# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  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.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_1

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C27 H23 La2 N5 O14'
_chemical_formula_sum            'C27 H23 La2 N5 O14'
_chemical_formula_weight         919.32

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'
La La -0.2871 2.4523 '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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   8.1241(3)
_cell_length_b                   30.3843(10)
_cell_length_c                   15.6616(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3866.0(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    110(2)
_cell_measurement_reflns_used    3262
_cell_measurement_theta_min      2.40
_cell_measurement_theta_max      26.45

_exptl_crystal_description       needle
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.579
_exptl_crystal_F_000             1784
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    2.243
_shelx_estimated_absorpt_T_min   0.507
_shelx_estimated_absorpt_T_max   0.807
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.507
_exptl_absorpt_correction_T_max  0.807
_exptl_absorpt_process_details   'Sadabs, Bruker-AXS'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      110(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'ImuS microsource'
_diffrn_measurement_device_type  'ApexDuo, Bruker-AXS'
_diffrn_measurement_method       '1 deg. φ scans'
_diffrn_detector_area_resol_mean 1.75
_diffrn_reflns_number            24239
_diffrn_reflns_av_unetI/netI     0.0280
_diffrn_reflns_av_R_equivalents  0.0313
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.395
_diffrn_reflns_theta_max         26.450
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.934
_diffrn_measured_fraction_theta_full 0.966
_diffrn_reflns_Laue_measured_fraction_max 0.934
_diffrn_reflns_Laue_measured_fraction_full 0.966
_diffrn_reflns_point_group_measured_fraction_max 0.934
_diffrn_reflns_point_group_measured_fraction_full 0.966
_reflns_number_total             3799
_reflns_number_gt                3262
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Apex2, Bruker-AXS'
_computing_cell_refinement       'Apex2, Bruker-AXS'
_computing_data_reduction        'Saint, Bruker-AXS'
_computing_structure_solution    'Saint, Bruker-AXS'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 THe crystal contains also DMF crystallization solvent, positioned on,
 and disordered about the mirror planes, which could not be reliably
 modeled by discrete atoms. Its contribution was subtracted from the
 diffraction pattern, using the Squeeze technique and Platon software
 (Spek, 2009). The peripheral NMe2 residue of the metal-coordinated
 DMF ligand reveals partial disorder as well.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0435P)²+4.1176P] 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         3799
_refine_ls_number_parameters     228
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0510
_refine_ls_R_factor_gt           0.0434
_refine_ls_wR_factor_ref         0.1113
_refine_ls_wR_factor_gt          0.1085
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_restrained_S_all      1.080
_refine_ls_shift/su_max          0.032
_refine_ls_shift/su_mean         0.013

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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
La1 La 0.93440(4) 0.59121(2) 0.70363(2) 0.00748(12) Uani 1 1 d . . . . .
O2 O 0.8897(5) 0.46119(13) 0.3895(3) 0.0158(9) Uani 1 1 d . . . . .
O3 O 0.7418(5) 0.40625(12) 0.3387(2) 0.0125(9) Uani 1 1 d . . . . .
O4 O 0.4941(6) 0.52466(13) 0.7102(2) 0.0161(9) Uani 1 1 d . . . . .
O5 O 0.7389(5) 0.53863(13) 0.6513(3) 0.0206(10) Uani 1 1 d . . . . .
O6 O 1.1554(5) 0.63204(11) 0.8160(2) 0.0101(8) Uani 1 1 d . . . . .
O7 O 0.9888(5) 0.67043(12) 0.7339(3) 0.0162(9) Uani 1 1 d . . . . .
C8 C 0.6608(7) 0.43974(17) 0.4719(3) 0.0098(11) Uani 1 1 d . . . . .
C9 C 0.5288(8) 0.41202(18) 0.4866(4) 0.0141(13) Uani 1 1 d . . . . .
H9 H 0.5069 0.3894 0.4463 0.017 Uiso 1 1 calc R U . . .
N10 N 0.4306(7) 0.41547(16) 0.5547(3) 0.0206(12) Uani 1 1 d . . . . .
C11 C 0.4595(7) 0.44872(19) 0.6088(4) 0.0134(12) Uani 1 1 d . . . . .
H11 H 0.3875 0.4523 0.6561 0.016 Uiso 1 1 calc R U . . .
C12 C 0.5892(7) 0.47823(17) 0.5995(3) 0.0101(11) Uani 1 1 d . . . . .
C13 C 0.6921(7) 0.47300(17) 0.5305(3) 0.0119(12) Uani 1 1 d . . . . .
H13 H 0.7839 0.4920 0.5230 0.014 Uiso 1 1 calc R U . . .
C14 C 0.7676(8) 0.43579(17) 0.3938(4) 0.0135(12) Uani 1 1 d . . . . .
C15 C 0.6089(7) 0.51632(17) 0.6586(3) 0.0113(12) Uani 1 1 d . . . . .
C16 C 1.1480(7) 0.71064(16) 0.8315(4) 0.0104(11) Uani 1 1 d . . . . .
C17 C 1.2456(8) 0.71234(18) 0.9044(4) 0.0152(13) Uani 1 1 d . . . . .
H17 H 1.2804 0.6854 0.9293 0.018 Uiso 1 1 calc R U . . .
N18 N 1.2929(10) 0.7500 0.9413(5) 0.0220(18) Uani 1 2 d S T P . .
C19 C 1.0977(10) 0.7500 0.7953(5) 0.0104(16) Uani 1 2 d S T P . .
H19 H 1.0294 0.7500 0.7461 0.013 Uiso 1 2 calc R U P . .
C20 C 1.0964(7) 0.66846(18) 0.7920(3) 0.0105(12) Uani 1 1 d . . . . .
O21 O 0.9390(6) 0.61618(13) 0.5501(2) 0.0177(9) Uani 1 1 d . . . . .
C22 C 0.9385(8) 0.5929(2) 0.4848(4) 0.0174(13) Uani 1 1 d . . . . .
H22 H 0.8952 0.5640 0.4905 0.021 Uiso 1 1 calc R U . . .
N23 N 0.9903(10) 0.6039(2) 0.4108(4) 0.048(2) Uani 1 1 d D . . . .
C24 C 0.9845(12) 0.5736(4) 0.3377(5) 0.048(3) Uani 1 1 d . . . . .
H24A H 1.0969 0.5671 0.3187 0.064 Uiso 1 1 calc R U . . .
H24B H 0.9231 0.5873 0.2908 0.064 Uiso 1 1 calc R U . . .
H24C H 0.9298 0.5463 0.3548 0.064 Uiso 1 1 calc R U . . .
C25A C 1.098(2) 0.6422(5) 0.3974(8) 0.044(6) Uani 0.58(3) 1 d D . P A 1
H25A H 1.1075 0.6587 0.4509 0.066 Uiso 0.58(3) 1 calc R U P A 1
H25B H 1.0501 0.6612 0.3532 0.066 Uiso 0.58(3) 1 calc R U P A 1
H25C H 1.2067 0.6322 0.3792 0.066 Uiso 0.58(3) 1 calc R U P A 1
C25B C 0.965(7) 0.6510(5) 0.393(3) 0.046(17) Uiso 0.42(3) 1 d D . P A 2
H25D H 0.8545 0.6556 0.3704 0.069 Uiso 0.42(3) 1 calc R U P A 2
H25E H 1.0471 0.6611 0.3516 0.069 Uiso 0.42(3) 1 calc R U P A 2
H25F H 0.9781 0.6678 0.4464 0.069 Uiso 0.42(3) 1 calc R U P A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
La1 O5 2.397(4) . ?
La1 O4 2.479(4) 6_657 ?
La1 O7 2.493(4) . ?
La1 O21 2.521(4) . ?
La1 O3 2.555(4) 2_665 ?
La1 O2 2.589(4) 5_766 ?
La1 O6 2.602(4) 6_557 ?
La1 O3 2.714(4) 5_766 ?
La1 O6 2.804(4) . ?
La1 C14 2.978(6) 5_766 ?
La1 C20 3.026(6) . ?
O2 C14 1.259(7) . ?
O2 La1 2.589(4) 5_766 ?
O3 C14 1.264(7) . ?
O3 La1 2.555(4) 2_664 ?
O3 La1 2.714(4) 5_766 ?
O4 C15 1.259(7) . ?
O4 La1 2.479(4) 6_557 ?
O5 C15 1.260(7) . ?
O6 C20 1.263(7) . ?
O6 La1 2.602(4) 6_657 ?
O7 C20 1.264(7) . ?
C8 C9 1.383(8) . ?
C8 C13 1.388(8) . ?
C8 C14 1.504(8) . ?
C9 N10 1.335(8) . ?
N10 C11 1.340(7) . ?
C11 C12 1.391(8) . ?
C12 C13 1.376(8) . ?
C12 C15 1.491(7) . ?
C14 La1 2.978(6) 5_766 ?
C16 C19 1.385(7) . ?
C16 C17 1.391(8) . ?
C16 C20 1.483(7) . ?
C17 N18 1.338(7) . ?
N18 C17 1.338(7) 7_575 ?
C19 C16 1.385(7) 7_575 ?
O21 C22 1.243(7) . ?
C22 N23 1.277(8) . ?
N23 C25A 1.469(3) . ?
N23 C24 1.470(10) . ?
N23 C25B 1.471(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
O5 La1 O4 76.82(14) . 6_657 ?
O5 La1 O7 145.70(14) . . ?
O4 La1 O7 130.49(13) 6_657 . ?
O5 La1 O21 83.37(14) . . ?
O4 La1 O21 139.62(13) 6_657 . ?
O7 La1 O21 83.57(13) . . ?
O5 La1 O3 86.08(14) . 2_665 ?
O4 La1 O3 71.54(13) 6_657 2_665 ?
O7 La1 O3 85.01(13) . 2_665 ?
O21 La1 O3 142.05(13) . 2_665 ?
O5 La1 O2 76.31(14) . 5_766 ?
O4 La1 O2 72.38(13) 6_657 5_766 ?
O7 La1 O2 127.08(14) . 5_766 ?
O21 La1 O2 68.88(13) . 5_766 ?
O3 La1 O2 142.56(12) 2_665 5_766 ?
O5 La1 O6 72.55(13) . 6_557 ?
O4 La1 O6 128.57(13) 6_657 6_557 ?
O7 La1 O6 73.55(13) . 6_557 ?
O21 La1 O6 75.92(13) . 6_557 ?
O3 La1 O6 66.13(12) 2_665 6_557 ?
O2 La1 O6 135.01(13) 5_766 6_557 ?
O5 La1 O3 125.30(13) . 5_766 ?
O4 La1 O3 88.08(13) 6_657 5_766 ?
O7 La1 O3 81.20(13) . 5_766 ?
O21 La1 O3 75.18(13) . 5_766 ?
O3 La1 O3 138.10(11) 2_665 5_766 ?
O2 La1 O3 49.09(12) 5_766 5_766 ?
O6 La1 O3 143.32(11) 6_557 5_766 ?
O5 La1 O6 159.02(13) . . ?
O4 La1 O6 83.90(12) 6_657 . ?
O7 La1 O6 48.69(12) . . ?
O21 La1 O6 117.14(13) . . ?
O3 La1 O6 79.96(12) 2_665 . ?
O2 La1 O6 105.81(12) 5_766 . ?
O6 La1 O6 114.91(12) 6_557 . ?
O3 La1 O6 61.31(11) 5_766 . ?
O5 La1 C14 100.37(15) . 5_766 ?
O4 La1 C14 84.00(14) 6_657 5_766 ?
O7 La1 C14 102.66(15) . 5_766 ?
O21 La1 C14 65.28(15) . 5_766 ?
O3 La1 C14 152.66(14) 2_665 5_766 ?
O2 La1 C14 24.91(14) 5_766 5_766 ?
O6 La1 C14 141.17(14) 6_557 5_766 ?
O3 La1 C14 25.11(14) 5_766 5_766 ?
O6 La1 C14 85.59(14) . 5_766 ?
O5 La1 C20 164.03(15) . . ?
O4 La1 C20 107.36(14) 6_657 . ?
O7 La1 C20 24.08(14) . . ?
O21 La1 C20 101.33(14) . . ?
O3 La1 C20 80.88(14) 2_665 . ?
O2 La1 C20 119.65(14) 5_766 . ?
O6 La1 C20 93.63(13) 6_557 . ?
O3 La1 C20 70.62(13) 5_766 . ?
O6 La1 C20 24.65(13) . . ?
C14 La1 C20 95.43(16) 5_766 . ?
C14 O2 La1 95.1(3) . 5_766 ?
C14 O3 La1 129.6(3) . 2_664 ?
C14 O3 La1 89.2(3) . 5_766 ?
La1 O3 La1 109.90(13) 2_664 5_766 ?
C15 O4 La1 131.2(4) . 6_557 ?
C15 O5 La1 152.0(4) . . ?
C20 O6 La1 135.5(4) . 6_657 ?
C20 O6 La1 87.6(3) . . ?
La1 O6 La1 105.82(12) 6_657 . ?
C20 O7 La1 102.3(3) . . ?
C9 C8 C13 118.4(5) . . ?
C9 C8 C14 122.3(5) . . ?
C13 C8 C14 119.3(5) . . ?
N10 C9 C8 123.3(5) . . ?
C9 N10 C11 117.4(5) . . ?
N10 C11 C12 123.5(5) . . ?
C13 C12 C11 117.9(5) . . ?
C13 C12 C15 120.8(5) . . ?
C11 C12 C15 121.1(5) . . ?
C12 C13 C8 119.5(5) . . ?
O2 C14 O3 121.9(5) . . ?
O2 C14 C8 116.7(5) . . ?
O3 C14 C8 121.2(5) . . ?
O2 C14 La1 60.0(3) . 5_766 ?
O3 C14 La1 65.7(3) . 5_766 ?
C8 C14 La1 155.2(4) . 5_766 ?
O4 C15 O5 124.8(5) . . ?
O4 C15 C12 118.3(5) . . ?
O5 C15 C12 116.8(5) . . ?
C19 C16 C17 118.2(5) . . ?
C19 C16 C20 119.5(5) . . ?
C17 C16 C20 122.4(5) . . ?
N18 C17 C16 123.4(5) . . ?
C17 N18 C17 117.5(7) . 7_575 ?
C16 C19 C16 119.4(7) 7_575 . ?
O6 C20 O7 121.2(5) . . ?
O6 C20 C16 121.7(5) . . ?
O7 C20 C16 117.0(5) . . ?
O6 C20 La1 67.8(3) . . ?
O7 C20 La1 53.6(3) . . ?
C16 C20 La1 169.6(4) . . ?
C22 O21 La1 127.9(4) . . ?
O21 C22 N23 126.7(6) . . ?
C22 N23 C25A 122.1(7) . . ?
C22 N23 C24 122.2(7) . . ?
C25A N23 C24 113.8(8) . . ?
C22 N23 C25B 112.2(19) . . ?
C24 N23 C25B 117.4(18) . . ?

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.023 0.250 0.750 530 131 ' '
2 -0.043 0.750 0.250 530 131 ' '
_platon_squeeze_details          
;
 The residual density accounts for molecules of DMF crystallization
 solvent.
;

# start Validation report
_vrf_PLAT220_1                   
;
PROBLEM:  High Ueq for C24 and C25
RESPONSE:
The N-dimethyl residue of the metal-coordinated DMF ligand is
partly disordered.
;
# end Validation reply form

_refine_diff_density_max         2.277
_refine_diff_density_min         -2.023
_refine_diff_density_rms         0.155



_database_code_depnum_ccdc_archive 'CCDC 979166'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  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.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_2

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C27 H23 Ce2 N5 O14'
_chemical_formula_sum            'C27 H23 Ce2 N5 O14'
_chemical_formula_weight         921.74

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'
Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P nma'

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

_cell_length_a                   8.1162(4)
_cell_length_b                   30.2842(14)
_cell_length_c                   15.6709(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3851.8(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    110(2)
_cell_measurement_reflns_used    2869
_cell_measurement_theta_min      2.40
_cell_measurement_theta_max      25.1

_exptl_crystal_description       needles
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.07
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.589
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1792
_exptl_absorpt_coefficient_mu    2.397
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4791
_exptl_absorpt_correction_T_max  0.8502
_exptl_absorpt_process_details   'Sadabs, Bruker-AXS'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      110(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  'ApexDuo, Bruker-AXS'
_diffrn_measurement_method       '1 deg. φ and ω scans'
_diffrn_detector_area_resol_mean 1.75
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            15168
_diffrn_reflns_av_R_equivalents  0.0338
_diffrn_reflns_av_sigmaI/netI    0.0311
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         2.40
_diffrn_reflns_theta_max         25.10
_reflns_number_total             3379
_reflns_number_gt                2869
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Apex2, Bruker-AXS'
_computing_cell_refinement       'Saint, Bruker-AXS'
_computing_data_reduction        'Saint, Bruker-AXS'
_computing_structure_solution    'SHELXTL-2012 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_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. 

 The crystals contain severely disordered molecules of the DMF
 crystallization solvent within the interstitial voids, which could not
 be modeled reliably by discrete atoms. Its contribution to the
 diffraction pattern was thus subtracted by the Squeeze procedure,
 using the PLATON software (Spek, 2009).
 The metal coordinated DMF ligand is also partly disordered.


;

_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)+(0.0469P)²+6.1116P] 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         3379
_refine_ls_number_parameters     218
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0478
_refine_ls_R_factor_gt           0.0401
_refine_ls_wR_factor_ref         0.1028
_refine_ls_wR_factor_gt          0.1004
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_restrained_S_all      1.087
_refine_ls_shift/su_max          0.033
_refine_ls_shift/su_mean         0.002

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
Ce1 Ce 0.43911(4) 0.908691(9) 0.703925(18) 0.00767(13) Uani 1 1 d . . .
O2 O 0.6625(5) 0.86861(11) 0.8162(2) 0.0093(8) Uani 1 1 d . . .
O3 O 0.3865(5) 1.03933(12) 0.3871(2) 0.0137(9) Uani 1 1 d . . .
O4 O 0.2483(5) 0.96207(12) 0.6512(3) 0.0185(9) Uani 1 1 d . A .
O5 O 0.4933(5) 0.83022(12) 0.7345(2) 0.0138(9) Uani 1 1 d . . .
O6 O 0.2343(5) 1.09476(12) 0.3383(2) 0.0127(9) Uani 1 1 d . . .
O7 O 0.0027(5) 0.97380(13) 0.7094(2) 0.0149(9) Uani 1 1 d . . .
N8 N -0.0736(6) 1.08316(15) 0.5550(3) 0.0185(12) Uani 1 1 d . A .
N9 N 0.8025(10) 0.7500 0.9406(4) 0.0198(17) Uani 1 2 d S . .
C10 C 0.6015(7) 0.83181(18) 0.7914(3) 0.0098(12) Uani 1 1 d . . .
C11 C 0.6010(10) 0.7500 0.7953(5) 0.0094(16) Uani 1 2 d S . .
H11 H 0.5295 0.7500 0.7473 0.011 Uiso 1 2 calc SR . .
C12 C 0.1568(7) 1.06026(17) 0.4710(3) 0.0085(11) Uani 1 1 d . A .
C13 C 0.0232(7) 1.08705(17) 0.4867(4) 0.0123(12) Uani 1 1 d . . .
H13 H -0.0014 1.1096 0.4466 0.015 Uiso 1 1 calc R . .
C14 C 0.1158(7) 0.98313(17) 0.6587(3) 0.0096(12) Uani 1 1 d . . .
C15 C 0.2640(7) 1.06457(16) 0.3928(3) 0.0096(12) Uani 1 1 d . . .
C16 C -0.0404(7) 1.05007(18) 0.6091(4) 0.0127(12) Uani 1 1 d . . .
H16 H -0.1110 1.0461 0.6569 0.015 Uiso 1 1 calc R A .
C17 C 0.6543(7) 0.78963(16) 0.8311(3) 0.0106(12) Uani 1 1 d . . .
C18 C 0.0918(7) 1.02120(17) 0.5992(3) 0.0118(11) Uani 1 1 d . A .
C19 C 0.7517(7) 0.78767(17) 0.9038(3) 0.0139(13) Uani 1 1 d . A .
H19 H 0.7846 0.8148 0.9292 0.017 Uiso 1 1 calc R . .
C20 C 0.1934(7) 1.02692(16) 0.5298(3) 0.0107(12) Uani 1 1 d . . .
H20 H 0.2870 1.0085 0.5220 0.013 Uiso 1 1 calc R A .
O21 O 0.4448(5) 0.88346(13) 0.5523(2) 0.0187(9) Uani 1 1 d . A 1
C22 C 0.4434(7) 0.90695(19) 0.4872(4) 0.0175(13) Uani 1 1 d . A 1
H22 H 0.3891 0.9347 0.4928 0.021 Uiso 1 1 d R A 1
N23B N 0.463(3) 0.8865(7) 0.4085(11) 0.027(5) Uiso 0.35(2) 1 d P A 1
C24B C 0.478(3) 0.9144(9) 0.3308(15) 0.030(6) Uiso 0.35(2) 1 d P A 1
H24D H 0.4630 0.9460 0.3454 0.045 Uiso 0.35 1 d P A 1
H24E H 0.3786 0.9081 0.2876 0.045 Uiso 0.35 1 d P A 1
H24F H 0.5766 0.9090 0.3004 0.045 Uiso 0.35 1 d P A 1
C25B C 0.469(4) 0.8389(12) 0.394(2) 0.038(12) Uiso 0.35(2) 1 d P A 1
H25D H 0.4563 0.8231 0.4421 0.057 Uiso 0.35 1 d P A 1
H25E H 0.4941 0.8303 0.3406 0.057 Uiso 0.35 1 d P A 1
H25F H 0.3075 0.8348 0.3765 0.057 Uiso 0.35 1 d P A 1
N23A N 0.5076(14) 0.8999(3) 0.4138(5) 0.016(2) Uiso 0.65(2) 1 d P A 2
C24A C 0.4891(14) 0.9308(4) 0.3431(7) 0.021(3) Uiso 0.65(2) 1 d P A 2
H24A H 0.4254 0.9573 0.3609 0.032 Uiso 0.65 1 d P A 2
H24B H 0.4279 0.9183 0.2904 0.032 Uiso 0.65 1 d P A 2
H24C H 0.5989 0.9406 0.3213 0.032 Uiso 0.65 1 d P A 2
C25A C 0.5953(17) 0.8577(4) 0.3978(8) 0.043(4) Uiso 0.65(2) 1 d P A 2
H25A H 0.7012 0.8634 0.3756 0.064 Uiso 0.65 1 d P A 2
H25B H 0.5281 0.8398 0.3529 0.064 Uiso 0.65 1 d P A 2
H25C H 0.5950 0.8403 0.4512 0.064 Uiso 0.65 1 d P A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ce1 O4 2.386(4) . ?
Ce1 O7 2.449(4) 6_657 ?
Ce1 O5 2.464(4) . ?
Ce1 O21 2.496(4) . ?
Ce1 O6 2.535(4) 2_575 ?
Ce1 O3 2.552(4) 5_676 ?
Ce1 O2 2.572(4) 6_557 ?
Ce1 O6 2.734(4) 5_676 ?
Ce1 O2 2.803(4) . ?
Ce1 C15 2.960(6) 5_676 ?
Ce1 C10 3.007(5) . ?
O2 C10 1.280(6) . ?
O2 Ce1 2.572(4) 6_657 ?
O3 C15 1.257(7) . ?
O3 Ce1 2.552(4) 5_676 ?
O4 C14 1.256(7) . ?
O5 C10 1.253(7) . ?
O6 C15 1.274(6) . ?
O6 Ce1 2.535(4) 2_574 ?
O6 Ce1 2.734(4) 5_676 ?
O7 C14 1.247(7) . ?
O7 Ce1 2.449(4) 6_557 ?
N8 C13 1.333(8) . ?
N8 C16 1.340(7) . ?
N9 C19 1.343(6) 7_575 ?
N9 C19 1.343(6) . ?
C10 C17 1.484(7) . ?
C11 C17 1.394(6) . ?
C11 C17 1.394(6) 7_575 ?
C12 C13 1.377(8) . ?
C12 C20 1.399(7) . ?
C12 C15 1.508(8) . ?
C14 C18 1.495(7) . ?
C15 Ce1 2.960(6) 5_676 ?
C16 C18 1.393(8) . ?
C17 C19 1.388(8) . ?
C18 C20 1.375(8) . ?
O21 C22 1.244(7) . ?
C22 N23B 1.39(2) . ?
N23B C25B 1.46(4) . ?
N23B C24B 1.49(3) . ?
N23A C24A 1.460(14) . ?
N23A C25A 1.484(15) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4 Ce1 O7 77.49(14) . 6_657 ?
O4 Ce1 O5 146.79(14) . . ?
O7 Ce1 O5 129.13(13) 6_657 . ?
O4 Ce1 O21 83.67(14) . . ?
O7 Ce1 O21 140.38(13) 6_657 . ?
O5 Ce1 O21 83.48(13) . . ?
O4 Ce1 O6 87.44(13) . 2_575 ?
O7 Ce1 O6 71.91(12) 6_657 2_575 ?
O5 Ce1 O6 84.14(13) . 2_575 ?
O21 Ce1 O6 142.03(13) . 2_575 ?
O4 Ce1 O3 75.44(13) . 5_676 ?
O7 Ce1 O3 72.33(13) 6_657 5_676 ?
O5 Ce1 O3 127.18(13) . 5_676 ?
O21 Ce1 O3 69.32(12) . 5_676 ?
O6 Ce1 O3 142.88(11) 2_575 5_676 ?
O4 Ce1 O2 73.18(13) . 6_557 ?
O7 Ce1 O2 129.20(13) 6_657 6_557 ?
O5 Ce1 O2 74.01(12) . 6_557 ?
O21 Ce1 O2 75.80(13) . 6_557 ?
O6 Ce1 O2 66.29(12) 2_575 6_557 ?
O3 Ce1 O2 134.96(12) 5_676 6_557 ?
O4 Ce1 O6 124.83(12) . 5_676 ?
O7 Ce1 O6 87.75(13) 6_657 5_676 ?
O5 Ce1 O6 80.62(12) . 5_676 ?
O21 Ce1 O6 74.93(12) . 5_676 ?
O6 Ce1 O6 137.54(11) 2_575 5_676 ?
O3 Ce1 O6 49.51(11) 5_676 5_676 ?
O2 Ce1 O6 143.00(11) 6_557 5_676 ?
O4 Ce1 O2 158.50(12) . . ?
O7 Ce1 O2 82.19(12) 6_657 . ?
O5 Ce1 O2 49.06(11) . . ?
O21 Ce1 O2 116.95(12) . . ?
O6 Ce1 O2 79.61(12) 2_575 . ?
O3 Ce1 O2 105.02(12) 5_676 . ?
O2 Ce1 O2 115.93(11) 6_557 . ?
O6 Ce1 O2 60.56(11) 5_676 . ?
O4 Ce1 C15 99.53(14) . 5_676 ?
O7 Ce1 C15 83.81(14) 6_657 5_676 ?
O5 Ce1 C15 102.59(14) . 5_676 ?
O21 Ce1 C15 65.24(14) . 5_676 ?
O6 Ce1 C15 152.72(13) 2_575 5_676 ?
O3 Ce1 C15 24.99(13) 5_676 5_676 ?
O2 Ce1 C15 140.98(13) 6_557 5_676 ?
O6 Ce1 C15 25.47(13) 5_676 5_676 ?
O2 Ce1 C15 85.04(13) . 5_676 ?
O4 Ce1 C10 165.26(15) . . ?
O7 Ce1 C10 106.14(14) 6_657 . ?
O5 Ce1 C10 23.95(14) . . ?
O21 Ce1 C10 100.90(14) . . ?
O6 Ce1 C10 80.36(13) 2_575 . ?
O3 Ce1 C10 119.29(14) 5_676 . ?
O2 Ce1 C10 94.20(13) 6_557 . ?
O6 Ce1 C10 69.87(13) 5_676 . ?
O2 Ce1 C10 25.13(13) . . ?
C15 Ce1 C10 95.08(15) 5_676 . ?
C10 O2 Ce1 135.3(3) . 6_657 ?
C10 O2 Ce1 86.4(3) . . ?
Ce1 O2 Ce1 106.44(12) 6_657 . ?
C15 O3 Ce1 96.0(3) . 5_676 ?
C14 O4 Ce1 150.2(4) . . ?
C10 O5 Ce1 103.1(3) . . ?
C15 O6 Ce1 129.2(3) . 2_574 ?
C15 O6 Ce1 87.2(3) . 5_676 ?
Ce1 O6 Ce1 109.61(13) 2_574 5_676 ?
C14 O7 Ce1 133.7(4) . 6_557 ?
C13 N8 C16 117.1(5) . . ?
C19 N9 C19 116.3(7) 7_575 . ?
O5 C10 O2 121.4(5) . . ?
O5 C10 C17 117.9(5) . . ?
O2 C10 C17 120.7(5) . . ?
O5 C10 Ce1 53.0(3) . . ?
O2 C10 Ce1 68.5(3) . . ?
C17 C10 Ce1 169.9(4) . . ?
C17 C11 C17 118.9(7) . 7_575 ?
C13 C12 C20 118.3(5) . . ?
C13 C12 C15 123.3(5) . . ?
C20 C12 C15 118.4(5) . . ?
N8 C13 C12 123.8(5) . . ?
O7 C14 O4 125.1(5) . . ?
O7 C14 C18 118.5(5) . . ?
O4 C14 C18 116.4(5) . . ?
O3 C15 O6 122.5(5) . . ?
O3 C15 C12 117.5(5) . . ?
O6 C15 C12 119.9(5) . . ?
O3 C15 Ce1 59.0(3) . 5_676 ?
O6 C15 Ce1 67.3(3) . 5_676 ?
C12 C15 Ce1 155.4(4) . 5_676 ?
N8 C16 C18 123.6(5) . . ?
C19 C17 C11 118.1(5) . . ?
C19 C17 C10 123.0(5) . . ?
C11 C17 C10 118.9(5) . . ?
C20 C18 C16 118.1(5) . . ?
C20 C18 C14 120.8(5) . . ?
C16 C18 C14 121.0(5) . . ?
N9 C19 C17 124.3(5) . . ?
C18 C20 C12 119.0(5) . . ?
C22 O21 Ce1 127.3(4) . . ?
O21 C22 N23B 118.2(10) . . ?
C22 N23B C25B 125.4(19) . . ?
C22 N23B C24B 118.9(17) . . ?
C25B N23B C24B 116(2) . . ?
C24A N23A C25A 118.2(9) . . ?

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.025 0.250 0.750 444 243 ' '
2 -0.062 0.750 0.250 444 244 ' '
_platon_squeeze_details          
;
 The residual density accounts for disordered DMF crystallization
 solvent
;

# start Validation Reply Form
_vrf_PLAT201_2                   
;
PROBLEM:  isotropic atoms in the main residue
RESPONSE:  The metal-coordinated DMF ligand exhibits 2-fold disorder.
          The disordered NMe2 residue was thus assigned isotropic-Us only.
;
_vrf_PLAT220_2                   
;
PROBLEM:  large non-solvent Ueq(max)/Ueq(min)
RESPONSE: The disordered methyl residue has considerably higher ADPs
          than the heavy Ce ion.
;
#end Validation Reply Form

_diffrn_reflns_theta_full        25.10
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measured_fraction_theta_full 0.966
_refine_diff_density_max         1.928
_refine_diff_density_min         -2.310
_refine_diff_density_rms         0.146

_database_code_depnum_ccdc_archive 'CCDC 979167'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  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.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_gt26sq

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C27 H23 N5 O14 Tb2'
_chemical_formula_sum            'C27 H23 N5 O14 Tb2'
_chemical_formula_weight         959.34

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   8.5085(4)
_cell_length_b                   16.0156(8)
_cell_length_c                   27.9393(14)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3807.3(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    110(2)
_cell_measurement_reflns_used    6494
_cell_measurement_theta_min      1.93
_cell_measurement_theta_max      25.2

_exptl_crystal_description       needles
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.674
_exptl_crystal_F_000             1848
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    3.748
_shelx_estimated_absorpt_T_min   0.420
_shelx_estimated_absorpt_T_max   0.835
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.420
_exptl_absorpt_correction_T_max  0.835
_exptl_absorpt_process_details   'Sadabs, Bruker-AXS'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      110(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'ImuS micro source'
_diffrn_measurement_device_type  'ApexDuo, Bruler-AXS'
_diffrn_measurement_method       '1 deg. φ scans'
_diffrn_detector_area_resol_mean 1.75
_diffrn_reflns_number            18953
_diffrn_reflns_av_unetI/netI     0.0506
_diffrn_reflns_av_R_equivalents  0.0364
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_theta_min         1.934
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             7745
_reflns_number_gt                6494
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.778
_reflns_Friedel_fraction_max     1.000
_reflns_Friedel_fraction_full    1.000

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Apex2, Bruker-AXS'
_computing_cell_refinement       'Apex2, Bruker-AXS'
_computing_data_reduction        'Saint, Bruker-AXS'
_computing_structure_solution    'Saint, Bruker-AXS'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 Refined as a 2-component perfect inversion twin.

 The terminal NMe2 residues of the metal-coordinated DMF are partially
 disordered.
 The non-coordinated DMF solvent trapped in the lattice voids could not
 be reliably modeled by discrete atoms. Correspondingly, its contribution
 to the diffraction pattern was subtracted by the Squeeze technique,
 using the Platon software (Spek, 2009).
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0595P)²] 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_abs_structure_details 
;
 Refined as a perfect inversion twin.
;
_refine_ls_abs_structure_Flack   0.5
_chemical_absolute_configuration unk
_refine_ls_number_reflns         7745
_refine_ls_number_parameters     437
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0513
_refine_ls_R_factor_gt           0.0418
_refine_ls_wR_factor_ref         0.1050
_refine_ls_wR_factor_gt          0.1008
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_restrained_S_all      1.060
_refine_ls_shift/su_max          0.031
_refine_ls_shift/su_mean         0.004

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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Tb1 Tb 0.77034(9) 0.80614(2) 0.33229(2) 0.01160(15) Uani 1 1 d . . . . .
Tb2 Tb 0.73059(9) 1.20398(3) 0.16917(2) 0.01194(15) Uani 1 1 d . . . . .
O3 O 0.5208(13) 0.7122(5) 0.3714(3) 0.021(2) Uani 1 1 d . . . . .
O4 O 0.9416(12) 1.1188(5) 0.1839(3) 0.021(2) Uani 1 1 d . . . . .
O5 O 1.1465(14) 0.7628(5) 0.2648(3) 0.032(3) Uani 1 1 d . . . . .
O6 O 0.6672(13) 1.0660(5) 0.1450(3) 0.036(3) Uani 1 1 d . . . . .
O7 O 0.5152(11) 0.7067(5) 0.6271(3) 0.020(2) Uani 1 1 d . . . . .
O8 O 1.1749(13) 1.1638(5) 0.1601(4) 0.041(3) Uani 1 1 d . . . . .
O9 O 0.6842(12) 0.7887(5) 0.5897(3) 0.024(3) Uani 1 1 d . . . . .
O10 O 0.3214(10) 0.8441(5) 0.3368(3) 0.026(2) Uani 1 1 d . . . . .
O11 O 0.6855(11) 0.7929(5) 0.4115(3) 0.024(2) Uani 1 1 d . . . . .
O12 O 0.9401(14) 0.8471(6) 0.2717(3) 0.033(3) Uani 1 1 d . . . . .
O13 O 0.5605(14) 1.1668(6) 0.2292(3) 0.032(3) Uani 1 1 d . . . . .
O14 O 0.5572(13) 0.8947(5) 0.3158(4) 0.032(3) Uani 1 1 d . . . . .
O15 O 0.8270(13) 0.9453(5) 0.3564(3) 0.030(3) Uani 1 1 d . . . . .
O16 O 0.3453(13) 1.2471(5) 0.2346(3) 0.028(3) Uani 1 1 d . . . . .
N17 N 0.1287(16) 1.0799(6) 0.3248(4) 0.033(3) Uani 1 1 d . . . . .
N18 N 0.4148(10) 0.5828(5) 0.4971(4) 0.026(2) Uani 1 1 d . . . . .
N19 N 1.3713(15) 0.9281(6) 0.1746(4) 0.033(3) Uani 1 1 d . . . . .
N20 N 0.738(2) 0.9321(6) 0.1378(4) 0.041(3) Uani 1 1 d . . . . .
N21 N 0.751(3) 1.0788(6) 0.3660(4) 0.059(5) Uani 1 1 d . . . . .
C22 C 0.5796(18) 0.7367(7) 0.4093(4) 0.017(3) Uani 1 1 d . . . . .
C23 C 1.0880(15) 1.1103(6) 0.1761(4) 0.011(2) Uani 1 1 d . . . . .
C24 C 0.431(2) 1.1817(8) 0.2442(5) 0.036(5) Uani 1 1 d . . . . .
C25 C 0.3501(16) 0.9867(7) 0.3145(5) 0.018(3) Uani 1 1 d . . . . .
C26 C 1.1590(16) 1.0252(7) 0.1847(4) 0.013(3) Uani 1 1 d . . . . .
C27 C 0.4548(18) 0.6235(7) 0.4570(4) 0.021(3) Uani 1 1 d . . . . .
H27 H 0.4275 0.5991 0.4271 0.025 Uiso 1 1 calc R U . . .
C28 C 1.147(2) 0.8890(8) 0.2217(4) 0.024(4) Uani 1 1 d . . . . .
C29 C 1.293(2) 0.8726(8) 0.2000(5) 0.029(4) Uani 1 1 d . . . . .
H29 H 1.3378 0.8187 0.2039 0.035 Uiso 1 1 calc R U . . .
C30 C 0.6995(17) 0.9929(7) 0.1614(5) 0.026(4) Uani 1 1 d . . . . .
H30 H 0.6926 0.9854 0.1950 0.031 Uiso 1 1 calc R U . . .
C31 C 0.3510(16) 1.1181(7) 0.2767(4) 0.016(3) Uani 1 1 d . . . . .
C32 C 1.0819(17) 0.9663(7) 0.2131(4) 0.016(3) Uani 1 1 d . . . . .
H32 H 0.9828 0.9798 0.2267 0.019 Uiso 1 1 calc R U . . .
C33 C 0.5319(16) 0.6974(7) 0.4566(4) 0.014(3) Uani 1 1 d . . . . .
C34 C 0.4263(17) 1.0468(7) 0.2865(4) 0.016(3) Uani 1 1 d . . . . .
H34 H 0.5294 1.0371 0.2747 0.019 Uiso 1 1 calc R U . . .
C35 C 0.5433(18) 0.6949(7) 0.5421(4) 0.020(3) Uani 1 1 d . . . . .
C36 C 0.1974(18) 1.0078(7) 0.3327(5) 0.027(4) Uani 1 1 d . . . . .
H36 H 0.1432 0.9675 0.3514 0.032 Uiso 1 1 calc R U . . .
C37 C 1.3039(17) 1.0034(7) 0.1667(6) 0.027(4) Uani 1 1 d . . . . .
H37 H 1.3592 1.0432 0.1479 0.032 Uiso 1 1 calc R U . . .
C38 C 0.5821(10) 0.7339(6) 0.4983(5) 0.0169(19) Uani 1 1 d . . . . .
H38 H 0.6416 0.7841 0.4978 0.020 Uiso 1 1 calc R U . . .
C39 C 0.5820(18) 0.7336(7) 0.5882(5) 0.020(3) Uani 1 1 d . . . . .
C40 C 0.4160(19) 0.9036(7) 0.3248(5) 0.027(4) Uani 1 1 d . . . . .
C41 C 0.4553(17) 0.6184(8) 0.5391(4) 0.020(3) Uani 1 1 d . . . . .
H41 H 0.4244 0.5918 0.5679 0.024 Uiso 1 1 calc R U . . .
C42 C 0.2014(18) 1.1335(7) 0.2960(4) 0.020(3) Uani 1 1 d . . . . .
H42 H 0.1499 1.1843 0.2881 0.024 Uiso 1 1 calc R U . . .
C43 C 0.7974(19) 1.0144(7) 0.3402(5) 0.029(4) Uani 1 1 d . . . . .
H43 H 0.8088 1.0223 0.3067 0.035 Uiso 1 1 calc R U . . .
C44 C 1.0781(17) 0.8265(8) 0.2550(4) 0.022(3) Uani 1 1 d . . . . .
C45 C 0.759(3) 0.8471(8) 0.1569(7) 0.070(6) Uani 1 1 d . . . . .
H45A H 0.8614 0.8253 0.1468 0.105 Uiso 1 1 calc R U . . .
H45B H 0.6754 0.8109 0.1446 0.105 Uiso 1 1 calc R U . . .
H45C H 0.7543 0.8487 0.1919 0.105 Uiso 1 1 calc R U . . .
C46 C 0.745(4) 1.1624(8) 0.3448(5) 0.066(7) Uani 1 1 d . . . . .
H46A H 0.7806 1.1598 0.3115 0.099 Uiso 1 1 calc R U . . .
H46B H 0.8133 1.2001 0.3629 0.099 Uiso 1 1 calc R U . . .
H46C H 0.6367 1.1833 0.3458 0.099 Uiso 1 1 calc R U . . .
C47A C 0.814(4) 1.0855(19) 0.4205(10) 0.047(8) Uiso 0.5 1 d . . P A 1
H47A H 0.8233 1.0294 0.4342 0.070 Uiso 0.5 1 calc R U P A 1
H47B H 0.7404 1.1186 0.4395 0.070 Uiso 0.5 1 calc R U P A 1
H47C H 0.9176 1.1126 0.4206 0.070 Uiso 0.5 1 calc R U P A 1
C48A C 0.825(8) 0.966(3) 0.046(2) 0.08(2) Uiso 0.5 1 d . . P B 1
H48A H 0.7573 0.9638 0.0672 0.120 Uiso 0.5 1 calc R U P B 1
H48B H 0.9195 0.9322 0.0898 0.120 Uiso 0.5 1 calc R U P B 1
H48C H 0.8557 1.0239 0.1018 0.120 Uiso 0.5 1 calc R U P B 1
C47B C 0.667(5) 1.056(2) 0.4080(12) 0.052(11) Uiso 0.5 1 d . . P A 2
H47D H 0.6366 0.9971 0.4061 0.078 Uiso 0.5 1 calc R U P A 2
H47E H 0.5717 1.0905 0.4107 0.078 Uiso 0.5 1 calc R U P A 2
H47F H 0.7331 1.0649 0.4362 0.078 Uiso 0.5 1 calc R U P A 2
C48B C 0.759(4) 0.9321(16) 0.0846(9) 0.036(6) Uiso 0.5 1 d . . P B 2
H48D H 0.6604 0.9149 0.0693 0.122 Uiso 0.5 1 calc R U P B 2
H48E H 0.8427 0.8930 0.0758 0.122 Uiso 0.5 1 calc R U P B 2
H48F H 0.7870 0.9884 0.0739 0.122 Uiso 0.5 1 calc R U P B 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tb1 O16 2.314(9) 3_645 ?
Tb1 O12 2.320(10) . ?
Tb1 O11 2.338(8) . ?
Tb1 O8 2.337(8) 3_745 ?
Tb1 O14 2.348(9) . ?
Tb1 O15 2.377(8) . ?
Tb1 O7 2.381(9) 4_566 ?
Tb1 O3 2.822(10) . ?
Tb1 C22 2.915(13) . ?
Tb2 O10 2.293(8) 3_655 ?
Tb2 O4 2.293(9) . ?
Tb2 O13 2.294(10) . ?
Tb2 O5 2.321(9) 3_755 ?
Tb2 O9 2.340(8) 2_674 ?
Tb2 O6 2.373(9) . ?
Tb2 O3 2.423(11) 3_655 ?
Tb2 O7 2.847(9) 2_674 ?
Tb2 C39 2.942(14) 2_674 ?
O3 C22 1.235(15) . ?
O3 Tb2 2.423(11) 3_645 ?
O4 C23 1.272(15) . ?
O5 C44 1.205(15) . ?
O5 Tb2 2.321(9) 3_745 ?
O6 C30 1.286(14) . ?
O7 C39 1.300(15) . ?
O7 Tb1 2.381(9) 4_466 ?
O7 Tb2 2.847(9) 2_675 ?
O8 C23 1.217(15) . ?
O8 Tb1 2.337(8) 3_755 ?
O9 C39 1.240(16) . ?
O9 Tb2 2.340(8) 2_675 ?
O10 C40 1.292(15) . ?
O10 Tb2 2.293(8) 3_645 ?
O11 C22 1.275(15) . ?
O12 C44 1.306(17) . ?
O13 C24 1.20(2) . ?
O14 C40 1.235(18) . ?
O15 C43 1.221(14) . ?
O16 C24 1.303(19) . ?
O16 Tb1 2.314(9) 3_655 ?
N17 C36 1.313(17) . ?
N17 C42 1.330(16) . ?
N18 C27 1.342(15) . ?
N18 C41 1.348(16) . ?
N19 C29 1.318(18) . ?
N19 C37 1.354(16) . ?
N20 C30 1.221(16) . ?
N20 C45 1.472(16) . ?
N21 C43 1.319(16) . ?
N21 C46 1.465(15) . ?
C22 C33 1.519(16) . ?
C23 C26 1.510(15) . ?
C24 C31 1.525(18) . ?
C25 C34 1.399(18) . ?
C25 C36 1.435(18) . ?
C25 C40 1.473(17) . ?
C26 C37 1.376(17) . ?
C26 C32 1.395(16) . ?
C27 C33 1.353(17) . ?
C28 C32 1.376(18) . ?
C28 C29 1.41(2) . ?
C28 C44 1.487(18) . ?
C31 C34 1.338(17) . ?
C31 C42 1.405(18) . ?
C33 C38 1.373(17) . ?
C35 C38 1.411(17) . ?
C35 C41 1.438(17) . ?
C35 C39 1.469(18) . ?
C39 Tb2 2.942(14) 2_675 ?

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
O16 Tb1 O12 78.0(3) 3_645 . ?
O16 Tb1 O11 126.6(3) 3_645 . ?
O12 Tb1 O11 155.3(3) . . ?
O16 Tb1 O8 76.1(3) 3_645 3_745 ?
O12 Tb1 O8 102.6(4) . 3_745 ?
O11 Tb1 O8 83.5(3) . 3_745 ?
O16 Tb1 O14 76.1(3) 3_645 . ?
O12 Tb1 O14 99.6(4) . . ?
O11 Tb1 O14 90.1(3) . . ?
O8 Tb1 O14 139.6(4) 3_745 . ?
O16 Tb1 O15 134.3(3) 3_645 . ?
O12 Tb1 O15 79.3(3) . . ?
O11 Tb1 O15 83.1(3) . . ?
O8 Tb1 O15 148.1(4) 3_745 . ?
O14 Tb1 O15 69.2(3) . . ?
O16 Tb1 O7 136.2(3) 3_645 4_566 ?
O12 Tb1 O7 80.0(3) . 4_566 ?
O11 Tb1 O7 79.1(3) . 4_566 ?
O8 Tb1 O7 72.4(3) 3_745 4_566 ?
O14 Tb1 O7 145.2(3) . 4_566 ?
O15 Tb1 O7 76.6(3) . 4_566 ?
O16 Tb1 O3 77.0(3) 3_645 . ?
O12 Tb1 O3 154.4(3) . . ?
O11 Tb1 O3 49.7(3) . . ?
O8 Tb1 O3 66.1(3) 3_745 . ?
O14 Tb1 O3 79.4(3) . . ?
O15 Tb1 O3 122.9(3) . . ?
O7 Tb1 O3 115.4(3) 4_566 . ?
O16 Tb1 C22 101.7(3) 3_645 . ?
O12 Tb1 C22 173.2(4) . . ?
O11 Tb1 C22 25.2(3) . . ?
O8 Tb1 C22 70.8(4) 3_745 . ?
O14 Tb1 C22 86.8(4) . . ?
O15 Tb1 C22 105.2(3) . . ?
O7 Tb1 C22 95.9(3) 4_566 . ?
O3 Tb1 C22 24.8(3) . . ?
O10 Tb2 O4 138.3(3) 3_655 . ?
O10 Tb2 O13 100.7(3) 3_655 . ?
O4 Tb2 O13 102.0(3) . . ?
O10 Tb2 O5 75.4(3) 3_655 3_755 ?
O4 Tb2 O5 75.3(3) . 3_755 ?
O13 Tb2 O5 79.0(4) . 3_755 ?
O10 Tb2 O9 86.7(3) 3_655 2_674 ?
O4 Tb2 O9 87.6(3) . 2_674 ?
O13 Tb2 O9 154.5(4) . 2_674 ?
O5 Tb2 O9 126.5(4) 3_755 2_674 ?
O10 Tb2 O6 147.9(3) 3_655 . ?
O4 Tb2 O6 71.0(3) . . ?
O13 Tb2 O6 79.8(4) . . ?
O5 Tb2 O6 134.9(3) 3_755 . ?
O9 Tb2 O6 81.2(3) 2_674 . ?
O10 Tb2 O3 75.1(3) 3_655 3_655 ?
O4 Tb2 O3 143.9(3) . 3_655 ?
O13 Tb2 O3 78.4(3) . 3_655 ?
O5 Tb2 O3 138.3(3) 3_755 3_655 ?
O9 Tb2 O3 80.0(3) 2_674 3_655 ?
O6 Tb2 O3 73.6(3) . 3_655 ?
O10 Tb2 O7 68.0(3) 3_655 2_674 ?
O4 Tb2 O7 77.2(3) . 2_674 ?
O13 Tb2 O7 155.7(3) . 2_674 ?
O5 Tb2 O7 77.4(3) 3_755 2_674 ?
O9 Tb2 O7 49.3(3) 2_674 2_674 ?
O6 Tb2 O7 121.6(3) . 2_674 ?
O3 Tb2 O7 116.7(3) 3_655 2_674 ?
O10 Tb2 C39 73.5(3) 3_655 2_674 ?
O4 Tb2 C39 85.2(3) . 2_674 ?
O13 Tb2 C39 172.8(4) . 2_674 ?
O5 Tb2 C39 103.2(4) 3_755 2_674 ?
O9 Tb2 C39 23.8(3) 2_674 2_674 ?
O6 Tb2 C39 102.8(4) . 2_674 ?
O3 Tb2 C39 95.8(3) 3_655 2_674 ?
O7 Tb2 C39 25.9(3) 2_674 2_674 ?
C22 O3 Tb2 140.9(10) . 3_645 ?
C22 O3 Tb1 81.8(8) . . ?
Tb2 O3 Tb1 120.8(3) 3_645 . ?
C23 O4 Tb2 143.1(8) . . ?
C44 O5 Tb2 137.8(9) . 3_745 ?
C30 O6 Tb2 134.3(8) . . ?
C39 O7 Tb1 144.1(9) . 4_466 ?
C39 O7 Tb2 81.1(8) . 2_675 ?
Tb1 O7 Tb2 120.8(3) 4_466 2_675 ?
C23 O8 Tb1 140.8(9) . 3_755 ?
C39 O9 Tb2 106.4(8) . 2_675 ?
C40 O10 Tb2 145.4(9) . 3_645 ?
C22 O11 Tb1 103.6(7) . . ?
C44 O12 Tb1 138.5(9) . . ?
C24 O13 Tb2 141.3(9) . . ?
C40 O14 Tb1 141.4(9) . . ?
C43 O15 Tb1 134.7(10) . . ?
C24 O16 Tb1 137.0(8) . 3_655 ?
C36 N17 C42 117.5(12) . . ?
C27 N18 C41 117.2(8) . . ?
C29 N19 C37 118.3(13) . . ?
C30 N20 C45 125.0(14) . . ?
C43 N21 C46 120.3(12) . . ?
O3 C22 O11 123.5(11) . . ?
O3 C22 C33 120.4(12) . . ?
O11 C22 C33 116.0(11) . . ?
O3 C22 Tb1 73.4(7) . . ?
O11 C22 Tb1 51.2(6) . . ?
C33 C22 Tb1 161.6(10) . . ?
O8 C23 O4 125.7(11) . . ?
O8 C23 C26 116.8(12) . . ?
O4 C23 C26 117.4(10) . . ?
O13 C24 O16 126.9(13) . . ?
O13 C24 C31 118.8(14) . . ?
O16 C24 C31 114.2(16) . . ?
C34 C25 C36 117.1(12) . . ?
C34 C25 C40 123.6(13) . . ?
C36 C25 C40 119.2(13) . . ?
C37 C26 C32 117.2(12) . . ?
C37 C26 C23 121.9(12) . . ?
C32 C26 C23 120.9(12) . . ?
N18 C27 C33 123.7(11) . . ?
C32 C28 C29 116.6(13) . . ?
C32 C28 C44 123.9(14) . . ?
C29 C28 C44 119.3(13) . . ?
N19 C29 C28 123.4(13) . . ?
N20 C30 O6 126.3(14) . . ?
C34 C31 C42 120.4(13) . . ?
C34 C31 C24 118.6(13) . . ?
C42 C31 C24 121.0(13) . . ?
C28 C32 C26 121.2(13) . . ?
C27 C33 C38 121.1(10) . . ?
C27 C33 C22 119.9(10) . . ?
C38 C33 C22 118.7(11) . . ?
C31 C34 C25 118.6(13) . . ?
C38 C35 C41 116.6(11) . . ?
C38 C35 C39 121.4(11) . . ?
C41 C35 C39 121.8(11) . . ?
N17 C36 C25 123.4(12) . . ?
N19 C37 C26 123.1(13) . . ?
C33 C38 C35 118.3(8) . . ?
O9 C39 O7 121.1(12) . . ?
O9 C39 C35 119.1(12) . . ?
O7 C39 C35 119.7(12) . . ?
O9 C39 Tb2 49.7(6) . 2_675 ?
O7 C39 Tb2 73.0(7) . 2_675 ?
C35 C39 Tb2 160.1(11) . 2_675 ?
O14 C40 O10 125.0(12) . . ?
O14 C40 C25 115.8(12) . . ?
O10 C40 C25 118.7(14) . . ?
N18 C41 C35 122.9(10) . . ?
N17 C42 C31 122.7(13) . . ?
O15 C43 N21 124.7(13) . . ?
O5 C44 O12 124.6(13) . . ?
O5 C44 C28 121.5(14) . . ?
O12 C44 C28 113.9(12) . . ?

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.005 -0.250 0.000 465 112 ' '
2 0.029 0.250 0.500 465 112 ' '
_platon_squeeze_details          
;
 The residual electron density accounts for the disordered DMF solvent
;

# start Validation Reply FOrm
_vrf_PLAT113_gt26sq              
;
PROBLEM:  ADDSYM suggests new possible space group Pnma
RESPONSE: The diffraction pattern contains numerous reflections that
violate the systematic absences required by the glide planes in Pnma.
Then, in the centrosymmetric space group the least-squares refinement
of the equivalent structural model converges at R=0.10 as opposed to
R=0.04 in P212121. Twinned structure in P212121 seems to fit better
the diffraction data than the corresponding 'racemic' model in Pnma.
;
_vrf_PLAT111_gt26sq              
;
PROBLEM:  ADDSYM suggests new possible space group Pnma
RESPONSE: The diffraction pattern contains numerous reflections that
violate the systematic absences required by the glide planes in Pnma.
Then, in the centrosymmetric space group the least-squares refinement
of the equivalent structural model converges at R=0.10 as opposed to
R=0.04 in P212121. Twinned structure in P212121 seems to fit better
the diffraction data than the corresponding 'racemic' model in Pnma.
;
_vrf_PLAT220_gt26sq              
;
PROBLEM:  Large Non-solvent C/H Ueq/Uiso values
RESPONSE: The terminal NMe2 fragments of the metal-coordinated
DMF ligand are partially disordered.
;
# end Validation reply form. 

_refine_diff_density_max         2.133
_refine_diff_density_min         -2.505
_refine_diff_density_rms         0.172

#=============================END============================



_database_code_depnum_ccdc_archive 'CCDC 981479'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  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.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_gt21sq

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H14 Br4 Co2 N4 O9'
_chemical_formula_sum            'C24 H14 Br4 Co2 N4 O9'
_chemical_formula_weight         939.85

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/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                   14.2109(5)
_cell_length_b                   17.6868(6)
_cell_length_c                   14.2110(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 118.306(2)
_cell_angle_gamma                90.00
_cell_volume                     3144.77(19)
_cell_formula_units_Z            4
_cell_measurement_temperature    110(2)
_cell_measurement_reflns_used    4638
_cell_measurement_theta_min      1.67
_cell_measurement_theta_max      25.00

_exptl_crystal_description       prism
_exptl_crystal_colour            magenta
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.985
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1808
_exptl_absorpt_coefficient_mu    6.191
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3067
_exptl_absorpt_correction_T_max  0.4020
_exptl_absorpt_process_details   'Sadabs, Bruker-AXS'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      110(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  'ApexDuo, Bruker-AXS'
_diffrn_measurement_method       '1 deg. φ and ω scans'
_diffrn_detector_area_resol_mean 1.75
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            24928
_diffrn_reflns_av_R_equivalents  0.0390
_diffrn_reflns_av_sigmaI/netI    0.0348
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.67
_diffrn_reflns_theta_max         25.00
_reflns_number_total             5517
_reflns_number_gt                4638
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Apex2, Bruker-AXS'
_computing_cell_refinement       'Saint, Bruker-AXS'
_computing_data_reduction        'Saint, Bruker-AXS'
_computing_structure_solution    'SHELXTL-2013 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_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)+(0.0550P)²+9.3021P] 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         5517
_refine_ls_number_parameters     416
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0463
_refine_ls_R_factor_gt           0.0373
_refine_ls_wR_factor_ref         0.1068
_refine_ls_wR_factor_gt          0.1034
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_restrained_S_all      1.089
_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
Br2 Br 0.99096(5) 0.59976(4) 1.18273(6) 0.04004(19) Uani 1 1 d . . .
Br1A Br 0.8752(18) 0.1764(16) 0.6209(10) 0.075(4) Uani 0.209(19) 1 d P A 1
Br3A Br 0.2453(18) 0.0961(14) 0.8893(12) 0.072(5) Uani 0.209(19) 1 d P A 1
Br4A Br 0.0793(11) 0.3855(7) 0.2039(9) 0.074(5) Uani 0.209(19) 1 d P A 1
Br1B Br 0.8906(2) 0.19308(13) 0.6165(2) 0.0237(6) Uani 0.791(19) 1 d P A 2
Br3B Br 0.2167(3) 0.11413(16) 0.8984(2) 0.0353(5) Uani 0.791(19) 1 d P A 2
Br4B Br 0.07246(17) 0.38094(12) 0.20708(16) 0.0199(6) Uani 0.791(19) 1 d P A 2
C1 C 0.8036(4) 0.2858(2) 0.8670(3) 0.0085(9) Uani 1 1 d . A .
H1 H 0.7860 0.3074 0.9179 0.010 Uiso 1 1 calc R . .
C2 C 0.8903(4) 0.2367(2) 0.9036(3) 0.0077(9) Uani 1 1 d . . .
C3 C 0.9168(4) 0.2057(3) 0.8291(4) 0.0131(10) Uani 1 1 d . A .
H3 H 0.9750 0.1716 0.8504 0.016 Uiso 1 1 calc R . .
C4 C 0.8555(4) 0.2263(3) 0.7231(4) 0.0164(11) Uani 1 1 d . . .
C5 C 0.7699(4) 0.2745(3) 0.6927(4) 0.0134(10) Uani 1 1 d . A .
H5 H 0.7282 0.2869 0.6192 0.016 Uiso 1 1 calc R . .
C6 C 0.6377(4) 0.5381(2) 1.0522(3) 0.0108(9) Uani 1 1 d . . .
H6 H 0.5630 0.5295 1.0222 0.013 Uiso 1 1 calc R . .
C7 C 0.6907(4) 0.5074(3) 1.0006(4) 0.0177(11) Uani 1 1 d . . .
C8 C 0.7975(4) 0.5243(3) 1.0382(4) 0.0229(12) Uani 1 1 d . . .
H8 H 0.8360 0.5055 1.0037 0.028 Uiso 1 1 calc R . .
C9 C 0.8462(4) 0.5697(3) 1.1282(4) 0.0269(12) Uani 1 1 d . . .
C10 C 0.7897(4) 0.5962(3) 1.1786(4) 0.0218(12) Uani 1 1 d . . .
H10 H 0.8253 0.6270 1.2405 0.026 Uiso 1 1 calc R . .
C11 C 0.2449(4) 0.2672(3) 0.6533(3) 0.0106(9) Uani 1 1 d . A .
H11 H 0.2506 0.3005 0.6038 0.013 Uiso 1 1 calc R . .
C12 C 0.1638(4) 0.2138(2) 0.6138(3) 0.0105(10) Uani 1 1 d . . .
C13 C 0.1559(4) 0.1644(3) 0.6862(4) 0.0165(11) Uani 1 1 d . A .
H13 H 0.1024 0.1263 0.6633 0.020 Uiso 1 1 calc R . .
C14 C 0.2292(4) 0.1734(3) 0.7924(4) 0.0231(12) Uani 1 1 d . . .
C15 C 0.3068(4) 0.2281(3) 0.8262(4) 0.0171(11) Uani 1 1 d . A .
H15 H 0.3553 0.2330 0.9002 0.021 Uiso 1 1 calc R . .
C16 C 0.3598(4) 0.5204(2) 0.4473(3) 0.0086(9) Uani 1 1 d . A .
H16 H 0.4215 0.5478 0.4956 0.010 Uiso 1 1 calc R . .
C17 C 0.3232(4) 0.4618(2) 0.4872(3) 0.0079(9) Uani 1 1 d . . .
C18 C 0.2346(4) 0.4203(3) 0.4167(4) 0.0143(10) Uani 1 1 d . A .
H18 H 0.2073 0.3802 0.4412 0.017 Uiso 1 1 calc R . .
C19 C 0.1875(4) 0.4394(3) 0.3095(4) 0.0154(10) Uani 1 1 d . . .
C20 C 0.2278(4) 0.4987(3) 0.2757(4) 0.0137(10) Uani 1 1 d . A .
H20 H 0.1946 0.5107 0.2017 0.016 Uiso 1 1 calc R . .
C21 C 0.9533(4) 0.2203(2) 1.0220(3) 0.0095(10) Uani 1 1 d . . .
C23 C 0.3871(4) 0.4423(2) 0.6041(3) 0.0122(9) Uani 1 1 d . A .
C27 C 0.6267(4) 0.4618(2) 0.9002(3) 0.0100(10) Uani 1 1 d . A .
C55 C 0.0880(4) 0.2130(2) 0.4955(3) 0.0088(9) Uani 1 1 d . . .
Co1 Co 0.60970(5) 0.38063(3) 0.70946(4) 0.00652(15) Uani 1 1 d . . .
Co2 Co 0.42037(5) 0.37041(3) 0.80469(4) 0.00686(15) Uani 1 1 d . . .
N1 N 0.7435(3) 0.3045(2) 0.7639(3) 0.0088(8) Uani 1 1 d . . .
N2 N 0.6856(3) 0.5794(2) 1.1422(3) 0.0185(9) Uani 1 1 d . . .
N3 N 0.3154(3) 0.2747(2) 0.7565(3) 0.0101(8) Uani 1 1 d . . .
N4 N 0.3115(3) 0.5398(2) 0.3435(3) 0.0094(8) Uani 1 1 d . . .
O1 O 0.6791(2) 0.43155(17) 0.8593(2) 0.0099(7) Uani 1 1 d . . .
O2 O 0.5282(3) 0.45879(17) 0.8678(2) 0.0111(7) Uani 1 1 d . . .
O3 O 0.3393(2) 0.41201(16) 0.6495(2) 0.0089(6) Uani 1 1 d . . .
O4 O 0.4849(2) 0.45701(17) 0.6449(2) 0.0096(7) Uani 1 1 d . . .
O5 O 0.9224(3) 0.25411(18) 1.0797(2) 0.0134(7) Uani 1 1 d . . .
O6 O 1.0298(2) 0.17425(17) 1.0533(2) 0.0106(7) Uani 1 1 d . . .
O7 O 0.1127(3) 0.25483(18) 0.4392(2) 0.0180(8) Uani 1 1 d . . .
O8 O 0.0071(2) 0.17165(17) 0.4626(2) 0.0108(7) Uani 1 1 d . . .
O9 O 0.5225(2) 0.31086(17) 0.7587(2) 0.0120(7) Uani 1 1 d . . .
H9A H 0.5624 0.2926 0.8104 0.009 Uiso 1 1 d R A .
H9B H 0.4946 0.2879 0.7065 0.013 Uiso 1 1 d R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Br2 C9 1.898(5) . ?
Br1A C4 1.831(12) . ?
Br3A C14 1.876(11) . ?
Br4A C19 1.827(13) . ?
Br1B C4 1.899(5) . ?
Br3B C14 1.912(5) . ?
Br4B C19 1.898(5) . ?
C1 N1 1.341(6) . ?
C1 C2 1.391(6) . ?
C2 C3 1.393(6) . ?
C2 C21 1.512(6) . ?
C3 C4 1.385(6) . ?
C4 C5 1.376(7) . ?
C5 N1 1.343(6) . ?
C6 N2 1.343(6) . ?
C6 C7 1.387(7) . ?
C7 C8 1.382(8) . ?
C7 C27 1.511(6) . ?
C8 C9 1.386(7) . ?
C9 C10 1.387(7) . ?
C10 N2 1.349(7) . ?
C11 N3 1.334(6) . ?
C11 C12 1.386(7) . ?
C12 C13 1.395(6) . ?
C12 C55 1.507(6) . ?
C13 C14 1.377(7) . ?
C14 C15 1.372(7) . ?
C15 N3 1.337(6) . ?
C16 N4 1.343(6) . ?
C16 C17 1.395(6) . ?
C17 C18 1.391(7) . ?
C17 C23 1.507(6) . ?
C18 C19 1.383(6) . ?
C19 C20 1.386(7) . ?
C20 N4 1.336(6) . ?
C21 O5 1.252(5) . ?
C21 O6 1.258(6) . ?
C23 O4 1.253(6) . ?
C23 O3 1.258(5) . ?
C27 O2 1.250(6) . ?
C27 O1 1.261(5) . ?
C55 O8 1.251(5) . ?
C55 O7 1.255(5) . ?
Co1 O4 2.066(3) . ?
Co1 O1 2.080(3) . ?
Co1 O9 2.091(3) . ?
Co1 N4 2.145(4) 3_666 ?
Co1 N1 2.153(4) . ?
Co1 O6 2.184(3) 4_565 ?
Co2 O2 2.072(3) . ?
Co2 O3 2.079(3) . ?
Co2 O8 2.118(3) 4_666 ?
Co2 O9 2.131(3) . ?
Co2 N3 2.143(4) . ?
Co2 N2 2.169(4) 3_667 ?
N2 Co2 2.169(4) 3_667 ?
N4 Co1 2.145(4) 3_666 ?
O6 Co1 2.184(3) 4_666 ?
O8 Co2 2.118(3) 4_565 ?

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
N1 C1 C2 123.7(4) . . ?
C1 C2 C3 118.1(4) . . ?
C1 C2 C21 119.3(4) . . ?
C3 C2 C21 122.6(4) . . ?
C4 C3 C2 117.8(4) . . ?
C5 C4 C3 120.7(4) . . ?
C5 C4 Br1A 119.6(5) . . ?
C3 C4 Br1A 118.9(6) . . ?
C5 C4 Br1B 118.0(4) . . ?
C3 C4 Br1B 121.3(4) . . ?
N1 C5 C4 121.9(4) . . ?
N2 C6 C7 124.0(4) . . ?
C8 C7 C6 118.9(4) . . ?
C8 C7 C27 122.6(4) . . ?
C6 C7 C27 118.3(4) . . ?
C7 C8 C9 117.3(5) . . ?
C8 C9 C10 121.0(5) . . ?
C8 C9 Br2 120.6(4) . . ?
C10 C9 Br2 118.4(4) . . ?
N2 C10 C9 121.7(5) . . ?
N3 C11 C12 124.0(4) . . ?
C11 C12 C13 118.1(4) . . ?
C11 C12 C55 118.4(4) . . ?
C13 C12 C55 123.5(4) . . ?
C14 C13 C12 116.8(4) . . ?
C15 C14 C13 122.0(4) . . ?
C15 C14 Br3A 117.4(5) . . ?
C13 C14 Br3A 119.0(6) . . ?
C15 C14 Br3B 118.1(4) . . ?
C13 C14 Br3B 119.7(4) . . ?
N3 C15 C14 121.1(4) . . ?
N4 C16 C17 122.8(4) . . ?
C18 C17 C16 118.9(4) . . ?
C18 C17 C23 122.7(4) . . ?
C16 C17 C23 118.2(4) . . ?
C19 C18 C17 117.7(4) . . ?
C18 C19 C20 120.2(4) . . ?
C18 C19 Br4A 123.8(6) . . ?
C20 C19 Br4A 115.8(6) . . ?
C18 C19 Br4B 120.1(4) . . ?
C20 C19 Br4B 119.6(4) . . ?
N4 C20 C19 122.3(4) . . ?
O5 C21 O6 126.2(4) . . ?
O5 C21 C2 115.4(4) . . ?
O6 C21 C2 118.3(4) . . ?
O4 C23 O3 126.9(4) . . ?
O4 C23 C17 114.8(4) . . ?
O3 C23 C17 118.2(4) . . ?
O2 C27 O1 128.0(4) . . ?
O2 C27 C7 116.0(4) . . ?
O1 C27 C7 116.0(4) . . ?
O8 C55 O7 126.2(4) . . ?
O8 C55 C12 117.8(4) . . ?
O7 C55 C12 115.9(4) . . ?
O4 Co1 O1 93.55(12) . . ?
O4 Co1 O9 90.80(12) . . ?
O1 Co1 O9 88.93(12) . . ?
O4 Co1 N4 84.04(13) . 3_666 ?
O1 Co1 N4 90.13(13) . 3_666 ?
O9 Co1 N4 174.69(13) . 3_666 ?
O4 Co1 N1 174.11(13) . . ?
O1 Co1 N1 89.65(13) . . ?
O9 Co1 N1 94.20(13) . . ?
N4 Co1 N1 91.02(14) 3_666 . ?
O4 Co1 O6 85.20(12) . 4_565 ?
O1 Co1 O6 177.09(12) . 4_565 ?
O9 Co1 O6 88.46(11) . 4_565 ?
N4 Co1 O6 92.36(13) 3_666 4_565 ?
N1 Co1 O6 91.82(12) . 4_565 ?
O2 Co2 O3 96.66(12) . . ?
O2 Co2 O8 82.37(12) . 4_666 ?
O3 Co2 O8 178.36(13) . 4_666 ?
O2 Co2 O9 91.96(12) . . ?
O3 Co2 O9 87.99(11) . . ?
O8 Co2 O9 90.71(11) 4_666 . ?
O2 Co2 N3 173.92(13) . . ?
O3 Co2 N3 89.36(13) . . ?
O8 Co2 N3 91.63(13) 4_666 . ?
O9 Co2 N3 89.06(13) . . ?
O2 Co2 N2 91.94(14) . 3_667 ?
O3 Co2 N2 95.61(14) . 3_667 ?
O8 Co2 N2 85.76(14) 4_666 3_667 ?
O9 Co2 N2 174.35(14) . 3_667 ?
N3 Co2 N2 86.64(15) . 3_667 ?
C1 N1 C5 117.7(4) . . ?
C1 N1 Co1 122.9(3) . . ?
C5 N1 Co1 119.4(3) . . ?
C6 N2 C10 117.0(4) . . ?
C6 N2 Co2 115.5(3) . 3_667 ?
C10 N2 Co2 126.3(3) . 3_667 ?
C11 N3 C15 117.9(4) . . ?
C11 N3 Co2 118.4(3) . . ?
C15 N3 Co2 123.0(3) . . ?
C20 N4 C16 118.0(4) . . ?
C20 N4 Co1 122.6(3) . 3_666 ?
C16 N4 Co1 118.2(3) . 3_666 ?
C27 O1 Co1 123.9(3) . . ?
C27 O2 Co2 131.4(3) . . ?
C23 O3 Co2 122.2(3) . . ?
C23 O4 Co1 126.8(3) . . ?
C21 O6 Co1 126.3(3) . 4_666 ?
C55 O8 Co2 124.8(3) . 4_565 ?
Co1 O9 Co2 114.14(13) . . ?

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.500 0.500 143 51 ' '
2 0.500 0.000 1.000 143 51 ' '
_platon_squeeze_details          
;
;

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         1.077
_refine_diff_density_min         -1.902
_refine_diff_density_rms         0.126
_database_code_depnum_ccdc_archive 'CCDC 981480'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  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.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_gt28

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H6 Br2 Cd N2 O4'
_chemical_formula_sum            'C12 H6 Br2 Cd N2 O4'
_chemical_formula_weight         514.41

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'
Br Br -0.2901 2.4595 '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'
O O 0.0106 0.0060 '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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/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                   12.0504(3)
_cell_length_b                   9.9837(2)
_cell_length_c                   24.8139(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 101.2980(10)
_cell_angle_gamma                90.00
_cell_volume                     2927.45(11)
_cell_formula_units_Z            8
_cell_measurement_temperature    110(2)
_cell_measurement_reflns_used    2730
_cell_measurement_theta_min      1.67
_cell_measurement_theta_max      26.36

_exptl_crystal_description       plates
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.334
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1936
_exptl_absorpt_coefficient_mu    6.966
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.2748
_exptl_absorpt_correction_T_max  0.5426
_exptl_absorpt_process_details   'Sadabs, Bruker-AXS'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      110(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  'ApexDuo, Bruker-AXS'
_diffrn_measurement_method       '1 deg.  φ and ω scans'
_diffrn_detector_area_resol_mean 1.75
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            12286
_diffrn_reflns_av_R_equivalents  0.0248
_diffrn_reflns_av_sigmaI/netI    0.0228
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         1.67
_diffrn_reflns_theta_max         26.36
_reflns_number_total             2990
_reflns_number_gt                2730
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Apex2, Bruker-AXS'
_computing_cell_refinement       'Saint, Bruker-AXS'
_computing_data_reduction        'Saint, Bruker-AXS'
_computing_structure_solution    'SHELXTL-2013 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_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)+(0.0081P)²+3.7346P] 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         2990
_refine_ls_number_parameters     200
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0275
_refine_ls_R_factor_gt           0.0233
_refine_ls_wR_factor_ref         0.0468
_refine_ls_wR_factor_gt          0.0457
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_restrained_S_all      1.084
_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
Br1 Br 0.47199(3) -0.10052(3) -0.123733(12) 0.01878(8) Uani 1 1 d . . .
Br2A Br 0.2269(3) 0.3712(3) 0.30617(12) 0.0348(7) Uani 0.53(4) 1 d P A 1
Br2B Br 0.201(3) 0.395(3) 0.3008(8) 0.054(4) Uani 0.47(4) 1 d P A 2
C1 C 0.4006(2) -0.1945(3) 0.04776(12) 0.0101(6) Uani 1 1 d . . .
H1 H 0.3835 -0.2192 0.0822 0.012 Uiso 1 1 calc R . .
C2 C 0.3363(2) -0.0949(3) 0.01705(12) 0.0108(6) Uani 1 1 d . . .
C3 C 0.3574(2) -0.0644(3) -0.03440(12) 0.0115(6) Uani 1 1 d . . .
H3 H 0.3147 0.0024 -0.0566 0.014 Uiso 1 1 calc R . .
C4 C 0.4427(2) -0.1338(3) -0.05258(11) 0.0106(6) Uani 1 1 d . . .
C5 C 0.5077(2) -0.2271(3) -0.01921(12) 0.0111(6) Uani 1 1 d . . .
H5 H 0.5683 -0.2704 -0.0316 0.013 Uiso 1 1 calc R . .
C6 C 0.2487(2) -0.0212(3) 0.04056(12) 0.0105(6) Uani 1 1 d . . .
C7 C 0.1782(3) 0.2650(3) 0.19798(12) 0.0167(6) Uani 1 1 d . A .
H7 H 0.1201 0.2178 0.2109 0.020 Uiso 1 1 calc R . .
C8 C 0.2445(3) 0.3541(3) 0.23245(13) 0.0201(7) Uani 1 1 d . . .
C9 C 0.3301(3) 0.4248(3) 0.21510(13) 0.0170(6) Uani 1 1 d . A .
H9 H 0.3775 0.4850 0.2389 0.020 Uiso 1 1 calc R . .
C10 C 0.3436(2) 0.4039(3) 0.16145(13) 0.0136(6) Uani 1 1 d . . .
C11 C 0.2751(2) 0.3119(3) 0.12880(12) 0.0102(6) Uani 1 1 d . A .
H11 H 0.2863 0.2968 0.0924 0.012 Uiso 1 1 calc R . .
C12 C 0.4327(2) 0.4792(3) 0.13848(12) 0.0108(6) Uani 1 1 d . . .
Cd1 Cd 0.090408(16) 0.090045(19) 0.088934(8) 0.00797(6) Uani 1 1 d . . .
N1 N 0.48616(18) -0.2571(2) 0.03050(10) 0.0099(5) Uani 1 1 d . . .
N2 N 0.19358(19) 0.2432(2) 0.14662(10) 0.0112(5) Uani 1 1 d . . .
O1 O 0.20318(17) -0.0820(2) 0.07528(9) 0.0154(4) Uani 1 1 d . . .
O2 O 0.22531(17) 0.09709(19) 0.02570(8) 0.0147(4) Uani 1 1 d . . .
O3 O 0.43163(17) 0.4662(2) 0.08796(9) 0.0167(5) Uani 1 1 d . . .
O4 O 0.50214(18) 0.5502(2) 0.16973(9) 0.0199(5) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Br1 C4 1.897(3) . ?
Br2A C8 1.890(4) . ?
Br2B C8 1.915(12) . ?
C1 N1 1.345(3) . ?
C1 C2 1.393(4) . ?
C2 C3 1.384(4) . ?
C2 C6 1.496(4) . ?
C3 C4 1.386(4) . ?
C4 C5 1.383(4) . ?
C5 N1 1.343(4) . ?
C6 O2 1.253(3) . ?
C6 O1 1.264(3) . ?
C6 Cd1 2.685(3) . ?
C7 N2 1.341(4) . ?
C7 C8 1.376(4) . ?
C8 C9 1.387(4) . ?
C9 C10 1.388(4) . ?
C10 C11 1.385(4) . ?
C10 C12 1.511(4) . ?
C11 N2 1.342(4) . ?
C12 O4 1.245(3) . ?
C12 O3 1.258(3) . ?
C12 Cd1 2.695(3) 3 ?
Cd1 O1 2.2568(19) . ?
Cd1 O3 2.274(2) 3_445 ?
Cd1 N2 2.288(2) . ?
Cd1 N1 2.301(2) 3_455 ?
Cd1 O2 2.472(2) . ?
Cd1 O4 2.479(2) 3_445 ?
Cd1 C12 2.695(3) 3_445 ?
N1 Cd1 2.301(2) 3_545 ?
O3 Cd1 2.2741(19) 3 ?
O4 Cd1 2.479(2) 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
N1 C1 C2 122.4(3) . . ?
C3 C2 C1 118.6(3) . . ?
C3 C2 C6 121.5(3) . . ?
C1 C2 C6 119.8(3) . . ?
C2 C3 C4 118.2(3) . . ?
C5 C4 C3 120.7(3) . . ?
C5 C4 Br1 119.2(2) . . ?
C3 C4 Br1 120.0(2) . . ?
N1 C5 C4 120.7(3) . . ?
O2 C6 O1 123.5(3) . . ?
O2 C6 C2 118.9(3) . . ?
O1 C6 C2 117.6(2) . . ?
O2 C6 Cd1 66.63(15) . . ?
O1 C6 Cd1 56.83(14) . . ?
C2 C6 Cd1 174.4(2) . . ?
N2 C7 C8 121.6(3) . . ?
C7 C8 C9 120.9(3) . . ?
C7 C8 Br2A 119.9(3) . . ?
C9 C8 Br2A 119.1(2) . . ?
C7 C8 Br2B 117.5(5) . . ?
C9 C8 Br2B 121.1(3) . . ?
C8 C9 C10 117.1(3) . . ?
C11 C10 C9 119.5(3) . . ?
C11 C10 C12 119.7(3) . . ?
C9 C10 C12 120.8(3) . . ?
N2 C11 C10 122.5(3) . . ?
O4 C12 O3 123.6(3) . . ?
O4 C12 C10 119.3(3) . . ?
O3 C12 C10 117.1(2) . . ?
O4 C12 Cd1 66.55(15) . 3 ?
O3 C12 Cd1 57.18(14) . 3 ?
C10 C12 Cd1 173.3(2) . 3 ?
O1 Cd1 O3 96.59(7) . 3_445 ?
O1 Cd1 N2 109.47(8) . . ?
O3 Cd1 N2 136.29(8) 3_445 . ?
O1 Cd1 N1 132.90(8) . 3_455 ?
O3 Cd1 N1 89.98(8) 3_445 3_455 ?
N2 Cd1 N1 96.51(8) . 3_455 ?
O1 Cd1 O2 55.67(7) . . ?
O3 Cd1 O2 131.71(7) 3_445 . ?
N2 Cd1 O2 91.94(8) . . ?
N1 Cd1 O2 85.81(7) 3_455 . ?
O1 Cd1 O4 111.46(7) . 3_445 ?
O3 Cd1 O4 55.11(7) 3_445 3_445 ?
N2 Cd1 O4 82.41(8) . 3_445 ?
N1 Cd1 O4 110.37(8) 3_455 3_445 ?
O2 Cd1 O4 163.30(7) . 3_445 ?
O1 Cd1 C6 27.95(8) . . ?
O3 Cd1 C6 116.12(8) 3_445 . ?
N2 Cd1 C6 102.10(8) . . ?
N1 Cd1 C6 109.91(8) 3_455 . ?
O2 Cd1 C6 27.72(7) . . ?
O4 Cd1 C6 138.61(8) 3_445 . ?
O1 Cd1 C12 104.79(8) . 3_445 ?
O3 Cd1 C12 27.70(8) 3_445 3_445 ?
N2 Cd1 C12 109.53(9) . 3_445 ?
N1 Cd1 C12 102.29(8) 3_455 3_445 ?
O2 Cd1 C12 155.73(8) . 3_445 ?
O4 Cd1 C12 27.44(8) 3_445 3_445 ?
C6 Cd1 C12 131.33(8) . 3_445 ?
C5 N1 C1 119.1(2) . . ?
C5 N1 Cd1 123.13(17) . 3_545 ?
C1 N1 Cd1 117.72(19) . 3_545 ?
C7 N2 C11 118.5(2) . . ?
C7 N2 Cd1 122.92(19) . . ?
C11 N2 Cd1 118.58(19) . . ?
C6 O1 Cd1 95.22(16) . . ?
C6 O2 Cd1 85.64(17) . . ?
C12 O3 Cd1 95.12(16) . 3 ?
C12 O4 Cd1 86.01(17) . 3 ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        26.36
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.460
_refine_diff_density_min         -0.599
_refine_diff_density_rms         0.088
_database_code_depnum_ccdc_archive 'CCDC 981481'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  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.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_gt20sq

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C31 H30 Mn3 N6 O15'
_chemical_formula_sum            'C31 H30 Mn3 N6 O15'
_chemical_formula_weight         891.43

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

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/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                   13.2579(5)
_cell_length_b                   11.4380(3)
_cell_length_c                   28.7450(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 99.887(2)
_cell_angle_gamma                90.00
_cell_volume                     4294.3(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    110(2)
_cell_measurement_reflns_used    6555
_cell_measurement_theta_min      1.83
_cell_measurement_theta_max      25.73

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.379
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1812
_exptl_absorpt_coefficient_mu    0.935
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7061
_exptl_absorpt_correction_T_max  0.8724
_exptl_absorpt_process_details   'Sadabs, Bruker-AXS'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      110(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  'ApexDuo, Bruker-AXS'
_diffrn_measurement_method       '1.0 deg. φ and ω scans'
_diffrn_detector_area_resol_mean 1.75
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            29739
_diffrn_reflns_av_R_equivalents  0.0402
_diffrn_reflns_av_sigmaI/netI    0.0476
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_theta_min         1.83
_diffrn_reflns_theta_max         25.73
_reflns_number_total             8108
_reflns_number_gt                6555
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Apex2, Bruker-AXS'
_computing_cell_refinement       'Saint, Bruker-AXS'
_computing_data_reduction        'Saint, Bruker-AXS'
_computing_structure_solution    'SHELXTL-2012 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_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. 

 The crystals contain severely disordered molecules of the DMA
 crystallization solvent within the interstitial voids, which could not
 be modeled reliably by discrete atoms. Its contribution to the
 diffraction pattern was thus subtracted by the Squeeze procedure,
 using the PLATON software (Spek, 2009).
 Three of the metal coordinated DMA ligands are also partly disordered.



;

_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)+(0.0806P)²+4.1436P] 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         8108
_refine_ls_number_parameters     491
_refine_ls_number_restraints     127
_refine_ls_R_factor_all          0.0810
_refine_ls_R_factor_gt           0.0668
_refine_ls_wR_factor_ref         0.1797
_refine_ls_wR_factor_gt          0.1727
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_restrained_S_all      1.036
_refine_ls_shift/su_max          0.040
_refine_ls_shift/su_mean         0.002

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn1 Mn 0.95899(5) 0.54889(6) 0.66863(2) 0.01236(18) Uani 1 1 d U . .
Mn2 Mn 1.14660(6) 0.82855(6) 0.63550(2) 0.01424(18) Uani 1 1 d U . .
Mn3 Mn 0.71472(6) 0.79780(6) 0.85688(2) 0.01517(19) Uani 1 1 d U . .
O4 O 0.9854(2) 0.8642(3) 0.62988(11) 0.0161(7) Uani 1 1 d U . .
O5 O 1.5596(3) 0.7513(3) 0.86279(12) 0.0187(7) Uani 1 1 d U . .
O6 O 1.1737(3) 0.5199(3) 0.38561(11) 0.0155(7) Uani 1 1 d U . .
O7 O 1.0507(3) 0.5241(3) 0.61572(12) 0.0212(7) Uani 1 1 d U . .
O8 O 0.8977(3) 0.7204(3) 0.65734(12) 0.0180(7) Uani 1 1 d U . .
O9 O 0.6454(3) 1.0358(3) 0.78101(12) 0.0204(8) Uani 1 1 d U . .
O10 O 1.2303(3) 0.6660(3) 0.43285(11) 0.0200(7) Uani 1 1 d U . .
O11 O 1.4840(3) 0.8763(3) 0.80785(12) 0.0218(8) Uani 1 1 d U . .
O12 O 1.0806(3) 0.6001(3) 0.72428(12) 0.0238(8) Uani 1 1 d U . .
O13 O 1.1634(3) 0.7589(3) 0.70468(12) 0.0275(9) Uani 1 1 d U . .
O14 O 1.1414(3) 0.6743(3) 0.59432(12) 0.0250(8) Uani 1 1 d U . .
O15 O 0.7101(3) 0.8544(3) 0.78721(13) 0.0330(10) Uani 1 1 d U . .
N16 N 0.7834(3) 1.1095(3) 0.66748(13) 0.0155(8) Uani 1 1 d U . .
N17 N 1.3255(3) 0.5112(3) 0.82730(14) 0.0168(8) Uani 1 1 d U . .
N18 N 1.1082(4) 0.3271(3) 0.50191(15) 0.0253(10) Uani 1 1 d U . .
C19 C 0.8511(4) 0.9146(4) 0.67017(15) 0.0128(9) Uani 1 1 d U . .
C20 C 1.3983(4) 0.7011(4) 0.81803(17) 0.0167(10) Uani 1 1 d U . .
C21 C 1.2418(4) 0.6450(4) 0.76880(17) 0.0175(10) Uani 1 1 d U . .
C22 C 1.1194(4) 0.5079(4) 0.54542(16) 0.0158(9) Uani 1 1 d U . .
C23 C 1.3188(4) 0.7264(4) 0.78194(16) 0.0167(10) Uani 1 1 d U . .
H23 H 1.3167 0.7994 0.7661 0.020 Uiso 1 1 calc R . .
C24 C 0.9180(4) 0.8258(4) 0.65066(15) 0.0129(9) Uani 1 1 d U . .
C25 C 0.8415(4) 1.0264(4) 0.65212(16) 0.0147(9) Uani 1 1 d U . .
H25 H 0.8780 1.0459 0.6275 0.018 Uiso 1 1 calc R . .
C26 C 1.1528(4) 0.5654(4) 0.50853(16) 0.0155(9) Uani 1 1 d U . .
H26 H 1.1702 0.6460 0.5112 0.019 Uiso 1 1 calc R . .
C27 C 1.1022(4) 0.5750(4) 0.58903(16) 0.0145(9) Uani 1 1 d U . .
C28 C 1.3980(4) 0.5926(4) 0.84056(16) 0.0152(9) Uani 1 1 d U . .
H28 H 1.4513 0.5757 0.8663 0.018 Uiso 1 1 calc R . .
C29 C 1.1901(4) 0.5666(4) 0.42629(16) 0.0144(9) Uani 1 1 d U . .
C30 C 0.7460(4) 0.9736(4) 0.72558(16) 0.0155(9) Uani 1 1 d U . .
C31 C 1.2493(4) 0.5385(4) 0.79207(16) 0.0167(10) Uani 1 1 d U . .
H31 H 1.1976 0.4817 0.7825 0.020 Uiso 1 1 calc R . .
C32 C 1.1546(4) 0.6688(4) 0.72898(17) 0.0199(10) Uani 1 1 d U . .
C33 C 0.8016(4) 0.8870(4) 0.70744(16) 0.0161(10) Uani 1 1 d U . .
H33 H 0.8057 0.8104 0.7203 0.019 Uiso 1 1 calc R . .
C34 C 0.7371(4) 1.0828(4) 0.70405(16) 0.0160(10) Uani 1 1 d U . .
H34 H 0.6967 1.1408 0.7157 0.019 Uiso 1 1 calc R . .
C35 C 1.4870(4) 0.7832(4) 0.83109(16) 0.0155(10) Uani 1 1 d U . .
C36 C 1.1606(4) 0.5039(4) 0.46752(16) 0.0160(9) Uani 1 1 d U . .
C37 C 1.1374(4) 0.3847(4) 0.46637(17) 0.0192(10) Uani 1 1 d U . .
H37 H 1.1429 0.3423 0.4385 0.023 Uiso 1 1 calc R . .
C38 C 0.6958(4) 0.9532(4) 0.76839(17) 0.0197(10) Uani 1 1 d U . .
C39 C 1.0985(4) 0.3895(4) 0.54062(17) 0.0204(11) Uani 1 1 d U . .
H39 H 1.0760 0.3501 0.5661 0.024 Uiso 1 1 calc R . .
O40 O 0.8784(4) 0.7976(5) 0.8606(2) 0.0622(15) Uani 1 1 d U . .
C41 C 0.9680(6) 0.8001(7) 0.8780(3) 0.0551(18) Uani 1 1 d U . .
C42 C 0.9934(8) 0.7963(12) 0.9314(4) 0.103(4) Uani 1 1 d U . .
H42A H 0.9299 0.7908 0.9444 0.154 Uiso 1 1 calc R . .
H42B H 1.0303 0.8676 0.9430 0.154 Uiso 1 1 calc R . .
H42C H 1.0364 0.7280 0.9413 0.154 Uiso 1 1 calc R . .
N43 N 1.0426(5) 0.8115(6) 0.8521(3) 0.0601(17) Uani 1 1 d U . .
C44 C 1.0136(8) 0.8096(10) 0.8021(3) 0.085(3) Uani 1 1 d U . .
H44A H 0.9989 0.7290 0.7915 0.127 Uiso 1 1 calc R . .
H44B H 1.0696 0.8407 0.7875 0.127 Uiso 1 1 calc R . .
H44C H 0.9523 0.8577 0.7928 0.127 Uiso 1 1 calc R . .
C45 C 1.1514(6) 0.8060(10) 0.8709(4) 0.086(3) Uani 1 1 d U . .
H45A H 1.1628 0.8241 0.9048 0.129 Uiso 1 1 calc R . .
H45B H 1.1880 0.8630 0.8545 0.129 Uiso 1 1 calc R . .
H45C H 1.1770 0.7273 0.8662 0.129 Uiso 1 1 calc R . .
O46 O 1.3164(3) 0.8240(3) 0.64373(14) 0.0319(9) Uani 1 1 d U . .
C47 C 1.3972(10) 0.7916(10) 0.6671(4) 0.093(3) Uiso 1 1 d U A 1
N48A N 1.4306(8) 0.6980(9) 0.6854(3) 0.033(2) Uiso 0.50 1 d PU B 2
C49A C 1.3655(7) 0.6073(8) 0.6679(3) 0.0161(19) Uiso 0.50 1 d PU B 2
H49A H 1.3043 0.6393 0.6480 0.024 Uiso 0.50 1 calc PR B 2
H49B H 1.3455 0.5639 0.6943 0.024 Uiso 0.50 1 calc PR B 2
H49C H 1.4007 0.5547 0.6491 0.024 Uiso 0.50 1 calc PR B 2
C50A C 1.5266(13) 0.6613(15) 0.7161(6) 0.047(4) Uiso 0.50 1 d PU B 2
H50A H 1.5119 0.5981 0.7370 0.071 Uiso 0.50 1 calc PR B 2
H50B H 1.5561 0.7279 0.7352 0.071 Uiso 0.50 1 calc PR B 2
H50C H 1.5754 0.6337 0.6966 0.071 Uiso 0.50 1 calc PR B 2
N48B N 1.4783(19) 0.801(2) 0.6829(8) 0.117(7) Uiso 0.50 1 d PU C 3
C49B C 1.4845(7) 0.9070(8) 0.6839(3) 0.0137(18) Uiso 0.50 1 d PU C 3
H49D H 1.4863 0.9345 0.7164 0.021 Uiso 0.50 1 calc PR C 3
H49E H 1.4250 0.9407 0.6633 0.021 Uiso 0.50 1 calc PR C 3
H49F H 1.5473 0.9314 0.6729 0.021 Uiso 0.50 1 calc PR C 3
C50B C 1.5469(14) 0.7032(17) 0.7100(7) 0.058(5) Uiso 0.50 1 d PU C 3
H50D H 1.6048 0.7391 0.7309 0.087 Uiso 0.50 1 calc PR C 3
H50E H 1.5726 0.6521 0.6872 0.087 Uiso 0.50 1 calc PR C 3
H50F H 1.5063 0.6570 0.7288 0.087 Uiso 0.50 1 calc PR C 3
O51 O 1.1361(3) 0.9243(3) 0.57027(13) 0.0336(9) Uani 1 1 d U . .
C52 C 1.1651(9) 0.9619(10) 0.5403(4) 0.092(3) Uiso 1 1 d U A 1
N53A N 1.1535(9) 0.9690(10) 0.4974(4) 0.038(2) Uiso 0.50 1 d PU D 2
C54A C 1.0804(7) 0.8863(8) 0.4784(3) 0.0138(18) Uiso 0.50 1 d PU D 2
H54A H 1.0282 0.9240 0.4549 0.021 Uiso 0.50 1 calc PR D 2
H54B H 1.0482 0.8531 0.5036 0.021 Uiso 0.50 1 calc PR D 2
H54C H 1.1137 0.8239 0.4632 0.021 Uiso 0.50 1 calc PR D 2
C55A C 1.1909(11) 1.0570(12) 0.4659(5) 0.037(3) Uiso 0.50 1 d PU D 2
H55A H 1.1996 1.0194 0.4363 0.055 Uiso 0.50 1 calc PR D 2
H55B H 1.2567 1.0887 0.4816 0.055 Uiso 0.50 1 calc PR D 2
H55C H 1.1409 1.1205 0.4593 0.055 Uiso 0.50 1 calc PR D 2
N53B N 1.2016(14) 1.0129(16) 0.5102(6) 0.082(5) Uiso 0.50 1 d PU E 3
C54B C 1.2629(10) 1.0692(12) 0.5633(5) 0.042(3) Uiso 0.50 1 d PU E 3
H54D H 1.2661 1.1546 0.5611 0.063 Uiso 0.50 1 calc PR E 3
H54E H 1.3325 1.0375 0.5706 0.063 Uiso 0.50 1 calc PR E 3
H54F H 1.2249 1.0475 0.5884 0.063 Uiso 0.50 1 calc PR E 3
C55B C 1.2348(17) 1.012(2) 0.4655(8) 0.080(6) Uiso 0.50 1 d PU E 3
H55D H 1.2452 1.0920 0.4556 0.120 Uiso 0.50 1 calc PR E 3
H55E H 1.1826 0.9738 0.4421 0.120 Uiso 0.50 1 calc PR E 3
H55F H 1.2992 0.9682 0.4682 0.120 Uiso 0.50 1 calc PR E 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
Mn1 O7 2.123(3) . ?
Mn1 O8 2.126(3) . ?
Mn1 O12 2.148(3) . ?
Mn1 O9 2.173(3) 2_646 ?
Mn1 O11 2.179(3) 2_746 ?
Mn1 O6 2.281(3) 3_766 ?
Mn2 O13 2.118(3) . ?
Mn2 O14 2.119(3) . ?
Mn2 O4 2.154(3) . ?
Mn2 O51 2.155(4) . ?
Mn2 O46 2.224(4) . ?
Mn2 N17 2.347(4) 2_756 ?
Mn3 O15 2.095(4) . ?
Mn3 O40 2.155(5) . ?
Mn3 O5 2.159(3) 1_455 ?
Mn3 O10 2.197(3) 4_576 ?
Mn3 N16 2.266(4) 2_646 ?
Mn3 O6 2.341(3) 4_576 ?
Mn3 C29 2.592(5) 4_576 ?
O4 C24 1.238(6) . ?
O5 C35 1.260(6) . ?
O5 Mn3 2.159(3) 1_655 ?
O6 C29 1.270(6) . ?
O6 Mn1 2.281(3) 3_766 ?
O6 Mn3 2.341(3) 4_675 ?
O7 C27 1.254(6) . ?
O8 C24 1.257(5) . ?
O9 C38 1.247(6) . ?
O9 Mn1 2.173(3) 2_656 ?
O10 C29 1.256(6) . ?
O10 Mn3 2.197(3) 4_675 ?
O11 C35 1.255(6) . ?
O11 Mn1 2.179(3) 2_756 ?
O12 C32 1.246(6) . ?
O13 C32 1.262(6) . ?
O14 C27 1.248(6) . ?
O15 C38 1.254(6) . ?
N16 C34 1.340(6) . ?
N16 C25 1.345(6) . ?
N16 Mn3 2.266(4) 2_656 ?
N17 C31 1.339(6) . ?
N17 C28 1.345(6) . ?
N17 Mn2 2.347(4) 2_746 ?
N18 C37 1.328(6) . ?
N18 C39 1.347(6) . ?
C19 C25 1.378(6) . ?
C19 C33 1.385(6) . ?
C19 C24 1.518(6) . ?
C20 C23 1.377(7) . ?
C20 C28 1.400(6) . ?
C20 C35 1.502(7) . ?
C21 C23 1.385(7) . ?
C21 C31 1.386(6) . ?
C21 C32 1.505(7) . ?
C22 C26 1.384(7) . ?
C22 C39 1.384(7) . ?
C22 C27 1.520(6) . ?
C26 C36 1.392(6) . ?
C29 C36 1.494(6) . ?
C29 Mn3 2.592(5) 4_675 ?
C30 C33 1.389(6) . ?
C30 C34 1.390(6) . ?
C30 C38 1.514(6) . ?
C36 C37 1.397(6) . ?
O40 C41 1.207(9) . ?
C41 N43 1.342(10) . ?
C41 C42 1.514(13) . ?
N43 C44 1.425(11) . ?
N43 C45 1.452(11) . ?
O46 C47 1.220(13) . ?
N48A C49A 1.387(13) . ?
N48A C50A 1.481(19) . ?
N48B C49B 1.22(2) . ?
N48B C50B 1.56(3) . ?
O51 C52 1.089(13) . ?
N53A C54A 1.397(15) . ?
N53A C55A 1.494(17) . ?
N53B C55B 1.43(3) . ?
N53B C54B 1.73(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
O7 Mn1 O8 105.35(13) . . ?
O7 Mn1 O12 96.94(14) . . ?
O8 Mn1 O12 94.61(13) . . ?
O7 Mn1 O9 167.62(13) . 2_646 ?
O8 Mn1 O9 83.96(13) . 2_646 ?
O12 Mn1 O9 90.30(14) . 2_646 ?
O7 Mn1 O11 83.72(13) . 2_746 ?
O8 Mn1 O11 170.35(13) . 2_746 ?
O12 Mn1 O11 80.80(13) . 2_746 ?
O9 Mn1 O11 87.56(13) 2_646 2_746 ?
O7 Mn1 O6 86.20(13) . 3_766 ?
O8 Mn1 O6 89.07(12) . 3_766 ?
O12 Mn1 O6 174.33(12) . 3_766 ?
O9 Mn1 O6 85.80(13) 2_646 3_766 ?
O11 Mn1 O6 94.91(12) 2_746 3_766 ?
O13 Mn2 O14 101.50(14) . . ?
O13 Mn2 O4 94.87(14) . . ?
O14 Mn2 O4 100.31(14) . . ?
O13 Mn2 O51 171.33(15) . . ?
O14 Mn2 O51 86.92(15) . . ?
O4 Mn2 O51 85.60(14) . . ?
O13 Mn2 O46 87.13(16) . . ?
O14 Mn2 O46 88.59(14) . . ?
O4 Mn2 O46 170.27(14) . . ?
O51 Mn2 O46 91.00(16) . . ?
O13 Mn2 N17 85.65(14) . 2_756 ?
O14 Mn2 N17 169.43(14) . 2_756 ?
O4 Mn2 N17 86.69(13) . 2_756 ?
O51 Mn2 N17 85.73(15) . 2_756 ?
O46 Mn2 N17 83.96(14) . 2_756 ?
O15 Mn3 O40 84.9(2) . . ?
O15 Mn3 O5 106.22(16) . 1_455 ?
O40 Mn3 O5 163.92(19) . 1_455 ?
O15 Mn3 O10 150.94(14) . 4_576 ?
O40 Mn3 O10 91.66(18) . 4_576 ?
O5 Mn3 O10 84.04(13) 1_455 4_576 ?
O15 Mn3 N16 89.90(14) . 2_646 ?
O40 Mn3 N16 87.12(17) . 2_646 ?
O5 Mn3 N16 81.47(13) 1_455 2_646 ?
O10 Mn3 N16 118.81(13) 4_576 2_646 ?
O15 Mn3 O6 95.25(12) . 4_576 ?
O40 Mn3 O6 106.04(16) . 4_576 ?
O5 Mn3 O6 84.81(12) 1_455 4_576 ?
O10 Mn3 O6 57.97(11) 4_576 4_576 ?
N16 Mn3 O6 166.21(13) 2_646 4_576 ?
O15 Mn3 C29 124.33(14) . 4_576 ?
O40 Mn3 C29 102.77(17) . 4_576 ?
O5 Mn3 C29 80.76(14) 1_455 4_576 ?
O10 Mn3 C29 28.95(13) 4_576 4_576 ?
N16 Mn3 C29 144.71(14) 2_646 4_576 ?
O6 Mn3 C29 29.28(13) 4_576 4_576 ?
C24 O4 Mn2 133.3(3) . . ?
C35 O5 Mn3 119.4(3) . 1_655 ?
C29 O6 Mn1 139.9(3) . 3_766 ?
C29 O6 Mn3 86.4(3) . 4_675 ?
Mn1 O6 Mn3 105.34(12) 3_766 4_675 ?
C27 O7 Mn1 144.6(3) . . ?
C24 O8 Mn1 145.2(3) . . ?
C38 O9 Mn1 132.9(3) . 2_656 ?
C29 O10 Mn3 93.2(3) . 4_675 ?
C35 O11 Mn1 128.8(3) . 2_756 ?
C32 O12 Mn1 136.8(3) . . ?
C32 O13 Mn2 145.3(3) . . ?
C27 O14 Mn2 143.0(3) . . ?
C38 O15 Mn3 131.9(3) . . ?
C34 N16 C25 117.5(4) . . ?
C34 N16 Mn3 119.3(3) . 2_656 ?
C25 N16 Mn3 122.2(3) . 2_656 ?
C31 N17 C28 117.6(4) . . ?
C31 N17 Mn2 126.2(3) . 2_746 ?
C28 N17 Mn2 116.0(3) . 2_746 ?
C37 N18 C39 117.0(4) . . ?
C25 C19 C33 118.5(4) . . ?
C25 C19 C24 120.3(4) . . ?
C33 C19 C24 121.2(4) . . ?
C23 C20 C28 118.2(4) . . ?
C23 C20 C35 121.5(4) . . ?
C28 C20 C35 120.2(4) . . ?
C23 C21 C31 118.1(4) . . ?
C23 C21 C32 121.3(4) . . ?
C31 C21 C32 120.5(4) . . ?
C26 C22 C39 118.2(4) . . ?
C26 C22 C27 120.3(4) . . ?
C39 C22 C27 121.4(4) . . ?
C20 C23 C21 119.8(4) . . ?
O4 C24 O8 127.3(4) . . ?
O4 C24 C19 117.2(4) . . ?
O8 C24 C19 115.6(4) . . ?
N16 C25 C19 123.6(4) . . ?
C22 C26 C36 119.3(4) . . ?
O14 C27 O7 127.4(4) . . ?
O14 C27 C22 116.2(4) . . ?
O7 C27 C22 116.4(4) . . ?
N17 C28 C20 122.7(4) . . ?
O10 C29 O6 121.4(4) . . ?
O10 C29 C36 118.5(4) . . ?
O6 C29 C36 120.1(4) . . ?
O10 C29 Mn3 57.8(2) . 4_675 ?
O6 C29 Mn3 64.4(2) . 4_675 ?
C36 C29 Mn3 169.4(3) . 4_675 ?
C33 C30 C34 118.9(4) . . ?
C33 C30 C38 122.1(4) . . ?
C34 C30 C38 119.0(4) . . ?
N17 C31 C21 123.5(4) . . ?
O12 C32 O13 127.0(5) . . ?
O12 C32 C21 117.1(4) . . ?
O13 C32 C21 115.9(4) . . ?
C19 C33 C30 118.8(4) . . ?
N16 C34 C30 122.6(4) . . ?
O11 C35 O5 125.6(4) . . ?
O11 C35 C20 116.5(4) . . ?
O5 C35 C20 117.9(4) . . ?
C26 C36 C37 117.7(4) . . ?
C26 C36 C29 119.9(4) . . ?
C37 C36 C29 122.4(4) . . ?
N18 C37 C36 124.0(4) . . ?
O9 C38 O15 127.4(4) . . ?
O9 C38 C30 116.9(4) . . ?
O15 C38 C30 115.8(4) . . ?
N18 C39 C22 123.7(4) . . ?
C41 O40 Mn3 158.7(6) . . ?
O40 C41 N43 122.6(8) . . ?
O40 C41 C42 116.8(7) . . ?
N43 C41 C42 120.5(8) . . ?
C41 N43 C44 117.5(7) . . ?
C41 N43 C45 124.7(8) . . ?
C44 N43 C45 117.0(7) . . ?
C47 O46 Mn2 147.4(7) . . ?
C49A N48A C50A 115.0(10) . . ?
C49B N48B C50B 132(2) . . ?
C52 O51 Mn2 155.3(7) . . ?
C54A N53A C55A 119.9(10) . . ?
C55B N53B C54B 128.9(16) . . ?

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 -0.013 0.000 338 79 ' '
2 0.500 0.043 0.500 338 79 ' '
_platon_squeeze_details          
;
 The residual density accounts for the disordered DMA crystallization solvent.
;

# start Validation Reply Form
_vrf_PLAT201_gt20sq              
;
PROBLEM:  isotropic atoms in the main residue
RESPONSE:  The metal-coordinated DMA ligands exhibit severe disorder.
          The disordered DMA residues (except for the metal-bound O-atoms
          were assigned isotropic ADPs.
;
_vrf_PLAT220_gt20sq              
;
PROBLEM:  large non-solvent Ueq(max)/Ueq(min)
RESPONSE: The disordered DMA residues have considerably higher ADPs than
          the metal ions and the ligand framework atoms.
;
#end Validation Reply Form

_diffrn_measured_fraction_theta_max 0.989
_diffrn_reflns_theta_full        25.73
_diffrn_measured_fraction_theta_full 0.989
_refine_diff_density_max         1.707
_refine_diff_density_min         -0.942
_refine_diff_density_rms         0.127
_database_code_depnum_ccdc_archive 'CCDC 981482'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  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.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_gt18

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C11 H12 N2 O5 Zn, C4 H9 N O'
_chemical_formula_sum            'C15 H21 N3 O6 Zn'
_chemical_formula_weight         404.72
_chemical_absolute_configuration ad

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P 212121'

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

_cell_length_a                   10.8285(4)
_cell_length_b                   11.1933(4)
_cell_length_c                   14.7990(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1793.74(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    110(2)
_cell_measurement_reflns_used    4186
_cell_measurement_theta_min      2.28
_cell_measurement_theta_max      28.37

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.499
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             840
_exptl_absorpt_coefficient_mu    1.405
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6391
_exptl_absorpt_correction_T_max  0.8169
_exptl_absorpt_process_details   'Sadabs, Bruker-AXS'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      110(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  'ApexDuo, Bruker-AXS'
_diffrn_measurement_method       '1 deg. φ and ω scans'
_diffrn_detector_area_resol_mean 1.75
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            17170
_diffrn_reflns_av_R_equivalents  0.0282
_diffrn_reflns_av_sigmaI/netI    0.0313
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.28
_diffrn_reflns_theta_max         28.37
_reflns_number_total             4464
_reflns_number_gt                4186
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Apex2, Bruker-AXS'
_computing_cell_refinement       'Saint, Bruker-AXS'
_computing_data_reduction        'Saint, Bruker-AXS'
_computing_structure_solution    'SHELXTL-2013 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_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. 

 The non-coordinated DMA solvent reveals rotational disorder.
;

_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)+(0.0292P)²+0.9721P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.406(10)
_refine_ls_number_reflns         4464
_refine_ls_number_parameters     252
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0320
_refine_ls_R_factor_gt           0.0283
_refine_ls_wR_factor_ref         0.0651
_refine_ls_wR_factor_gt          0.0639
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_restrained_S_all      1.042
_refine_ls_shift/su_max          0.039
_refine_ls_shift/su_mean         0.003

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.34279(2) 0.81577(2) 0.158400(17) 0.01233(6) Uani 1 1 d . . .
O2 O 0.23995(14) 0.75282(15) 0.06238(11) 0.0191(3) Uani 1 1 d . . .
O3 O 0.39398(15) 0.62953(16) 0.02490(13) 0.0262(4) Uani 1 1 d . . .
O4 O 0.40304(14) 0.70387(15) 0.24790(11) 0.0197(4) Uani 1 1 d . . .
O5 O 0.21025(15) 0.69836(18) 0.29872(13) 0.0331(5) Uani 1 1 d . . .
N6 N 0.50299(16) 0.89689(16) 0.12003(12) 0.0134(4) Uani 1 1 d . . .
C7 C 0.46436(19) 0.49909(18) 0.33816(17) 0.0141(4) Uani 1 1 d . . .
H7 H 0.5220 0.5363 0.2988 0.017 Uiso 1 1 calc R . .
C8 C 0.41604(19) 0.34601(18) 0.43704(14) 0.0128(4) Uani 1 1 d . . .
H8 H 0.4386 0.2739 0.4667 0.015 Uiso 1 1 calc R . .
C9 C 0.30105(19) 0.3949(2) 0.45414(15) 0.0142(4) Uani 1 1 d . . .
C10 C 0.26720(19) 0.4995(2) 0.40980(16) 0.0135(4) Uani 1 1 d . . .
H10 H 0.1885 0.5345 0.4201 0.016 Uiso 1 1 calc R . .
C11 C 0.3502(2) 0.55179(17) 0.35045(15) 0.0145(4) Uani 1 1 d . . .
C12 C 0.2880(2) 0.6644(2) 0.01874(16) 0.0152(4) Uani 1 1 d . . .
C13 C 0.3158(2) 0.6609(2) 0.29602(16) 0.0171(5) Uani 1 1 d . . .
O14 O 0.26266(14) 0.95797(14) 0.21071(12) 0.0194(3) Uani 1 1 d . . .
C15 C 0.1537(2) 0.97056(18) 0.23973(14) 0.0168(4) Uani 1 1 d . . .
C16 C 0.0489(2) 0.9003(2) 0.20232(18) 0.0258(5) Uani 1 1 d . . .
H16A H 0.0786 0.8493 0.1531 0.039 Uiso 1 1 calc R . .
H16B H -0.0144 0.9549 0.1792 0.039 Uiso 1 1 calc R . .
H16C H 0.0133 0.8503 0.2501 0.039 Uiso 1 1 calc R . .
N17 N 0.13187(19) 1.04988(19) 0.30360(14) 0.0255(5) Uani 1 1 d . . .
C18 C 0.0060(3) 1.0740(3) 0.3360(2) 0.0416(7) Uani 1 1 d . . .
H18A H -0.0431 1.1086 0.2869 0.062 Uiso 1 1 calc R . .
H18B H 0.0093 1.1304 0.3866 0.062 Uiso 1 1 calc R . .
H18C H -0.0322 0.9992 0.3561 0.062 Uiso 1 1 calc R . .
C19 C 0.2276(3) 1.1292(3) 0.3357(2) 0.0407(7) Uani 1 1 d . . .
H19A H 0.2301 1.1270 0.4019 0.061 Uiso 1 1 calc R . .
H19B H 0.2100 1.2109 0.3156 0.061 Uiso 1 1 calc R . .
H19C H 0.3075 1.1036 0.3115 0.061 Uiso 1 1 calc R . .
O20 O 0.1271(2) 1.2427(3) 0.13641(17) 0.0711(9) Uani 1 1 d . A 1
C21 C 0.2341(7) 1.2593(8) 0.1074(5) 0.037(2) Uani 0.555(16) 1 d P A 1
C22 C 0.3312(4) 1.3477(3) 0.1405(3) 0.0609(11) Uani 1 1 d . A 1
H22A H 0.2949 1.3999 0.1866 0.091 Uiso 1 1 calc R A 1
H22B H 0.3602 1.3962 0.0896 0.091 Uiso 1 1 calc R A 1
H22C H 0.4010 1.3039 0.1666 0.091 Uiso 1 1 calc R A 1
N23 N 0.2710(7) 1.1874(7) 0.0408(5) 0.044(2) Uani 0.555(16) 1 d P A 1
C24 C 0.3968(4) 1.2002(5) 0.0023(3) 0.0837(17) Uani 1 1 d . A 1
H24A H 0.4384 1.2685 0.0305 0.126 Uiso 1 1 calc R A 1
H24B H 0.3909 1.2134 -0.0630 0.126 Uiso 1 1 calc R A 1
H24C H 0.4443 1.1273 0.0140 0.126 Uiso 1 1 calc R A 1
C25 C 0.1812(5) 1.0981(4) 0.0074(3) 0.0807(16) Uani 1 1 d . A 1
H25A H 0.1010 1.1117 0.0363 0.121 Uiso 1 1 calc R A 1
H25B H 0.2106 1.0177 0.0221 0.121 Uiso 1 1 calc R A 1
H25C H 0.1725 1.1060 -0.0582 0.121 Uiso 1 1 calc R A 1
N23A N 0.3107(8) 1.2523(10) 0.0740(6) 0.047(3) Uani 0.445(16) 1 d P A 2
C25A C 0.2007(10) 1.1980(11) 0.0774(7) 0.041(3) Uani 0.445(16) 1 d P A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 O4 1.9362(16) . ?
Zn1 O2 1.9381(16) . ?
Zn1 O14 1.9712(15) . ?
Zn1 N6 2.0386(18) . ?
O2 C12 1.292(3) . ?
O3 C12 1.215(3) . ?
O4 C13 1.277(3) . ?
O5 C13 1.218(3) . ?
N6 C8 1.344(3) 3_655 ?
N6 C7 1.348(3) 3_655 ?
C7 N6 1.348(3) 3_645 ?
C7 C11 1.382(3) . ?
C7 H7 0.9500 . ?
C8 N6 1.344(3) 3_645 ?
C8 C9 1.383(3) . ?
C8 H8 0.9500 . ?
C9 C10 1.392(3) . ?
C9 C12 1.511(3) 4_565 ?
C10 C11 1.386(3) . ?
C10 H10 0.9500 . ?
C11 C13 1.510(3) . ?
C12 C9 1.511(3) 4_564 ?
O14 C15 1.263(3) . ?
C15 N17 1.318(3) . ?
C15 C16 1.488(3) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
N17 C19 1.445(3) . ?
N17 C18 1.470(3) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
O20 C21 1.249(8) . ?
C21 N23 1.334(14) . ?
C21 C22 1.525(10) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
N23 C24 1.483(8) . ?
N23 C25 1.479(11) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
N23A C25A 1.338(19) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4 Zn1 O2 117.39(7) . . ?
O4 Zn1 O14 113.71(7) . . ?
O2 Zn1 O14 109.18(7) . . ?
O4 Zn1 N6 101.07(7) . . ?
O2 Zn1 N6 116.53(7) . . ?
O14 Zn1 N6 97.14(7) . . ?
C12 O2 Zn1 114.43(14) . . ?
C13 O4 Zn1 112.08(14) . . ?
C8 N6 C7 118.49(19) 3_655 3_655 ?
C8 N6 Zn1 122.78(15) 3_655 . ?
C7 N6 Zn1 118.25(15) 3_655 . ?
N6 C7 C11 122.4(2) 3_645 . ?
N6 C7 H7 118.8 3_645 . ?
C11 C7 H7 118.8 . . ?
N6 C8 C9 122.31(19) 3_645 . ?
N6 C8 H8 118.8 3_645 . ?
C9 C8 H8 118.8 . . ?
C8 C9 C10 118.9(2) . . ?
C8 C9 C12 121.1(2) . 4_565 ?
C10 C9 C12 119.96(19) . 4_565 ?
C11 C10 C9 118.91(19) . . ?
C11 C10 H10 120.5 . . ?
C9 C10 H10 120.5 . . ?
C7 C11 C10 118.88(19) . . ?
C7 C11 C13 119.70(19) . . ?
C10 C11 C13 121.34(19) . . ?
O3 C12 O2 126.1(2) . . ?
O3 C12 C9 120.6(2) . 4_564 ?
O2 C12 C9 113.28(18) . 4_564 ?
O5 C13 O4 125.7(2) . . ?
O5 C13 C11 119.5(2) . . ?
O4 C13 C11 114.84(18) . . ?
C15 O14 Zn1 129.39(14) . . ?
O14 C15 N17 119.1(2) . . ?
O14 C15 C16 121.8(2) . . ?
N17 C15 C16 119.1(2) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 N17 C19 121.4(2) . . ?
C15 N17 C18 121.6(2) . . ?
C19 N17 C18 116.4(2) . . ?
N17 C18 H18A 109.5 . . ?
N17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
N17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N17 C19 H19A 109.5 . . ?
N17 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
N17 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
O20 C21 N23 116.3(10) . . ?
O20 C21 C22 128.7(7) . . ?
N23 C21 C22 114.9(8) . . ?
C21 N23 C24 120.1(10) . . ?
C21 N23 C25 117.1(8) . . ?
C24 N23 C25 122.8(6) . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        28.37
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.461
_refine_diff_density_min         -0.331
_refine_diff_density_rms         0.062
_database_code_depnum_ccdc_archive 'CCDC 981483'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  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.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_gt22

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C15 H21 Cd N3 O6'
_chemical_formula_sum            'C15 H21 Cd N3 O6'
_chemical_formula_weight         451.75
_chemical_absolute_configuration ad

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           monoclinic
_symmetry_space_group_name_H-M   'P 21'

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

_cell_length_a                   9.2879(3)
_cell_length_b                   11.9733(3)
_cell_length_c                   16.3513(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 101.7090(16)
_cell_angle_gamma                90.00
_cell_volume                     1780.54(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    110(2)
_cell_measurement_reflns_used    6186
_cell_measurement_theta_min      2.12
_cell_measurement_theta_max      26.37

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.685
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             912
_exptl_absorpt_coefficient_mu    1.262
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7687
_exptl_absorpt_correction_T_max  0.8841
_exptl_absorpt_process_details   'Sadabs, Bruker-AXS'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      110(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  'ApexDuo, Bruker-AXS'
_diffrn_measurement_method       '1 deg. φ and ω scans'
_diffrn_detector_area_resol_mean 1.75
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            14664
_diffrn_reflns_av_R_equivalents  0.0249
_diffrn_reflns_av_sigmaI/netI    0.0427
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.12
_diffrn_reflns_theta_max         26.37
_reflns_number_total             6933
_reflns_number_gt                6186
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Apex2, Bruker-AXS'
_computing_cell_refinement       'Saint, Bruker-AXS'
_computing_data_reduction        'Saint, Bruker-AXS'
_computing_structure_solution    'SHELXTL-2013 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_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. 

 The metal-coordinated DMA ligands are partly disordered.
;

_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)+(0.0091P)²+4.5581P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.03(2)
_refine_ls_number_reflns         6933
_refine_ls_number_parameters     463
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0398
_refine_ls_R_factor_gt           0.0328
_refine_ls_wR_factor_ref         0.0685
_refine_ls_wR_factor_gt          0.0653
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_restrained_S_all      1.061
_refine_ls_shift/su_max          0.049
_refine_ls_shift/su_mean         0.003

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 -0.06727(3) 0.49945(2) 0.647858(18) 0.01029(7) Uani 1 1 d . . .
Cd2 Cd 0.36495(3) 0.50636(4) 0.121466(19) 0.01004(7) Uani 1 1 d . . .
O3 O 0.3224(4) 0.3700(3) 0.2108(2) 0.0199(8) Uani 1 1 d . . .
O4 O 0.2134(5) 0.5242(3) 0.2376(3) 0.0271(10) Uani 1 1 d . . .
O5 O 0.4869(4) 0.3677(3) 0.0658(2) 0.0147(7) Uani 1 1 d . . .
O6 O 0.5380(5) 0.5310(2) 0.0159(3) 0.0205(10) Uani 1 1 d . . .
O7 O 0.8362(4) 0.5315(3) -0.2113(3) 0.0181(9) Uani 1 1 d . . .
O8 O 0.9014(4) 0.3689(3) -0.2558(2) 0.0174(8) Uani 1 1 d . . .
O9 O 0.0273(5) 0.5204(3) 0.5120(2) 0.0311(11) Uani 1 1 d . . .
O10 O -0.0115(4) 0.3570(3) 0.5642(2) 0.0192(8) Uani 1 1 d . . .
N11 N 0.1087(4) 0.1891(3) 0.3675(3) 0.0128(9) Uani 1 1 d . . .
N12 N 0.6849(4) 0.1949(3) -0.0992(2) 0.0093(8) Uani 1 1 d . . .
C13 C 0.1679(5) 0.2488(4) 0.3129(3) 0.0118(10) Uani 1 1 d . . .
H13 H 0.1997 0.2102 0.2689 0.034 Uiso 1 1 calc R . .
C14 C 0.1848(5) 0.3636(4) 0.3175(3) 0.0127(10) Uani 1 1 d . . .
C15 C 0.1425(5) 0.4197(4) 0.3827(3) 0.0137(10) Uani 1 1 d . . .
H15 H 0.1550 0.4983 0.3880 0.036 Uiso 1 1 calc R . .
C16 C 0.0814(5) 0.3600(4) 0.4405(3) 0.0132(10) Uani 1 1 d . . .
C17 C 0.0660(5) 0.2454(4) 0.4304(3) 0.0132(10) Uani 1 1 d . . .
H17 H 0.0236 0.2045 0.4693 0.036 Uiso 1 1 calc R . .
C18 C 0.2436(6) 0.4256(4) 0.2501(3) 0.0148(11) Uani 1 1 d . . .
C19 C 0.0295(6) 0.4178(4) 0.5109(3) 0.0152(11) Uani 1 1 d . . .
C20 C 0.7564(5) 0.2520(4) -0.1496(3) 0.0108(10) Uani 1 1 d . . .
H20 H 0.7993 0.2119 -0.1887 0.033 Uiso 1 1 calc R . .
C21 C 0.7698(5) 0.3676(4) -0.1464(3) 0.0090(9) Uani 1 1 d . . .
C22 C 0.7056(5) 0.4268(4) -0.0898(3) 0.0110(10) Uani 1 1 d . . .
H22 H 0.7136 0.5059 -0.0863 0.033 Uiso 1 1 calc R . .
C23 C 0.6293(5) 0.3678(3) -0.0384(3) 0.0087(9) Uani 1 1 d . . .
C24 C 0.6230(5) 0.2525(4) -0.0449(3) 0.0100(9) Uani 1 1 d . . .
H24 H 0.5726 0.2123 -0.0092 0.032 Uiso 1 1 calc R . .
C25 C 0.5474(6) 0.4273(4) 0.0194(4) 0.0145(12) Uani 1 1 d . . .
C26 C 0.8426(6) 0.4291(4) -0.2081(3) 0.0124(11) Uani 1 1 d . . .
O27 O 0.1768(4) 0.5160(4) 0.7026(2) 0.0250(9) Uani 1 1 d . . .
C28 C 0.2558(6) 0.5781(4) 0.7543(3) 0.0193(11) Uani 1 1 d . . .
C29 C 0.1901(6) 0.6462(5) 0.8158(4) 0.0273(14) Uani 1 1 d . . .
H29A H 0.0887 0.6220 0.8139 0.041 Uiso 1 1 calc R . .
H29B H 0.1909 0.7254 0.8011 0.041 Uiso 1 1 calc R . .
H29C H 0.2483 0.6351 0.8723 0.041 Uiso 1 1 calc R . .
N30 N 0.3988(4) 0.5863(3) 0.7566(3) 0.0156(9) Uani 1 1 d . . .
C31 C 0.4645(5) 0.5212(4) 0.6980(3) 0.0230(12) Uani 1 1 d . . .
H31A H 0.5026 0.4507 0.7242 0.035 Uiso 1 1 calc R . .
H31B H 0.5452 0.5637 0.6826 0.035 Uiso 1 1 calc R . .
H31C H 0.3898 0.5055 0.6477 0.035 Uiso 1 1 calc R . .
C32 C 0.4955(6) 0.6569(4) 0.8168(4) 0.0254(13) Uani 1 1 d . . .
H32A H 0.4595 0.7341 0.8115 0.038 Uiso 1 1 calc R . .
H32B H 0.5954 0.6543 0.8059 0.038 Uiso 1 1 calc R . .
H32C H 0.4966 0.6299 0.8735 0.038 Uiso 1 1 calc R . .
O34 O -0.3119(4) 0.4625(3) 0.5801(2) 0.0262(9) Uani 1 1 d . . .
C35 C -0.3391(7) 0.3735(7) 0.5362(5) 0.0478(19) Uani 1 1 d . . .
C36 C -0.3229(8) 0.2569(5) 0.5807(5) 0.0476(19) Uani 1 1 d . . .
H36A H -0.4195 0.2209 0.5731 0.071 Uiso 1 1 calc R . .
H36B H -0.2830 0.2672 0.6405 0.071 Uiso 1 1 calc R . .
H36C H -0.2561 0.2098 0.5565 0.071 Uiso 1 1 calc R . .
N37 N -0.3878(7) 0.3755(6) 0.4609(4) 0.0612(19) Uani 1 1 d . . .
C38 C -0.3965(10) 0.4881(8) 0.4215(4) 0.074(2) Uani 1 1 d . . .
H38A H -0.4149 0.5443 0.4618 0.110 Uiso 1 1 calc R . .
H38B H -0.4768 0.4893 0.3723 0.110 Uiso 1 1 calc R . .
H38C H -0.3035 0.5048 0.4046 0.110 Uiso 1 1 calc R . .
C39 C -0.4130(10) 0.2724(8) 0.4088(6) 0.085(3) Uani 1 1 d . . .
H39A H -0.3181 0.2384 0.4059 0.128 Uiso 1 1 calc R . .
H39B H -0.4656 0.2916 0.3523 0.128 Uiso 1 1 calc R . .
H39C H -0.4717 0.2193 0.4339 0.128 Uiso 1 1 calc R . .
O40 O 0.5558(4) 0.5744(3) 0.2197(3) 0.0290(9) Uani 1 1 d . . .
C41 C 0.6907(7) 0.5706(4) 0.2388(4) 0.0244(13) Uani 1 1 d . . .
C42 C 0.7745(7) 0.4682(4) 0.2177(4) 0.0340(15) Uani 1 1 d . . .
H42A H 0.7049 0.4139 0.1870 0.051 Uiso 1 1 calc R . .
H42B H 0.8283 0.4340 0.2695 0.051 Uiso 1 1 calc R . .
H42C H 0.8442 0.4909 0.1832 0.051 Uiso 1 1 calc R . .
N43 N 0.7702(5) 0.6518(4) 0.2791(3) 0.0239(10) Uani 1 1 d . . .
C44 C 0.9286(6) 0.6489(4) 0.3093(4) 0.0244(12) Uani 1 1 d . . .
H44A H 0.9506 0.6227 0.3673 0.037 Uiso 1 1 calc R . .
H44B H 0.9691 0.7240 0.3064 0.037 Uiso 1 1 calc R . .
H44C H 0.9729 0.5979 0.2745 0.037 Uiso 1 1 calc R . .
C45 C 0.6930(7) 0.7488(4) 0.3056(4) 0.0319(14) Uani 1 1 d . . .
H45A H 0.5979 0.7584 0.2674 0.048 Uiso 1 1 calc R . .
H45B H 0.7526 0.8162 0.3047 0.048 Uiso 1 1 calc R . .
H45C H 0.6773 0.7364 0.3624 0.048 Uiso 1 1 calc R . .
O46 O 0.1642(4) 0.4551(3) 0.0178(2) 0.0274(9) Uani 1 1 d . . .
C47 C 0.1504(10) 0.3636(6) -0.0136(7) 0.080(5) Uani 1 1 d . . .
C48 C 0.2328(7) 0.3580(7) -0.1067(4) 0.0465(19) Uani 1 1 d . . .
H48A H 0.2991 0.2937 -0.1026 0.070 Uiso 1 1 calc R . .
H48B H 0.2883 0.4268 -0.1104 0.070 Uiso 1 1 calc R . .
H48C H 0.1548 0.3506 -0.1567 0.070 Uiso 1 1 calc R . .
N49 N 0.1171(8) 0.2810(5) -0.0227(6) 0.088(3) Uani 1 1 d . . .
C50 C 0.1078(6) 0.1723(4) -0.0582(4) 0.0303(14) Uani 1 1 d . . .
H50A H 0.0699 0.1775 -0.1186 0.045 Uiso 1 1 calc R . .
H50B H 0.0413 0.1263 -0.0328 0.045 Uiso 1 1 calc R . .
H50C H 0.2057 0.1382 -0.0477 0.045 Uiso 1 1 calc R . .
C51 C 0.0360(7) 0.2828(7) 0.0677(4) 0.050(2) Uani 1 1 d . . .
H51A H 0.0458 0.3576 0.0925 0.076 Uiso 1 1 calc R . .
H51B H 0.0862 0.2285 0.1086 0.076 Uiso 1 1 calc R . .
H51C H -0.0684 0.2632 0.0516 0.076 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cd1 O27 2.270(3) . ?
Cd1 O8 2.279(3) 1_456 ?
Cd1 N11 2.309(4) 2_556 ?
Cd1 O10 2.309(3) . ?
Cd1 O34 2.359(4) . ?
Cd1 O9 2.561(4) . ?
Cd1 C19 2.756(5) . ?
Cd2 O3 2.278(3) . ?
Cd2 O40 2.287(4) . ?
Cd2 O5 2.300(3) . ?
Cd2 N12 2.318(3) 2_655 ?
Cd2 O46 2.333(4) . ?
Cd2 O4 2.592(4) . ?
Cd2 O6 2.603(4) . ?
Cd2 C18 2.755(5) . ?
O3 C18 1.258(6) . ?
O4 C18 1.221(6) . ?
O5 C25 1.254(7) . ?
O6 C25 1.245(6) . ?
O7 C26 1.227(6) . ?
O8 C26 1.265(6) . ?
O8 Cd1 2.279(3) 1_654 ?
O9 C19 1.228(7) . ?
O10 C19 1.254(6) . ?
N11 C13 1.345(6) . ?
N11 C17 1.354(6) . ?
N11 Cd1 2.309(4) 2_546 ?
N12 C24 1.343(6) . ?
N12 C20 1.345(6) . ?
N12 Cd2 2.318(3) 2_645 ?
C13 C14 1.384(6) . ?
C14 C15 1.382(7) . ?
C14 C18 1.520(7) . ?
C15 C16 1.394(7) . ?
C16 C17 1.386(6) . ?
C16 C19 1.504(7) . ?
C20 C21 1.389(6) . ?
C21 C22 1.392(6) . ?
C21 C26 1.515(7) . ?
C22 C23 1.397(6) . ?
C23 C24 1.385(6) . ?
C23 C25 1.506(7) . ?
O27 C28 1.246(6) . ?
C28 N30 1.325(6) . ?
C28 C29 1.515(7) . ?
N30 C32 1.460(6) . ?
N30 C31 1.462(6) . ?
O34 C35 1.281(8) . ?
C35 N37 1.222(9) . ?
C35 C36 1.568(10) . ?
N37 C38 1.489(11) . ?
N37 C39 1.492(9) . ?
O40 C41 1.228(7) . ?
C41 N43 1.315(7) . ?
C41 C42 1.529(7) . ?
N43 C44 1.454(7) . ?
N43 C45 1.476(7) . ?
O46 C47 1.206(8) . ?
C47 N49 1.038(9) . ?
C47 C48 1.838(15) . ?
N49 C50 1.420(7) . ?
N49 C51 1.791(12) . ?

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
O27 Cd1 O8 92.56(14) . 1_456 ?
O27 Cd1 N11 95.05(15) . 2_556 ?
O8 Cd1 N11 135.08(13) 1_456 2_556 ?
O27 Cd1 O10 88.41(13) . . ?
O8 Cd1 O10 88.75(12) 1_456 . ?
N11 Cd1 O10 135.60(13) 2_556 . ?
O27 Cd1 O34 172.30(14) . . ?
O8 Cd1 O34 87.15(13) 1_456 . ?
N11 Cd1 O34 90.56(14) 2_556 . ?
O10 Cd1 O34 83.90(13) . . ?
O27 Cd1 O9 80.97(14) . . ?
O8 Cd1 O9 141.33(11) 1_456 . ?
N11 Cd1 O9 83.58(12) 2_556 . ?
O10 Cd1 O9 53.22(11) . . ?
O34 Cd1 O9 94.46(14) . . ?
O27 Cd1 C19 83.54(14) . . ?
O8 Cd1 C19 115.27(13) 1_456 . ?
N11 Cd1 C19 109.57(14) 2_556 . ?
O10 Cd1 C19 26.85(13) . . ?
O34 Cd1 C19 89.62(14) . . ?
O9 Cd1 C19 26.38(14) . . ?
O3 Cd2 O40 90.89(14) . . ?
O3 Cd2 O5 84.26(12) . . ?
O40 Cd2 O5 99.29(14) . . ?
O3 Cd2 N12 138.03(13) . 2_655 ?
O40 Cd2 N12 82.27(14) . 2_655 ?
O5 Cd2 N12 137.69(12) . 2_655 ?
O3 Cd2 O46 93.46(14) . . ?
O40 Cd2 O46 174.38(15) . . ?
O5 Cd2 O46 84.70(13) . . ?
N12 Cd2 O46 92.12(13) 2_655 . ?
O3 Cd2 O4 53.03(11) . . ?
O40 Cd2 O4 85.11(15) . . ?
O5 Cd2 O4 137.23(11) . . ?
N12 Cd2 O4 85.07(12) 2_655 . ?
O46 Cd2 O4 94.67(14) . . ?
O3 Cd2 O6 135.83(11) . . ?
O40 Cd2 O6 86.02(14) . . ?
O5 Cd2 O6 53.07(10) . . ?
N12 Cd2 O6 85.18(12) 2_655 . ?
O46 Cd2 O6 93.32(14) . . ?
O4 Cd2 O6 167.60(11) . . ?
O3 Cd2 C18 26.86(13) . . ?
O40 Cd2 C18 88.14(15) . . ?
O5 Cd2 C18 111.07(14) . . ?
N12 Cd2 C18 111.24(14) 2_655 . ?
O46 Cd2 C18 94.13(15) . . ?
O4 Cd2 C18 26.18(14) . . ?
O6 Cd2 C18 161.67(13) . . ?
C18 O3 Cd2 98.2(3) . . ?
C18 O4 Cd2 84.4(4) . . ?
C25 O5 Cd2 98.4(3) . . ?
C25 O6 Cd2 84.5(4) . . ?
C26 O8 Cd1 99.6(3) . 1_654 ?
C19 O9 Cd1 85.7(3) . . ?
C19 O10 Cd1 96.9(3) . . ?
C13 N11 C17 117.5(4) . . ?
C13 N11 Cd1 122.1(3) . 2_546 ?
C17 N11 Cd1 120.3(3) . 2_546 ?
C24 N12 C20 118.3(4) . . ?
C24 N12 Cd2 120.4(3) . 2_645 ?
C20 N12 Cd2 120.4(3) . 2_645 ?
N11 C13 C14 123.2(4) . . ?
C15 C14 C13 118.6(4) . . ?
C15 C14 C18 121.5(4) . . ?
C13 C14 C18 119.9(4) . . ?
C14 C15 C16 119.5(4) . . ?
C17 C16 C15 118.2(4) . . ?
C17 C16 C19 120.4(4) . . ?
C15 C16 C19 121.4(4) . . ?
N11 C17 C16 123.0(4) . . ?
O4 C18 O3 124.3(5) . . ?
O4 C18 C14 119.3(5) . . ?
O3 C18 C14 116.4(4) . . ?
O4 C18 Cd2 69.4(3) . . ?
O3 C18 Cd2 54.9(2) . . ?
C14 C18 Cd2 171.2(4) . . ?
O9 C19 O10 124.2(5) . . ?
O9 C19 C16 118.7(5) . . ?
O10 C19 C16 117.1(4) . . ?
O9 C19 Cd1 67.9(3) . . ?
O10 C19 Cd1 56.3(2) . . ?
C16 C19 Cd1 173.3(3) . . ?
N12 C20 C21 122.4(4) . . ?
C20 C21 C22 119.0(4) . . ?
C20 C21 C26 120.5(4) . . ?
C22 C21 C26 120.2(4) . . ?
C21 C22 C23 118.7(4) . . ?
C24 C23 C22 118.5(4) . . ?
C24 C23 C25 120.0(4) . . ?
C22 C23 C25 121.4(4) . . ?
N12 C24 C23 123.1(4) . . ?
O6 C25 O5 124.0(6) . . ?
O6 C25 C23 118.8(5) . . ?
O5 C25 C23 117.1(4) . . ?
O7 C26 O8 124.5(6) . . ?
O7 C26 C21 119.3(6) . . ?
O8 C26 C21 116.1(4) . . ?
C28 O27 Cd1 136.3(3) . . ?
O27 C28 N30 120.8(5) . . ?
O27 C28 C29 120.6(5) . . ?
N30 C28 C29 118.5(4) . . ?
C28 N30 C32 122.6(4) . . ?
C28 N30 C31 119.4(4) . . ?
C32 N30 C31 118.0(4) . . ?
C35 O34 Cd1 118.8(4) . . ?
N37 C35 O34 122.6(8) . . ?
N37 C35 C36 117.8(7) . . ?
O34 C35 C36 119.4(6) . . ?
C35 N37 C38 115.4(7) . . ?
C35 N37 C39 122.8(8) . . ?
C38 N37 C39 121.0(7) . . ?
C41 O40 Cd2 140.4(4) . . ?
O40 C41 N43 122.8(5) . . ?
O40 C41 C42 120.8(5) . . ?
N43 C41 C42 116.5(5) . . ?
C41 N43 C44 125.4(5) . . ?
C41 N43 C45 118.2(5) . . ?
C44 N43 C45 116.0(4) . . ?
C47 O46 Cd2 123.3(4) . . ?
N49 C47 O46 158.5(17) . . ?
N49 C47 C48 90.4(10) . . ?
O46 C47 C48 111.1(9) . . ?
C47 N49 C50 157.5(14) . . ?
C47 N49 C51 91.9(11) . . ?
C50 N49 C51 110.3(7) . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        26.37
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.963
_refine_diff_density_min         -0.679
_refine_diff_density_rms         0.106
_database_code_depnum_ccdc_archive 'CCDC 981484'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  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.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_gt23sq

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C27 H23 N5 O14 Sm2'
_chemical_formula_sum            'C27 H23 N5 O14 Sm2'
_chemical_formula_weight         942.20

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'
Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P nma'

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

_cell_length_a                   8.02340(10)
_cell_length_b                   30.2439(5)
_cell_length_c                   15.3280(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3719.48(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    110(2)
_cell_measurement_reflns_used    4076
_cell_measurement_theta_min      1.35
_cell_measurement_theta_max      28.33

_exptl_crystal_description       needle
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.683
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1824
_exptl_absorpt_coefficient_mu    3.192
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3847
_exptl_absorpt_correction_T_max  0.6460
_exptl_absorpt_process_details   'Sadabs, Bruker-AXS'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      110(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  'ApexDuo, Bruker-AXS'
_diffrn_measurement_method       '1.0 deg. φ and ω scans'
_diffrn_detector_area_resol_mean 1.75
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            19671
_diffrn_reflns_av_R_equivalents  0.0264
_diffrn_reflns_av_sigmaI/netI    0.0243
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.35
_diffrn_reflns_theta_max         28.33
_reflns_number_total             4694
_reflns_number_gt                4076
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Apex2, Bruker-AXS'
_computing_cell_refinement       'Saint, Bruker-AXS'
_computing_data_reduction        'Saint, Bruker-AXS'
_computing_structure_solution    'SHELXTL-2013 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_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. 

 The crystals contain severely disordered molecules of the DMF
 crystallization solvent within the interstitial voids, which could not
 be modeled reliably by discrete atoms. Its contribution to the
 diffraction pattern was thus subtracted by the Squeeze procedure,
 using the PLATON software (Spek, 2009).
 The metal coordinated DMF ligand is also partly disordered.

;

_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)+(0.0396P)²+1.7768P] 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         4694
_refine_ls_number_parameters     218
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0340
_refine_ls_R_factor_gt           0.0294
_refine_ls_wR_factor_ref         0.0781
_refine_ls_wR_factor_gt          0.0758
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_restrained_S_all      1.000
_refine_ls_shift/su_max          0.007
_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
Sm1 Sm 0.43608(2) 0.907010(5) 0.704300(10) 0.00620(6) Uani 1 1 d . . .
O2 O 0.6573(3) 0.86874(7) 0.81759(15) 0.0088(4) Uani 1 1 d . . .
O3 O 0.3913(3) 1.04198(8) 0.38552(15) 0.0127(5) Uani 1 1 d . . .
O4 O 0.2543(3) 0.95998(8) 0.65063(16) 0.0144(5) Uani 1 1 d . A .
O5 O 0.4882(3) 0.83050(8) 0.73235(16) 0.0129(5) Uani 1 1 d . . .
O6 O 0.2364(3) 1.09708(8) 0.33781(15) 0.0123(5) Uani 1 1 d . . .
O7 O 0.0013(3) 0.96958(8) 0.70828(14) 0.0121(5) Uani 1 1 d . . .
N8 N -0.0746(4) 1.08242(10) 0.5601(2) 0.0162(6) Uani 1 1 d . A .
N9 N 0.7875(6) 0.7500 0.9478(3) 0.0160(9) Uani 1 2 d S . .
C10 C 0.5963(4) 0.83219(11) 0.7916(2) 0.0073(6) Uani 1 1 d . . .
C11 C 0.5986(6) 0.7500 0.7945(3) 0.0100(9) Uani 1 2 d S . .
H11 H 0.5322 0.7500 0.7432 0.012 Uiso 1 2 calc SR . .
C12 C 0.1602(4) 1.06078(10) 0.4721(2) 0.0076(6) Uani 1 1 d . A .
C13 C 0.0242(5) 1.08790(11) 0.4904(2) 0.0135(7) Uani 1 1 d . . .
H13 H 0.0002 1.1115 0.4514 0.016 Uiso 1 1 calc R . .
C14 C 0.1191(4) 0.97985(10) 0.6584(2) 0.0082(6) Uani 1 1 d . . .
C15 C 0.2661(4) 1.06641(10) 0.3927(2) 0.0096(6) Uani 1 1 d . . .
C16 C -0.0415(4) 1.04793(11) 0.6123(2) 0.0128(6) Uani 1 1 d . . .
H16 H -0.1139 1.0427 0.6602 0.015 Uiso 1 1 calc R A .
C17 C 0.6482(4) 0.78958(10) 0.8328(2) 0.0097(6) Uani 1 1 d . . .
C18 C 0.0925(4) 1.01942(10) 0.6003(2) 0.0083(6) Uani 1 1 d . A .
C19 C 0.7424(4) 0.78794(11) 0.9089(2) 0.0129(7) Uani 1 1 d . A .
H19 H 0.7765 0.8150 0.9347 0.015 Uiso 1 1 calc R . .
C20 C 0.1959(4) 1.02656(10) 0.5298(2) 0.0097(6) Uani 1 1 d . . .
H20 H 0.2906 1.0083 0.5207 0.012 Uiso 1 1 calc R A .
O21 O 0.4383(3) 0.88243(8) 0.55347(16) 0.0159(5) Uani 1 1 d . A 1
C22 C 0.4401(4) 0.90602(12) 0.4868(2) 0.0145(7) Uani 1 1 d . A 1
H22 H 0.3858 0.9338 0.4925 0.017 Uiso 1 1 d R A 1
N23B N 0.4514(12) 0.8870(3) 0.4052(5) 0.0192(19) Uiso 0.435(12) 1 d P A 1
C24B C 0.4694(14) 0.9148(4) 0.3283(7) 0.022(2) Uiso 0.435(12) 1 d P A 1
H24D H 0.4630 0.9460 0.3454 0.033 Uiso 0.44 1 d P A 1
H24E H 0.3786 0.9081 0.2876 0.033 Uiso 0.44 1 d P A 1
H24F H 0.5766 0.9090 0.3004 0.033 Uiso 0.44 1 d P A 1
C25B C 0.4245(15) 0.8404(4) 0.3896(8) 0.040(3) Uiso 0.435(12) 1 d P A 1
H25D H 0.4563 0.8231 0.4421 0.060 Uiso 0.44 1 d P A 1
H25E H 0.4941 0.8303 0.3406 0.060 Uiso 0.44 1 d P A 1
H25F H 0.3075 0.8348 0.3765 0.060 Uiso 0.44 1 d P A 1
N23A N 0.5020(10) 0.8984(2) 0.4123(4) 0.0201(15) Uiso 0.565(12) 1 d P A 2
C24A C 0.4866(10) 0.9304(3) 0.3396(5) 0.0213(18) Uiso 0.565(12) 1 d P A 2
H24A H 0.4254 0.9573 0.3609 0.032 Uiso 0.56 1 d P A 2
H24B H 0.4279 0.9183 0.2904 0.032 Uiso 0.56 1 d P A 2
H24C H 0.5989 0.9406 0.3213 0.032 Uiso 0.56 1 d P A 2
C25A C 0.5916(11) 0.8577(3) 0.3951(6) 0.037(2) Uiso 0.565(12) 1 d P A 2
H25A H 0.7012 0.8634 0.3756 0.055 Uiso 0.56 1 d P A 2
H25B H 0.5281 0.8398 0.3529 0.055 Uiso 0.56 1 d P A 2
H25C H 0.5950 0.8403 0.4512 0.055 Uiso 0.56 1 d P A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sm1 O4 2.318(2) . ?
Sm1 O7 2.377(2) 6_657 ?
Sm1 O5 2.390(2) . ?
Sm1 O21 2.429(2) . ?
Sm1 O6 2.474(2) 2_575 ?
Sm1 O3 2.489(2) 5_676 ?
Sm1 O2 2.540(2) 6_557 ?
Sm1 O6 2.708(3) 5_676 ?
Sm1 O2 2.740(2) . ?
Sm1 C10 2.926(3) . ?
Sm1 C15 2.927(3) 5_676 ?
O2 C10 1.273(4) . ?
O2 Sm1 2.541(2) 6_657 ?
O3 C15 1.252(4) . ?
O3 Sm1 2.489(2) 5_676 ?
O4 C14 1.246(4) . ?
O5 C10 1.257(4) . ?
O6 C15 1.275(4) . ?
O6 Sm1 2.474(2) 2_574 ?
O6 Sm1 2.708(3) 5_676 ?
O7 C14 1.255(4) . ?
O7 Sm1 2.377(2) 6_557 ?
N8 C16 1.341(4) . ?
N8 C13 1.342(5) . ?
N9 C19 1.343(4) 7_575 ?
N9 C19 1.343(4) . ?
C10 C17 1.494(4) . ?
C11 C17 1.391(4) . ?
C11 C17 1.391(4) 7_575 ?
C12 C20 1.391(4) . ?
C12 C13 1.393(5) . ?
C12 C15 1.494(4) . ?
C14 C18 1.507(4) . ?
C15 Sm1 2.927(3) 5_676 ?
C16 C18 1.391(4) . ?
C17 C19 1.391(5) . ?
C18 C20 1.379(5) . ?
O21 C22 1.247(4) . ?
C22 N23B 1.380(9) . ?
N23B C25B 1.445(15) . ?
N23B C24B 1.454(13) . ?
N23A C25A 1.450(11) . ?
N23A C24A 1.480(10) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4 Sm1 O7 77.78(9) . 6_657 ?
O4 Sm1 O5 147.46(9) . . ?
O7 Sm1 O5 129.11(8) 6_657 . ?
O4 Sm1 O21 83.01(9) . . ?
O7 Sm1 O21 141.14(8) 6_657 . ?
O5 Sm1 O21 82.74(9) . . ?
O4 Sm1 O6 88.63(9) . 2_575 ?
O7 Sm1 O6 72.34(8) 6_657 2_575 ?
O5 Sm1 O6 84.29(8) . 2_575 ?
O21 Sm1 O6 140.93(8) . 2_575 ?
O4 Sm1 O3 74.06(8) . 5_676 ?
O7 Sm1 O3 72.30(8) 6_657 5_676 ?
O5 Sm1 O3 127.04(8) . 5_676 ?
O21 Sm1 O3 70.06(8) . 5_676 ?
O6 Sm1 O3 143.14(8) 2_575 5_676 ?
O4 Sm1 O2 73.38(8) . 6_557 ?
O7 Sm1 O2 129.11(8) 6_657 6_557 ?
O5 Sm1 O2 74.73(8) . 6_557 ?
O21 Sm1 O2 75.01(8) . 6_557 ?
O6 Sm1 O2 66.04(8) 2_575 6_557 ?
O3 Sm1 O2 134.36(8) 5_676 6_557 ?
O4 Sm1 O6 123.89(8) . 5_676 ?
O7 Sm1 O6 87.56(8) 6_657 5_676 ?
O5 Sm1 O6 80.15(8) . 5_676 ?
O21 Sm1 O6 75.63(8) . 5_676 ?
O6 Sm1 O6 137.53(7) 2_575 5_676 ?
O3 Sm1 O6 49.96(7) 5_676 5_676 ?
O2 Sm1 O6 143.29(7) 6_557 5_676 ?
O4 Sm1 O2 157.64(8) . . ?
O7 Sm1 O2 80.59(8) 6_657 . ?
O5 Sm1 O2 50.49(8) . . ?
O21 Sm1 O2 117.98(8) . . ?
O6 Sm1 O2 79.46(8) 2_575 . ?
O3 Sm1 O2 104.60(8) 5_676 . ?
O2 Sm1 O2 117.49(8) 6_557 . ?
O6 Sm1 O2 60.21(7) 5_676 . ?
O4 Sm1 C10 166.73(9) . . ?
O7 Sm1 C10 105.14(9) 6_657 . ?
O5 Sm1 C10 24.82(9) . . ?
O21 Sm1 C10 101.26(9) . . ?
O6 Sm1 C10 80.14(8) 2_575 . ?
O3 Sm1 C10 119.21(8) 5_676 . ?
O2 Sm1 C10 95.44(8) 6_557 . ?
O6 Sm1 C10 69.36(8) 5_676 . ?
O2 Sm1 C10 25.70(8) . . ?
O4 Sm1 C15 98.26(9) . 5_676 ?
O7 Sm1 C15 83.59(9) 6_657 5_676 ?
O5 Sm1 C15 102.38(9) . 5_676 ?
O21 Sm1 C15 66.06(8) . 5_676 ?
O6 Sm1 C15 152.99(8) 2_575 5_676 ?
O3 Sm1 C15 25.10(8) 5_676 5_676 ?
O2 Sm1 C15 140.95(8) 6_557 5_676 ?
O6 Sm1 C15 25.78(8) 5_676 5_676 ?
O2 Sm1 C15 84.79(8) . 5_676 ?
C10 Sm1 C15 94.94(9) . 5_676 ?
C10 O2 Sm1 133.9(2) . 6_657 ?
C10 O2 Sm1 85.35(18) . . ?
Sm1 O2 Sm1 107.11(8) 6_657 . ?
C15 O3 Sm1 97.44(19) . 5_676 ?
C14 O4 Sm1 148.0(2) . . ?
C10 O5 Sm1 102.2(2) . . ?
C15 O6 Sm1 127.9(2) . 2_574 ?
C15 O6 Sm1 86.7(2) . 5_676 ?
Sm1 O6 Sm1 110.08(9) 2_574 5_676 ?
C14 O7 Sm1 134.9(2) . 6_557 ?
C16 N8 C13 117.0(3) . . ?
C19 N9 C19 117.4(4) 7_575 . ?
O5 C10 O2 121.8(3) . . ?
O5 C10 C17 117.6(3) . . ?
O2 C10 C17 120.6(3) . . ?
O5 C10 Sm1 52.98(17) . . ?
O2 C10 Sm1 68.95(17) . . ?
C17 C10 Sm1 169.3(2) . . ?
C17 C11 C17 118.7(4) . 7_575 ?
C20 C12 C13 118.2(3) . . ?
C20 C12 C15 119.0(3) . . ?
C13 C12 C15 122.8(3) . . ?
N8 C13 C12 123.3(3) . . ?
O4 C14 O7 126.5(3) . . ?
O4 C14 C18 116.7(3) . . ?
O7 C14 C18 116.8(3) . . ?
O3 C15 O6 121.4(3) . . ?
O3 C15 C12 117.5(3) . . ?
O6 C15 C12 121.0(3) . . ?
O3 C15 Sm1 57.46(17) . 5_676 ?
O6 C15 Sm1 67.49(18) . 5_676 ?
C12 C15 Sm1 155.4(2) . 5_676 ?
N8 C16 C18 123.8(3) . . ?
C11 C17 C19 118.6(3) . . ?
C11 C17 C10 119.0(3) . . ?
C19 C17 C10 122.4(3) . . ?
C20 C18 C16 118.2(3) . . ?
C20 C18 C14 120.2(3) . . ?
C16 C18 C14 121.6(3) . . ?
N9 C19 C17 123.3(3) . . ?
C18 C20 C12 119.4(3) . . ?
C22 O21 Sm1 127.3(2) . . ?
O21 C22 N23B 120.4(5) . . ?
C22 N23B C25B 123.1(8) . . ?
C22 N23B C24B 120.0(8) . . ?
C25B N23B C24B 116.4(9) . . ?
C25A N23A C24A 117.3(6) . . ?

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.018 0.250 0.750 426 166 ' '
2 -0.046 0.750 0.250 426 166 ' '
_platon_squeeze_details          
;
 The residual density accounts of the disordered DMF crystallization
 solvent.
;

# start Validation Reply Form
_vrf_PLAT201_gt23sq              
;
PROBLEM:  isotropic atoms in the main residue
RESPONSE:  The metal-coordinated DMF ligand exhibits 2-fold disorder.
          The disordered NMe2 residue was thus assigned isotropic-U only
;
_vrf_PLAT220_gt23sq              
;
PROBLEM:  large non-solvent Ueq(max)/Ueq(min)
RESPONSE: The disordered methyl residue has considerably higher ADPs
          than the heavy Sm ion.
;
#end Validation Reply Form


_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        28.33
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         1.690
_refine_diff_density_min         -1.746
_refine_diff_density_rms         0.137
_database_code_depnum_ccdc_archive 'CCDC 981485'
