# Electronic Supplementary Material (ESI) for Dalton Transactions.
# 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_datam

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C17 H13 N3 O2'
_chemical_formula_sum            'C17 H13 N3 O2'
_chemical_formula_weight         291.30

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'

_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                   10.737(6)
_cell_length_b                   8.327(5)
_cell_length_c                   16.382(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 94.588(10)
_cell_angle_gamma                90.00
_cell_volume                     1459.9(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    301(2)
_cell_measurement_reflns_used    2057
_cell_measurement_theta_min      3.0
_cell_measurement_theta_max      27.5

_exptl_crystal_description       Block
_exptl_crystal_colour            Colorless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.325
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             608
_exptl_absorpt_coefficient_mu    0.090
_exptl_absorpt_correction_type   Empirical
_exptl_absorpt_correction_T_min  0.9823
_exptl_absorpt_correction_T_max  0.9911
_exptl_absorpt_process_details   'Acta Crystallogr A. (1995), 51, 33'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      301(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  
;
Rigaku Saturn724+ (4x4 bin mode)
;
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            11565
_diffrn_reflns_av_R_equivalents  0.0469
_diffrn_reflns_av_sigmaI/netI    0.0448
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.10
_diffrn_reflns_theta_max         26.50
_reflns_number_total             3015
_reflns_number_gt                1954
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrystalClear-SM Expert 2.0 r14k (Rigaku, 2012)
;
_computing_cell_refinement       
;
CrystalClear-SM Expert 2.0 r14k (Rigaku, 2012)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 2.0 r14k (Rigaku, 2012)
;
_computing_structure_solution    'SHELXTL (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0780P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3015
_refine_ls_number_parameters     203
_refine_ls_number_restraints     56
_refine_ls_R_factor_all          0.0860
_refine_ls_R_factor_gt           0.0534
_refine_ls_wR_factor_ref         0.1523
_refine_ls_wR_factor_gt          0.1360
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_restrained_S_all      1.042
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
N22 N 0.85880(16) 0.16037(18) 0.18859(9) 0.0493(4) Uani 1 1 d U . .
C21 C 1.0358(2) 0.4035(2) 0.27954(10) 0.0488(5) Uani 1 1 d U . .
H21A H 0.9770 0.4568 0.2446 0.059 Uiso 1 1 calc R . .
N20 N 0.87153(16) 0.23274(19) 0.32631(8) 0.0514(4) Uani 1 1 d U . .
C19 C 0.99856(19) 0.2787(2) 0.32892(10) 0.0450(5) Uani 1 1 d U . .
C18 C 1.24886(19) 0.3713(2) 0.33477(10) 0.0466(5) Uani 1 1 d U . .
C17 C 0.80022(19) 0.2223(2) 0.25029(11) 0.0440(5) Uani 1 1 d U . .
C16 C 1.0878(2) 0.2002(2) 0.38001(11) 0.0514(5) Uani 1 1 d U . .
H16A H 1.0643 0.1155 0.4124 0.062 Uiso 1 1 calc R . .
C15 C 1.2112(2) 0.2465(2) 0.38319(10) 0.0510(5) Uani 1 1 d U . .
H15A H 1.2700 0.1934 0.4182 0.061 Uiso 1 1 calc R . .
O14 O 1.40438(17) 0.5486(2) 0.29982(10) 0.0798(5) Uani 1 1 d U . .
C13 C 1.3817(2) 0.4212(3) 0.34218(12) 0.0559(5) Uani 1 1 d U . .
C12 C 1.1595(2) 0.4479(2) 0.28246(10) 0.0491(5) Uani 1 1 d U . .
H12A H 1.1836 0.5305 0.2489 0.059 Uiso 1 1 calc R . .
C8 C 0.8557(3) 0.2963(3) 0.46716(11) 0.0688(7) Uani 1 1 d U . .
H8A H 0.9215 0.3686 0.4660 0.083 Uiso 1 1 calc R . .
O10 O 1.46210(18) 0.3539(2) 0.38469(13) 0.1084(7) Uani 1 1 d U . .
C9 C 0.6778(2) 0.2746(2) 0.24093(12) 0.0526(5) Uani 1 1 d U . .
H9A H 0.6396 0.3177 0.2850 0.063 Uiso 1 1 calc R . .
N11 N 0.7180(2) 0.0999(2) 0.39704(13) 0.0826(7) Uani 1 1 d U . .
C7 C 0.8135(2) 0.2093(2) 0.39994(11) 0.0534(5) Uani 1 1 d U . .
C6 C 0.7941(2) 0.1497(2) 0.11518(11) 0.0600(6) Uani 1 1 d U . .
H6A H 0.8341 0.1079 0.0716 0.072 Uiso 1 1 calc R . .
C5 C 0.6140(2) 0.2619(3) 0.16540(14) 0.0635(6) Uani 1 1 d U . .
H5A H 0.5316 0.2968 0.1574 0.076 Uiso 1 1 calc R . .
C4 C 0.6727(2) 0.1969(3) 0.10133(13) 0.0682(7) Uani 1 1 d U . .
H4A H 0.6304 0.1855 0.0498 0.082 Uiso 1 1 calc R . .
C3 C 0.6977(5) 0.1644(6) 0.5374(3) 0.152(2) Uani 1 1 d U . .
H3A H 0.6569 0.1488 0.5848 0.183 Uiso 1 1 calc R . .
C2 C 0.7948(4) 0.2703(5) 0.53665(17) 0.1238(15) Uani 1 1 d U . .
H2A H 0.8203 0.3262 0.5843 0.149 Uiso 1 1 calc R . .
C1 C 0.6616(3) 0.0819(4) 0.4675(3) 0.1215(13) Uani 1 1 d U . .
H1A H 0.5953 0.0102 0.4683 0.146 Uiso 1 1 calc R . .
H14 H 1.499(3) 0.586(3) 0.3077(15) 0.113(10) Uiso 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
N22 C17 1.336(2) . ?
N22 C6 1.343(3) . ?
C21 C12 1.375(3) . ?
C21 C19 1.395(2) . ?
C21 H21A 0.9300 . ?
N20 C17 1.411(2) . ?
N20 C19 1.414(3) . ?
N20 C7 1.415(2) . ?
C19 C16 1.385(3) . ?
C18 C15 1.387(3) . ?
C18 C12 1.390(3) . ?
C18 C13 1.481(3) . ?
C17 C9 1.381(3) . ?
C16 C15 1.376(3) . ?
C16 H16A 0.9300 . ?
C15 H15A 0.9300 . ?
O14 C13 1.302(2) . ?
O14 H14 1.06(3) . ?
C13 O10 1.203(3) . ?
C12 H12A 0.9300 . ?
C8 C7 1.365(3) . ?
C8 C2 1.375(4) . ?
C8 H8A 0.9300 . ?
C9 C5 1.370(3) . ?
C9 H9A 0.9300 . ?
N11 C1 1.354(3) . ?
N11 C7 1.370(3) . ?
C6 C4 1.363(3) . ?
C6 H6A 0.9300 . ?
C5 C4 1.377(3) . ?
C5 H5A 0.9300 . ?
C4 H4A 0.9300 . ?
C3 C1 1.365(6) . ?
C3 C2 1.367(6) . ?
C3 H3A 0.9300 . ?
C2 H2A 0.9300 . ?
C1 H1A 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C17 N22 C6 117.50(19) . . ?
C12 C21 C19 120.07(19) . . ?
C12 C21 H21A 120.0 . . ?
C19 C21 H21A 120.0 . . ?
C17 N20 C19 119.82(14) . . ?
C17 N20 C7 119.91(18) . . ?
C19 N20 C7 120.09(16) . . ?
C16 C19 C21 119.02(19) . . ?
C16 C19 N20 120.64(17) . . ?
C21 C19 N20 120.34(18) . . ?
C15 C18 C12 118.55(19) . . ?
C15 C18 C13 119.07(18) . . ?
C12 C18 C13 122.36(17) . . ?
N22 C17 C9 122.62(18) . . ?
N22 C17 N20 115.87(18) . . ?
C9 C17 N20 121.50(17) . . ?
C15 C16 C19 120.53(17) . . ?
C15 C16 H16A 119.7 . . ?
C19 C16 H16A 119.7 . . ?
C16 C15 C18 120.79(19) . . ?
C16 C15 H15A 119.6 . . ?
C18 C15 H15A 119.6 . . ?
C13 O14 H14 113.1(15) . . ?
O10 C13 O14 122.1(2) . . ?
O10 C13 C18 124.0(2) . . ?
O14 C13 C18 113.88(19) . . ?
C21 C12 C18 121.02(17) . . ?
C21 C12 H12A 119.5 . . ?
C18 C12 H12A 119.5 . . ?
C7 C8 C2 115.8(3) . . ?
C7 C8 H8A 122.1 . . ?
C2 C8 H8A 122.1 . . ?
C5 C9 C17 118.6(2) . . ?
C5 C9 H9A 120.7 . . ?
C17 C9 H9A 120.7 . . ?
C1 N11 C7 115.4(3) . . ?
C8 C7 N11 125.5(2) . . ?
C8 C7 N20 118.3(2) . . ?
N11 C7 N20 116.23(19) . . ?
N22 C6 C4 123.34(19) . . ?
N22 C6 H6A 118.3 . . ?
C4 C6 H6A 118.3 . . ?
C9 C5 C4 119.5(2) . . ?
C9 C5 H5A 120.3 . . ?
C4 C5 H5A 120.3 . . ?
C6 C4 C5 118.4(2) . . ?
C6 C4 H4A 120.8 . . ?
C5 C4 H4A 120.8 . . ?
C1 C3 C2 118.8(3) . . ?
C1 C3 H3A 120.6 . . ?
C2 C3 H3A 120.6 . . ?
C3 C2 C8 121.6(3) . . ?
C3 C2 H2A 119.2 . . ?
C8 C2 H2A 119.2 . . ?
N11 C1 C3 123.0(4) . . ?
N11 C1 H1A 118.5 . . ?
C3 C1 H1A 118.5 . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        26.50
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.221
_refine_diff_density_min         -0.200
_refine_diff_density_rms         0.036
_vrf_PLAT230_datam               
;
PROBLEM:Hirshfeld Test Diff for    C2     --  C8      ..       13.3 su
RESPONSE: The data was collected at room temperature and the rotational
freedom the pyridyl moiety could be a probable reason for the error. However,
the probability of disorder, model or data errors can be ruled out, since 
our disorder modelling resulted in unstable refinement and also the residual
electron density is neglegible.
;


_database_code_depnum_ccdc_archive 'CCDC 980347'
#######################################################################
#
#                 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_datam

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C51 H40 Gd N9 O8'
_chemical_formula_sum            'C51 H40 Gd N9 O8'
_chemical_formula_weight         1064.17

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'
Gd Gd -0.1653 3.9035 '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                   30.229(8)
_cell_length_b                   14.919(3)
_cell_length_c                   10.217(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 102.947(3)
_cell_angle_gamma                90.00
_cell_volume                     4490.5(19)
_cell_formula_units_Z            4
_cell_measurement_temperature    300(2)
_cell_measurement_reflns_used    3298
_cell_measurement_theta_min      3.0
_cell_measurement_theta_max      27.5

_exptl_crystal_description       Block
_exptl_crystal_colour            Colorless
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.574
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2148
_exptl_absorpt_coefficient_mu    1.545
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.6543
_exptl_absorpt_correction_T_max  0.7475
_exptl_absorpt_process_details   'SADABS; Sheldrick, 1997'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      300(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  
;
Rigaku Saturn724+ (4x4 bin mode)
;
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            19060
_diffrn_reflns_av_R_equivalents  0.0540
_diffrn_reflns_av_sigmaI/netI    0.0443
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         3.06
_diffrn_reflns_theta_max         27.47
_reflns_number_total             5057
_reflns_number_gt                4121
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrystalClear-SM Expert 2.0 r14k (Rigaku, 2012)
;
_computing_cell_refinement       
;
CrystalClear-SM Expert 2.0 r14k (Rigaku, 2012)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 2.0 r14k (Rigaku, 2012)
;
_computing_structure_solution    'SHELXTL (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0338P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5057
_refine_ls_number_parameters     318
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0403
_refine_ls_R_factor_gt           0.0282
_refine_ls_wR_factor_ref         0.0709
_refine_ls_wR_factor_gt          0.0651
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_restrained_S_all      1.020
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Gd1 Gd 0.5000 0.000922(10) 0.2500 0.01900(6) Uani 1 2 d S . .
O36 O 0.48013(7) 0.14021(13) 0.1099(2) 0.0356(5) Uani 1 1 d . . .
H36 H 0.4716 0.1262 0.0306 0.053 Uiso 1 1 calc R . .
C35 C 0.37330(7) 0.06472(14) 0.4234(2) 0.0206(5) Uani 1 1 d . . .
C34 C 0.42244(8) 0.03875(16) 0.4452(3) 0.0238(5) Uani 1 1 d . . .
O33 O 0.52161(7) -0.14971(11) 0.1766(2) 0.0364(5) Uani 1 1 d . . .
N32 N 0.22006(8) 0.03494(17) 0.4923(3) 0.0380(6) Uani 1 1 d . . .
O31 O 0.43768(6) 0.02389(13) 0.3430(2) 0.0332(5) Uani 1 1 d . . .
C30 C 0.34555(8) 0.06290(16) 0.2955(3) 0.0271(5) Uani 1 1 d . . .
H30 H 0.3575 0.0452 0.2231 0.033 Uiso 1 1 calc R . .
C29 C 0.30983(8) 0.11822(16) 0.5083(3) 0.0282(6) Uani 1 1 d . . .
H29 H 0.2978 0.1366 0.5801 0.034 Uiso 1 1 calc R . .
C28 C 0.28268(8) 0.11579(16) 0.3799(3) 0.0271(6) Uani 1 1 d . . .
O27 O 0.55470(6) -0.03433(15) 0.4376(2) 0.0388(5) Uani 1 1 d . . .
C26 C 0.30047(8) 0.08712(17) 0.2743(3) 0.0306(6) Uani 1 1 d . . .
H26 H 0.2820 0.0841 0.1884 0.037 Uiso 1 1 calc R . .
N25 N 0.23630(7) 0.14643(14) 0.3533(2) 0.0316(5) Uani 1 1 d . . .
C24 C 0.35512(8) 0.09319(16) 0.5296(3) 0.0253(5) Uani 1 1 d . . .
H24 H 0.3734 0.0955 0.6158 0.030 Uiso 1 1 calc R . .
N23 N 0.18249(8) 0.22122(16) 0.1889(3) 0.0472(7) Uani 1 1 d . . .
C22 C 0.45924(9) -0.62278(17) 0.2393(3) 0.0344(6) Uani 1 1 d . . .
N21 N 0.46177(8) -0.69913(15) 0.3095(3) 0.0436(6) Uani 1 1 d . . .
C20 C 0.20579(8) 0.10976(17) 0.4247(3) 0.0305(6) Uani 1 1 d . . .
C19 C 0.5000 -0.2926(2) 0.2500 0.0341(9) Uani 1 2 d S . .
C18 C 0.22473(9) 0.21861(17) 0.2612(3) 0.0309(6) Uani 1 1 d . . .
C17 C 0.5000 -0.1913(2) 0.2500 0.0306(8) Uani 1 2 d S . .
C16 C 0.52336(11) -0.43269(17) 0.1699(3) 0.0463(8) Uani 1 1 d . . .
H16 H 0.5389 -0.4638 0.1151 0.056 Uiso 1 1 calc R . .
N15 N 0.5000 -0.57550(19) 0.2500 0.0385(8) Uani 1 2 d S . .
C14 C 0.52372(11) -0.33972(18) 0.1710(3) 0.0445(8) Uani 1 1 d . . .
H14 H 0.5400 -0.3088 0.1182 0.053 Uiso 1 1 calc R . .
C13 C 0.25688(10) 0.2830(2) 0.2534(3) 0.0393(7) Uani 1 1 d . . .
H13 H 0.2862 0.2784 0.3056 0.047 Uiso 1 1 calc R . .
C12 C 0.16385(9) 0.1485(2) 0.4269(3) 0.0444(8) Uani 1 1 d . . .
H12 H 0.1538 0.1995 0.3765 0.053 Uiso 1 1 calc R . .
C11 C 0.38233(11) -0.7201(2) 0.2203(4) 0.0588(10) Uani 1 1 d . . .
H11 H 0.3565 -0.7549 0.2156 0.071 Uiso 1 1 calc R . .
C10 C 0.41934(10) -0.5920(2) 0.1606(3) 0.0510(8) Uani 1 1 d . . .
H10 H 0.4186 -0.5381 0.1142 0.061 Uiso 1 1 calc R . .
C9 C 0.38045(11) -0.6417(2) 0.1510(4) 0.0613(10) Uani 1 1 d . . .
H9 H 0.3531 -0.6220 0.0976 0.074 Uiso 1 1 calc R . .
C8 C 0.42302(11) -0.74575(19) 0.2966(4) 0.0571(10) Uani 1 1 d . . .
H8 H 0.4242 -0.7995 0.3433 0.069 Uiso 1 1 calc R . .
C7 C 0.19392(12) -0.0001(2) 0.5692(4) 0.0488(9) Uani 1 1 d . . .
H7 H 0.2042 -0.0514 0.6185 0.059 Uiso 1 1 calc R . .
C6 C 0.13781(10) 0.1091(2) 0.5060(4) 0.0540(9) Uani 1 1 d . . .
H6 H 0.1097 0.1334 0.5091 0.065 Uiso 1 1 calc R . .
C5 C 0.5000 -0.4793(2) 0.2500 0.0356(10) Uani 1 2 d S . .
C4 C 0.15316(11) 0.0348(3) 0.5794(4) 0.0547(9) Uani 1 1 d . . .
H4 H 0.1363 0.0085 0.6350 0.066 Uiso 1 1 calc R . .
C3 C 0.20074(15) 0.3596(2) 0.0929(4) 0.0606(11) Uani 1 1 d . . .
H3 H 0.1915 0.4073 0.0346 0.073 Uiso 1 1 calc R . .
C2 C 0.17122(13) 0.2933(2) 0.1075(3) 0.0606(10) Uani 1 1 d . . .
H2 H 0.1414 0.2978 0.0585 0.073 Uiso 1 1 calc R . .
C1 C 0.24463(14) 0.3539(2) 0.1668(4) 0.0545(9) Uani 1 1 d . . .
H1 H 0.2658 0.3974 0.1584 0.065 Uiso 1 1 calc R . .
H37 H 0.4897(11) 0.187(2) 0.126(3) 0.050(11) Uiso 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
Gd1 O27 2.2944(19) . ?
Gd1 O27 2.2944(19) 2_655 ?
Gd1 O31 2.3176(18) 2_655 ?
Gd1 O31 2.3176(18) . ?
Gd1 O33 2.5019(17) . ?
Gd1 O33 2.5019(17) 2_655 ?
Gd1 O36 2.5185(19) 2_655 ?
Gd1 O36 2.5185(19) . ?
Gd1 C17 2.868(3) . ?
O36 H36 0.8200 . ?
O36 H37 0.76(3) . ?
C35 C30 1.386(3) . ?
C35 C24 1.388(3) . ?
C35 C34 1.503(3) . ?
C34 O27 1.243(3) 5_656 ?
C34 O31 1.252(3) . ?
O33 C17 1.262(2) . ?
N32 C20 1.332(4) . ?
N32 C7 1.339(4) . ?
C30 C26 1.379(3) . ?
C30 H30 0.9300 . ?
C29 C28 1.383(4) . ?
C29 C24 1.388(3) . ?
C29 H29 0.9300 . ?
C28 C26 1.377(4) . ?
C28 N25 1.442(3) . ?
O27 C34 1.243(3) 5_656 ?
C26 H26 0.9300 . ?
N25 C20 1.408(3) . ?
N25 C18 1.421(3) . ?
C24 H24 0.9300 . ?
N23 C18 1.325(3) . ?
N23 C2 1.355(4) . ?
C22 N21 1.339(3) . ?
C22 C10 1.371(4) . ?
C22 N15 1.403(3) . ?
N21 C8 1.343(4) . ?
C20 C12 1.398(3) . ?
C19 C14 1.386(3) . ?
C19 C14 1.386(3) 2_655 ?
C19 C17 1.511(4) . ?
C18 C13 1.381(4) . ?
C17 O33 1.262(2) 2_655 ?
C16 C5 1.382(3) . ?
C16 C14 1.387(4) . ?
C16 H16 0.9300 . ?
N15 C22 1.403(3) 2_655 ?
N15 C5 1.436(4) . ?
C14 H14 0.9300 . ?
C13 C1 1.375(4) . ?
C13 H13 0.9300 . ?
C12 C6 1.380(4) . ?
C12 H12 0.9300 . ?
C11 C8 1.355(4) . ?
C11 C9 1.361(5) . ?
C11 H11 0.9300 . ?
C10 C9 1.375(4) . ?
C10 H10 0.9300 . ?
C9 H9 0.9300 . ?
C8 H8 0.9300 . ?
C7 C4 1.363(5) . ?
C7 H7 0.9300 . ?
C6 C4 1.361(5) . ?
C6 H6 0.9300 . ?
C5 C16 1.382(3) 2_655 ?
C4 H4 0.9300 . ?
C3 C2 1.363(5) . ?
C3 C1 1.375(5) . ?
C3 H3 0.9300 . ?
C2 H2 0.9300 . ?
C1 H1 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O27 Gd1 O27 153.50(11) . 2_655 ?
O27 Gd1 O31 82.90(7) . 2_655 ?
O27 Gd1 O31 101.03(7) 2_655 2_655 ?
O27 Gd1 O31 101.03(7) . . ?
O27 Gd1 O31 82.90(7) 2_655 . ?
O31 Gd1 O31 162.99(9) 2_655 . ?
O27 Gd1 O33 81.77(7) . . ?
O27 Gd1 O33 74.42(7) 2_655 . ?
O31 Gd1 O33 73.69(6) 2_655 . ?
O31 Gd1 O33 123.13(6) . . ?
O27 Gd1 O33 74.42(7) . 2_655 ?
O27 Gd1 O33 81.77(7) 2_655 2_655 ?
O31 Gd1 O33 123.13(6) 2_655 2_655 ?
O31 Gd1 O33 73.69(6) . 2_655 ?
O33 Gd1 O33 52.14(8) . 2_655 ?
O27 Gd1 O36 71.27(7) . 2_655 ?
O27 Gd1 O36 134.38(7) 2_655 2_655 ?
O31 Gd1 O36 89.92(7) 2_655 2_655 ?
O31 Gd1 O36 75.96(7) . 2_655 ?
O33 Gd1 O36 150.06(7) . 2_655 ?
O33 Gd1 O36 128.01(6) 2_655 2_655 ?
O27 Gd1 O36 134.38(7) . . ?
O27 Gd1 O36 71.27(7) 2_655 . ?
O31 Gd1 O36 75.96(7) 2_655 . ?
O31 Gd1 O36 89.92(7) . . ?
O33 Gd1 O36 128.01(6) . . ?
O33 Gd1 O36 150.06(7) 2_655 . ?
O36 Gd1 O36 68.80(10) 2_655 . ?
O27 Gd1 C17 76.75(6) . . ?
O27 Gd1 C17 76.75(6) 2_655 . ?
O31 Gd1 C17 98.50(5) 2_655 . ?
O31 Gd1 C17 98.50(5) . . ?
O33 Gd1 C17 26.07(4) . . ?
O33 Gd1 C17 26.07(4) 2_655 . ?
O36 Gd1 C17 145.60(5) 2_655 . ?
O36 Gd1 C17 145.60(5) . . ?
Gd1 O36 H36 109.5 . . ?
Gd1 O36 H37 127(3) . . ?
H36 O36 H37 118.2 . . ?
C30 C35 C24 118.8(2) . . ?
C30 C35 C34 120.2(2) . . ?
C24 C35 C34 121.0(2) . . ?
O27 C34 O31 124.4(2) 5_656 . ?
O27 C34 C35 118.3(2) 5_656 . ?
O31 C34 C35 117.3(2) . . ?
C17 O33 Gd1 93.37(17) . . ?
C20 N32 C7 117.8(3) . . ?
C34 O31 Gd1 148.53(18) . . ?
C26 C30 C35 120.7(2) . . ?
C26 C30 H30 119.7 . . ?
C35 C30 H30 119.7 . . ?
C28 C29 C24 119.8(2) . . ?
C28 C29 H29 120.1 . . ?
C24 C29 H29 120.1 . . ?
C26 C28 C29 119.9(2) . . ?
C26 C28 N25 119.0(2) . . ?
C29 C28 N25 121.1(2) . . ?
C34 O27 Gd1 163.35(19) 5_656 . ?
C28 C26 C30 120.3(2) . . ?
C28 C26 H26 119.9 . . ?
C30 C26 H26 119.9 . . ?
C20 N25 C18 123.0(2) . . ?
C20 N25 C28 120.1(2) . . ?
C18 N25 C28 116.7(2) . . ?
C35 C24 C29 120.6(2) . . ?
C35 C24 H24 119.7 . . ?
C29 C24 H24 119.7 . . ?
C18 N23 C2 116.4(3) . . ?
N21 C22 C10 122.5(3) . . ?
N21 C22 N15 116.3(2) . . ?
C10 C22 N15 121.3(2) . . ?
C22 N21 C8 116.3(3) . . ?
N32 C20 C12 121.8(3) . . ?
N32 C20 N25 114.9(2) . . ?
C12 C20 N25 123.3(3) . . ?
C14 C19 C14 119.0(3) . 2_655 ?
C14 C19 C17 120.51(17) . . ?
C14 C19 C17 120.51(17) 2_655 . ?
N23 C18 C13 123.4(3) . . ?
N23 C18 N25 117.0(2) . . ?
C13 C18 N25 119.6(3) . . ?
O33 C17 O33 121.1(3) . 2_655 ?
O33 C17 C19 119.43(15) . . ?
O33 C17 C19 119.43(15) 2_655 . ?
O33 C17 Gd1 60.57(15) . . ?
O33 C17 Gd1 60.57(15) 2_655 . ?
C19 C17 Gd1 180.0 . . ?
C5 C16 C14 120.1(3) . . ?
C5 C16 H16 119.9 . . ?
C14 C16 H16 119.9 . . ?
C22 N15 C22 119.6(3) 2_655 . ?
C22 N15 C5 120.19(14) 2_655 . ?
C22 N15 C5 120.19(14) . . ?
C19 C14 C16 120.5(3) . . ?
C19 C14 H14 119.7 . . ?
C16 C14 H14 119.7 . . ?
C1 C13 C18 118.7(3) . . ?
C1 C13 H13 120.6 . . ?
C18 C13 H13 120.6 . . ?
C6 C12 C20 118.1(3) . . ?
C6 C12 H12 120.9 . . ?
C20 C12 H12 120.9 . . ?
C8 C11 C9 117.9(3) . . ?
C8 C11 H11 121.0 . . ?
C9 C11 H11 121.0 . . ?
C22 C10 C9 119.1(3) . . ?
C22 C10 H10 120.4 . . ?
C9 C10 H10 120.4 . . ?
C11 C9 C10 119.4(3) . . ?
C11 C9 H9 120.3 . . ?
C10 C9 H9 120.3 . . ?
N21 C8 C11 124.7(3) . . ?
N21 C8 H8 117.6 . . ?
C11 C8 H8 117.6 . . ?
N32 C7 C4 123.9(3) . . ?
N32 C7 H7 118.0 . . ?
C4 C7 H7 118.0 . . ?
C4 C6 C12 120.1(3) . . ?
C4 C6 H6 120.0 . . ?
C12 C6 H6 120.0 . . ?
C16 C5 C16 119.7(3) 2_655 . ?
C16 C5 N15 120.17(17) 2_655 . ?
C16 C5 N15 120.17(17) . . ?
C6 C4 C7 118.1(3) . . ?
C6 C4 H4 120.9 . . ?
C7 C4 H4 120.9 . . ?
C2 C3 C1 118.0(3) . . ?
C2 C3 H3 121.0 . . ?
C1 C3 H3 121.0 . . ?
N23 C2 C3 124.2(3) . . ?
N23 C2 H2 117.9 . . ?
C3 C2 H2 117.9 . . ?
C3 C1 C13 119.3(3) . . ?
C3 C1 H1 120.4 . . ?
C13 C1 H1 120.4 . . ?

_diffrn_measured_fraction_theta_max 0.982
_diffrn_reflns_theta_full        27.47
_diffrn_measured_fraction_theta_full 0.982
_refine_diff_density_max         0.666
_refine_diff_density_min         -0.661
_refine_diff_density_rms         0.073
_database_code_depnum_ccdc_archive 'CCDC 975130'
