# Electronic Supplementary Material (ESI) for CrystEngComm
# This journal is © The Royal Society of Chemistry 2013


#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
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# 
#  This CIF contains data from an original supplementary publication 
#  deposited with the CCDC, and may include chemical, crystal,   
#  experimental, refinement, atomic coordinates, 
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted. 
# 
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#  fide research purposes only. It may contain copyright material 
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data_a1
_database_code_depnum_ccdc_archive 'CCDC 910084'
#TrackingRef '(1){ [Cd2(NDC)2(H2MDP)].(H2O)}.CIF'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C35 H30 Cd2 N4 O9'
_chemical_formula_weight         875.43
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd 0.1185 4.6533 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   p21/n
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                   15.3134(3)
_cell_length_b                   14.0411(2)
_cell_length_c                   16.3451(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.2190(10)
_cell_angle_gamma                90.00
_cell_volume                     3514.45(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?
_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.655
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1744
_exptl_absorpt_coefficient_mu    10.197
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.2349
_exptl_absorpt_correction_T_max  0.2349
_exptl_absorpt_process_details   ?
_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'superNova (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            33966
_diffrn_reflns_av_R_equivalents  0.0320
_diffrn_reflns_av_sigmaI/netI    0.0203
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.95
_diffrn_reflns_theta_max         76.52
_reflns_number_total             7338
_reflns_number_gt                6048
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.1858P)^2^+2.8022P] where P=(Fo^2^+2Fc^2^)/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     SHELXL
_refine_ls_extinction_coef       0.00068(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns         7338
_refine_ls_number_parameters     460
_refine_ls_number_restraints     794
_refine_ls_R_factor_all          0.0551
_refine_ls_R_factor_gt           0.0450
_refine_ls_wR_factor_ref         0.2457
_refine_ls_wR_factor_gt          0.2223
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_restrained_S_all      1.068
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cd1 Cd 0.20860(2) 0.13822(2) 0.02584(2) 0.0223(2) Uani 1 1 d . . .
Cd2 Cd 0.20583(2) 0.36641(2) 0.02191(2) 0.0223(2) Uani 1 1 d . . .
O8 O 0.6155(4) 0.1719(4) 0.4223(3) 0.0522(13) Uani 1 1 d . . .
O4 O 0.3004(3) 0.3482(4) 0.1256(3) 0.0494(12) Uani 1 1 d . . .
O6 O -0.1949(3) 0.3226(4) 0.4242(3) 0.0507(13) Uani 1 1 d . . .
O7 O 0.6036(3) 0.3289(4) 0.4384(3) 0.0469(11) Uani 1 1 d . . .
C32 C 0.5878(5) 0.2519(3) 0.4033(4) 0.0350(13) Uani 1 1 d U . .
O5 O -0.1812(3) 0.1642(4) 0.4407(3) 0.0472(12) Uani 1 1 d . . .
C31 C 0.5262(4) 0.2558(3) 0.3311(4) 0.0341(11) Uani 1 1 d U . .
O3 O 0.3137(3) 0.1921(4) 0.1065(3) 0.0522(12) Uani 1 1 d . . .
C30 C -0.1600(5) 0.2432(4) 0.4099(4) 0.0357(13) Uani 1 1 d U . .
C29 C 0.4033(4) 0.2649(4) 0.2042(4) 0.0378(11) Uani 1 1 d U . .
C28 C -0.0868(4) 0.2418(4) 0.3482(4) 0.0329(11) Uani 1 1 d U . .
O2 O 0.1104(3) 0.2917(4) 0.1072(3) 0.0527(12) Uani 1 1 d . . .
C27 C 0.3332(4) 0.2682(5) 0.1396(4) 0.0388(11) Uani 1 1 d U . .
C26 C 0.0362(4) 0.2313(5) 0.2221(3) 0.0372(11) Uani 1 1 d U . .
O1 O 0.1264(3) 0.1387(3) 0.1376(3) 0.0523(12) Uani 1 1 d . . .
C25 C 0.1597(5) 0.5814(4) -0.0368(5) 0.0492(14) Uani 1 1 d U . .
N2 N 0.2556(4) 0.5783(4) 0.0580(3) 0.0498(13) Uani 1 1 d . . .
H2A H 0.2874 0.5581 0.0979 0.060 Uiso 1 1 calc R . .
C24 C 0.0962(4) 0.2206(5) 0.1506(3) 0.0379(10) Uani 1 1 d U . .
C23 C 0.6208(4) 0.3726(4) 0.2573(4) 0.0410(11) Uani 1 1 d U . .
H23A H 0.6609 0.3728 0.3002 0.049 Uiso 1 1 calc R . .
C2 C 0.5420(3) 0.3184(4) 0.2642(3) 0.0339(10) Uani 1 1 d U . .
C21 C 0.1859(6) 0.9107(5) -0.0161(5) 0.0598(15) Uani 1 1 d U . .
C20 C 0.4993(4) 0.3797(5) 0.1293(4) 0.0461(12) Uani 1 1 d U . .
H20A H 0.4590 0.3838 0.0868 0.055 Uiso 1 1 calc R . .
C19 C -0.0236(3) 0.3157(4) 0.3411(3) 0.0342(10) Uani 1 1 d U . .
C18 C 0.0383(3) 0.3112(4) 0.2757(3) 0.0341(10) Uani 1 1 d U . .
C17 C 0.4808(3) 0.3228(4) 0.1996(3) 0.0357(10) Uani 1 1 d U . .
C16 C 0.4543(4) 0.1981(4) 0.3312(3) 0.0386(10) Uani 1 1 d U . .
H16A H 0.4460 0.1552 0.3739 0.046 Uiso 1 1 calc R . .
C15 C -0.0223(4) 0.1595(4) 0.2344(4) 0.0393(11) Uani 1 1 d U . .
H15A H -0.0204 0.1056 0.2013 0.047 Uiso 1 1 calc R . .
N4 N 0.2848(4) 0.9809(4) -0.0831(4) 0.0538(14) Uani 1 1 d . . .
H4A H 0.3215 1.0237 -0.0983 0.065 Uiso 1 1 calc R . .
C14 C 0.2002(5) 0.6714(4) -0.0348(5) 0.0587(14) Uani 1 1 d U . .
C13 C -0.0163(4) 0.3906(5) 0.3980(4) 0.0445(11) Uani 1 1 d U . .
H13A H -0.0543 0.3931 0.4421 0.053 Uiso 1 1 calc R . .
C12 C 0.3931(4) 0.2029(4) 0.2676(3) 0.0394(11) Uani 1 1 d U . .
H12A H 0.3446 0.1632 0.2686 0.047 Uiso 1 1 calc R . .
C11 C 0.0885(5) 0.5519(5) -0.0933(6) 0.072(2) Uani 1 1 d U . .
H11A H 0.0726 0.4870 -0.0823 0.107 Uiso 1 1 calc R . .
H11B H 0.1081 0.5573 -0.1488 0.107 Uiso 1 1 calc R . .
H11C H 0.0386 0.5923 -0.0854 0.107 Uiso 1 1 calc R . .
C10 C -0.0850(4) 0.1659(4) 0.2958(4) 0.0406(11) Uani 1 1 d U . .
H10A H -0.1263 0.1177 0.3012 0.049 Uiso 1 1 calc R . .
C9 C 0.1022(4) 0.3842(5) 0.2692(4) 0.0443(11) Uani 1 1 d U . .
H9A H 0.1422 0.3825 0.2266 0.053 Uiso 1 1 calc R . .
N1 N 0.1946(3) 0.5248(3) 0.0196(3) 0.0379(10) Uani 1 1 d . . .
C8 C 0.6375(4) 0.4235(5) 0.1888(4) 0.0524(13) Uani 1 1 d U . .
H8A H 0.6903 0.4558 0.1842 0.063 Uiso 1 1 calc R . .
C7 C 0.1810(8) 0.7493(4) -0.0976(7) 0.0696(17) Uani 1 1 d U . .
H7A H 0.2050 0.7293 -0.1497 0.083 Uiso 1 1 calc R . .
H7B H 0.1181 0.7537 -0.1043 0.083 Uiso 1 1 calc R . .
N3 N 0.2286(3) 0.9912(3) -0.0205(3) 0.0400(11) Uani 1 1 d . . .
C6 C 0.2609(5) 0.6656(5) 0.0273(5) 0.0620(15) Uani 1 1 d U . .
C5 C 0.2153(6) 0.8468(5) -0.0787(5) 0.0617(15) Uani 1 1 d U . .
C4 C 0.5768(4) 0.4285(5) 0.1247(4) 0.0525(13) Uani 1 1 d U . .
H4B H 0.5890 0.4650 0.0788 0.063 Uiso 1 1 calc R . .
C3 C 0.2761(6) 0.8942(5) -0.1191(5) 0.0639(16) Uani 1 1 d U . .
C22 C 0.1056(4) 0.4568(5) 0.3245(4) 0.0528(13) Uani 1 1 d U . .
H22A H 0.1475 0.5042 0.3193 0.063 Uiso 1 1 calc R . .
C1 C 0.0458(4) 0.4598(5) 0.3894(4) 0.0533(13) Uani 1 1 d U . .
H1A H 0.0484 0.5095 0.4269 0.064 Uiso 1 1 calc R . .
O1W O 0.3125(5) 0.5274(5) 0.2170(4) 0.0835(18) Uani 1 1 d D . .
C35 C 0.1154(7) 0.8978(7) 0.0450(7) 0.092(3) Uani 1 1 d U . .
H35A H 0.1108 0.9540 0.0781 0.137 Uiso 1 1 calc R . .
H35B H 0.1287 0.8441 0.0791 0.137 Uiso 1 1 calc R . .
H35C H 0.0609 0.8869 0.0171 0.137 Uiso 1 1 calc R . .
C33 C 0.3251(8) 0.7353(6) 0.0604(8) 0.088(3) Uani 1 1 d U . .
H33A H 0.3569 0.7067 0.1048 0.132 Uiso 1 1 calc R . .
H33B H 0.2948 0.7906 0.0799 0.132 Uiso 1 1 calc R . .
H33C H 0.3650 0.7534 0.0181 0.132 Uiso 1 1 calc R . .
C34 C 0.3315(8) 0.8688(7) -0.1914(7) 0.096(3) Uani 1 1 d U . .
H34A H 0.3173 0.8056 -0.2095 0.143 Uiso 1 1 calc R . .
H34B H 0.3921 0.8714 -0.1760 0.143 Uiso 1 1 calc R . .
H34C H 0.3207 0.9132 -0.2350 0.143 Uiso 1 1 calc R . .
H1WB H 0.333(7) 0.473(4) 0.203(7) 0.13(5) Uiso 1 1 d D . .
H1WA H 0.346(7) 0.553(9) 0.252(6) 0.14(5) Uiso 1 1 d D . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cd1 0.0233(3) 0.0254(3) 0.0181(3) -0.00101(10) 0.00115(18) 0.00180(10)
Cd2 0.0240(3) 0.0237(3) 0.0192(3) 0.00112(10) -0.00048(18) -0.00048(10)
O8 0.072(3) 0.043(3) 0.042(2) 0.000(2) -0.035(2) 0.012(2)
O4 0.044(2) 0.064(3) 0.040(2) 0.002(2) -0.0180(19) 0.013(2)
O6 0.053(3) 0.051(3) 0.049(3) 0.005(2) 0.025(2) 0.031(2)
O7 0.055(3) 0.045(3) 0.041(2) -0.013(2) -0.025(2) 0.005(2)
C32 0.035(3) 0.040(3) 0.030(3) -0.0040(17) -0.007(2) 0.0056(17)
O5 0.049(3) 0.047(3) 0.045(3) 0.003(2) 0.032(2) -0.005(2)
C31 0.034(2) 0.037(2) 0.031(2) -0.0061(16) -0.010(2) 0.0072(16)
O3 0.051(3) 0.060(3) 0.045(3) -0.008(2) -0.021(2) -0.002(2)
C30 0.036(3) 0.042(3) 0.030(3) 0.0008(18) 0.012(2) 0.0063(18)
C29 0.038(2) 0.043(2) 0.032(2) -0.0026(19) -0.007(2) 0.005(2)
C28 0.034(2) 0.037(2) 0.028(2) 0.0013(16) 0.010(2) 0.0068(17)
O2 0.047(2) 0.078(3) 0.033(2) 0.015(2) 0.0121(18) -0.009(2)
C27 0.036(2) 0.050(3) 0.030(2) 0.000(2) -0.008(2) 0.000(2)
C26 0.038(2) 0.046(2) 0.028(2) -0.0006(19) 0.008(2) 0.005(2)
O1 0.057(3) 0.067(3) 0.034(2) -0.0058(19) 0.015(2) 0.013(2)
C25 0.064(3) 0.022(2) 0.061(3) -0.003(2) -0.023(3) -0.003(2)
N2 0.071(4) 0.033(3) 0.045(3) -0.007(2) -0.025(3) -0.002(2)
C24 0.036(2) 0.052(3) 0.025(2) -0.002(2) 0.0028(19) 0.000(2)
C23 0.041(2) 0.039(2) 0.043(2) -0.0050(19) -0.007(2) 0.0026(19)
C2 0.035(2) 0.033(2) 0.033(2) -0.0068(18) -0.0078(17) 0.0059(18)
C21 0.077(3) 0.030(3) 0.072(3) 0.003(3) -0.006(3) -0.009(3)
C20 0.047(2) 0.051(2) 0.040(2) 0.002(2) -0.006(2) 0.003(2)
C19 0.036(2) 0.037(2) 0.029(2) -0.0022(18) 0.0049(17) 0.0070(18)
C18 0.034(2) 0.039(2) 0.029(2) 0.0015(18) 0.0037(17) 0.0037(18)
C17 0.036(2) 0.037(2) 0.034(2) -0.0026(18) -0.0044(18) 0.0040(18)
C16 0.041(2) 0.043(2) 0.031(2) -0.0012(19) -0.0080(19) -0.001(2)
C15 0.041(2) 0.042(2) 0.035(2) -0.005(2) 0.0096(19) 0.001(2)
N4 0.067(3) 0.031(2) 0.064(3) -0.012(2) 0.030(3) 0.003(2)
C14 0.083(3) 0.024(2) 0.069(3) -0.007(2) -0.025(3) -0.007(2)
C13 0.046(2) 0.049(2) 0.039(2) -0.011(2) 0.005(2) 0.004(2)
C12 0.038(2) 0.045(2) 0.035(2) -0.002(2) -0.0103(19) -0.002(2)
C11 0.080(4) 0.038(3) 0.096(5) 0.006(3) -0.053(4) 0.001(3)
C10 0.041(2) 0.041(2) 0.040(2) -0.002(2) 0.009(2) 0.001(2)
C9 0.045(2) 0.048(2) 0.039(2) -0.001(2) 0.004(2) -0.004(2)
N1 0.044(2) 0.029(2) 0.041(2) -0.0006(19) -0.0122(19) 0.0023(19)
C8 0.048(3) 0.050(3) 0.059(3) -0.001(3) -0.005(2) -0.004(2)
C7 0.095(4) 0.035(3) 0.078(4) 0.000(2) -0.025(3) -0.010(2)
N3 0.055(3) 0.026(2) 0.039(2) -0.0015(19) 0.011(2) -0.001(2)
C6 0.080(3) 0.035(3) 0.071(3) -0.004(3) -0.030(3) -0.008(3)
C5 0.087(4) 0.027(2) 0.071(3) 0.000(3) -0.020(3) -0.005(3)
C4 0.055(3) 0.054(3) 0.049(3) 0.007(2) 0.003(2) -0.004(2)
C3 0.086(4) 0.032(3) 0.074(4) -0.014(3) -0.004(3) 0.006(3)
C22 0.054(3) 0.051(3) 0.053(3) -0.002(2) 0.002(2) -0.012(2)
C1 0.057(3) 0.051(3) 0.053(3) -0.015(2) 0.002(2) -0.003(2)
O1W 0.119(5) 0.071(4) 0.061(4) -0.004(3) -0.027(4) 0.010(4)
C35 0.106(6) 0.069(5) 0.099(6) 0.011(5) 0.011(5) -0.039(5)
C33 0.110(6) 0.057(4) 0.097(6) -0.006(4) -0.046(5) -0.028(4)
C34 0.127(7) 0.075(5) 0.085(6) -0.037(4) 0.016(5) 0.020(5)
_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 O7 2.197(4) 4_565 ?
Cd1 O3 2.210(4) . ?
Cd1 O1 2.222(4) . ?
Cd1 N3 2.221(4) 1_545 ?
Cd1 O6 2.295(4) 4_665 ?
Cd1 Cd2 3.2050(5) . ?
Cd2 O8 2.199(4) 4_565 ?
Cd2 O5 2.227(4) 4_665 ?
Cd2 N1 2.231(5) . ?
Cd2 O4 2.240(4) . ?
Cd2 O2 2.280(4) . ?
O8 C32 1.240(7) . ?
O8 Cd2 2.199(4) 4_666 ?
O4 C27 1.251(8) . ?
O6 C30 1.258(7) . ?
O6 Cd1 2.295(4) 4_566 ?
O7 C32 1.247(7) . ?
O7 Cd1 2.197(4) 4_666 ?
C32 C31 1.509(9) . ?
O5 C30 1.261(7) . ?
O5 Cd2 2.227(4) 4_566 ?
C31 C16 1.367(9) . ?
C31 C2 1.424(8) . ?
O3 C27 1.233(8) . ?
C30 C28 1.511(8) . ?
C29 C12 1.363(9) . ?
C29 C17 1.439(9) . ?
C29 C27 1.505(9) . ?
C28 C10 1.368(8) . ?
C28 C19 1.424(8) . ?
O2 C24 1.244(9) . ?
C26 C15 1.365(9) . ?
C26 C18 1.422(8) . ?
C26 C24 1.497(7) . ?
O1 C24 1.258(8) . ?
C25 N1 1.328(8) . ?
C25 C14 1.408(9) . ?
C25 C11 1.485(9) . ?
N2 C6 1.328(9) . ?
N2 N1 1.352(7) . ?
C23 C8 1.355(9) . ?
C23 C2 1.431(8) . ?
C2 C17 1.411(7) . ?
C21 N3 1.308(8) . ?
C21 C5 1.434(12) . ?
C21 C35 1.484(13) . ?
C20 C4 1.371(9) . ?
C20 C17 1.430(8) . ?
C19 C13 1.408(8) . ?
C19 C18 1.433(7) . ?
C18 C9 1.422(8) . ?
C16 C12 1.398(7) . ?
C15 C10 1.394(8) . ?
N4 N3 1.347(6) . ?
N4 C3 1.357(8) . ?
C14 C6 1.375(10) . ?
C14 C7 1.528(11) . ?
C13 C1 1.366(9) . ?
C9 C22 1.363(9) . ?
C8 C4 1.399(9) . ?
C7 C5 1.498(9) . ?
N3 Cd1 2.221(4) 1_565 ?
C6 C33 1.487(10) . ?
C5 C3 1.324(12) . ?
C3 C34 1.502(13) . ?
C22 C1 1.404(9) . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O7 Cd1 O3 147.8(2) 4_565 . ?
O7 Cd1 O1 96.8(2) 4_565 . ?
O3 Cd1 O1 85.53(19) . . ?
O7 Cd1 N3 94.29(19) 4_565 1_545 ?
O3 Cd1 N3 114.89(19) . 1_545 ?
O1 Cd1 N3 111.25(17) . 1_545 ?
O7 Cd1 O6 87.1(2) 4_565 4_665 ?
O3 Cd1 O6 83.15(18) . 4_665 ?
O1 Cd1 O6 164.32(18) . 4_665 ?
N3 Cd1 O6 83.44(17) 1_545 4_665 ?
O7 Cd1 Cd2 76.54(13) 4_565 . ?
O3 Cd1 Cd2 71.30(14) . . ?
O1 Cd1 Cd2 90.34(13) . . ?
N3 Cd1 Cd2 157.58(12) 1_545 . ?
O6 Cd1 Cd2 75.79(13) 4_665 . ?
O8 Cd2 O5 90.0(2) 4_565 4_665 ?
O8 Cd2 N1 100.55(18) 4_565 . ?
O5 Cd2 N1 104.06(18) 4_665 . ?
O8 Cd2 O4 159.3(2) 4_565 . ?
O5 Cd2 O4 85.83(19) 4_665 . ?
N1 Cd2 O4 100.13(17) . . ?
O8 Cd2 O2 86.41(19) 4_565 . ?
O5 Cd2 O2 141.00(19) 4_665 . ?
N1 Cd2 O2 114.8(2) . . ?
O4 Cd2 O2 84.21(18) . . ?
O8 Cd2 Cd1 77.21(13) 4_565 . ?
O5 Cd2 Cd1 78.96(13) 4_665 . ?
N1 Cd2 Cd1 176.32(12) . . ?
O4 Cd2 Cd1 82.10(13) . . ?
O2 Cd2 Cd1 62.36(15) . . ?
C32 O8 Cd2 128.4(4) . 4_666 ?
C27 O4 Cd2 119.9(4) . . ?
C30 O6 Cd1 128.4(4) . 4_566 ?
C32 O7 Cd1 128.5(4) . 4_666 ?
O8 C32 O7 127.2(7) . . ?
O8 C32 C31 116.2(5) . . ?
O7 C32 C31 116.6(5) . . ?
C30 O5 Cd2 127.6(4) . 4_566 ?
C16 C31 C2 120.5(6) . . ?
C16 C31 C32 118.5(6) . . ?
C2 C31 C32 121.0(6) . . ?
C27 O3 Cd1 137.1(5) . . ?
O6 C30 O5 126.5(6) . . ?
O6 C30 C28 116.9(5) . . ?
O5 C30 C28 116.6(5) . . ?
C12 C29 C17 119.8(6) . . ?
C12 C29 C27 118.0(6) . . ?
C17 C29 C27 122.1(6) . . ?
C10 C28 C19 120.1(5) . . ?
C10 C28 C30 116.4(5) . . ?
C19 C28 C30 123.4(5) . . ?
C24 O2 Cd2 146.3(4) . . ?
O3 C27 O4 127.0(6) . . ?
O3 C27 C29 116.9(6) . . ?
O4 C27 C29 116.1(6) . . ?
C15 C26 C18 120.4(5) . . ?
C15 C26 C24 116.5(6) . . ?
C18 C26 C24 123.1(6) . . ?
C24 O1 Cd1 110.6(4) . . ?
N1 C25 C14 110.1(6) . . ?
N1 C25 C11 123.9(6) . . ?
C14 C25 C11 125.9(6) . . ?
C6 N2 N1 112.4(5) . . ?
O2 C24 O1 124.8(6) . . ?
O2 C24 C26 118.3(6) . . ?
O1 C24 C26 116.8(6) . . ?
C8 C23 C2 120.5(6) . . ?
C23 C2 C31 122.3(5) . . ?
C23 C2 C17 118.5(5) . . ?
C31 C2 C17 119.1(5) . . ?
N3 C21 C5 110.1(7) . . ?
N3 C21 C35 120.5(7) . . ?
C5 C21 C35 129.3(7) . . ?
C4 C20 C17 119.8(6) . . ?
C13 C19 C28 122.9(5) . . ?
C13 C19 C18 118.3(5) . . ?
C28 C19 C18 118.7(5) . . ?
C9 C18 C26 122.5(5) . . ?
C9 C18 C19 118.7(5) . . ?
C26 C18 C19 118.7(5) . . ?
C2 C17 C20 119.5(5) . . ?
C2 C17 C29 118.8(5) . . ?
C20 C17 C29 121.6(5) . . ?
C31 C16 C12 120.4(6) . . ?
C26 C15 C10 120.8(6) . . ?
N3 N4 C3 111.3(6) . . ?
C6 C14 C25 105.2(6) . . ?
C6 C14 C7 131.7(7) . . ?
C25 C14 C7 122.9(7) . . ?
C1 C13 C19 121.1(6) . . ?
C29 C12 C16 121.2(6) . . ?
C28 C10 C15 121.1(6) . . ?
C22 C9 C18 121.0(6) . . ?
C25 N1 N2 105.4(5) . . ?
C25 N1 Cd2 129.7(4) . . ?
N2 N1 Cd2 119.6(4) . . ?
C23 C8 C4 121.2(6) . . ?
C5 C7 C14 116.7(8) . . ?
C21 N3 N4 105.7(6) . . ?
C21 N3 Cd1 135.6(5) . 1_565 ?
N4 N3 Cd1 116.6(4) . 1_565 ?
N2 C6 C14 106.9(6) . . ?
N2 C6 C33 120.7(7) . . ?
C14 C6 C33 132.4(7) . . ?
C3 C5 C21 105.3(6) . . ?
C3 C5 C7 127.1(9) . . ?
C21 C5 C7 127.5(9) . . ?
C20 C4 C8 120.4(6) . . ?
C5 C3 N4 107.6(7) . . ?
C5 C3 C34 132.4(7) . . ?
N4 C3 C34 119.9(8) . . ?
C9 C22 C1 120.0(6) . . ?
C13 C1 C22 120.8(6) . . ?
_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        76.52
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         0.904
_refine_diff_density_min         -1.139
_refine_diff_density_rms         0.120


data_a2
_database_code_depnum_ccdc_archive 'CCDC 910085'
#TrackingRef '(2) [Cd(NDC)(H2MDP)].CIF'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C23 H21 Cd N4 O4'
_chemical_formula_weight         529.84
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd 0.1185 4.6533 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   c2/c
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
_cell_length_a                   20.3025(12)
_cell_length_b                   14.0277(3)
_cell_length_c                   19.7191(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 120.074(5)
_cell_angle_gamma                90.00
_cell_volume                     4859.9(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?
_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.17
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.448
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2136
_exptl_absorpt_coefficient_mu    7.488
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3159
_exptl_absorpt_correction_T_max  0.3625
_exptl_absorpt_process_details   ?
_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'superNova (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            9414
_diffrn_reflns_av_R_equivalents  0.0457
_diffrn_reflns_av_sigmaI/netI    0.0413
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         4.03
_diffrn_reflns_theta_max         74.40
_reflns_number_total             4821
_reflns_number_gt                3902
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.1807P)^2^+4.0000P] where P=(Fo^2^+2Fc^2^)/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     SHELXL
_refine_ls_extinction_coef       0.00041(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns         4821
_refine_ls_number_parameters     363
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.0924
_refine_ls_R_factor_gt           0.0823
_refine_ls_wR_factor_ref         0.2654
_refine_ls_wR_factor_gt          0.2423
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_restrained_S_all      1.092
_refine_ls_shift/su_max          0.028
_refine_ls_shift/su_mean         0.005
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 0.54464(3) 0.24095(4) 0.04551(2) 0.0731(3) Uani 1 1 d . . .
N4 N 0.9086(4) -0.0445(5) 0.3903(4) 0.0798(16) Uani 1 1 d . A .
H4A H 0.9523 -0.0382 0.3936 0.096 Uiso 1 1 calc R . .
N2 N 0.6138(3) 0.0481(5) 0.1277(3) 0.0751(15) Uani 1 1 d . . .
H2A H 0.5933 0.0248 0.0812 0.090 Uiso 1 1 calc R A .
O1A O 0.5690(13) 0.2310(16) -0.0525(12) 0.085(5) Uani 0.47(3) 1 d PU A 1
O3A O 0.4286(14) 0.223(2) -0.0017(16) 0.120(8) Uani 0.47(3) 1 d P A 1
O4A O 0.4713(8) 0.3359(12) 0.0853(8) 0.090(5) Uani 0.47(3) 1 d PU A 1
O1B O 0.5340(14) 0.2478(13) -0.0700(11) 0.090(5) Uani 0.53(3) 1 d P A 2
O3B O 0.4189(8) 0.1629(19) -0.0076(10) 0.104(6) Uani 0.53(3) 1 d P A 2
O4B O 0.4312(13) 0.2868(16) 0.0591(17) 0.111(10) Uani 0.53(3) 1 d P A 2
N1 N 0.6114(3) 0.1401(4) 0.1431(3) 0.0687(13) Uani 1 1 d . A .
C1 C 0.6571(6) 0.2412(5) 0.2600(5) 0.083(2) Uani 1 1 d . . .
H1A H 0.6333 0.2897 0.2207 0.124 Uiso 1 1 calc R . .
H1B H 0.7101 0.2562 0.2931 0.124 Uiso 1 1 calc R . .
H1C H 0.6329 0.2384 0.2911 0.124 Uiso 1 1 calc R . .
C16 C 0.5133(3) 0.0572(4) -0.2083(3) 0.0562(12) Uani 1 1 d . . .
C15 C 0.5112(6) 0.2294(6) -0.2102(5) 0.084(2) Uani 1 1 d . . .
H15A H 0.5179 0.2872 -0.1845 0.100 Uiso 1 1 calc R . .
C3 C 0.6760(3) 0.0583(5) 0.2554(3) 0.0625(14) Uani 1 1 d . . .
C14 C 0.5231(3) 0.1470(5) -0.1698(3) 0.0665(15) Uani 1 1 d . A .
O2 O 0.5444(4) 0.0912(5) -0.0441(3) 0.1031(18) Uani 1 1 d U A .
C8 C 0.7949(4) -0.0141(5) 0.3664(3) 0.0662(14) Uani 1 1 d . . .
C17 C 0.5273(3) -0.0310(5) -0.1702(3) 0.0655(15) Uani 1 1 d . . .
H17A H 0.5460 -0.0320 -0.1165 0.079 Uiso 1 1 calc R . .
C2 C 0.6495(3) 0.1474(5) 0.2216(3) 0.0635(14) Uani 1 1 d . A .
N3 N 0.8859(4) -0.1234(5) 0.4118(4) 0.0880(18) Uani 1 1 d . . .
C7 C 0.8546(4) 0.0230(5) 0.3629(3) 0.0692(15) Uani 1 1 d . A .
C6 C 0.8658(5) 0.1190(6) 0.3368(6) 0.099(3) Uani 1 1 d . . .
H6A H 0.9159 0.1225 0.3433 0.148 Uiso 1 1 calc R A .
H6B H 0.8603 0.1676 0.3678 0.148 Uiso 1 1 calc R . .
H6C H 0.8285 0.1283 0.2826 0.148 Uiso 1 1 calc R . .
C4 C 0.6520(3) -0.0039(5) 0.1935(4) 0.0732(16) Uani 1 1 d . A .
C18 C 0.5144(4) -0.1158(5) -0.2092(4) 0.0688(15) Uani 1 1 d . . .
H18A H 0.5246 -0.1731 -0.1820 0.083 Uiso 1 1 calc R . .
C13 C 0.5431(4) 0.1569(6) -0.0844(4) 0.0754(19) Uani 1 1 d . . .
C9 C 0.8159(5) -0.1049(6) 0.3968(4) 0.0816(19) Uani 1 1 d . A .
C5 C 0.7181(4) 0.0340(6) 0.3400(4) 0.0790(18) Uani 1 1 d . A .
H5A H 0.6869 -0.0082 0.3513 0.095 Uiso 1 1 calc R . .
H5B H 0.7266 0.0918 0.3703 0.095 Uiso 1 1 calc R . .
C11 C 0.6608(5) -0.1077(7) 0.1908(6) 0.105(3) Uani 1 1 d . . .
H11A H 0.6368 -0.1283 0.1372 0.157 Uiso 1 1 calc R A .
H11B H 0.6375 -0.1392 0.2166 0.157 Uiso 1 1 calc R . .
H11C H 0.7140 -0.1234 0.2167 0.157 Uiso 1 1 calc R . .
C10 C 0.7737(8) -0.1795(8) 0.4118(8) 0.137(4) Uani 1 1 d . . .
H10A H 0.8052 -0.2351 0.4328 0.205 Uiso 1 1 calc R A .
H10B H 0.7285 -0.1958 0.3637 0.205 Uiso 1 1 calc R . .
H10C H 0.7599 -0.1563 0.4489 0.205 Uiso 1 1 calc R . .
C20 C 0.4225(13) 0.289(2) 0.0414(16) 0.067(8) Uani 0.50 1 d P A .
C33 C 0.1952(4) 0.2887(6) -0.0003(4) 0.0730(17) Uani 1 1 d . . .
C32 C 0.2327(7) 0.3728(11) 0.0268(6) 0.067(3) Uani 0.50 1 d P . .
C30 C 0.3411(7) 0.2882(12) 0.0270(7) 0.067(3) Uani 0.50 1 d P . .
C31 C 0.3110(6) 0.3743(10) 0.0430(6) 0.064(3) Uani 0.50 1 d P A .
C41 C 0.3519(10) 0.4599(13) 0.0691(12) 0.095(5) Uani 0.50 1 d P . .
H41A H 0.4012 0.4624 0.0775 0.114 Uiso 0.50 1 calc PR A .
C44 C 0.2048(10) 0.4608(15) 0.0371(11) 0.097(5) Uani 0.50 1 d P A .
H44A H 0.1536 0.4648 0.0222 0.117 Uiso 0.50 1 calc PR . .
C42 C 0.3220(13) 0.5385(15) 0.0822(19) 0.139(9) Uani 0.50 1 d P A .
H42A H 0.3515 0.5932 0.1018 0.166 Uiso 0.50 1 calc PR . .
C43 C 0.2478(10) 0.5379(16) 0.0668(18) 0.142(11) Uani 0.50 1 d P . .
H43A H 0.2278 0.5919 0.0772 0.171 Uiso 0.50 1 calc PR A .
C56 C 0.3906(9) 0.2238(16) 0.0163(8) 0.073(4) Uani 0.50 1 d P . .
C55 C 0.2796(10) 0.2911(13) 0.0144(10) 0.080(4) Uani 0.50 1 d P . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cd1 0.0936(5) 0.0794(4) 0.0413(4) -0.00289(15) 0.0301(3) -0.0136(2)
N4 0.077(3) 0.090(4) 0.073(3) 0.013(3) 0.038(3) 0.012(3)
N2 0.067(3) 0.095(4) 0.048(3) -0.018(3) 0.017(2) 0.002(3)
O1A 0.109(9) 0.097(8) 0.058(7) -0.018(6) 0.049(7) -0.015(7)
O3A 0.096(13) 0.16(2) 0.120(15) -0.035(15) 0.063(12) 0.019(14)
O4A 0.070(7) 0.096(9) 0.102(8) -0.002(6) 0.041(6) -0.008(6)
O1B 0.116(13) 0.108(11) 0.054(9) -0.011(6) 0.049(9) -0.003(8)
O3B 0.058(5) 0.173(18) 0.088(7) -0.026(11) 0.042(5) 0.001(9)
O4B 0.113(16) 0.104(13) 0.15(2) -0.001(13) 0.094(16) -0.038(11)
N1 0.072(3) 0.085(4) 0.046(2) -0.003(2) 0.028(2) -0.005(3)
C1 0.105(6) 0.081(5) 0.052(4) -0.007(3) 0.030(4) -0.014(4)
C16 0.053(2) 0.082(4) 0.044(3) -0.006(2) 0.031(2) -0.007(2)
C15 0.116(6) 0.081(4) 0.072(5) -0.009(4) 0.061(5) -0.006(4)
C3 0.060(3) 0.078(4) 0.052(3) 0.001(3) 0.030(2) 0.005(3)
C14 0.069(3) 0.094(4) 0.048(3) -0.007(3) 0.037(2) -0.009(3)
O2 0.151(5) 0.115(4) 0.054(2) -0.001(3) 0.060(3) 0.010(4)
C8 0.073(3) 0.079(4) 0.048(3) 0.010(3) 0.031(2) 0.010(3)
C17 0.069(3) 0.092(4) 0.046(2) 0.008(3) 0.037(2) 0.002(3)
C2 0.061(3) 0.086(4) 0.044(3) -0.007(3) 0.027(2) -0.010(3)
N3 0.113(5) 0.080(4) 0.063(3) 0.017(3) 0.039(3) 0.023(3)
C7 0.075(4) 0.069(4) 0.051(3) 0.002(3) 0.023(3) -0.001(3)
C6 0.099(6) 0.075(5) 0.115(7) 0.016(4) 0.048(5) -0.006(4)
C4 0.058(3) 0.086(4) 0.066(3) -0.010(3) 0.025(3) 0.008(3)
C18 0.086(4) 0.073(4) 0.065(3) 0.008(3) 0.051(3) 0.005(3)
C13 0.078(4) 0.105(5) 0.054(3) -0.027(4) 0.042(3) -0.024(4)
C9 0.099(5) 0.079(4) 0.072(4) 0.020(3) 0.047(4) 0.011(4)
C5 0.082(4) 0.103(5) 0.059(3) 0.013(3) 0.040(3) 0.013(4)
C11 0.091(5) 0.087(5) 0.104(6) -0.020(5) 0.024(5) 0.019(4)
C10 0.175(11) 0.108(8) 0.154(10) 0.057(8) 0.102(9) 0.012(8)
C20 0.054(10) 0.093(17) 0.057(8) 0.014(9) 0.030(7) 0.042(12)
C33 0.077(4) 0.082(4) 0.058(4) 0.010(3) 0.033(3) 0.008(4)
C32 0.062(6) 0.098(9) 0.044(5) 0.008(5) 0.029(5) 0.009(6)
C30 0.057(7) 0.102(10) 0.040(5) 0.013(6) 0.023(5) 0.011(6)
C31 0.055(5) 0.091(9) 0.048(5) 0.006(5) 0.027(5) 0.000(6)
C41 0.084(9) 0.094(11) 0.117(13) 0.001(10) 0.058(9) 0.004(8)
C44 0.085(9) 0.116(13) 0.109(12) -0.005(10) 0.062(9) 0.021(9)
C42 0.128(16) 0.076(11) 0.23(3) -0.010(15) 0.106(19) -0.004(11)
C43 0.076(10) 0.107(14) 0.23(3) -0.065(17) 0.066(14) 0.000(10)
C56 0.071(9) 0.108(12) 0.036(6) 0.011(7) 0.024(6) -0.006(9)
C55 0.079(9) 0.091(10) 0.072(8) 0.009(8) 0.038(7) -0.003(8)
_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 O1B 2.180(17) . ?
Cd1 O3A 2.07(3) . ?
Cd1 N1 2.219(5) . ?
Cd1 N3 2.265(6) 4_655 ?
Cd1 O1A 2.23(2) . ?
Cd1 O4A 2.404(12) . ?
Cd1 O3B 2.476(17) . ?
Cd1 O4B 2.53(2) . ?
Cd1 C20 2.532(18) . ?
N4 C7 1.341(9) . ?
N4 N3 1.348(9) . ?
N2 N1 1.332(9) . ?
N2 C4 1.346(9) . ?
O1A C13 1.19(2) . ?
O3A C56 1.00(3) . ?
O3A C20 1.30(4) . ?
O4A C20 1.14(4) . ?
O4A C56 2.18(3) . ?
O1B C13 1.339(19) . ?
O3B C56 1.25(3) . ?
O3B C20 2.00(4) . ?
O4B C20 0.30(5) . ?
O4B C56 1.21(3) . ?
O4B C30 1.61(2) . ?
N1 C2 1.344(7) . ?
C1 C2 1.488(10) . ?
C16 C17 1.401(9) . ?
C16 C14 1.432(9) . ?
C16 C16 1.450(9) 2_654 ?
C15 C14 1.356(10) . ?
C15 C15 1.397(17) 2_654 ?
C3 C4 1.376(9) . ?
C3 C2 1.391(9) . ?
C3 C5 1.485(8) . ?
C14 C13 1.528(7) . ?
O2 C13 1.208(10) . ?
C8 C7 1.352(9) . ?
C8 C9 1.381(10) . ?
C8 C5 1.531(9) . ?
C17 C18 1.368(9) . ?
N3 C9 1.322(10) . ?
N3 Cd1 2.265(6) 4_645 ?
C7 C6 1.499(10) . ?
C4 C11 1.471(12) . ?
C18 C18 1.410(12) 2_654 ?
C9 C10 1.475(13) . ?
C20 C56 1.09(4) . ?
C20 C30 1.53(3) . ?
C33 C30 1.262(18) 7 ?
C33 C55 1.32(2) 7 ?
C33 C32 1.360(17) . ?
C33 C55 1.588(19) . ?
C33 C56 1.617(18) 7 ?
C32 C44 1.41(2) . ?
C32 C31 1.455(16) . ?
C32 C55 1.58(2) . ?
C30 C55 1.14(2) . ?
C30 C33 1.262(18) 7 ?
C30 C56 1.44(3) . ?
C30 C31 1.46(2) . ?
C31 C55 1.31(2) . ?
C31 C41 1.40(2) . ?
C41 C42 1.34(3) . ?
C44 C43 1.33(3) . ?
C42 C43 1.38(3) . ?
C56 C33 1.617(18) 7 ?
C55 C33 1.32(2) 7 ?
C55 C55 1.55(4) 7 ?
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
O1B Cd1 O3A 92.3(10) . . ?
O1B Cd1 N1 129.2(6) . . ?
O3A Cd1 N1 112.1(10) . . ?
O1B Cd1 N3 93.9(5) . 4_655 ?
O3A Cd1 N3 128.7(9) . 4_655 ?
N1 Cd1 N3 102.6(2) . 4_655 ?
O1B Cd1 O1A 17.2(5) . . ?
O3A Cd1 O1A 107.5(9) . . ?
N1 Cd1 O1A 114.1(6) . . ?
N3 Cd1 O1A 90.4(6) 4_655 . ?
O1B Cd1 O4A 124.3(7) . . ?
O3A Cd1 O4A 57.4(6) . . ?
N1 Cd1 O4A 106.2(4) . . ?
N3 Cd1 O4A 77.6(4) 4_655 . ?
O1A Cd1 O4A 139.6(7) . . ?
O1B Cd1 O3B 92.1(7) . . ?
O3A Cd1 O3B 19.4(7) . . ?
N1 Cd1 O3B 97.9(6) . . ?
N3 Cd1 O3B 147.9(6) 4_655 . ?
O1A Cd1 O3B 103.6(7) . . ?
O4A Cd1 O3B 73.0(5) . . ?
O1B Cd1 O4B 118.7(10) . . ?
O3A Cd1 O4B 35.6(9) . . ?
N1 Cd1 O4B 105.3(6) . . ?
N3 Cd1 O4B 100.3(6) 4_655 . ?
O1A Cd1 O4B 135.8(9) . . ?
O4A Cd1 O4B 23.0(6) . . ?
O3B Cd1 O4B 50.0(7) . . ?
O1B Cd1 C20 111.8(8) . . ?
O3A Cd1 C20 30.9(10) . . ?
N1 Cd1 C20 111.2(6) . . ?
N3 Cd1 C20 101.8(8) 4_655 . ?
O1A Cd1 C20 129.0(9) . . ?
O4A Cd1 C20 26.5(8) . . ?
O3B Cd1 C20 47.1(10) . . ?
O4B Cd1 C20 6.9(10) . . ?
C7 N4 N3 111.5(6) . . ?
N1 N2 C4 112.1(5) . . ?
C13 O1A Cd1 106.4(13) . . ?
C56 O3A C20 55(2) . . ?
C56 O3A Cd1 139(2) . . ?
C20 O3A Cd1 95(2) . . ?
C20 O4A C56 11.2(13) . . ?
C20 O4A Cd1 83.0(12) . . ?
C56 O4A Cd1 78.0(7) . . ?
C13 O1B Cd1 103.1(10) . . ?
C56 O3B C20 28.7(14) . . ?
C56 O3B Cd1 96.3(16) . . ?
C20 O3B Cd1 67.9(9) . . ?
C20 O4B C56 59(9) . . ?
C20 O4B C30 70(7) . . ?
C56 O4B C30 59.6(14) . . ?
C20 O4B Cd1 87(7) . . ?
C56 O4B Cd1 94.4(16) . . ?
C30 O4B Cd1 151.3(17) . . ?
N2 N1 C2 105.7(6) . . ?
N2 N1 Cd1 119.8(4) . . ?
C2 N1 Cd1 134.4(5) . . ?
C17 C16 C14 123.7(5) . . ?
C17 C16 C16 117.9(3) . 2_654 ?
C14 C16 C16 118.4(3) . 2_654 ?
C14 C15 C15 121.5(4) . 2_654 ?
C4 C3 C2 105.4(5) . . ?
C4 C3 C5 126.8(7) . . ?
C2 C3 C5 127.7(6) . . ?
C15 C14 C16 120.1(5) . . ?
C15 C14 C13 116.2(7) . . ?
C16 C14 C13 123.6(6) . . ?
C7 C8 C9 106.7(6) . . ?
C7 C8 C5 126.8(6) . . ?
C9 C8 C5 126.5(7) . . ?
C18 C17 C16 122.4(5) . . ?
N1 C2 C3 110.2(6) . . ?
N1 C2 C1 120.5(7) . . ?
C3 C2 C1 129.3(5) . . ?
C9 N3 N4 105.5(6) . . ?
C9 N3 Cd1 130.3(6) . 4_645 ?
N4 N3 Cd1 123.9(5) . 4_645 ?
N4 C7 C8 106.3(6) . . ?
N4 C7 C6 122.5(7) . . ?
C8 C7 C6 131.1(7) . . ?
N2 C4 C3 106.7(6) . . ?
N2 C4 C11 121.6(7) . . ?
C3 C4 C11 131.7(7) . . ?
C17 C18 C18 119.6(3) . 2_654 ?
O1A C13 O2 117.4(11) . . ?
O1A C13 O1B 29.4(10) . . ?
O2 C13 O1B 123.2(9) . . ?
O1A C13 C14 117.6(12) . . ?
O2 C13 C14 124.2(7) . . ?
O1B C13 C14 109.3(10) . . ?
N3 C9 C8 110.0(7) . . ?
N3 C9 C10 118.9(8) . . ?
C8 C9 C10 131.1(8) . . ?
C3 C5 C8 113.4(5) . . ?
O4B C20 O4A 54(9) . . ?
O4B C20 C56 107(10) . . ?
O4A C20 C56 157(2) . . ?
O4B C20 O3A 119(9) . . ?
O4A C20 O3A 125(2) . . ?
C56 C20 O3A 48(2) . . ?
O4B C20 C30 99(7) . . ?
O4A C20 C30 126(2) . . ?
C56 C20 C30 64.3(19) . . ?
O3A C20 C30 109(3) . . ?
O4B C20 O3B 108(9) . . ?
O4A C20 O3B 133.0(14) . . ?
C56 C20 O3B 33.4(13) . . ?
O3A C20 O3B 18.1(19) . . ?
C30 C20 O3B 97.3(19) . . ?
O4B C20 Cd1 87(7) . . ?
O4A C20 Cd1 70.4(11) . . ?
C56 C20 Cd1 98.0(15) . . ?
O3A C20 Cd1 54.5(13) . . ?
C30 C20 Cd1 162(2) . . ?
O3B C20 Cd1 65.0(7) . . ?
C30 C33 C55 52.6(11) 7 7 ?
C30 C33 C32 178.4(11) 7 . ?
C55 C33 C32 128.3(11) 7 . ?
C30 C33 C55 116.5(11) 7 . ?
C55 C33 C55 63.9(13) 7 . ?
C32 C33 C55 64.5(9) . . ?
C30 C33 C56 58.7(10) 7 7 ?
C55 C33 C56 111.2(13) 7 7 ?
C32 C33 C56 120.4(11) . 7 ?
C55 C33 C56 175.0(12) . 7 ?
C33 C32 C44 128.9(12) . . ?
C33 C32 C31 115.7(12) . . ?
C44 C32 C31 115.3(14) . . ?
C33 C32 C55 64.8(10) . . ?
C44 C32 C55 165.4(14) . . ?
C31 C32 C55 51.0(9) . . ?
C55 C30 C33 66.1(13) . 7 ?
C55 C30 C56 139.0(19) . . ?
C33 C30 C56 73.0(12) 7 . ?
C55 C30 C31 59.2(12) . . ?
C33 C30 C31 125.3(11) 7 . ?
C56 C30 C31 161.5(15) . . ?
C55 C30 C20 176.9(19) . . ?
C33 C30 C20 115.8(16) 7 . ?
C56 C30 C20 42.8(13) . . ?
C31 C30 C20 118.9(17) . . ?
C55 C30 O4B 170.9(17) . . ?
C33 C30 O4B 117.7(14) 7 . ?
C56 C30 O4B 46.5(13) . . ?
C31 C30 O4B 116.3(14) . . ?
C20 C30 O4B 10.7(17) . . ?
C55 C31 C41 171.3(15) . . ?
C55 C31 C32 69.6(11) . . ?
C41 C31 C32 118.3(13) . . ?
C55 C31 C30 48.4(11) . . ?
C41 C31 C30 123.6(12) . . ?
C32 C31 C30 118.0(13) . . ?
C42 C41 C31 122.1(17) . . ?
C43 C44 C32 123.5(15) . . ?
C41 C42 C43 120(2) . . ?
C44 C43 C42 120.4(18) . . ?
C20 C56 O3A 77(3) . . ?
C20 C56 O3B 118(2) . . ?
O3A C56 O3B 44(2) . . ?
C20 C56 C30 72.8(17) . . ?
O3A C56 C30 141(3) . . ?
O3B C56 C30 166.2(17) . . ?
C20 C56 O4B 14(2) . . ?
O3A C56 O4B 83(2) . . ?
O3B C56 O4B 118.8(19) . . ?
C30 C56 O4B 73.9(18) . . ?
C20 C56 C33 121.1(19) . 7 ?
O3A C56 C33 152(2) . 7 ?
O3B C56 C33 120.6(18) . 7 ?
C30 C56 C33 48.3(9) . 7 ?
O4B C56 C33 120.2(18) . 7 ?
C20 C56 O4A 11.7(12) . . ?
O3A C56 O4A 76(2) . . ?
O3B C56 O4A 112.6(15) . . ?
C30 C56 O4A 79.5(12) . . ?
O4B C56 O4A 7.2(11) . . ?
C33 C56 O4A 126.7(13) 7 . ?
C30 C55 C33 61.2(13) . 7 ?
C30 C55 C31 72.4(14) . . ?
C33 C55 C31 133.6(16) 7 . ?
C30 C55 C55 128(2) . 7 ?
C33 C55 C55 66.6(14) 7 7 ?
C31 C55 C55 159(2) . 7 ?
C30 C55 C33 176.2(18) . . ?
C33 C55 C33 116.1(13) 7 . ?
C31 C55 C33 110.1(14) . . ?
C55 C55 C33 49.5(11) 7 . ?
C30 C55 C32 131.8(18) . . ?
C33 C55 C32 166.9(16) 7 . ?
C31 C55 C32 59.4(11) . . ?
C55 C55 C32 100.3(17) 7 . ?
C33 C55 C32 50.8(8) . . ?
_diffrn_measured_fraction_theta_max 0.969
_diffrn_reflns_theta_full        74.40
_diffrn_measured_fraction_theta_full 0.969
_refine_diff_density_max         1.375
_refine_diff_density_min         -2.017
_refine_diff_density_rms         0.144


data_a3
_database_code_depnum_ccdc_archive 'CCDC 910086'
#TrackingRef '(3) {[ Cd2(NDC)(HNDC)2(h2mdp)2](H2O)0.5}.CIF'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C58 H46 Cd2 N8 O12.50'
_chemical_formula_weight         1279.83
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd 0.1185 4.6533 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   p-1
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a                   13.4430(4)
_cell_length_b                   13.8010(5)
_cell_length_c                   18.8121(4)
_cell_angle_alpha                90.970(2)
_cell_angle_beta                 104.982(2)
_cell_angle_gamma                116.719(3)
_cell_volume                     2975.43(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?
_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.429
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1292
_exptl_absorpt_coefficient_mu    6.280
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3665
_exptl_absorpt_correction_T_max  0.4332
_exptl_absorpt_process_details   ?
_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'superNova (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            30931
_diffrn_reflns_av_R_equivalents  0.0302
_diffrn_reflns_av_sigmaI/netI    0.0285
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         3.63
_diffrn_reflns_theta_max         76.56
_reflns_number_total             12355
_reflns_number_gt                10417
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.1230P)^2^+2.2000P] where P=(Fo^2^+2Fc^2^)/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         12355
_refine_ls_number_parameters     802
_refine_ls_number_restraints     2148
_refine_ls_R_factor_all          0.0635
_refine_ls_R_factor_gt           0.0551
_refine_ls_wR_factor_ref         0.1852
_refine_ls_wR_factor_gt          0.1726
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_restrained_S_all      1.070
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cd1 Cd 0.63047(3) -0.03430(2) 0.560186(14) 0.04400(9) Uani 1 1 d . . .
Cd2 Cd 0.64998(3) -0.30751(2) 0.003871(14) 0.04592(9) Uani 1 1 d . . .
O6 O 0.6986(3) -0.4433(3) 0.0017(2) 0.0582(7) Uani 1 1 d U . .
O4 O 0.6769(3) -0.1494(3) 0.09374(15) 0.0531(7) Uani 1 1 d U . .
O5 O 0.5186(3) -0.5829(3) -0.04344(18) 0.0535(7) Uani 1 1 d U . .
O3 O 0.7403(3) -0.2676(3) 0.13050(16) 0.0534(6) Uani 1 1 d U . .
O2 O 0.6907(3) -0.0172(3) 0.45848(17) 0.0578(7) Uani 1 1 d U . .
N2 N 0.4952(3) -0.1337(3) 0.6160(2) 0.0510(8) Uani 1 1 d . . .
N7 N 0.5253(4) -0.3495(3) 0.8881(2) 0.0522(9) Uani 1 1 d . . .
O10 O 0.5534(4) 0.1038(3) 0.5496(3) 0.0870(12) Uani 1 1 d U . .
O8 O 0.6462(4) -0.9758(3) 0.0856(3) 0.0791(11) Uani 1 1 d U . .
H8B H 0.6599 -1.0280 0.0887 0.119 Uiso 1 1 calc R . .
O1 O 0.6910(4) -0.1707(3) 0.48573(18) 0.0668(9) Uani 1 1 d U . .
N8 N 0.4764(4) -0.4537(3) 0.8518(2) 0.0569(10) Uani 1 1 d . . .
H8A H 0.4906 -0.5043 0.8702 0.068 Uiso 1 1 calc R . .
N5 N 0.8174(3) -0.0554(3) 0.98953(19) 0.0506(8) Uani 1 1 d . . .
H5A H 0.7988 -0.0353 1.0255 0.061 Uiso 1 1 calc R . .
N3 N 0.7709(3) -0.0465(3) 0.65282(19) 0.0497(8) Uani 1 1 d . . .
C41 C 0.8139(4) -0.1587(3) 0.2872(2) 0.0434(7) Uani 1 1 d U . .
C40 C 0.8077(4) -0.0097(4) 0.7254(2) 0.0505(9) Uani 1 1 d U . .
C24 C 0.4030(5) -0.4682(4) 0.7839(3) 0.0590(11) Uani 1 1 d U . .
C38 C 0.4812(4) -0.2976(4) 0.8406(2) 0.0505(9) Uani 1 1 d U . .
N1 N 0.4127(4) -0.1074(3) 0.6218(2) 0.0529(8) Uani 1 1 d . . .
H1A H 0.4071 -0.0514 0.6060 0.063 Uiso 1 1 calc R . .
N4 N 0.8318(3) -0.0985(3) 0.64352(19) 0.0501(8) Uani 1 1 d . . .
H4B H 0.8242 -0.1301 0.6012 0.060 Uiso 1 1 calc R . .
N6 N 0.7878(4) -0.1609(3) 0.9662(2) 0.0516(8) Uani 1 1 d . . .
O7 O 0.8399(4) -0.8801(4) 0.1145(2) 0.0758(10) Uani 1 1 d U . .
C37 C 0.6249(4) -0.5433(4) -0.0079(3) 0.0509(8) Uani 1 1 d U . .
C32 C 0.6977(4) -0.1033(4) 0.4427(2) 0.0501(9) Uani 1 1 d U . .
C35 C 0.9060(4) -0.1790(4) 0.2817(2) 0.0503(8) Uani 1 1 d U . .
H35A H 0.9106 -0.1949 0.2347 0.060 Uiso 1 1 calc R . .
C34 C 0.3788(4) -0.2547(4) 0.6738(2) 0.0518(9) Uani 1 1 d U . .
C33 C 0.8926(4) -0.0385(4) 0.7632(2) 0.0480(9) Uani 1 1 d U . .
C28 C 0.3394(4) -0.1796(4) 0.6553(3) 0.0534(9) Uani 1 1 d U . .
C31 C 0.9618(4) -0.0075(4) 0.8444(2) 0.0517(9) Uani 1 1 d U . .
H31A H 1.0173 -0.0359 0.8528 0.062 Uiso 1 1 calc R . .
H31B H 1.0060 0.0719 0.8560 0.062 Uiso 1 1 calc R . .
C30 C 0.7238(4) -0.7893(4) 0.0715(3) 0.0540(9) Uani 1 1 d U . .
C29 C 0.3236(5) -0.3526(4) 0.7103(3) 0.0621(11) Uani 1 1 d U . .
H29A H 0.2851 -0.4177 0.6730 0.075 Uiso 1 1 calc R . .
H29B H 0.2638 -0.3468 0.7271 0.075 Uiso 1 1 calc R . .
C18 C 0.8796(4) 0.0143(4) 0.9495(2) 0.0490(9) Uani 1 1 d U . .
C27 C 0.8070(4) -0.1375(3) 0.3601(2) 0.0447(8) Uani 1 1 d U . .
C26 C 0.8910(4) -0.0481(4) 0.8973(2) 0.0463(8) Uani 1 1 d U . .
C25 C 0.7165(4) -0.1927(3) 0.1454(2) 0.0464(8) Uani 1 1 d U . .
C36 C 0.6330(4) -0.1194(4) 0.3060(2) 0.0527(9) Uani 1 1 d U . .
H36A H 0.5727 -0.1072 0.3116 0.063 Uiso 1 1 calc R . .
C23 C 0.6337(5) -0.8114(4) 0.0080(3) 0.0602(10) Uani 1 1 d U . .
H23A H 0.5898 -0.8821 -0.0187 0.072 Uiso 1 1 calc R . .
C22 C 0.4042(4) -0.3692(4) 0.7755(2) 0.0531(10) Uani 1 1 d U . .
C21 C 0.6678(4) -0.6234(4) 0.0234(3) 0.0504(8) Uani 1 1 d U . .
C20 C 0.6556(6) 0.1766(4) 0.5687(4) 0.0694(11) Uani 1 1 d U . .
C19 C 0.7266(4) -0.1596(3) 0.2241(2) 0.0443(7) Uani 1 1 d U . .
C8 C 0.9066(4) -0.0950(4) 0.7090(2) 0.0502(9) Uani 1 1 d U . .
C17 C 0.8324(4) -0.1563(4) 0.9093(2) 0.0479(9) Uani 1 1 d U . .
C16 C 0.7135(4) -0.1199(3) 0.3672(2) 0.0470(8) Uani 1 1 d U . .
C15 C 0.8963(4) -0.1325(4) 0.4236(3) 0.0541(9) Uani 1 1 d U . .
H15A H 0.8945 -0.1160 0.4712 0.065 Uiso 1 1 calc R . .
C14 C 0.7445(5) -0.8842(4) 0.0947(3) 0.0580(10) Uani 1 1 d U . .
C13 C 0.4761(4) -0.2241(4) 0.6481(3) 0.0534(9) Uani 1 1 d U . .
C12 C 0.8223(5) -0.4935(5) 0.1358(3) 0.0635(10) Uani 1 1 d U . .
H12A H 0.8024 -0.4386 0.1222 0.076 Uiso 1 1 calc R . .
C11 C 0.6410(4) -0.1375(4) 0.2341(2) 0.0517(8) Uani 1 1 d U . .
H11A H 0.5872 -0.1344 0.1929 0.062 Uiso 1 1 calc R . .
O9 O 0.7366(4) 0.1548(3) 0.5872(3) 0.0835(10) Uani 1 1 d U . .
C10 C 0.9889(4) -0.1759(4) 0.3436(3) 0.0571(10) Uani 1 1 d U . .
H10A H 1.0482 -0.1900 0.3382 0.068 Uiso 1 1 calc R . .
C9 C 0.7601(4) -0.5978(4) 0.0904(3) 0.0529(8) Uani 1 1 d U . .
C39 C 0.9188(5) 0.1355(4) 0.9633(3) 0.0639(12) Uani 1 1 d U . .
H39A H 0.8958 0.1515 1.0044 0.096 Uiso 1 1 calc R . .
H39B H 0.8833 0.1568 0.9196 0.096 Uiso 1 1 calc R . .
H39C H 1.0021 0.1754 0.9747 0.096 Uiso 1 1 calc R . .
C7 C 0.6080(5) -0.7274(4) -0.0165(3) 0.0566(9) Uani 1 1 d U . .
H7A H 0.5492 -0.7425 -0.0606 0.068 Uiso 1 1 calc R . .
C6 C 0.7628(5) 0.0582(5) 0.7565(3) 0.0634(12) Uani 1 1 d U . .
H6A H 0.7050 0.0644 0.7173 0.095 Uiso 1 1 calc R . .
H6B H 0.8261 0.1300 0.7781 0.095 Uiso 1 1 calc R . .
H6C H 0.7285 0.0235 0.7941 0.095 Uiso 1 1 calc R . .
C5 C 0.9867(5) -0.1423(5) 0.7122(3) 0.0707(14) Uani 1 1 d U . .
H5B H 1.0321 -0.1324 0.7630 0.106 Uiso 1 1 calc R . .
H5C H 1.0378 -0.1060 0.6829 0.106 Uiso 1 1 calc R . .
H5D H 0.9422 -0.2193 0.6929 0.106 Uiso 1 1 calc R . .
C4 C 0.9843(5) -0.1516(5) 0.4149(3) 0.0636(11) Uani 1 1 d U . .
H4A H 1.0414 -0.1484 0.4566 0.076 Uiso 1 1 calc R . .
C3 C 0.7902(4) -0.6830(4) 0.1137(3) 0.0532(8) Uani 1 1 d U . .
C1 C 0.5186(5) -0.1786(4) 0.8590(3) 0.0648(12) Uani 1 1 d U . .
H1B H 0.5728 -0.1508 0.9081 0.097 Uiso 1 1 calc R . .
H1C H 0.4517 -0.1688 0.8570 0.097 Uiso 1 1 calc R . .
H1D H 0.5554 -0.1394 0.8236 0.097 Uiso 1 1 calc R . .
C45 C 0.8835(5) -0.6568(5) 0.1788(3) 0.0648(11) Uani 1 1 d U . .
H45A H 0.9050 -0.7101 0.1942 0.078 Uiso 1 1 calc R . .
C42 C 0.5490(5) -0.2796(5) 0.6510(4) 0.0693(13) Uani 1 1 d U . .
H42A H 0.6096 -0.2394 0.6289 0.104 Uiso 1 1 calc R . .
H42B H 0.5013 -0.3529 0.6241 0.104 Uiso 1 1 calc R . .
H42C H 0.5833 -0.2825 0.7019 0.104 Uiso 1 1 calc R . .
C46 C 0.9423(6) -0.5547(5) 0.2194(4) 0.0757(14) Uani 1 1 d U . .
H46A H 1.0049 -0.5386 0.2614 0.091 Uiso 1 1 calc R . .
C43 C 0.2348(6) -0.1722(5) 0.6660(4) 0.0786(15) Uani 1 1 d U . .
H43A H 0.2325 -0.1088 0.6471 0.118 Uiso 1 1 calc R . .
H43B H 0.2410 -0.1661 0.7180 0.118 Uiso 1 1 calc R . .
H43C H 0.1646 -0.2370 0.6395 0.118 Uiso 1 1 calc R . .
C44 C 0.3428(7) -0.5740(5) 0.7339(4) 0.090(2) Uani 1 1 d U . .
H44A H 0.3625 -0.6261 0.7586 0.135 Uiso 1 1 calc R . .
H44B H 0.3667 -0.5641 0.6895 0.135 Uiso 1 1 calc R . .
H44C H 0.2600 -0.6008 0.7209 0.135 Uiso 1 1 calc R . .
C47 C 0.9101(6) -0.4724(5) 0.1988(3) 0.0748(13) Uani 1 1 d U . .
H47A H 0.9492 -0.4038 0.2284 0.090 Uiso 1 1 calc R . .
C55 C 0.8143(5) -0.2589(4) 0.8669(3) 0.0638(12) Uani 1 1 d U . .
H55A H 0.7699 -0.3214 0.8877 0.096 Uiso 1 1 calc R . .
H55B H 0.8886 -0.2548 0.8703 0.096 Uiso 1 1 calc R . .
H55C H 0.7727 -0.2660 0.8156 0.096 Uiso 1 1 calc R . .
O11 O 0.6592(5) 0.6238(4) 0.4750(3) 0.1032(16) Uani 1 1 d U . .
H11B H 0.6664 0.6861 0.4763 0.155 Uiso 1 1 calc R . .
C73 C 0.6822(6) 0.2944(5) 0.5614(4) 0.0790(12) Uani 1 1 d U . .
O12 O 0.8193(6) 0.7056(4) 0.5609(4) 0.140(2) Uani 1 1 d U . .
C74 C 0.7178(6) 0.5087(5) 0.5391(5) 0.0905(13) Uani 1 1 d U . .
C52 C 0.7338(7) 0.6220(5) 0.5267(5) 0.0929(15) Uani 1 1 d U . .
C79 C 0.5967(9) 0.3258(7) 0.5474(6) 0.0819(14) Uani 0.70 1 d PU . .
C80 C 0.6150(9) 0.4328(7) 0.5336(7) 0.0875(16) Uani 0.70 1 d PU . .
C76 C 0.7926(10) 0.3761(8) 0.5498(7) 0.0920(15) Uani 0.70 1 d PU . .
C75 C 0.8139(10) 0.4857(8) 0.5419(7) 0.0953(16) Uani 0.70 1 d PU . .
C78 C 0.9398(11) 0.5719(9) 0.5625(8) 0.107(2) Uani 0.70 1 d PU . .
C49 C 0.8984(11) 0.3545(9) 0.5820(8) 0.1040(19) Uani 0.70 1 d PU . .
C71 C 0.675(2) 0.3502(16) 0.6346(15) 0.0822(19) Uani 0.30 1 d PU . .
C72 C 0.682(2) 0.5123(16) 0.6966(15) 0.086(2) Uani 0.30 1 d PU . .
C69 C 0.724(2) 0.4472(16) 0.5073(15) 0.086(2) Uani 0.30 1 d PU . .
C77 C 0.711(2) 0.3386(18) 0.5138(16) 0.0876(19) Uani 0.30 1 d PU . .
O1W O 0.9630(17) -0.5468(17) -0.0277(11) 0.203(8) Uani 0.50 1 d PU . .
C96 C 1.0298(12) 0.5452(10) 0.5831(9) 0.114(2) Uani 0.70 1 d PU . .
C85 C 0.665(2) 0.4595(18) 0.7547(16) 0.089(3) Uani 0.30 1 d PU . .
C84 C 0.686(2) 0.4587(16) 0.6283(15) 0.0837(19) Uani 0.30 1 d PU . .
C50 C 0.661(2) 0.3026(17) 0.7051(15) 0.083(2) Uani 0.30 1 d PU . .
C87 C 0.666(2) 0.3708(18) 0.7654(15) 0.087(3) Uani 0.30 1 d PU . .
C83 C 1.0108(12) 0.4383(10) 0.5915(9) 0.117(2) Uani 0.70 1 d PU . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cd1 0.06347(17) 0.04343(14) 0.03353(14) 0.01804(10) 0.01806(11) 0.02984(12)
Cd2 0.07116(18) 0.04843(15) 0.03260(14) 0.01803(11) 0.02204(12) 0.03630(13)
O6 0.0831(17) 0.0515(14) 0.0625(16) 0.0217(12) 0.0353(14) 0.0428(13)
O4 0.0880(18) 0.0608(15) 0.0331(12) 0.0206(11) 0.0242(12) 0.0503(14)
O5 0.0752(16) 0.0561(15) 0.0568(16) 0.0307(12) 0.0310(13) 0.0471(13)
O3 0.0855(16) 0.0549(14) 0.0395(13) 0.0133(11) 0.0227(12) 0.0473(13)
O2 0.0942(18) 0.0603(15) 0.0435(14) 0.0138(12) 0.0278(13) 0.0528(14)
N2 0.065(2) 0.0503(18) 0.0524(19) 0.0302(15) 0.0263(16) 0.0336(16)
N7 0.074(2) 0.0524(19) 0.0383(17) 0.0182(14) 0.0190(16) 0.0350(17)
O10 0.097(2) 0.0543(17) 0.092(2) 0.0211(17) 0.0153(19) 0.0276(17)
O8 0.090(2) 0.0633(19) 0.113(3) 0.041(2) 0.040(2) 0.0537(18)
O1 0.120(3) 0.0497(16) 0.0442(15) 0.0190(13) 0.0387(17) 0.0429(17)
N8 0.082(3) 0.0463(18) 0.0446(18) 0.0227(15) 0.0140(17) 0.0340(18)
N5 0.072(2) 0.0549(19) 0.0341(16) 0.0128(14) 0.0190(15) 0.0356(17)
N3 0.0618(19) 0.059(2) 0.0361(16) 0.0156(14) 0.0163(14) 0.0339(17)
C41 0.0628(16) 0.0415(15) 0.0380(15) 0.0171(12) 0.0215(13) 0.0308(13)
C40 0.0629(19) 0.061(2) 0.0377(17) 0.0180(15) 0.0195(15) 0.0344(17)
C24 0.074(2) 0.049(2) 0.047(2) 0.0242(17) 0.0133(18) 0.0247(18)
C38 0.067(2) 0.0529(19) 0.0467(18) 0.0239(15) 0.0274(16) 0.0344(16)
N1 0.074(2) 0.0541(19) 0.0487(19) 0.0276(15) 0.0261(16) 0.0407(17)
N4 0.064(2) 0.060(2) 0.0348(16) 0.0120(14) 0.0147(14) 0.0363(17)
N6 0.075(2) 0.0538(19) 0.0392(17) 0.0175(14) 0.0240(16) 0.0370(17)
O7 0.087(2) 0.083(2) 0.084(2) 0.0246(19) 0.0191(19) 0.0646(19)
C37 0.076(2) 0.0516(18) 0.0543(19) 0.0215(15) 0.0363(16) 0.0445(16)
C32 0.076(2) 0.0514(18) 0.0392(17) 0.0112(14) 0.0257(16) 0.0391(16)
C35 0.0632(18) 0.0528(17) 0.0459(17) 0.0191(14) 0.0260(15) 0.0308(15)
C34 0.0609(19) 0.0530(19) 0.0462(18) 0.0285(15) 0.0190(15) 0.0285(16)
C33 0.0562(18) 0.0587(19) 0.0358(16) 0.0198(15) 0.0179(14) 0.0300(16)
C28 0.066(2) 0.059(2) 0.048(2) 0.0257(17) 0.0240(17) 0.0356(17)
C31 0.0574(18) 0.064(2) 0.0362(17) 0.0182(15) 0.0169(15) 0.0290(16)
C30 0.0731(19) 0.0597(18) 0.0560(19) 0.0231(15) 0.0274(16) 0.0488(15)
C29 0.067(2) 0.058(2) 0.058(2) 0.0338(18) 0.0178(18) 0.0263(18)
C18 0.064(2) 0.0528(19) 0.0373(17) 0.0159(15) 0.0154(15) 0.0324(16)
C27 0.0672(17) 0.0431(15) 0.0366(15) 0.0159(12) 0.0200(14) 0.0337(13)
C26 0.0578(18) 0.0563(19) 0.0301(15) 0.0159(14) 0.0132(14) 0.0308(15)
C25 0.0705(19) 0.0471(17) 0.0361(16) 0.0141(13) 0.0226(15) 0.0361(15)
C36 0.0746(19) 0.0602(18) 0.0423(17) 0.0113(15) 0.0216(15) 0.0452(16)
C23 0.078(2) 0.0582(19) 0.062(2) 0.0187(17) 0.0191(18) 0.0479(17)
C22 0.065(2) 0.0503(18) 0.0462(18) 0.0284(15) 0.0212(16) 0.0263(16)
C21 0.0698(17) 0.0569(17) 0.0515(17) 0.0240(14) 0.0291(15) 0.0459(14)
C20 0.089(2) 0.0494(18) 0.080(2) 0.0101(18) 0.024(2) 0.0414(17)
C19 0.0693(17) 0.0456(15) 0.0337(15) 0.0145(12) 0.0217(13) 0.0365(14)
C8 0.061(2) 0.060(2) 0.0391(18) 0.0194(16) 0.0176(15) 0.0344(17)
C17 0.064(2) 0.055(2) 0.0336(16) 0.0167(15) 0.0190(15) 0.0335(17)
C16 0.0726(18) 0.0465(16) 0.0377(16) 0.0155(13) 0.0237(14) 0.0372(14)
C15 0.071(2) 0.0557(18) 0.0418(17) 0.0147(15) 0.0157(16) 0.0354(16)
C14 0.080(2) 0.062(2) 0.058(2) 0.0218(17) 0.0276(18) 0.0516(18)
C13 0.067(2) 0.0520(19) 0.051(2) 0.0274(16) 0.0179(17) 0.0356(16)
C12 0.081(2) 0.0639(19) 0.060(2) 0.0182(17) 0.0249(17) 0.0432(17)
C11 0.0747(19) 0.0590(18) 0.0372(16) 0.0118(14) 0.0150(15) 0.0454(15)
O9 0.097(2) 0.0582(16) 0.104(2) 0.0136(16) 0.0194(18) 0.0495(15)
C10 0.058(2) 0.059(2) 0.060(2) 0.0159(18) 0.0184(17) 0.0323(17)
C9 0.0730(18) 0.0579(17) 0.0532(17) 0.0229(14) 0.0322(15) 0.0443(14)
C39 0.084(3) 0.052(2) 0.054(2) 0.008(2) 0.016(2) 0.033(2)
C7 0.0764(19) 0.0572(18) 0.0574(19) 0.0196(16) 0.0233(16) 0.0469(15)
C6 0.078(3) 0.082(3) 0.045(2) 0.012(2) 0.018(2) 0.051(2)
C5 0.082(3) 0.087(4) 0.058(3) 0.015(3) 0.020(2) 0.052(3)
C4 0.067(2) 0.067(2) 0.054(2) 0.0179(19) 0.0116(18) 0.0327(19)
C3 0.0680(18) 0.0632(18) 0.0533(18) 0.0247(15) 0.0288(15) 0.0456(15)
C1 0.092(3) 0.061(3) 0.058(3) 0.017(2) 0.022(2) 0.049(2)
C45 0.078(2) 0.070(2) 0.060(2) 0.0226(18) 0.0232(18) 0.0450(18)
C42 0.077(3) 0.064(3) 0.085(3) 0.038(2) 0.031(2) 0.044(2)
C46 0.083(3) 0.078(3) 0.064(2) 0.017(2) 0.016(2) 0.039(2)
C43 0.090(3) 0.082(3) 0.091(4) 0.038(3) 0.049(3) 0.051(3)
C44 0.119(5) 0.047(3) 0.072(3) 0.016(2) 0.000(3) 0.027(3)
C47 0.088(3) 0.070(2) 0.064(2) 0.010(2) 0.022(2) 0.036(2)
C55 0.087(3) 0.062(3) 0.052(2) 0.011(2) 0.028(2) 0.039(2)
O11 0.145(4) 0.049(2) 0.105(3) 0.013(2) 0.023(3) 0.044(2)
C73 0.084(2) 0.0494(17) 0.111(2) 0.0053(19) 0.022(2) 0.0426(16)
O12 0.156(4) 0.058(2) 0.159(4) -0.005(3) -0.020(4) 0.048(3)
C74 0.096(2) 0.0499(19) 0.126(3) 0.005(2) 0.011(2) 0.0458(17)
C52 0.100(3) 0.049(2) 0.127(3) 0.001(2) 0.011(3) 0.0455(19)
C79 0.090(2) 0.052(2) 0.111(2) 0.011(2) 0.022(2) 0.0436(18)
C80 0.093(2) 0.054(2) 0.120(3) 0.013(2) 0.019(2) 0.045(2)
C76 0.095(2) 0.058(2) 0.123(2) 0.010(2) 0.022(2) 0.042(2)
C75 0.098(2) 0.058(2) 0.129(3) 0.007(2) 0.025(2) 0.041(2)
C78 0.103(3) 0.068(3) 0.134(3) 0.006(3) 0.018(3) 0.037(2)
C49 0.101(3) 0.069(3) 0.126(3) 0.008(3) 0.016(3) 0.037(2)
C71 0.092(2) 0.053(2) 0.109(3) 0.008(2) 0.024(2) 0.044(2)
C72 0.096(3) 0.053(3) 0.113(3) 0.002(3) 0.025(3) 0.043(3)
C69 0.096(3) 0.051(2) 0.116(3) 0.008(3) 0.018(3) 0.047(2)
C77 0.096(2) 0.054(2) 0.115(3) 0.008(2) 0.018(2) 0.044(2)
O1W 0.176(12) 0.204(14) 0.167(12) 0.020(11) 0.101(10) 0.012(11)
C96 0.105(3) 0.077(3) 0.137(4) 0.010(3) 0.013(3) 0.036(3)
C85 0.099(4) 0.059(4) 0.107(5) 0.002(4) 0.027(4) 0.037(4)
C84 0.093(3) 0.052(2) 0.115(3) 0.005(3) 0.023(3) 0.046(2)
C50 0.094(3) 0.054(3) 0.106(3) 0.009(3) 0.025(3) 0.041(3)
C87 0.096(4) 0.059(4) 0.105(5) 0.006(4) 0.028(4) 0.037(4)
C83 0.107(3) 0.078(3) 0.140(4) 0.007(3) 0.016(3) 0.031(3)
_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 O2 2.240(3) . ?
Cd1 N2 2.255(4) . ?
Cd1 N3 2.286(4) . ?
Cd1 O9 2.310(4) . ?
Cd1 O10 2.535(5) . ?
Cd1 O10 2.542(5) 2_656 ?
Cd2 O6 2.248(3) . ?
Cd2 N7 2.255(4) 1_554 ?
Cd2 O3 2.305(3) . ?
Cd2 N6 2.321(4) 1_554 ?
Cd2 O5 2.409(3) 2_645 ?
Cd2 O4 2.569(3) . ?
O6 C37 1.261(6) . ?
O4 C25 1.275(5) . ?
O5 C37 1.257(6) . ?
O5 Cd2 2.409(3) 2_645 ?
O3 C25 1.258(5) . ?
O2 C32 1.270(5) . ?
N2 N1 1.340(6) . ?
N2 C13 1.344(5) . ?
N7 C38 1.338(6) . ?
N7 N8 1.361(5) . ?
N7 Cd2 2.255(4) 1_556 ?
O10 C20 1.232(8) . ?
O10 Cd1 2.542(5) 2_656 ?
O8 C14 1.321(7) . ?
O1 C32 1.232(6) . ?
N8 C24 1.345(6) . ?
N5 C18 1.349(6) . ?
N5 N6 1.356(5) . ?
N3 C40 1.331(5) . ?
N3 N4 1.346(5) . ?
C41 C35 1.414(6) . ?
C41 C27 1.432(5) . ?
C41 C19 1.434(6) . ?
C40 C33 1.401(6) . ?
C40 C6 1.502(7) . ?
C24 C22 1.372(7) . ?
C24 C44 1.473(8) . ?
C38 C22 1.390(7) . ?
C38 C1 1.490(7) . ?
N1 C28 1.350(6) . ?
N4 C8 1.359(5) . ?
N6 C17 1.345(6) . ?
N6 Cd2 2.321(4) 1_556 ?
O7 C14 1.213(6) . ?
C37 C21 1.524(6) . ?
C32 C16 1.518(6) . ?
C35 C10 1.373(7) . ?
C34 C28 1.374(7) . ?
C34 C13 1.401(7) . ?
C34 C29 1.496(6) . ?
C33 C8 1.374(6) . ?
C33 C31 1.507(6) . ?
C28 C43 1.517(8) . ?
C31 C26 1.496(6) . ?
C30 C23 1.376(7) . ?
C30 C3 1.412(7) . ?
C30 C14 1.507(6) . ?
C29 C22 1.508(6) . ?
C18 C26 1.377(6) . ?
C18 C39 1.504(7) . ?
C27 C16 1.421(6) . ?
C27 C15 1.433(6) . ?
C26 C17 1.396(6) . ?
C25 C19 1.495(5) . ?
C36 C16 1.363(6) . ?
C36 C11 1.410(6) . ?
C23 C7 1.404(6) . ?
C21 C7 1.372(7) . ?
C21 C9 1.427(7) . ?
C20 O9 1.224(7) . ?
C20 C73 1.516(7) . ?
C19 C11 1.371(6) . ?
C8 C5 1.479(7) . ?
C17 C55 1.499(7) . ?
C15 C4 1.369(8) . ?
C13 C42 1.482(7) . ?
C12 C47 1.356(8) . ?
C12 C9 1.417(7) . ?
C10 C4 1.400(8) . ?
C9 C3 1.447(6) . ?
C3 C45 1.410(7) . ?
C45 C46 1.357(8) . ?
C46 C47 1.413(9) . ?
O11 C52 1.213(9) . ?
C73 C77 1.14(3) . ?
C73 C79 1.368(11) . ?
C73 C76 1.482(14) . ?
C73 C71 1.61(3) . ?
O12 C52 1.211(9) . ?
C74 C69 1.07(2) . ?
C74 C80 1.281(13) . ?
C74 C75 1.451(13) . ?
C74 C52 1.510(8) . ?
C74 C84 1.90(3) . ?
C79 C80 1.425(12) . ?
C79 C71 1.64(3) . ?
C79 C77 1.75(3) . ?
C79 C84 2.03(2) . ?
C80 C69 1.60(3) . ?
C80 C84 1.73(3) . ?
C76 C77 1.01(3) . ?
C76 C75 1.425(13) . ?
C76 C49 1.555(16) . ?
C76 C69 1.71(2) . ?
C75 C69 1.08(2) . ?
C75 C78 1.505(16) . ?
C75 C77 1.84(2) . ?
C78 C96 1.383(18) . ?
C49 C83 1.391(18) . ?
C71 C84 1.45(3) . ?
C71 C50 1.51(4) . ?
C72 C85 1.34(4) . ?
C72 C84 1.50(3) . ?
C69 C77 1.44(3) . ?
O1W O1W 1.42(4) 2_745 ?
C96 C83 1.399(18) . ?
C85 C87 1.25(3) . ?
C50 C87 1.43(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
O2 Cd1 N2 147.95(14) . . ?
O2 Cd1 N3 106.21(13) . . ?
N2 Cd1 N3 89.96(14) . . ?
O2 Cd1 O9 85.77(16) . . ?
N2 Cd1 O9 122.67(17) . . ?
N3 Cd1 O9 89.30(15) . . ?
O2 Cd1 O10 100.15(15) . . ?
N2 Cd1 O10 88.69(15) . . ?
N3 Cd1 O10 131.14(15) . . ?
O9 Cd1 O10 52.20(15) . . ?
O2 Cd1 O10 74.47(16) . 2_656 ?
N2 Cd1 O10 79.92(15) . 2_656 ?
N3 Cd1 O10 156.67(14) . 2_656 ?
O9 Cd1 O10 113.88(15) . 2_656 ?
O10 Cd1 O10 70.06(17) . 2_656 ?
O6 Cd2 N7 100.02(14) . 1_554 ?
O6 Cd2 O3 87.67(12) . . ?
N7 Cd2 O3 166.42(14) 1_554 . ?
O6 Cd2 N6 106.34(13) . 1_554 ?
N7 Cd2 N6 89.15(14) 1_554 1_554 ?
O3 Cd2 N6 99.48(13) . 1_554 ?
O6 Cd2 O5 92.84(11) . 2_645 ?
N7 Cd2 O5 86.60(13) 1_554 2_645 ?
O3 Cd2 O5 81.81(12) . 2_645 ?
N6 Cd2 O5 160.79(12) 1_554 2_645 ?
O6 Cd2 O4 140.97(11) . . ?
N7 Cd2 O4 118.66(12) 1_554 . ?
O3 Cd2 O4 53.40(10) . . ?
N6 Cd2 O4 80.69(12) 1_554 . ?
O5 Cd2 O4 84.95(11) 2_645 . ?
C37 O6 Cd2 122.7(3) . . ?
C25 O4 Cd2 85.8(2) . . ?
C37 O5 Cd2 129.2(3) . 2_645 ?
C25 O3 Cd2 98.5(3) . . ?
C32 O2 Cd1 107.6(3) . . ?
N1 N2 C13 106.3(4) . . ?
N1 N2 Cd1 121.9(3) . . ?
C13 N2 Cd1 131.9(3) . . ?
C38 N7 N8 105.0(4) . . ?
C38 N7 Cd2 137.0(3) . 1_556 ?
N8 N7 Cd2 118.0(3) . 1_556 ?
C20 O10 Cd1 87.6(4) . . ?
C20 O10 Cd1 139.7(4) . 2_656 ?
Cd1 O10 Cd1 109.94(17) . 2_656 ?
C24 N8 N7 112.1(4) . . ?
C18 N5 N6 111.7(4) . . ?
C40 N3 N4 105.4(4) . . ?
C40 N3 Cd1 129.5(3) . . ?
N4 N3 Cd1 125.1(3) . . ?
C35 C41 C27 118.0(4) . . ?
C35 C41 C19 123.7(4) . . ?
C27 C41 C19 118.4(4) . . ?
N3 C40 C33 111.0(4) . . ?
N3 C40 C6 120.6(4) . . ?
C33 C40 C6 128.3(4) . . ?
N8 C24 C22 106.2(4) . . ?
N8 C24 C44 121.4(5) . . ?
C22 C24 C44 132.4(5) . . ?
N7 C38 C22 110.3(4) . . ?
N7 C38 C1 121.3(4) . . ?
C22 C38 C1 128.4(4) . . ?
N2 N1 C28 111.8(4) . . ?
N3 N4 C8 111.9(4) . . ?
C17 N6 N5 105.1(4) . . ?
C17 N6 Cd2 131.3(3) . 1_556 ?
N5 N6 Cd2 121.9(3) . 1_556 ?
O5 C37 O6 124.9(4) . . ?
O5 C37 C21 117.1(4) . . ?
O6 C37 C21 118.0(4) . . ?
O1 C32 O2 122.1(4) . . ?
O1 C32 C16 121.4(4) . . ?
O2 C32 C16 116.5(4) . . ?
C10 C35 C41 121.8(4) . . ?
C28 C34 C13 106.1(4) . . ?
C28 C34 C29 126.3(5) . . ?
C13 C34 C29 127.6(5) . . ?
C8 C33 C40 105.2(4) . . ?
C8 C33 C31 126.3(4) . . ?
C40 C33 C31 128.3(4) . . ?
N1 C28 C34 106.5(4) . . ?
N1 C28 C43 122.8(4) . . ?
C34 C28 C43 130.7(5) . . ?
C26 C31 C33 115.1(4) . . ?
C23 C30 C3 120.9(4) . . ?
C23 C30 C14 116.8(4) . . ?
C3 C30 C14 122.2(4) . . ?
C34 C29 C22 116.4(4) . . ?
N5 C18 C26 107.0(4) . . ?
N5 C18 C39 121.5(4) . . ?
C26 C18 C39 131.5(4) . . ?
C16 C27 C41 119.1(4) . . ?
C16 C27 C15 122.2(4) . . ?
C41 C27 C15 118.7(4) . . ?
C18 C26 C17 105.5(4) . . ?
C18 C26 C31 127.2(4) . . ?
C17 C26 C31 127.1(4) . . ?
O3 C25 O4 120.9(4) . . ?
O3 C25 C19 119.7(4) . . ?
O4 C25 C19 119.3(4) . . ?
C16 C36 C11 120.2(4) . . ?
C30 C23 C7 120.0(5) . . ?
C24 C22 C38 106.5(4) . . ?
C24 C22 C29 123.5(4) . . ?
C38 C22 C29 129.6(5) . . ?
C7 C21 C9 120.2(4) . . ?
C7 C21 C37 115.1(4) . . ?
C9 C21 C37 124.6(4) . . ?
O9 C20 O10 121.3(5) . . ?
O9 C20 C73 119.0(6) . . ?
O10 C20 C73 119.4(6) . . ?
C11 C19 C41 120.1(4) . . ?
C11 C19 C25 116.3(4) . . ?
C41 C19 C25 123.4(4) . . ?
C33 C8 N4 106.5(4) . . ?
C33 C8 C5 131.8(4) . . ?
N4 C8 C5 121.6(4) . . ?
N6 C17 C26 110.7(4) . . ?
N6 C17 C55 121.0(4) . . ?
C26 C17 C55 128.3(4) . . ?
C36 C16 C27 121.0(4) . . ?
C36 C16 C32 117.5(4) . . ?
C27 C16 C32 121.5(4) . . ?
C4 C15 C27 120.8(4) . . ?
O7 C14 O8 123.1(5) . . ?
O7 C14 C30 124.2(5) . . ?
O8 C14 C30 112.4(4) . . ?
N2 C13 C34 109.3(4) . . ?
N2 C13 C42 122.1(5) . . ?
C34 C13 C42 128.5(4) . . ?
C47 C12 C9 121.2(5) . . ?
C19 C11 C36 121.1(4) . . ?
C20 O9 Cd1 98.6(4) . . ?
C35 C10 C4 120.2(5) . . ?
C12 C9 C21 123.1(4) . . ?
C12 C9 C3 118.5(5) . . ?
C21 C9 C3 118.3(4) . . ?
C21 C7 C23 121.4(5) . . ?
C15 C4 C10 120.5(5) . . ?
C45 C3 C30 122.7(4) . . ?
C45 C3 C9 118.3(5) . . ?
C30 C3 C9 119.0(4) . . ?
C46 C45 C3 120.9(5) . . ?
C45 C46 C47 121.2(6) . . ?
C12 C47 C46 119.9(6) . . ?
C77 C73 C79 87.6(14) . . ?
C77 C73 C76 43.0(13) . . ?
C79 C73 C76 113.9(7) . . ?
C77 C73 C20 125.0(13) . . ?
C79 C73 C20 121.8(7) . . ?
C76 C73 C20 122.5(6) . . ?
C77 C73 C71 125.4(14) . . ?
C79 C73 C71 66.1(10) . . ?
C76 C73 C71 104.5(10) . . ?
C20 C73 C71 109.4(10) . . ?
C69 C74 C80 84.8(15) . . ?
C69 C74 C75 47.9(13) . . ?
C80 C74 C75 122.3(7) . . ?
C69 C74 C52 132.4(17) . . ?
C80 C74 C52 118.3(7) . . ?
C75 C74 C52 118.3(8) . . ?
C69 C74 C84 109.2(16) . . ?
C80 C74 C84 62.5(10) . . ?
C75 C74 C84 99.2(9) . . ?
C52 C74 C84 118.3(8) . . ?
O11 C52 O12 121.5(7) . . ?
O11 C52 C74 115.0(6) . . ?
O12 C52 C74 123.2(7) . . ?
C73 C79 C80 124.0(9) . . ?
C73 C79 C71 64.1(9) . . ?
C80 C79 C71 101.9(10) . . ?
C73 C79 C77 40.9(9) . . ?
C80 C79 C77 91.8(10) . . ?
C71 C79 C77 93.1(14) . . ?
C73 C79 C84 95.3(9) . . ?
C80 C79 C84 57.2(9) . . ?
C71 C79 C84 45.0(10) . . ?
C77 C79 C84 98.8(11) . . ?
C74 C80 C79 120.1(9) . . ?
C74 C80 C69 42.1(9) . . ?
C79 C80 C69 88.2(10) . . ?
C74 C80 C84 76.6(11) . . ?
C79 C80 C84 79.1(9) . . ?
C69 C80 C84 95.9(13) . . ?
C77 C76 C75 96.3(16) . . ?
C77 C76 C73 50.4(18) . . ?
C75 C76 C73 121.1(10) . . ?
C77 C76 C49 140.3(16) . . ?
C75 C76 C49 118.9(10) . . ?
C73 C76 C49 114.4(9) . . ?
C77 C76 C69 57.4(15) . . ?
C75 C76 C69 39.1(8) . . ?
C73 C76 C69 90.0(11) . . ?
C49 C76 C69 155.5(13) . . ?
C69 C75 C76 84.6(13) . . ?
C69 C75 C74 47.5(13) . . ?
C76 C75 C74 116.2(10) . . ?
C69 C75 C78 153.4(19) . . ?
C76 C75 C78 116.3(10) . . ?
C74 C75 C78 124.2(9) . . ?
C69 C75 C77 51.6(13) . . ?
C76 C75 C77 33.2(9) . . ?
C74 C75 C77 90.1(10) . . ?
C78 C75 C77 145.7(12) . . ?
C96 C78 C75 121.7(10) . . ?
C83 C49 C76 119.4(11) . . ?
C84 C71 C50 120(2) . . ?
C84 C71 C73 113(2) . . ?
C50 C71 C73 127.3(15) . . ?
C84 C71 C79 81.9(16) . . ?
C50 C71 C79 137.6(18) . . ?
C73 C71 C79 49.8(9) . . ?
C85 C72 C84 120.9(19) . . ?
C74 C69 C75 84.5(18) . . ?
C74 C69 C77 137(3) . . ?
C75 C69 C77 92.4(18) . . ?
C74 C69 C80 53.0(12) . . ?
C75 C69 C80 126(2) . . ?
C77 C69 C80 97.6(19) . . ?
C74 C69 C76 121(2) . . ?
C75 C69 C76 56.2(12) . . ?
C77 C69 C76 36.3(11) . . ?
C80 C69 C76 114.5(17) . . ?
C76 C77 C73 87(2) . . ?
C76 C77 C69 86.3(19) . . ?
C73 C77 C69 122(2) . . ?
C76 C77 C79 118(2) . . ?
C73 C77 C79 51.5(12) . . ?
C69 C77 C79 82.2(16) . . ?
C76 C77 C75 50.4(12) . . ?
C73 C77 C75 114.2(19) . . ?
C69 C77 C75 36.1(11) . . ?
C79 C77 C75 102.2(12) . . ?
C83 C96 C78 122.7(12) . . ?
C87 C85 C72 128(3) . . ?
C72 C84 C71 113(2) . . ?
C72 C84 C80 135.8(17) . . ?
C71 C84 C80 96.5(16) . . ?
C72 C84 C74 133.2(16) . . ?
C71 C84 C74 113.2(18) . . ?
C80 C84 C74 40.9(8) . . ?
C72 C84 C79 143.9(19) . . ?
C71 C84 C79 53.2(12) . . ?
C80 C84 C79 43.7(7) . . ?
C74 C84 C79 73.2(10) . . ?
C87 C50 C71 117.5(19) . . ?
C85 C87 C50 119(3) . . ?
C49 C83 C96 120.1(14) . . ?
_diffrn_measured_fraction_theta_max 0.989
_diffrn_reflns_theta_full        76.56
_diffrn_measured_fraction_theta_full 0.989
_refine_diff_density_max         1.632
_refine_diff_density_min         -1.054
_refine_diff_density_rms         0.125


data_a4
_database_code_depnum_ccdc_archive 'CCDC 910087'
#TrackingRef '(4) [Cd(NH2-BDC)(H2MDP)2].CIF'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H36 Cd N9 O4'
_chemical_formula_weight         699.08
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd 0.1185 4.6533 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   p2/c
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
_cell_length_a                   9.7163(4)
_cell_length_b                   9.3623(3)
_cell_length_c                   18.4041(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 105.392(4)
_cell_angle_gamma                90.00
_cell_volume                     1614.12(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?
_exptl_crystal_description       rod
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.438
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             718
_exptl_absorpt_coefficient_mu    5.823
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4754
_exptl_absorpt_correction_T_max  0.7595
_exptl_absorpt_process_details   ?
_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'superNova (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10701
_diffrn_reflns_av_R_equivalents  0.0283
_diffrn_reflns_av_sigmaI/netI    0.0254
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         4.72
_diffrn_reflns_theta_max         74.19
_reflns_number_total             3234
_reflns_number_gt                2956
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0375P)^2^+0.6220P] where P=(Fo^2^+2Fc^2^)/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         3234
_refine_ls_number_parameters     208
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0331
_refine_ls_R_factor_gt           0.0287
_refine_ls_wR_factor_ref         0.0738
_refine_ls_wR_factor_gt          0.0703
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_restrained_S_all      1.028
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cd1 Cd 0.0000 -0.35696(2) -0.2500 0.04279(9) Uani 1 2 d S . .
O1 O -0.20686(19) -0.3525(2) -0.35144(10) 0.0523(4) Uani 1 1 d . . .
O2 O -0.3910(2) -0.3752(2) -0.30224(11) 0.0644(5) Uani 1 1 d . . .
N4 N 0.2407(3) -1.1896(2) -0.30839(12) 0.0519(5) Uani 1 1 d . . .
H17 H 0.2968 -1.2572 -0.2869 0.062 Uiso 1 1 d R . .
N3 N 0.1012(3) -1.1813(2) -0.30955(11) 0.0475(5) Uani 1 1 d . . .
N6 N -0.5908(5) -0.5478(6) -0.3746(3) 0.0669(15) Uani 0.50 1 d P . .
H6A H -0.6666 -0.5977 -0.3780 0.080 Uiso 0.50 1 d PR . .
H6B H -0.5446 -0.5131 -0.3318 0.080 Uiso 0.50 1 d PR . .
N2 N -0.0458(3) -0.5498(2) -0.39394(12) 0.0528(5) Uani 1 1 d . . .
H11 H -0.1126 -0.4877 -0.4087 0.063 Uiso 1 1 d R . .
N1 N 0.0501(3) -0.5467(2) -0.32590(11) 0.0491(5) Uani 1 1 d . . .
C15 C -0.4230(3) -0.4434(3) -0.43014(13) 0.0456(5) Uani 1 1 d . . .
C14 C -0.3804(3) -0.4195(3) -0.49520(14) 0.0519(6) Uani 1 1 d . . .
H3 H -0.2995 -0.3644 -0.4922 0.062 Uiso 1 1 calc R . .
C13 C -0.5457(3) -0.5249(3) -0.43472(14) 0.0509(6) Uani 1 1 d . . .
C12 C -0.3354(3) -0.3850(3) -0.35516(14) 0.0482(6) Uani 1 1 d . . .
C11 C 0.0907(3) -0.7340(2) -0.39430(14) 0.0461(5) Uani 1 1 d . . .
C10 C -0.0256(3) -0.6608(3) -0.43631(14) 0.0508(6) Uani 1 1 d . . .
C9 C 0.1341(3) -0.6597(3) -0.32540(15) 0.0498(6) Uani 1 1 d . . .
C8 C 0.1557(4) -0.8643(3) -0.41992(16) 0.0555(7) Uani 1 1 d . . .
H14A H 0.2519 -0.8406 -0.4218 0.067 Uiso 1 1 calc R . .
H14B H 0.1012 -0.8872 -0.4708 0.067 Uiso 1 1 calc R . .
C7 C 0.1625(3) -0.9958(3) -0.37182(13) 0.0483(6) Uani 1 1 d . . .
C6 C 0.2814(3) -1.0799(3) -0.34489(14) 0.0520(6) Uani 1 1 d . . .
C5 C 0.0521(3) -1.0625(3) -0.34880(13) 0.0470(6) Uani 1 1 d . . .
C4 C -0.0998(4) -1.0181(3) -0.36253(18) 0.0617(7) Uani 1 1 d . . .
H20A H -0.1561 -1.0983 -0.3550 0.093 Uiso 1 1 calc R . .
H20B H -0.1345 -0.9841 -0.4133 0.093 Uiso 1 1 calc R . .
H20C H -0.1069 -0.9432 -0.3281 0.093 Uiso 1 1 calc R . .
C3 C 0.4286(4) -1.0672(4) -0.3538(2) 0.0750(9) Uani 1 1 d . . .
H21A H 0.4839 -1.1485 -0.3313 0.113 Uiso 1 1 calc R . .
H21B H 0.4722 -0.9816 -0.3294 0.113 Uiso 1 1 calc R . .
H21C H 0.4248 -1.0632 -0.4064 0.113 Uiso 1 1 calc R . .
C2 C 0.2508(5) -0.6969(4) -0.2580(2) 0.0851(12) Uani 1 1 d . . .
H22A H 0.3392 -0.6581 -0.2632 0.128 Uiso 1 1 calc R . .
H22B H 0.2587 -0.7989 -0.2533 0.128 Uiso 1 1 calc R . .
H22C H 0.2302 -0.6578 -0.2138 0.128 Uiso 1 1 calc R . .
C1 C -0.1239(4) -0.6879(4) -0.51273(18) 0.0792(10) Uani 1 1 d . . .
H23A H -0.2043 -0.7429 -0.5077 0.119 Uiso 1 1 calc R . .
H23B H -0.0740 -0.7397 -0.5429 0.119 Uiso 1 1 calc R . .
H23C H -0.1566 -0.5984 -0.5366 0.119 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cd1 0.06047(16) 0.03026(12) 0.03218(12) 0.000 0.00271(9) 0.000
O1 0.0504(10) 0.0507(10) 0.0474(10) -0.0076(8) -0.0019(8) -0.0002(8)
O2 0.0750(13) 0.0709(14) 0.0461(10) -0.0155(9) 0.0137(9) -0.0068(11)
N4 0.0664(14) 0.0395(11) 0.0432(11) 0.0053(9) 0.0028(10) 0.0052(10)
N3 0.0652(14) 0.0340(10) 0.0387(10) 0.0025(8) 0.0056(9) 0.0021(9)
N6 0.061(3) 0.096(4) 0.041(2) -0.001(2) 0.008(2) -0.032(3)
N2 0.0690(14) 0.0430(12) 0.0406(11) -0.0064(9) 0.0044(10) 0.0081(10)
N1 0.0697(14) 0.0374(11) 0.0363(10) -0.0043(8) 0.0072(9) 0.0020(9)
C15 0.0478(13) 0.0433(13) 0.0400(12) -0.0014(10) 0.0014(10) 0.0021(10)
C14 0.0496(14) 0.0571(15) 0.0431(13) 0.0014(11) 0.0021(10) -0.0089(12)
C13 0.0504(14) 0.0583(16) 0.0405(12) 0.0013(11) 0.0060(10) -0.0026(12)
C12 0.0579(15) 0.0384(13) 0.0421(13) -0.0031(10) 0.0025(11) 0.0036(11)
C11 0.0696(16) 0.0291(11) 0.0409(12) -0.0002(9) 0.0172(11) -0.0013(11)
C10 0.0738(17) 0.0392(13) 0.0373(12) -0.0051(10) 0.0112(11) -0.0018(12)
C9 0.0674(16) 0.0354(12) 0.0428(13) -0.0028(10) 0.0080(11) 0.0023(11)
C8 0.088(2) 0.0357(13) 0.0491(14) 0.0040(11) 0.0282(14) 0.0063(13)
C7 0.0751(17) 0.0319(12) 0.0376(12) -0.0033(9) 0.0142(11) 0.0018(11)
C6 0.0675(17) 0.0421(13) 0.0427(13) -0.0020(11) 0.0085(11) -0.0011(12)
C5 0.0705(16) 0.0325(12) 0.0358(11) 0.0010(9) 0.0103(10) 0.0034(11)
C4 0.077(2) 0.0479(15) 0.0624(17) 0.0126(13) 0.0222(14) 0.0082(14)
C3 0.073(2) 0.070(2) 0.082(2) 0.0147(18) 0.0204(17) 0.0065(17)
C2 0.106(3) 0.063(2) 0.0636(19) -0.0148(16) -0.0172(18) 0.023(2)
C1 0.105(3) 0.071(2) 0.0478(16) -0.0185(15) -0.0041(16) 0.0161(19)
_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 N3 2.333(2) 1_565 ?
Cd1 N3 2.333(2) 2_564 ?
Cd1 O1 2.3526(17) 2_554 ?
Cd1 O1 2.3526(17) . ?
Cd1 N1 2.389(2) . ?
Cd1 N1 2.389(2) 2_554 ?
O1 C12 1.269(3) . ?
O2 C12 1.237(3) . ?
N4 C6 1.342(4) . ?
N4 N3 1.352(3) . ?
N4 H17 0.8601 . ?
N3 C5 1.343(3) . ?
N3 Cd1 2.333(2) 1_545 ?
N6 C13 1.312(5) . ?
N6 H6A 0.8603 . ?
N6 H6B 0.8601 . ?
N2 C10 1.344(3) . ?
N2 N1 1.348(3) . ?
N2 H11 0.8600 . ?
N1 C9 1.335(3) . ?
C15 C14 1.385(4) . ?
C15 C13 1.399(4) . ?
C15 C12 1.518(3) . ?
C14 C13 1.399(4) 3_444 ?
C14 H3 0.9300 . ?
C13 C14 1.399(4) 3_444 ?
C11 C10 1.371(4) . ?
C11 C9 1.409(3) . ?
C11 C8 1.506(3) . ?
C10 C1 1.497(4) . ?
C9 C2 1.483(4) . ?
C8 C7 1.508(3) . ?
C8 H14A 0.9700 . ?
C8 H14B 0.9700 . ?
C7 C6 1.377(4) . ?
C7 C5 1.400(4) . ?
C6 C3 1.487(5) . ?
C5 C4 1.490(4) . ?
C4 H20A 0.9600 . ?
C4 H20B 0.9600 . ?
C4 H20C 0.9600 . ?
C3 H21A 0.9600 . ?
C3 H21B 0.9600 . ?
C3 H21C 0.9600 . ?
C2 H22A 0.9600 . ?
C2 H22B 0.9600 . ?
C2 H22C 0.9600 . ?
C1 H23A 0.9600 . ?
C1 H23B 0.9600 . ?
C1 H23C 0.9600 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3 Cd1 N3 90.39(11) 1_565 2_564 ?
N3 Cd1 O1 89.00(7) 1_565 2_554 ?
N3 Cd1 O1 89.57(7) 2_564 2_554 ?
N3 Cd1 O1 89.57(7) 1_565 . ?
N3 Cd1 O1 89.00(7) 2_564 . ?
O1 Cd1 O1 177.97(9) 2_554 . ?
N3 Cd1 N1 94.17(8) 1_565 . ?
N3 Cd1 N1 167.31(8) 2_564 . ?
O1 Cd1 N1 102.32(7) 2_554 . ?
O1 Cd1 N1 79.21(7) . . ?
N3 Cd1 N1 167.31(8) 1_565 2_554 ?
N3 Cd1 N1 94.17(8) 2_564 2_554 ?
O1 Cd1 N1 79.22(7) 2_554 2_554 ?
O1 Cd1 N1 102.32(7) . 2_554 ?
N1 Cd1 N1 83.88(10) . 2_554 ?
C12 O1 Cd1 131.27(17) . . ?
C6 N4 N3 112.1(2) . . ?
C6 N4 H17 123.9 . . ?
N3 N4 H17 124.0 . . ?
C5 N3 N4 105.5(2) . . ?
C5 N3 Cd1 134.6(2) . 1_545 ?
N4 N3 Cd1 119.88(15) . 1_545 ?
C13 N6 H6A 119.9 . . ?
C13 N6 H6B 120.0 . . ?
H6A N6 H6B 120.0 . . ?
C10 N2 N1 112.6(2) . . ?
C10 N2 H11 123.6 . . ?
N1 N2 H11 123.8 . . ?
C9 N1 N2 105.1(2) . . ?
C9 N1 Cd1 143.58(17) . . ?
N2 N1 Cd1 111.17(16) . . ?
C14 C15 C13 118.8(2) . . ?
C14 C15 C12 120.2(2) . . ?
C13 C15 C12 121.0(2) . . ?
C15 C14 C13 122.6(3) . 3_444 ?
C15 C14 H3 118.7 . . ?
C13 C14 H3 118.7 3_444 . ?
N6 C13 C15 120.6(3) . . ?
N6 C13 C14 120.8(3) . 3_444 ?
C15 C13 C14 118.6(2) . 3_444 ?
O2 C12 O1 124.7(2) . . ?
O2 C12 C15 119.1(2) . . ?
O1 C12 C15 116.2(2) . . ?
C10 C11 C9 105.4(2) . . ?
C10 C11 C8 125.4(2) . . ?
C9 C11 C8 129.2(3) . . ?
N2 C10 C11 106.6(2) . . ?
N2 C10 C1 121.4(3) . . ?
C11 C10 C1 132.0(3) . . ?
N1 C9 C11 110.4(2) . . ?
N1 C9 C2 121.5(2) . . ?
C11 C9 C2 128.1(3) . . ?
C11 C8 C7 115.7(2) . . ?
C11 C8 H14A 108.3 . . ?
C7 C8 H14A 108.3 . . ?
C11 C8 H14B 108.3 . . ?
C7 C8 H14B 108.3 . . ?
H14A C8 H14B 107.4 . . ?
C6 C7 C5 105.8(2) . . ?
C6 C7 C8 125.5(3) . . ?
C5 C7 C8 128.6(3) . . ?
N4 C6 C7 106.7(3) . . ?
N4 C6 C3 122.4(3) . . ?
C7 C6 C3 130.8(3) . . ?
N3 C5 C7 109.9(2) . . ?
N3 C5 C4 121.1(2) . . ?
C7 C5 C4 128.9(2) . . ?
C5 C4 H20A 109.5 . . ?
C5 C4 H20B 109.5 . . ?
H20A C4 H20B 109.5 . . ?
C5 C4 H20C 109.5 . . ?
H20A C4 H20C 109.5 . . ?
H20B C4 H20C 109.5 . . ?
C6 C3 H21A 109.5 . . ?
C6 C3 H21B 109.5 . . ?
H21A C3 H21B 109.5 . . ?
C6 C3 H21C 109.5 . . ?
H21A C3 H21C 109.5 . . ?
H21B C3 H21C 109.5 . . ?
C9 C2 H22A 109.5 . . ?
C9 C2 H22B 109.5 . . ?
H22A C2 H22B 109.5 . . ?
C9 C2 H22C 109.5 . . ?
H22A C2 H22C 109.5 . . ?
H22B C2 H22C 109.5 . . ?
C10 C1 H23A 109.5 . . ?
C10 C1 H23B 109.5 . . ?
H23A C1 H23B 109.5 . . ?
C10 C1 H23C 109.5 . . ?
H23A C1 H23C 109.5 . . ?
H23B C1 H23C 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
N3 Cd1 O1 C12 -154.8(2) 1_565 . . . ?
N3 Cd1 O1 C12 -64.4(2) 2_564 . . . ?
O1 Cd1 O1 C12 -109.6(2) 2_554 . . . ?
N1 Cd1 O1 C12 110.9(2) . . . . ?
N1 Cd1 O1 C12 29.7(2) 2_554 . . . ?
C6 N4 N3 C5 0.5(3) . . . . ?
C6 N4 N3 Cd1 -179.71(16) . . . 1_545 ?
C10 N2 N1 C9 0.2(3) . . . . ?
C10 N2 N1 Cd1 -176.22(19) . . . . ?
N3 Cd1 N1 C9 106.7(3) 1_565 . . . ?
N3 Cd1 N1 C9 -142.5(3) 2_564 . . . ?
O1 Cd1 N1 C9 16.8(3) 2_554 . . . ?
O1 Cd1 N1 C9 -164.6(3) . . . . ?
N1 Cd1 N1 C9 -60.7(3) 2_554 . . . ?
N3 Cd1 N1 N2 -79.19(18) 1_565 . . . ?
N3 Cd1 N1 N2 31.6(4) 2_564 . . . ?
O1 Cd1 N1 N2 -169.08(17) 2_554 . . . ?
O1 Cd1 N1 N2 9.58(17) . . . . ?
N1 Cd1 N1 N2 113.4(2) 2_554 . . . ?
C13 C15 C14 C13 -0.8(5) . . . 3_444 ?
C12 C15 C14 C13 177.7(3) . . . 3_444 ?
C14 C15 C13 N6 -178.8(4) . . . . ?
C12 C15 C13 N6 2.7(5) . . . . ?
C14 C15 C13 C14 0.8(5) . . . 3_444 ?
C12 C15 C13 C14 -177.7(3) . . . 3_444 ?
Cd1 O1 C12 O2 29.3(4) . . . . ?
Cd1 O1 C12 C15 -149.07(17) . . . . ?
C14 C15 C12 O2 161.9(3) . . . . ?
C13 C15 C12 O2 -19.6(4) . . . . ?
C14 C15 C12 O1 -19.7(4) . . . . ?
C13 C15 C12 O1 158.8(2) . . . . ?
N1 N2 C10 C11 -0.6(3) . . . . ?
N1 N2 C10 C1 177.4(3) . . . . ?
C9 C11 C10 N2 0.8(3) . . . . ?
C8 C11 C10 N2 -178.1(2) . . . . ?
C9 C11 C10 C1 -177.0(4) . . . . ?
C8 C11 C10 C1 4.2(5) . . . . ?
N2 N1 C9 C11 0.3(3) . . . . ?
Cd1 N1 C9 C11 174.7(2) . . . . ?
N2 N1 C9 C2 -177.5(3) . . . . ?
Cd1 N1 C9 C2 -3.1(5) . . . . ?
C10 C11 C9 N1 -0.7(3) . . . . ?
C8 C11 C9 N1 178.1(3) . . . . ?
C10 C11 C9 C2 176.9(4) . . . . ?
C8 C11 C9 C2 -4.3(5) . . . . ?
C10 C11 C8 C7 -122.0(3) . . . . ?
C9 C11 C8 C7 59.4(4) . . . . ?
C11 C8 C7 C6 -130.9(3) . . . . ?
C11 C8 C7 C5 53.0(4) . . . . ?
N3 N4 C6 C7 -0.4(3) . . . . ?
N3 N4 C6 C3 -177.9(3) . . . . ?
C5 C7 C6 N4 0.1(3) . . . . ?
C8 C7 C6 N4 -176.7(2) . . . . ?
C5 C7 C6 C3 177.4(3) . . . . ?
C8 C7 C6 C3 0.5(5) . . . . ?
N4 N3 C5 C7 -0.4(3) . . . . ?
Cd1 N3 C5 C7 179.85(16) 1_545 . . . ?
N4 N3 C5 C4 179.6(2) . . . . ?
Cd1 N3 C5 C4 -0.2(4) 1_545 . . . ?
C6 C7 C5 N3 0.2(3) . . . . ?
C8 C7 C5 N3 176.9(2) . . . . ?
C6 C7 C5 C4 -179.8(3) . . . . ?
C8 C7 C5 C4 -3.1(4) . . . . ?
_diffrn_measured_fraction_theta_max 0.984
_diffrn_reflns_theta_full        74.19
_diffrn_measured_fraction_theta_full 0.984
_refine_diff_density_max         0.994
_refine_diff_density_min         -0.471
_refine_diff_density_rms         0.055


data_a
_database_code_depnum_ccdc_archive 'CCDC 910088'
#TrackingRef '(5) [Cd(NH2-BDC)(H2MDP)2].CIF'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H34 Cd N9 O4'
_chemical_formula_weight         697.06
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd 0.1185 4.6533 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   c2/c
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
_cell_length_a                   29.2901(8)
_cell_length_b                   9.4068(3)
_cell_length_c                   17.3833(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 124.817(3)
_cell_angle_gamma                90.00
_cell_volume                     3932.1(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?
_exptl_crystal_description       lamellar
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.177
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1428
_exptl_absorpt_coefficient_mu    4.780
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4194
_exptl_absorpt_correction_T_max  0.4799
_exptl_absorpt_process_details   ?
_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'superNova (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            7685
_diffrn_reflns_av_R_equivalents  0.0413
_diffrn_reflns_av_sigmaI/netI    0.0400
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         5.05
_diffrn_reflns_theta_max         74.27
_reflns_number_total             3887
_reflns_number_gt                3572
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.1161P)^2^+0.6835P] where P=(Fo^2^+2Fc^2^)/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         3887
_refine_ls_number_parameters     204
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0552
_refine_ls_R_factor_gt           0.0510
_refine_ls_wR_factor_ref         0.1531
_refine_ls_wR_factor_gt          0.1458
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_restrained_S_all      1.040
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cd1 Cd 0.0000 0.29349(3) 0.2500 0.04176(16) Uani 1 2 d S . .
O2 O 0.13154(15) 0.2900(3) 0.2548(2) 0.0666(9) Uani 1 1 d . . .
O1 O 0.09969(11) 0.2955(3) 0.3448(2) 0.0556(8) Uani 1 1 d . . .
N5 N 0.2325(5) 0.2154(14) 0.3254(9) 0.103(4) Uani 0.50 1 d P . .
N2 N 0.07502(14) 0.1029(4) 0.4318(2) 0.0526(7) Uani 1 1 d . . .
H4A H 0.0997 0.1647 0.4427 0.063 Uiso 1 1 calc R . .
N1 N 0.02160(13) 0.1066(3) 0.3568(2) 0.0485(7) Uani 1 1 d . . .
N3 N -0.00238(13) -0.5278(3) 0.3405(2) 0.0489(7) Uani 1 1 d . . .
N4 N -0.04609(13) -0.5256(4) 0.3468(2) 0.0498(7) Uani 1 1 d . . .
H1B H -0.0718 -0.5890 0.3228 0.060 Uiso 1 1 calc R . .
C2 C -0.06318(19) -0.0344(5) 0.2958(4) 0.0694(12) Uani 1 1 d . . .
H15A H -0.0786 0.0360 0.2471 0.104 Uiso 1 1 calc R . .
H15B H -0.0823 -0.0315 0.3258 0.104 Uiso 1 1 calc R . .
H15C H -0.0674 -0.1269 0.2691 0.104 Uiso 1 1 calc R . .
C1 C 0.1420(2) -0.0384(7) 0.5740(3) 0.0838(15) Uani 1 1 d . . .
H14A H 0.1674 0.0329 0.5805 0.126 Uiso 1 1 calc R . .
H14B H 0.1543 -0.1303 0.5689 0.126 Uiso 1 1 calc R . .
H14C H 0.1407 -0.0366 0.6279 0.126 Uiso 1 1 calc R . .
C3 C -0.0895(2) -0.3871(6) 0.4097(4) 0.0710(12) Uani 1 1 d . . .
H13A H -0.1168 -0.4613 0.3796 0.106 Uiso 1 1 calc R . .
H13B H -0.1068 -0.2969 0.3832 0.106 Uiso 1 1 calc R . .
H13C H -0.0738 -0.3870 0.4756 0.106 Uiso 1 1 calc R . .
C4 C 0.0798(2) -0.3785(5) 0.3943(4) 0.0735(13) Uani 1 1 d . . .
H12A H 0.0859 -0.4485 0.3609 0.110 Uiso 1 1 calc R . .
H12B H 0.1106 -0.3786 0.4591 0.110 Uiso 1 1 calc R . .
H12C H 0.0764 -0.2863 0.3678 0.110 Uiso 1 1 calc R . .
C10 C 0.08517(18) -0.0094(4) 0.4877(3) 0.0573(10) Uani 1 1 d . . .
C5 C 0.02789(17) -0.4127(4) 0.3868(3) 0.0517(9) Uani 1 1 d . . .
C6 C -0.04453(17) -0.4119(4) 0.3952(3) 0.0515(8) Uani 1 1 d . . .
C13 C 0.23948(18) 0.2317(5) 0.4112(3) 0.0570(10) Uani 1 1 d . . .
C11 C 0.03554(18) -0.0806(4) 0.4480(3) 0.0514(8) Uani 1 1 d . . .
C15 C 0.19611(16) 0.2671(4) 0.4191(3) 0.0505(9) Uani 1 1 d . . .
C8 C 0.0244(3) -0.2097(4) 0.4864(3) 0.0612(12) Uani 1 1 d . . .
H5A H 0.0587 -0.2357 0.5452 0.073 Uiso 1 1 calc R . .
H5B H -0.0023 -0.1839 0.5000 0.073 Uiso 1 1 calc R . .
C9 C -0.00275(17) -0.0044(4) 0.3664(3) 0.0491(8) Uani 1 1 d . . .
C7 C 0.00291(18) -0.3381(4) 0.4237(3) 0.0505(8) Uani 1 1 d . . .
C12 C 0.13791(18) 0.2856(4) 0.3316(3) 0.0513(9) Uani 1 1 d . . .
C14 C 0.20673(18) 0.2850(4) 0.5067(3) 0.0542(10) Uani 1 1 d . . .
H1A H 0.1776 0.3087 0.5115 0.065 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cd1 0.0410(2) 0.0339(2) 0.0396(2) 0.000 0.01670(17) 0.000
O2 0.0533(18) 0.081(3) 0.0522(18) 0.0090(14) 0.0220(15) 0.0119(14)
O1 0.0340(14) 0.0563(18) 0.0572(17) 0.0073(11) 0.0146(13) 0.0001(10)
N5 0.074(7) 0.142(13) 0.076(7) -0.014(6) 0.033(6) 0.000(6)
N2 0.0518(16) 0.0446(16) 0.0466(15) 0.0024(13) 0.0194(13) -0.0028(14)
N1 0.0545(17) 0.0351(15) 0.0444(15) 0.0021(12) 0.0215(13) -0.0012(13)
N3 0.0521(17) 0.0395(16) 0.0495(16) -0.0061(13) 0.0257(14) -0.0008(13)
N4 0.0530(17) 0.0426(16) 0.0465(15) -0.0035(13) 0.0241(14) -0.0006(13)
C2 0.060(2) 0.057(2) 0.073(3) 0.011(2) 0.027(2) -0.006(2)
C1 0.073(3) 0.076(3) 0.059(3) 0.016(2) 0.012(2) 0.007(3)
C3 0.082(3) 0.068(3) 0.074(3) 0.002(2) 0.051(3) 0.009(2)
C4 0.077(3) 0.058(3) 0.090(3) -0.024(3) 0.050(3) -0.022(2)
C10 0.067(2) 0.043(2) 0.0420(18) 0.0012(15) 0.0198(17) 0.0020(18)
C5 0.060(2) 0.0379(18) 0.0464(19) -0.0056(15) 0.0237(17) -0.0027(16)
C6 0.065(2) 0.0404(18) 0.0445(17) 0.0048(15) 0.0285(17) 0.0051(16)
C13 0.043(2) 0.066(3) 0.049(2) 0.0014(19) 0.0190(18) 0.0036(18)
C11 0.071(2) 0.0358(17) 0.0419(17) -0.0029(14) 0.0294(17) 0.0001(16)
C15 0.0363(18) 0.0452(19) 0.050(2) 0.0031(16) 0.0126(15) -0.0004(15)
C8 0.099(4) 0.036(2) 0.045(2) -0.0046(14) 0.039(2) -0.0076(18)
C9 0.061(2) 0.0347(17) 0.0476(18) 0.0004(14) 0.0289(17) -0.0018(16)
C7 0.070(2) 0.0330(16) 0.0437(18) 0.0015(15) 0.0294(18) 0.0016(17)
C12 0.043(2) 0.043(2) 0.049(2) 0.0048(14) 0.0145(17) 0.0019(14)
C14 0.0370(19) 0.061(3) 0.053(2) 0.0027(17) 0.0188(17) 0.0048(15)
_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 N3 2.330(3) 2_565 ?
Cd1 N3 2.330(3) 1_565 ?
Cd1 N1 2.365(3) 2 ?
Cd1 N1 2.365(3) . ?
Cd1 O1 2.397(3) . ?
Cd1 O1 2.397(3) 2 ?
O2 C12 1.238(6) . ?
O1 C12 1.269(6) . ?
N5 C13 1.394(14) . ?
N2 C10 1.348(5) . ?
N2 N1 1.349(4) . ?
N2 H4A 0.8600 . ?
N1 C9 1.328(5) . ?
N3 C5 1.339(5) . ?
N3 N4 1.346(4) . ?
N3 Cd1 2.330(3) 1_545 ?
N4 C6 1.345(5) . ?
N4 H1B 0.8600 . ?
C2 C9 1.496(6) . ?
C2 H15A 0.9600 . ?
C2 H15B 0.9600 . ?
C2 H15C 0.9600 . ?
C1 C10 1.497(6) . ?
C1 H14A 0.9600 . ?
C1 H14B 0.9600 . ?
C1 H14C 0.9600 . ?
C3 C6 1.494(6) . ?
C3 H13A 0.9600 . ?
C3 H13B 0.9600 . ?
C3 H13C 0.9600 . ?
C4 C5 1.484(6) . ?
C4 H12A 0.9600 . ?
C4 H12B 0.9600 . ?
C4 H12C 0.9600 . ?
C10 C11 1.376(6) . ?
C5 C7 1.405(6) . ?
C6 C7 1.368(6) . ?
C13 C15 1.394(6) . ?
C13 C14 1.406(6) 7_556 ?
C11 C9 1.403(5) . ?
C11 C8 1.508(5) . ?
C15 C14 1.380(7) . ?
C15 C12 1.513(5) . ?
C8 C7 1.503(5) . ?
C8 H5A 0.9700 . ?
C8 H5B 0.9700 . ?
C14 C13 1.406(6) 7_556 ?
C14 H1A 0.9300 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3 Cd1 N3 87.66(16) 2_565 1_565 ?
N3 Cd1 N1 95.98(12) 2_565 2 ?
N3 Cd1 N1 165.50(11) 1_565 2 ?
N3 Cd1 N1 165.50(11) 2_565 . ?
N3 Cd1 N1 95.98(12) 1_565 . ?
N1 Cd1 N1 83.99(15) 2 . ?
N3 Cd1 O1 87.95(10) 2_565 . ?
N3 Cd1 O1 91.40(11) 1_565 . ?
N1 Cd1 O1 102.73(11) 2 . ?
N1 Cd1 O1 77.95(10) . . ?
N3 Cd1 O1 91.40(11) 2_565 2 ?
N3 Cd1 O1 87.95(10) 1_565 2 ?
N1 Cd1 O1 77.95(10) 2 2 ?
N1 Cd1 O1 102.73(11) . 2 ?
O1 Cd1 O1 179.10(13) . 2 ?
C12 O1 Cd1 136.8(3) . . ?
C10 N2 N1 112.0(3) . . ?
C10 N2 H4A 124.0 . . ?
N1 N2 H4A 124.0 . . ?
C9 N1 N2 105.5(3) . . ?
C9 N1 Cd1 139.5(3) . . ?
N2 N1 Cd1 114.9(2) . . ?
C5 N3 N4 105.8(3) . . ?
C5 N3 Cd1 136.4(3) . 1_545 ?
N4 N3 Cd1 117.6(2) . 1_545 ?
C6 N4 N3 111.7(3) . . ?
C6 N4 H1B 124.2 . . ?
N3 N4 H1B 124.2 . . ?
C9 C2 H15A 109.5 . . ?
C9 C2 H15B 109.5 . . ?
H15A C2 H15B 109.5 . . ?
C9 C2 H15C 109.5 . . ?
H15A C2 H15C 109.5 . . ?
H15B C2 H15C 109.5 . . ?
C10 C1 H14A 109.5 . . ?
C10 C1 H14B 109.5 . . ?
H14A C1 H14B 109.5 . . ?
C10 C1 H14C 109.5 . . ?
H14A C1 H14C 109.5 . . ?
H14B C1 H14C 109.5 . . ?
C6 C3 H13A 109.5 . . ?
C6 C3 H13B 109.5 . . ?
H13A C3 H13B 109.5 . . ?
C6 C3 H13C 109.5 . . ?
H13A C3 H13C 109.5 . . ?
H13B C3 H13C 109.5 . . ?
C5 C4 H12A 109.5 . . ?
C5 C4 H12B 109.5 . . ?
H12A C4 H12B 109.5 . . ?
C5 C4 H12C 109.5 . . ?
H12A C4 H12C 109.5 . . ?
H12B C4 H12C 109.5 . . ?
N2 C10 C11 106.5(3) . . ?
N2 C10 C1 121.8(4) . . ?
C11 C10 C1 131.7(4) . . ?
N3 C5 C7 109.8(4) . . ?
N3 C5 C4 121.4(4) . . ?
C7 C5 C4 128.7(4) . . ?
N4 C6 C7 107.1(4) . . ?
N4 C6 C3 120.8(4) . . ?
C7 C6 C3 132.1(4) . . ?
C15 C13 C14 118.8(4) . 7_556 ?
C15 C13 N5 123.2(6) . . ?
C14 C13 N5 117.9(6) 7_556 . ?
C10 C11 C9 105.3(3) . . ?
C10 C11 C8 127.1(4) . . ?
C9 C11 C8 127.5(4) . . ?
C14 C15 C13 119.6(4) . . ?
C14 C15 C12 120.7(4) . . ?
C13 C15 C12 119.7(4) . . ?
C7 C8 C11 115.7(4) . . ?
C7 C8 H5A 108.3 . . ?
C11 C8 H5A 108.3 . . ?
C7 C8 H5B 108.3 . . ?
C11 C8 H5B 108.3 . . ?
H5A C8 H5B 107.4 . . ?
N1 C9 C11 110.6(4) . . ?
N1 C9 C2 120.9(4) . . ?
C11 C9 C2 128.5(4) . . ?
C6 C7 C5 105.5(3) . . ?
C6 C7 C8 126.1(4) . . ?
C5 C7 C8 128.3(4) . . ?
O2 C12 O1 126.0(4) . . ?
O2 C12 C15 118.5(4) . . ?
O1 C12 C15 115.5(4) . . ?
C15 C14 C13 121.5(4) . 7_556 ?
C15 C14 H1A 119.2 . . ?
C13 C14 H1A 119.2 7_556 . ?
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
N3 Cd1 O1 C12 -52.8(3) 2_565 . . . ?
N3 Cd1 O1 C12 -140.4(3) 1_565 . . . ?
N1 Cd1 O1 C12 42.9(4) 2 . . . ?
N1 Cd1 O1 C12 123.8(4) . . . . ?
O1 Cd1 O1 C12 -96.6(3) 2 . . . ?
C10 N2 N1 C9 1.1(4) . . . . ?
C10 N2 N1 Cd1 -177.3(3) . . . . ?
N3 Cd1 N1 C9 -150.0(5) 2_565 . . . ?
N3 Cd1 N1 C9 106.0(4) 1_565 . . . ?
N1 Cd1 N1 C9 -59.4(4) 2 . . . ?
O1 Cd1 N1 C9 -163.8(4) . . . . ?
O1 Cd1 N1 C9 16.8(4) 2 . . . ?
N3 Cd1 N1 N2 27.6(6) 2_565 . . . ?
N3 Cd1 N1 N2 -76.4(3) 1_565 . . . ?
N1 Cd1 N1 N2 118.2(3) 2 . . . ?
O1 Cd1 N1 N2 13.8(2) . . . . ?
O1 Cd1 N1 N2 -165.6(2) 2 . . . ?
C5 N3 N4 C6 0.4(4) . . . . ?
Cd1 N3 N4 C6 -175.5(2) 1_545 . . . ?
N1 N2 C10 C11 -1.3(5) . . . . ?
N1 N2 C10 C1 178.2(4) . . . . ?
N4 N3 C5 C7 0.8(4) . . . . ?
Cd1 N3 C5 C7 175.5(3) 1_545 . . . ?
N4 N3 C5 C4 -179.5(4) . . . . ?
Cd1 N3 C5 C4 -4.7(6) 1_545 . . . ?
N3 N4 C6 C7 -1.4(4) . . . . ?
N3 N4 C6 C3 179.2(4) . . . . ?
N2 C10 C11 C9 1.0(4) . . . . ?
C1 C10 C11 C9 -178.4(5) . . . . ?
N2 C10 C11 C8 -177.0(4) . . . . ?
C1 C10 C11 C8 3.6(8) . . . . ?
C14 C13 C15 C14 0.0(7) 7_556 . . . ?
N5 C13 C15 C14 -178.2(8) . . . . ?
C14 C13 C15 C12 180.0(4) 7_556 . . . ?
N5 C13 C15 C12 1.7(10) . . . . ?
C10 C11 C8 C7 -121.8(5) . . . . ?
C9 C11 C8 C7 60.7(6) . . . . ?
N2 N1 C9 C11 -0.4(4) . . . . ?
Cd1 N1 C9 C11 177.3(3) . . . . ?
N2 N1 C9 C2 179.4(4) . . . . ?
Cd1 N1 C9 C2 -2.9(6) . . . . ?
C10 C11 C9 N1 -0.4(5) . . . . ?
C8 C11 C9 N1 177.6(4) . . . . ?
C10 C11 C9 C2 179.9(4) . . . . ?
C8 C11 C9 C2 -2.2(7) . . . . ?
N4 C6 C7 C5 1.8(4) . . . . ?
C3 C6 C7 C5 -178.9(4) . . . . ?
N4 C6 C7 C8 -174.8(4) . . . . ?
C3 C6 C7 C8 4.5(7) . . . . ?
N3 C5 C7 C6 -1.6(4) . . . . ?
C4 C5 C7 C6 178.7(5) . . . . ?
N3 C5 C7 C8 174.9(4) . . . . ?
C4 C5 C7 C8 -4.8(7) . . . . ?
C11 C8 C7 C6 -125.6(5) . . . . ?
C11 C8 C7 C5 58.5(7) . . . . ?
Cd1 O1 C12 O2 10.6(6) . . . . ?
Cd1 O1 C12 C15 -169.5(2) . . . . ?
C14 C15 C12 O2 169.2(4) . . . . ?
C13 C15 C12 O2 -10.7(6) . . . . ?
C14 C15 C12 O1 -10.7(6) . . . . ?
C13 C15 C12 O1 169.3(4) . . . . ?
C13 C15 C14 C13 0.0(8) . . . 7_556 ?
C12 C15 C14 C13 -180.0(4) . . . 7_556 ?
_diffrn_measured_fraction_theta_max 0.969
_diffrn_reflns_theta_full        74.27
_diffrn_measured_fraction_theta_full 0.969
_refine_diff_density_max         1.246
_refine_diff_density_min         -0.784
_refine_diff_density_rms         0.132


data_a6
_database_code_depnum_ccdc_archive 'CCDC 910089'
#TrackingRef '(6)[Cd(H2MDP)(Br-BDC)0.5(Br-HBDC)].CIF'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C23 H20 Br3 Cd Co0 Ho0 N4 O6'
_chemical_formula_weight         800.56
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co -2.3653 3.6143 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ho Ho -14.9734 3.7046 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd 0.1185 4.6533 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   p-1
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a                   10.1726(6)
_cell_length_b                   11.8494(7)
_cell_length_c                   13.6326(8)
_cell_angle_alpha                68.340(6)
_cell_angle_beta                 70.388(6)
_cell_angle_gamma                68.920(5)
_cell_volume                     1385.48(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?
_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.919
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             774
_exptl_absorpt_coefficient_mu    11.764
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.2019
_exptl_absorpt_correction_T_max  0.2547
_exptl_absorpt_process_details   ?
_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'superNova (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            9436
_diffrn_reflns_av_R_equivalents  0.0444
_diffrn_reflns_av_sigmaI/netI    0.0409
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         3.59
_diffrn_reflns_theta_max         74.41
_reflns_number_total             5433
_reflns_number_gt                4910
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.1026P)^2^+1.1915P] where P=(Fo^2^+2Fc^2^)/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         5433
_refine_ls_number_parameters     338
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0541
_refine_ls_R_factor_gt           0.0499
_refine_ls_wR_factor_ref         0.1422
_refine_ls_wR_factor_gt          0.1362
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_restrained_S_all      1.016
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cd1 Cd 0.41187(3) 0.68683(3) 0.57534(2) 0.02287(13) Uani 1 1 d . . .
Br1 Br -0.13769(6) 0.56068(7) 0.83532(5) 0.04834(19) Uani 1 1 d . . .
Br3 Br 0.46321(11) 0.80179(6) 0.89077(6) 0.0646(3) Uani 1 1 d . . .
Br2 Br 0.49052(8) 0.13981(7) 0.83501(5) 0.0566(2) Uani 1 1 d . . .
O6 O 0.3378(4) 0.6387(3) 0.7663(3) 0.0321(8) Uani 1 1 d . . .
O2 O 0.4188(4) 0.3133(3) 0.5791(3) 0.0355(8) Uani 1 1 d . . .
O5 O 0.5691(4) 0.6211(4) 0.6988(3) 0.0400(9) Uani 1 1 d . . .
N26 N 0.3342(5) 0.8888(4) 0.5862(3) 0.0335(9) Uani 1 1 d . . .
O1 O 0.4684(4) 0.4551(3) 0.6227(3) 0.0338(8) Uani 1 1 d . . .
O4 O -0.1328(5) 0.4101(4) 1.0647(3) 0.0495(11) Uani 1 1 d . . .
H4A H -0.1971 0.3926 1.1185 0.074 Uiso 1 1 calc R . .
N2 N 0.2138(4) 0.7032(4) 0.5226(3) 0.0292(8) Uani 1 1 d . . .
N1 N 0.2332(5) 0.6376(4) 0.4536(4) 0.0308(9) Uani 1 1 d . . .
H31 H 0.3160 0.5937 0.4258 0.037 Uiso 1 1 calc R . .
C6 C 0.4830(6) 0.6263(4) 0.9529(4) 0.0326(11) Uani 1 1 d . . .
C27 C 0.3106(5) 1.0008(5) 0.5109(4) 0.0278(10) Uani 1 1 d . . .
N25 N 0.2568(5) 0.9149(4) 0.6814(4) 0.0353(10) Uani 1 1 d . . .
H25 H 0.2534 0.8592 0.7436 0.042 Uiso 1 1 calc R . .
C8 C 0.4661(5) 0.6090(4) 0.7761(4) 0.0277(10) Uani 1 1 d . . .
C14 C 0.2849(5) 0.3599(5) 0.7432(4) 0.0264(9) Uani 1 1 d . . .
C5 C 0.4856(5) 0.5539(5) 0.8920(4) 0.0284(10) Uani 1 1 d . . .
C23 C 0.2166(5) 1.0962(4) 0.5577(4) 0.0263(9) Uani 1 1 d . . .
C15 C 0.1505(5) 0.4474(5) 0.7479(4) 0.0293(10) Uani 1 1 d . . .
H15 H 0.1337 0.5156 0.6874 0.035 Uiso 1 1 calc R . .
C29 C 0.0001(5) 0.7253(4) 0.4925(4) 0.0263(9) Uani 1 1 d . . .
C16 C 0.0395(6) 0.4347(5) 0.8423(4) 0.0312(10) Uani 1 1 d . . .
C20 C 0.4001(5) 0.3780(4) 0.6392(4) 0.0260(9) Uani 1 1 d . . .
C7 C 0.5035(6) 0.4264(5) 0.9407(4) 0.0361(11) Uani 1 1 d . . .
H7 H 0.5065 0.3753 0.9017 0.043 Uiso 1 1 calc R . .
C33 C 0.0716(5) 0.7578(4) 0.5470(4) 0.0270(9) Uani 1 1 d . . .
C24 C 0.1856(6) 1.0381(5) 0.6677(4) 0.0338(11) Uani 1 1 d . . .
C30 C 0.1079(6) 0.6494(5) 0.4338(4) 0.0311(10) Uani 1 1 d . . .
C11 C 0.0620(6) 0.3324(5) 0.9329(4) 0.0338(11) Uani 1 1 d . . .
C28 C -0.1600(5) 0.7660(4) 0.4984(4) 0.0311(10) Uani 1 1 d . . .
H28A H -0.2117 0.7487 0.5741 0.037 Uiso 1 1 calc R . .
H28B H -0.1805 0.7157 0.4659 0.037 Uiso 1 1 calc R . .
C34 C 0.0078(6) 0.8373(6) 0.6233(5) 0.0394(12) Uani 1 1 d . . .
H34A H 0.0662 0.8088 0.6749 0.059 Uiso 1 1 calc R . .
H34B H -0.0888 0.8305 0.6610 0.059 Uiso 1 1 calc R . .
H34C H 0.0047 0.9236 0.5833 0.059 Uiso 1 1 calc R . .
C36 C 0.3846(7) 1.0084(5) 0.3947(5) 0.0410(13) Uani 1 1 d . . .
H36A H 0.4043 1.0891 0.3585 0.049 Uiso 1 1 calc R . .
H36B H 0.3231 0.9980 0.3603 0.049 Uiso 1 1 calc R . .
H36C H 0.4740 0.9430 0.3905 0.049 Uiso 1 1 calc R . .
C12 C 0.1959(7) 0.2450(5) 0.9282(4) 0.0391(12) Uani 1 1 d . . .
H12 H 0.2124 0.1761 0.9882 0.047 Uiso 1 1 calc R . .
C13 C 0.3065(6) 0.2589(5) 0.8345(4) 0.0344(11) Uani 1 1 d . . .
O3 O -0.0560(8) 0.2043(5) 1.0924(4) 0.087(2) Uani 1 1 d . . .
C17 C -0.0502(7) 0.3080(6) 1.0385(4) 0.0418(13) Uani 1 1 d . . .
C35 C 0.1031(7) 0.5857(6) 0.3590(6) 0.0471(14) Uani 1 1 d . . .
H35A H 0.1311 0.6339 0.2852 0.071 Uiso 1 1 calc R . .
H35B H 0.0065 0.5796 0.3733 0.071 Uiso 1 1 calc R . .
H35C H 0.1687 0.5027 0.3707 0.071 Uiso 1 1 calc R . .
C37 C 0.0934(8) 1.0874(6) 0.7623(5) 0.0543(17) Uani 1 1 d . . .
H37A H -0.0069 1.1070 0.7629 0.082 Uiso 1 1 calc R . .
H37B H 0.1156 1.1622 0.7564 0.082 Uiso 1 1 calc R . .
H37C H 0.1125 1.0246 0.8284 0.082 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cd1 0.0257(2) 0.02326(18) 0.01150(18) -0.00040(12) -0.00638(12) -0.00017(13)
Br1 0.0321(3) 0.0616(4) 0.0326(3) -0.0118(3) -0.0013(2) 0.0011(3)
Br3 0.1261(7) 0.0306(3) 0.0389(4) 0.0105(3) -0.0421(4) -0.0229(4)
Br2 0.0544(4) 0.0510(4) 0.0341(3) -0.0053(3) -0.0104(3) 0.0134(3)
O6 0.0285(18) 0.043(2) 0.0114(14) -0.0013(14) -0.0048(13) -0.0013(15)
O2 0.046(2) 0.0380(19) 0.0196(17) -0.0089(15) 0.0020(15) -0.0155(17)
O5 0.0321(19) 0.057(2) 0.0173(17) 0.0026(16) -0.0060(14) -0.0103(18)
N26 0.039(2) 0.029(2) 0.023(2) -0.0020(17) -0.0126(18) 0.0000(18)
O1 0.0281(18) 0.0313(17) 0.0317(19) -0.0066(15) 0.0025(14) -0.0077(14)
O4 0.055(3) 0.055(3) 0.028(2) -0.0143(19) 0.0160(18) -0.023(2)
N2 0.028(2) 0.030(2) 0.025(2) -0.0051(16) -0.0109(16) -0.0008(16)
N1 0.024(2) 0.030(2) 0.033(2) -0.0110(17) -0.0062(17) 0.0003(16)
C6 0.043(3) 0.021(2) 0.022(2) 0.0060(18) -0.013(2) -0.003(2)
C27 0.028(2) 0.028(2) 0.023(2) -0.0016(18) -0.0103(19) -0.0049(19)
N25 0.048(3) 0.025(2) 0.024(2) -0.0015(16) -0.0158(19) 0.0015(18)
C8 0.034(3) 0.028(2) 0.011(2) 0.0023(17) -0.0071(18) -0.0024(19)
C14 0.028(2) 0.031(2) 0.018(2) -0.0073(18) -0.0014(18) -0.0089(19)
C5 0.033(3) 0.033(2) 0.0112(19) 0.0038(17) -0.0075(18) -0.008(2)
C23 0.026(2) 0.020(2) 0.028(2) -0.0023(18) -0.0113(19) -0.0011(17)
C15 0.030(2) 0.033(2) 0.017(2) -0.0030(18) -0.0010(18) -0.008(2)
C29 0.029(2) 0.0182(19) 0.025(2) 0.0010(17) -0.0103(19) -0.0025(17)
C16 0.030(2) 0.036(3) 0.023(2) -0.007(2) -0.0014(19) -0.009(2)
C20 0.027(2) 0.025(2) 0.014(2) 0.0012(17) -0.0018(17) -0.0036(18)
C7 0.051(3) 0.035(3) 0.019(2) -0.001(2) -0.014(2) -0.009(2)
C33 0.032(2) 0.022(2) 0.020(2) 0.0003(17) -0.0073(18) -0.0053(18)
C24 0.039(3) 0.025(2) 0.034(3) -0.008(2) -0.015(2) 0.002(2)
C30 0.029(2) 0.024(2) 0.034(3) -0.004(2) -0.012(2) -0.0002(19)
C11 0.037(3) 0.038(3) 0.020(2) -0.007(2) 0.003(2) -0.013(2)
C28 0.029(2) 0.020(2) 0.037(3) -0.0006(19) -0.011(2) -0.0014(18)
C34 0.036(3) 0.046(3) 0.033(3) -0.017(2) -0.006(2) -0.002(2)
C36 0.042(3) 0.037(3) 0.028(3) -0.005(2) -0.001(2) -0.004(2)
C12 0.052(3) 0.032(3) 0.018(2) 0.000(2) 0.001(2) -0.010(2)
C13 0.038(3) 0.033(3) 0.019(2) -0.004(2) -0.002(2) -0.003(2)
O3 0.107(5) 0.051(3) 0.047(3) -0.002(2) 0.039(3) -0.023(3)
C17 0.051(3) 0.048(3) 0.017(2) -0.004(2) 0.006(2) -0.021(3)
C35 0.044(3) 0.043(3) 0.057(4) -0.028(3) -0.022(3) 0.007(3)
C37 0.068(4) 0.040(3) 0.038(3) -0.013(3) -0.007(3) 0.002(3)
_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 O2 2.228(4) 2_666 ?
Cd1 N26 2.279(4) . ?
Cd1 N2 2.281(4) . ?
Cd1 O6 2.359(3) . ?
Cd1 O5 2.437(4) . ?
Cd1 O1 2.468(4) . ?
Cd1 C8 2.726(4) . ?
Br1 C16 1.887(5) . ?
Br3 C6 1.897(5) . ?
Br2 C13 1.897(5) . ?
O6 C8 1.264(6) . ?
O2 C20 1.245(6) . ?
O2 Cd1 2.228(3) 2_666 ?
O5 C8 1.219(6) . ?
N26 C27 1.343(6) . ?
N26 N25 1.354(6) . ?
O1 C20 1.253(6) . ?
O4 C17 1.297(7) . ?
N2 C33 1.335(6) . ?
N2 N1 1.354(6) . ?
N1 C30 1.339(7) . ?
C6 C7 1.384(7) 2_667 ?
C6 C5 1.385(7) . ?
C27 C23 1.395(7) . ?
C27 C36 1.492(7) . ?
N25 C24 1.349(6) . ?
C8 C5 1.522(6) . ?
C14 C15 1.386(7) . ?
C14 C13 1.388(7) . ?
C14 C20 1.506(6) . ?
C5 C7 1.378(7) . ?
C23 C24 1.378(7) . ?
C23 C28 1.511(6) 2_576 ?
C15 C16 1.399(7) . ?
C29 C30 1.372(7) . ?
C29 C33 1.417(7) . ?
C29 C28 1.505(7) . ?
C16 C11 1.391(7) . ?
C7 C6 1.384(7) 2_667 ?
C33 C34 1.490(7) . ?
C24 C37 1.495(8) . ?
C30 C35 1.497(8) . ?
C11 C12 1.381(8) . ?
C11 C17 1.512(7) . ?
C28 C23 1.511(6) 2_576 ?
C12 C13 1.392(7) . ?
O3 C17 1.188(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
O2 Cd1 N26 106.10(15) 2_666 . ?
O2 Cd1 N2 101.08(15) 2_666 . ?
N26 Cd1 N2 94.13(15) . . ?
O2 Cd1 O6 152.23(14) 2_666 . ?
N26 Cd1 O6 82.85(14) . . ?
N2 Cd1 O6 104.46(14) . . ?
O2 Cd1 O5 98.72(13) 2_666 . ?
N26 Cd1 O5 92.09(15) . . ?
N2 Cd1 O5 156.68(14) . . ?
O6 Cd1 O5 54.11(12) . . ?
O2 Cd1 O1 89.66(13) 2_666 . ?
N26 Cd1 O1 162.87(14) . . ?
N2 Cd1 O1 89.24(14) . . ?
O6 Cd1 O1 80.05(13) . . ?
O5 Cd1 O1 78.65(14) . . ?
O2 Cd1 C8 124.90(15) 2_666 . ?
N26 Cd1 C8 88.44(15) . . ?
N2 Cd1 C8 131.21(15) . . ?
O6 Cd1 C8 27.60(14) . . ?
O5 Cd1 C8 26.55(13) . . ?
O1 Cd1 C8 76.81(14) . . ?
C8 O6 Cd1 92.6(3) . . ?
C20 O2 Cd1 124.4(3) . 2_666 ?
C8 O5 Cd1 90.1(3) . . ?
C27 N26 N25 104.3(4) . . ?
C27 N26 Cd1 132.2(3) . . ?
N25 N26 Cd1 120.5(3) . . ?
C20 O1 Cd1 135.4(3) . . ?
C33 N2 N1 105.8(4) . . ?
C33 N2 Cd1 136.4(3) . . ?
N1 N2 Cd1 117.6(3) . . ?
C30 N1 N2 111.7(4) . . ?
C7 C6 C5 121.7(5) 2_667 . ?
C7 C6 Br3 118.1(4) 2_667 . ?
C5 C6 Br3 120.3(4) . . ?
N26 C27 C23 111.4(4) . . ?
N26 C27 C36 119.1(5) . . ?
C23 C27 C36 129.5(4) . . ?
C24 N25 N26 112.5(4) . . ?
O5 C8 O6 123.0(4) . . ?
O5 C8 C5 121.4(4) . . ?
O6 C8 C5 115.6(4) . . ?
O5 C8 Cd1 63.4(3) . . ?
O6 C8 Cd1 59.8(2) . . ?
C5 C8 Cd1 172.9(3) . . ?
C15 C14 C13 118.2(4) . . ?
C15 C14 C20 118.7(4) . . ?
C13 C14 C20 123.1(4) . . ?
C7 C5 C6 117.7(4) . . ?
C7 C5 C8 119.1(5) . . ?
C6 C5 C8 123.2(4) . . ?
C24 C23 C27 105.2(4) . . ?
C24 C23 C28 126.7(5) . 2_576 ?
C27 C23 C28 128.1(5) . 2_576 ?
C14 C15 C16 120.9(5) . . ?
C30 C29 C33 105.2(4) . . ?
C30 C29 C28 127.9(5) . . ?
C33 C29 C28 126.9(5) . . ?
C11 C16 C15 120.3(5) . . ?
C11 C16 Br1 123.8(4) . . ?
C15 C16 Br1 115.8(4) . . ?
O2 C20 O1 126.7(4) . . ?
O2 C20 C14 116.4(4) . . ?
O1 C20 C14 116.8(4) . . ?
C5 C7 C6 120.7(5) . 2_667 ?
N2 C33 C29 109.8(4) . . ?
N2 C33 C34 121.5(4) . . ?
C29 C33 C34 128.6(5) . . ?
N25 C24 C23 106.6(5) . . ?
N25 C24 C37 121.3(5) . . ?
C23 C24 C37 132.1(5) . . ?
N1 C30 C29 107.4(5) . . ?
N1 C30 C35 121.2(5) . . ?
C29 C30 C35 131.4(5) . . ?
C12 C11 C16 118.8(5) . . ?
C12 C11 C17 116.3(5) . . ?
C16 C11 C17 124.9(5) . . ?
C29 C28 C23 113.9(4) . 2_576 ?
C11 C12 C13 120.7(5) . . ?
C14 C13 C12 121.0(5) . . ?
C14 C13 Br2 120.2(4) . . ?
C12 C13 Br2 118.7(4) . . ?
O3 C17 O4 124.7(5) . . ?
O3 C17 C11 121.9(6) . . ?
O4 C17 C11 113.3(5) . . ?
_diffrn_measured_fraction_theta_max 0.960
_diffrn_reflns_theta_full        74.41
_diffrn_measured_fraction_theta_full 0.960
_refine_diff_density_max         1.238
_refine_diff_density_min         -1.892
_refine_diff_density_rms         0.169


data_a1
_database_code_depnum_ccdc_archive 'CCDC 910090'
#TrackingRef '(7)____ [Co[(H2MDP)].(Br-BDC)].0.5H2O.CIF'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C19 H19 Br2 Co N4 O4.50'
_chemical_formula_weight         594.13
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co -2.3653 3.6143 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   c2/c
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
_cell_length_a                   19.639(3)
_cell_length_b                   13.6527(10)
_cell_length_c                   19.0257(14)
_cell_angle_alpha                90.00
_cell_angle_beta                 119.568(7)
_cell_angle_gamma                90.00
_cell_volume                     4436.9(8)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?
_exptl_crystal_description       block
_exptl_crystal_colour            purple
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.779
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2352
_exptl_absorpt_coefficient_mu    10.598
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.2993
_exptl_absorpt_correction_T_max  0.3628
_exptl_absorpt_process_details   ?
_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'superNova (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            8551
_diffrn_reflns_av_R_equivalents  0.0404
_diffrn_reflns_av_sigmaI/netI    0.0524
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         4.15
_diffrn_reflns_theta_max         72.07
_reflns_number_total             4305
_reflns_number_gt                2960
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0750P)^2^+22.0000P] where P=(Fo^2^+2Fc^2^)/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         4305
_refine_ls_number_parameters     336
_refine_ls_number_restraints     117
_refine_ls_R_factor_all          0.0960
_refine_ls_R_factor_gt           0.0646
_refine_ls_wR_factor_ref         0.1786
_refine_ls_wR_factor_gt          0.1609
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_restrained_S_all      1.120
_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
Co1 Co 0.44990(5) 0.23468(8) 0.45030(6) 0.0405(3) Uani 1 1 d . . .
Br3 Br 0.6979(5) 0.4684(4) 0.4196(7) 0.0804(18) Uani 0.57(3) 1 d PDU A 1
O1 O 0.5439(9) 0.3454(19) 0.3894(9) 0.107(6) Uani 0.57(3) 1 d PDU A 1
O2 O 0.5641(10) 0.2439(15) 0.4939(9) 0.053(3) Uani 0.57(3) 1 d PU A 1
O3 O 0.4458(11) 0.1980(17) 0.5467(12) 0.060(4) Uani 0.57(3) 1 d PU A 1
O4 O 0.4125(13) 0.0421(17) 0.5359(10) 0.080(6) Uani 0.57(3) 1 d PU A 1
Br3B Br 0.6896(9) 0.4693(7) 0.4278(10) 0.091(3) Uani 0.43(3) 1 d PDU A 2
O1B O 0.5647(12) 0.3832(13) 0.424(2) 0.096(7) Uani 0.43(3) 1 d PDU A 2
O2B O 0.5520(13) 0.2480(19) 0.4628(16) 0.058(4) Uani 0.43(3) 1 d PU A 2
O4B O 0.4495(17) 0.037(2) 0.5455(14) 0.077(7) Uani 0.43(3) 1 d PU A 2
O3B O 0.4734(13) 0.187(2) 0.5564(16) 0.051(4) Uani 0.43(3) 1 d PU A 2
N1 N 0.4145(3) 0.4411(5) 0.3937(4) 0.0539(15) Uani 1 1 d . . .
H1C H 0.4597 0.4463 0.3974 0.065 Uiso 1 1 calc R A .
N2 N 0.3910(3) 0.3620(4) 0.4188(3) 0.0465(13) Uani 1 1 d . A .
N3 N 0.1188(3) 0.5446(5) 0.1212(3) 0.0508(15) Uani 1 1 d . . .
H3A H 0.1011 0.5217 0.0732 0.061 Uiso 1 1 calc R . .
N4 N 0.1107(3) 0.6399(5) 0.1379(3) 0.0464(13) Uani 1 1 d . . .
C3 C 0.1462(4) 0.6446(5) 0.2201(4) 0.0451(16) Uani 1 1 d . . .
C4 C 0.1754(3) 0.5534(6) 0.2525(3) 0.0435(16) Uani 1 1 d . . .
C5 C 0.2192(4) 0.5273(6) 0.3417(4) 0.0534(18) Uani 1 1 d . A .
H5A H 0.2291 0.5869 0.3731 0.064 Uiso 1 1 calc R . .
H5B H 0.1862 0.4855 0.3536 0.064 Uiso 1 1 calc R . .
C6 C 0.2957(4) 0.4761(5) 0.3679(3) 0.0435(15) Uani 1 1 d . . .
C7 C 0.3173(4) 0.3834(6) 0.4031(4) 0.0450(15) Uani 1 1 d . A .
C9 C 0.1572(4) 0.4921(6) 0.1877(4) 0.0499(17) Uani 1 1 d . . .
C11 C 0.1717(5) 0.3837(7) 0.1848(5) 0.073(2) Uani 1 1 d . . .
H11A H 0.1307 0.3564 0.1355 0.110 Uiso 1 1 calc R . .
H11B H 0.1725 0.3515 0.2300 0.110 Uiso 1 1 calc R . .
H11C H 0.2212 0.3744 0.1869 0.110 Uiso 1 1 calc R . .
C12 C 0.1435(5) 0.7369(6) 0.2592(4) 0.064(2) Uani 1 1 d . . .
H12A H 0.1326 0.7905 0.2224 0.096 Uiso 1 1 calc R . .
H12B H 0.1930 0.7474 0.3070 0.096 Uiso 1 1 calc R . .
H12C H 0.1031 0.7329 0.2735 0.096 Uiso 1 1 calc R . .
C13 C 0.3590(4) 0.5103(6) 0.3624(4) 0.0492(16) Uani 1 1 d . A .
C15 C 0.3712(5) 0.6054(7) 0.3313(6) 0.083(3) Uani 1 1 d . . .
H15A H 0.3218 0.6295 0.2893 0.125 Uiso 1 1 calc R A .
H15B H 0.4059 0.5957 0.3099 0.125 Uiso 1 1 calc R . .
H15C H 0.3936 0.6522 0.3746 0.125 Uiso 1 1 calc R . .
C16 C 0.2727(4) 0.3107(8) 0.4228(6) 0.074(3) Uani 1 1 d . . .
H16A H 0.3087 0.2688 0.4657 0.111 Uiso 1 1 calc R A .
H16B H 0.2405 0.2719 0.3759 0.111 Uiso 1 1 calc R . .
H16C H 0.2403 0.3444 0.4397 0.111 Uiso 1 1 calc R . .
C18 C 0.5884(4) 0.2986(9) 0.4507(4) 0.066(2) Uani 1 1 d D . .
C21 C 0.4502(4) 0.1141(7) 0.5779(4) 0.0556(19) Uani 1 1 d . . .
C23 C 0.4706(4) 0.1148(6) 0.6680(4) 0.0533(18) Uani 1 1 d D A .
C24 C 0.4872(3) 0.0298(6) 0.7079(4) 0.0455(16) Uani 1 1 d D . .
H24A H 0.4820 -0.0288 0.6809 0.055 Uiso 0.453(2) 1 calc PR A 1
Br1 Br 0.43172(11) 0.32667(14) 0.65486(11) 0.0773(7) Uani 0.547(2) 1 d PD A 2
C25 C 0.4870(4) 0.1986(7) 0.7079(5) 0.087(3) Uani 1 1 d DU . .
H25A H 0.4814 0.2574 0.6810 0.105 Uiso 0.547(2) 1 calc PR A 1
Br2 Br 0.45804(10) -0.09510(16) 0.66560(11) 0.0638(7) Uani 0.453(2) 1 d PD A 2
C26 C 0.6724(4) 0.2778(7) 0.4754(4) 0.056(2) Uani 1 1 d . . .
C27 C 0.7235(4) 0.3413(6) 0.4673(4) 0.0527(18) Uani 1 1 d D . .
C28 C 0.7994(4) 0.3134(7) 0.4919(4) 0.057(2) Uani 1 1 d . . .
H28A H 0.8326 0.3573 0.4862 0.068 Uiso 1 1 calc R . .
O1W O 0.5000 0.451(3) 0.2500 0.47(3) Uani 1 2 d S . .
H1A H 0.5141 0.4151 0.2912 0.712 Uiso 0.50 1 d PR . .
H1B H 0.4859 0.4151 0.2088 0.712 Uiso 0.50 1 d PR . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Co1 0.0318(5) 0.0548(7) 0.0298(5) 0.0042(5) 0.0114(4) -0.0023(5)
Br3 0.0630(17) 0.089(3) 0.096(4) 0.004(2) 0.044(2) 0.0039(18)
O1 0.029(7) 0.231(16) 0.042(7) 0.041(9) 0.003(5) 0.023(9)
O2 0.026(6) 0.092(7) 0.032(6) 0.003(7) 0.007(6) 0.000(5)
O3 0.047(8) 0.090(8) 0.031(6) 0.018(5) 0.011(7) 0.003(7)
O4 0.094(11) 0.100(11) 0.026(6) -0.005(7) 0.015(8) -0.047(10)
Br3B 0.088(6) 0.107(4) 0.069(3) 0.008(2) 0.031(4) 0.029(3)
O1B 0.025(8) 0.160(16) 0.091(15) 0.044(13) 0.020(9) 0.006(9)
O2B 0.027(7) 0.081(8) 0.051(9) 0.016(9) 0.006(8) -0.004(6)
O4B 0.094(14) 0.090(12) 0.023(7) 0.005(7) 0.011(10) 0.042(12)
O3B 0.037(8) 0.076(8) 0.028(7) 0.012(6) 0.007(8) 0.001(8)
N1 0.035(3) 0.066(4) 0.059(3) 0.009(3) 0.021(3) -0.005(3)
N2 0.036(3) 0.054(4) 0.046(3) 0.009(3) 0.018(2) 0.002(3)
N3 0.055(3) 0.060(4) 0.028(3) -0.003(3) 0.014(2) 0.016(3)
N4 0.044(3) 0.061(4) 0.027(2) -0.001(2) 0.012(2) 0.005(3)
C3 0.037(3) 0.063(5) 0.033(3) -0.003(3) 0.015(3) 0.000(3)
C4 0.030(3) 0.066(5) 0.030(3) -0.001(3) 0.012(2) 0.005(3)
C5 0.045(3) 0.077(5) 0.033(3) 0.009(3) 0.015(3) 0.019(4)
C6 0.037(3) 0.060(4) 0.026(3) 0.004(3) 0.009(2) 0.008(3)
C7 0.036(3) 0.064(5) 0.033(3) 0.002(3) 0.015(3) 0.000(3)
C9 0.047(3) 0.062(5) 0.038(3) -0.002(3) 0.019(3) 0.010(3)
C11 0.082(6) 0.078(6) 0.050(4) 0.004(4) 0.025(4) 0.029(5)
C12 0.074(5) 0.067(5) 0.037(3) -0.011(3) 0.017(4) -0.001(4)
C13 0.042(3) 0.053(4) 0.045(4) 0.007(3) 0.015(3) 0.001(3)
C15 0.068(5) 0.077(7) 0.096(7) 0.031(5) 0.033(5) -0.001(5)
C16 0.047(4) 0.099(7) 0.082(6) 0.026(5) 0.036(4) -0.002(4)
C18 0.039(4) 0.115(8) 0.042(4) 0.001(5) 0.018(3) 0.007(5)
C21 0.055(4) 0.079(6) 0.033(3) 0.002(4) 0.022(3) 0.002(4)
C23 0.061(4) 0.063(5) 0.035(3) 0.000(3) 0.023(3) -0.007(4)
C24 0.036(3) 0.061(4) 0.032(3) -0.008(3) 0.011(2) 0.001(3)
Br1 0.0839(12) 0.0699(12) 0.0814(12) 0.0192(9) 0.0432(10) 0.0199(9)
C25 0.146(8) 0.058(5) 0.047(4) 0.004(4) 0.039(5) -0.004(5)
Br2 0.0557(10) 0.0730(14) 0.0612(11) -0.0203(9) 0.0277(9) -0.0041(9)
C26 0.032(3) 0.098(7) 0.030(3) -0.014(4) 0.011(3) -0.001(4)
C27 0.037(3) 0.081(6) 0.035(3) -0.010(3) 0.014(3) 0.001(3)
C28 0.037(3) 0.092(6) 0.040(4) -0.009(4) 0.017(3) -0.010(4)
O1W 0.53(6) 0.42(6) 0.24(3) 0.000 0.01(4) 0.000
_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 O2B 1.91(2) . ?
Co1 O3B 1.95(3) . ?
Co1 O3 1.94(2) . ?
Co1 O2 1.975(17) . ?
Co1 N4 1.984(6) 4_545 ?
Co1 N2 2.010(6) . ?
Br3 C27 1.908(10) . ?
O1 C18 1.235(12) . ?
O2 C18 1.36(2) . ?
O3 C21 1.27(2) . ?
O4 C21 1.253(19) . ?
Br3B C27 1.889(11) . ?
O1B C18 1.253(14) . ?
O2B C18 1.10(3) . ?
O4B C21 1.22(3) . ?
O3B C21 1.24(3) . ?
N1 C13 1.339(9) . ?
N1 N2 1.351(8) . ?
N1 H1C 0.8600 . ?
N2 C7 1.357(8) . ?
N3 C9 1.320(9) . ?
N3 N4 1.368(8) . ?
N3 H3A 0.8600 . ?
N4 C3 1.363(8) . ?
N4 Co1 1.984(6) 4 ?
C3 C4 1.382(10) . ?
C3 C12 1.478(10) . ?
C4 C9 1.382(9) . ?
C4 C5 1.520(8) . ?
C5 C6 1.502(9) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 C13 1.380(9) . ?
C6 C7 1.396(10) . ?
C7 C16 1.489(10) . ?
C9 C11 1.515(11) . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 C15 1.495(11) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C18 C26 1.504(10) . ?
C21 C23 1.556(9) . ?
C23 C25 1.323(11) . ?
C23 C24 1.336(10) . ?
C24 C24 1.421(12) 2_656 ?
C24 Br2 1.852(7) . ?
C24 H24A 0.9300 . ?
Br1 C25 2.042(9) . ?
C25 C25 1.420(16) 2_656 ?
C25 H25A 0.9300 . ?
C26 C28 1.381(12) 7_656 ?
C26 C27 1.390(11) . ?
C27 C28 1.378(10) . ?
C28 C26 1.381(12) 7_656 ?
C28 H28A 0.9300 . ?
O1W H1A 0.8501 . ?
O1W H1B 0.8501 . ?
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
O2B Co1 O3B 101.9(7) . . ?
O2B Co1 O3 116.0(6) . . ?
O3B Co1 O3 14.8(6) . . ?
O2B Co1 O2 15.3(6) . . ?
O3B Co1 O2 87.0(6) . . ?
O3 Co1 O2 100.8(5) . . ?
O2B Co1 N4 108.8(9) . 4_545 ?
O3B Co1 N4 113.1(8) . 4_545 ?
O3 Co1 N4 110.1(7) . 4_545 ?
O2 Co1 N4 118.7(5) . 4_545 ?
O2B Co1 N2 111.7(8) . . ?
O3B Co1 N2 114.0(8) . . ?
O3 Co1 N2 102.6(7) . . ?
O2 Co1 N2 116.0(6) . . ?
N4 Co1 N2 107.2(2) 4_545 . ?
C18 O2 Co1 116.5(11) . . ?
C21 O3 Co1 130.4(16) . . ?
C18 O2B Co1 141.9(19) . . ?
C21 O3B Co1 132.2(18) . . ?
C13 N1 N2 112.1(5) . . ?
C13 N1 H1C 123.9 . . ?
N2 N1 H1C 123.9 . . ?
N1 N2 C7 105.3(6) . . ?
N1 N2 Co1 123.3(4) . . ?
C7 N2 Co1 130.3(5) . . ?
C9 N3 N4 111.7(5) . . ?
C9 N3 H3A 124.2 . . ?
N4 N3 H3A 124.2 . . ?
C3 N4 N3 105.1(5) . . ?
C3 N4 Co1 133.9(5) . 4 ?
N3 N4 Co1 120.9(4) . 4 ?
N4 C3 C4 109.5(6) . . ?
N4 C3 C12 119.5(6) . . ?
C4 C3 C12 130.9(6) . . ?
C3 C4 C9 106.3(6) . . ?
C3 C4 C5 126.2(6) . . ?
C9 C4 C5 127.5(7) . . ?
C6 C5 C4 113.7(5) . . ?
C6 C5 H5A 108.8 . . ?
C4 C5 H5A 108.8 . . ?
C6 C5 H5B 108.8 . . ?
C4 C5 H5B 108.8 . . ?
H5A C5 H5B 107.7 . . ?
C13 C6 C7 105.8(6) . . ?
C13 C6 C5 127.5(7) . . ?
C7 C6 C5 126.8(6) . . ?
N2 C7 C6 109.8(6) . . ?
N2 C7 C16 119.8(7) . . ?
C6 C7 C16 130.4(6) . . ?
N3 C9 C4 107.5(6) . . ?
N3 C9 C11 121.6(6) . . ?
C4 C9 C11 130.9(7) . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C3 C12 H12A 109.5 . . ?
C3 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C3 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N1 C13 C6 107.0(6) . . ?
N1 C13 C15 122.4(7) . . ?
C6 C13 C15 130.6(7) . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C7 C16 H16A 109.5 . . ?
C7 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C7 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
O2B C18 O1 107.0(14) . . ?
O2B C18 O1B 120.7(17) . . ?
O1 C18 O1B 36.5(11) . . ?
O2B C18 O2 21.3(13) . . ?
O1 C18 O2 124.0(12) . . ?
O1B C18 O2 125.1(16) . . ?
O2B C18 C26 123.0(16) . . ?
O1 C18 C26 123.2(11) . . ?
O1B C18 C26 115.7(13) . . ?
O2 C18 C26 111.5(10) . . ?
O4B C21 O3B 116(2) . . ?
O4B C21 O4 31.0(11) . . ?
O3B C21 O4 127.9(15) . . ?
O4B C21 O3 124.2(17) . . ?
O3B C21 O3 23.0(10) . . ?
O4 C21 O3 121.8(15) . . ?
O4B C21 C23 119.6(14) . . ?
O3B C21 C23 114.9(14) . . ?
O4 C21 C23 117.2(10) . . ?
O3 C21 C23 115.4(12) . . ?
C25 C23 C24 120.1(7) . . ?
C25 C23 C21 119.7(7) . . ?
C24 C23 C21 118.7(7) . . ?
C23 C24 C24 119.5(4) . 2_656 ?
C23 C24 Br2 128.0(5) . . ?
C24 C24 Br2 110.6(2) 2_656 . ?
C23 C24 H24A 120.2 . . ?
C24 C24 H24A 120.2 2_656 . ?
Br2 C24 H24A 16.3 . . ?
C23 C25 C25 119.9(5) . 2_656 ?
C23 C25 Br1 122.5(6) . . ?
C25 C25 Br1 111.4(3) 2_656 . ?
C23 C25 H25A 120.1 . . ?
C25 C25 H25A 120.1 2_656 . ?
Br1 C25 H25A 25.7 . . ?
C28 C26 C27 117.6(6) 7_656 . ?
C28 C26 C18 116.4(8) 7_656 . ?
C27 C26 C18 126.1(9) . . ?
C28 C27 C26 120.6(8) . . ?
C28 C27 Br3B 120.0(8) . . ?
C26 C27 Br3B 119.3(8) . . ?
C28 C27 Br3 113.6(7) . . ?
C26 C27 Br3 125.8(6) . . ?
Br3B C27 Br3 8.3(9) . . ?
C27 C28 C26 121.8(8) . 7_656 ?
C27 C28 H28A 119.1 . . ?
C26 C28 H28A 119.1 7_656 . ?
H1A O1W H1B 108.7 . . ?
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
O2B Co1 O2 C18 28(4) . . . . ?
O3B Co1 O2 C18 -164.3(14) . . . . ?
O3 Co1 O2 C18 -158.9(14) . . . . ?
N4 Co1 O2 C18 80.9(14) 4_545 . . . ?
N2 Co1 O2 C18 -49.0(14) . . . . ?
O2B Co1 O3 C21 -83.2(19) . . . . ?
O3B Co1 O3 C21 -64(5) . . . . ?
O2 Co1 O3 C21 -85.3(18) . . . . ?
N4 Co1 O3 C21 40.9(18) 4_545 . . . ?
N2 Co1 O3 C21 154.7(16) . . . . ?
O3B Co1 O2B C18 -134(4) . . . . ?
O3 Co1 O2B C18 -129(3) . . . . ?
O2 Co1 O2B C18 -121(8) . . . . ?
N4 Co1 O2B C18 106(4) 4_545 . . . ?
N2 Co1 O2B C18 -12(4) . . . . ?
O2B Co1 O3B C21 -126(2) . . . . ?
O3 Co1 O3B C21 71(5) . . . . ?
O2 Co1 O3B C21 -130(2) . . . . ?
N4 Co1 O3B C21 -10(3) 4_545 . . . ?
N2 Co1 O3B C21 113(2) . . . . ?
C13 N1 N2 C7 -0.6(8) . . . . ?
C13 N1 N2 Co1 168.6(5) . . . . ?
O2B Co1 N2 N1 12.6(11) . . . . ?
O3B Co1 N2 N1 127.5(9) . . . . ?
O3 Co1 N2 N1 137.5(8) . . . . ?
O2 Co1 N2 N1 28.7(8) . . . . ?
N4 Co1 N2 N1 -106.5(5) 4_545 . . . ?
O2B Co1 N2 C7 178.9(10) . . . . ?
O3B Co1 N2 C7 -66.2(10) . . . . ?
O3 Co1 N2 C7 -56.2(8) . . . . ?
O2 Co1 N2 C7 -165.0(7) . . . . ?
N4 Co1 N2 C7 59.8(6) 4_545 . . . ?
C9 N3 N4 C3 -0.4(8) . . . . ?
C9 N3 N4 Co1 -176.3(5) . . . 4 ?
N3 N4 C3 C4 0.1(7) . . . . ?
Co1 N4 C3 C4 175.2(5) 4 . . . ?
N3 N4 C3 C12 -175.8(6) . . . . ?
Co1 N4 C3 C12 -0.7(10) 4 . . . ?
N4 C3 C4 C9 0.2(7) . . . . ?
C12 C3 C4 C9 175.5(7) . . . . ?
N4 C3 C4 C5 179.8(6) . . . . ?
C12 C3 C4 C5 -4.8(12) . . . . ?
C3 C4 C5 C6 -128.3(7) . . . . ?
C9 C4 C5 C6 51.3(10) . . . . ?
C4 C5 C6 C13 59.0(10) . . . . ?
C4 C5 C6 C7 -121.1(7) . . . . ?
N1 N2 C7 C6 0.2(7) . . . . ?
Co1 N2 C7 C6 -167.9(4) . . . . ?
N1 N2 C7 C16 179.4(7) . . . . ?
Co1 N2 C7 C16 11.2(10) . . . . ?
C13 C6 C7 N2 0.3(7) . . . . ?
C5 C6 C7 N2 -179.7(6) . . . . ?
C13 C6 C7 C16 -178.8(8) . . . . ?
C5 C6 C7 C16 1.3(12) . . . . ?
N4 N3 C9 C4 0.6(8) . . . . ?
N4 N3 C9 C11 178.4(7) . . . . ?
C3 C4 C9 N3 -0.4(8) . . . . ?
C5 C4 C9 N3 179.9(6) . . . . ?
C3 C4 C9 C11 -178.1(8) . . . . ?
C5 C4 C9 C11 2.3(13) . . . . ?
N2 N1 C13 C6 0.8(8) . . . . ?
N2 N1 C13 C15 179.2(7) . . . . ?
C7 C6 C13 N1 -0.6(8) . . . . ?
C5 C6 C13 N1 179.3(6) . . . . ?
C7 C6 C13 C15 -178.8(8) . . . . ?
C5 C6 C13 C15 1.1(13) . . . . ?
Co1 O2B C18 O1 -30(4) . . . . ?
Co1 O2B C18 O1B 7(4) . . . . ?
Co1 O2B C18 O2 115(8) . . . . ?
Co1 O2B C18 C26 178(2) . . . . ?
Co1 O2 C18 O2B -37(5) . . . . ?
Co1 O2 C18 O1 4(2) . . . . ?
Co1 O2 C18 O1B 48(2) . . . . ?
Co1 O2 C18 C26 -163.9(8) . . . . ?
Co1 O3B C21 O4B 46(3) . . . . ?
Co1 O3B C21 O4 12(4) . . . . ?
Co1 O3B C21 O3 -71(5) . . . . ?
Co1 O3B C21 C23 -167.9(16) . . . . ?
Co1 O3 C21 O4B -8(3) . . . . ?
Co1 O3 C21 O3B 67(5) . . . . ?
Co1 O3 C21 O4 -45(3) . . . . ?
Co1 O3 C21 C23 161.7(11) . . . . ?
O4B C21 C23 C25 166.4(18) . . . . ?
O3B C21 C23 C25 21.2(15) . . . . ?
O4 C21 C23 C25 -158.4(15) . . . . ?
O3 C21 C23 C25 -4.3(13) . . . . ?
O4B C21 C23 C24 0(2) . . . . ?
O3B C21 C23 C24 -145.0(13) . . . . ?
O4 C21 C23 C24 35.3(17) . . . . ?
O3 C21 C23 C24 -170.5(11) . . . . ?
C25 C23 C24 C24 8.2(7) . . . 2_656 ?
C21 C23 C24 C24 174.4(7) . . . 2_656 ?
C25 C23 C24 Br2 170.8(5) . . . . ?
C21 C23 C24 Br2 -23.0(7) . . . . ?
C24 C23 C25 C25 -7.8(9) . . . 2_656 ?
C21 C23 C25 C25 -173.9(9) . . . 2_656 ?
C24 C23 C25 Br1 -157.8(5) . . . . ?
C21 C23 C25 Br1 36.1(7) . . . . ?
O2B C18 C26 C28 6(2) . . . 7_656 ?
O1 C18 C26 C28 -141.7(19) . . . 7_656 ?
O1B C18 C26 C28 176.9(19) . . . 7_656 ?
O2 C18 C26 C28 25.9(12) . . . 7_656 ?
O2B C18 C26 C27 -175.1(19) . . . . ?
O1 C18 C26 C27 38(2) . . . . ?
O1B C18 C26 C27 -4(2) . . . . ?
O2 C18 C26 C27 -154.9(10) . . . . ?
C28 C26 C27 C28 -0.4(11) 7_656 . . . ?
C18 C26 C27 C28 -179.6(6) . . . . ?
C28 C26 C27 Br3B -176.9(8) 7_656 . . . ?
C18 C26 C27 Br3B 3.8(11) . . . . ?
C28 C26 C27 Br3 176.9(7) 7_656 . . . ?
C18 C26 C27 Br3 -2.4(11) . . . . ?
C26 C27 C28 C26 0.4(11) . . . 7_656 ?
Br3B C27 C28 C26 176.9(8) . . . 7_656 ?
Br3 C27 C28 C26 -177.2(7) . . . 7_656 ?
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
N1 H1C O1B 0.86 2.05 2.822(19) 148.8 .
N1 H1C O1 0.86 2.21 2.895(18) 136.0 .
N3 H3A O4B 0.86 1.98 2.77(2) 152.3 4
N3 H3A O4 0.86 1.98 2.738(19) 146.9 4
O1W H1A O1 0.85 1.91 2.76(3) 173.8 .
O1W H1A O1B 0.85 2.26 3.06(3) 155.3 .
O1W H1B O1 0.85 1.91 2.76(3) 173.8 2_655
O1W H1B O1B 0.85 2.26 3.06(3) 155.3 2_655
_diffrn_measured_fraction_theta_max 0.986
_diffrn_reflns_theta_full        72.07
_diffrn_measured_fraction_theta_full 0.986
_refine_diff_density_max         0.670
_refine_diff_density_min         -0.704
_refine_diff_density_rms         0.090