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

data_global
_journal_name_full               CrystEngComm

_journal_coden_Cambridge         1350

_publ_contact_author_name        'Dong Li'
_publ_contact_author_email       DFLI@MAIL.CCNU.EDU.CN

_publ_section_title              
;
Structures, Photoluminescence and Photocatalytic
Properties of Three New Metal-Organic Frameworks Based on Flexible
Bridges
;
loop_

_publ_author_name
'Dong Li'
'Kejian Deng'
'Kangle Lv'
'Chenggang Wang'
'Dong-E Wang'
;
Li-Li Wen
;

# Attachment 'new.cif'

#Structures, Photoluminescence and Photocatalytic Properties of Three New Metal-Organic Frameworks Based on Non-Rigid Long Bridges
data_071114cm
_database_code_depnum_ccdc_archive 'CCDC 705563'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C52 H30 Cd3 N8 O28'
_chemical_formula_weight         1552.04

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

_cell_length_a                   9.8675(11)
_cell_length_b                   11.8984(13)
_cell_length_c                   12.7498(15)
_cell_angle_alpha                116.905(2)
_cell_angle_beta                 92.962(2)
_cell_angle_gamma                93.923(2)
_cell_volume                     1326.0(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    295(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          0.16
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.944
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             766
_exptl_absorpt_coefficient_mu    1.299
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.812
_exptl_absorpt_correction_T_max  0.823
_exptl_absorpt_process_details   'SADABS(Bruker, 2000)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            12575
_diffrn_reflns_av_R_equivalents  0.0617
_diffrn_reflns_av_sigmaI/netI    0.0818
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         1.80
_diffrn_reflns_theta_max         27.00
_reflns_number_total             5674
_reflns_number_gt                4197
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0434P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5674
_refine_ls_number_parameters     460
_refine_ls_number_restraints     119
_refine_ls_R_factor_all          0.0664
_refine_ls_R_factor_gt           0.0424
_refine_ls_wR_factor_ref         0.1060
_refine_ls_wR_factor_gt          0.0850
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_restrained_S_all      1.042
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cd1 Cd 0.5000 0.5000 0.5000 0.02954(14) Uani 1 2 d S . .
Cd2 Cd 0.49320(3) 0.17531(3) 0.32208(3) 0.02798(12) Uani 1 1 d U . .
C1 C 0.4485(5) 0.3369(5) 0.2190(4) 0.0327(12) Uani 1 1 d . . .
C2 C 0.3996(5) 0.4116(4) 0.1578(4) 0.0286(11) Uani 1 1 d . B .
C3 C 0.2857(5) 0.3630(4) 0.0753(4) 0.0370(13) Uani 1 1 d . . .
H3 H 0.2401 0.2843 0.0564 0.044 Uiso 1 1 calc R . .
N3 N 0.1251(5) 0.3803(5) -0.0689(5) 0.0538(14) Uani 1 1 d D . .
C4 C 0.2421(5) 0.4350(5) 0.0220(4) 0.0317(12) Uani 1 1 d . B .
C5 C 0.3060(5) 0.5514(4) 0.0470(4) 0.0370(12) Uani 1 1 d . . .
H5 H 0.2731 0.5980 0.0108 0.044 Uiso 1 1 calc R B .
C6 C 0.5029(5) 0.7199(4) 0.1531(4) 0.0346(12) Uani 1 1 d . . .
C7 C 0.4216(5) 0.5986(4) 0.1282(4) 0.0301(11) Uani 1 1 d . B .
C8 C 0.4655(5) 0.5292(4) 0.1832(4) 0.0351(12) Uani 1 1 d . . .
H8 H 0.5411 0.5620 0.2387 0.042 Uiso 1 1 calc R B .
C9 C 0.7585(5) 0.7314(4) 0.5747(5) 0.0314(11) Uani 1 1 d . . .
C10 C 0.8659(4) 0.6603(4) 0.4968(4) 0.0285(11) Uani 1 1 d . . .
C11 C 0.8286(5) 0.5567(4) 0.3884(4) 0.0332(11) Uani 1 1 d . . .
H11 H 0.7372 0.5308 0.3603 0.040 Uiso 1 1 calc R . .
N4 N 0.8932(5) 0.3792(4) 0.2080(4) 0.0472(12) Uani 1 1 d . . .
C12 C 0.9302(5) 0.4928(4) 0.3229(4) 0.0333(12) Uani 1 1 d . . .
C13 C 1.0672(5) 0.5285(4) 0.3606(5) 0.0348(12) Uani 1 1 d . . .
H13 H 1.1336 0.4829 0.3149 0.042 Uiso 1 1 calc R . .
C14 C 1.2539(5) 0.6685(5) 0.5118(5) 0.0344(12) Uani 1 1 d . . .
C15 C 1.1029(5) 0.6340(4) 0.4682(5) 0.0330(12) Uani 1 1 d . . .
C16 C 1.0023(5) 0.7000(4) 0.5360(5) 0.0333(12) Uani 1 1 d . . .
H16 H 1.0267 0.7711 0.6082 0.040 Uiso 1 1 calc R . .
C19 C 0.9353(4) 0.0046(4) 0.0267(4) 0.0267(11) Uani 1 1 d D . .
N1 N 0.6888(4) 0.0121(3) 0.1225(3) 0.0298(10) Uani 1 1 d D . .
C17 C 0.6939(17) 0.0057(15) 0.0155(8) 0.047(3) Uani 0.602(19) 1 d PDU A 1
H17 H 0.6142 0.0081 -0.0254 0.057 Uiso 0.602(19) 1 calc PR A 1
C18 C 0.8125(9) -0.0040(16) -0.0342(12) 0.046(3) Uani 0.602(19) 1 d PDU A 1
H18 H 0.8114 -0.0169 -0.1119 0.055 Uiso 0.602(19) 1 calc PR A 1
C20 C 0.9296(15) 0.0157(14) 0.1400(8) 0.035(3) Uani 0.602(19) 1 d PDU A 1
H20 H 1.0094 0.0197 0.1842 0.043 Uiso 0.602(19) 1 calc PR A 1
C21 C 0.8052(10) 0.0209(14) 0.1867(11) 0.035(3) Uani 0.602(19) 1 d PDU A 1
H21 H 0.8021 0.0305 0.2631 0.042 Uiso 0.602(19) 1 calc PR A 1
C17B C 0.702(3) 0.0521(19) 0.0408(14) 0.042(4) Uani 0.398(19) 1 d PDU A 2
H17B H 0.6274 0.0815 0.0164 0.050 Uiso 0.398(19) 1 calc PR A 2
C18B C 0.8256(15) 0.0504(18) -0.0087(17) 0.040(4) Uani 0.398(19) 1 d PDU A 2
H18B H 0.8342 0.0798 -0.0646 0.048 Uiso 0.398(19) 1 calc PR A 2
C20B C 0.914(2) -0.0320(19) 0.1138(14) 0.040(4) Uani 0.398(19) 1 d PDU A 2
H20B H 0.9866 -0.0595 0.1420 0.048 Uiso 0.398(19) 1 calc PR A 2
C21B C 0.7925(17) -0.0303(19) 0.1608(18) 0.036(3) Uani 0.398(19) 1 d PDU A 2
H21B H 0.7823 -0.0578 0.2179 0.043 Uiso 0.398(19) 1 calc PR A 2
C22 C 0.2321(5) -0.0798(5) 0.3362(4) 0.0390(13) Uani 1 1 d . . .
H22 H 0.2511 -0.1360 0.2605 0.047 Uiso 1 1 calc R . .
C23 C 0.1027(5) -0.0855(5) 0.3692(4) 0.0412(14) Uani 1 1 d . . .
H23 H 0.0356 -0.1463 0.3161 0.049 Uiso 1 1 calc R . .
C24 C 0.0702(5) -0.0012(4) 0.4818(4) 0.0316(11) Uani 1 1 d . . .
C25 C 0.1775(5) 0.0802(5) 0.5602(5) 0.0378(13) Uani 1 1 d . . .
H25 H 0.1619 0.1343 0.6375 0.045 Uiso 1 1 calc R . .
C26 C 0.3062(5) 0.0815(4) 0.5246(4) 0.0350(12) Uani 1 1 d . . .
H26 H 0.3774 0.1350 0.5786 0.042 Uiso 1 1 calc R . .
N2 N 0.3308(4) 0.0050(4) 0.4108(4) 0.0324(10) Uani 1 1 d . . .
O1 O 0.5321(4) 0.3942(3) 0.3088(3) 0.0417(9) Uani 1 1 d U . .
O2 O 0.4065(4) 0.2232(3) 0.1775(3) 0.0501(10) Uani 1 1 d . . .
O3 O 0.0767(5) 0.2731(4) -0.0977(4) 0.0815(16) Uani 1 1 d . B .
O4 O 0.0731(10) 0.4509(9) -0.1038(11) 0.064(3) Uani 0.75(3) 1 d PDU B 1
O4B O 0.121(3) 0.414(3) -0.148(2) 0.071(5) Uani 0.25(3) 1 d PDU B 2
O5 O 0.4420(4) 0.7870(3) 0.1094(3) 0.0422(9) Uani 1 1 d . B .
H5A H 0.4902 0.8530 0.1270 0.063 Uiso 1 1 calc R . .
O6 O 0.6138(4) 0.7525(3) 0.2088(3) 0.0469(10) Uani 1 1 d . B .
O7 O 0.6322(3) 0.6861(3) 0.5368(3) 0.0350(8) Uani 1 1 d . . .
O8 O 0.7908(3) 0.8285(3) 0.6663(3) 0.0388(9) Uani 1 1 d . . .
O9 O 1.2869(3) 0.7715(3) 0.6029(3) 0.0486(10) Uani 1 1 d . . .
O10 O 1.3316(4) 0.5885(4) 0.4544(3) 0.0503(10) Uani 1 1 d . . .
O11 O 0.9838(4) 0.3174(4) 0.1582(4) 0.0792(16) Uani 1 1 d . . .
O12 O 0.7748(4) 0.3542(4) 0.1686(4) 0.0729(15) Uani 1 1 d . . .
O13 O 0.5677(3) 0.0084(3) 0.1644(3) 0.0373(9) Uani 1 1 d . A .
O14 O 0.4520(3) 0.0170(3) 0.3741(3) 0.0378(9) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cd1 O10 2.214(4) 2_766 ?
Cd1 O10 2.214(4) 1_455 ?
Cd1 O1 2.233(3) . ?
Cd1 O1 2.233(3) 2_666 ?
Cd1 O7 2.329(3) . ?
Cd1 O7 2.329(3) 2_666 ?
Cd1 Cd2 3.4774(5) . ?
Cd1 Cd2 3.4774(5) 2_666 ?
Cd2 O9 2.252(3) 2_766 ?
Cd2 O14 2.282(3) . ?
Cd2 O13 2.294(3) . ?
Cd2 O2 2.304(4) . ?
Cd2 O7 2.305(3) 2_666 ?
C1 O2 1.238(6) . ?
C1 O1 1.255(6) . ?
C1 C2 1.510(7) . ?
C2 C8 1.389(6) . ?
C2 C3 1.394(6) . ?
C3 C4 1.389(7) . ?
C3 H3 0.9300 . ?
N3 O3 1.210(6) . ?
N3 O4B 1.241(10) . ?
N3 O4 1.241(7) . ?
N3 C4 1.475(6) . ?
C4 C5 1.371(7) . ?
C5 C7 1.398(7) . ?
C5 H5 0.9300 . ?
C6 O6 1.210(6) . ?
C6 O5 1.320(6) . ?
C6 C7 1.492(6) . ?
C7 C8 1.379(7) . ?
C8 H8 0.9300 . ?
C9 O8 1.221(5) . ?
C9 O7 1.300(5) . ?
C9 C10 1.515(6) . ?
C10 C11 1.382(6) . ?
C10 C16 1.383(6) . ?
C11 C12 1.377(6) . ?
C11 H11 0.9300 . ?
N4 O12 1.209(6) . ?
N4 O11 1.213(5) . ?
N4 C12 1.481(6) . ?
C12 C13 1.381(7) . ?
C13 C15 1.383(7) . ?
C13 H13 0.9300 . ?
C14 O10 1.247(5) . ?
C14 O9 1.255(6) . ?
C14 C15 1.524(6) . ?
C15 C16 1.390(6) . ?
C16 H16 0.9300 . ?
C19 C18 1.377(7) . ?
C19 C20B 1.384(8) . ?
C19 C18B 1.388(8) . ?
C19 C20 1.394(7) . ?
C19 C19 1.466(9) 2_755 ?
N1 C17B 1.335(8) . ?
N1 C21B 1.335(8) . ?
N1 C17 1.335(7) . ?
N1 O13 1.340(5) . ?
N1 C21 1.345(7) . ?
C17 C18 1.346(16) . ?
C17 H17 0.9300 . ?
C18 H18 0.9300 . ?
C20 C21 1.385(15) . ?
C20 H20 0.9300 . ?
C21 H21 0.9300 . ?
C17B C18B 1.40(3) . ?
C17B H17B 0.9300 . ?
C18B H18B 0.9300 . ?
C20B C21B 1.36(2) . ?
C20B H20B 0.9300 . ?
C21B H21B 0.9300 . ?
C22 N2 1.332(6) . ?
C22 C23 1.371(7) . ?
C22 H22 0.9300 . ?
C23 C24 1.399(6) . ?
C23 H23 0.9300 . ?
C24 C25 1.390(6) . ?
C24 C24 1.482(9) 2_556 ?
C25 C26 1.372(7) . ?
C25 H25 0.9300 . ?
C26 N2 1.365(6) . ?
C26 H26 0.9300 . ?
N2 O14 1.328(5) . ?
O5 H5A 0.8200 . ?
O7 Cd2 2.305(3) 2_666 ?
O9 Cd2 2.252(3) 2_766 ?
O10 Cd1 2.214(4) 1_655 ?

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
O10 Cd1 O10 180.000(1) 2_766 1_455 ?
O10 Cd1 O1 90.36(14) 2_766 . ?
O10 Cd1 O1 89.64(14) 1_455 . ?
O10 Cd1 O1 89.64(14) 2_766 2_666 ?
O10 Cd1 O1 90.36(14) 1_455 2_666 ?
O1 Cd1 O1 180.00(11) . 2_666 ?
O10 Cd1 O7 95.42(13) 2_766 . ?
O10 Cd1 O7 84.58(13) 1_455 . ?
O1 Cd1 O7 96.48(12) . . ?
O1 Cd1 O7 83.52(12) 2_666 . ?
O10 Cd1 O7 84.58(13) 2_766 2_666 ?
O10 Cd1 O7 95.42(13) 1_455 2_666 ?
O1 Cd1 O7 83.52(12) . 2_666 ?
O1 Cd1 O7 96.48(12) 2_666 2_666 ?
O7 Cd1 O7 180.0 . 2_666 ?
O10 Cd1 Cd2 65.40(10) 2_766 . ?
O10 Cd1 Cd2 114.60(10) 1_455 . ?
O1 Cd1 Cd2 50.64(9) . . ?
O1 Cd1 Cd2 129.36(9) 2_666 . ?
O7 Cd1 Cd2 138.89(8) . . ?
O7 Cd1 Cd2 41.11(8) 2_666 . ?
O10 Cd1 Cd2 114.60(10) 2_766 2_666 ?
O10 Cd1 Cd2 65.40(10) 1_455 2_666 ?
O1 Cd1 Cd2 129.36(9) . 2_666 ?
O1 Cd1 Cd2 50.64(9) 2_666 2_666 ?
O7 Cd1 Cd2 41.11(8) . 2_666 ?
O7 Cd1 Cd2 138.89(8) 2_666 2_666 ?
Cd2 Cd1 Cd2 180.000(13) . 2_666 ?
O9 Cd2 O14 96.38(13) 2_766 . ?
O9 Cd2 O13 86.65(12) 2_766 . ?
O14 Cd2 O13 79.41(12) . . ?
O9 Cd2 O2 122.35(15) 2_766 . ?
O14 Cd2 O2 136.20(13) . . ?
O13 Cd2 O2 83.03(13) . . ?
O9 Cd2 O7 106.58(12) 2_766 2_666 ?
O14 Cd2 O7 94.42(12) . 2_666 ?
O13 Cd2 O7 166.05(11) . 2_666 ?
O2 Cd2 O7 93.22(13) . 2_666 ?
O9 Cd2 Cd1 78.18(9) 2_766 . ?
O14 Cd2 Cd1 127.80(9) . . ?
O13 Cd2 Cd1 149.78(8) . . ?
O2 Cd2 Cd1 83.32(9) . . ?
O7 Cd2 Cd1 41.63(8) 2_666 . ?
O2 C1 O1 123.8(5) . . ?
O2 C1 C2 118.9(4) . . ?
O1 C1 C2 117.3(4) . . ?
C8 C2 C3 119.1(5) . . ?
C8 C2 C1 121.1(4) . . ?
C3 C2 C1 119.8(4) . . ?
C4 C3 C2 118.4(5) . . ?
C4 C3 H3 120.8 . . ?
C2 C3 H3 120.8 . . ?
O3 N3 O4B 115.8(13) . . ?
O3 N3 O4 123.0(5) . . ?
O4B N3 O4 35.3(14) . . ?
O3 N3 C4 118.7(5) . . ?
O4B N3 C4 117.0(13) . . ?
O4 N3 C4 117.9(5) . . ?
C5 C4 C3 122.9(5) . . ?
C5 C4 N3 119.1(5) . . ?
C3 C4 N3 117.9(5) . . ?
C4 C5 C7 118.4(5) . . ?
C4 C5 H5 120.8 . . ?
C7 C5 H5 120.8 . . ?
O6 C6 O5 124.0(5) . . ?
O6 C6 C7 122.4(5) . . ?
O5 C6 C7 113.7(4) . . ?
C8 C7 C5 119.5(5) . . ?
C8 C7 C6 118.9(4) . . ?
C5 C7 C6 121.6(5) . . ?
C7 C8 C2 121.7(5) . . ?
C7 C8 H8 119.2 . . ?
C2 C8 H8 119.2 . . ?
O8 C9 O7 122.5(4) . . ?
O8 C9 C10 120.8(4) . . ?
O7 C9 C10 116.6(4) . . ?
C11 C10 C16 120.3(4) . . ?
C11 C10 C9 120.7(4) . . ?
C16 C10 C9 119.1(4) . . ?
C12 C11 C10 118.3(4) . . ?
C12 C11 H11 120.9 . . ?
C10 C11 H11 120.9 . . ?
O12 N4 O11 123.8(5) . . ?
O12 N4 C12 118.3(4) . . ?
O11 N4 C12 118.0(5) . . ?
C11 C12 C13 122.9(4) . . ?
C11 C12 N4 119.5(4) . . ?
C13 C12 N4 117.6(4) . . ?
C12 C13 C15 118.1(4) . . ?
C12 C13 H13 120.9 . . ?
C15 C13 H13 120.9 . . ?
O10 C14 O9 126.8(5) . . ?
O10 C14 C15 115.9(4) . . ?
O9 C14 C15 117.3(4) . . ?
C13 C15 C16 120.1(4) . . ?
C13 C15 C14 117.7(4) . . ?
C16 C15 C14 122.1(4) . . ?
C10 C16 C15 120.3(4) . . ?
C10 C16 H16 119.8 . . ?
C15 C16 H16 119.8 . . ?
C18 C19 C20B 109.6(12) . . ?
C18 C19 C18B 24.2(7) . . ?
C20B C19 C18B 115.9(14) . . ?
C18 C19 C20 116.5(9) . . ?
C20B C19 C20 21.5(8) . . ?
C18B C19 C20 113.0(11) . . ?
C18 C19 C19 121.9(7) . 2_755 ?
C20B C19 C19 123.0(11) . 2_755 ?
C18B C19 C19 121.1(10) . 2_755 ?
C20 C19 C19 121.5(7) . 2_755 ?
C17B N1 C21B 121.8(16) . . ?
C17B N1 C17 21.4(10) . . ?
C21B N1 C17 116.4(13) . . ?
C17B N1 O13 119.9(12) . . ?
C21B N1 O13 118.1(11) . . ?
C17 N1 O13 119.7(8) . . ?
C17B N1 C21 115.3(13) . . ?
C21B N1 C21 23.5(8) . . ?
C17 N1 C21 119.7(10) . . ?
O13 N1 C21 120.6(7) . . ?
N1 C17 C18 121.1(13) . . ?
N1 C17 H17 119.4 . . ?
C18 C17 H17 119.4 . . ?
C17 C18 C19 121.8(11) . . ?
C17 C18 H18 119.1 . . ?
C19 C18 H18 119.1 . . ?
C21 C20 C19 120.0(11) . . ?
C21 C20 H20 120.0 . . ?
C19 C20 H20 120.0 . . ?
N1 C21 C20 120.5(11) . . ?
N1 C21 H21 119.7 . . ?
C20 C21 H21 119.7 . . ?
N1 C17B C18B 121(2) . . ?
N1 C17B H17B 119.6 . . ?
C18B C17B H17B 119.6 . . ?
C19 C18B C17B 119.3(17) . . ?
C19 C18B H18B 120.4 . . ?
C17B C18B H18B 120.4 . . ?
C21B C20B C19 124.1(18) . . ?
C21B C20B H20B 117.9 . . ?
C19 C20B H20B 117.9 . . ?
N1 C21B C20B 118.0(18) . . ?
N1 C21B H21B 121.0 . . ?
C20B C21B H21B 121.0 . . ?
N2 C22 C23 120.9(4) . . ?
N2 C22 H22 119.5 . . ?
C23 C22 H22 119.5 . . ?
C22 C23 C24 121.0(4) . . ?
C22 C23 H23 119.5 . . ?
C24 C23 H23 119.5 . . ?
C25 C24 C23 116.6(4) . . ?
C25 C24 C24 120.8(5) . 2_556 ?
C23 C24 C24 122.6(5) . 2_556 ?
C26 C25 C24 120.6(5) . . ?
C26 C25 H25 119.7 . . ?
C24 C25 H25 119.7 . . ?
N2 C26 C25 120.7(5) . . ?
N2 C26 H26 119.7 . . ?
C25 C26 H26 119.7 . . ?
O14 N2 C22 120.2(4) . . ?
O14 N2 C26 120.0(4) . . ?
C22 N2 C26 119.8(4) . . ?
C1 O1 Cd1 131.1(3) . . ?
C1 O2 Cd2 101.3(3) . . ?
C6 O5 H5A 109.5 . . ?
C9 O7 Cd2 104.8(3) . 2_666 ?
C9 O7 Cd1 135.3(3) . . ?
Cd2 O7 Cd1 97.26(12) 2_666 . ?
C14 O9 Cd2 119.4(3) . 2_766 ?
C14 O10 Cd1 135.0(4) . 1_655 ?
N1 O13 Cd2 124.3(2) . . ?
N2 O14 Cd2 117.5(3) . . ?

_diffrn_measured_fraction_theta_max 0.980
_diffrn_reflns_theta_full        27.00
_diffrn_measured_fraction_theta_full 0.980
_refine_diff_density_max         0.753
_refine_diff_density_min         -0.871
_refine_diff_density_rms         0.153

#===END

data_3
_database_code_depnum_ccdc_archive 'CCDC 705564'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C21 H19 Gd N3 O17'
_chemical_formula_weight         742.64

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

_cell_length_a                   9.9484(9)
_cell_length_b                   10.7880(10)
_cell_length_c                   13.8678(13)
_cell_angle_alpha                92.9090(10)
_cell_angle_beta                 108.763(2)
_cell_angle_gamma                117.2770(10)
_cell_volume                     1217.32(19)
_cell_formula_units_Z            2
_cell_measurement_temperature    299(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.13
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.026
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             732
_exptl_absorpt_coefficient_mu    2.820
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   'SADABS(Bruker, 2000)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      299(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13606
_diffrn_reflns_av_R_equivalents  0.0331
_diffrn_reflns_av_sigmaI/netI    0.0458
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.60
_diffrn_reflns_theta_max         27.00
_reflns_number_total             5184
_reflns_number_gt                4612
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0223P)²+3.6652P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5184
_refine_ls_number_parameters     406
_refine_ls_number_restraints     13
_refine_ls_R_factor_all          0.0388
_refine_ls_R_factor_gt           0.0304
_refine_ls_wR_factor_ref         0.0801
_refine_ls_wR_factor_gt          0.0637
_refine_ls_goodness_of_fit_ref   1.148
_refine_ls_restrained_S_all      1.147
_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
Gd1 Gd 0.76607(3) 1.03453(2) -0.003442(17) 0.01638(8) Uani 1 1 d . . .
C1 C 0.9800(6) 1.1436(5) 0.3373(4) 0.0253(11) Uani 1 1 d . . .
C2 C 0.8803(6) 1.0847(5) 0.3932(4) 0.0252(11) Uani 1 1 d . . .
H2 H 0.7700 1.0161 0.3577 0.030 Uiso 1 1 calc R . .
C3 C 0.9467(7) 1.1292(5) 0.5022(4) 0.0272(11) Uani 1 1 d . . .
C4 C 1.1089(6) 1.2333(5) 0.5546(4) 0.0273(11) Uani 1 1 d . . .
H4 H 1.1524 1.2679 0.6268 0.033 Uiso 1 1 calc R . .
C5 C 1.2048(6) 1.2849(5) 0.4977(4) 0.0259(11) Uani 1 1 d . . .
C6 C 1.1456(6) 1.2433(5) 0.3892(4) 0.0275(11) Uani 1 1 d . . .
H6 H 1.2139 1.2806 0.3530 0.033 Uiso 1 1 calc R . .
C7 C 0.9064(6) 1.1004(5) 0.2191(4) 0.0227(10) Uani 1 1 d . . .
C8 C 0.8473(7) 1.0716(5) 0.5666(4) 0.0272(11) Uani 1 1 d . . .
N3 N 1.3801(6) 1.3927(5) 0.5574(3) 0.0342(11) Uani 1 1 d . . .
C10 C 0.3371(6) 0.5970(4) -0.0852(3) 0.0184(9) Uani 1 1 d . . .
C11 C 0.4452(5) 0.5839(5) -0.1213(3) 0.0184(9) Uani 1 1 d . . .
H11 H 0.5276 0.6637 -0.1308 0.022 Uiso 1 1 calc R . .
C12 C 0.4286(6) 0.4506(5) -0.1428(3) 0.0203(10) Uani 1 1 d . . .
C13 C 0.3135(5) 0.3304(5) -0.1253(4) 0.0195(9) Uani 1 1 d . . .
H13 H 0.3066 0.2420 -0.1397 0.023 Uiso 1 1 calc R . .
C14 C 0.2083(6) 0.3443(5) -0.0856(3) 0.0196(10) Uani 1 1 d . . .
C15 C 0.2160(5) 0.4765(4) -0.0686(3) 0.0171(9) Uani 1 1 d . . .
H15 H 0.1411 0.4847 -0.0463 0.020 Uiso 1 1 calc R . .
C16 C 0.3573(6) 0.7443(4) -0.0587(3) 0.0179(9) Uani 1 1 d . . .
N2 N 0.5449(6) 0.4384(5) -0.1803(3) 0.0306(10) Uani 1 1 d . . .
C18 C 0.0961(6) 0.2179(4) -0.0544(3) 0.0208(10) Uani 1 1 d . . .
C19 C 0.3244(6) 0.7326(5) 0.4972(4) 0.0281(11) Uani 1 1 d . . .
H19 H 0.3764 0.7717 0.4524 0.034 Uiso 1 1 calc R . .
C20 C 0.1682(7) 0.6195(6) 0.4572(4) 0.0320(12) Uani 1 1 d . . .
H20 H 0.1161 0.5807 0.3852 0.038 Uiso 1 1 calc R . .
C21 C 0.0848(6) 0.5605(5) 0.5212(4) 0.0236(10) Uani 1 1 d . . .
C22 C 0.1702(6) 0.6245(5) 0.6287(4) 0.0290(11) Uani 1 1 d . . .
H22 H 0.1190 0.5905 0.6748 0.035 Uiso 1 1 calc R . .
C23 C 0.3277(7) 0.7362(5) 0.6662(4) 0.0311(12) Uani 1 1 d . . .
H23 H 0.3834 0.7772 0.7378 0.037 Uiso 1 1 calc R . .
N1 N 0.4034(5) 0.7877(4) 0.6005(3) 0.0257(9) Uani 1 1 d . . .
O1 O 0.7542(4) 1.0172(4) 0.1722(3) 0.0272(8) Uani 1 1 d . . .
O2 O 0.9995(4) 1.1518(3) 0.1707(2) 0.0253(7) Uani 1 1 d . . .
O3 O 0.6959(5) 0.9776(4) 0.5128(3) 0.0424(10) Uani 1 1 d D . .
H3 H 0.649(8) 0.947(7) 0.552(5) 0.064 Uiso 1 1 d D . .
O4 O 0.9082(5) 1.1111(4) 0.6617(3) 0.0394(10) Uani 1 1 d . . .
O5 O 1.4124(5) 1.4895(5) 0.6264(3) 0.0517(12) Uani 1 1 d . . .
O6 O 1.4806(5) 1.3785(5) 0.5341(4) 0.0528(12) Uani 1 1 d . . .
O7 O 0.4981(4) 0.8501(3) -0.0375(3) 0.0266(8) Uani 1 1 d . . .
O8 O 0.2365(4) 0.7527(3) -0.0583(3) 0.0260(8) Uani 1 1 d . . .
O9 O 0.6693(5) 0.5487(4) -0.1710(3) 0.0398(9) Uani 1 1 d . . .
O10 O 0.5150(6) 0.3192(5) -0.2162(4) 0.0623(14) Uani 1 1 d . . .
O11 O 0.1329(4) 0.1207(3) -0.0393(3) 0.0254(7) Uani 1 1 d . . .
O12 O -0.0248(4) 0.2156(3) -0.0432(3) 0.0256(7) Uani 1 1 d . . .
O13 O 0.5845(5) 1.0628(4) -0.1520(3) 0.0298(8) Uani 1 1 d D . .
H13A H 0.624(6) 1.116(5) -0.188(4) 0.045 Uiso 1 1 d D . .
H13B H 0.497(4) 1.058(6) -0.163(5) 0.045 Uiso 1 1 d D . .
O14 O 0.7377(5) 0.9011(4) -0.1626(3) 0.0294(8) Uani 1 1 d D . .
H14A H 0.810(5) 0.886(7) -0.163(4) 0.044 Uiso 1 1 d D . .
H14B H 0.688(6) 0.899(7) -0.223(2) 0.044 Uiso 1 1 d D . .
O15 O 0.5584(5) 0.8940(4) 0.6401(3) 0.0381(9) Uani 1 1 d . . .
O16 O 0.2633(5) 0.7770(4) 0.2642(3) 0.0442(10) Uani 1 1 d D . .
H16A H 0.200(6) 0.805(6) 0.267(6) 0.066 Uiso 1 1 d D . .
H16B H 0.203(6) 0.693(3) 0.229(5) 0.066 Uiso 1 1 d D . .
O17 O 0.0716(6) 0.4716(5) 0.2102(4) 0.0465(11) Uani 1 1 d D . .
H17A H 0.151(5) 0.464(8) 0.212(5) 0.070 Uiso 1 1 d D . .
H17B H -0.004(5) 0.416(6) 0.156(3) 0.070 Uiso 1 1 d D . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Gd1 O11 2.329(3) 2_665 ?
Gd1 O7 2.350(3) . ?
Gd1 O12 2.360(3) 1_665 ?
Gd1 O13 2.404(3) . ?
Gd1 O8 2.423(3) 2_675 ?
Gd1 O14 2.435(3) . ?
Gd1 O1 2.489(3) . ?
Gd1 O2 2.493(3) . ?
Gd1 C7 2.842(5) . ?
C1 C6 1.387(7) . ?
C1 C2 1.397(7) . ?
C1 C7 1.510(6) . ?
C2 C3 1.395(7) . ?
C2 H2 0.9300 . ?
C3 C4 1.376(7) . ?
C3 C8 1.491(7) . ?
C4 C5 1.372(7) . ?
C4 H4 0.9300 . ?
C5 C6 1.391(7) . ?
C5 N3 1.481(6) . ?
C6 H6 0.9300 . ?
C7 O2 1.258(6) . ?
C7 O1 1.258(6) . ?
C8 O4 1.217(6) . ?
C8 O3 1.286(6) . ?
N3 O6 1.213(6) . ?
N3 O5 1.225(6) . ?
C10 C11 1.380(6) . ?
C10 C15 1.402(6) . ?
C10 C16 1.516(6) . ?
C11 C12 1.376(6) . ?
C11 H11 0.9300 . ?
C12 C13 1.379(6) . ?
C12 N2 1.465(6) . ?
C13 C14 1.389(6) . ?
C13 H13 0.9300 . ?
C14 C15 1.396(6) . ?
C14 C18 1.505(6) . ?
C15 H15 0.9300 . ?
C16 O8 1.248(5) . ?
C16 O7 1.260(5) . ?
N2 O10 1.216(6) . ?
N2 O9 1.223(6) . ?
C18 O12 1.250(6) . ?
C18 O11 1.267(5) . ?
C19 N1 1.336(6) . ?
C19 C20 1.360(7) . ?
C19 H19 0.9300 . ?
C20 C21 1.389(7) . ?
C20 H20 0.9300 . ?
C21 C22 1.401(7) . ?
C21 C21 1.471(10) 2_566 ?
C22 C23 1.363(7) . ?
C22 H22 0.9300 . ?
C23 N1 1.347(6) . ?
C23 H23 0.9300 . ?
N1 O15 1.328(5) . ?
O3 H3 0.82(2) . ?
O8 Gd1 2.423(3) 2_675 ?
O11 Gd1 2.329(3) 2_665 ?
O12 Gd1 2.360(3) 1_445 ?
O13 H13A 0.823(19) . ?
O13 H13B 0.812(19) . ?
O14 H14A 0.810(19) . ?
O14 H14B 0.816(19) . ?
O16 H16A 0.83(2) . ?
O16 H16B 0.82(2) . ?
O17 H17A 0.82(2) . ?
O17 H17B 0.82(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O11 Gd1 O7 90.78(12) 2_665 . ?
O11 Gd1 O12 101.91(12) 2_665 1_665 ?
O7 Gd1 O12 155.70(12) . 1_665 ?
O11 Gd1 O13 139.38(12) 2_665 . ?
O7 Gd1 O13 72.85(12) . . ?
O12 Gd1 O13 84.23(12) 1_665 . ?
O11 Gd1 O8 146.50(12) 2_665 2_675 ?
O7 Gd1 O8 102.69(11) . 2_675 ?
O12 Gd1 O8 77.96(11) 1_665 2_675 ?
O13 Gd1 O8 74.12(12) . 2_675 ?
O11 Gd1 O14 70.55(12) 2_665 . ?
O7 Gd1 O14 85.48(12) . . ?
O12 Gd1 O14 79.49(12) 1_665 . ?
O13 Gd1 O14 71.27(13) . . ?
O8 Gd1 O14 140.14(12) 2_675 . ?
O11 Gd1 O1 79.24(12) 2_665 . ?
O7 Gd1 O1 75.02(12) . . ?
O12 Gd1 O1 127.40(11) 1_665 . ?
O13 Gd1 O1 128.47(12) . . ?
O8 Gd1 O1 75.01(11) 2_675 . ?
O14 Gd1 O1 143.67(12) . . ?
O11 Gd1 O2 72.03(11) 2_665 . ?
O7 Gd1 O2 126.55(11) . . ?
O12 Gd1 O2 77.44(11) 1_665 . ?
O13 Gd1 O2 147.00(12) . . ?
O8 Gd1 O2 75.35(11) 2_675 . ?
O14 Gd1 O2 130.27(12) . . ?
O1 Gd1 O2 52.49(11) . . ?
O11 Gd1 C7 74.54(12) 2_665 . ?
O7 Gd1 C7 100.93(13) . . ?
O12 Gd1 C7 102.39(13) 1_665 . ?
O13 Gd1 C7 144.01(13) . . ?
O8 Gd1 C7 72.87(12) 2_675 . ?
O14 Gd1 C7 144.59(13) . . ?
O1 Gd1 C7 26.25(12) . . ?
O2 Gd1 C7 26.26(12) . . ?
C6 C1 C2 120.8(5) . . ?
C6 C1 C7 119.4(4) . . ?
C2 C1 C7 119.8(4) . . ?
C3 C2 C1 119.8(5) . . ?
C3 C2 H2 120.1 . . ?
C1 C2 H2 120.1 . . ?
C4 C3 C2 120.2(5) . . ?
C4 C3 C8 117.2(4) . . ?
C2 C3 C8 122.6(5) . . ?
C5 C4 C3 118.5(4) . . ?
C5 C4 H4 120.8 . . ?
C3 C4 H4 120.8 . . ?
C4 C5 C6 123.7(5) . . ?
C4 C5 N3 116.8(4) . . ?
C6 C5 N3 119.5(5) . . ?
C1 C6 C5 116.9(5) . . ?
C1 C6 H6 121.5 . . ?
C5 C6 H6 121.5 . . ?
O2 C7 O1 122.2(4) . . ?
O2 C7 C1 118.6(4) . . ?
O1 C7 C1 119.2(4) . . ?
O2 C7 Gd1 61.2(2) . . ?
O1 C7 Gd1 61.0(2) . . ?
C1 C7 Gd1 176.4(3) . . ?
O4 C8 O3 124.4(5) . . ?
O4 C8 C3 121.5(5) . . ?
O3 C8 C3 114.1(4) . . ?
O6 N3 O5 125.1(5) . . ?
O6 N3 C5 117.5(5) . . ?
O5 N3 C5 117.5(5) . . ?
C11 C10 C15 120.0(4) . . ?
C11 C10 C16 118.9(4) . . ?
C15 C10 C16 121.0(4) . . ?
C12 C11 C10 118.7(4) . . ?
C12 C11 H11 120.7 . . ?
C10 C11 H11 120.7 . . ?
C11 C12 C13 122.9(4) . . ?
C11 C12 N2 118.1(4) . . ?
C13 C12 N2 118.9(4) . . ?
C12 C13 C14 118.5(4) . . ?
C12 C13 H13 120.8 . . ?
C14 C13 H13 120.8 . . ?
C13 C14 C15 119.9(4) . . ?
C13 C14 C18 118.7(4) . . ?
C15 C14 C18 121.3(4) . . ?
C14 C15 C10 119.9(4) . . ?
C14 C15 H15 120.1 . . ?
C10 C15 H15 120.1 . . ?
O8 C16 O7 124.8(4) . . ?
O8 C16 C10 118.8(4) . . ?
O7 C16 C10 116.4(4) . . ?
O10 N2 O9 123.6(5) . . ?
O10 N2 C12 118.4(4) . . ?
O9 N2 C12 118.0(4) . . ?
O12 C18 O11 124.0(4) . . ?
O12 C18 C14 119.0(4) . . ?
O11 C18 C14 117.0(4) . . ?
N1 C19 C20 120.3(5) . . ?
N1 C19 H19 119.8 . . ?
C20 C19 H19 119.8 . . ?
C19 C20 C21 121.5(5) . . ?
C19 C20 H20 119.2 . . ?
C21 C20 H20 119.2 . . ?
C20 C21 C22 116.3(5) . . ?
C20 C21 C21 122.1(5) . 2_566 ?
C22 C21 C21 121.6(6) . 2_566 ?
C23 C22 C21 120.6(5) . . ?
C23 C22 H22 119.7 . . ?
C21 C22 H22 119.7 . . ?
N1 C23 C22 120.6(5) . . ?
N1 C23 H23 119.7 . . ?
C22 C23 H23 119.7 . . ?
O15 N1 C19 120.3(4) . . ?
O15 N1 C23 119.0(4) . . ?
C19 N1 C23 120.7(4) . . ?
C7 O1 Gd1 92.7(3) . . ?
C7 O2 Gd1 92.5(3) . . ?
C8 O3 H3 110(5) . . ?
C16 O7 Gd1 175.4(3) . . ?
C16 O8 Gd1 127.4(3) . 2_675 ?
C18 O11 Gd1 172.6(3) . 2_665 ?
C18 O12 Gd1 129.3(3) . 1_445 ?
Gd1 O13 H13A 119(4) . . ?
Gd1 O13 H13B 131(4) . . ?
H13A O13 H13B 105(3) . . ?
Gd1 O14 H14A 120(4) . . ?
Gd1 O14 H14B 127(4) . . ?
H14A O14 H14B 107(3) . . ?
H16A O16 H16B 105(3) . . ?
H17A O17 H17B 105(3) . . ?

_diffrn_measured_fraction_theta_max 0.976
_diffrn_reflns_theta_full        27.00
_diffrn_measured_fraction_theta_full 0.976
_refine_diff_density_max         1.376
_refine_diff_density_min         -0.755
_refine_diff_density_rms         0.170
#===END


# Attachment '080515bm.cif'

data_080515bm
_database_code_depnum_ccdc_archive 'CCDC 705565'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C26 H21 Mn N5 O6'
_chemical_formula_weight         554.42

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P21/n
_symmetry_space_group_name_Hall  '-P 2yn'

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

_cell_length_a                   9.7413(9)
_cell_length_b                   13.2603(13)
_cell_length_c                   18.4924(18)
_cell_angle_alpha                90.00
_cell_angle_beta                 98.520(2)
_cell_angle_gamma                90.00
_cell_volume                     2362.3(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       plate
_exptl_crystal_colour            'light yellow'
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.559
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1140
_exptl_absorpt_coefficient_mu    0.614
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   'SADABS(Bruker, 2000)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            14961
_diffrn_reflns_av_R_equivalents  0.1005
_diffrn_reflns_av_sigmaI/netI    0.0984
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.90
_diffrn_reflns_theta_max         26.00
_reflns_number_total             4638
_reflns_number_gt                3079
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0477P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4638
_refine_ls_number_parameters     343
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0891
_refine_ls_R_factor_gt           0.0556
_refine_ls_wR_factor_ref         0.1186
_refine_ls_wR_factor_gt          0.1051
_refine_ls_goodness_of_fit_ref   0.894
_refine_ls_restrained_S_all      0.894
_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
N2 N 0.2145(3) 0.59464(19) 0.48233(14) 0.0364(6) Uani 1 1 d . . .
C9 C 0.2230(3) 0.5323(2) 0.53820(17) 0.0364(8) Uani 1 1 d . . .
H9 H 0.2927 0.4842 0.5482 0.044 Uiso 1 1 calc R . .
N3 N 0.1210(3) 0.54476(19) 0.57973(13) 0.0336(6) Uani 1 1 d . . .
C10 C 0.1160(4) 0.4993(2) 0.65118(18) 0.0423(9) Uani 1 1 d . . .
H10A H 0.1847 0.4460 0.6595 0.051 Uiso 1 1 calc R . .
H10B H 0.0253 0.4693 0.6516 0.051 Uiso 1 1 calc R . .
Mn1 Mn -0.13716(5) 0.91233(3) 0.90129(2) 0.03172(16) Uani 1 1 d . . .
C1 C -0.0480(3) 1.1422(2) 0.94667(19) 0.0357(8) Uani 1 1 d . . .
C2 C -0.0437(3) 1.2401(2) 0.90483(16) 0.0309(7) Uani 1 1 d . . .
C3 C -0.1103(3) 1.2479(2) 0.83292(17) 0.0361(8) Uani 1 1 d . . .
H3 H -0.1528 1.1914 0.8097 0.043 Uiso 1 1 calc R . .
C4 C -0.1896(3) 1.3491(4) 0.71769(19) 0.0501(10) Uani 1 1 d . . .
C5 C -0.1144(3) 1.3389(2) 0.79539(17) 0.0367(8) Uani 1 1 d . . .
C6 C -0.0488(3) 1.4219(2) 0.82980(18) 0.0405(8) Uani 1 1 d . . .
H6 H -0.0523 1.4839 0.8061 0.049 Uiso 1 1 calc R . .
C7 C 0.0219(3) 1.4119(2) 0.89973(17) 0.0355(8) Uani 1 1 d . . .
C8 C 0.0244(3) 1.3229(2) 0.93865(16) 0.0324(7) Uani 1 1 d . . .
H8 H 0.0705 1.3187 0.9863 0.039 Uiso 1 1 calc R . .
C11 C 0.0387(3) 0.6234(2) 0.54848(17) 0.0316(7) Uani 1 1 d . . .
C12 C -0.0784(3) 0.6692(2) 0.56872(18) 0.0420(8) Uani 1 1 d . . .
H12 H -0.1181 0.6470 0.6086 0.050 Uiso 1 1 calc R . .
C13 C -0.1320(3) 0.7491(3) 0.52639(19) 0.0461(9) Uani 1 1 d . . .
H13 H -0.2097 0.7825 0.5381 0.055 Uiso 1 1 calc R . .
C14 C -0.0725(4) 0.7817(3) 0.46606(19) 0.0466(9) Uani 1 1 d . . .
H14 H -0.1115 0.8363 0.4388 0.056 Uiso 1 1 calc R . .
C15 C 0.0423(4) 0.7349(2) 0.44611(17) 0.0433(9) Uani 1 1 d . . .
H15 H 0.0809 0.7565 0.4057 0.052 Uiso 1 1 calc R . .
C16 C 0.0986(3) 0.6544(2) 0.48843(16) 0.0319(7) Uani 1 1 d . . .
C17 C 0.1437(4) 0.5770(2) 0.71301(17) 0.0427(9) Uani 1 1 d . . .
H17A H 0.0613 0.6182 0.7128 0.051 Uiso 1 1 calc R . .
H17B H 0.1598 0.5415 0.7593 0.051 Uiso 1 1 calc R . .
C18 C 0.2657(3) 0.6454(2) 0.70808(17) 0.0418(8) Uani 1 1 d . . .
H18A H 0.2501 0.6810 0.6618 0.050 Uiso 1 1 calc R . .
H18B H 0.3485 0.6046 0.7088 0.050 Uiso 1 1 calc R . .
C19 C 0.2902(3) 0.7218(3) 0.76955(19) 0.0472(9) Uani 1 1 d . . .
H19A H 0.3108 0.6859 0.8156 0.057 Uiso 1 1 calc R . .
H19B H 0.3712 0.7617 0.7635 0.057 Uiso 1 1 calc R . .
C20 C 0.1094(3) 0.8049(2) 0.83304(17) 0.0378(8) Uani 1 1 d . . .
H20 H 0.1301 0.7680 0.8760 0.045 Uiso 1 1 calc R . .
C21 C 0.0161(3) 0.9106(2) 0.75299(17) 0.0363(8) Uani 1 1 d . . .
C22 C -0.0645(4) 0.9855(2) 0.7138(2) 0.0469(9) Uani 1 1 d . . .
H22 H -0.1313 1.0210 0.7344 0.056 Uiso 1 1 calc R . .
C23 C -0.0410(4) 1.0043(3) 0.6439(2) 0.0552(10) Uani 1 1 d . . .
H23 H -0.0940 1.0531 0.6165 0.066 Uiso 1 1 calc R . .
C24 C 0.0606(4) 0.9522(3) 0.6121(2) 0.0551(10) Uani 1 1 d . . .
H24 H 0.0744 0.9679 0.5647 0.066 Uiso 1 1 calc R . .
C25 C 0.1396(4) 0.8786(3) 0.64999(19) 0.0486(9) Uani 1 1 d . . .
H25 H 0.2068 0.8437 0.6292 0.058 Uiso 1 1 calc R . .
C26 C 0.1150(3) 0.8582(2) 0.72118(17) 0.0357(8) Uani 1 1 d . . .
N1 N 0.1001(3) 1.4994(2) 0.93418(18) 0.0522(8) Uani 1 1 d . . .
N4 N 0.0148(3) 0.87641(19) 0.82432(14) 0.0356(6) Uani 1 1 d . . .
N5 N 0.1742(3) 0.78984(19) 0.77369(14) 0.0376(7) Uani 1 1 d . . .
O1 O -0.0168(2) 1.14557(16) 1.01492(12) 0.0440(6) Uani 1 1 d . . .
O2 O -0.0877(3) 1.06601(16) 0.90932(14) 0.0524(7) Uani 1 1 d . . .
O3 O -0.2383(3) 1.2722(2) 0.68557(13) 0.0702(8) Uani 1 1 d . . .
O4 O -0.2005(3) 1.4356(2) 0.69060(13) 0.0618(8) Uani 1 1 d . . .
O5 O 0.0943(4) 1.57852(19) 0.90032(17) 0.0838(10) Uani 1 1 d . . .
O6 O 0.1679(3) 1.48818(19) 0.99469(16) 0.0675(8) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N2 C9 1.316(4) . ?
N2 C16 1.398(4) . ?
N2 Mn1 2.233(2) 4_675 ?
C9 N3 1.353(4) . ?
C9 H9 0.9300 . ?
N3 C11 1.388(4) . ?
N3 C10 1.460(4) . ?
C10 C17 1.533(4) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
Mn1 O2 2.094(2) . ?
Mn1 O1 2.133(2) 3_577 ?
Mn1 O4 2.165(3) 2_446 ?
Mn1 N2 2.233(3) 4_576 ?
Mn1 N4 2.251(3) . ?
C1 O2 1.253(4) . ?
C1 O1 1.254(4) . ?
C1 C2 1.514(4) . ?
C2 C8 1.383(4) . ?
C2 C3 1.395(4) . ?
C3 C5 1.389(4) . ?
C3 H3 0.9300 . ?
C4 O3 1.238(4) . ?
C4 O4 1.250(4) . ?
C4 C5 1.519(4) . ?
C5 C6 1.380(4) . ?
C6 C7 1.379(4) . ?
C6 H6 0.9300 . ?
C7 C8 1.381(4) . ?
C7 N1 1.479(4) . ?
C8 H8 0.9300 . ?
C11 C16 1.391(4) . ?
C11 C12 1.391(4) . ?
C12 C13 1.374(4) . ?
C12 H12 0.9300 . ?
C13 C14 1.399(4) . ?
C13 H13 0.9300 . ?
C14 C15 1.376(4) . ?
C14 H14 0.9300 . ?
C15 C16 1.388(4) . ?
C15 H15 0.9300 . ?
C17 C18 1.508(4) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C18 C19 1.515(4) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C19 N5 1.457(4) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 N4 1.315(4) . ?
C20 N5 1.359(4) . ?
C20 H20 0.9300 . ?
C21 C26 1.388(4) . ?
C21 N4 1.397(4) . ?
C21 C22 1.399(4) . ?
C22 C23 1.369(5) . ?
C22 H22 0.9300 . ?
C23 C24 1.405(5) . ?
C23 H23 0.9300 . ?
C24 C25 1.369(5) . ?
C24 H24 0.9300 . ?
C25 C26 1.399(4) . ?
C25 H25 0.9300 . ?
C26 N5 1.389(4) . ?
N1 O5 1.219(3) . ?
N1 O6 1.221(4) . ?
O1 Mn1 2.133(2) 3_577 ?
O4 Mn1 2.165(3) 2_456 ?

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
C9 N2 C16 104.5(3) . . ?
C9 N2 Mn1 121.9(2) . 4_675 ?
C16 N2 Mn1 133.5(2) . 4_675 ?
N2 C9 N3 113.8(3) . . ?
N2 C9 H9 123.1 . . ?
N3 C9 H9 123.1 . . ?
C9 N3 C11 106.4(3) . . ?
C9 N3 C10 126.1(3) . . ?
C11 N3 C10 126.3(3) . . ?
N3 C10 C17 111.8(2) . . ?
N3 C10 H10A 109.3 . . ?
C17 C10 H10A 109.3 . . ?
N3 C10 H10B 109.3 . . ?
C17 C10 H10B 109.3 . . ?
H10A C10 H10B 107.9 . . ?
O2 Mn1 O1 99.73(10) . 3_577 ?
O2 Mn1 O4 92.92(11) . 2_446 ?
O1 Mn1 O4 167.02(10) 3_577 2_446 ?
O2 Mn1 N2 99.08(9) . 4_576 ?
O1 Mn1 N2 87.29(9) 3_577 4_576 ?
O4 Mn1 N2 93.60(10) 2_446 4_576 ?
O2 Mn1 N4 94.86(9) . . ?
O1 Mn1 N4 85.75(9) 3_577 . ?
O4 Mn1 N4 90.35(9) 2_446 . ?
N2 Mn1 N4 165.29(9) 4_576 . ?
O2 C1 O1 126.3(3) . . ?
O2 C1 C2 116.0(3) . . ?
O1 C1 C2 117.6(3) . . ?
C8 C2 C3 119.7(3) . . ?
C8 C2 C1 119.8(3) . . ?
C3 C2 C1 120.5(3) . . ?
C5 C3 C2 121.1(3) . . ?
C5 C3 H3 119.5 . . ?
C2 C3 H3 119.5 . . ?
O3 C4 O4 124.0(4) . . ?
O3 C4 C5 118.5(4) . . ?
O4 C4 C5 117.5(4) . . ?
C6 C5 C3 119.0(3) . . ?
C6 C5 C4 119.4(3) . . ?
C3 C5 C4 121.6(3) . . ?
C7 C6 C5 119.3(3) . . ?
C7 C6 H6 120.4 . . ?
C5 C6 H6 120.4 . . ?
C6 C7 C8 122.6(3) . . ?
C6 C7 N1 118.9(3) . . ?
C8 C7 N1 118.5(3) . . ?
C7 C8 C2 118.2(3) . . ?
C7 C8 H8 120.9 . . ?
C2 C8 H8 120.9 . . ?
N3 C11 C16 105.6(3) . . ?
N3 C11 C12 131.5(3) . . ?
C16 C11 C12 122.9(3) . . ?
C13 C12 C11 116.2(3) . . ?
C13 C12 H12 121.9 . . ?
C11 C12 H12 121.9 . . ?
C12 C13 C14 121.7(3) . . ?
C12 C13 H13 119.2 . . ?
C14 C13 H13 119.2 . . ?
C15 C14 C13 121.6(3) . . ?
C15 C14 H14 119.2 . . ?
C13 C14 H14 119.2 . . ?
C14 C15 C16 117.7(3) . . ?
C14 C15 H15 121.2 . . ?
C16 C15 H15 121.2 . . ?
C15 C16 C11 120.0(3) . . ?
C15 C16 N2 130.3(3) . . ?
C11 C16 N2 109.7(3) . . ?
C18 C17 C10 114.4(3) . . ?
C18 C17 H17A 108.7 . . ?
C10 C17 H17A 108.7 . . ?
C18 C17 H17B 108.7 . . ?
C10 C17 H17B 108.7 . . ?
H17A C17 H17B 107.6 . . ?
C17 C18 C19 113.3(3) . . ?
C17 C18 H18A 108.9 . . ?
C19 C18 H18A 108.9 . . ?
C17 C18 H18B 108.9 . . ?
C19 C18 H18B 108.9 . . ?
H18A C18 H18B 107.7 . . ?
N5 C19 C18 114.6(3) . . ?
N5 C19 H19A 108.6 . . ?
C18 C19 H19A 108.6 . . ?
N5 C19 H19B 108.6 . . ?
C18 C19 H19B 108.6 . . ?
H19A C19 H19B 107.6 . . ?
N4 C20 N5 114.1(3) . . ?
N4 C20 H20 123.0 . . ?
N5 C20 H20 123.0 . . ?
C26 C21 N4 110.0(3) . . ?
C26 C21 C22 120.5(3) . . ?
N4 C21 C22 129.6(3) . . ?
C23 C22 C21 117.4(3) . . ?
C23 C22 H22 121.3 . . ?
C21 C22 H22 121.3 . . ?
C22 C23 C24 122.1(4) . . ?
C22 C23 H23 118.9 . . ?
C24 C23 H23 118.9 . . ?
C25 C24 C23 120.9(3) . . ?
C25 C24 H24 119.5 . . ?
C23 C24 H24 119.5 . . ?
C24 C25 C26 117.2(3) . . ?
C24 C25 H25 121.4 . . ?
C26 C25 H25 121.4 . . ?
C21 C26 N5 105.8(3) . . ?
C21 C26 C25 121.9(3) . . ?
N5 C26 C25 132.3(3) . . ?
O5 N1 O6 123.6(3) . . ?
O5 N1 C7 118.2(3) . . ?
O6 N1 C7 118.3(3) . . ?
C20 N4 C21 104.2(3) . . ?
C20 N4 Mn1 126.1(2) . . ?
C21 N4 Mn1 128.8(2) . . ?
C20 N5 C26 105.9(3) . . ?
C20 N5 C19 126.2(3) . . ?
C26 N5 C19 127.7(3) . . ?
C1 O1 Mn1 139.3(2) . 3_577 ?
C1 O2 Mn1 150.8(2) . . ?
C4 O4 Mn1 101.1(2) . 2_456 ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.396
_refine_diff_density_min         -0.325
_refine_diff_density_rms         0.077


