z            2

_cell_measurement_temperature    293(2)

_cell_measurement_reflns_used    ?

_cell_measurement_theta_min      ?

_cell_measurement_theta_max      ?



_exptl_crystal_description       ?

_exptl_crystal_colour            ?

_exptl_crystal_size_max          ?

_exptl_crystal_size_mid          ?

_exptl_crystal_size_min          ?

_exptl_crystal_density_meas      ?

_exptl_crystal_density_diffrn    1.732

_exptl_crystal_density_method    'not measured'

_exptl_crystal_F_000             1496

_exptl_absorpt_coefficient_mu    4.283

_exptl_absorpt_correction_type   ?

_exptl_absorpt_correction_T_min  ?

_exptl_absorpt_correction_T_max  ?

_exptl_absorpt_process_details   ?



_exptl_special_details           
;

?

;



_diffrn_ambient_temperature      293(2)

_diffrn_radiation_wavelength     0.71073

_diffrn_radiation_type           MoK\a

_diffrn_radiation_source         'fine-focus sealed tube'

_diffrn_radiation_monochromator  graphite

_diffrn_measurement_device_type  ?

_diffrn_measurement_method       ?

_diffrn_detector_area_resol_mean ?

_diffrn_standards_number         ?

_diffrn_standards_interval_count ?

_diffrn_standards_interval_time  ?

_diffrn_standards_decay_%        ?

_diffrn_reflns_number            21431

_diffrn_reflns_av_R_equivalents  0.0667

_diffrn_reflns_av_sigmaI/netI    0.0489

_diffrn_reflns_limit_h_min       -15

_diffrn_reflns_limit_h_max       15

_diffrn_reflns_limit_k_min       -15

_diffrn_reflns_limit_k_max       15

_diffrn_reflns_limit_l_min       -20

_diffrn_reflns_limit_l_max       20

_diffrn_reflns_theta_min         1.20

_diffrn_reflns_theta_max         25.02

_reflns_number_total             2583

_reflns_number_gt                1816

_reflns_threshold_expression     >2sigma(I)



_computing_data_collection       ?

_computing_cell_refinement       ?

_computing_data_reduction        ?

_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)+(0.0531P)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_number_reflns         2583

_refine_ls_number_parameters     201

_refine_ls_number_restraints     16

_refine_ls_R_factor_all          0.0691

_refine_ls_R_factor_gt           0.0367

_refine_ls_wR_factor_ref         0.1224

_refine_ls_wR_factor_gt          0.0996

_refine_ls_goodness_of_fit_ref   1.315

_refine_ls_restrained_S_all      1.315

_refine_ls_shift/su_max          15.000

_refine_ls_shift/su_mean         0.086



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











































Re1 Re 0.2500 0.2500 0.07859(4) 0.0286(2) Uani 1 4 d S . .
ReA Re 0.2500 0.2500 0.172(2) 2.00(5) Uiso 1 4 d S . .
Re2 Re 0.2500 0.2500 0.20970(4) 0.0292(2) Uani 1 4 d S . .
Cl1 Cl 0.2500 0.2500 0.3478(5) 0.091(2) Uani 1 4 d S . .
N1 N 0.2175(5) 0.0955(5) 0.0735(4) 0.0337(18) Uani 1 1 d . . .
N2 N 0.2038(6) 0.0965(5) 0.2100(4) 0.0328(18) Uani 1 1 d . . .
O10 O 0.1610(6) -0.1314(6) -0.2030(4) 0.066(2) Uani 1 1 d . . .
O20 O 0.0360(6) -0.1261(6) 0.4607(4) 0.067(2) Uani 1 1 d . . .
CB1 C 0.1981(7) 0.0478(7) 0.1413(6) 0.037(2) Uani 1 1 d . . .
HB1A H 0.1802 -0.0210 0.1405 0.045 Uiso 1 1 calc R . .
C11 C 0.2044(7) 0.0352(6) 0.0023(6) 0.034(2) Uani 1 1 d . . .
C12 C 0.1285(8) -0.0356(8) -0.0053(7) 0.057(3) Uani 1 1 d . . .
H12A H 0.0843 -0.0474 0.0366 0.069 Uiso 1 1 calc R . .
C13 C 0.1165(10) -0.0897(9) -0.0741(7) 0.070(4) Uani 1 1 d . . .
H13A H 0.0641 -0.1374 -0.0779 0.083 Uiso 1 1 calc R . .
C14 C 0.1804(8) -0.0750(8) -0.1374(6) 0.047(2) Uani 1 1 d . . .
C15 C 0.2555(8) -0.0014(8) -0.1311(5) 0.049(3) Uani 1 1 d . . .
H15A H 0.2984 0.0118 -0.1735 0.058 Uiso 1 1 calc R . .
C16 C 0.2669(7) 0.0528(7) -0.0613(6) 0.046(2) Uani 1 1 d . . .
H16A H 0.3179 0.1020 -0.0575 0.055 Uiso 1 1 calc R . .
C17 C 0.2235(9) -0.1151(10) -0.2712(6) 0.072(4) Uani 1 1 d . . .
H17A H 0.2005 -0.1585 -0.3133 0.108 Uiso 1 1 calc R . .
H17B H 0.2932 -0.1311 -0.2588 0.108 Uiso 1 1 calc R . .
H17C H 0.2187 -0.0450 -0.2873 0.108 Uiso 1 1 calc R . .
C21 C 0.1614(7) 0.0397(6) 0.2758(5) 0.034(2) Uani 1 1 d . . .
C22 C 0.0590(7) 0.0164(7) 0.2752(6) 0.043(2) Uani 1 1 d . . .
H22A H 0.0188 0.0380 0.2331 0.052 Uiso 1 1 calc R . .
C23 C 0.0146(8) -0.0386(7) 0.3357(6) 0.048(3) Uani 1 1 d . . .
H23A H -0.0548 -0.0535 0.3341 0.058 Uiso 1 1 calc R . .
C24 C 0.0734(9) -0.0715(8) 0.3990(6) 0.049(3) Uani 1 1 d . . .
C25 C 0.1759(8) -0.0492(9) 0.3985(6) 0.054(3) Uani 1 1 d . . .
H25A H 0.2168 -0.0721 0.4397 0.065 Uiso 1 1 calc R . .
C26 C 0.2195(8) 0.0065(8) 0.3381(5) 0.045(2) Uani 1 1 d . . .
H26A H 0.2889 0.0216 0.3396 0.055 Uiso 1 1 calc R . .
C27 C -0.0727(9) -0.1412(10) 0.4655(6) 0.074(4) Uani 1 1 d . . .
H27A H -0.0884 -0.1820 0.5110 0.111 Uiso 1 1 calc R . .
H27B H -0.0961 -0.1754 0.4189 0.111 Uiso 1 1 calc R . .
H27C H -0.1061 -0.0761 0.4700 0.111 Uiso 1 1 calc R . .
B1 B 0.2500 0.2500 -0.2627(11) 0.027(4) Uani 1 4 d SD . .
F1 F 0.2500 0.2500 -0.1863(10) 0.110(6) Uani 1 4 d SD . .
F2 F 0.170(3) 0.206(7) -0.296(3) 0.21(4) Uiso 0.25 1 d PD . .
F3 F 0.264(6) 0.3437(16) -0.293(2) 0.111(17) Uiso 0.25 1 d PD . .
F4 F 0.334(3) 0.195(5) -0.278(3) 0.109(17) Uiso 0.25 1 d PD . .






_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




































































Re1 ReA 1.59(3) . ?
Re1 N1 2.068(7) 2 ?
Re1 N1 2.068(7) 4 ?
Re1 N1 2.068(7) . ?
Re1 N1 2.068(7) 3 ?
Re1 Re2 2.2234(10) . ?
ReA Re2 0.63(4) . ?
ReA N2 2.193(12) 2 ?
ReA N2 2.193(12) 3 ?
ReA N2 2.193(12) 4 ?
ReA N2 2.193(12) . ?
ReA N1 2.66(2) . ?
ReA N1 2.66(2) 4 ?
ReA N1 2.66(2) 2 ?
ReA N1 2.66(2) 3 ?
Re2 N2 2.098(7) 2 ?
Re2 N2 2.098(7) 3 ?
Re2 N2 2.098(7) . ?
Re2 N2 2.098(7) 4 ?
Re2 Cl1 2.343(8) . ?
N1 CB1 1.332(10) . ?
N1 C11 1.454(11) . ?
N2 CB1 1.331(10) . ?
N2 C21 1.452(10) . ?
O10 C14 1.360(11) . ?
O10 C17 1.433(12) . ?
O20 C24 1.360(11) . ?
O20 C27 1.439(13) . ?
C11 C12 1.365(12) . ?
C11 C16 1.372(12) . ?
C12 C13 1.374(14) . ?
C13 C14 1.374(14) . ?
C14 C15 1.380(13) . ?
C15 C16 1.388(12) . ?
C21 C26 1.371(12) . ?
C21 C22 1.375(12) . ?
C22 C23 1.382(12) . ?
C23 C24 1.389(14) . ?
C24 C25 1.372(14) . ?
C25 C26 1.381(13) . ?
B1 F1 1.295(15) . ?
B1 F2 1.323(17) . ?
B1 F2 1.323(17) 3 ?
B1 F2 1.323(17) 2 ?
B1 F2 1.323(17) 4 ?
B1 F4 1.343(16) 4 ?
B1 F4 1.343(16) . ?
B1 F4 1.343(16) 2 ?
B1 F4 1.343(16) 3 ?
B1 F3 1.344(17) 2 ?
B1 F3 1.344(17) 3 ?
B1 F3 1.344(17) . ?
F2 F4 0.69(6) 4 ?
F2 F3 0.77(5) 3 ?
F2 F3 1.09(6) 2 ?
F2 F4 1.33(6) 2 ?
F2 F2 1.70(4) 3 ?
F2 F2 1.70(4) 4 ?
F3 F4 0.62(5) 3 ?
F3 F2 0.77(5) 4 ?
F3 F2 1.09(6) 2 ?
F3 F4 1.40(5) 2 ?
F3 F3 1.75(3) 3 ?
F3 F3 1.75(3) 4 ?
F4 F3 0.62(5) 4 ?
F4 F2 0.69(6) 3 ?
F4 F2 1.33(6) 2 ?
F4 F3 1.40(5) 2 ?



loop_

_geom_angle_atom_site_label_1

_geom_angle_atom_site_label_2

_geom_angle_atom_site_label_3

_geom_angle

_geom_angle_site_symmetry_1

_geom_angle_site_symmetry_3

_geom_angle_publ_flag










































































































































































































































ReA Re1 N1 92.4(2) . 2 ?
ReA Re1 N1 92.4(2) . 4 ?
N1 Re1 N1 89.902(17) 2 4 ?
ReA Re1 N1 92.4(2) . . ?
N1 Re1 N1 175.3(4) 2 . ?
N1 Re1 N1 89.902(17) 4 . ?
ReA Re1 N1 92.4(2) . 3 ?
N1 Re1 N1 89.902(17) 2 3 ?
N1 Re1 N1 175.3(4) 4 3 ?
N1 Re1 N1 89.902(17) . 3 ?
ReA Re1 Re2 0.000(2) . . ?
N1 Re1 Re2 92.4(2) 2 . ?
N1 Re1 Re2 92.4(2) 4 . ?
N1 Re1 Re2 92.4(2) . . ?
N1 Re1 Re2 92.4(2) 3 . ?
Re1 ReA Re2 180.0 . . ?
Re1 ReA N2 107.0(9) . 2 ?
Re2 ReA N2 73.0(9) . 2 ?
Re1 ReA N2 107.0(9) . 3 ?
Re2 ReA N2 73.0(9) . 3 ?
N2 ReA N2 85.1(5) 2 3 ?
Re1 ReA N2 107.0(9) . 4 ?
Re2 ReA N2 73.0(9) . 4 ?
N2 ReA N2 85.1(5) 2 4 ?
N2 ReA N2 146.1(18) 3 4 ?
Re1 ReA N2 107.0(9) . . ?
Re2 ReA N2 73.0(9) . . ?
N2 ReA N2 146.1(18) 2 . ?
N2 ReA N2 85.1(5) 3 . ?
N2 ReA N2 85.1(5) 4 . ?
Re1 ReA N1 51.0(6) . . ?
Re2 ReA N1 129.0(6) . . ?
N2 ReA N1 157.5(15) 2 . ?
N2 ReA N1 96.9(5) 3 . ?
N2 ReA N1 104.3(5) 4 . ?
N2 ReA N1 56.2(4) . . ?
Re1 ReA N1 51.0(6) . 4 ?
Re2 ReA N1 129.0(6) . 4 ?
N2 ReA N1 104.3(5) 2 4 ?
N2 ReA N1 157.5(15) 3 4 ?
N2 ReA N1 56.2(4) 4 4 ?
N2 ReA N1 96.9(5) . 4 ?
N1 ReA N1 66.6(7) . 4 ?
Re1 ReA N1 51.0(6) . 2 ?
Re2 ReA N1 129.0(6) . 2 ?
N2 ReA N1 56.2(4) 2 2 ?
N2 ReA N1 104.3(5) 3 2 ?
N2 ReA N1 96.9(5) 4 2 ?
N2 ReA N1 157.5(15) . 2 ?
N1 ReA N1 101.9(12) . 2 ?
N1 ReA N1 66.6(7) 4 2 ?
Re1 ReA N1 51.0(6) . 3 ?
Re2 ReA N1 129.0(6) . 3 ?
N2 ReA N1 96.9(5) 2 3 ?
N2 ReA N1 56.2(4) 3 3 ?
N2 ReA N1 157.5(15) 4 3 ?
N2 ReA N1 104.3(5) . 3 ?
N1 ReA N1 66.6(7) . 3 ?
N1 ReA N1 101.9(12) 4 3 ?
N1 ReA N1 66.6(7) 2 3 ?
ReA Re2 N2 90.16(19) . 2 ?
ReA Re2 N2 90.16(19) . 3 ?
N2 Re2 N2 89.999(2) 2 3 ?
ReA Re2 N2 90.16(19) . . ?
N2 Re2 N2 179.7(4) 2 . ?
N2 Re2 N2 90.000(1) 3 . ?
ReA Re2 N2 90.16(19) . 4 ?
N2 Re2 N2 90.000(1) 2 4 ?
N2 Re2 N2 179.7(4) 3 4 ?
N2 Re2 N2 90.000(2) . 4 ?
ReA Re2 Re1 0.000(4) . . ?
N2 Re2 Re1 90.16(19) 2 . ?
N2 Re2 Re1 90.16(19) 3 . ?
N2 Re2 Re1 90.16(19) . . ?
N2 Re2 Re1 90.16(19) 4 . ?
ReA Re2 Cl1 180.000(5) . . ?
N2 Re2 Cl1 89.84(19) 2 . ?
N2 Re2 Cl1 89.84(19) 3 . ?
N2 Re2 Cl1 89.84(19) . . ?
N2 Re2 Cl1 89.84(19) 4 . ?
Re1 Re2 Cl1 180.000(1) . . ?
CB1 N1 C11 116.1(8) . . ?
CB1 N1 Re1 117.5(6) . . ?
C11 N1 Re1 126.1(6) . . ?
CB1 N1 ReA 81.0(7) . . ?
C11 N1 ReA 162.8(9) . . ?
Re1 N1 ReA 36.7(6) . . ?
CB1 N2 C21 114.0(7) . . ?
CB1 N2 Re2 118.2(6) . . ?
C21 N2 Re2 127.1(6) . . ?
CB1 N2 ReA 101.5(10) . . ?
C21 N2 ReA 143.0(10) . . ?
Re2 N2 ReA 16.8(9) . . ?
C14 O10 C17 118.3(9) . . ?
C24 O20 C27 118.2(9) . . ?
N2 CB1 N1 121.3(8) . . ?
C12 C11 C16 118.3(9) . . ?
C12 C11 N1 122.2(8) . . ?
C16 C11 N1 119.4(8) . . ?
C11 C12 C13 120.9(10) . . ?
C14 C13 C12 121.4(10) . . ?
O10 C14 C13 116.7(9) . . ?
O10 C14 C15 125.1(9) . . ?
C13 C14 C15 118.1(9) . . ?
C14 C15 C16 120.0(9) . . ?
C11 C16 C15 121.3(9) . . ?
C26 C21 C22 118.5(9) . . ?
C26 C21 N2 122.8(8) . . ?
C22 C21 N2 118.7(8) . . ?
C21 C22 C23 121.3(9) . . ?
C22 C23 C24 120.1(10) . . ?
O20 C24 C25 118.0(10) . . ?
O20 C24 C23 123.9(10) . . ?
C25 C24 C23 118.1(9) . . ?
C24 C25 C26 121.4(10) . . ?
C21 C26 C25 120.6(9) . . ?
F1 B1 F2 115(2) . . ?
F1 B1 F2 115(2) . 3 ?
F2 B1 F2 79.8(16) . 3 ?
F1 B1 F2 115(2) . 2 ?
F2 B1 F2 130(4) . 2 ?
F2 B1 F2 79.8(16) 3 2 ?
F1 B1 F2 115(2) . 4 ?
F2 B1 F2 79.8(16) . 4 ?
F2 B1 F2 130(4) 3 4 ?
F2 B1 F2 79.8(16) 2 4 ?
F1 B1 F4 101(2) . 4 ?
F2 B1 F4 30(3) . 4 ?
F2 B1 F4 60(3) 3 4 ?
F2 B1 F4 135(3) 2 4 ?
F2 B1 F4 110(2) 4 4 ?
F1 B1 F4 101(2) . . ?
F2 B1 F4 110(2) . . ?
F2 B1 F4 30(3) 3 . ?
F2 B1 F4 60(3) 2 . ?
F2 B1 F4 135(3) 4 . ?
F4 B1 F4 87.9(9) 4 . ?
F1 B1 F4 101(2) . 2 ?
F2 B1 F4 60(3) . 2 ?
F2 B1 F4 135(3) 3 2 ?
F2 B1 F4 110(2) 2 2 ?
F2 B1 F4 30(3) 4 2 ?
F4 B1 F4 87.9(9) 4 2 ?
F4 B1 F4 158(5) . 2 ?
F1 B1 F4 101(2) . 3 ?
F2 B1 F4 135(3) . 3 ?
F2 B1 F4 110(2) 3 3 ?
F2 B1 F4 30(3) 2 3 ?
F2 B1 F4 60(3) 4 3 ?
F4 B1 F4 158(5) 4 3 ?
F4 B1 F4 87.9(9) . 3 ?
F4 B1 F4 87.9(9) 2 3 ?
F1 B1 F3 112.7(18) . 2 ?
F2 B1 F3 48(3) . 2 ?
F2 B1 F3 34(2) 3 2 ?
F2 B1 F3 109.8(19) 2 2 ?
F2 B1 F3 121(3) 4 2 ?
F4 B1 F3 26(2) 4 2 ?
F4 B1 F3 63(2) . 2 ?
F4 B1 F3 107.9(18) 2 2 ?
F4 B1 F3 138(3) 3 2 ?
F1 B1 F3 112.7(18) . 3 ?
F2 B1 F3 34(2) . 3 ?
F2 B1 F3 109.8(19) 3 3 ?
F2 B1 F3 121(3) 2 3 ?
F2 B1 F3 48(3) 4 3 ?
F4 B1 F3 63(2) 4 3 ?
F4 B1 F3 138(3) . 3 ?
F4 B1 F3 26(2) 2 3 ?
F4 B1 F3 107.9(18) 3 3 ?
F3 B1 F3 81.4(13) 2 3 ?
F1 B1 F3 112.7(18) . . ?
F2 B1 F3 109.8(19) . . ?
F2 B1 F3 121(3) 3 . ?
F2 B1 F3 48(3) 2 . ?
F2 B1 F3 34(2) 4 . ?
F4 B1 F3 138(3) 4 . ?
F4 B1 F3 107.9(18) . . ?
F4 B1 F3 63(2) 2 . ?
F4 B1 F3 26(2) 3 . ?
F3 B1 F3 135(4) 2 . ?
F3 B1 F3 81.4(13) 3 . ?
F4 F2 F3 146(6) 4 3 ?
F4 F2 F3 31(5) 4 2 ?
F3 F2 F3 139(4) 3 2 ?
F4 F2 F4 132(6) 4 2 ?
F3 F2 F4 15(2) 3 2 ?
F3 F2 F4 127(2) 2 2 ?
F4 F2 B1 77(2) 4 . ?
F3 F2 B1 74.7(19) 3 . ?
F3 F2 B1 66.8(16) 2 . ?
F4 F2 B1 60.8(16) 2 . ?
F4 F2 F2 47(5) 4 3 ?
F3 F2 F2 119(3) 3 3 ?
F3 F2 F2 20(3) 2 3 ?
F4 F2 F2 108.1(18) 2 3 ?
B1 F2 F2 50.1(8) . 3 ?
F4 F2 F2 127(2) 4 4 ?
F3 F2 F2 30(4) 3 4 ?
F3 F2 F2 110(2) 2 4 ?
F4 F2 F2 23(3) 2 4 ?
B1 F2 F2 50.1(8) . 4 ?
F2 F2 F2 90.000(5) 3 4 ?
F4 F3 F2 147(4) 3 4 ?
F4 F3 F2 36(6) 3 2 ?
F2 F3 F2 130(5) 4 2 ?
F4 F3 B1 77(2) 3 . ?
F2 F3 B1 71.7(17) 4 . ?
F2 F3 B1 64.8(16) 2 . ?
F4 F3 F4 131(5) 3 2 ?
F2 F3 F4 16(3) 4 2 ?
F2 F3 F4 122(3) 2 2 ?
B1 F3 F4 58.6(15) . 2 ?
F4 F3 F3 126(2) 3 3 ?
F2 F3 F3 24(3) 4 3 ?
F2 F3 F3 106(2) 2 3 ?
B1 F3 F3 49.3(6) . 3 ?
F4 F3 F3 19(2) 2 3 ?
F4 F3 F3 46(5) 3 4 ?
F2 F3 F3 114(3) 4 4 ?
F2 F3 F3 17(2) 2 4 ?
B1 F3 F3 49.3(6) . 4 ?
F4 F3 F3 105.0(15) 2 4 ?
F3 F3 F3 90.000(10) 3 4 ?
F3 F4 F2 113(10) 4 3 ?
F3 F4 F2 19(3) 4 2 ?
F2 F4 F2 110(7) 3 2 ?
F3 F4 B1 77(2) 4 . ?
F2 F4 B1 73(2) 3 . ?
F2 F4 B1 59.3(15) 2 . ?
F3 F4 F3 115(7) 4 2 ?
F2 F4 F3 18(3) 3 2 ?
F2 F4 F3 106(4) 2 2 ?
B1 F4 F3 58.6(14) . 2 ?



_diffrn_measured_fraction_theta_max 1.000

_diffrn_reflns_theta_full        25.02

_diffrn_measured_fraction_theta_full 1.000

_refine_diff_density_max         2.048

_refine_diff_density_min         -1.844

_refine_diff_density_rms         0.240



####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_bb
_database_code_depnum_ccdc_archive 'CCDC 1417406'
_audit_update_record             
;
2015-08-06 deposited with the CCDC.
2016-04-29 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C20 H24 Cd N2 O5'
_chemical_formula_weight         484.81

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'
Cd Cd -0.8075 1.2024 '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                   8.7092(7)
_cell_length_b                   17.5095(15)
_cell_length_c                   12.4774(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1902.7(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    7411
_cell_measurement_theta_min      2.61
_cell_measurement_theta_max      27.57

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_crystal_density_meas      0
_exptl_crystal_density_diffrn    1.692
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             984
_exptl_absorpt_coefficient_mu    1.183
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            15651
_diffrn_reflns_av_R_equivalents  0.0257
_diffrn_reflns_av_sigmaI/netI    0.0251
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.00
_diffrn_reflns_theta_max         27.58
_reflns_number_total             4214
_reflns_number_gt                3767
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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)+(0.0487P)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   0.56(3)
_refine_ls_number_reflns         4214
_refine_ls_number_parameters     253
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0317
_refine_ls_R_factor_gt           0.0237
_refine_ls_wR_factor_ref         0.0834
_refine_ls_wR_factor_gt          0.0636
_refine_ls_goodness_of_fit_ref   1.198
_refine_ls_restrained_S_all      1.198
_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
Cd1 Cd 0.97694(2) 0.125999(12) 0.92696(6) 0.02566(8) Uani 1 1 d . . .
C4 C 1.1001(5) 0.1220(2) 1.2863(3) 0.0359(9) Uani 1 1 d . . .
H4 H 1.0704 0.0921 1.3443 0.043 Uiso 1 1 calc R . .
C5 C 1.0505(5) 0.1041(2) 1.1843(3) 0.0335(8) Uani 1 1 d . . .
H5 H 0.9852 0.0624 1.1760 0.040 Uiso 1 1 calc R . .
C9 C 1.3716(5) 0.3737(2) 1.5641(3) 0.0393(9) Uani 1 1 d . . .
H9 H 1.4108 0.4004 1.5058 0.047 Uiso 1 1 calc R . .
C1 C 1.1876(5) 0.2013(2) 1.1112(3) 0.0337(8) Uani 1 1 d . . .
H1 H 1.2212 0.2279 1.0511 0.040 Uiso 1 1 calc R . .
C3 C 1.1946(5) 0.1849(2) 1.3019(3) 0.0352(9) Uani 1 1 d . . .
C2 C 1.2404(5) 0.2242(2) 1.2100(4) 0.0380(9) Uani 1 1 d . . .
H2 H 1.3064 0.2657 1.2155 0.046 Uiso 1 1 calc R . .
O5 O 0.8149(3) 0.02595(15) 0.9931(3) 0.0424(7) Uani 1 1 d . . .
C6 C 1.2455(6) 0.2082(2) 1.4111(4) 0.0459(11) Uani 1 1 d . . .
H6A H 1.3544 0.1975 1.4180 0.055 Uiso 1 1 calc R . .
H6B H 1.1920 0.1770 1.4635 0.055 Uiso 1 1 calc R . .
C14 C 0.6279(4) -0.04201(19) 1.2585(3) 0.0294(7) Uani 1 1 d . . .
H14 H 0.5301 -0.0586 1.2896 0.035 Uiso 1 1 calc R . .
C12 C 1.2093(5) 0.2797(2) 1.6399(3) 0.0409(10) Uani 1 1 d . . .
H12 H 1.1367 0.2409 1.6340 0.049 Uiso 1 1 calc R . .
C13 C 0.7579(4) -0.0716(2) 1.3293(3) 0.0288(8) Uani 1 1 d . . .
O2 O 0.7557(3) -0.14080(15) 1.3590(3) 0.0388(7) Uani 1 1 d . . .
C16 C 0.5525(4) 0.0405(2) 1.0559(3) 0.0293(8) Uani 1 1 d . . .
H16 H 0.4715 0.0576 1.0069 0.035 Uiso 1 1 calc R . .
C8 C 1.2662(5) 0.3142(2) 1.5480(3) 0.0370(9) Uani 1 1 d . . .
N1 N 1.0908(4) 0.14311(18) 1.0968(2) 0.0302(7) Uani 1 1 d . . .
C15 C 0.7041(4) 0.0695(2) 1.0108(3) 0.0291(8) Uani 1 1 d . . .
C7 C 1.2187(6) 0.2905(2) 1.4373(5) 0.0571(13) Uani 1 1 d . . .
H7A H 1.1102 0.3014 1.4286 0.069 Uiso 1 1 calc R . .
H7B H 1.2741 0.3216 1.3858 0.069 Uiso 1 1 calc R . .
O4 O 0.7150(4) 0.14072(15) 0.9911(3) 0.0403(7) Uani 1 1 d . . .
O3 O 0.8691(3) -0.02934(16) 1.3520(2) 0.0407(7) Uani 1 1 d . . .
O1 O 0.9767(3) 0.26470(13) 0.9256(4) 0.0417(6) Uani 1 1 d . . .
N2 N 1.3658(4) 0.35726(17) 1.7539(3) 0.0314(7) Uani 1 1 d . . .
C11 C 1.2593(5) 0.3022(2) 1.7404(3) 0.0385(9) Uani 1 1 d . . .
H11 H 1.2181 0.2786 1.8007 0.046 Uiso 1 1 calc R . .
C10 C 1.4168(5) 0.3926(2) 1.6659(3) 0.0368(9) Uani 1 1 d . . .
H10 H 1.4870 0.4322 1.6742 0.044 Uiso 1 1 calc R . .
C17 C 0.5170(4) 0.0746(2) 1.1649(4) 0.0343(9) Uani 1 1 d . . .
H17A H 0.4123 0.0621 1.1847 0.041 Uiso 1 1 calc R . .
H17B H 0.5252 0.1298 1.1609 0.041 Uiso 1 1 calc R . .
C19 C 0.5416(4) -0.0465(2) 1.0622(4) 0.0371(9) Uani 1 1 d . . .
H19A H 0.5693 -0.0681 0.9932 0.045 Uiso 1 1 calc R . .
H19B H 0.4363 -0.0609 1.0773 0.045 Uiso 1 1 calc R . .
C20 C 0.6463(5) -0.0801(2) 1.1486(3) 0.0333(8) Uani 1 1 d . . .
H20A H 0.7522 -0.0749 1.1256 0.040 Uiso 1 1 calc R . .
H20B H 0.6246 -0.1342 1.1557 0.040 Uiso 1 1 calc R . .
C18 C 0.6265(4) 0.04474(19) 1.2504(3) 0.0327(8) Uani 1 1 d . . .
H18A H 0.7295 0.0624 1.2343 0.039 Uiso 1 1 calc R . .
H18B H 0.5973 0.0659 1.3193 0.039 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
Cd1 O3 2.353(3) 2_754 ?
Cd1 N1 2.358(3) . ?
Cd1 N2 2.384(3) 4_454 ?
Cd1 O5 2.396(3) . ?
Cd1 O1 2.429(2) . ?
Cd1 O4 2.431(3) . ?
Cd1 O2 2.491(3) 2_754 ?
C4 C5 1.381(6) . ?
C4 C3 1.388(6) . ?
C5 N1 1.335(5) . ?
C9 C10 1.370(6) . ?
C9 C8 1.403(6) . ?
C1 N1 1.335(5) . ?
C1 C2 1.374(6) . ?
C3 C2 1.396(6) . ?
C3 C6 1.490(6) . ?
O5 C15 1.249(4) . ?
C6 C7 1.497(5) . ?
C14 C18 1.522(5) . ?
C14 C13 1.526(5) . ?
C14 C20 1.533(5) . ?
C12 C11 1.385(6) . ?
C12 C8 1.389(6) . ?
C13 O3 1.251(4) . ?
C13 O2 1.268(4) . ?
O2 Cd1 2.491(3) 2_755 ?
C16 C17 1.517(6) . ?
C16 C15 1.523(5) . ?
C16 C19 1.529(6) . ?
C8 C7 1.500(6) . ?
C15 O4 1.275(4) . ?
O3 Cd1 2.353(3) 2_755 ?
N2 C10 1.337(5) . ?
N2 C11 1.348(5) . ?
N2 Cd1 2.384(3) 4_556 ?
C17 C18 1.524(6) . ?
C19 C20 1.530(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Cd1 N1 102.06(11) 2_754 . ?
O3 Cd1 N2 87.70(11) 2_754 4_454 ?
N1 Cd1 N2 165.61(11) . 4_454 ?
O3 Cd1 O5 86.94(9) 2_754 . ?
N1 Cd1 O5 91.79(12) . . ?
N2 Cd1 O5 99.35(11) 4_454 . ?
O3 Cd1 O1 135.79(12) 2_754 . ?
N1 Cd1 O1 83.08(14) . . ?
N2 Cd1 O1 82.56(14) 4_454 . ?
O5 Cd1 O1 137.15(10) . . ?
O3 Cd1 O4 137.89(9) 2_754 . ?
N1 Cd1 O4 94.89(12) . . ?
N2 Cd1 O4 84.50(11) 4_454 . ?
O5 Cd1 O4 53.95(9) . . ?
O1 Cd1 O4 84.01(9) . . ?
O3 Cd1 O2 53.63(9) 2_754 2_754 ?
N1 Cd1 O2 84.24(11) . 2_754 ?
N2 Cd1 O2 93.35(11) 4_454 2_754 ?
O5 Cd1 O2 138.04(9) . 2_754 ?
O1 Cd1 O2 83.93(10) . 2_754 ?
O4 Cd1 O2 167.92(8) . 2_754 ?
C5 C4 C3 119.7(4) . . ?
N1 C5 C4 123.7(4) . . ?
C10 C9 C8 120.0(4) . . ?
N1 C1 C2 123.7(4) . . ?
C4 C3 C2 116.5(4) . . ?
C4 C3 C6 121.4(4) . . ?
C2 C3 C6 122.1(4) . . ?
C1 C2 C3 119.8(4) . . ?
C15 O5 Cd1 94.0(2) . . ?
C3 C6 C7 114.6(3) . . ?
C18 C14 C13 112.5(3) . . ?
C18 C14 C20 112.0(3) . . ?
C13 C14 C20 107.0(3) . . ?
C11 C12 C8 120.8(4) . . ?
O3 C13 O2 120.7(3) . . ?
O3 C13 C14 120.3(3) . . ?
O2 C13 C14 118.8(3) . . ?
C13 O2 Cd1 89.2(2) . 2_755 ?
C17 C16 C15 112.1(3) . . ?
C17 C16 C19 109.5(3) . . ?
C15 C16 C19 113.9(3) . . ?
C12 C8 C9 116.0(4) . . ?
C12 C8 C7 122.8(4) . . ?
C9 C8 C7 121.2(4) . . ?
C5 N1 C1 116.5(3) . . ?
C5 N1 Cd1 124.0(3) . . ?
C1 N1 Cd1 118.9(2) . . ?
O5 C15 O4 120.3(3) . . ?
O5 C15 C16 122.2(3) . . ?
O4 C15 C16 117.5(3) . . ?
C6 C7 C8 115.1(4) . . ?
C15 O4 Cd1 91.7(2) . . ?
C13 O3 Cd1 96.1(2) . 2_755 ?
C10 N2 C11 117.2(4) . . ?
C10 N2 Cd1 123.5(3) . 4_556 ?
C11 N2 Cd1 118.7(3) . 4_556 ?
N2 C11 C12 122.2(4) . . ?
N2 C10 C9 123.7(4) . . ?
C16 C17 C18 111.4(3) . . ?
C16 C19 C20 112.5(3) . . ?
C19 C20 C14 113.7(3) . . ?
C14 C18 C17 113.2(3) . . ?

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        27.58
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         0.520
_refine_diff_density_min         -0.492
_refine_diff_density_rms         0.164
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_z3
_database_code_depnum_ccdc_archive 'CCDC 1449851'
_audit_update_record             
;
2016-04-18 deposited with the CCDC.
2016-04-29 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C42 H48 Cd2 N4 O8'
_chemical_formula_weight         961.64

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'
Cd Cd 0.1185 4.6533 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   10.0056(5)
_cell_length_b                   10.2640(5)
_cell_length_c                   22.7508(10)
_cell_angle_alpha                84.883(4)
_cell_angle_beta                 81.606(4)
_cell_angle_gamma                63.403(5)
_cell_volume                     2066.07(17)
_cell_formula_units_Z            2
_cell_measurement_temperature    100.0(3)
_cell_measurement_reflns_used    5054
_cell_measurement_theta_min      4.964
_cell_measurement_theta_max      72.943

_exptl_crystal_description       Prism
_exptl_crystal_colour            Colorless
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.14
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.546
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             976
_exptl_absorpt_coefficient_mu    8.706
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.155
_exptl_absorpt_correction_T_max  0.296
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100.0(3)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            14665
_diffrn_reflns_av_R_equivalents  0.0357
_diffrn_reflns_av_sigmaI/netI    0.0479
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         3.93
_diffrn_reflns_theta_max         73.60
_reflns_number_total             8095
_reflns_number_gt                6298
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker FRAMBO'
_computing_cell_refinement       'Bruker FRAMBO'
_computing_data_reduction        'Bruker SAINT'
_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)+(0.0514P)²+3.6885P] 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_number_reflns         8095
_refine_ls_number_parameters     568
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0642
_refine_ls_R_factor_gt           0.0450
_refine_ls_wR_factor_ref         0.1179
_refine_ls_wR_factor_gt          0.1058
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_restrained_S_all      1.023
_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
Cd1 Cd 0.91049(4) 0.41287(4) 0.065630(14) 0.03686(11) Uani 1 1 d . . .
Cd2 Cd 0.82045(4) 0.10332(4) 0.437942(15) 0.04249(12) Uani 1 1 d . . .
O1 O 0.8361(4) 0.2837(4) 0.14764(17) 0.0544(11) Uani 1 1 d . . .
O2 O 0.6646(4) 0.4934(4) 0.11480(15) 0.0453(9) Uani 1 1 d . . .
O3 O 0.6682(5) 0.1173(5) 0.36649(18) 0.0537(10) Uani 1 1 d . . .
O4 O 0.6593(4) 0.3260(4) 0.38650(16) 0.0468(9) Uani 1 1 d . . .
O5 O 0.8489(4) 0.7760(4) -0.06798(15) 0.0440(9) Uani 1 1 d . . .
O6 O 0.8502(4) 0.6260(4) 0.00666(15) 0.0449(9) Uani 1 1 d . . .
O7 O 0.8734(5) -0.1280(4) 0.46338(18) 0.0563(10) Uani 1 1 d . . .
O8 O 1.0848(5) -0.1781(5) 0.49737(19) 0.0651(12) Uani 1 1 d . . .
N1 N 0.9552(5) 0.5386(5) 0.13404(18) 0.0454(11) Uani 1 1 d . . .
N2 N 0.3808(5) 0.8311(5) 0.48596(19) 0.0439(10) Uani 1 1 d . . .
N3 N 1.0186(5) 0.0617(6) 0.36275(19) 0.0470(11) Uani 1 1 d . . .
N4 N 1.1473(5) -0.3123(6) 0.0082(2) 0.0474(11) Uani 1 1 d . . .
C1 C 0.7033(6) 0.3856(6) 0.1509(2) 0.0438(13) Uani 1 1 d . . .
C2 C 0.5860(5) 0.3832(6) 0.2008(2) 0.0388(11) Uani 1 1 d . . .
H2 H 0.4856 0.4321 0.1855 0.047 Uiso 1 1 calc R . .
C3 C 0.6100(6) 0.2305(6) 0.2237(2) 0.0426(12) Uani 1 1 d . . .
H3A H 0.6082 0.1747 0.1907 0.051 Uiso 1 1 calc R . .
H3B H 0.7099 0.1786 0.2381 0.051 Uiso 1 1 calc R . .
C4 C 0.4879(6) 0.2383(6) 0.2740(2) 0.0424(12) Uani 1 1 d . . .
H4A H 0.5090 0.1385 0.2893 0.051 Uiso 1 1 calc R . .
H4B H 0.3893 0.2809 0.2583 0.051 Uiso 1 1 calc R . .
C5 C 0.4791(6) 0.3302(6) 0.3251(2) 0.0410(12) Uani 1 1 d . . .
H5 H 0.3863 0.3440 0.3525 0.049 Uiso 1 1 calc R . .
C6 C 0.4589(6) 0.4826(6) 0.3024(2) 0.0422(12) Uani 1 1 d . . .
H6A H 0.3591 0.5368 0.2880 0.051 Uiso 1 1 calc R . .
H6B H 0.4623 0.5369 0.3356 0.051 Uiso 1 1 calc R . .
C7 C 0.5822(6) 0.4735(6) 0.2519(2) 0.0390(11) Uani 1 1 d . . .
H7A H 0.6812 0.4283 0.2674 0.047 Uiso 1 1 calc R . .
H7B H 0.5633 0.5730 0.2368 0.047 Uiso 1 1 calc R . .
C8 C 0.6113(6) 0.2536(7) 0.3613(2) 0.0436(12) Uani 1 1 d . . .
C9 C 0.7843(5) 0.7432(5) -0.02181(19) 0.0323(10) Uani 1 1 d . . .
C10 C 0.6265(5) 0.8518(5) 0.0016(2) 0.0332(10) Uani 1 1 d . . .
H10 H 0.5869 0.8047 0.0355 0.040 Uiso 1 1 calc R . .
C11 C 0.6338(5) 0.9841(6) 0.0245(2) 0.0422(12) Uani 1 1 d . . .
H11A H 0.6962 0.9524 0.0578 0.051 Uiso 1 1 calc R . .
H11B H 0.6828 1.0252 -0.0077 0.051 Uiso 1 1 calc R . .
C12 C 0.5228(5) 0.8974(6) -0.0459(2) 0.0403(12) Uani 1 1 d . . .
H12A H 0.5134 0.8115 -0.0576 0.048 Uiso 1 1 calc R . .
H12B H 0.5667 0.9344 -0.0814 0.048 Uiso 1 1 calc R . .
C13 C 0.9854(6) -0.2111(6) 0.4889(2) 0.0383(11) Uani 1 1 d . . .
C14 C 1.0076(7) -0.3634(6) 0.5088(3) 0.0503(14) Uani 1 1 d . . .
H14 H 1.0636 -0.3914 0.5444 0.060 Uiso 1 1 calc R . .
C15 C 1.1087(6) -0.4674(6) 0.4588(3) 0.0483(13) Uani 1 1 d . . .
H15A H 1.0607 -0.4352 0.4217 0.058 Uiso 1 1 calc R . .
H15B H 1.2067 -0.4631 0.4517 0.058 Uiso 1 1 calc R . .
C16 C 0.8651(7) -0.3782(7) 0.5259(3) 0.0599(17) Uani 1 1 d . . .
H16A H 0.8030 -0.3413 0.4926 0.072 Uiso 1 1 calc R . .
H16B H 0.8078 -0.3169 0.5606 0.072 Uiso 1 1 calc R . .
C17 C 1.0565(6) 0.4712(7) 0.1709(3) 0.0506(14) Uani 1 1 d . . .
H17 H 1.1290 0.3740 0.1628 0.061 Uiso 1 1 calc R . .
C18 C 1.0633(6) 0.5341(8) 0.2207(3) 0.0577(16) Uani 1 1 d . . .
H18 H 1.1376 0.4794 0.2464 0.069 Uiso 1 1 calc R . .
C19 C 0.9633(7) 0.6751(7) 0.2333(3) 0.0550(15) Uani 1 1 d . . .
C20 C 0.8588(10) 0.7467(9) 0.1936(3) 0.083(2) Uani 1 1 d U . .
H20 H 0.7873 0.8452 0.1998 0.099 Uiso 1 1 calc R . .
C21 C 0.8584(9) 0.6766(8) 0.1461(3) 0.087(3) Uani 1 1 d . . .
H21 H 0.7850 0.7286 0.1198 0.105 Uiso 1 1 calc R . .
C22 C 0.9635(8) 0.7460(9) 0.2886(3) 0.068(2) Uani 1 1 d . . .
H22A H 1.0528 0.6797 0.3083 0.082 Uiso 1 1 calc R . .
H22B H 0.9738 0.8366 0.2767 0.082 Uiso 1 1 calc R . .
C23 C 0.8304(8) 0.7816(10) 0.3311(3) 0.080(3) Uani 1 1 d . . .
H23A H 0.8563 0.8015 0.3686 0.096 Uiso 1 1 calc R . .
H23B H 0.7536 0.8758 0.3170 0.096 Uiso 1 1 calc R . .
C24 C 0.7577(10) 0.6955(10) 0.3468(4) 0.083(2) Uani 1 1 d U . .
H24A H 0.8312 0.6014 0.3625 0.099 Uiso 1 1 calc R . .
H24B H 0.7293 0.6747 0.3101 0.099 Uiso 1 1 calc R . .
C25 C 0.6154(9) 0.7523(9) 0.3927(3) 0.068(2) Uani 1 1 d . . .
C26 C 0.5685(7) 0.6518(8) 0.4215(3) 0.0572(16) Uani 1 1 d . . .
H26 H 0.6160 0.5533 0.4096 0.069 Uiso 1 1 calc R . .
C27 C 0.4535(7) 0.6957(7) 0.4670(3) 0.0507(14) Uani 1 1 d . . .
H27 H 0.4241 0.6249 0.4862 0.061 Uiso 1 1 calc R . .
C28 C 0.4229(7) 0.9294(7) 0.4591(2) 0.0453(13) Uani 1 1 d . . .
H28 H 0.3717 1.0272 0.4719 0.054 Uiso 1 1 calc R . .
C29 C 0.5403(8) 0.8932(8) 0.4126(2) 0.0574(17) Uani 1 1 d . . .
H29 H 0.5684 0.9658 0.3947 0.069 Uiso 1 1 calc R . .
C30 C 0.9953(8) 0.1435(7) 0.3124(3) 0.0615(17) Uani 1 1 d . . .
H30 H 0.9018 0.2275 0.3106 0.074 Uiso 1 1 calc R . .
C31 C 1.1025(8) 0.1100(8) 0.2631(3) 0.0661(19) Uani 1 1 d . . .
H31 H 1.0806 0.1685 0.2277 0.079 Uiso 1 1 calc R . .
C32 C 1.2425(6) -0.0095(6) 0.2653(2) 0.0469(13) Uani 1 1 d . A .
C33 C 1.2651(6) -0.0914(7) 0.3178(2) 0.0472(13) Uani 1 1 d . . .
H33 H 1.3587 -0.1739 0.3215 0.057 Uiso 1 1 calc R . .
C34 C 1.1518(6) -0.0534(7) 0.3648(2) 0.0491(14) Uani 1 1 d . . .
H34 H 1.1696 -0.1120 0.4002 0.059 Uiso 1 1 calc R . .
C35 C 1.3629(7) -0.0529(7) 0.2122(3) 0.0541(15) Uani 1 1 d . . .
H35A H 1.3547 0.0353 0.1883 0.065 Uiso 1 1 d R A .
H35B H 1.4640 -0.1012 0.2259 0.065 Uiso 1 1 d R . .
C36A C 1.3435(15) -0.1531(16) 0.1753(6) 0.044(3) Uani 0.50 1 d P A 1
H36A H 1.3434 -0.2372 0.2002 0.053 Uiso 0.50 1 calc PR A 1
H36B H 1.4295 -0.1908 0.1436 0.053 Uiso 0.50 1 calc PR A 1
C37A C 1.1961(11) -0.0777(11) 0.1467(4) 0.038(2) Uani 0.50 1 d P A 1
H37A H 1.1109 -0.0604 0.1782 0.046 Uiso 0.50 1 calc PR A 1
H37B H 1.1856 0.0187 0.1303 0.046 Uiso 0.50 1 calc PR A 1
C38A C 1.254(2) -0.361(2) 0.0368(11) 0.048(5) Uani 0.50 1 d P A 1
H38A H 1.3306 -0.4546 0.0252 0.057 Uiso 0.50 1 calc PR A 1
C39A C 1.2831(16) -0.3028(16) 0.0837(6) 0.040(3) Uani 0.50 1 d P A 1
H39A H 1.3672 -0.3583 0.1048 0.048 Uiso 0.50 1 calc PR A 1
C40A C 1.1830(13) -0.1585(12) 0.0985(5) 0.034(2) Uani 0.50 1 d P A 1
C41A C 1.0624(11) -0.0894(12) 0.0635(5) 0.041(2) Uani 0.50 1 d P A 1
H41A H 0.9904 0.0081 0.0716 0.049 Uiso 0.50 1 calc PR A 1
C42A C 1.0468(12) -0.1588(13) 0.0186(6) 0.040(3) Uani 0.50 1 d P A 1
H42A H 0.9697 -0.1069 -0.0062 0.048 Uiso 0.50 1 calc PR A 1
C36B C 1.3201(19) -0.0975(19) 0.1552(6) 0.051(4) Uani 0.50 1 d P A 2
H36D H 1.2347 -0.0116 0.1402 0.061 Uiso 0.50 1 calc PR A 2
H36C H 1.4068 -0.1252 0.1237 0.061 Uiso 0.50 1 calc PR A 2
C37B C 1.2778(14) -0.2206(14) 0.1665(5) 0.049(3) Uani 0.50 1 d P A 2
H37C H 1.1919 -0.1940 0.1983 0.059 Uiso 0.50 1 calc PR A 2
H37D H 1.3636 -0.3077 0.1806 0.059 Uiso 0.50 1 calc PR A 2
C38B C 1.293(2) -0.405(2) 0.0290(9) 0.036(4) Uani 0.50 1 d P A 2
H38B H 1.3574 -0.4932 0.0091 0.043 Uiso 0.50 1 calc PR A 2
C39B C 1.3368(15) -0.3702(18) 0.0755(6) 0.048(4) Uani 0.50 1 d P A 2
H39B H 1.4379 -0.4224 0.0841 0.058 Uiso 0.50 1 calc PR A 2
C40B C 1.2346(15) -0.2579(18) 0.1107(6) 0.040(3) Uani 0.50 1 d P A 2
C41B C 1.0928(13) -0.1756(15) 0.0937(5) 0.047(3) Uani 0.50 1 d P A 2
H41B H 1.0218 -0.0941 0.1161 0.057 Uiso 0.50 1 calc PR A 2
C42B C 1.0552(11) -0.2124(14) 0.0442(5) 0.040(3) Uani 0.50 1 d P A 2
H42B H 0.9538 -0.1604 0.0358 0.048 Uiso 0.50 1 calc PR A 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
Cd1 N4 2.313(5) 2_755 ?
Cd1 N1 2.316(5) . ?
Cd1 O5 2.324(3) 2_765 ?
Cd1 O6 2.341(3) . ?
Cd1 O2 2.351(3) . ?
Cd1 O1 2.414(4) . ?
Cd1 O6 2.590(4) 2_765 ?
Cd1 C1 2.718(5) . ?
Cd2 O8 2.216(4) 2_756 ?
Cd2 O7 2.229(4) . ?
Cd2 N3 2.329(4) . ?
Cd2 O3 2.339(4) . ?
Cd2 N2 2.341(4) 2_666 ?
Cd2 O4 2.443(4) . ?
Cd2 C8 2.737(6) . ?
O1 C1 1.267(6) . ?
O2 C1 1.263(6) . ?
O3 C8 1.254(7) . ?
O4 C8 1.259(7) . ?
O5 C9 1.252(5) . ?
O5 Cd1 2.324(3) 2_765 ?
O6 C9 1.256(6) . ?
O6 Cd1 2.590(4) 2_765 ?
O7 C13 1.252(6) . ?
O8 C13 1.229(6) . ?
O8 Cd2 2.216(4) 2_756 ?
N1 C17 1.314(7) . ?
N1 C21 1.336(7) . ?
N2 C27 1.325(7) . ?
N2 C28 1.329(7) . ?
N2 Cd2 2.341(4) 2_666 ?
N3 C34 1.331(7) . ?
N3 C30 1.342(7) . ?
N4 C38A 1.22(3) . ?
N4 C42B 1.285(12) . ?
N4 C42A 1.458(13) . ?
N4 C38B 1.458(17) . ?
N4 Cd1 2.313(5) 2_755 ?
C1 C2 1.516(7) . ?
C2 C3 1.529(7) . ?
C2 C7 1.538(7) . ?
C3 C4 1.527(7) . ?
C4 C5 1.529(7) . ?
C5 C8 1.523(7) . ?
C5 C6 1.535(7) . ?
C6 C7 1.534(7) . ?
C9 C10 1.518(6) . ?
C10 C12 1.506(6) . ?
C10 C11 1.532(7) . ?
C11 C12 1.532(6) 2_675 ?
C12 C11 1.532(6) 2_675 ?
C13 C14 1.513(8) . ?
C14 C16 1.492(8) . ?
C14 C15 1.540(8) . ?
C15 C16 1.502(8) 2_746 ?
C16 C15 1.502(8) 2_746 ?
C17 C18 1.378(8) . ?
C18 C19 1.368(9) . ?
C19 C20 1.384(9) . ?
C19 C22 1.509(8) . ?
C20 C21 1.353(9) . ?
C22 C23 1.447(9) . ?
C23 C24 1.372(10) . ?
C24 C25 1.546(10) . ?
C25 C29 1.380(10) . ?
C25 C26 1.392(9) . ?
C26 C27 1.367(8) . ?
C28 C29 1.397(8) . ?
C30 C31 1.385(8) . ?
C31 C32 1.393(9) . ?
C32 C33 1.384(8) . ?
C32 C35 1.516(8) . ?
C33 C34 1.380(8) . ?
C35 C36A 1.478(16) . ?
C35 C36B 1.588(15) . ?
C36A C37A 1.538(16) . ?
C37A C40A 1.485(15) . ?
C38A C39A 1.39(3) . ?
C39A C40A 1.405(16) . ?
C40A C41A 1.417(15) . ?
C41A C42A 1.360(17) . ?
C36B C37B 1.494(19) . ?
C37B C40B 1.530(17) . ?
C38B C39B 1.34(3) . ?
C39B C40B 1.373(18) . ?
C40B C41B 1.380(17) . ?
C41B C42B 1.371(16) . ?

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
N4 Cd1 N1 173.56(16) 2_755 . ?
N4 Cd1 O5 94.27(15) 2_755 2_765 ?
N1 Cd1 O5 90.54(14) . 2_765 ?
N4 Cd1 O6 88.79(16) 2_755 . ?
N1 Cd1 O6 84.94(15) . . ?
O5 Cd1 O6 124.97(12) 2_765 . ?
N4 Cd1 O2 91.11(14) 2_755 . ?
N1 Cd1 O2 87.80(15) . . ?
O5 Cd1 O2 141.17(12) 2_765 . ?
O6 Cd1 O2 93.52(12) . . ?
N4 Cd1 O1 96.14(16) 2_755 . ?
N1 Cd1 O1 88.48(16) . . ?
O5 Cd1 O1 85.75(12) 2_765 . ?
O6 Cd1 O1 148.53(12) . . ?
O2 Cd1 O1 55.44(12) . . ?
N4 Cd1 O6 84.74(14) 2_755 2_765 ?
N1 Cd1 O6 94.85(14) . 2_765 ?
O5 Cd1 O6 52.48(11) 2_765 2_765 ?
O6 Cd1 O6 73.27(12) . 2_765 ?
O2 Cd1 O6 166.19(11) . 2_765 ?
O1 Cd1 O6 138.05(11) . 2_765 ?
N4 Cd1 C1 94.85(16) 2_755 . ?
N1 Cd1 C1 87.13(17) . . ?
O5 Cd1 C1 113.50(14) 2_765 . ?
O6 Cd1 C1 120.95(14) . . ?
O2 Cd1 C1 27.67(14) . . ?
O1 Cd1 C1 27.78(14) . . ?
O6 Cd1 C1 165.78(13) 2_765 . ?
O8 Cd2 O7 106.11(16) 2_756 . ?
O8 Cd2 N3 95.01(17) 2_756 . ?
O7 Cd2 N3 98.41(17) . . ?
O8 Cd2 O3 158.82(17) 2_756 . ?
O7 Cd2 O3 93.70(15) . . ?
N3 Cd2 O3 89.29(15) . . ?
O8 Cd2 N2 81.52(17) 2_756 2_666 ?
O7 Cd2 N2 87.05(16) . 2_666 ?
N3 Cd2 N2 174.20(17) . 2_666 ?
O3 Cd2 N2 92.33(15) . 2_666 ?
O8 Cd2 O4 104.66(16) 2_756 . ?
O7 Cd2 O4 146.90(14) . . ?
N3 Cd2 O4 90.76(15) . . ?
O3 Cd2 O4 54.46(13) . . ?
N2 Cd2 O4 85.66(14) 2_666 . ?
O8 Cd2 C8 131.72(18) 2_756 . ?
O7 Cd2 C8 120.01(16) . . ?
N3 Cd2 C8 91.86(15) . . ?
O3 Cd2 C8 27.19(15) . . ?
N2 Cd2 C8 87.06(15) 2_666 . ?
O4 Cd2 C8 27.39(15) . . ?
C1 O1 Cd1 89.6(3) . . ?
C1 O2 Cd1 92.5(3) . . ?
C8 O3 Cd2 94.4(3) . . ?
C8 O4 Cd2 89.4(3) . . ?
C9 O5 Cd1 99.3(3) . 2_765 ?
C9 O6 Cd1 165.3(3) . . ?
C9 O6 Cd1 86.6(3) . 2_765 ?
Cd1 O6 Cd1 106.73(12) . 2_765 ?
C13 O7 Cd2 123.3(4) . . ?
C13 O8 Cd2 146.4(4) . 2_756 ?
C17 N1 C21 116.3(5) . . ?
C17 N1 Cd1 121.7(4) . . ?
C21 N1 Cd1 120.5(4) . . ?
C27 N2 C28 117.8(5) . . ?
C27 N2 Cd2 121.2(4) . 2_666 ?
C28 N2 Cd2 121.0(4) . 2_666 ?
C34 N3 C30 117.7(5) . . ?
C34 N3 Cd2 121.6(4) . . ?
C30 N3 Cd2 120.1(4) . . ?
C38A N4 C42B 97.6(10) . . ?
C38A N4 C42A 113.6(11) . . ?
C42B N4 C42A 30.9(5) . . ?
C38A N4 C38B 17.5(13) . . ?
C42B N4 C38B 114.8(10) . . ?
C42A N4 C38B 130.2(10) . . ?
C38A N4 Cd1 131.3(9) . 2_755 ?
C42B N4 Cd1 127.5(6) . 2_755 ?
C42A N4 Cd1 114.8(6) . 2_755 ?
C38B N4 Cd1 114.0(8) . 2_755 ?
O2 C1 O1 122.4(5) . . ?
O2 C1 C2 117.7(4) . . ?
O1 C1 C2 119.8(5) . . ?
O2 C1 Cd1 59.8(3) . . ?
O1 C1 Cd1 62.7(3) . . ?
C2 C1 Cd1 174.7(4) . . ?
C1 C2 C3 114.5(4) . . ?
C1 C2 C7 108.5(4) . . ?
C3 C2 C7 110.2(4) . . ?
C4 C3 C2 110.9(4) . . ?
C3 C4 C5 112.1(4) . . ?
C8 C5 C4 112.5(4) . . ?
C8 C5 C6 112.6(5) . . ?
C4 C5 C6 110.9(4) . . ?
C7 C6 C5 111.3(4) . . ?
C6 C7 C2 111.0(4) . . ?
O3 C8 O4 121.2(5) . . ?
O3 C8 C5 118.1(5) . . ?
O4 C8 C5 120.6(5) . . ?
O3 C8 Cd2 58.4(3) . . ?
O4 C8 Cd2 63.2(3) . . ?
C5 C8 Cd2 171.3(4) . . ?
O5 C9 O6 121.2(4) . . ?
O5 C9 C10 118.9(4) . . ?
O6 C9 C10 119.8(4) . . ?
C12 C10 C9 111.0(4) . . ?
C12 C10 C11 110.8(4) . . ?
C9 C10 C11 108.9(4) . . ?
C12 C11 C10 112.0(4) 2_675 . ?
C10 C12 C11 111.7(4) . 2_675 ?
O8 C13 O7 123.4(5) . . ?
O8 C13 C14 116.4(5) . . ?
O7 C13 C14 120.2(5) . . ?
C16 C14 C13 114.6(5) . . ?
C16 C14 C15 111.3(5) . . ?
C13 C14 C15 107.7(5) . . ?
C16 C15 C14 111.7(5) 2_746 . ?
C14 C16 C15 113.1(5) . 2_746 ?
N1 C17 C18 123.6(5) . . ?
C19 C18 C17 120.1(6) . . ?
C18 C19 C20 116.2(6) . . ?
C18 C19 C22 121.7(6) . . ?
C20 C19 C22 122.1(6) . . ?
C21 C20 C19 120.1(7) . . ?
N1 C21 C20 123.8(6) . . ?
C23 C22 C19 114.5(6) . . ?
C24 C23 C22 125.9(7) . . ?
C23 C24 C25 118.7(7) . . ?
C29 C25 C26 116.6(6) . . ?
C29 C25 C24 124.8(6) . . ?
C26 C25 C24 118.2(7) . . ?
C27 C26 C25 119.6(6) . . ?
N2 C27 C26 123.9(6) . . ?
N2 C28 C29 121.9(6) . . ?
C25 C29 C28 120.3(6) . . ?
N3 C30 C31 122.4(6) . . ?
C30 C31 C32 119.9(6) . . ?
C33 C32 C31 116.8(5) . . ?
C33 C32 C35 121.0(5) . . ?
C31 C32 C35 122.2(5) . . ?
C34 C33 C32 120.1(6) . . ?
N3 C34 C33 123.0(5) . . ?
C36A C35 C32 109.6(7) . . ?
C36A C35 C36B 25.1(6) . . ?
C32 C35 C36B 115.6(7) . . ?
C35 C36A C37A 112.0(10) . . ?
C40A C37A C36A 115.6(9) . . ?
N4 C38A C39A 130.6(13) . . ?
C38A C39A C40A 117.3(14) . . ?
C39A C40A C41A 115.1(11) . . ?
C39A C40A C37A 125.0(11) . . ?
C41A C40A C37A 119.8(10) . . ?
C42A C41A C40A 121.8(10) . . ?
C41A C42A N4 120.6(10) . . ?
C37B C36B C35 113.7(10) . . ?
C36B C37B C40B 111.9(10) . . ?
C39B C38B N4 121.7(14) . . ?
C38B C39B C40B 119.3(14) . . ?
C39B C40B C41B 118.7(12) . . ?
C39B C40B C37B 121.0(12) . . ?
C41B C40B C37B 120.3(14) . . ?
C42B C41B C40B 119.5(11) . . ?
N4 C42B C41B 124.6(9) . . ?

_diffrn_measured_fraction_theta_max 0.970
_diffrn_reflns_theta_full        73.60
_diffrn_measured_fraction_theta_full 0.970
_refine_diff_density_max         1.801
_refine_diff_density_min         -1.201
_refine_diff_density_rms         0.097
