# Electronic Supplementary Material for CrystEngComm
# This journal is (c) The Royal Society of Chemistry 2008

data_global
_journal_name_full               CrystEngComm

_journal_coden_Cambridge         1350
_journal_volume                  ?
_journal_page_first              ?
_journal_year                    ?

_publ_contact_author_name        rongcao
_publ_contact_author_email       rongcao@fjirsm.ac.cn
_publ_contact_author_address     
;
State Key Laboratory of Structural Chemistry,
Fujian Institute of Research on the Structure of Matter,
Chinese Academy of Sciences,
Fujian, Fuzhou 350002, China
;
_publ_section_title              
;
Conformation Control of Flexible 1,4-phenylenediacetate
Ligand in Coordination Complexes:
A Rigidity-Modulated Strategy
;
_publ_author_address             
;
State Key Laboratory of Structural Chemistry,
Fujian Institute of Research on the Structure of Matter,
Chinese Academy of Sciences,
Fujian, Fuzhou 350002, China
;
loop_
_publ_author_name
'Rong Cao.'
'Zhengang Guo.'
'Tianfu Liu.'
'Jian Lu.'
L.-X.Shi

# Attachment '1a.CIF'

data_1a
_database_code_depnum_ccdc_archive 'CCDC 695288'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C10 H8 O4 Zn '
_chemical_formula_sum            'C10 H8 O4 Zn'
_chemical_formula_weight         257.55

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'
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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P21/c
_symmetry_space_group_name_Hall  '-P 2ybc'

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

_cell_length_a                   19.70(2)
_cell_length_b                   4.891(6)
_cell_length_c                   9.640(12)
_cell_angle_alpha                90.00
_cell_angle_beta                 95.33(2)
_cell_angle_gamma                90.00
_cell_volume                     924.8(19)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    1004
_cell_measurement_theta_min      0.977
_cell_measurement_theta_max      27.460

_exptl_crystal_description       Prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.850
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             520
_exptl_absorpt_coefficient_mu    2.643
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_max  0.768
_exptl_absorpt_correction_T_min  0.536
_exptl_absorpt_process_details   CrystalClear

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.7107
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  
;
Mercury2 (2x2 bin mode)
;
_diffrn_measurement_method       CCD_Profile_fitting
_diffrn_detector_area_resol_mean 13.6612
_diffrn_standards_number         none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        none
_diffrn_reflns_number            6653
_diffrn_reflns_av_R_equivalents  0.0481
_diffrn_reflns_av_sigmaI/netI    0.0448
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.08
_diffrn_reflns_theta_max         27.46
_reflns_number_total             2069
_reflns_number_gt                1749
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_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)+(0.1079P)²+1.1550P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2117
_refine_ls_number_parameters     136
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0587
_refine_ls_R_factor_gt           0.0463
_refine_ls_wR_factor_ref         0.1696
_refine_ls_wR_factor_gt          0.1372
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_restrained_S_all      1.080
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.23886(2) 0.80574(10) 0.29451(5) 0.0215(2) Uani 1 1 d . . .
O1 O 0.2164(2) 1.1954(6) 0.3019(4) 0.0338(9) Uani 1 1 d . . .
O2 O 0.16030(15) 1.5804(6) 0.3269(3) 0.0269(7) Uani 1 1 d . . .
O3 O 0.32012(17) 0.7172(8) 0.4187(3) 0.0309(8) Uani 1 1 d . . .
O4 O 0.26155(19) 0.7357(8) 0.6004(4) 0.0319(8) Uani 1 1 d . . .
C1 C 0.1667(2) 1.3243(9) 0.3457(5) 0.0212(9) Uani 1 1 d . . .
C2 C 0.1159(2) 1.1772(9) 0.4259(5) 0.0270(10) Uani 1 1 d . . .
H2A H 0.1398 1.1105 0.5144 0.032 Uiso 1 1 calc R . .
H2B H 0.0992 1.0150 0.3716 0.032 Uiso 1 1 calc R . .
C3 C 0.0547(2) 1.3455(9) 0.4598(5) 0.0239(9) Uani 1 1 d . . .
C4 C 0.0649(2) 1.5488(10) 0.5654(5) 0.0272(9) Uani 1 1 d . . .
H4 H 0.1090 1.5797 0.6115 0.033 Uiso 1 1 calc R . .
C5 C -0.0087(3) 1.2966(9) 0.3997(5) 0.0261(10) Uani 1 1 d . . .
H5 H -0.0156 1.1549 0.3325 0.031 Uiso 1 1 calc R . .
C6 C 0.3149(2) 0.6799(9) 0.5462(4) 0.0236(9) Uani 1 1 d . . .
C7 C 0.3749(3) 0.5579(16) 0.6350(5) 0.0463(16) Uani 1 1 d . . .
H7A H 0.3850 0.6749 0.7181 0.056 Uiso 1 1 calc R . .
H7B H 0.3615 0.3757 0.6679 0.056 Uiso 1 1 calc R . .
C8 C 0.4391(2) 0.5265(12) 0.5631(4) 0.0312(11) Uani 1 1 d . . .
C9 C 0.4459(3) 0.3277(12) 0.4630(7) 0.0431(14) Uani 1 1 d . . .
H9 H 0.4089 0.2076 0.4376 0.052 Uiso 1 1 calc R . .
C10 C 0.4951(3) 0.6982(12) 0.5995(6) 0.0395(13) Uani 1 1 d . . .
H10 H 0.4918 0.8346 0.6687 0.047 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
Zn1 O2 1.949(3) 1_545 ?
Zn1 O3 1.957(4) . ?
Zn1 O1 1.960(4) . ?
Zn1 O4 1.974(4) 4_575 ?
O1 C1 1.269(5) . ?
O2 C1 1.270(6) . ?
O2 Zn1 1.949(3) 1_565 ?
O3 C6 1.256(6) . ?
O4 C6 1.247(6) . ?
O4 Zn1 1.974(4) 4_576 ?
C1 C2 1.503(6) . ?
C2 C3 1.521(6) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C5 1.350(7) . ?
C3 C4 1.423(6) . ?
C4 C5 1.407(6) 3_586 ?
C4 H4 0.9500 . ?
C5 C4 1.407(6) 3_586 ?
C5 H5 0.9500 . ?
C6 C7 1.516(6) . ?
C7 C8 1.506(6) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C9 1.384(8) . ?
C8 C10 1.405(8) . ?
C9 C10 1.364(8) 3_666 ?
C9 H9 0.9500 . ?
C10 C9 1.364(8) 3_666 ?
C10 H10 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Zn1 O3 113.17(16) 1_545 . ?
O2 Zn1 O1 111.01(16) 1_545 . ?
O3 Zn1 O1 111.60(17) . . ?
O2 Zn1 O4 110.32(15) 1_545 4_575 ?
O3 Zn1 O4 108.24(17) . 4_575 ?
O1 Zn1 O4 101.89(16) . 4_575 ?
C1 O1 Zn1 132.8(3) . . ?
C1 O2 Zn1 120.7(3) . 1_565 ?
C6 O3 Zn1 119.6(3) . . ?
C6 O4 Zn1 130.4(3) . 4_576 ?
O1 C1 O2 120.8(4) . . ?
O1 C1 C2 120.3(4) . . ?
O2 C1 C2 118.9(4) . . ?
C1 C2 C3 115.5(4) . . ?
C1 C2 H2A 108.4 . . ?
C3 C2 H2A 108.4 . . ?
C1 C2 H2B 108.4 . . ?
C3 C2 H2B 108.4 . . ?
H2A C2 H2B 107.5 . . ?
C5 C3 C4 119.6(4) . . ?
C5 C3 C2 122.2(4) . . ?
C4 C3 C2 118.0(4) . . ?
C5 C4 C3 119.0(4) 3_586 . ?
C5 C4 H4 120.5 3_586 . ?
C3 C4 H4 120.5 . . ?
C3 C5 C4 121.3(4) . 3_586 ?
C3 C5 H5 119.3 . . ?
C4 C5 H5 119.3 3_586 . ?
O4 C6 O3 121.8(4) . . ?
O4 C6 C7 119.6(4) . . ?
O3 C6 C7 118.6(4) . . ?
C8 C7 C6 115.1(4) . . ?
C8 C7 H7A 108.5 . . ?
C6 C7 H7A 108.5 . . ?
C8 C7 H7B 108.5 . . ?
C6 C7 H7B 108.5 . . ?
H7A C7 H7B 107.5 . . ?
C9 C8 C10 118.0(4) . . ?
C9 C8 C7 122.1(5) . . ?
C10 C8 C7 119.8(5) . . ?
C10 C9 C8 121.0(5) 3_666 . ?
C10 C9 H9 119.5 3_666 . ?
C8 C9 H9 119.5 . . ?
C9 C10 C8 121.0(5) 3_666 . ?
C9 C10 H10 119.5 3_666 . ?
C8 C10 H10 119.5 . . ?

_diffrn_measured_fraction_theta_max 0.977
_diffrn_reflns_theta_full        27.46
_diffrn_measured_fraction_theta_full 0.99
_refine_diff_density_max         0.658
_refine_diff_density_min         -0.721
_refine_diff_density_rms         0.152

# Attachment '1b.CIF'

data_1b
_database_code_depnum_ccdc_archive 'CCDC 695289'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C10 H12 Mn O6 '
_chemical_formula_sum            'C10 H12 Mn O6'
_chemical_formula_weight         283.14

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'
O O 0.0106 0.0060 '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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P21/c
_symmetry_space_group_name_Hall  '-P 2ybc '

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

_cell_length_a                   9.836(7)
_cell_length_b                   6.149(4)
_cell_length_c                   8.882(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 100.850(15)
_cell_angle_gamma                90.00
_cell_volume                     527.6(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    2184
_cell_measurement_theta_min      3.0825
_cell_measurement_theta_max      27.4526

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.782
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             282.0
_exptl_absorpt_coefficient_mu    1.264
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_max  0.680
_exptl_absorpt_correction_T_min  0.600
_exptl_absorpt_process_details   CrystalClear

_exptl_special_details           
;
empirical from equivalent reflections (XEMP in
SHELXTL; Siemens,1994)
;

_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  'Graphite '
_diffrn_measurement_device_type  
;
Mercury70 (2x2 bin mode)
;
_diffrn_measurement_method       CCD_Profile_fitting
_diffrn_detector_area_resol_mean 13.6612
_diffrn_standards_number         1308
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_decay_%        none
_diffrn_reflns_number            3878
_diffrn_reflns_av_R_equivalents  0.0295
_diffrn_reflns_av_sigmaI/netI    0.0268
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         3.93
_diffrn_reflns_theta_max         27.48
_reflns_number_total             1203
_reflns_number_gt                1076
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXS-97 (Sheldrick, 1990)'
_computing_publication_material  'SHELXS-97 (Sheldrick, 1990)'

_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
[1.00000+0.00000exp(0.00(sinθ/λ)²)]/
[σ²(Fo²)+0.0000+0.0000*P+(0.1600P)²+0.0000sinθ/λ]
where P = 0.00000Fo² + 1.00000Fc²
;
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         1189
_refine_ls_number_parameters     79
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0690
_refine_ls_R_factor_gt           0.0398
_refine_ls_wR_factor_ref         0.1789
_refine_ls_wR_factor_gt          0.1348
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_restrained_S_all      1.001
_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
Mn1 Mn 0.5000 0.0000 1.0000 0.0230(3) Uani 1 2 d S . .
O1 O 0.67090(17) 0.1033(3) 0.8980(2) 0.0311(5) Uani 1 1 d . . .
C3 C 0.9129(2) 0.3903(4) 0.8791(3) 0.0234(5) Uani 1 1 d . . .
O2 O 0.57303(19) 0.3329(3) 0.7173(2) 0.0396(5) Uani 1 1 d . . .
O3 O 0.6086(2) -0.3029(3) 1.0878(2) 0.0430(6) Uani 1 1 d . . .
C5 C 1.0314(2) 0.2910(4) 0.9604(3) 0.0261(5) Uani 1 1 d . . .
H5 H 1.0542 0.1476 0.9339 0.031 Uiso 1 1 calc R . .
C1 C 0.6774(2) 0.2339(4) 0.7912(3) 0.0230(5) Uani 1 1 d . . .
C4 C 0.8832(2) 0.6017(4) 0.9204(3) 0.0266(6) Uani 1 1 d . . .
H4 H 0.8032 0.6733 0.8660 0.032 Uiso 1 1 calc R . .
C2 C 0.8179(3) 0.2731(4) 0.7507(3) 0.0289(6) Uani 1 1 d . . .
H2B H 0.8070 0.3613 0.6559 0.035 Uiso 1 1 calc R . .
H2A H 0.8598 0.1321 0.7308 0.035 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

Mn1 O1 2.150(2) 3_657 ?
Mn1 O2 2.185(2) 4_566 ?
Mn1 O3 2.215(2) 3_657 ?
O1 C1 1.253(3) . ?
C3 C5 1.391(3) . ?
C3 C4 1.397(4) . ?
C3 C2 1.514(3) . ?
O2 C1 1.265(3) . ?
C5 C4 1.388(3) 3_767 ?
C1 C2 1.512(3) . ?

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 Mn1 O1 180.00(4) . 3_657 ?
O1 Mn1 O2 94.60(8) . 4_566 ?
O1 Mn1 O2 85.40(8) 3_657 4_566 ?
O1 Mn1 O2 85.40(8) . 2_646 ?
O1 Mn1 O2 94.60(8) 3_657 2_646 ?
O2 Mn1 O2 180.0 4_566 2_646 ?
O1 Mn1 O3 88.11(8) . 3_657 ?
O1 Mn1 O3 91.89(8) 3_657 3_657 ?
O2 Mn1 O3 88.40(9) 4_566 3_657 ?
O2 Mn1 O3 91.60(9) 2_646 3_657 ?
O1 Mn1 O3 91.89(8) . . ?
O1 Mn1 O3 88.11(8) 3_657 . ?
O2 Mn1 O3 91.60(9) 4_566 . ?
O2 Mn1 O3 88.40(9) 2_646 . ?
O3 Mn1 O3 180.000(1) 3_657 . ?
C1 O1 Mn1 131.52(16) . . ?
C5 C3 C4 117.9(2) . . ?
C5 C3 C2 121.3(2) . . ?
C4 C3 C2 120.7(2) . . ?
C1 O2 Mn1 141.63(18) . 2_656 ?
C4 C5 C3 121.0(2) 3_767 . ?
O1 C1 O2 123.3(2) . . ?
O1 C1 C2 117.5(2) . . ?
O2 C1 C2 119.2(2) . . ?
C5 C4 C3 121.1(2) 3_767 . ?
C1 C2 C3 111.05(19) . . ?

_diffrn_measured_fraction_theta_max 0.988
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.988
_refine_diff_density_max         1.629
_refine_diff_density_min         -2.167
_refine_diff_density_rms         0.491

# Attachment '2a.cif'

# Attachment '2a.CIF'

data_2a
_database_code_depnum_ccdc_archive 'CCDC 695290'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C20 H18 N2 O5 Zn'
_chemical_formula_sum            'C20 H18 N2 O5 Zn'
_chemical_formula_weight         431.73

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'
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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1
_symmetry_space_group_name_Hall  '-P 1'

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

_cell_length_a                   9.700(4)
_cell_length_b                   10.470(5)
_cell_length_c                   10.500(5)
_cell_angle_alpha                113.980(4)
_cell_angle_beta                 96.830(4)
_cell_angle_gamma                105.560(2)
_cell_volume                     906.6(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    2184
_cell_measurement_theta_min      3.0825
_cell_measurement_theta_max      27.4526

_exptl_crystal_description       Prism
_exptl_crystal_colour            White
_exptl_crystal_size_max          0.1500
_exptl_crystal_size_mid          0.1000
_exptl_crystal_size_min          0.0500
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.574
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             440
_exptl_absorpt_coefficient_mu    1.390
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_max  0.930
_exptl_absorpt_correction_T_min  0.846
_exptl_absorpt_process_details   CrystalClear

_exptl_special_details           
;
empirical from equivalent reflections (XEMP in
SHELXTL; Siemens,1994)
;

_diffrn_ambient_temperature      298(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  
;
Mercury70 (2x2 bin mode)
;
_diffrn_measurement_method       CCD_Profile_fitting
_diffrn_detector_area_resol_mean 14.6306
_diffrn_standards_number         none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_decay_%        none
_diffrn_reflns_number            7100
_diffrn_reflns_av_R_equivalents  0.0324
_diffrn_reflns_av_sigmaI/netI    0.0619
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.26
_diffrn_reflns_theta_max         27.48
_reflns_number_total             4101
_reflns_number_gt                2994
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_cell_refinement       'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_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)+(0.1119P)²+2.0327P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4101
_refine_ls_number_parameters     243
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.0968
_refine_ls_R_factor_gt           0.0703
_refine_ls_wR_factor_ref         0.2047
_refine_ls_wR_factor_gt          0.1814
_refine_ls_goodness_of_fit_ref   0.979
_refine_ls_restrained_S_all      0.976
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.37663(7) 0.34535(6) 0.54590(6) 0.0360(2) Uani 1 1 d . . .
C1 C 0.2997(6) 0.6136(6) 0.7348(5) 0.0365(11) Uani 1 1 d . . .
H1A H 0.2379 0.5839 0.6431 0.044 Uiso 1 1 calc R . .
C2 C 0.2896(6) 0.7299(6) 0.8541(5) 0.0364(11) Uani 1 1 d . . .
H2A H 0.2214 0.7777 0.8439 0.044 Uiso 1 1 calc R . .
C3 C 0.3810(5) 0.7764(5) 0.9897(5) 0.0300(10) Uani 1 1 d . . .
C4 C 0.4768(6) 0.7002(5) 0.9975(5) 0.0356(11) Uani 1 1 d . . .
H4A H 0.5403 0.7274 1.0875 0.043 Uiso 1 1 calc R . .
C5 C 0.4782(6) 0.5835(5) 0.8715(5) 0.0353(11) Uani 1 1 d . . .
H5A H 0.5436 0.5319 0.8781 0.042 Uiso 1 1 calc R . .
C6 C 0.3740(6) 0.9035(5) 1.1178(5) 0.0343(11) Uani 1 1 d . . .
C7 C 0.3419(6) 1.0196(5) 1.1037(5) 0.0393(12) Uani 1 1 d . . .
H7A H 0.3226 1.0173 1.0118 0.047 Uiso 1 1 calc R . .
C8 C 0.3384(6) 1.1386(5) 1.2249(5) 0.0380(12) Uani 1 1 d . . .
H8A H 0.3159 1.2167 1.2130 0.046 Uiso 1 1 calc R . .
C9 C 0.3910(9) 1.0359(7) 1.3688(6) 0.063(2) Uani 1 1 d . . .
H9A H 0.4059 1.0396 1.4615 0.076 Uiso 1 1 calc R . .
C10 C 0.3981(8) 0.9134(7) 1.2550(6) 0.0556(17) Uani 1 1 d . . .
H10A H 0.4192 0.8365 1.2703 0.067 Uiso 1 1 calc R . .
C11 C 0.1732(7) 0.1888(8) 0.6315(6) 0.0582(18) Uani 1 1 d . . .
C12 C 0.0423(7) 0.1384(7) 0.6859(6) 0.0550(16) Uani 1 1 d . . .
H12A H -0.0456 0.1470 0.6363 0.066 Uiso 1 1 calc R . .
H12B H 0.0201 0.0322 0.6626 0.066 Uiso 1 1 calc R . .
C13 C 0.0723(6) 0.2302(6) 0.8459(6) 0.0423(12) Uani 1 1 d . . .
C14 C 0.0448(7) 0.1662(6) 0.9361(6) 0.0503(14) Uani 1 1 d . . .
H14A H 0.0102 0.0606 0.8972 0.060 Uiso 1 1 calc R . .
C15 C 0.0669(7) 0.2532(7) 1.0828(6) 0.0493(14) Uani 1 1 d . . .
H15A H 0.0445 0.2063 1.1423 0.059 Uiso 1 1 calc R . .
C16 C 0.1209(6) 0.4070(6) 1.1437(6) 0.0435(13) Uani 1 1 d . . .
C17 C 0.1514(7) 0.4717(6) 1.0546(6) 0.0456(13) Uani 1 1 d . . .
H17A H 0.1896 0.5773 1.0943 0.055 Uiso 1 1 calc R . .
C18 C 0.1270(7) 0.3845(6) 0.9075(6) 0.0458(13) Uani 1 1 d . . .
H18A H 0.1481 0.4316 0.8479 0.055 Uiso 1 1 calc R . .
C19 C 0.1509(8) 0.5036(8) 1.3050(6) 0.0590(17) Uani 1 1 d . . .
H19A H 0.0792 0.4536 1.3445 0.071 Uiso 1 1 calc R . .
H19B H 0.1402 0.6006 1.3239 0.071 Uiso 1 1 calc R . .
C20 C 0.3079(7) 0.5280(6) 1.3766(5) 0.0427(14) Uani 1 1 d . . .
N1 N 0.3924(5) 0.5409(4) 0.7424(4) 0.0332(9) Uani 1 1 d . . .
N2 N 0.3645(5) 1.1500(5) 1.3567(4) 0.0406(10) Uani 1 1 d . . .
O1 O 0.1599(6) 0.2536(7) 0.5550(5) 0.0855(12) Uani 1 1 d U . .
O2 O 0.2885(7) 0.1720(7) 0.6648(5) 0.0855(12) Uani 1 1 d U . .
O3 O 0.4109(6) 0.6316(5) 1.3778(5) 0.0656(10) Uani 1 1 d U . .
O4 O 0.3244(6) 0.4402(5) 1.4213(5) 0.0656(10) Uani 1 1 d U . .
O5W O 0.1218(13) 0.8058(13) 0.6275(10) 0.177(5) 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
Zn1 O4 2.030(4) 1_554 ?
Zn1 O3 2.033(5) 2_667 ?
Zn1 O1 2.095(6) . ?
Zn1 N2 2.158(4) 1_544 ?
Zn1 N1 2.190(4) . ?
C1 N1 1.340(6) . ?
C1 C2 1.384(6) . ?
C1 H1A 0.9500 . ?
C2 C3 1.398(7) . ?
C2 H2A 0.9500 . ?
C3 C4 1.393(7) . ?
C3 C6 1.482(6) . ?
C4 C5 1.394(7) . ?
C4 H4A 0.9500 . ?
C5 N1 1.331(6) . ?
C5 H5A 0.9500 . ?
C6 C10 1.388(7) . ?
C6 C7 1.391(7) . ?
C7 C8 1.385(7) . ?
C7 H7A 0.9500 . ?
C8 N2 1.327(6) . ?
C8 H8A 0.9500 . ?
C9 N2 1.337(7) . ?
C9 C10 1.378(8) . ?
C9 H9A 0.9500 . ?
C10 H10A 0.9500 . ?
C11 O2 1.211(8) . ?
C11 O1 1.260(9) . ?
C11 C12 1.507(10) . ?
C12 C13 1.501(8) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C14 1.377(8) . ?
C13 C18 1.386(8) . ?
C14 C15 1.388(8) . ?
C14 H14A 0.9500 . ?
C15 C16 1.381(8) . ?
C15 H15A 0.9500 . ?
C16 C17 1.376(8) . ?
C16 C19 1.519(8) . ?
C17 C18 1.388(8) . ?
C17 H17A 0.9500 . ?
C18 H18A 0.9500 . ?
C19 C20 1.521(9) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 O4 1.226(6) . ?
C20 O3 1.257(8) . ?

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
O4 Zn1 O3 122.1(2) 1_554 2_667 ?
O4 Zn1 O1 96.2(3) 1_554 . ?
O3 Zn1 O1 141.6(2) 2_667 . ?
O4 Zn1 N2 90.58(17) 1_554 1_544 ?
O3 Zn1 N2 87.78(17) 2_667 1_544 ?
O1 Zn1 N2 94.5(2) . 1_544 ?
O4 Zn1 N1 91.31(16) 1_554 . ?
O3 Zn1 N1 90.89(17) 2_667 . ?
O1 Zn1 N1 85.71(18) . . ?
N2 Zn1 N1 178.07(15) 1_544 . ?
N1 C1 C2 123.2(4) . . ?
N1 C1 H1A 118.4 . . ?
C2 C1 H1A 118.4 . . ?
C1 C2 C3 119.2(4) . . ?
C1 C2 H2A 120.4 . . ?
C3 C2 H2A 120.4 . . ?
C4 C3 C2 117.5(4) . . ?
C4 C3 C6 122.7(4) . . ?
C2 C3 C6 119.8(4) . . ?
C3 C4 C5 119.2(4) . . ?
C3 C4 H4A 120.4 . . ?
C5 C4 H4A 120.4 . . ?
N1 C5 C4 123.1(4) . . ?
N1 C5 H5A 118.4 . . ?
C4 C5 H5A 118.4 . . ?
C10 C6 C7 116.9(4) . . ?
C10 C6 C3 122.9(4) . . ?
C7 C6 C3 120.2(4) . . ?
C8 C7 C6 119.4(4) . . ?
C8 C7 H7A 120.3 . . ?
C6 C7 H7A 120.3 . . ?
N2 C8 C7 123.8(5) . . ?
N2 C8 H8A 118.1 . . ?
C7 C8 H8A 118.1 . . ?
N2 C9 C10 124.0(5) . . ?
N2 C9 H9A 118.0 . . ?
C10 C9 H9A 118.0 . . ?
C9 C10 C6 119.4(5) . . ?
C9 C10 H10A 120.3 . . ?
C6 C10 H10A 120.3 . . ?
O2 C11 O1 121.4(7) . . ?
O2 C11 C12 120.9(7) . . ?
O1 C11 C12 117.7(6) . . ?
C13 C12 C11 111.3(5) . . ?
C13 C12 H12A 109.4 . . ?
C11 C12 H12A 109.4 . . ?
C13 C12 H12B 109.4 . . ?
C11 C12 H12B 109.4 . . ?
H12A C12 H12B 108.0 . . ?
C14 C13 C18 117.7(5) . . ?
C14 C13 C12 122.1(5) . . ?
C18 C13 C12 120.2(5) . . ?
C13 C14 C15 121.1(5) . . ?
C13 C14 H14A 119.4 . . ?
C15 C14 H14A 119.4 . . ?
C16 C15 C14 121.0(6) . . ?
C16 C15 H15A 119.5 . . ?
C14 C15 H15A 119.5 . . ?
C17 C16 C15 118.1(5) . . ?
C17 C16 C19 120.3(6) . . ?
C15 C16 C19 121.5(6) . . ?
C16 C17 C18 120.9(5) . . ?
C16 C17 H17A 119.6 . . ?
C18 C17 H17A 119.6 . . ?
C13 C18 C17 121.2(5) . . ?
C13 C18 H18A 119.4 . . ?
C17 C18 H18A 119.4 . . ?
C16 C19 C20 108.3(5) . . ?
C16 C19 H19A 110.0 . . ?
C20 C19 H19A 110.0 . . ?
C16 C19 H19B 110.0 . . ?
C20 C19 H19B 110.0 . . ?
H19A C19 H19B 108.4 . . ?
O4 C20 O3 125.3(6) . . ?
O4 C20 C19 117.5(6) . . ?
O3 C20 C19 117.1(5) . . ?
C5 N1 C1 117.8(4) . . ?
C5 N1 Zn1 124.0(3) . . ?
C1 N1 Zn1 117.8(3) . . ?
C8 N2 C9 116.5(4) . . ?
C8 N2 Zn1 122.8(3) . 1_566 ?
C9 N2 Zn1 120.6(3) . 1_566 ?
C11 O1 Zn1 104.2(5) . . ?
C20 O3 Zn1 118.3(4) . 2_667 ?
C20 O4 Zn1 164.7(4) . 1_556 ?

_diffrn_measured_fraction_theta_max 0.984
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.984
_refine_diff_density_max         1.144
_refine_diff_density_min         -1.019
_refine_diff_density_rms         0.105

# Attachment '2b.CIF'

data_2b

_database_code_depnum_ccdc_archive 'CCDC 695291'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C20 H18 Co N2 O4, O'
_chemical_formula_sum            'C20 H18 Co N2 O5'
_chemical_formula_weight         425.29

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1
_symmetry_space_group_name_Hall  '-P 1'

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

_cell_length_a                   9.814(3)
_cell_length_b                   10.545(3)
_cell_length_c                   10.595(3)
_cell_angle_alpha                112.508(6)
_cell_angle_beta                 106.884(11)
_cell_angle_gamma                96.478(4)
_cell_volume                     937.6(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    1001
_cell_measurement_theta_min      2.2039
_cell_measurement_theta_max      27.4835

_exptl_crystal_description       Prism
_exptl_crystal_colour            Colorless
_exptl_crystal_size_max          0.2000
_exptl_crystal_size_mid          0.2000
_exptl_crystal_size_min          0.2000
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.499
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             434
_exptl_absorpt_coefficient_mu    0.950
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_max  0.826
_exptl_absorpt_correction_T_min  0.825
_exptl_absorpt_process_details   CrystalClear

_exptl_special_details           
;
empirical from equivalent reflections (XEMP in
SHELXTL; Siemens,1994)
;

_diffrn_ambient_temperature      298(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  
;
Mercury2 (2x2 bin mode)
;
_diffrn_measurement_method       CCD_Profile_fitting
_diffrn_detector_area_resol_mean 13.6612
_diffrn_standards_number         4109
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_decay_%        none
_diffrn_reflns_number            7054
_diffrn_reflns_av_R_equivalents  0.0402
_diffrn_reflns_av_sigmaI/netI    0.0640
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.52
_diffrn_reflns_theta_max         28.08
_reflns_number_total             4551
_reflns_number_gt                3107
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_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)+(0.1088P)²+0.1353P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4090
_refine_ls_number_parameters     253
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0765
_refine_ls_R_factor_gt           0.0557
_refine_ls_wR_factor_ref         0.1918
_refine_ls_wR_factor_gt          0.1548
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_restrained_S_all      1.075
_refine_ls_shift/su_max          0.007
_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
Co1 Co -0.12531(6) 0.04361(5) 0.33657(5) 0.0339(2) Uani 1 1 d . . .
C1 C 0.1993(5) 0.1167(4) 0.4834(4) 0.0388(9) Uani 1 1 d . . .
C2 C 0.3594(5) 0.1866(4) 0.5130(5) 0.0442(10) Uani 1 1 d . . .
H2A H 0.3740 0.1675 0.4194 0.053 Uiso 1 1 calc R . .
H2B H 0.4293 0.1488 0.5683 0.053 Uiso 1 1 calc R . .
C3 C 0.3843(4) 0.3485(4) 0.6043(4) 0.0369(8) Uani 1 1 d . . .
C4 C 0.3585(5) 0.4392(4) 0.5409(5) 0.0440(10) Uani 1 1 d . . .
H4 H 0.3278 0.4025 0.4373 0.053 Uiso 1 1 calc R . .
C5 C 0.3758(5) 0.5848(4) 0.6240(5) 0.0458(10) Uani 1 1 d . . .
H5 H 0.3543 0.6420 0.5736 0.055 Uiso 1 1 calc R . .
C6 C 0.4220(5) 0.6483(4) 0.7740(5) 0.0421(9) Uani 1 1 d . . .
C7 C 0.4475(5) 0.5572(4) 0.8386(5) 0.0493(11) Uani 1 1 d . . .
H7 H 0.4771 0.5943 0.9422 0.059 Uiso 1 1 calc R . .
C8 C 0.4311(5) 0.4105(5) 0.7557(5) 0.0504(11) Uani 1 1 d . . .
H8 H 0.4528 0.3531 0.8058 0.061 Uiso 1 1 calc R . .
C9 C 0.4476(6) 0.8098(5) 0.8662(6) 0.0645(15) Uani 1 1 d . . .
H9A H 0.4526 0.8274 0.9664 0.077 Uiso 1 1 calc R . .
H9B H 0.5436 0.8600 0.8744 0.077 Uiso 1 1 calc R . .
C10 C 0.3269(5) 0.8713(4) 0.8006(4) 0.0444(10) Uani 1 1 d . . .
C11 C -0.0230(4) 0.3669(4) 0.5736(4) 0.0342(8) Uani 1 1 d . . .
H11 H 0.0434 0.3741 0.5254 0.041 Uiso 1 1 calc R . .
C12 C -0.0235(4) 0.4942(4) 0.6911(4) 0.0341(8) Uani 1 1 d . . .
H12 H 0.0397 0.5826 0.7171 0.041 Uiso 1 1 calc R . .
C13 C -0.1187(4) 0.4868(4) 0.7674(4) 0.0315(8) Uani 1 1 d . . .
C14 C -0.2124(4) 0.3532(4) 0.7200(4) 0.0361(8) Uani 1 1 d . . .
H14 H -0.2799 0.3431 0.7662 0.043 Uiso 1 1 calc R . .
C15 C -0.2053(5) 0.2339(4) 0.6028(4) 0.0379(9) Uani 1 1 d . . .
H15 H -0.2694 0.1450 0.5735 0.045 Uiso 1 1 calc R . .
C16 C -0.1240(4) 0.6157(4) 0.8961(4) 0.0327(8) Uani 1 1 d . . .
C17 C -0.1035(5) 0.7523(4) 0.9053(5) 0.0480(11) Uani 1 1 d . . .
H17 H -0.0838 0.7693 0.8298 0.058 Uiso 1 1 calc R . .
C18 C -0.1120(6) 0.8671(4) 1.0284(5) 0.0504(11) Uani 1 1 d . . .
H18 H -0.1009 0.9582 1.0292 0.061 Uiso 1 1 calc R . .
C19 C -0.1557(5) 0.7219(4) 1.1286(4) 0.0407(9) Uani 1 1 d . . .
H19 H -0.1743 0.7074 1.2058 0.049 Uiso 1 1 calc R . .
C20 C -0.1529(5) 0.6017(4) 1.0093(4) 0.0408(9) Uani 1 1 d . . .
H20 H -0.1712 0.5108 1.0080 0.049 Uiso 1 1 calc R . .
N1 N -0.1119(4) 0.2373(3) 0.5279(3) 0.0345(7) Uani 1 1 d . . .
N2 N -0.1343(4) 0.8548(3) 1.1410(3) 0.0373(7) Uani 1 1 d . . .
O1 O 0.1730(4) 0.0855(3) 0.5768(4) 0.0593(9) Uani 1 1 d . . .
O2 O 0.0986(3) 0.1028(3) 0.3722(3) 0.0464(7) Uani 1 1 d . . .
O3 O 0.1943(4) 0.8390(3) 0.7922(4) 0.0544(8) Uani 1 1 d . . .
O4 O 0.3619(4) 0.9528(3) 0.7488(3) 0.0512(8) Uani 1 1 d . . .
O5 O 0.3621(7) 0.8704(7) 0.1898(8) 0.143(3) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 O1 1.994(3) 2_556 ?
Co1 O2 2.095(3) . ?
Co1 O3 2.191(3) 2_566 ?
Co1 N1 2.216(3) . ?
Co1 N2 2.227(3) 1_544 ?
Co1 O4 2.244(3) 2_566 ?
C1 O1 1.238(5) . ?
C1 O2 1.243(5) . ?
C1 C2 1.544(6) . ?
C2 C3 1.554(5) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.370(6) . ?
C3 C8 1.383(6) . ?
C4 C5 1.408(6) . ?
C4 H4 0.9500 . ?
C5 C6 1.370(6) . ?
C5 H5 0.9500 . ?
C6 C7 1.383(6) . ?
C6 C9 1.551(6) . ?
C7 C8 1.418(6) . ?
C7 H7 0.9500 . ?
C8 H8 0.9500 . ?
C9 C10 1.532(6) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 O4 1.250(5) . ?
C10 O3 1.275(6) . ?
C11 N1 1.358(5) . ?
C11 C12 1.441(5) . ?
C11 H11 0.9500 . ?
C12 C13 1.416(5) . ?
C12 H12 0.9500 . ?
C13 C14 1.407(5) . ?
C13 C16 1.531(5) . ?
C14 C15 1.415(5) . ?
C14 H14 0.9500 . ?
C15 N1 1.381(5) . ?
C15 H15 0.9500 . ?
C16 C20 1.365(5) . ?
C16 C17 1.393(5) . ?
C17 C18 1.432(6) . ?
C17 H17 0.9500 . ?
C18 N2 1.324(5) . ?
C18 H18 0.9500 . ?
C19 N2 1.342(5) . ?
C19 C20 1.417(5) . ?
C19 H19 0.9500 . ?
C20 H20 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
O1 Co1 O2 114.29(14) 2_556 . ?
O1 Co1 O3 150.71(16) 2_556 2_566 ?
O2 Co1 O3 94.97(12) . 2_566 ?
O1 Co1 N1 93.53(12) 2_556 . ?
O2 Co1 N1 93.39(12) . . ?
O3 Co1 N1 85.67(12) 2_566 . ?
O1 Co1 N2 88.81(13) 2_556 1_544 ?
O2 Co1 N2 85.13(12) . 1_544 ?
O3 Co1 N2 92.56(12) 2_566 1_544 ?
N1 Co1 N2 177.59(11) . 1_544 ?
O1 Co1 O4 91.77(14) 2_556 2_566 ?
O2 Co1 O4 153.92(12) . 2_566 ?
O3 Co1 O4 59.01(12) 2_566 2_566 ?
N1 Co1 O4 83.62(12) . 2_566 ?
N2 Co1 O4 96.87(12) 1_544 2_566 ?
O1 C1 O2 121.4(4) . . ?
O1 C1 C2 119.0(4) . . ?
O2 C1 C2 119.4(4) . . ?
C1 C2 C3 106.5(3) . . ?
C1 C2 H2A 110.4 . . ?
C3 C2 H2A 110.4 . . ?
C1 C2 H2B 110.4 . . ?
C3 C2 H2B 110.4 . . ?
H2A C2 H2B 108.6 . . ?
C4 C3 C8 115.3(4) . . ?
C4 C3 C2 122.6(4) . . ?
C8 C3 C2 122.0(4) . . ?
C3 C4 C5 122.3(4) . . ?
C3 C4 H4 118.9 . . ?
C5 C4 H4 118.9 . . ?
C6 C5 C4 123.3(4) . . ?
C6 C5 H5 118.4 . . ?
C4 C5 H5 118.4 . . ?
C5 C6 C7 114.7(4) . . ?
C5 C6 C9 123.4(4) . . ?
C7 C6 C9 121.9(4) . . ?
C6 C7 C8 122.3(4) . . ?
C6 C7 H7 118.8 . . ?
C8 C7 H7 118.8 . . ?
C3 C8 C7 122.0(4) . . ?
C3 C8 H8 119.0 . . ?
C7 C8 H8 119.0 . . ?
C10 C9 C6 113.2(4) . . ?
C10 C9 H9A 108.9 . . ?
C6 C9 H9A 108.9 . . ?
C10 C9 H9B 108.9 . . ?
C6 C9 H9B 108.9 . . ?
H9A C9 H9B 107.8 . . ?
O4 C10 O3 119.8(4) . . ?
O4 C10 C9 116.9(4) . . ?
O3 C10 C9 123.2(4) . . ?
N1 C11 C12 123.7(3) . . ?
N1 C11 H11 118.1 . . ?
C12 C11 H11 118.1 . . ?
C13 C12 C11 119.7(3) . . ?
C13 C12 H12 120.2 . . ?
C11 C12 H12 120.2 . . ?
C14 C13 C12 117.1(3) . . ?
C14 C13 C16 119.7(3) . . ?
C12 C13 C16 123.3(3) . . ?
C13 C14 C15 119.5(3) . . ?
C13 C14 H14 120.3 . . ?
C15 C14 H14 120.3 . . ?
N1 C15 C14 124.8(3) . . ?
N1 C15 H15 117.6 . . ?
C14 C15 H15 117.6 . . ?
C20 C16 C17 115.5(4) . . ?
C20 C16 C13 121.0(3) . . ?
C17 C16 C13 123.5(3) . . ?
C16 C17 C18 120.2(4) . . ?
C16 C17 H17 119.9 . . ?
C18 C17 H17 119.9 . . ?
N2 C18 C17 124.3(4) . . ?
N2 C18 H18 117.8 . . ?
C17 C18 H18 117.8 . . ?
N2 C19 C20 125.1(4) . . ?
N2 C19 H19 117.4 . . ?
C20 C19 H19 117.4 . . ?
C16 C20 C19 120.5(3) . . ?
C16 C20 H20 119.8 . . ?
C19 C20 H20 119.8 . . ?
C11 N1 C15 115.3(3) . . ?
C11 N1 Co1 124.3(3) . . ?
C15 N1 Co1 120.3(2) . . ?
C18 N2 C19 114.3(3) . . ?
C18 N2 Co1 121.5(3) . 1_566 ?
C19 N2 Co1 124.2(3) . 1_566 ?
C1 O1 Co1 156.0(3) . 2_556 ?
C1 O2 Co1 123.5(3) . . ?
C10 O3 Co1 91.4(3) . 2_566 ?
C10 O4 Co1 89.6(3) . 2_566 ?

_diffrn_measured_fraction_theta_max 27.4835
_diffrn_reflns_theta_full        27.4835
_diffrn_measured_fraction_theta_full 99.4000
_refine_diff_density_max         0.589
_refine_diff_density_min         -0.534
_refine_diff_density_rms         0.093

# Attachment '2c.CIF'

data_2c
_database_code_depnum_ccdc_archive 'CCDC 695292'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C20 H18 Cd N2 O4, O'
_chemical_formula_sum            'C20 H18 Cd N2 O5'
_chemical_formula_weight         478.76

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'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1
_symmetry_space_group_name_Hall  '-P 1'

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

_cell_length_a                   9.814(3)
_cell_length_b                   10.545(3)
_cell_length_c                   10.595(3)
_cell_angle_alpha                112.508(6)
_cell_angle_beta                 106.884(11)
_cell_angle_gamma                96.478(4)
_cell_volume                     937.6(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    2050
_cell_measurement_theta_min      2.1609
_cell_measurement_theta_max      27.4632

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.696
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             476.0
_exptl_absorpt_coefficient_mu    1.199
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.749
_exptl_absorpt_correction_T_max  0.788
_exptl_absorpt_process_details   CrystalClear

_exptl_special_details           
;
empirical from equivalent reflections (XEMP in
SHELXTL; Siemens,1994)
;

_diffrn_ambient_temperature      298(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  
;
Mercury2 (2x2 bin mode)
;
_diffrn_measurement_method       CCD_Profile_fitting
_diffrn_detector_area_resol_mean 13.6612
_diffrn_standards_number         4091
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_decay_%        none
_diffrn_reflns_number            7146
_diffrn_reflns_av_R_equivalents  0.0487
_diffrn_reflns_av_sigmaI/netI    0.0842
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.33
_diffrn_reflns_theta_max         27.47
_reflns_number_total             4302
_reflns_number_gt                2693
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_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)+(0.0953P)²+0.9312P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4073
_refine_ls_number_parameters     253
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1003
_refine_ls_R_factor_gt           0.0603
_refine_ls_wR_factor_ref         0.1933
_refine_ls_wR_factor_gt          0.1474
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_restrained_S_all      1.072
_refine_ls_shift/su_max          0.007
_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
Cd1 Cd -0.11658(7) 0.05243(5) 0.34682(6) 0.0395(2) Uani 1 1 d . . .
C1 C 0.1929(10) 0.1366(8) 0.4581(10) 0.047(2) Uani 1 1 d . . .
C2 C 0.3574(10) 0.2000(11) 0.5116(13) 0.067(3) Uani 1 1 d . . .
H2A H 0.4125 0.1572 0.5721 0.080 Uiso 1 1 calc R . .
H2B H 0.3894 0.1814 0.4272 0.080 Uiso 1 1 calc R . .
C3 C 0.3862(8) 0.3580(9) 0.6021(10) 0.047(2) Uani 1 1 d . . .
C4 C 0.3586(10) 0.4489(9) 0.5400(10) 0.051(2) Uani 1 1 d . . .
H4 H 0.3210 0.4118 0.4362 0.061 Uiso 1 1 calc R . .
C5 C 0.3838(10) 0.5966(9) 0.6250(10) 0.050(2) Uani 1 1 d . . .
H5 H 0.3628 0.6560 0.5772 0.061 Uiso 1 1 calc R . .
C6 C 0.4376(8) 0.6543(9) 0.7735(10) 0.0469(19) Uani 1 1 d . . .
C7 C 0.4660(10) 0.5653(11) 0.8404(12) 0.066(3) Uani 1 1 d . . .
H7 H 0.5024 0.6034 0.9444 0.079 Uiso 1 1 calc R . .
C8 C 0.4415(10) 0.4197(9) 0.7561(11) 0.054(2) Uani 1 1 d . . .
H8 H 0.4629 0.3608 0.8044 0.064 Uiso 1 1 calc R . .
C9 C 0.4736(11) 0.8138(9) 0.8646(10) 0.060(2) Uani 1 1 d . . .
H9A H 0.5641 0.8601 0.8596 0.072 Uiso 1 1 calc R . .
H9B H 0.4915 0.8352 0.9684 0.072 Uiso 1 1 calc R . .
C10 C 0.3430(11) 0.8729(9) 0.8055(9) 0.055(2) Uani 1 1 d . . .
C11 C -0.0226(9) 0.3844(8) 0.5901(8) 0.0380(16) Uani 1 1 d . . .
H11 H 0.0416 0.3924 0.5399 0.046 Uiso 1 1 calc R . .
C12 C -0.0264(9) 0.5077(8) 0.7060(8) 0.0376(17) Uani 1 1 d . . .
H12 H 0.0347 0.5977 0.7339 0.045 Uiso 1 1 calc R . .
C13 C -0.1213(8) 0.4940(8) 0.7781(8) 0.0355(16) Uani 1 1 d . . .
C14 C -0.2058(9) 0.3575(7) 0.7335(8) 0.0377(17) Uani 1 1 d . . .
H14 H -0.2709 0.3429 0.7806 0.045 Uiso 1 1 calc R . .
C15 C -0.1928(9) 0.2431(8) 0.6184(9) 0.0428(18) Uani 1 1 d . . .
H15 H -0.2493 0.1505 0.5890 0.051 Uiso 1 1 calc R . .
C16 C -0.1264(8) 0.6141(8) 0.9011(8) 0.0370(16) Uani 1 1 d . . .
C17 C -0.1002(11) 0.7550(8) 0.9134(10) 0.054(2) Uani 1 1 d . . .
H17 H -0.0767 0.7733 0.8401 0.065 Uiso 1 1 calc R . .
C18 C -0.1090(11) 0.8638(8) 1.0318(10) 0.058(2) Uani 1 1 d . . .
H18 H -0.0994 0.9549 1.0327 0.069 Uiso 1 1 calc R . .
C19 C -0.1576(9) 0.7202(8) 1.1365(8) 0.0415(18) Uani 1 1 d . . .
H19 H -0.1767 0.7072 1.2142 0.050 Uiso 1 1 calc R . .
C20 C -0.1595(8) 0.6033(7) 1.0193(8) 0.0367(16) Uani 1 1 d . . .
H20 H -0.1835 0.5123 1.0168 0.044 Uiso 1 1 calc R . .
N1 N -0.1066(7) 0.2591(6) 0.5510(7) 0.0384(14) Uani 1 1 d . . .
N2 N -0.1303(7) 0.8512(6) 1.1472(7) 0.0393(15) Uani 1 1 d . . .
O1 O 0.1436(7) 0.0780(6) 0.5254(7) 0.0587(16) Uani 1 1 d . . .
O2 O 0.1114(7) 0.1486(6) 0.3531(6) 0.0535(15) Uani 1 1 d . . .
O3 O 0.2265(8) 0.8420(7) 0.8183(8) 0.0629(17) Uani 1 1 d . . .
O4 O 0.3677(7) 0.9522(7) 0.7460(8) 0.0627(17) Uani 1 1 d . . .
O5 O 0.3415(15) 0.8589(15) 0.1541(19) 0.183(6) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cd1 N2 2.308(5) 1_544 ?
Cd1 O1 2.313(5) 2_556 ?
Cd1 O2 2.321(6) . ?
Cd1 O4 2.361(7) 2_566 ?
Cd1 N1 2.379(6) . ?
Cd1 O3 2.476(7) 2_566 ?
Cd1 C10 2.729(10) 2_566 ?
C1 O2 1.228(10) . ?
C1 O1 1.262(9) . ?
C1 C2 1.520(12) . ?
C2 C3 1.513(13) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.364(12) . ?
C3 C8 1.405(13) . ?
C4 C5 1.417(11) . ?
C4 H4 0.9500 . ?
C5 C6 1.355(12) . ?
C5 H5 0.9500 . ?
C6 C7 1.383(12) . ?
C6 C9 1.520(11) . ?
C7 C8 1.398(13) . ?
C7 H7 0.9500 . ?
C8 H8 0.9500 . ?
C9 C10 1.560(13) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 O3 1.213(11) . ?
C10 O4 1.266(10) . ?
C10 Cd1 2.729(10) 2_566 ?
C11 N1 1.317(9) . ?
C11 C12 1.419(10) . ?
C11 H11 0.9500 . ?
C12 C13 1.393(10) . ?
C12 H12 0.9500 . ?
C13 C14 1.402(10) . ?
C13 C16 1.446(11) . ?
C14 C15 1.399(10) . ?
C14 H14 0.9500 . ?
C15 N1 1.290(9) . ?
C15 H15 0.9500 . ?
C16 C20 1.422(10) . ?
C16 C17 1.428(10) . ?
C17 C18 1.372(11) . ?
C17 H17 0.9500 . ?
C18 N2 1.349(10) . ?
C18 H18 0.9500 . ?
C19 N2 1.332(9) . ?
C19 C20 1.368(10) . ?
C19 H19 0.9500 . ?
C20 H20 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
N2 Cd1 O1 91.3(2) 1_544 2_556 ?
N2 Cd1 O2 87.8(2) 1_544 . ?
O1 Cd1 O2 122.5(2) 2_556 . ?
N2 Cd1 O4 94.9(2) 1_544 2_566 ?
O1 Cd1 O4 96.2(2) 2_556 2_566 ?
O2 Cd1 O4 141.1(2) . 2_566 ?
N2 Cd1 N1 179.1(2) 1_544 . ?
O1 Cd1 N1 88.7(2) 2_556 . ?
O2 Cd1 N1 93.0(2) . . ?
O4 Cd1 N1 84.2(2) 2_566 . ?
N2 Cd1 O3 90.1(2) 1_544 2_566 ?
O1 Cd1 O3 150.0(2) 2_556 2_566 ?
O2 Cd1 O3 87.5(2) . 2_566 ?
O4 Cd1 O3 53.8(2) 2_566 2_566 ?
N1 Cd1 O3 89.5(2) . 2_566 ?
N2 Cd1 O1 98.6(2) 1_544 . ?
O1 Cd1 O1 71.5(2) 2_556 . ?
O2 Cd1 O1 51.99(19) . . ?
O4 Cd1 O1 161.8(2) 2_566 . ?
N1 Cd1 O1 82.2(2) . . ?
O3 Cd1 O1 137.8(2) 2_566 . ?
N2 Cd1 C10 95.3(2) 1_544 2_566 ?
O1 Cd1 C10 123.8(3) 2_556 2_566 ?
O2 Cd1 C10 113.5(3) . 2_566 ?
O4 Cd1 C10 27.6(2) 2_566 2_566 ?
N1 Cd1 C10 84.0(2) . 2_566 ?
O3 Cd1 C10 26.4(2) 2_566 2_566 ?
O1 Cd1 C10 159.1(2) . 2_566 ?
O2 C1 O1 122.0(8) . . ?
O2 C1 C2 118.5(7) . . ?
O1 C1 C2 119.5(9) . . ?
C3 C2 C1 107.4(7) . . ?
C3 C2 H2A 110.2 . . ?
C1 C2 H2A 110.2 . . ?
C3 C2 H2B 110.2 . . ?
C1 C2 H2B 110.2 . . ?
H2A C2 H2B 108.5 . . ?
C4 C3 C8 115.9(8) . . ?
C4 C3 C2 122.5(9) . . ?
C8 C3 C2 121.6(8) . . ?
C3 C4 C5 122.4(8) . . ?
C3 C4 H4 118.8 . . ?
C5 C4 H4 118.8 . . ?
C6 C5 C4 120.9(8) . . ?
C6 C5 H5 119.6 . . ?
C4 C5 H5 119.6 . . ?
C5 C6 C7 118.4(8) . . ?
C5 C6 C9 120.8(8) . . ?
C7 C6 C9 120.7(9) . . ?
C6 C7 C8 120.5(9) . . ?
C6 C7 H7 119.8 . . ?
C8 C7 H7 119.8 . . ?
C7 C8 C3 121.9(8) . . ?
C7 C8 H8 119.0 . . ?
C3 C8 H8 119.0 . . ?
C6 C9 C10 109.9(7) . . ?
C6 C9 H9A 109.7 . . ?
C10 C9 H9A 109.7 . . ?
C6 C9 H9B 109.7 . . ?
C10 C9 H9B 109.7 . . ?
H9A C9 H9B 108.2 . . ?
O3 C10 O4 124.0(9) . . ?
O3 C10 C9 119.9(8) . . ?
O4 C10 C9 116.1(9) . . ?
O3 C10 Cd1 65.1(5) . 2_566 ?
O4 C10 Cd1 59.8(5) . 2_566 ?
C9 C10 Cd1 169.5(6) . 2_566 ?
N1 C11 C12 121.0(7) . . ?
N1 C11 H11 119.5 . . ?
C12 C11 H11 119.5 . . ?
C13 C12 C11 118.8(7) . . ?
C13 C12 H12 120.6 . . ?
C11 C12 H12 120.6 . . ?
C12 C13 C14 117.6(7) . . ?
C12 C13 C16 121.7(7) . . ?
C14 C13 C16 120.6(7) . . ?
C15 C14 C13 118.9(7) . . ?
C15 C14 H14 120.5 . . ?
C13 C14 H14 120.5 . . ?
N1 C15 C14 122.2(7) . . ?
N1 C15 H15 118.9 . . ?
C14 C15 H15 118.9 . . ?
C20 C16 C17 113.8(6) . . ?
C20 C16 C13 123.7(6) . . ?
C17 C16 C13 122.5(6) . . ?
C18 C17 C16 119.6(7) . . ?
C18 C17 H17 120.2 . . ?
C16 C17 H17 120.2 . . ?
N2 C18 C17 124.9(7) . . ?
N2 C18 H18 117.6 . . ?
C17 C18 H18 117.6 . . ?
N2 C19 C20 123.4(7) . . ?
N2 C19 H19 118.3 . . ?
C20 C19 H19 118.3 . . ?
C19 C20 C16 121.9(6) . . ?
C19 C20 H20 119.1 . . ?
C16 C20 H20 119.1 . . ?
C15 N1 C11 121.5(6) . . ?
C15 N1 Cd1 116.3(5) . . ?
C11 N1 Cd1 122.2(5) . . ?
C19 N2 C18 116.2(6) . . ?
C19 N2 Cd1 124.5(5) . 1_566 ?
C18 N2 Cd1 119.3(5) . 1_566 ?
C1 O1 Cd1 162.9(6) . 2_556 ?
C1 O1 Cd1 85.7(5) . . ?
Cd1 O1 Cd1 108.5(2) 2_556 . ?
C1 O2 Cd1 100.3(5) . . ?
C10 O3 Cd1 88.5(6) . 2_566 ?
C10 O4 Cd1 92.6(6) . 2_566 ?

_diffrn_measured_fraction_theta_max 27.4632
_diffrn_reflns_theta_full        27.47
_diffrn_measured_fraction_theta_full 95.2000
_refine_diff_density_max         1.054
_refine_diff_density_min         -1.106
_refine_diff_density_rms         0.163


