# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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_a
_database_code_depnum_ccdc_archive 'CCDC 1833733'
_audit_update_record             
;
2018-03-30 deposited with the CCDC.
2018-10-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H15 N O8 Zn2'
_chemical_formula_sum            'C24 H15 N O8 Zn2'
_chemical_formula_weight         576.11

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           Monoclinic
_symmetry_space_group_name_H-M   'P2(1)/n  '
_symmetry_space_group_name_Hall  '-P 2yn'

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

_cell_length_a                   9.6600(11)
_cell_length_b                   22.258(3)
_cell_length_c                   11.3838(13)
_cell_angle_alpha                90.00
_cell_angle_beta                 106.975(2)
_cell_angle_gamma                90.00
_cell_volume                     2341.0(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2462
_cell_measurement_theta_min      2.44
_cell_measurement_theta_max      23.32

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.256
_exptl_crystal_size_mid          0.213
_exptl_crystal_size_min          0.186
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.635
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1160
_exptl_absorpt_coefficient_mu    2.099
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.591
_exptl_absorpt_correction_T_max  0.677
_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  'CCD area detector'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_decay_%        none
_diffrn_reflns_number            12716
_diffrn_reflns_av_R_equivalents  0.0397
_diffrn_reflns_av_sigmaI/netI    0.0479
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.83
_diffrn_reflns_theta_max         26.02
_reflns_number_total             4595
_reflns_number_gt                3523
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 2002)'
_computing_cell_refinement       'SAINT (Bruker, 2002)'
_computing_data_reduction        'SHELXS97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXS97 (Sheldrick, 1997)'
_computing_publication_material  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)+(0.0245P)²+5.4231P] 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         4595
_refine_ls_number_parameters     316
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0585
_refine_ls_R_factor_gt           0.0405
_refine_ls_wR_factor_ref         0.1014
_refine_ls_wR_factor_gt          0.0947
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_restrained_S_all      1.088
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 1.0416(5) 0.02661(18) 0.8190(4) 0.0301(10) Uani 1 1 d . . .
C2 C 1.0553(4) 0.04626(18) 0.6990(4) 0.0256(9) Uani 1 1 d . . .
C3 C 1.1660(4) 0.02360(17) 0.6549(4) 0.0261(9) Uani 1 1 d . . .
H3A H 1.2338 -0.0032 0.7017 0.031 Uiso 1 1 calc R . .
C4 C 1.1724(4) 0.04158(17) 0.5423(4) 0.0246(9) Uani 1 1 d . . .
C5 C 1.0710(4) 0.08087(17) 0.4700(4) 0.0259(9) Uani 1 1 d . . .
H5A H 1.0798 0.0928 0.3943 0.031 Uiso 1 1 calc R . .
C6 C 0.9553(4) 0.10291(16) 0.5094(4) 0.0249(9) Uani 1 1 d . . .
C7 C 0.9549(4) 0.08633(17) 0.6274(4) 0.0264(9) Uani 1 1 d . . .
H7A H 0.8849 0.1026 0.6594 0.032 Uiso 1 1 calc R . .
C8 C 1.2853(4) 0.01673(17) 0.4890(4) 0.0249(9) Uani 1 1 d . . .
C9 C 0.8497(5) 0.15645(18) 0.3119(4) 0.0373(11) Uani 1 1 d . . .
H9A H 0.7513 0.1568 0.2577 0.045 Uiso 1 1 calc R . .
H9B H 0.9037 0.1270 0.2802 0.045 Uiso 1 1 calc R . .
C10 C 0.9164(5) 0.21814(19) 0.3079(4) 0.0361(11) Uani 1 1 d . . .
C11 C 0.8444(6) 0.2613(2) 0.2289(5) 0.0618(18) Uani 1 1 d . . .
H11A H 0.7554 0.2521 0.1733 0.074 Uiso 1 1 calc R . .
C12 C 0.9003(7) 0.3188(2) 0.2289(6) 0.0676(19) Uani 1 1 d . . .
H12A H 0.8495 0.3470 0.1724 0.081 Uiso 1 1 calc R . .
C13 C 1.0285(5) 0.33412(19) 0.3107(4) 0.0376(11) Uani 1 1 d . . .
C14 C 1.1034(7) 0.2911(2) 0.3880(6) 0.075(2) Uani 1 1 d . . .
H14A H 1.1926 0.3004 0.4433 0.091 Uiso 1 1 calc R . .
C15 C 1.0486(7) 0.2334(3) 0.3854(7) 0.087(3) Uani 1 1 d . . .
H15A H 1.1030 0.2044 0.4377 0.105 Uiso 1 1 calc R . .
C16 C 1.0884(5) 0.39633(19) 0.3162(5) 0.0360(11) Uani 1 1 d . . .
C17 C 0.7247(5) 0.15971(18) 0.4721(5) 0.0360(11) Uani 1 1 d . . .
H17A H 0.7101 0.1333 0.5352 0.043 Uiso 1 1 calc R . .
H17B H 0.6379 0.1584 0.4028 0.043 Uiso 1 1 calc R . .
C18 C 0.7467(5) 0.22359(18) 0.5219(4) 0.0363(11) Uani 1 1 d . . .
C19 C 0.6443(6) 0.2659(2) 0.4795(6) 0.0655(19) Uani 1 1 d . . .
H19A H 0.5567 0.2550 0.4237 0.079 Uiso 1 1 calc R . .
C20 C 0.6668(7) 0.3252(2) 0.5172(6) 0.075(2) Uani 1 1 d . . .
H20A H 0.5952 0.3536 0.4850 0.091 Uiso 1 1 calc R . .
C21 C 0.7926(5) 0.34227(19) 0.6009(4) 0.0362(11) Uani 1 1 d . . .
C22 C 0.8944(7) 0.2996(2) 0.6466(6) 0.073(2) Uani 1 1 d . . .
H22A H 0.9808 0.3102 0.7045 0.088 Uiso 1 1 calc R . .
C23 C 0.8711(7) 0.2408(2) 0.6081(6) 0.081(2) Uani 1 1 d . . .
H23A H 0.9416 0.2121 0.6416 0.097 Uiso 1 1 calc R . .
C24 C 0.8196(6) 0.40584(19) 0.6409(4) 0.0360(11) Uani 1 1 d . . .
N N 0.8467(4) 0.13745(15) 0.4331(3) 0.0300(8) Uani 1 1 d . . .
O1 O 1.1201(4) -0.01634(14) 0.8728(3) 0.0405(8) Uani 1 1 d . . .
O2 O 0.9478(3) 0.05297(13) 0.8585(3) 0.0362(8) Uani 1 1 d . . .
O3 O 1.3736(3) -0.02165(12) 0.5504(3) 0.0318(7) Uani 1 1 d . . .
O4 O 1.2826(4) 0.03331(15) 0.3830(3) 0.0419(8) Uani 1 1 d . . .
O7 O 0.9388(4) 0.41977(14) 0.7149(3) 0.0428(8) Uani 1 1 d . . .
O8 O 0.7179(4) 0.44240(14) 0.5994(3) 0.0553(10) Uani 1 1 d . . .
O5 O 1.1816(4) 0.41131(14) 0.4130(3) 0.0496(9) Uani 1 1 d . . .
O6 O 1.0408(4) 0.42917(14) 0.2240(3) 0.0522(10) Uani 1 1 d . . .
Zn1 Zn 1.17783(5) -0.02506(2) 1.04932(5) 0.02746(14) Uani 1 1 d . . .
Zn2 Zn 1.55580(6) -0.01160(2) 0.67832(4) 0.02660(14) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.262(5) . ?
C1 O2 1.266(5) . ?
C1 C2 1.478(6) . ?
C2 C7 1.393(6) . ?
C2 C3 1.400(5) . ?
C3 C4 1.362(6) . ?
C4 C5 1.389(6) . ?
C4 C8 1.500(5) . ?
C5 C6 1.408(6) . ?
C6 N 1.383(5) . ?
C6 C7 1.394(6) . ?
C8 O4 1.255(5) . ?
C8 O3 1.264(5) . ?
C9 N 1.451(6) . ?
C9 C10 1.523(6) . ?
C10 C11 1.360(6) . ?
C10 C15 1.366(7) . ?
C11 C12 1.388(7) . ?
C12 C13 1.358(7) . ?
C13 C14 1.358(7) . ?
C13 C16 1.495(6) . ?
C14 C15 1.386(7) . ?
C16 O5 1.248(6) . ?
C16 O6 1.252(5) . ?
C17 N 1.462(6) . ?
C17 C18 1.522(6) . ?
C18 C19 1.348(6) . ?
C18 C23 1.366(7) . ?
C19 C20 1.385(7) . ?
C20 C21 1.362(7) . ?
C21 C22 1.356(7) . ?
C21 C24 1.486(6) . ?
C22 C23 1.379(7) . ?
C24 O7 1.251(6) . ?
C24 O8 1.257(5) . ?
O1 Zn1 1.932(3) . ?
O2 Zn1 1.925(3) 3_757 ?
O3 Zn2 1.942(3) . ?
O4 Zn2 1.948(3) 3_856 ?
O7 Zn2 1.943(3) 2_756 ?
O8 Zn1 1.931(3) 4_565 ?
O5 Zn1 1.922(3) 2_756 ?
O6 Zn2 1.924(3) 4_565 ?
Zn1 O5 1.922(3) 2_746 ?
Zn1 O2 1.925(3) 3_757 ?
Zn1 O8 1.931(3) 4_666 ?
Zn2 O6 1.924(3) 4_666 ?
Zn2 O7 1.943(3) 2_746 ?
Zn2 O4 1.948(3) 3_856 ?

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 C1 O2 124.7(4) . . ?
O1 C1 C2 118.0(4) . . ?
O2 C1 C2 117.3(4) . . ?
C7 C2 C3 119.7(4) . . ?
C7 C2 C1 119.7(4) . . ?
C3 C2 C1 120.6(4) . . ?
C4 C3 C2 118.7(4) . . ?
C3 C4 C5 121.6(4) . . ?
C3 C4 C8 120.7(4) . . ?
C5 C4 C8 117.6(4) . . ?
C4 C5 C6 121.3(4) . . ?
N C6 C7 122.5(4) . . ?
N C6 C5 121.4(4) . . ?
C7 C6 C5 116.1(4) . . ?
C2 C7 C6 122.4(4) . . ?
O4 C8 O3 123.5(4) . . ?
O4 C8 C4 117.8(4) . . ?
O3 C8 C4 118.6(4) . . ?
N C9 C10 114.6(4) . . ?
C11 C10 C15 116.9(4) . . ?
C11 C10 C9 121.2(4) . . ?
C15 C10 C9 121.9(4) . . ?
C10 C11 C12 121.8(5) . . ?
C13 C12 C11 120.6(5) . . ?
C14 C13 C12 118.3(4) . . ?
C14 C13 C16 120.0(4) . . ?
C12 C13 C16 121.7(4) . . ?
C13 C14 C15 120.7(5) . . ?
C10 C15 C14 121.6(5) . . ?
O5 C16 O6 125.3(4) . . ?
O5 C16 C13 117.1(4) . . ?
O6 C16 C13 117.6(4) . . ?
N C17 C18 113.1(4) . . ?
C19 C18 C23 117.4(4) . . ?
C19 C18 C17 120.8(4) . . ?
C23 C18 C17 121.8(4) . . ?
C18 C19 C20 121.5(5) . . ?
C21 C20 C19 120.6(5) . . ?
C22 C21 C20 118.2(4) . . ?
C22 C21 C24 120.4(5) . . ?
C20 C21 C24 121.4(4) . . ?
C21 C22 C23 120.7(5) . . ?
C18 C23 C22 121.5(5) . . ?
O7 C24 O8 123.9(4) . . ?
O7 C24 C21 119.2(4) . . ?
O8 C24 C21 116.9(4) . . ?
C6 N C9 122.5(4) . . ?
C6 N C17 121.9(4) . . ?
C9 N C17 115.6(4) . . ?
C1 O1 Zn1 122.0(3) . . ?
C1 O2 Zn1 132.4(3) . 3_757 ?
C8 O3 Zn2 130.9(3) . . ?
C8 O4 Zn2 118.6(3) . 3_856 ?
C24 O7 Zn2 117.9(3) . 2_756 ?
C24 O8 Zn1 142.7(3) . 4_565 ?
C16 O5 Zn1 132.4(3) . 2_756 ?
C16 O6 Zn2 138.2(3) . 4_565 ?
O5 Zn1 O2 99.08(15) 2_746 3_757 ?
O5 Zn1 O8 124.63(16) 2_746 4_666 ?
O2 Zn1 O8 104.52(15) 3_757 4_666 ?
O5 Zn1 O1 106.04(14) 2_746 . ?
O2 Zn1 O1 124.27(14) 3_757 . ?
O8 Zn1 O1 100.56(14) 4_666 . ?
O6 Zn2 O3 100.90(13) 4_666 . ?
O6 Zn2 O7 124.83(15) 4_666 2_746 ?
O3 Zn2 O7 103.38(13) . 2_746 ?
O6 Zn2 O4 117.69(15) 4_666 3_856 ?
O3 Zn2 O4 110.39(13) . 3_856 ?
O7 Zn2 O4 98.70(14) 2_746 3_856 ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        26.02
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.493
_refine_diff_density_min         -0.391
_refine_diff_density_rms         0.086
####################################################################### 
# 
# 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_a_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1847206'
_audit_update_record             
;
2018-06-05 deposited with the CCDC.
2018-10-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C27 H26 N2 O13 Pb2'
_chemical_formula_sum            'C27 H26 N2 O13 Pb2'
_chemical_formula_weight         1000.88

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P-1   '
_symmetry_space_group_name_Hall  -P1
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.1170(10)
_cell_length_b                   11.2139(10)
_cell_length_c                   13.6948(12)
_cell_angle_alpha                104.0590(10)
_cell_angle_beta                 100.2590(10)
_cell_angle_gamma                93.090(2)
_cell_volume                     1621.2(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2546
_cell_measurement_theta_min      2.67
_cell_measurement_theta_max      24.21

_exptl_crystal_description       block
_exptl_crystal_colour            white
_exptl_crystal_size_max          0.259
_exptl_crystal_size_mid          0.215
_exptl_crystal_size_min          0.184
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.050
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             940
_exptl_absorpt_coefficient_mu    10.435
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.078
_exptl_absorpt_correction_T_max  0.147
_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  'CCD area detector'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_decay_%        none
_diffrn_reflns_number            9157
_diffrn_reflns_av_R_equivalents  0.0258
_diffrn_reflns_av_sigmaI/netI    0.0620
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.56
_diffrn_reflns_theta_max         26.36
_reflns_number_total             6360
_reflns_number_gt                4701
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       'SMART (Bruker, 2002)'
_computing_cell_refinement       'SAINT (Bruker, 2002)'
_computing_data_reduction        'SHELXS97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXS97 (Sheldrick, 1997)'
_computing_publication_material  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 > 2σ(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)+(0.1097P)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         6360
_refine_ls_number_parameters     379
_refine_ls_number_restraints     79
_refine_ls_R_factor_all          0.0742
_refine_ls_R_factor_gt           0.0562
_refine_ls_wR_factor_ref         0.1823
_refine_ls_wR_factor_gt          0.1677
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_restrained_S_all      1.073
_refine_ls_shift/su_max          0.017
_refine_ls_shift/su_mean         0.001

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 1.2471(18) 0.9906(16) 0.8741(14) 0.029(4) Uani 0.60 1 d P . .
C1' C 1.328(4) 0.837(4) 0.899(3) 0.057(10) Uani 0.40 1 d PU . .
C2' C 1.198(3) 0.784(3) 0.827(2) 0.027(6) Uani 0.40 1 d PU . .
C2 C 1.1266(11) 0.8841(12) 0.8118(9) 0.001(2) Uani 0.60 1 d PU . .
C3 C 1.053(2) 0.937(2) 0.751(2) 0.111(8) Uani 1 1 d U . .
C4' C 1.002(2) 0.824(2) 0.7466(19) 0.018(5) Uani 0.40 1 d PU . .
C4 C 0.9573(19) 0.852(2) 0.6870(16) 0.035(5) Uani 0.60 1 d PU . .
C5 C 0.9595(16) 0.7182(18) 0.6911(11) 0.067(6) Uani 1 1 d D . .
C6 C 1.042(2) 0.697(2) 0.7605(19) 0.045(6) Uani 0.60 1 d PU . .
C6' C 1.067(3) 0.617(4) 0.716(3) 0.048(9) Uani 0.40 1 d PDU . .
C7' C 1.181(3) 0.667(3) 0.789(2) 0.030(6) Uani 0.40 1 d PU . .
C7 C 1.130(2) 0.781(2) 0.8224(18) 0.045(6) Uani 0.60 1 d PU . .
C8 C 0.8532(13) 0.6384(11) 0.6141(9) 0.040(3) Uani 1 1 d . . .
H8A H 0.7792 0.6793 0.6205 0.048 Uiso 1 1 calc R . .
H8B H 0.8680 0.6341 0.5457 0.048 Uiso 1 1 calc R . .
C9 C 0.8557(13) 0.4125(12) 0.5425(10) 0.044(3) Uani 1 1 d . . .
H9A H 0.9077 0.3594 0.5734 0.052 Uiso 1 1 calc R . .
H9B H 0.9007 0.4469 0.4995 0.052 Uiso 1 1 calc R . .
C10 C 0.7387(11) 0.3348(11) 0.4753(9) 0.032(3) Uani 1 1 d . . .
C11 C 0.7483(12) 0.2210(12) 0.4091(9) 0.039(3) Uani 1 1 d . . .
H11 H 0.8247 0.1910 0.4096 0.046 Uiso 1 1 calc R . .
C12 C 0.6492(12) 0.1546(13) 0.3448(10) 0.040(3) Uani 1 1 d U . .
H12 H 0.6589 0.0783 0.3031 0.047 Uiso 1 1 calc R . .
C13 C 0.5342(12) 0.1937(12) 0.3376(10) 0.038(3) Uani 1 1 d . . .
C14 C 0.5190(18) 0.2968(17) 0.4039(14) 0.071(5) Uani 1 1 d U . .
H14 H 0.4399 0.3182 0.4075 0.085 Uiso 1 1 calc R . .
C15 C 0.6275(16) 0.3801(15) 0.4735(13) 0.073(6) Uani 1 1 d . . .
H15 H 0.6190 0.4582 0.5130 0.088 Uiso 1 1 calc R . .
C16 C 0.4214(14) 0.1242(13) 0.2680(9) 0.042(3) Uani 1 1 d . . .
C17 C 0.7906(11) 0.4921(11) 0.7072(8) 0.031(3) Uani 1 1 d . . .
C18 C 0.7834(10) 0.3710(11) 0.7215(9) 0.030(3) Uani 1 1 d U . .
H18 H 0.8075 0.3062 0.6748 0.036 Uiso 1 1 calc R . .
C19 C 0.7398(11) 0.3492(11) 0.8067(9) 0.030(3) Uani 1 1 d . . .
C20 C 0.6979(11) 0.4472(11) 0.8733(9) 0.030(3) Uani 1 1 d . . .
H20 H 0.6681 0.4332 0.9293 0.036 Uiso 1 1 calc R . .
C21 C 0.7003(10) 0.5625(10) 0.8570(8) 0.026(2) Uani 1 1 d . . .
C22 C 0.7470(11) 0.5847(10) 0.7754(9) 0.032(3) Uani 1 1 d . . .
H22 H 0.7494 0.6641 0.7659 0.039 Uiso 1 1 calc R . .
C23 C 0.7467(11) 0.2230(10) 0.8305(8) 0.030(3) Uani 1 1 d . . .
C24 C 0.6530(12) 0.6661(11) 0.9279(10) 0.039(3) Uani 1 1 d . . .
N1 N 0.8296(12) 0.5121(10) 0.6228(9) 0.047(3) Uani 1 1 d . . .
O1 O 0.7935(9) 0.1442(8) 0.7730(7) 0.044(2) Uani 1 1 d . . .
O2 O 0.7092(9) 0.2086(8) 0.9078(7) 0.039(2) Uani 1 1 d . . .
O1W O 0.5631(15) 0.7321(18) 1.2031(13) 0.118(6) Uani 1 1 d . . .
O3 O 0.6758(10) 0.7740(9) 0.9277(8) 0.056(3) Uani 1 1 d . . .
O4 O 0.5870(11) 0.6362(9) 0.9880(9) 0.066(3) Uani 1 1 d . . .
O5 O 0.3183(9) 0.1482(9) 0.2846(7) 0.045(2) Uani 1 1 d . . .
O6 O 0.4362(7) 0.0356(7) 0.1904(6) 0.034(2) Uani 1 1 d . . .
O7 O 1.3250(9) 0.9596(8) 0.9536(6) 0.040(2) Uani 1 1 d . . .
O8 O 1.2698(14) 1.0820(12) 0.8437(10) 0.035(3) Uani 0.60 1 d P . .
O8' O 1.405(2) 0.772(2) 0.9071(15) 0.042(6) Uani 0.40 1 d P . .
Pb1 Pb 0.77853(4) -0.00067(4) 0.88620(3) 0.03420(17) Uani 1 1 d . . .
Pb2 Pb 0.53748(5) 0.84425(4) 1.06076(4) 0.03637(18) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O8 1.23(2) . ?
C1 O7 1.39(2) . ?
C1 C2 1.70(2) . ?
C1 Pb2 2.81(2) 2_777 ?
C1' O8' 1.16(4) . ?
C1' O7 1.41(4) . ?
C1' C2' 1.59(5) . ?
C2' C7 0.74(3) . ?
C2' C7' 1.27(4) . ?
C2' C2 1.45(3) . ?
C2' C6 1.90(4) . ?
C2 C7 1.21(3) . ?
C2 C3 1.32(3) . ?
C2 C4' 1.53(3) . ?
C3 C4' 1.34(3) . ?
C3 C4 1.40(3) . ?
C4' C4 1.00(3) . ?
C4' C5 1.26(3) . ?
C4' C6 1.57(3) . ?
C4' C7 1.77(3) . ?
C4 C5 1.51(3) . ?
C5 C6 1.28(3) . ?
C5 C8 1.515(18) . ?
C5 C6' 1.74(4) . ?
C6 C6' 1.03(4) . ?
C6 C7 1.33(3) . ?
C6 C7' 1.60(4) . ?
C6' C7' 1.45(4) . ?
C7' C7 1.43(4) . ?
C8 N1 1.463(16) . ?
C9 N1 1.446(15) . ?
C9 C10 1.537(17) . ?
C10 C15 1.36(2) . ?
C10 C11 1.396(17) . ?
C11 C12 1.338(17) . ?
C12 C13 1.368(18) . ?
C13 C14 1.32(2) . ?
C13 C16 1.48(2) . ?
C14 C15 1.51(2) . ?
C16 O5 1.238(17) . ?
C16 O6 1.308(14) . ?
C16 Pb1 2.809(13) 2_656 ?
C17 N1 1.366(16) . ?
C17 C22 1.390(15) . ?
C17 C18 1.418(16) . ?
C18 C19 1.409(16) . ?
C19 C20 1.405(15) . ?
C19 C23 1.530(16) . ?
C20 C21 1.364(16) . ?
C21 C22 1.381(17) . ?
C21 C24 1.506(16) . ?
C23 O1 1.236(14) . ?
C23 O2 1.247(14) . ?
C23 Pb1 2.815(12) . ?
C24 O3 1.224(15) . ?
C24 O4 1.284(17) . ?
O1 Pb1 2.521(9) . ?
O2 Pb1 2.475(8) . ?
O1W Pb2 2.548(16) . ?
O3 Pb2 2.596(10) . ?
O4 Pb2 2.438(9) . ?
O5 Pb1 2.529(9) 2_656 ?
O6 Pb1 2.400(8) 2_656 ?
O7 Pb1 2.611(8) 2_767 ?
O7 Pb2 2.677(8) 2_777 ?
O8 Pb2 2.296(14) 2_777 ?
O8' Pb2 2.276(19) 1_655 ?
Pb1 O6 2.400(8) 2_656 ?
Pb1 O5 2.529(9) 2_656 ?
Pb1 O7 2.611(8) 2_767 ?
Pb1 C16 2.809(13) 2_656 ?
Pb2 O8' 2.276(19) 1_455 ?
Pb2 O8 2.296(14) 2_777 ?
Pb2 O7 2.677(8) 2_777 ?
Pb2 C1 2.81(2) 2_777 ?

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
O8 C1 O7 122.8(16) . . ?
O8 C1 C2 121.4(15) . . ?
O7 C1 C2 115.3(14) . . ?
O8 C1 Pb2 53.1(10) . 2_777 ?
O7 C1 Pb2 69.9(8) . 2_777 ?
C2 C1 Pb2 168.4(12) . 2_777 ?
O8' C1' O7 129(4) . . ?
O8' C1' C2' 120(4) . . ?
O7 C1' C2' 110(3) . . ?
C7 C2' C7' 86(4) . . ?
C7 C2' C2 56(3) . . ?
C7' C2' C2 134(3) . . ?
C7 C2' C1' 146(4) . . ?
C7' C2' C1' 116(3) . . ?
C2 C2' C1' 110(2) . . ?
C7 C2' C6 33(3) . . ?
C7' C2' C6 56.6(19) . . ?
C2 C2' C6 78.8(17) . . ?
C1' C2' C6 167(3) . . ?
C7 C2 C3 135(2) . . ?
C7 C2 C2' 30.8(14) . . ?
C3 C2 C2' 150.4(19) . . ?
C7 C2 C4' 79.9(17) . . ?
C3 C2 C4' 55.5(15) . . ?
C2' C2 C4' 106.1(18) . . ?
C7 C2 C1 118.2(15) . . ?
C3 C2 C1 106.7(16) . . ?
C2' C2 C1 91.7(15) . . ?
C4' C2 C1 161.8(15) . . ?
C2 C3 C4' 69.9(18) . . ?
C2 C3 C4 111(2) . . ?
C4' C3 C4 42.7(15) . . ?
C4 C4' C5 83(2) . . ?
C4 C4' C3 72(2) . . ?
C5 C4' C3 147(3) . . ?
C4 C4' C2 125(3) . . ?
C5 C4' C2 136(2) . . ?
C3 C4' C2 54.6(15) . . ?
C4 C4' C6 133(3) . . ?
C5 C4' C6 52.4(15) . . ?
C3 C4' C6 139(2) . . ?
C2 C4' C6 88.2(16) . . ?
C4 C4' C7 156(3) . . ?
C5 C4' C7 98(2) . . ?
C3 C4' C7 96(2) . . ?
C2 C4' C7 42.1(11) . . ?
C6 C4' C7 46.6(14) . . ?
C4' C4 C3 65(2) . . ?
C4' C4 C5 56(2) . . ?
C3 C4 C5 117.4(19) . . ?
C4' C5 C6 76.2(18) . . ?
C4' C5 C4 41.1(14) . . ?
C6 C5 C4 116.0(17) . . ?
C4' C5 C8 148(2) . . ?
C6 C5 C8 133(2) . . ?
C4 C5 C8 110.5(16) . . ?
C4' C5 C6' 107(2) . . ?
C6 C5 C6' 36.0(16) . . ?
C4 C5 C6' 138.5(18) . . ?
C8 C5 C6' 105.3(18) . . ?
C6' C6 C5 97(3) . . ?
C6' C6 C7 119(3) . . ?
C5 C6 C7 125(2) . . ?
C6' C6 C4' 138(3) . . ?
C5 C6 C4' 51.4(15) . . ?
C7 C6 C4' 74.8(19) . . ?
C6' C6 C7' 63(3) . . ?
C5 C6 C7' 145(2) . . ?
C7 C6 C7' 57.6(18) . . ?
C4' C6 C7' 125(2) . . ?
C6' C6 C2' 102(3) . . ?
C5 C6 C2' 131(2) . . ?
C7 C6 C2' 17.5(15) . . ?
C4' C6 C2' 86.1(17) . . ?
C7' C6 C2' 41.7(15) . . ?
C6 C6' C7' 78(3) . . ?
C6 C6' C5 47(2) . . ?
C7' C6' C5 119(3) . . ?
C2' C7' C7 31.1(15) . . ?
C2' C7' C6' 117(3) . . ?
C7 C7' C6' 90(2) . . ?
C2' C7' C6 82(2) . . ?
C7 C7' C6 51.8(16) . . ?
C6' C7' C6 39.0(18) . . ?
C2' C7 C2 93(4) . . ?
C2' C7 C6 130(4) . . ?
C2 C7 C6 116(2) . . ?
C2' C7 C7' 63(3) . . ?
C2 C7 C7' 143(3) . . ?
C6 C7 C7' 70.6(19) . . ?
C2' C7 C4' 138(4) . . ?
C2 C7 C4' 58.0(14) . . ?
C6 C7 C4' 58.5(16) . . ?
C7' C7 C4' 122(2) . . ?
N1 C8 C5 116.5(13) . . ?
N1 C9 C10 112.6(12) . . ?
C15 C10 C11 119.7(12) . . ?
C15 C10 C9 120.7(12) . . ?
C11 C10 C9 119.4(12) . . ?
C12 C11 C10 121.0(13) . . ?
C11 C12 C13 123.1(14) . . ?
C14 C13 C12 118.1(15) . . ?
C14 C13 C16 116.3(13) . . ?
C12 C13 C16 125.4(13) . . ?
C13 C14 C15 121.2(17) . . ?
C10 C15 C14 116.3(13) . . ?
O5 C16 O6 122.1(12) . . ?
O5 C16 C13 120.9(11) . . ?
O6 C16 C13 117.0(12) . . ?
O5 C16 Pb1 64.2(7) . 2_656 ?
O6 C16 Pb1 58.5(6) . 2_656 ?
C13 C16 Pb1 172.0(10) . 2_656 ?
N1 C17 C22 122.0(12) . . ?
N1 C17 C18 119.6(10) . . ?
C22 C17 C18 118.1(11) . . ?
C19 C18 C17 119.8(11) . . ?
C20 C19 C18 119.1(11) . . ?
C20 C19 C23 120.6(10) . . ?
C18 C19 C23 120.2(10) . . ?
C21 C20 C19 120.9(11) . . ?
C20 C21 C22 119.9(11) . . ?
C20 C21 C24 120.4(11) . . ?
C22 C21 C24 119.7(11) . . ?
C21 C22 C17 122.0(11) . . ?
O1 C23 O2 125.0(12) . . ?
O1 C23 C19 117.0(11) . . ?
O2 C23 C19 118.0(10) . . ?
O1 C23 Pb1 63.6(7) . . ?
O2 C23 Pb1 61.5(6) . . ?
C19 C23 Pb1 175.1(8) . . ?
O3 C24 O4 121.5(12) . . ?
O3 C24 C21 121.4(13) . . ?
O4 C24 C21 117.2(11) . . ?
C17 N1 C9 122.4(11) . . ?
C17 N1 C8 120.0(10) . . ?
C9 N1 C8 117.5(11) . . ?
C23 O1 Pb1 90.4(8) . . ?
C23 O2 Pb1 92.3(7) . . ?
C24 O3 Pb2 90.5(8) . . ?
C24 O4 Pb2 96.5(8) . . ?
C16 O5 Pb1 89.6(7) . 2_656 ?
C16 O6 Pb1 93.9(8) . 2_656 ?
C1 O7 C1' 95.1(18) . . ?
C1 O7 Pb1 108.2(10) . 2_767 ?
C1' O7 Pb1 118.4(18) . 2_767 ?
C1 O7 Pb2 80.8(9) . 2_777 ?
C1' O7 Pb2 125.6(18) . 2_777 ?
Pb1 O7 Pb2 114.2(3) 2_767 2_777 ?
C1 O8 Pb2 101.7(12) . 2_777 ?
C1' O8' Pb2 111(2) . 1_655 ?
O6 Pb1 O2 75.3(3) 2_656 . ?
O6 Pb1 O1 85.8(3) 2_656 . ?
O2 Pb1 O1 52.3(3) . . ?
O6 Pb1 O5 53.7(3) 2_656 2_656 ?
O2 Pb1 O5 113.4(3) . 2_656 ?
O1 Pb1 O5 81.5(3) . 2_656 ?
O6 Pb1 O7 77.6(3) 2_656 2_767 ?
O2 Pb1 O7 73.3(3) . 2_767 ?
O1 Pb1 O7 125.5(3) . 2_767 ?
O5 Pb1 O7 123.5(3) 2_656 2_767 ?
O6 Pb1 C16 27.7(3) 2_656 2_656 ?
O2 Pb1 C16 96.7(3) . 2_656 ?
O1 Pb1 C16 85.0(4) . 2_656 ?
O5 Pb1 C16 26.2(3) 2_656 2_656 ?
O7 Pb1 C16 100.5(4) 2_767 2_656 ?
O6 Pb1 C23 80.2(3) 2_656 . ?
O2 Pb1 C23 26.3(3) . . ?
O1 Pb1 C23 26.1(3) . . ?
O5 Pb1 C23 98.4(3) 2_656 . ?
O7 Pb1 C23 99.5(3) 2_767 . ?
C16 Pb1 C23 91.5(3) 2_656 . ?
O8' Pb2 O8 151.3(7) 1_455 2_777 ?
O8' Pb2 O4 73.6(6) 1_455 . ?
O8 Pb2 O4 96.3(5) 2_777 . ?
O8' Pb2 O1W 123.9(8) 1_455 . ?
O8 Pb2 O1W 75.6(5) 2_777 . ?
O4 Pb2 O1W 72.4(5) . . ?
O8' Pb2 O3 74.7(6) 1_455 . ?
O8 Pb2 O3 78.1(4) 2_777 . ?
O4 Pb2 O3 51.4(3) . . ?
O1W Pb2 O3 113.5(5) . . ?
O8' Pb2 O7 106.7(7) 1_455 2_777 ?
O8 Pb2 O7 54.5(4) 2_777 2_777 ?
O4 Pb2 O7 119.9(3) . 2_777 ?
O1W Pb2 O7 128.7(4) . 2_777 ?
O3 Pb2 O7 70.3(3) . 2_777 ?
O8' Pb2 C1 133.2(8) 1_455 2_777 ?
O8 Pb2 C1 25.3(5) 2_777 2_777 ?
O4 Pb2 C1 110.1(5) . 2_777 ?
O1W Pb2 C1 100.1(5) . 2_777 ?
O3 Pb2 C1 73.5(5) . 2_777 ?
O7 Pb2 C1 29.2(4) 2_777 2_777 ?

_diffrn_measured_fraction_theta_max 0.963
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.974
_refine_diff_density_max         2.508
_refine_diff_density_min         -1.851
_refine_diff_density_rms         0.318
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.004 -0.020 0.480 568 156 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          ?
####################################################################### 
# 
# 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_5
_database_code_depnum_ccdc_archive 'CCDC 1833734'
_audit_update_record             
;
2018-03-30 deposited with the CCDC.
2018-10-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H19 Mn N O9'
_chemical_formula_sum            'C24 H19 Mn N O9'
_chemical_formula_weight         520.34

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthogonal
_symmetry_space_group_name_H-M   Pna21
_symmetry_space_group_name_Hall  'P 2c -2n'

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                   14.751(5)
_cell_length_b                   12.781(5)
_cell_length_c                   11.161(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2104.2(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    2489
_cell_measurement_theta_min      2.45
_cell_measurement_theta_max      25.38

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.276
_exptl_crystal_size_mid          0.243
_exptl_crystal_size_min          0.198
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.643
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1068
_exptl_absorpt_coefficient_mu    0.688
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.827
_exptl_absorpt_correction_T_max  0.873
_exptl_absorpt_process_details   '(SADABS; Bruker, 2002)'


_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71069
_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       ω
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_decay_%        none
_diffrn_reflns_number            11084
_diffrn_reflns_av_R_equivalents  0.0438
_diffrn_reflns_av_sigmaI/netI    0.0543
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.11
_diffrn_reflns_theta_max         26.03
_reflns_number_total             3952
_reflns_number_gt                3269
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 2002)'
_computing_cell_refinement       'SAINT (Bruker, 2002)'
_computing_data_reduction        'SHELXS97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXS97 (Sheldrick, 1997)'
_computing_publication_material  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)+(0.0308P)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   0.030(17)
_refine_ls_number_reflns         3952
_refine_ls_number_parameters     316
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0484
_refine_ls_R_factor_gt           0.0358
_refine_ls_wR_factor_ref         0.0762
_refine_ls_wR_factor_gt          0.0712
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_restrained_S_all      1.033
_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
Mn Mn 0.88883(3) 0.63285(3) 0.69498(5) 0.02210(11) Uani 1 1 d . . .
O5 O 0.90584(15) 0.46876(16) 0.7229(2) 0.0385(6) Uani 1 1 d . . .
O6 O 0.87408(17) 0.35847(19) 0.5745(2) 0.0435(7) Uani 1 1 d . . .
H2 H 0.8809 0.4130 0.5335 0.065 Uiso 1 1 calc R . .
O4 O 1.11356(13) 0.19657(13) 1.1858(3) 0.0277(5) Uani 1 1 d . . .
O3 O 1.25095(14) 0.13308(15) 1.1475(2) 0.0367(6) Uani 1 1 d . . .
H4 H 1.2664 0.1820 1.1935 0.055 Uiso 1 1 calc R . .
O1 O 1.28071(14) -0.11932(16) 0.8110(2) 0.0331(5) Uani 1 1 d . . .
O2 O 1.16754(14) -0.23032(16) 0.7783(2) 0.0321(5) Uani 1 1 d . . .
O7 O 0.87256(15) -0.35807(18) 1.5149(2) 0.0391(6) Uani 1 1 d . . .
O8 O 0.89796(16) -0.50347(17) 1.4122(2) 0.0419(6) Uani 1 1 d . . .
O1W O 1.01696(15) 0.64401(15) 0.7742(2) 0.0396(6) Uani 1 1 d . . .
H9A H 1.0201 0.6023 0.8335 0.059 Uiso 1 1 d R . .
H9B H 1.0592 0.6896 0.7754 0.059 Uiso 1 1 d R . .
N N 0.89982(14) -0.05482(17) 0.9834(2) 0.0210(5) Uani 1 1 d . . .
C16 C 0.88669(19) 0.3802(2) 0.6874(4) 0.0274(6) Uani 1 1 d . . .
C13 C 0.8770(2) 0.2924(2) 0.7709(3) 0.0272(7) Uani 1 1 d . . .
C14 C 0.8862(2) 0.3078(3) 0.8919(3) 0.0339(8) Uani 1 1 d . . .
H3 H 0.8994 0.3758 0.9216 0.041 Uiso 1 1 calc R . .
C15 C 0.8765(2) 0.2250(3) 0.9717(3) 0.0326(8) Uani 1 1 d . . .
H4A H 0.8836 0.2367 1.0552 0.039 Uiso 1 1 calc R . .
C10 C 0.8566(2) 0.1262(2) 0.9304(3) 0.0245(7) Uani 1 1 d . . .
C11 C 0.8489(2) 0.1103(2) 0.8090(3) 0.0361(9) Uani 1 1 d . . .
H6 H 0.8366 0.0419 0.7800 0.043 Uiso 1 1 calc R . .
C12 C 0.8585(2) 0.1910(2) 0.7286(3) 0.0354(9) Uani 1 1 d . . .
H7 H 0.8528 0.1784 0.6451 0.042 Uiso 1 1 calc R . .
C9 C 0.8423(2) 0.0344(2) 1.0159(3) 0.0249(7) Uani 1 1 d . . .
H8A H 0.8567 0.0568 1.0987 0.030 Uiso 1 1 calc R . .
H8B H 0.7779 0.0128 1.0138 0.030 Uiso 1 1 calc R . .
C5 C 1.03328(19) 0.0362(2) 1.0560(3) 0.0226(7) Uani 1 1 d . . .
H10 H 0.9962 0.0797 1.1045 0.027 Uiso 1 1 calc R . .
C4 C 1.12702(19) 0.0511(2) 1.0556(3) 0.0228(7) Uani 1 1 d . . .
C8 C 1.1636(2) 0.1335(2) 1.1347(3) 0.0249(7) Uani 1 1 d . . .
C3 C 1.18232(19) -0.0100(2) 0.9817(3) 0.0225(6) Uani 1 1 d . . .
H13 H 1.2459 0.0017 0.9791 0.027 Uiso 1 1 calc R . .
C2 C 1.14309(19) -0.0878(2) 0.9121(3) 0.0199(6) Uani 1 1 d . . .
C1 C 1.2013(2) -0.1512(2) 0.8284(3) 0.0227(7) Uani 1 1 d . . .
C7 C 1.04990(18) -0.1042(2) 0.9158(3) 0.0229(7) Uani 1 1 d . . .
H16 H 1.0242 -0.1591 0.8695 0.027 Uiso 1 1 calc R . .
C6 C 0.99329(18) -0.0418(2) 0.9861(3) 0.0194(6) Uani 1 1 d . . .
C17 C 0.8610(2) -0.1591(2) 0.9813(3) 0.0260(7) Uani 1 1 d . . .
H18A H 0.8891 -0.1986 0.9147 0.031 Uiso 1 1 calc R . .
H18B H 0.7955 -0.1529 0.9636 0.031 Uiso 1 1 calc R . .
C18 C 0.8722(2) -0.2225(2) 1.0961(3) 0.0248(7) Uani 1 1 d . . .
C19 C 0.8754(2) -0.1751(2) 1.2063(4) 0.0375(8) Uani 1 1 d . . .
H20 H 0.8745 -0.1009 1.2120 0.045 Uiso 1 1 calc R . .
C20 C 0.8798(2) -0.2357(3) 1.3099(3) 0.0376(10) Uani 1 1 d . . .
H21 H 0.8813 -0.2021 1.3858 0.045 Uiso 1 1 calc R . .
C21 C 0.8822(2) -0.3438(3) 1.3043(3) 0.0261(8) Uani 1 1 d . . .
C24 C 0.88551(19) -0.4067(3) 1.4174(3) 0.0274(7) Uani 1 1 d . . .
C22 C 0.88053(19) -0.3909(2) 1.1921(4) 0.0306(7) Uani 1 1 d . . .
H24 H 0.8824 -0.4650 1.1859 0.037 Uiso 1 1 calc R . .
C23 C 0.8762(2) -0.3306(3) 1.0895(3) 0.0285(8) Uani 1 1 d . . .
H25 H 0.8760 -0.3638 1.0133 0.034 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
Mn O7 2.028(3) 1_564 ?
Mn O1 2.062(2) 4_455 ?
Mn O1W 2.091(2) . ?
Mn O5 2.135(2) . ?
Mn O4 2.1829(19) 2_764 ?
O5 C16 1.231(4) . ?
O6 C16 1.303(6) . ?
O6 H2 0.8400 . ?
O4 C8 1.232(4) . ?
O4 Mn 2.1829(19) 2_765 ?
O3 C8 1.297(4) . ?
O3 H4 0.8400 . ?
O1 C1 1.255(3) . ?
O1 Mn 2.062(2) 4 ?
O2 C1 1.259(3) . ?
O7 C24 1.267(4) . ?
O7 Mn 2.028(3) 1_546 ?
O8 C24 1.252(4) . ?
O1W H9A 0.8511 . ?
O1W H9B 0.8525 . ?
N C6 1.389(3) . ?
N C17 1.450(4) . ?
N C9 1.468(4) . ?
C16 C13 1.466(5) . ?
C13 C14 1.372(5) . ?
C13 C12 1.405(4) . ?
C14 C15 1.391(5) . ?
C14 H3 0.9500 . ?
C15 C10 1.376(4) . ?
C15 H4A 0.9500 . ?
C10 C11 1.374(5) . ?
C10 C9 1.527(4) . ?
C11 C12 1.375(4) . ?
C11 H6 0.9500 . ?
C12 H7 0.9500 . ?
C9 H8A 0.9900 . ?
C9 H8B 0.9900 . ?
C5 C4 1.396(4) . ?
C5 C6 1.397(4) . ?
C5 H10 0.9500 . ?
C4 C3 1.398(4) . ?
C4 C8 1.477(4) . ?
C3 C2 1.389(4) . ?
C3 H13 0.9500 . ?
C2 C7 1.391(4) . ?
C2 C1 1.505(4) . ?
C7 C6 1.396(4) . ?
C7 H16 0.9500 . ?
C17 C18 1.525(5) . ?
C17 H18A 0.9900 . ?
C17 H18B 0.9900 . ?
C18 C19 1.372(6) . ?
C18 C23 1.386(5) . ?
C19 C20 1.393(6) . ?
C19 H20 0.9500 . ?
C20 C21 1.384(5) . ?
C20 H21 0.9500 . ?
C21 C22 1.390(6) . ?
C21 C24 1.497(5) . ?
C22 C23 1.382(5) . ?
C22 H24 0.9500 . ?
C23 H25 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
O7 Mn O1 122.41(10) 1_564 4_455 ?
O7 Mn O1W 121.46(10) 1_564 . ?
O1 Mn O1W 116.06(10) 4_455 . ?
O7 Mn O5 102.39(9) 1_564 . ?
O1 Mn O5 85.24(9) 4_455 . ?
O1W Mn O5 84.22(8) . . ?
O7 Mn O4 83.94(10) 1_564 2_764 ?
O1 Mn O4 95.78(9) 4_455 2_764 ?
O1W Mn O4 88.06(8) . 2_764 ?
O5 Mn O4 171.82(10) . 2_764 ?
C16 O5 Mn 146.0(2) . . ?
C16 O6 H2 109.5 . . ?
C8 O4 Mn 133.2(2) . 2_765 ?
C8 O3 H4 109.5 . . ?
C1 O1 Mn 142.3(2) . 4 ?
C24 O7 Mn 143.6(2) . 1_546 ?
Mn O1W H9A 109.5 . . ?
Mn O1W H9B 135.5 . . ?
H9A O1W H9B 112.1 . . ?
C6 N C17 120.1(2) . . ?
C6 N C9 118.4(2) . . ?
C17 N C9 119.3(2) . . ?
O5 C16 O6 122.7(3) . . ?
O5 C16 C13 121.4(4) . . ?
O6 C16 C13 115.9(3) . . ?
C14 C13 C12 118.8(3) . . ?
C14 C13 C16 120.4(3) . . ?
C12 C13 C16 120.8(3) . . ?
C13 C14 C15 120.7(3) . . ?
C13 C14 H3 119.6 . . ?
C15 C14 H3 119.6 . . ?
C10 C15 C14 120.4(3) . . ?
C10 C15 H4A 119.8 . . ?
C14 C15 H4A 119.8 . . ?
C11 C10 C15 118.9(3) . . ?
C11 C10 C9 119.4(3) . . ?
C15 C10 C9 121.6(3) . . ?
C10 C11 C12 121.6(3) . . ?
C10 C11 H6 119.2 . . ?
C12 C11 H6 119.2 . . ?
C11 C12 C13 119.5(3) . . ?
C11 C12 H7 120.2 . . ?
C13 C12 H7 120.2 . . ?
N C9 C10 111.2(2) . . ?
N C9 H8A 109.4 . . ?
C10 C9 H8A 109.4 . . ?
N C9 H8B 109.4 . . ?
C10 C9 H8B 109.4 . . ?
H8A C9 H8B 108.0 . . ?
C4 C5 C6 120.9(3) . . ?
C4 C5 H10 119.5 . . ?
C6 C5 H10 119.5 . . ?
C5 C4 C3 120.2(3) . . ?
C5 C4 C8 117.2(3) . . ?
C3 C4 C8 122.5(3) . . ?
O4 C8 O3 123.1(3) . . ?
O4 C8 C4 121.6(3) . . ?
O3 C8 C4 115.2(3) . . ?
C2 C3 C4 119.1(3) . . ?
C2 C3 H13 120.4 . . ?
C4 C3 H13 120.4 . . ?
C3 C2 C7 120.2(3) . . ?
C3 C2 C1 119.7(3) . . ?
C7 C2 C1 120.1(3) . . ?
O1 C1 O2 124.1(3) . . ?
O1 C1 C2 117.0(3) . . ?
O2 C1 C2 118.8(3) . . ?
C2 C7 C6 121.5(3) . . ?
C2 C7 H16 119.3 . . ?
C6 C7 H16 119.3 . . ?
N C6 C7 120.9(3) . . ?
N C6 C5 121.1(3) . . ?
C7 C6 C5 118.0(3) . . ?
N C17 C18 115.6(3) . . ?
N C17 H18A 108.4 . . ?
C18 C17 H18A 108.4 . . ?
N C17 H18B 108.4 . . ?
C18 C17 H18B 108.4 . . ?
H18A C17 H18B 107.4 . . ?
C19 C18 C23 119.1(3) . . ?
C19 C18 C17 121.5(3) . . ?
C23 C18 C17 119.3(3) . . ?
C18 C19 C20 120.0(3) . . ?
C18 C19 H20 120.0 . . ?
C20 C19 H20 120.0 . . ?
C21 C20 C19 121.3(4) . . ?
C21 C20 H21 119.4 . . ?
C19 C20 H21 119.4 . . ?
C20 C21 C22 118.2(3) . . ?
C20 C21 C24 119.9(3) . . ?
C22 C21 C24 121.9(3) . . ?
O8 C24 O7 123.1(3) . . ?
O8 C24 C21 119.8(3) . . ?
O7 C24 C21 117.1(3) . . ?
C23 C22 C21 120.4(3) . . ?
C23 C22 H24 119.8 . . ?
C21 C22 H24 119.8 . . ?
C22 C23 C18 120.9(3) . . ?
C22 C23 H25 119.5 . . ?
C18 C23 H25 119.5 . . ?

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
O7 Mn O5 C16 -30.5(4) 1_564 . . . ?
O1 Mn O5 C16 91.7(4) 4_455 . . . ?
O1W Mn O5 C16 -151.5(4) . . . . ?
O4 Mn O5 C16 -170.8(6) 2_764 . . . ?
Mn O5 C16 O6 33.0(6) . . . . ?
Mn O5 C16 C13 -147.2(3) . . . . ?
O5 C16 C13 C14 2.2(5) . . . . ?
O6 C16 C13 C14 -178.0(3) . . . . ?
O5 C16 C13 C12 -177.6(3) . . . . ?
O6 C16 C13 C12 2.2(4) . . . . ?
C12 C13 C14 C15 -0.7(5) . . . . ?
C16 C13 C14 C15 179.5(3) . . . . ?
C13 C14 C15 C10 -0.6(5) . . . . ?
C14 C15 C10 C11 1.7(5) . . . . ?
C14 C15 C10 C9 -177.9(3) . . . . ?
C15 C10 C11 C12 -1.5(5) . . . . ?
C9 C10 C11 C12 178.1(3) . . . . ?
C10 C11 C12 C13 0.2(5) . . . . ?
C14 C13 C12 C11 0.9(5) . . . . ?
C16 C13 C12 C11 -179.3(3) . . . . ?
C6 N C9 C10 61.8(4) . . . . ?
C17 N C9 C10 -134.8(3) . . . . ?
C11 C10 C9 N 52.9(4) . . . . ?
C15 C10 C9 N -127.5(3) . . . . ?
C6 C5 C4 C3 2.1(4) . . . . ?
C6 C5 C4 C8 -178.4(3) . . . . ?
Mn O4 C8 O3 54.0(5) 2_765 . . . ?
Mn O4 C8 C4 -127.2(3) 2_765 . . . ?
C5 C4 C8 O4 -10.3(4) . . . . ?
C3 C4 C8 O4 169.2(3) . . . . ?
C5 C4 C8 O3 168.6(3) . . . . ?
C3 C4 C8 O3 -11.9(4) . . . . ?
C5 C4 C3 C2 -2.2(5) . . . . ?
C8 C4 C3 C2 178.3(3) . . . . ?
C4 C3 C2 C7 0.3(5) . . . . ?
C4 C3 C2 C1 177.5(3) . . . . ?
Mn O1 C1 O2 16.4(5) 4 . . . ?
Mn O1 C1 C2 -161.7(2) 4 . . . ?
C3 C2 C1 O1 -11.3(4) . . . . ?
C7 C2 C1 O1 166.0(3) . . . . ?
C3 C2 C1 O2 170.5(3) . . . . ?
C7 C2 C1 O2 -12.3(4) . . . . ?
C3 C2 C7 C6 1.8(4) . . . . ?
C1 C2 C7 C6 -175.4(3) . . . . ?
C17 N C6 C7 41.6(4) . . . . ?
C9 N C6 C7 -155.1(3) . . . . ?
C17 N C6 C5 -140.6(3) . . . . ?
C9 N C6 C5 22.7(4) . . . . ?
C2 C7 C6 N 176.0(3) . . . . ?
C2 C7 C6 C5 -1.9(4) . . . . ?
C4 C5 C6 N -178.0(3) . . . . ?
C4 C5 C6 C7 -0.1(4) . . . . ?
C6 N C17 C18 69.1(4) . . . . ?
C9 N C17 C18 -94.1(3) . . . . ?
N C17 C18 C19 31.0(4) . . . . ?
N C17 C18 C23 -151.2(3) . . . . ?
C23 C18 C19 C20 -1.9(4) . . . . ?
C17 C18 C19 C20 175.9(3) . . . . ?
C18 C19 C20 C21 0.7(5) . . . . ?
C19 C20 C21 C22 0.4(5) . . . . ?
C19 C20 C21 C24 -179.1(3) . . . . ?
Mn O7 C24 O8 19.7(6) 1_546 . . . ?
Mn O7 C24 C21 -162.5(3) 1_546 . . . ?
C20 C21 C24 O8 -171.9(3) . . . . ?
C22 C21 C24 O8 8.6(5) . . . . ?
C20 C21 C24 O7 10.2(4) . . . . ?
C22 C21 C24 O7 -169.3(3) . . . . ?
C20 C21 C22 C23 -0.3(4) . . . . ?
C24 C21 C22 C23 179.1(3) . . . . ?
C21 C22 C23 C18 -0.9(4) . . . . ?
C19 C18 C23 C22 2.0(5) . . . . ?
C17 C18 C23 C22 -175.9(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
O6 H2 O8 0.84 1.74 2.553(3) 161.7 1_564
O3 H4 O2 0.84 1.76 2.573(3) 162.1 3_755
O1W H9A O8 0.85 1.96 2.679(3) 141.9 2_754
O1W H9B O2 0.85 1.90 2.741(3) 169.5 1_565

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        26.03
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.217
_refine_diff_density_min         -0.284
_refine_diff_density_rms         0.060
####################################################################### 
# 
# 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_w
_database_code_depnum_ccdc_archive 'CCDC 1833735'
_audit_update_record             
;
2018-03-30 deposited with the CCDC.
2018-10-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H23 Cd N O11'
_chemical_formula_sum            'C24 H23 Cd N O11'
_chemical_formula_weight         613.84

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 0.0020 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd -0.8080 1.2020 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   'Pbca '
_symmetry_space_group_name_Hall  '-P 2ac 2ab'

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

_cell_length_a                   10.8479(18)
_cell_length_b                   20.105(3)
_cell_length_c                   22.305(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4864.7(14)
_cell_formula_units_Z            8
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    5560
_cell_measurement_theta_min      2.22
_cell_measurement_theta_max      26.02

_exptl_crystal_description       block
_exptl_crystal_colour            white
_exptl_crystal_size_max          0.216
_exptl_crystal_size_mid          0.201
_exptl_crystal_size_min          0.159
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.676
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2480
_exptl_absorpt_coefficient_mu    0.962
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.812
_exptl_absorpt_correction_T_max  0.858
_exptl_absorpt_process_details   '(SADABS; Bruker, 2002)'

_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       ω
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_decay_%        none
_diffrn_reflns_number            25216
_diffrn_reflns_av_R_equivalents  0.0450
_diffrn_reflns_av_sigmaI/netI    0.0338
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.83
_diffrn_reflns_theta_max         26.07
_reflns_number_total             4827
_reflns_number_gt                3681
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 2002)'
_computing_cell_refinement       'SAINT (Bruker, 2002)'
_computing_data_reduction        'SHELXS97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXS97 (Sheldrick, 1997)'
_computing_publication_material  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)+(0.0417P)²+3.3120P] 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         4827
_refine_ls_number_parameters     329
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0502
_refine_ls_R_factor_gt           0.0333
_refine_ls_wR_factor_ref         0.0869
_refine_ls_wR_factor_gt          0.0789
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_restrained_S_all      1.023
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C -0.1971(3) 1.29295(14) 0.58748(14) 0.0285(7) Uani 1 1 d . . .
C2 C -0.1756(3) 1.22643(14) 0.61549(13) 0.0252(6) Uani 1 1 d . . .
C3 C -0.2276(3) 1.17031(14) 0.59030(13) 0.0267(6) Uani 1 1 d . . .
H13 H -0.2801 1.1740 0.5575 0.032 Uiso 1 1 calc R . .
C4 C -0.2008(3) 1.10833(14) 0.61439(13) 0.0246(6) Uani 1 1 d . . .
C5 C -0.1223(3) 1.10266(14) 0.66291(12) 0.0252(6) Uani 1 1 d . . .
H10 H -0.1045 1.0607 0.6782 0.030 Uiso 1 1 calc R . .
C6 C -0.0691(3) 1.15875(14) 0.68944(12) 0.0243(6) Uani 1 1 d . . .
C7 C -0.0986(3) 1.22098(14) 0.66526(13) 0.0271(6) Uani 1 1 d . . .
H16 H -0.0663 1.2592 0.6827 0.033 Uiso 1 1 calc R . .
C8 C -0.2513(3) 1.04577(14) 0.58748(12) 0.0255(6) Uani 1 1 d . . .
C9 C 0.0426(3) 1.08868(15) 0.76144(13) 0.0307(7) Uani 1 1 d . . .
H6A H -0.0319 1.0621 0.7636 0.037 Uiso 1 1 calc R . .
H6B H 0.0728 1.0943 0.8021 0.037 Uiso 1 1 calc R . .
C10 C 0.1381(3) 1.05039(15) 0.72601(12) 0.0262(6) Uani 1 1 d . . .
C11 C 0.1697(3) 0.98682(17) 0.74489(15) 0.0408(8) Uani 1 1 d . . .
H4 H 0.1300 0.9684 0.7779 0.049 Uiso 1 1 calc R . .
C12 C 0.2589(3) 0.95067(17) 0.71544(15) 0.0397(8) Uani 1 1 d . . .
H3 H 0.2786 0.9081 0.7287 0.048 Uiso 1 1 calc R . .
C13 C 0.3193(3) 0.97709(15) 0.66628(13) 0.0280(7) Uani 1 1 d . . .
C14 C 0.2868(3) 1.04026(16) 0.64650(13) 0.0307(7) Uani 1 1 d . . .
H8 H 0.3259 1.0585 0.6132 0.037 Uiso 1 1 calc R . .
C15 C 0.1970(3) 1.07598(15) 0.67591(14) 0.0323(7) Uani 1 1 d . . .
H7A H 0.1755 1.1180 0.6619 0.039 Uiso 1 1 calc R . .
C16 C 0.4209(3) 0.94095(15) 0.63653(14) 0.0308(7) Uani 1 1 d . . .
C17 C 0.0840(3) 1.21001(16) 0.75674(13) 0.0336(7) Uani 1 1 d . . .
H18A H 0.1074 1.2351 0.7214 0.040 Uiso 1 1 calc R . .
H18B H 0.1591 1.1937 0.7752 0.040 Uiso 1 1 calc R . .
C18 C 0.0207(3) 1.25681(15) 0.80041(12) 0.0289(7) Uani 1 1 d . . .
C19 C 0.0769(3) 1.31667(16) 0.81349(14) 0.0355(7) Uani 1 1 d . . .
H25 H 0.1499 1.3280 0.7942 0.043 Uiso 1 1 calc R . .
C20 C 0.0265(3) 1.36012(16) 0.85486(14) 0.0381(8) Uani 1 1 d . . .
H24 H 0.0658 1.4001 0.8634 0.046 Uiso 1 1 calc R . .
C21 C -0.0827(3) 1.34387(16) 0.88346(13) 0.0332(7) Uani 1 1 d . . .
C22 C -0.1408(3) 1.28443(19) 0.86962(17) 0.0485(10) Uani 1 1 d . . .
H21 H -0.2148 1.2734 0.8881 0.058 Uiso 1 1 calc R . .
C23 C -0.0888(3) 1.24156(18) 0.82836(16) 0.0467(9) Uani 1 1 d . . .
H20 H -0.1284 1.2018 0.8193 0.056 Uiso 1 1 calc R . .
C24 C -0.1326(3) 1.38990(17) 0.92941(15) 0.0364(8) Uani 1 1 d . . .
Cd Cd 0.67416(2) 0.925293(11) 0.544614(10) 0.03142(9) Uani 1 1 d . . .
N N 0.0108(2) 1.15340(12) 0.73790(10) 0.0285(6) Uani 1 1 d . . .
O1 O -0.2628(2) 1.29957(12) 0.54263(10) 0.0452(6) Uani 1 1 d . . .
O2 O -0.1444(2) 1.34345(10) 0.61083(10) 0.0391(6) Uani 1 1 d . . .
O1W O 0.5487(2) 0.88979(12) 0.47232(9) 0.0397(5) Uani 1 1 d . . .
H9A H 0.5245 0.8476 0.4703 0.060 Uiso 1 1 d R . .
H9B H 0.4897 0.9183 0.4667 0.060 Uiso 1 1 d R . .
O3 O -0.31411(18) 1.04866(11) 0.53878(8) 0.0281(5) Uani 1 1 d . . .
O2W O 0.8470(2) 0.93323(12) 0.48603(11) 0.0434(6) Uani 1 1 d . . .
H10A H 0.8705 0.9687 0.4694 0.065 Uiso 1 1 d R . .
H10B H 0.9133 0.9330 0.5083 0.065 Uiso 1 1 d R . .
O4 O -0.2315(2) 0.99178(10) 0.61288(9) 0.0356(5) Uani 1 1 d . . .
O3W O 0.4697(3) 0.76513(16) 0.50187(16) 0.0956(12) Uani 1 1 d . . .
H11A H 0.4883 0.7377 0.5293 0.143 Uiso 1 1 d R . .
H11B H 0.4067 0.7513 0.4830 0.143 Uiso 1 1 d R . .
O5 O 0.4786(2) 0.96364(11) 0.59451(10) 0.0394(5) Uani 1 1 d . . .
O6 O 0.4447(2) 0.88254(11) 0.66076(10) 0.0447(6) Uani 1 1 d . . .
H6 H 0.5015 0.8647 0.6426 0.067 Uiso 1 1 calc R . .
O7 O -0.0745(3) 1.43705(14) 0.94879(12) 0.0593(8) Uani 1 1 d . . .
O8 O -0.2442(2) 1.37693(12) 0.94835(9) 0.0410(6) Uiso 1 1 d . . .
H8A H -0.2692 1.3428 0.9324 0.061 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
C1 O1 1.236(4) . ?
C1 O2 1.276(4) . ?
C1 C2 1.494(4) . ?
C1 Cd 2.838(3) 7_665 ?
C2 C3 1.381(4) . ?
C2 C7 1.393(4) . ?
C3 C4 1.388(4) . ?
C3 H13 0.9300 . ?
C4 C5 1.381(4) . ?
C4 C8 1.497(4) . ?
C5 C6 1.398(4) . ?
C5 H10 0.9300 . ?
C6 N 1.390(4) . ?
C6 C7 1.399(4) . ?
C7 H16 0.9300 . ?
C8 O4 1.243(3) . ?
C8 O3 1.284(3) . ?
C8 Cd 2.727(3) 1_455 ?
C9 N 1.445(4) . ?
C9 C10 1.514(4) . ?
C9 H6A 0.9700 . ?
C9 H6B 0.9700 . ?
C10 C15 1.386(4) . ?
C10 C11 1.388(4) . ?
C11 C12 1.377(4) . ?
C11 H4 0.9300 . ?
C12 C13 1.384(4) . ?
C12 H3 0.9300 . ?
C13 C14 1.390(4) . ?
C13 C16 1.478(4) . ?
C14 C15 1.376(4) . ?
C14 H8 0.9300 . ?
C15 H7A 0.9300 . ?
C16 O5 1.215(4) . ?
C16 O6 1.318(4) . ?
C17 N 1.450(4) . ?
C17 C18 1.518(4) . ?
C17 H18A 0.9700 . ?
C17 H18B 0.9700 . ?
C18 C23 1.376(4) . ?
C18 C19 1.380(4) . ?
C19 C20 1.383(4) . ?
C19 H25 0.9300 . ?
C20 C21 1.385(5) . ?
C20 H24 0.9300 . ?
C21 C22 1.385(5) . ?
C21 C24 1.483(4) . ?
C22 C23 1.381(5) . ?
C22 H21 0.9300 . ?
C23 H20 0.9300 . ?
C24 O7 1.218(4) . ?
C24 O8 1.308(4) . ?
Cd O1W 2.227(2) . ?
Cd O2 2.234(2) 7_655 ?
Cd O4 2.270(2) 1_655 ?
Cd O2W 2.291(2) . ?
Cd O3 2.487(2) 1_655 ?
Cd O5 2.517(2) . ?
Cd O1 2.705(2) 7_655 ?
Cd C8 2.727(3) 1_655 ?
Cd C1 2.838(3) 7_655 ?
O1 Cd 2.705(2) 7_665 ?
O2 Cd 2.234(2) 7_665 ?
O1W H9A 0.8894 . ?
O1W H9B 0.8686 . ?
O3 Cd 2.487(2) 1_455 ?
O2W H10A 0.8425 . ?
O2W H10B 0.8742 . ?
O4 Cd 2.270(2) 1_455 ?
O3W H11A 0.8483 . ?
O3W H11B 0.8497 . ?
O6 H6 0.8200 . ?
O8 H8A 0.8200 . ?

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 C1 O2 120.2(3) . . ?
O1 C1 C2 121.7(3) . . ?
O2 C1 C2 118.1(3) . . ?
O1 C1 Cd 71.14(17) . 7_665 ?
O2 C1 Cd 49.64(15) . 7_665 ?
C2 C1 Cd 165.1(2) . 7_665 ?
C3 C2 C7 120.3(3) . . ?
C3 C2 C1 119.8(3) . . ?
C7 C2 C1 119.8(3) . . ?
C2 C3 C4 119.4(3) . . ?
C2 C3 H13 120.3 . . ?
C4 C3 H13 120.3 . . ?
C5 C4 C3 120.4(3) . . ?
C5 C4 C8 118.0(3) . . ?
C3 C4 C8 121.5(3) . . ?
C4 C5 C6 121.3(3) . . ?
C4 C5 H10 119.4 . . ?
C6 C5 H10 119.4 . . ?
N C6 C5 121.6(3) . . ?
N C6 C7 120.8(3) . . ?
C5 C6 C7 117.6(3) . . ?
C2 C7 C6 120.9(3) . . ?
C2 C7 H16 119.5 . . ?
C6 C7 H16 119.5 . . ?
O4 C8 O3 121.1(3) . . ?
O4 C8 C4 119.2(3) . . ?
O3 C8 C4 119.7(3) . . ?
O4 C8 Cd 55.62(15) . 1_455 ?
O3 C8 Cd 65.54(15) . 1_455 ?
C4 C8 Cd 174.4(2) . 1_455 ?
N C9 C10 115.6(3) . . ?
N C9 H6A 108.4 . . ?
C10 C9 H6A 108.4 . . ?
N C9 H6B 108.4 . . ?
C10 C9 H6B 108.4 . . ?
H6A C9 H6B 107.4 . . ?
C15 C10 C11 118.2(3) . . ?
C15 C10 C9 123.2(3) . . ?
C11 C10 C9 118.6(3) . . ?
C12 C11 C10 121.0(3) . . ?
C12 C11 H4 119.5 . . ?
C10 C11 H4 119.5 . . ?
C11 C12 C13 120.6(3) . . ?
C11 C12 H3 119.7 . . ?
C13 C12 H3 119.7 . . ?
C12 C13 C14 118.8(3) . . ?
C12 C13 C16 121.4(3) . . ?
C14 C13 C16 119.8(3) . . ?
C15 C14 C13 120.3(3) . . ?
C15 C14 H8 119.8 . . ?
C13 C14 H8 119.8 . . ?
C14 C15 C10 121.1(3) . . ?
C14 C15 H7A 119.4 . . ?
C10 C15 H7A 119.4 . . ?
O5 C16 O6 123.4(3) . . ?
O5 C16 C13 123.1(3) . . ?
O6 C16 C13 113.6(3) . . ?
N C17 C18 115.2(3) . . ?
N C17 H18A 108.5 . . ?
C18 C17 H18A 108.5 . . ?
N C17 H18B 108.5 . . ?
C18 C17 H18B 108.5 . . ?
H18A C17 H18B 107.5 . . ?
C23 C18 C19 118.7(3) . . ?
C23 C18 C17 122.9(3) . . ?
C19 C18 C17 118.5(3) . . ?
C18 C19 C20 121.2(3) . . ?
C18 C19 H25 119.4 . . ?
C20 C19 H25 119.4 . . ?
C19 C20 C21 119.8(3) . . ?
C19 C20 H24 120.1 . . ?
C21 C20 H24 120.1 . . ?
C20 C21 C22 119.3(3) . . ?
C20 C21 C24 118.9(3) . . ?
C22 C21 C24 121.8(3) . . ?
C23 C22 C21 120.1(3) . . ?
C23 C22 H21 120.0 . . ?
C21 C22 H21 120.0 . . ?
C18 C23 C22 121.0(3) . . ?
C18 C23 H20 119.5 . . ?
C22 C23 H20 119.5 . . ?
O7 C24 O8 121.3(3) . . ?
O7 C24 C21 122.8(3) . . ?
O8 C24 C21 115.9(3) . . ?
O1W Cd O2 98.87(9) . 7_655 ?
O1W Cd O4 161.76(8) . 1_655 ?
O2 Cd O4 93.18(8) 7_655 1_655 ?
O1W Cd O2W 96.28(9) . . ?
O2 Cd O2W 123.14(8) 7_655 . ?
O4 Cd O2W 88.44(9) 1_655 . ?
O1W Cd O3 108.24(8) . 1_655 ?
O2 Cd O3 140.93(7) 7_655 1_655 ?
O4 Cd O3 54.88(7) 1_655 1_655 ?
O2W Cd O3 81.88(8) . 1_655 ?
O1W Cd O5 84.45(8) . . ?
O2 Cd O5 79.13(8) 7_655 . ?
O4 Cd O5 84.43(8) 1_655 . ?
O2W Cd O5 157.04(8) . . ?
O3 Cd O5 76.16(7) 1_655 . ?
O1W Cd O1 84.59(8) . 7_655 ?
O2 Cd O1 51.25(7) 7_655 7_655 ?
O4 Cd O1 113.65(8) 1_655 7_655 ?
O2W Cd O1 76.40(8) . 7_655 ?
O3 Cd O1 155.92(7) 1_655 7_655 ?
O5 Cd O1 126.38(7) . 7_655 ?
O1W Cd C8 136.03(9) . 1_655 ?
O2 Cd C8 117.73(8) 7_655 1_655 ?
O4 Cd C8 26.87(8) 1_655 1_655 ?
O2W Cd C8 84.00(9) . 1_655 ?
O3 Cd C8 28.02(7) 1_655 1_655 ?
O5 Cd C8 79.79(8) . 1_655 ?
O1 Cd C8 136.93(9) 7_655 1_655 ?
O1W Cd C1 89.82(9) . 7_655 ?
O2 Cd C1 25.80(8) 7_655 7_655 ?
O4 Cd C1 106.66(8) 1_655 7_655 ?
O2W Cd C1 100.71(9) . 7_655 ?
O3 Cd C1 161.46(7) 1_655 7_655 ?
O5 Cd C1 102.24(8) . 7_655 ?
O1 Cd C1 25.62(7) 7_655 7_655 ?
C8 Cd C1 133.53(9) 1_655 7_655 ?
C6 N C9 120.1(2) . . ?
C6 N C17 120.4(3) . . ?
C9 N C17 118.1(2) . . ?
C1 O1 Cd 83.24(18) . 7_665 ?
C1 O2 Cd 104.56(19) . 7_665 ?
Cd O1W H9A 121.6 . . ?
Cd O1W H9B 110.1 . . ?
H9A O1W H9B 113.8 . . ?
C8 O3 Cd 86.43(16) . 1_455 ?
Cd O2W H10A 123.9 . . ?
Cd O2W H10B 110.4 . . ?
H10A O2W H10B 90.4 . . ?
C8 O4 Cd 97.51(17) . 1_455 ?
H11A O3W H11B 109.6 . . ?
C16 O5 Cd 131.3(2) . . ?
C16 O6 H6 109.5 . . ?
C24 O8 H8A 109.5 . . ?

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
O1 C1 C2 C3 1.5(5) . . . . ?
O2 C1 C2 C3 -177.8(3) . . . . ?
Cd C1 C2 C3 -145.4(7) 7_665 . . . ?
O1 C1 C2 C7 178.6(3) . . . . ?
O2 C1 C2 C7 -0.7(4) . . . . ?
Cd C1 C2 C7 31.7(10) 7_665 . . . ?
C7 C2 C3 C4 -1.1(4) . . . . ?
C1 C2 C3 C4 176.0(3) . . . . ?
C2 C3 C4 C5 -0.3(4) . . . . ?
C2 C3 C4 C8 -177.9(3) . . . . ?
C3 C4 C5 C6 0.8(4) . . . . ?
C8 C4 C5 C6 178.4(3) . . . . ?
C4 C5 C6 N -179.4(3) . . . . ?
C4 C5 C6 C7 0.3(4) . . . . ?
C3 C2 C7 C6 2.2(4) . . . . ?
C1 C2 C7 C6 -174.9(3) . . . . ?
N C6 C7 C2 177.9(3) . . . . ?
C5 C6 C7 C2 -1.7(4) . . . . ?
C5 C4 C8 O4 7.1(4) . . . . ?
C3 C4 C8 O4 -175.3(3) . . . . ?
C5 C4 C8 O3 -172.9(3) . . . . ?
C3 C4 C8 O3 4.7(4) . . . . ?
C5 C4 C8 Cd -15(2) . . . 1_455 ?
C3 C4 C8 Cd 162.7(19) . . . 1_455 ?
N C9 C10 C15 3.1(4) . . . . ?
N C9 C10 C11 -177.7(3) . . . . ?
C15 C10 C11 C12 1.3(5) . . . . ?
C9 C10 C11 C12 -177.9(3) . . . . ?
C10 C11 C12 C13 0.1(6) . . . . ?
C11 C12 C13 C14 -1.2(5) . . . . ?
C11 C12 C13 C16 175.9(3) . . . . ?
C12 C13 C14 C15 0.8(5) . . . . ?
C16 C13 C14 C15 -176.4(3) . . . . ?
C13 C14 C15 C10 0.7(5) . . . . ?
C11 C10 C15 C14 -1.7(5) . . . . ?
C9 C10 C15 C14 177.5(3) . . . . ?
C12 C13 C16 O5 -177.5(3) . . . . ?
C14 C13 C16 O5 -0.5(5) . . . . ?
C12 C13 C16 O6 1.0(4) . . . . ?
C14 C13 C16 O6 178.1(3) . . . . ?
N C17 C18 C23 10.8(4) . . . . ?
N C17 C18 C19 -170.5(3) . . . . ?
C23 C18 C19 C20 1.5(5) . . . . ?
C17 C18 C19 C20 -177.2(3) . . . . ?
C18 C19 C20 C21 -0.5(5) . . . . ?
C19 C20 C21 C22 -0.7(5) . . . . ?
C19 C20 C21 C24 177.6(3) . . . . ?
C20 C21 C22 C23 1.0(6) . . . . ?
C24 C21 C22 C23 -177.3(3) . . . . ?
C19 C18 C23 C22 -1.3(5) . . . . ?
C17 C18 C23 C22 177.4(3) . . . . ?
C21 C22 C23 C18 0.0(6) . . . . ?
C20 C21 C24 O7 -9.7(5) . . . . ?
C22 C21 C24 O7 168.6(4) . . . . ?
C20 C21 C24 O8 170.3(3) . . . . ?
C22 C21 C24 O8 -11.4(5) . . . . ?
C5 C6 N C9 1.1(4) . . . . ?
C7 C6 N C9 -178.5(3) . . . . ?
C5 C6 N C17 167.3(3) . . . . ?
C7 C6 N C17 -12.4(4) . . . . ?
C10 C9 N C6 78.5(4) . . . . ?
C10 C9 N C17 -88.0(3) . . . . ?
C18 C17 N C6 86.6(3) . . . . ?
C18 C17 N C9 -106.9(3) . . . . ?
O2 C1 O1 Cd 7.9(3) . . . 7_665 ?
C2 C1 O1 Cd -171.4(3) . . . 7_665 ?
O1 C1 O2 Cd -9.8(3) . . . 7_665 ?
C2 C1 O2 Cd 169.5(2) . . . 7_665 ?
O4 C8 O3 Cd -2.4(3) . . . 1_455 ?
C4 C8 O3 Cd 177.7(2) . . . 1_455 ?
O3 C8 O4 Cd 2.6(3) . . . 1_455 ?
C4 C8 O4 Cd -177.4(2) . . . 1_455 ?
O6 C16 O5 Cd -9.5(5) . . . . ?
C13 C16 O5 Cd 169.0(2) . . . . ?
O1W Cd O5 C16 104.5(3) . . . . ?
O2 Cd O5 C16 4.3(3) 7_655 . . . ?
O4 Cd O5 C16 -90.0(3) 1_655 . . . ?
O2W Cd O5 C16 -162.5(3) . . . . ?
O3 Cd O5 C16 -145.1(3) 1_655 . . . ?
O1 Cd O5 C16 25.4(3) 7_655 . . . ?
C8 Cd O5 C16 -116.7(3) 1_655 . . . ?
C1 Cd O5 C16 15.9(3) 7_655 . . . ?

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
O1W H9A O3W 0.89 1.90 2.730(4) 155.2 .
O1W H9B O3 0.87 2.02 2.841(3) 157.0 5_576
O2W H10A O7 0.84 2.04 2.867(3) 166.8 8_685
O2W H10B O7 0.87 2.00 2.865(4) 173.5 4_646

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        26.07
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.844
_refine_diff_density_min         -0.727
_refine_diff_density_rms         0.073
