# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1
_database_code_depnum_ccdc_archive 'CCDC 1401613'
_audit_update_record             
;
2015-05-19 deposited with the CCDC.
2015-10-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        NiGdCr
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H18 Cr Gd N8 Ni O8, 0.651(C O), 2(O)'
_chemical_formula_sum            'C24.65 H18 Cr Gd N8 Ni O10.65'
_chemical_formula_weight         864.64

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   13.071(3)
_cell_length_b                   12.139(2)
_cell_length_c                   21.735(4)
_cell_angle_alpha                90
_cell_angle_beta                 106.84(3)
_cell_angle_gamma                90
_cell_volume                     3300.8(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.740
_exptl_crystal_F_000             1692.5
_exptl_transmission_factor_min   0.520
_exptl_transmission_factor_max   0.560
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.17
_exptl_absorpt_coefficient_mu    2.938
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.540
_exptl_absorpt_correction_T_max  0.625
_exptl_absorpt_process_details   'Absorption correction given as multi-scan'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker Smart Aepex CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            15133
_diffrn_reflns_av_unetI/netI     0.0657
_diffrn_reflns_av_R_equivalents  0.0437
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         3.257
_diffrn_reflns_theta_max         26.015
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measured_fraction_theta_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_point_group_measured_fraction_full 0.991
_reflns_number_total             6311
_reflns_number_gt                5461
_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       'SMART (Bruker, 2000)'
_computing_cell_refinement       SMART
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics    'diamond 3.0'
_computing_publication_material  'diamond 3.0'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0429P)²+3.8543P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6311
_refine_ls_number_parameters     427
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0607
_refine_ls_R_factor_gt           0.0497
_refine_ls_wR_factor_ref         0.1050
_refine_ls_wR_factor_gt          0.0985
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_restrained_S_all      1.085
_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_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
C1 C 0.5526(4) 0.2280(4) 0.1762(3) 0.0185(12) Uani 1 1 d . . . . .
C2 C 0.6597(5) 0.4147(5) 0.1352(3) 0.0340(16) Uani 1 1 d . . . . .
C3 C 0.7477(5) 0.3156(5) 0.2584(3) 0.0256(13) Uani 1 1 d . . . . .
C4 C 0.8543(4) 0.2862(4) 0.1612(3) 0.0191(12) Uani 1 1 d . . . . .
C5 C 0.7535(5) 0.1003(5) 0.2004(3) 0.0279(14) Uani 1 1 d . . . . .
C6 C 0.6437(5) 0.1887(5) 0.0750(3) 0.0265(14) Uani 1 1 d . . . . .
C7 C 0.3418(4) 0.5004(5) 0.1466(3) 0.0235(13) Uani 1 1 d . . . . .
C8 C 0.3904(5) 0.6025(5) 0.1566(3) 0.0309(15) Uani 1 1 d . . . . .
H8 H 0.4395 0.6193 0.1958 0.037 Uiso 1 1 calc R U . . .
C9 C 0.3649(5) 0.6808(5) 0.1070(4) 0.0395(17) Uani 1 1 d . . . . .
H9 H 0.3975 0.7497 0.1135 0.047 Uiso 1 1 calc R U . . .
C10 C 0.2931(5) 0.6567(5) 0.0496(3) 0.0344(16) Uani 1 1 d . . . . .
H10 H 0.2779 0.7090 0.0169 0.041 Uiso 1 1 calc R U . . .
C11 C 0.2416(5) 0.5545(5) 0.0389(3) 0.0282(14) Uani 1 1 d . . . . .
C12 C 0.2661(5) 0.4755(5) 0.0884(3) 0.0234(13) Uani 1 1 d . . . . .
C13 C 0.1653(6) 0.5328(6) -0.0227(3) 0.048(2) Uani 1 1 d . . . . .
H13 H 0.1560 0.5867 -0.0542 0.058 Uiso 1 1 calc R U . . .
C14 C 0.0284(11) 0.4334(9) -0.1012(4) 0.129(6) Uani 1 1 d . . . . .
H14A H -0.0253 0.4904 -0.1058 0.154 Uiso 1 1 calc R U . . .
H14B H 0.0633 0.4446 -0.1345 0.154 Uiso 1 1 calc R U . . .
C15 C -0.0199(7) 0.3339(7) -0.1095(3) 0.059(2) Uani 1 1 d . . . . .
H15A H 0.0091 0.2897 -0.1377 0.071 Uiso 1 1 calc R U . . .
H15B H -0.0956 0.3438 -0.1304 0.071 Uiso 1 1 calc R U . . .
C16 C -0.0660(5) 0.1930(5) -0.0455(3) 0.0287(14) Uani 1 1 d . . . . .
H16 H -0.1192 0.1743 -0.0827 0.034 Uiso 1 1 calc R U . . .
C17 C -0.0578(4) 0.1279(5) 0.0112(3) 0.0232(13) Uani 1 1 d . . . . .
C18 C -0.1345(5) 0.0461(5) 0.0095(3) 0.0286(14) Uani 1 1 d . . . . .
H18 H -0.1898 0.0352 -0.0281 0.034 Uiso 1 1 calc R U . . .
C19 C -0.1294(5) -0.0173(5) 0.0617(3) 0.0304(15) Uani 1 1 d . . . . .
H19 H -0.1811 -0.0711 0.0595 0.036 Uiso 1 1 calc R U . . .
C20 C -0.0473(4) -0.0028(5) 0.1187(3) 0.0239(13) Uani 1 1 d . . . . .
H20 H -0.0444 -0.0458 0.1545 0.029 Uiso 1 1 calc R U . . .
C21 C 0.0302(4) 0.0771(5) 0.1211(2) 0.0195(12) Uani 1 1 d . . . . .
C22 C 0.0264(4) 0.1414(4) 0.0672(3) 0.0184(12) Uani 1 1 d . . . . .
C23 C 0.0945(5) 0.0733(5) 0.2357(3) 0.0275(14) Uani 1 1 d . . . . .
H23A H 0.0251 0.0993 0.2357 0.041 Uiso 1 1 calc R U . . .
H23B H 0.1480 0.1072 0.2704 0.041 Uiso 1 1 calc R U . . .
H23C H 0.0977 -0.0052 0.2411 0.041 Uiso 1 1 calc R U . . .
C24 C 0.4502(5) 0.4317(5) 0.2483(3) 0.0312(15) Uani 1 1 d . . . . .
H24A H 0.5142 0.4468 0.2366 0.047 Uiso 1 1 calc R U . . .
H24B H 0.4600 0.3664 0.2742 0.047 Uiso 1 1 calc R U . . .
H24C H 0.4346 0.4928 0.2722 0.047 Uiso 1 1 calc R U . . .
C25 C 0.328(2) 0.345(2) 0.3609(9) 0.134(10) Uani 0.651(13) 1 d . . P . .
Cr1 Cr 0.70279(7) 0.25569(7) 0.16654(4) 0.0171(2) Uani 1 1 d . . . . .
Gd1 Gd 0.26861(2) 0.22657(2) 0.15602(2) 0.01696(10) Uani 1 1 d . . . . .
N1 N 0.4669(4) 0.2135(4) 0.1797(2) 0.0260(11) Uani 1 1 d . . . . .
N2 N 0.6406(5) 0.5060(6) 0.1209(4) 0.072(2) Uani 1 1 d . . . . .
N3 N 0.7703(4) 0.3539(4) 0.3095(3) 0.0331(13) Uani 1 1 d . . . . .
N4 N 0.9410(4) 0.3085(4) 0.1631(2) 0.0309(12) Uani 1 1 d . . . . .
N5 N 0.7828(5) 0.0141(5) 0.2193(3) 0.0485(16) Uani 1 1 d . . . . .
N6 N 0.6026(4) 0.1453(5) 0.0267(3) 0.0370(14) Uani 1 1 d . . . . .
N7 N 0.1088(5) 0.4440(5) -0.0371(2) 0.0426(16) Uani 1 1 d . . . . .
N8 N -0.0058(4) 0.2742(4) -0.0485(2) 0.0261(12) Uani 1 1 d . . . . .
Ni1 Ni 0.10665(6) 0.32767(6) 0.01629(3) 0.02289(19) Uani 1 1 d . . . . .
O1 O 0.2226(3) 0.3753(3) 0.08238(18) 0.0284(10) Uani 1 1 d . . . . .
O2 O 0.1047(3) 0.2149(3) 0.07296(17) 0.0203(9) Uani 1 1 d . . . . .
O3 O 0.3622(3) 0.4156(3) 0.19066(18) 0.0232(9) Uani 1 1 d . . . . .
O4 O 0.1136(3) 0.1017(3) 0.17506(17) 0.0195(8) Uani 1 1 d . . . . .
O5 O 0.3304(3) 0.1872(3) 0.27007(18) 0.0276(9) Uani 1 1 d . . . . .
O6 O 0.3069(3) 0.0367(3) 0.14924(19) 0.0289(10) Uani 1 1 d . . . . .
O7 O 0.3169(3) 0.1871(4) 0.05405(19) 0.0372(11) Uani 1 1 d . . . . .
O8 O 0.1594(3) 0.3330(3) 0.20258(18) 0.0247(9) Uani 1 1 d . . . . .
O9 O 0.4488(4) -0.0080(4) 0.0797(2) 0.0427(12) Uani 1 1 d . . . . .
O10 O 0.6020(5) 0.6957(5) 0.0340(3) 0.0632(16) Uani 1 1 d . . . . .
O11 O 0.2560(7) 0.2926(7) 0.3543(4) 0.041(3) Uani 0.651(13) 1 d . . P . .


_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
C1 N1 1.158(7) . ?
C1 Cr1 2.062(6) . ?
C2 N2 1.159(8) . ?
C2 Cr1 2.069(7) . ?
C3 N3 1.162(7) . ?
C3 Cr1 2.044(6) . ?
C4 N4 1.155(7) . ?
C4 Cr1 2.050(6) . ?
C5 N5 1.148(8) . ?
C5 Cr1 2.063(7) . ?
C6 N6 1.159(7) . ?
C6 Cr1 2.080(6) . ?
C7 O3 1.379(7) . ?
C7 C8 1.381(8) . ?
C7 C12 1.395(8) . ?
C8 C9 1.403(9) . ?
C9 C10 1.359(9) . ?
C10 C11 1.398(8) . ?
C11 C12 1.407(8) . ?
C11 C13 1.443(9) . ?
C12 O1 1.333(7) . ?
C13 N7 1.294(8) . ?
C14 C15 1.350(11) . ?
C14 N7 1.487(9) . ?
C15 N8 1.474(8) . ?
C16 N8 1.274(7) . ?
C16 C17 1.443(8) . ?
C17 C22 1.393(7) . ?
C17 C18 1.404(8) . ?
C18 C19 1.356(9) . ?
C19 C20 1.395(8) . ?
C20 C21 1.392(8) . ?
C21 O4 1.383(6) . ?
C21 C22 1.398(8) . ?
C22 O2 1.336(6) . ?
C23 O4 1.451(6) . ?
C24 O3 1.447(6) . ?
C25 O11 1.11(3) . ?
Gd1 O8 2.360(4) . ?
Gd1 O1 2.371(4) . ?
Gd1 O6 2.373(4) . ?
Gd1 O2 2.373(4) . ?
Gd1 O5 2.422(4) . ?
Gd1 N1 2.497(5) . ?
Gd1 O7 2.520(4) . ?
Gd1 O3 2.606(4) . ?
Gd1 O4 2.657(4) . ?
Gd1 Ni1 3.3891(13) . ?
N7 Ni1 1.833(5) . ?
N8 Ni1 1.835(5) . ?
Ni1 O2 1.846(4) . ?
Ni1 O1 1.853(4) . ?

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 Cr1 177.8(5) . . ?
N2 C2 Cr1 175.8(7) . . ?
N3 C3 Cr1 176.7(6) . . ?
N4 C4 Cr1 174.1(5) . . ?
N5 C5 Cr1 179.3(5) . . ?
N6 C6 Cr1 172.4(5) . . ?
O3 C7 C8 125.0(5) . . ?
O3 C7 C12 114.3(5) . . ?
C8 C7 C12 120.7(6) . . ?
C7 C8 C9 119.5(6) . . ?
C10 C9 C8 120.5(6) . . ?
C9 C10 C11 121.0(6) . . ?
C10 C11 C12 119.1(5) . . ?
C10 C11 C13 119.1(6) . . ?
C12 C11 C13 121.8(6) . . ?
O1 C12 C7 117.2(5) . . ?
O1 C12 C11 123.4(5) . . ?
C7 C12 C11 119.3(5) . . ?
N7 C13 C11 124.8(6) . . ?
C15 C14 N7 112.2(7) . . ?
C14 C15 N8 112.8(6) . . ?
N8 C16 C17 125.1(5) . . ?
C22 C17 C18 119.0(5) . . ?
C22 C17 C16 121.7(5) . . ?
C18 C17 C16 119.3(5) . . ?
C19 C18 C17 121.2(5) . . ?
C18 C19 C20 120.6(5) . . ?
C21 C20 C19 119.1(5) . . ?
O4 C21 C20 124.7(5) . . ?
O4 C21 C22 114.7(5) . . ?
C20 C21 C22 120.6(5) . . ?
O2 C22 C17 123.4(5) . . ?
O2 C22 C21 117.0(5) . . ?
C17 C22 C21 119.6(5) . . ?
C3 Cr1 C4 89.0(2) . . ?
C3 Cr1 C1 88.3(2) . . ?
C4 Cr1 C1 177.3(2) . . ?
C3 Cr1 C5 90.3(2) . . ?
C4 Cr1 C5 88.3(2) . . ?
C1 Cr1 C5 91.8(2) . . ?
C3 Cr1 C2 87.9(3) . . ?
C4 Cr1 C2 89.3(2) . . ?
C1 Cr1 C2 90.5(2) . . ?
C5 Cr1 C2 177.0(2) . . ?
C3 Cr1 C6 174.4(2) . . ?
C4 Cr1 C6 96.5(2) . . ?
C1 Cr1 C6 86.2(2) . . ?
C5 Cr1 C6 88.6(2) . . ?
C2 Cr1 C6 93.4(3) . . ?
O8 Gd1 O1 78.82(14) . . ?
O8 Gd1 O6 136.34(14) . . ?
O1 Gd1 O6 135.60(14) . . ?
O8 Gd1 O2 80.43(13) . . ?
O1 Gd1 O2 62.31(13) . . ?
O6 Gd1 O2 93.17(13) . . ?
O8 Gd1 O5 74.51(13) . . ?
O1 Gd1 O5 141.72(14) . . ?
O6 Gd1 O5 81.85(14) . . ?
O2 Gd1 O5 136.64(13) . . ?
O8 Gd1 N1 131.84(14) . . ?
O1 Gd1 N1 103.44(15) . . ?
O6 Gd1 N1 74.10(15) . . ?
O2 Gd1 N1 143.88(15) . . ?
O5 Gd1 N1 75.99(15) . . ?
O8 Gd1 O7 144.89(14) . . ?
O1 Gd1 O7 68.30(15) . . ?
O6 Gd1 O7 69.48(15) . . ?
O2 Gd1 O7 73.77(13) . . ?
O5 Gd1 O7 140.22(14) . . ?
N1 Gd1 O7 70.11(15) . . ?
O8 Gd1 O3 71.68(13) . . ?
O1 Gd1 O3 62.03(12) . . ?
O6 Gd1 O3 141.57(12) . . ?
O2 Gd1 O3 121.13(12) . . ?
O5 Gd1 O3 83.59(13) . . ?
N1 Gd1 O3 67.92(14) . . ?
O7 Gd1 O3 101.85(14) . . ?
O8 Gd1 O4 70.27(13) . . ?
O1 Gd1 O4 118.93(12) . . ?
O6 Gd1 O4 68.87(13) . . ?
O2 Gd1 O4 61.52(12) . . ?
O5 Gd1 O4 76.79(13) . . ?
N1 Gd1 O4 136.43(14) . . ?
O7 Gd1 O4 115.15(13) . . ?
O3 Gd1 O4 140.57(12) . . ?
O8 Gd1 Ni1 83.55(10) . . ?
O1 Gd1 Ni1 31.70(9) . . ?
O6 Gd1 Ni1 112.61(10) . . ?
O2 Gd1 Ni1 31.54(9) . . ?
O5 Gd1 Ni1 157.69(10) . . ?
N1 Gd1 Ni1 123.32(11) . . ?
O7 Gd1 Ni1 62.05(10) . . ?
O3 Gd1 Ni1 93.39(8) . . ?
O4 Gd1 Ni1 92.27(8) . . ?
C1 N1 Gd1 160.6(4) . . ?
C13 N7 C14 119.9(6) . . ?
C13 N7 Ni1 126.9(4) . . ?
C14 N7 Ni1 113.0(5) . . ?
C16 N8 C15 120.6(5) . . ?
C16 N8 Ni1 127.0(4) . . ?
C15 N8 Ni1 112.3(4) . . ?
N7 Ni1 N8 86.6(2) . . ?
N7 Ni1 O2 177.5(2) . . ?
N8 Ni1 O2 95.01(19) . . ?
N7 Ni1 O1 95.3(2) . . ?
N8 Ni1 O1 177.4(2) . . ?
O2 Ni1 O1 83.13(16) . . ?
N7 Ni1 Gd1 136.59(17) . . ?
N8 Ni1 Gd1 135.53(15) . . ?
O2 Ni1 Gd1 42.24(11) . . ?
O1 Ni1 Gd1 42.26(12) . . ?
C12 O1 Ni1 126.2(4) . . ?
C12 O1 Gd1 127.7(3) . . ?
Ni1 O1 Gd1 106.05(17) . . ?
C22 O2 Ni1 126.2(3) . . ?
C22 O2 Gd1 127.6(3) . . ?
Ni1 O2 Gd1 106.22(16) . . ?
C7 O3 C24 116.4(4) . . ?
C7 O3 Gd1 118.5(3) . . ?
C24 O3 Gd1 123.9(3) . . ?
C21 O4 C23 114.7(4) . . ?
C21 O4 Gd1 116.2(3) . . ?
C23 O4 Gd1 128.0(3) . . ?

_refine_diff_density_max         0.911
_refine_diff_density_min         -1.182
_refine_diff_density_rms         0.148

_shelxl_version_number           2014/6

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_2
_database_code_depnum_ccdc_archive 'CCDC 1401614'
_audit_update_record             
;
2015-05-19 deposited with the CCDC.
2015-10-20 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        NiTbCr
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H18 Cr N8 Ni O8 Tb, 0.63(C H4 O), 2(O)'
_chemical_formula_sum            'C24.63 H20.52 Cr N8 Ni O10.63 Tb'
_chemical_formula_weight         868.28

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'
Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 '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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   13.051(3)
_cell_length_b                   12.150(2)
_cell_length_c                   21.711(4)
_cell_angle_alpha                90
_cell_angle_beta                 106.89(3)
_cell_angle_gamma                90
_cell_volume                     3294.0(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.751
_exptl_crystal_F_000             1705
_exptl_transmission_factor_min   0.529
_exptl_transmission_factor_max   0.540
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_absorpt_coefficient_mu    3.078
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   'Absorption correction given as multi-scan'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker Smart Aepex CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            15052
_diffrn_reflns_av_unetI/netI     0.0383
_diffrn_reflns_av_R_equivalents  0.0247
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         3.282
_diffrn_reflns_theta_max         26.020
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measured_fraction_theta_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_point_group_measured_fraction_full 0.988
_reflns_number_total             6281
_reflns_number_gt                5650
_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       'SMART (Bruker, 2000)'
_computing_cell_refinement       SMART
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics    'diamond 3.0'
_computing_publication_material  'diamond 3.0'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0379P)²+6.9299P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6281
_refine_ls_number_parameters     424
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0409
_refine_ls_R_factor_gt           0.0355
_refine_ls_wR_factor_ref         0.0840
_refine_ls_wR_factor_gt          0.0805
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_restrained_S_all      1.083
_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_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
C1 C 0.5519(3) 0.7714(3) 0.1758(2) 0.0165(9) Uani 1 1 d . . . . .
C2 C 0.6607(4) 0.5837(4) 0.1352(3) 0.0346(12) Uani 1 1 d . . . . .
C3 C 0.6450(4) 0.8111(4) 0.0760(2) 0.0243(10) Uani 1 1 d . . . . .
C4 C 0.7478(4) 0.6823(4) 0.2594(2) 0.0237(10) Uani 1 1 d . . . . .
C5 C 0.7537(4) 0.8986(4) 0.2021(2) 0.0268(11) Uani 1 1 d . . . . .
C6 C 0.8557(3) 0.7133(3) 0.1620(2) 0.0185(9) Uani 1 1 d . . . . .
C7 C 0.3422(3) 0.4980(4) 0.1464(2) 0.0220(10) Uani 1 1 d . . . . .
C8 C 0.3903(4) 0.3965(4) 0.1570(3) 0.0291(11) Uani 1 1 d . . . . .
H8 H 0.4392 0.3796 0.1965 0.035 Uiso 1 1 calc R U . . .
C9 C 0.3644(4) 0.3187(4) 0.1071(3) 0.0367(13) Uani 1 1 d . . . . .
H9 H 0.3972 0.2499 0.1135 0.044 Uiso 1 1 calc R U . . .
C10 C 0.2922(4) 0.3421(4) 0.0495(3) 0.0344(12) Uani 1 1 d . . . . .
H10 H 0.2765 0.2896 0.0169 0.041 Uiso 1 1 calc R U . . .
C11 C 0.2408(4) 0.4460(4) 0.0387(2) 0.0298(11) Uani 1 1 d . . . . .
C12 C 0.2667(4) 0.5244(4) 0.0881(2) 0.0230(10) Uani 1 1 d . . . . .
C13 C 0.1642(5) 0.4678(5) -0.0229(3) 0.0470(15) Uani 1 1 d . . . . .
H13 H 0.1546 0.4139 -0.0544 0.056 Uiso 1 1 calc R U . . .
C14 C 0.0271(8) 0.5657(7) -0.1005(4) 0.106(3) Uani 1 1 d . U . . .
H14A H 0.0607 0.5523 -0.1342 0.127 Uiso 1 1 calc R U . . .
H14B H -0.0273 0.5097 -0.1040 0.127 Uiso 1 1 calc R U . . .
C15 C -0.0209(5) 0.6666(6) -0.1099(3) 0.0556(18) Uani 1 1 d . . . . .
H15A H -0.0969 0.6576 -0.1309 0.067 Uiso 1 1 calc R U . . .
H15B H 0.0090 0.7099 -0.1381 0.067 Uiso 1 1 calc R U . . .
C16 C -0.0663(4) 0.8066(4) -0.0454(2) 0.0265(11) Uani 1 1 d . . . . .
H16 H -0.1206 0.8245 -0.0825 0.032 Uiso 1 1 calc R U . . .
C17 C -0.0572(3) 0.8720(4) 0.0111(2) 0.0216(10) Uani 1 1 d . . . . .
C18 C 0.0272(3) 0.8576(4) 0.0679(2) 0.0194(9) Uani 1 1 d . . . . .
C19 C 0.0307(3) 0.9225(3) 0.1216(2) 0.0176(9) Uani 1 1 d . . . . .
C20 C -0.0462(4) 1.0017(4) 0.1192(2) 0.0242(10) Uani 1 1 d . . . . .
H20 H -0.0429 1.0447 0.1552 0.029 Uiso 1 1 calc R U . . .
C21 C -0.1290(4) 1.0168(4) 0.0622(2) 0.0300(11) Uani 1 1 d . . . . .
H21 H -0.1807 1.0704 0.0604 0.036 Uiso 1 1 calc R U . . .
C22 C -0.1346(4) 0.9544(4) 0.0097(2) 0.0277(11) Uani 1 1 d . . . . .
H22 H -0.1902 0.9657 -0.0278 0.033 Uiso 1 1 calc R U . . .
C23 C 0.0959(4) 0.9252(4) 0.2363(2) 0.0255(10) Uani 1 1 d . . . . .
H23A H 0.1013 1.0035 0.2424 0.038 Uiso 1 1 calc R U . . .
H23B H 0.1485 0.8894 0.2708 0.038 Uiso 1 1 calc R U . . .
H23C H 0.0256 0.9012 0.2360 0.038 Uiso 1 1 calc R U . . .
C24 C 0.4502(4) 0.5661(4) 0.2482(2) 0.0296(11) Uani 1 1 d . . . . .
H24A H 0.4353 0.5034 0.2711 0.044 Uiso 1 1 calc R U . . .
H24B H 0.4591 0.6301 0.2751 0.044 Uiso 1 1 calc R U . . .
H24C H 0.5148 0.5532 0.2366 0.044 Uiso 1 1 calc R U . . .
C25 C 0.6483(10) 0.1327(13) 0.1411(9) 0.126(7) Uiso 0.630(10) 1 d D . P . .
H25A H 0.6692 0.0755 0.1728 0.189 Uiso 0.630(10) 1 calc R U P . .
H25B H 0.6253 0.1005 0.0989 0.189 Uiso 0.630(10) 1 calc R U P . .
H25C H 0.5905 0.1744 0.1486 0.189 Uiso 0.630(10) 1 calc R U P . .
Cr1 Cr 0.70311(5) 0.74337(5) 0.16701(3) 0.01541(15) Uani 1 1 d . . . . .
N1 N 0.4657(3) 0.7839(3) 0.17800(19) 0.0229(9) Uani 1 1 d . . . . .
N2 N 0.6416(4) 0.4933(5) 0.1205(4) 0.075(2) Uani 1 1 d . . . . .
N3 N 0.6041(4) 0.8546(4) 0.0274(2) 0.0381(11) Uani 1 1 d . . . . .
N4 N 0.7694(3) 0.6433(3) 0.3097(2) 0.0324(10) Uani 1 1 d . . . . .
N5 N 0.7831(4) 0.9847(4) 0.2210(3) 0.0470(13) Uani 1 1 d . . . . .
N6 N 0.9425(3) 0.6914(3) 0.1642(2) 0.0286(9) Uani 1 1 d . . . . .
N7 N -0.0054(3) 0.7257(3) -0.04857(19) 0.0267(9) Uani 1 1 d . . . . .
N8 N 0.1084(4) 0.5556(4) -0.0373(2) 0.0466(13) Uani 1 1 d . . . . .
Ni1 Ni 0.10672(5) 0.67220(5) 0.01630(3) 0.02209(14) Uani 1 1 d . . . . .
O1 O 0.2225(3) 0.6241(3) 0.08248(15) 0.0279(8) Uani 1 1 d . . . . .
O2 O 0.1051(2) 0.7841(2) 0.07346(14) 0.0192(7) Uani 1 1 d . . . . .
O3 O 0.1144(2) 0.8973(2) 0.17583(14) 0.0190(6) Uani 1 1 d . . . . .
O4 O 0.3624(2) 0.5833(3) 0.19075(15) 0.0224(7) Uani 1 1 d . . . . .
O5 O 0.3314(2) 0.8113(3) 0.26869(15) 0.0258(7) Uani 1 1 d . . . . .
O6 O 0.1604(2) 0.6671(2) 0.20141(15) 0.0217(7) Uani 1 1 d . . . . .
O7 O 0.3075(3) 0.9606(3) 0.14959(16) 0.0290(8) Uani 1 1 d . . . . .
O8 O 0.3161(3) 0.8119(3) 0.05321(16) 0.0379(9) Uani 1 1 d . . . . .
O9 O 0.4467(3) 0.0067(3) 0.07864(18) 0.0421(10) Uani 1 1 d . . . . .
O10 O 0.7404(5) 0.2063(5) 0.1457(3) 0.037(2) Uani 0.630(10) 1 d D . P . .
H10A H 0.7957 0.1699 0.1547 0.056 Uiso 0.630(10) 1 calc R U P . .
O11 O 0.6011(4) 0.3031(4) 0.0342(2) 0.0630(13) Uani 1 1 d . . . . .
Tb1 Tb 0.26887(2) 0.77220(2) 0.15541(2) 0.01575(8) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.150(6) . ?
C1 Cr1 2.066(4) . ?
C2 N2 1.151(7) . ?
C2 Cr1 2.079(5) . ?
C3 N3 1.163(6) . ?
C3 Cr1 2.070(5) . ?
C4 N4 1.149(6) . ?
C4 Cr1 2.057(5) . ?
C5 N5 1.148(6) . ?
C5 Cr1 2.069(5) . ?
C6 N6 1.152(6) . ?
C6 Cr1 2.058(4) . ?
C7 C8 1.373(6) . ?
C7 O4 1.386(5) . ?
C7 C12 1.397(6) . ?
C8 C9 1.404(7) . ?
C9 C10 1.359(8) . ?
C10 C11 1.416(7) . ?
C11 C12 1.401(7) . ?
C11 C13 1.442(7) . ?
C12 O1 1.331(5) . ?
C13 N8 1.278(7) . ?
C14 C15 1.365(10) . ?
C14 N8 1.475(8) . ?
C15 N7 1.474(6) . ?
C16 N7 1.279(6) . ?
C16 C17 1.437(6) . ?
C17 C18 1.405(6) . ?
C17 C22 1.416(6) . ?
C18 O2 1.333(5) . ?
C18 C19 1.397(6) . ?
C19 C20 1.381(6) . ?
C19 O3 1.388(5) . ?
C20 C21 1.398(7) . ?
C21 C22 1.353(7) . ?
C23 O3 1.443(5) . ?
C24 O4 1.443(5) . ?
C25 O10 1.478(5) . ?
N1 Tb1 2.475(4) . ?
N7 Ni1 1.830(4) . ?
N8 Ni1 1.838(4) . ?
Ni1 O2 1.845(3) . ?
Ni1 O1 1.851(3) . ?
Ni1 Tb1 3.3706(12) . ?
O1 Tb1 2.357(3) . ?
O2 Tb1 2.355(3) . ?
O3 Tb1 2.663(3) . ?
O4 Tb1 2.608(3) . ?
O5 Tb1 2.403(3) . ?
O6 Tb1 2.335(3) . ?
O7 Tb1 2.355(3) . ?
O8 Tb1 2.516(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 Cr1 176.6(4) . . ?
N2 C2 Cr1 176.2(6) . . ?
N3 C3 Cr1 172.6(4) . . ?
N4 C4 Cr1 176.3(4) . . ?
N5 C5 Cr1 178.8(4) . . ?
N6 C6 Cr1 174.0(4) . . ?
C8 C7 O4 124.8(4) . . ?
C8 C7 C12 121.7(4) . . ?
O4 C7 C12 113.5(4) . . ?
C7 C8 C9 118.7(5) . . ?
C10 C9 C8 121.1(5) . . ?
C9 C10 C11 120.5(5) . . ?
C12 C11 C10 118.8(5) . . ?
C12 C11 C13 122.2(4) . . ?
C10 C11 C13 119.0(5) . . ?
O1 C12 C7 117.7(4) . . ?
O1 C12 C11 123.1(4) . . ?
C7 C12 C11 119.2(4) . . ?
N8 C13 C11 125.0(5) . . ?
C15 C14 N8 112.8(6) . . ?
C14 C15 N7 111.5(6) . . ?
N7 C16 C17 124.9(4) . . ?
C18 C17 C22 118.6(4) . . ?
C18 C17 C16 122.0(4) . . ?
C22 C17 C16 119.4(4) . . ?
O2 C18 C19 117.6(4) . . ?
O2 C18 C17 123.1(4) . . ?
C19 C18 C17 119.3(4) . . ?
C20 C19 O3 124.7(4) . . ?
C20 C19 C18 121.0(4) . . ?
O3 C19 C18 114.3(4) . . ?
C19 C20 C21 119.4(4) . . ?
C22 C21 C20 120.7(4) . . ?
C21 C22 C17 121.0(4) . . ?
C4 Cr1 C6 89.03(18) . . ?
C4 Cr1 C1 88.68(17) . . ?
C6 Cr1 C1 177.70(18) . . ?
C4 Cr1 C5 90.0(2) . . ?
C6 Cr1 C5 88.32(17) . . ?
C1 Cr1 C5 91.56(17) . . ?
C4 Cr1 C3 174.37(17) . . ?
C6 Cr1 C3 96.42(18) . . ?
C1 Cr1 C3 85.87(17) . . ?
C5 Cr1 C3 88.7(2) . . ?
C4 Cr1 C2 87.7(2) . . ?
C6 Cr1 C2 89.14(18) . . ?
C1 Cr1 C2 90.89(18) . . ?
C5 Cr1 C2 176.6(2) . . ?
C3 Cr1 C2 93.8(2) . . ?
C1 N1 Tb1 162.9(3) . . ?
C16 N7 C15 119.9(4) . . ?
C16 N7 Ni1 127.0(3) . . ?
C15 N7 Ni1 113.0(3) . . ?
C13 N8 C14 120.2(5) . . ?
C13 N8 Ni1 126.7(4) . . ?
C14 N8 Ni1 112.8(4) . . ?
N7 Ni1 N8 86.57(19) . . ?
N7 Ni1 O2 95.34(15) . . ?
N8 Ni1 O2 177.04(18) . . ?
N7 Ni1 O1 177.58(16) . . ?
N8 Ni1 O1 95.22(17) . . ?
O2 Ni1 O1 82.93(13) . . ?
N7 Ni1 Tb1 135.64(13) . . ?
N8 Ni1 Tb1 136.51(15) . . ?
O2 Ni1 Tb1 42.15(9) . . ?
O1 Ni1 Tb1 42.28(10) . . ?
C12 O1 Ni1 126.4(3) . . ?
C12 O1 Tb1 127.8(3) . . ?
Ni1 O1 Tb1 105.81(13) . . ?
C18 O2 Ni1 126.2(3) . . ?
C18 O2 Tb1 127.7(3) . . ?
Ni1 O2 Tb1 106.13(13) . . ?
C19 O3 C23 115.0(3) . . ?
C19 O3 Tb1 115.6(2) . . ?
C23 O3 Tb1 128.4(3) . . ?
C7 O4 C24 115.8(3) . . ?
C7 O4 Tb1 118.4(3) . . ?
C24 O4 Tb1 124.6(3) . . ?
O6 Tb1 O2 80.02(11) . . ?
O6 Tb1 O7 136.06(11) . . ?
O2 Tb1 O7 93.52(11) . . ?
O6 Tb1 O1 78.50(11) . . ?
O2 Tb1 O1 62.59(10) . . ?
O7 Tb1 O1 136.33(12) . . ?
O6 Tb1 O5 74.81(11) . . ?
O2 Tb1 O5 136.47(11) . . ?
O7 Tb1 O5 81.29(11) . . ?
O1 Tb1 O5 141.53(11) . . ?
O6 Tb1 N1 132.06(11) . . ?
O2 Tb1 N1 143.90(12) . . ?
O7 Tb1 N1 74.26(12) . . ?
O1 Tb1 N1 103.07(12) . . ?
O5 Tb1 N1 76.21(12) . . ?
O6 Tb1 O8 144.72(12) . . ?
O2 Tb1 O8 73.93(11) . . ?
O7 Tb1 O8 69.82(12) . . ?
O1 Tb1 O8 68.59(12) . . ?
O5 Tb1 O8 140.11(11) . . ?
N1 Tb1 O8 69.98(12) . . ?
O6 Tb1 O4 71.53(10) . . ?
O2 Tb1 O4 121.39(10) . . ?
O7 Tb1 O4 141.42(10) . . ?
O1 Tb1 O4 62.14(10) . . ?
O5 Tb1 O4 83.22(11) . . ?
N1 Tb1 O4 67.80(11) . . ?
O8 Tb1 O4 102.39(11) . . ?
O6 Tb1 O3 70.04(10) . . ?
O2 Tb1 O3 61.71(9) . . ?
O7 Tb1 O3 68.79(10) . . ?
O1 Tb1 O3 119.27(10) . . ?
O5 Tb1 O3 76.41(10) . . ?
N1 Tb1 O3 136.57(11) . . ?
O8 Tb1 O3 115.38(11) . . ?
O4 Tb1 O3 139.98(9) . . ?
O6 Tb1 Ni1 83.42(8) . . ?
O2 Tb1 Ni1 31.72(7) . . ?
O7 Tb1 Ni1 113.00(8) . . ?
O1 Tb1 Ni1 31.90(7) . . ?
O5 Tb1 Ni1 157.88(8) . . ?
N1 Tb1 Ni1 122.92(9) . . ?
O8 Tb1 Ni1 61.96(9) . . ?
O4 Tb1 Ni1 93.71(7) . . ?
O3 Tb1 Ni1 92.67(7) . . ?

_refine_diff_density_max         1.033
_refine_diff_density_min         -0.795
_refine_diff_density_rms         0.121

_shelxl_version_number           2014/6

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_4
_database_code_depnum_ccdc_archive 'CCDC 1420594'
_audit_update_record             
;
2015-08-26 deposited with the CCDC.
2015-10-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C25 H18 Fe N8 Ni O11 Tb'
_chemical_formula_weight         879.95

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'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 '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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

_cell_length_a                   12.861(3)
_cell_length_b                   12.014(2)
_cell_length_c                   21.577(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 106.73(3)
_cell_angle_gamma                90.00
_cell_volume                     3193.0(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.19
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.831
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1724
_exptl_absorpt_coefficient_mu    3.291
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.485
_exptl_absorpt_correction_T_max  0.540
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173(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  'Bruker Smart Aepex CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            14367
_diffrn_reflns_av_R_equivalents  0.0266
_diffrn_reflns_av_sigmaI/netI    0.0368
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         3.37
_diffrn_reflns_theta_max         26.03
_reflns_number_total             6060
_reflns_number_gt                5526
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 2000)'
_computing_cell_refinement       SMART
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'diamond 3.0'
_computing_publication_material  'diamond 3.0'

_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)+(0.0412P)²+5.3582P] 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         6060
_refine_ls_number_parameters     426
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0364
_refine_ls_R_factor_gt           0.0323
_refine_ls_wR_factor_ref         0.0822
_refine_ls_wR_factor_gt          0.0786
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_restrained_S_all      1.053
_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
C1 C 1.0578(3) 0.7692(3) 0.17569(18) 0.0143(8) Uani 1 1 d . . .
C2 C 1.1603(3) 0.5934(4) 0.1359(2) 0.0282(10) Uani 1 1 d . . .
C3 C 1.2441(3) 0.6830(4) 0.2543(2) 0.0198(9) Uani 1 1 d . . .
C4 C 1.3489(3) 0.7149(3) 0.16467(19) 0.0165(8) Uani 1 1 d . . .
C5 C 1.2503(3) 0.8907(4) 0.2015(2) 0.0217(9) Uani 1 1 d . . .
C6 C 1.1481(3) 0.8103(4) 0.0831(2) 0.0215(9) Uani 1 1 d . . .
C7 C 0.5269(3) 0.9226(4) 0.12137(19) 0.0164(8) Uani 1 1 d . . .
C8 C 0.4494(3) 1.0029(4) 0.1193(2) 0.0212(9) Uani 1 1 d . . .
H8 H 0.4523 1.0460 0.1556 0.025 Uiso 1 1 calc R . .
C9 C 0.3660(4) 1.0187(4) 0.0615(2) 0.0269(10) Uani 1 1 d . . .
H9 H 0.3132 1.0724 0.0597 0.032 Uiso 1 1 calc R . .
C10 C 0.3616(3) 0.9568(4) 0.0087(2) 0.0240(10) Uani 1 1 d . . .
H10 H 0.3064 0.9693 -0.0293 0.029 Uiso 1 1 calc R . .
C11 C 0.4401(3) 0.8728(4) 0.01024(19) 0.0190(9) Uani 1 1 d . . .
C12 C 0.5249(3) 0.8581(4) 0.06699(19) 0.0164(8) Uani 1 1 d . . .
C13 C 0.4338(3) 0.8091(4) -0.0474(2) 0.0221(9) Uani 1 1 d . . .
H13 H 0.3809 0.8296 -0.0851 0.027 Uiso 1 1 calc R . .
C14 C 0.4850(5) 0.6720(5) -0.1137(2) 0.0410(14) Uani 1 1 d . . .
H14A H 0.4108 0.6763 -0.1413 0.049 Uiso 1 1 calc R . .
H14B H 0.5318 0.7084 -0.1356 0.049 Uiso 1 1 calc R . .
C15 C 0.5171(5) 0.5557(5) -0.1007(2) 0.0504(16) Uani 1 1 d . . .
H15A H 0.5432 0.5262 -0.1353 0.061 Uiso 1 1 calc R . .
H15B H 0.4554 0.5116 -0.0981 0.061 Uiso 1 1 calc R . .
C16 C 0.6621(4) 0.4615(4) -0.0231(2) 0.0311(11) Uani 1 1 d . . .
H16 H 0.6515 0.4065 -0.0546 0.037 Uiso 1 1 calc R . .
C17 C 0.7413(3) 0.4396(4) 0.0385(2) 0.0226(9) Uani 1 1 d . . .
C18 C 0.7935(4) 0.3350(4) 0.0493(2) 0.0281(10) Uani 1 1 d . . .
H18 H 0.7777 0.2818 0.0165 0.034 Uiso 1 1 calc R . .
C19 C 0.8668(4) 0.3114(4) 0.1072(2) 0.0302(11) Uani 1 1 d . . .
H19 H 0.9001 0.2419 0.1140 0.036 Uiso 1 1 calc R . .
C20 C 0.8924(3) 0.3906(4) 0.1564(2) 0.0251(10) Uani 1 1 d . . .
H20 H 0.9428 0.3740 0.1958 0.030 Uiso 1 1 calc R . .
C21 C 0.8433(3) 0.4934(4) 0.1469(2) 0.0179(9) Uani 1 1 d . . .
C22 C 0.7658(3) 0.5191(4) 0.08776(19) 0.0175(8) Uani 1 1 d . . .
C23 C 0.9526(3) 0.5631(4) 0.2492(2) 0.0246(10) Uani 1 1 d . . .
H23A H 0.9378 0.4994 0.2721 0.037 Uiso 1 1 calc R . .
H23B H 0.9605 0.6278 0.2763 0.037 Uiso 1 1 calc R . .
H23C H 1.0185 0.5510 0.2377 0.037 Uiso 1 1 calc R . .
C24 C 0.5921(3) 0.9251(4) 0.23678(19) 0.0223(9) Uani 1 1 d . . .
H24A H 0.5985 1.0042 0.2431 0.033 Uiso 1 1 calc R . .
H24B H 0.6447 0.8883 0.2715 0.033 Uiso 1 1 calc R . .
H24C H 0.5205 0.9017 0.2362 0.033 Uiso 1 1 calc R . .
C25 C 0.8457(17) 0.647(2) 0.3635(10) 0.233(9) Uani 1 1 d U . .
Fe1 Fe 1.20191(4) 0.74358(5) 0.16822(3) 0.01265(13) Uani 1 1 d . . .
N1 N 0.9702(3) 0.7827(3) 0.17849(17) 0.0191(8) Uani 1 1 d . . .
N2 N 1.1410(4) 0.5019(4) 0.1196(3) 0.0583(15) Uani 1 1 d . . .
N3 N 1.2675(3) 0.6435(3) 0.30530(18) 0.0278(9) Uani 1 1 d . . .
N4 N 1.4364(3) 0.6940(3) 0.16643(18) 0.0238(8) Uani 1 1 d . . .
N5 N 1.2809(3) 0.9772(4) 0.2208(2) 0.0367(10) Uani 1 1 d . . .
N6 N 1.1085(3) 0.8540(4) 0.03438(18) 0.0324(10) Uani 1 1 d . . .
N7 N 0.4943(3) 0.7276(3) -0.05103(17) 0.0225(8) Uani 1 1 d . . .
N8 N 0.6052(3) 0.5504(4) -0.03788(16) 0.0294(9) Uani 1 1 d . . .
Ni1 Ni 0.60552(4) 0.67005(5) 0.01543(2) 0.01744(13) Uani 1 1 d . . .
O1 O 0.7205(2) 0.6195(3) 0.08259(13) 0.0227(7) Uani 1 1 d . . .
O2 O 0.6042(2) 0.7839(2) 0.07281(13) 0.0167(6) Uani 1 1 d . . .
O3 O 0.8634(2) 0.5800(3) 0.19093(13) 0.0181(6) Uani 1 1 d . . .
O4 O 0.6113(2) 0.8966(2) 0.17590(12) 0.0167(6) Uani 1 1 d . . .
O5 O 0.8075(2) 0.9624(3) 0.14809(14) 0.0229(7) Uani 1 1 d . . .
O6 O 0.8320(2) 0.8143(3) 0.27066(13) 0.0232(7) Uani 1 1 d . . .
O7 O 0.6579(2) 0.6647(3) 0.20411(13) 0.0196(6) Uani 1 1 d . . .
O8 O 0.8186(2) 0.8080(3) 0.05265(14) 0.0303(8) Uani 1 1 d . . .
O9 O 0.9459(3) 0.0094(3) 0.07474(16) 0.0357(8) Uani 1 1 d . . .
O10 O 0.0957(3) 0.3098(4) 0.0336(2) 0.0527(11) Uani 1 1 d . . .
O11 O 0.7663(5) 0.7008(5) 0.3569(2) 0.0782(16) Uani 1 1 d . . .
Tb1 Tb 0.769873(14) 0.770869(17) 0.156207(9) 0.01422(7) 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
C1 N1 1.156(5) . ?
C1 Fe1 1.931(4) . ?
C2 N2 1.159(7) . ?
C2 Fe1 1.953(5) . ?
C3 N3 1.156(5) . ?
C3 Fe1 1.922(4) . ?
C4 N4 1.143(5) . ?
C4 Fe1 1.945(4) . ?
C5 N5 1.146(6) . ?
C5 Fe1 1.942(5) . ?
C6 N6 1.154(6) . ?
C6 Fe1 1.940(4) . ?
C7 C8 1.379(6) . ?
C7 O4 1.388(5) . ?
C7 C12 1.400(6) . ?
C8 C9 1.404(6) . ?
C9 C10 1.349(6) . ?
C10 C11 1.421(6) . ?
C11 C12 1.397(5) . ?
C11 C13 1.442(6) . ?
C12 O2 1.333(5) . ?
C13 N7 1.267(6) . ?
C14 C15 1.461(8) . ?
C14 N7 1.482(6) . ?
C15 N8 1.497(6) . ?
C16 N8 1.282(6) . ?
C16 C17 1.447(6) . ?
C17 C22 1.396(6) . ?
C17 C18 1.412(6) . ?
C18 C19 1.362(7) . ?
C19 C20 1.394(7) . ?
C20 C21 1.375(6) . ?
C21 O3 1.383(5) . ?
C21 C22 1.409(6) . ?
C22 O1 1.330(5) . ?
C23 O3 1.451(5) . ?
C24 O4 1.446(5) . ?
C25 O11 1.18(2) . ?
N1 Tb1 2.486(3) . ?
N7 Ni1 1.844(4) . ?
N8 Ni1 1.840(4) . ?
Ni1 O2 1.848(3) . ?
Ni1 O1 1.850(3) . ?
Ni1 Tb1 3.3861(12) . ?
O1 Tb1 2.378(3) . ?
O2 Tb1 2.366(3) . ?
O3 Tb1 2.598(3) . ?
O4 Tb1 2.668(3) . ?
O5 Tb1 2.369(3) . ?
O6 Tb1 2.423(3) . ?
O7 Tb1 2.372(3) . ?
O8 Tb1 2.528(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 Fe1 177.9(4) . . ?
N2 C2 Fe1 175.9(5) . . ?
N3 C3 Fe1 177.7(4) . . ?
N4 C4 Fe1 175.3(4) . . ?
N5 C5 Fe1 178.5(4) . . ?
N6 C6 Fe1 173.7(4) . . ?
C8 C7 O4 124.5(4) . . ?
C8 C7 C12 121.5(4) . . ?
O4 C7 C12 114.0(3) . . ?
C7 C8 C9 118.9(4) . . ?
C10 C9 C8 120.8(4) . . ?
C9 C10 C11 121.0(4) . . ?
C12 C11 C10 118.7(4) . . ?
C12 C11 C13 121.7(4) . . ?
C10 C11 C13 119.5(4) . . ?
O2 C12 C11 123.3(4) . . ?
O2 C12 C7 117.5(3) . . ?
C11 C12 C7 119.1(4) . . ?
N7 C13 C11 125.4(4) . . ?
C15 C14 N7 108.1(4) . . ?
C14 C15 N8 108.3(4) . . ?
N8 C16 C17 125.6(4) . . ?
C22 C17 C18 119.5(4) . . ?
C22 C17 C16 121.3(4) . . ?
C18 C17 C16 119.2(4) . . ?
C19 C18 C17 120.4(4) . . ?
C18 C19 C20 120.5(4) . . ?
C21 C20 C19 120.1(4) . . ?
C20 C21 O3 125.9(4) . . ?
C20 C21 C22 120.5(4) . . ?
O3 C21 C22 113.6(4) . . ?
O1 C22 C17 124.0(4) . . ?
O1 C22 C21 117.0(4) . . ?
C17 C22 C21 119.0(4) . . ?
C3 Fe1 C1 89.46(17) . . ?
C3 Fe1 C6 174.92(17) . . ?
C1 Fe1 C6 85.65(17) . . ?
C3 Fe1 C5 90.92(19) . . ?
C1 Fe1 C5 92.12(16) . . ?
C6 Fe1 C5 87.88(19) . . ?
C3 Fe1 C4 87.91(17) . . ?
C1 Fe1 C4 177.37(17) . . ?
C6 Fe1 C4 96.98(17) . . ?
C5 Fe1 C4 87.95(17) . . ?
C3 Fe1 C2 88.1(2) . . ?
C1 Fe1 C2 90.36(17) . . ?
C6 Fe1 C2 93.3(2) . . ?
C5 Fe1 C2 177.34(18) . . ?
C4 Fe1 C2 89.53(18) . . ?
C1 N1 Tb1 162.3(3) . . ?
C13 N7 C14 121.0(4) . . ?
C13 N7 Ni1 126.5(3) . . ?
C14 N7 Ni1 112.5(3) . . ?
C16 N8 C15 119.4(4) . . ?
C16 N8 Ni1 126.6(3) . . ?
C15 N8 Ni1 113.5(3) . . ?
N8 Ni1 N7 86.84(16) . . ?
N8 Ni1 O2 176.32(16) . . ?
N7 Ni1 O2 95.09(15) . . ?
N8 Ni1 O1 95.22(15) . . ?
N7 Ni1 O1 177.02(16) . . ?
O2 Ni1 O1 82.97(12) . . ?
N8 Ni1 Tb1 136.78(12) . . ?
N7 Ni1 Tb1 135.05(12) . . ?
O2 Ni1 Tb1 42.11(8) . . ?
O1 Ni1 Tb1 42.51(9) . . ?
C22 O1 Ni1 126.5(3) . . ?
C22 O1 Tb1 127.7(2) . . ?
Ni1 O1 Tb1 105.77(13) . . ?
C12 O2 Ni1 125.9(2) . . ?
C12 O2 Tb1 127.8(2) . . ?
Ni1 O2 Tb1 106.29(12) . . ?
C21 O3 C23 115.8(3) . . ?
C21 O3 Tb1 119.1(2) . . ?
C23 O3 Tb1 123.9(3) . . ?
C7 O4 C24 114.9(3) . . ?
C7 O4 Tb1 116.1(2) . . ?
C24 O4 Tb1 128.1(2) . . ?
O2 Tb1 O5 92.18(10) . . ?
O2 Tb1 O7 80.79(10) . . ?
O5 Tb1 O7 135.83(10) . . ?
O2 Tb1 O1 62.19(10) . . ?
O5 Tb1 O1 135.62(10) . . ?
O7 Tb1 O1 78.52(10) . . ?
O2 Tb1 O6 136.19(10) . . ?
O5 Tb1 O6 81.48(10) . . ?
O7 Tb1 O6 74.64(10) . . ?
O1 Tb1 O6 142.34(11) . . ?
O2 Tb1 N1 143.14(10) . . ?
O5 Tb1 N1 74.70(11) . . ?
O7 Tb1 N1 132.24(11) . . ?
O1 Tb1 N1 103.63(11) . . ?
O6 Tb1 N1 76.76(11) . . ?
O2 Tb1 O8 73.39(10) . . ?
O5 Tb1 O8 69.83(11) . . ?
O7 Tb1 O8 144.70(11) . . ?
O1 Tb1 O8 68.35(11) . . ?
O6 Tb1 O8 140.33(10) . . ?
N1 Tb1 O8 69.76(11) . . ?
O2 Tb1 O3 121.25(9) . . ?
O5 Tb1 O3 142.32(9) . . ?
O7 Tb1 O3 71.86(9) . . ?
O1 Tb1 O3 61.97(9) . . ?
O6 Tb1 O3 84.63(10) . . ?
N1 Tb1 O3 68.06(10) . . ?
O8 Tb1 O3 101.47(10) . . ?
O2 Tb1 O4 61.40(9) . . ?
O5 Tb1 O4 69.12(9) . . ?
O7 Tb1 O4 69.34(10) . . ?
O1 Tb1 O4 118.03(9) . . ?
O6 Tb1 O4 76.05(9) . . ?
N1 Tb1 O4 137.23(10) . . ?
O8 Tb1 O4 115.85(10) . . ?
O3 Tb1 O4 139.96(8) . . ?
O2 Tb1 Ni1 31.59(7) . . ?
O5 Tb1 Ni1 111.68(7) . . ?
O7 Tb1 Ni1 84.14(7) . . ?
O1 Tb1 Ni1 31.72(7) . . ?
O6 Tb1 Ni1 158.23(7) . . ?
N1 Tb1 Ni1 122.60(8) . . ?
O8 Tb1 Ni1 61.30(7) . . ?
O3 Tb1 Ni1 93.48(6) . . ?
O4 Tb1 Ni1 92.12(6) . . ?

_diffrn_measured_fraction_theta_max 0.964
_diffrn_reflns_theta_full        26.03
_diffrn_measured_fraction_theta_full 0.964
_refine_diff_density_max         1.173
_refine_diff_density_min         -0.944
_refine_diff_density_rms         0.118
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_3
_database_code_depnum_ccdc_archive 'CCDC 1420595'
_audit_update_record             
;
2015-08-26 deposited with the CCDC.
2015-10-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H18 Fe Gd N8 Ni O11'
_chemical_formula_weight         866.27

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'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   12.862(3)
_cell_length_b                   12.012(2)
_cell_length_c                   21.580(4)
_cell_angle_alpha                90
_cell_angle_beta                 106.72(3)
_cell_angle_gamma                90
_cell_volume                     3193.1(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.802
_exptl_crystal_F_000             1696
_exptl_transmission_factor_min   0.520
_exptl_transmission_factor_max   0.590
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.17
_exptl_absorpt_coefficient_mu    3.152
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker Smart Aepex CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            14590
_diffrn_reflns_av_unetI/netI     0.0370
_diffrn_reflns_av_R_equivalents  0.0255
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         3.308
_diffrn_reflns_theta_max         26.026
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measured_fraction_theta_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_point_group_measured_fraction_full 0.992
_reflns_number_total             6111
_reflns_number_gt                5424
_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       'SMART (Bruker, 2000)'
_computing_cell_refinement       SMART
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics    'diamond 3.0'
_computing_publication_material  'diamond 3.0'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0411P)²+4.9708P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6111
_refine_ls_number_parameters     417
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0397
_refine_ls_R_factor_gt           0.0338
_refine_ls_wR_factor_ref         0.0823
_refine_ls_wR_factor_gt          0.0787
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_restrained_S_all      1.058
_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_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
C1 C 1.0582(3) 0.2306(3) 0.17591(19) 0.0149(8) Uani 1 1 d . . . . .
C2 C 1.2509(4) 0.1103(4) 0.2018(2) 0.0231(9) Uani 1 1 d . . . . .
C3 C 1.3487(3) 0.2849(3) 0.16499(19) 0.0165(8) Uani 1 1 d . . . . .
C4 C 1.1612(4) 0.4066(4) 0.1360(2) 0.0306(11) Uani 1 1 d . . . . .
C5 C 1.1487(4) 0.1901(4) 0.0835(2) 0.0228(9) Uani 1 1 d . . . . .
C6 C 1.2441(3) 0.3170(4) 0.2546(2) 0.0216(9) Uani 1 1 d . . . . .
C7 C 0.8436(4) 0.5065(4) 0.1466(2) 0.0222(9) Uani 1 1 d . . . . .
C8 C 0.8931(4) 0.6096(4) 0.1566(2) 0.0269(10) Uani 1 1 d . . . . .
H8 H 0.9435 0.6263 0.1960 0.032 Uiso 1 1 calc R U . . .
C9 C 0.8668(4) 0.6883(4) 0.1071(2) 0.0315(11) Uani 1 1 d . . . . .
H9 H 0.8997 0.7579 0.1137 0.038 Uiso 1 1 calc R U . . .
C10 C 0.7931(4) 0.6644(4) 0.0490(2) 0.0284(11) Uani 1 1 d . . . . .
H10 H 0.7778 0.7175 0.0163 0.034 Uiso 1 1 calc R U . . .
C11 C 0.7403(4) 0.5610(4) 0.0381(2) 0.0244(10) Uani 1 1 d . . . . .
C12 C 0.7663(3) 0.4807(3) 0.0877(2) 0.0195(9) Uani 1 1 d . . . . .
C13 C 0.6623(4) 0.5393(4) -0.0233(2) 0.0346(12) Uani 1 1 d . . . . .
H13 H 0.6526 0.5939 -0.0551 0.041 Uiso 1 1 calc R U . . .
C14 C 0.5180(6) 0.4440(5) -0.1007(2) 0.0559(18) Uani 1 1 d . . . . .
H14A H 0.4562 0.4887 -0.0988 0.067 Uiso 1 1 calc R U . . .
H14B H 0.5450 0.4726 -0.1352 0.067 Uiso 1 1 calc R U . . .
C15 C 0.4857(5) 0.3281(5) -0.1132(2) 0.0441(14) Uani 1 1 d . . . . .
H15A H 0.5323 0.2913 -0.1350 0.053 Uiso 1 1 calc R U . . .
H15B H 0.4114 0.3238 -0.1407 0.053 Uiso 1 1 calc R U . . .
C16 C 0.4328(4) 0.1909(4) -0.0476(2) 0.0241(10) Uani 1 1 d . . . . .
H16 H 0.3791 0.1715 -0.0851 0.029 Uiso 1 1 calc R U . . .
C17 C 0.4403(3) 0.1266(3) 0.00997(19) 0.0191(9) Uani 1 1 d . . . . .
C18 C 0.3618(4) 0.0440(4) 0.0086(2) 0.0256(10) Uani 1 1 d . . . . .
H18 H 0.3059 0.0325 -0.0292 0.031 Uiso 1 1 calc R U . . .
C19 C 0.3663(4) -0.0191(4) 0.0616(2) 0.0291(11) Uani 1 1 d . . . . .
H19 H 0.3141 -0.0737 0.0596 0.035 Uiso 1 1 calc R U . . .
C20 C 0.4491(4) -0.0023(4) 0.1193(2) 0.0241(10) Uani 1 1 d . . . . .
H20 H 0.4514 -0.0444 0.1558 0.029 Uiso 1 1 calc R U . . .
C21 C 0.5276(3) 0.0776(3) 0.1213(2) 0.0181(9) Uani 1 1 d . . . . .
C22 C 0.5247(3) 0.1420(3) 0.0671(2) 0.0177(9) Uani 1 1 d . . . . .
C23 C 0.5924(4) 0.0753(4) 0.2371(2) 0.0249(10) Uani 1 1 d . . . . .
H23A H 0.5208 0.0989 0.2364 0.037 Uiso 1 1 calc R U . . .
H23B H 0.6450 0.1121 0.2717 0.037 Uiso 1 1 calc R U . . .
H23C H 0.5985 -0.0038 0.2435 0.037 Uiso 1 1 calc R U . . .
C24 C 0.9530(4) 0.4364(4) 0.2490(2) 0.0262(10) Uani 1 1 d . . . . .
H24A H 1.0191 0.4461 0.2374 0.039 Uiso 1 1 calc R U . . .
H24B H 0.9594 0.3726 0.2766 0.039 Uiso 1 1 calc R U . . .
H24C H 0.9396 0.5015 0.2714 0.039 Uiso 1 1 calc R U . . .
Fe1 Fe 1.20210(5) 0.25664(5) 0.16832(3) 0.01428(13) Uani 1 1 d . . . . .
Gd1 Gd 0.76996(2) 0.22922(2) 0.15614(2) 0.01436(7) Uani 1 1 d . . . . .
N1 N 0.9706(3) 0.2172(3) 0.17882(17) 0.0194(8) Uani 1 1 d . . . . .
N2 N 1.2812(4) 0.0235(3) 0.2212(2) 0.0409(11) Uani 1 1 d . . . . .
N3 N 1.4365(3) 0.3058(3) 0.16672(18) 0.0260(8) Uani 1 1 d . . . . .
N4 N 1.1405(4) 0.4976(4) 0.1197(3) 0.0614(15) Uani 1 1 d . . . . .
N5 N 1.1088(4) 0.1453(4) 0.03437(19) 0.0351(10) Uani 1 1 d . . . . .
N6 N 1.2677(3) 0.3569(3) 0.30557(18) 0.0293(9) Uani 1 1 d . . . . .
N7 N 0.6044(4) 0.4498(3) -0.03800(17) 0.0329(10) Uani 1 1 d . . . . .
N8 N 0.4948(3) 0.2732(3) -0.05077(17) 0.0246(8) Uani 1 1 d . . . . .
Ni1 Ni 0.60556(5) 0.33001(4) 0.01538(2) 0.01934(13) Uani 1 1 d . . . . .
O1 O 0.6043(2) 0.2162(2) 0.07286(13) 0.0180(6) Uani 1 1 d . . . . .
O2 O 0.7201(3) 0.3804(2) 0.08240(14) 0.0247(7) Uani 1 1 d . . . . .
O3 O 0.6119(2) 0.1035(2) 0.17594(12) 0.0176(6) Uani 1 1 d . . . . .
O4 O 0.8637(2) 0.4200(2) 0.19098(13) 0.0207(6) Uani 1 1 d . . . . .
O5 O 0.8187(3) 0.1923(3) 0.05293(14) 0.0332(8) Uani 1 1 d . . . . .
O6 O 0.6576(2) 0.3350(2) 0.20396(14) 0.0212(6) Uani 1 1 d . . . . .
O7 O 0.8077(2) 0.0371(2) 0.14819(14) 0.0253(7) Uani 1 1 d . . . . .
O8 O 0.8324(2) 0.1862(3) 0.27067(14) 0.0255(7) Uani 1 1 d . . . . .
O9 O 0.9464(3) 0.9907(3) 0.07486(16) 0.0393(9) Uani 1 1 d . . . . .
O10 O 0.7757(6) 0.3059(5) 0.3577(2) 0.109(2) Uani 1 1 d . . . . .
O11 O 0.0956(4) 0.6901(4) 0.0336(2) 0.0576(11) 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
C1 N1 1.157(5) . ?
C1 Fe1 1.930(4) . ?
C2 N2 1.148(6) . ?
C2 Fe1 1.936(4) . ?
C3 N3 1.147(5) . ?
C3 Fe1 1.937(4) . ?
C4 N4 1.156(6) . ?
C4 Fe1 1.949(5) . ?
C5 N5 1.167(6) . ?
C5 Fe1 1.934(4) . ?
C6 N6 1.158(5) . ?
C6 Fe1 1.924(5) . ?
C7 C8 1.380(6) . ?
C7 O4 1.386(5) . ?
C7 C12 1.405(6) . ?
C8 C9 1.393(7) . ?
C9 C10 1.367(7) . ?
C10 C11 1.403(6) . ?
C11 C12 1.407(6) . ?
C11 C13 1.437(6) . ?
C12 O2 1.335(5) . ?
C13 N7 1.293(6) . ?
C14 C15 1.456(8) . ?
C14 N7 1.485(6) . ?
C15 N8 1.473(6) . ?
C16 N8 1.285(6) . ?
C16 C17 1.443(6) . ?
C17 C22 1.401(6) . ?
C17 C18 1.409(6) . ?
C18 C19 1.360(6) . ?
C19 C20 1.400(6) . ?
C20 C21 1.385(6) . ?
C21 O3 1.388(5) . ?
C21 C22 1.394(6) . ?
C22 O1 1.335(5) . ?
C23 O3 1.452(5) . ?
C24 O4 1.448(5) . ?
Gd1 O1 2.364(3) . ?
Gd1 O6 2.371(3) . ?
Gd1 O7 2.375(3) . ?
Gd1 O2 2.378(3) . ?
Gd1 O8 2.425(3) . ?
Gd1 N1 2.489(4) . ?
Gd1 O5 2.521(3) . ?
Gd1 O4 2.598(3) . ?
Gd1 O3 2.664(3) . ?
Gd1 Ni1 3.3864(12) . ?
N7 Ni1 1.841(4) . ?
N8 Ni1 1.833(4) . ?
Ni1 O2 1.844(3) . ?
Ni1 O1 1.850(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 Fe1 177.9(4) . . ?
N2 C2 Fe1 178.9(4) . . ?
N3 C3 Fe1 175.4(4) . . ?
N4 C4 Fe1 176.5(5) . . ?
N5 C5 Fe1 173.5(4) . . ?
N6 C6 Fe1 177.5(4) . . ?
C8 C7 O4 125.4(4) . . ?
C8 C7 C12 120.9(4) . . ?
O4 C7 C12 113.7(4) . . ?
C7 C8 C9 119.3(4) . . ?
C10 C9 C8 120.8(4) . . ?
C9 C10 C11 120.9(4) . . ?
C10 C11 C12 118.7(4) . . ?
C10 C11 C13 119.4(4) . . ?
C12 C11 C13 121.8(4) . . ?
O2 C12 C7 117.3(4) . . ?
O2 C12 C11 123.5(4) . . ?
C7 C12 C11 119.3(4) . . ?
N7 C13 C11 125.2(4) . . ?
C15 C14 N7 108.2(4) . . ?
C14 C15 N8 108.4(4) . . ?
N8 C16 C17 124.7(4) . . ?
C22 C17 C18 118.7(4) . . ?
C22 C17 C16 122.0(4) . . ?
C18 C17 C16 119.3(4) . . ?
C19 C18 C17 121.2(4) . . ?
C18 C19 C20 120.3(4) . . ?
C21 C20 C19 119.3(4) . . ?
C20 C21 O3 124.5(4) . . ?
C20 C21 C22 121.0(4) . . ?
O3 C21 C22 114.5(3) . . ?
O1 C22 C21 117.2(4) . . ?
O1 C22 C17 123.3(4) . . ?
C21 C22 C17 119.4(4) . . ?
C6 Fe1 C1 89.29(17) . . ?
C6 Fe1 C5 174.79(18) . . ?
C1 Fe1 C5 85.72(18) . . ?
C6 Fe1 C2 90.58(19) . . ?
C1 Fe1 C2 92.12(17) . . ?
C5 Fe1 C2 88.10(19) . . ?
C6 Fe1 C3 87.99(18) . . ?
C1 Fe1 C3 177.27(17) . . ?
C5 Fe1 C3 96.98(18) . . ?
C2 Fe1 C3 87.62(17) . . ?
C6 Fe1 C4 88.3(2) . . ?
C1 Fe1 C4 90.77(18) . . ?
C5 Fe1 C4 93.3(2) . . ?
C2 Fe1 C4 176.87(19) . . ?
C3 Fe1 C4 89.43(18) . . ?
O1 Gd1 O6 80.66(10) . . ?
O1 Gd1 O7 92.22(10) . . ?
O6 Gd1 O7 135.62(10) . . ?
O1 Gd1 O2 62.05(10) . . ?
O6 Gd1 O2 78.53(10) . . ?
O7 Gd1 O2 135.67(10) . . ?
O1 Gd1 O8 136.25(10) . . ?
O6 Gd1 O8 74.65(10) . . ?
O7 Gd1 O8 81.47(10) . . ?
O2 Gd1 O8 142.33(10) . . ?
O1 Gd1 N1 143.35(11) . . ?
O6 Gd1 N1 132.27(10) . . ?
O7 Gd1 N1 74.69(11) . . ?
O2 Gd1 N1 103.95(11) . . ?
O8 Gd1 N1 76.50(11) . . ?
O1 Gd1 O5 73.49(10) . . ?
O6 Gd1 O5 144.72(10) . . ?
O7 Gd1 O5 69.96(11) . . ?
O2 Gd1 O5 68.34(11) . . ?
O8 Gd1 O5 140.30(10) . . ?
N1 Gd1 O5 69.87(11) . . ?
O1 Gd1 O4 121.33(9) . . ?
O6 Gd1 O4 72.03(9) . . ?
O7 Gd1 O4 142.27(10) . . ?
O2 Gd1 O4 62.18(9) . . ?
O8 Gd1 O4 84.45(10) . . ?
N1 Gd1 O4 68.03(10) . . ?
O5 Gd1 O4 101.43(10) . . ?
O1 Gd1 O3 61.44(9) . . ?
O6 Gd1 O3 69.23(9) . . ?
O7 Gd1 O3 69.00(10) . . ?
O2 Gd1 O3 117.96(10) . . ?
O8 Gd1 O3 76.10(10) . . ?
N1 Gd1 O3 137.01(10) . . ?
O5 Gd1 O3 115.94(10) . . ?
O4 Gd1 O3 139.97(9) . . ?
O1 Gd1 Ni1 31.62(7) . . ?
O6 Gd1 Ni1 84.12(7) . . ?
O7 Gd1 Ni1 111.75(7) . . ?
O2 Gd1 Ni1 31.57(7) . . ?
O8 Gd1 Ni1 158.25(7) . . ?
N1 Gd1 Ni1 122.80(8) . . ?
O5 Gd1 Ni1 61.33(8) . . ?
O4 Gd1 Ni1 93.56(6) . . ?
O3 Gd1 Ni1 92.19(6) . . ?
C1 N1 Gd1 162.1(3) . . ?
C13 N7 C14 119.3(4) . . ?
C13 N7 Ni1 126.6(3) . . ?
C14 N7 Ni1 113.7(3) . . ?
C16 N8 C15 120.4(4) . . ?
C16 N8 Ni1 126.9(3) . . ?
C15 N8 Ni1 112.7(3) . . ?
N8 Ni1 N7 86.51(17) . . ?
N8 Ni1 O2 177.21(15) . . ?
N7 Ni1 O2 95.46(15) . . ?
N8 Ni1 O1 95.30(14) . . ?
N7 Ni1 O1 176.13(16) . . ?
O2 Ni1 O1 82.85(12) . . ?
N8 Ni1 Gd1 135.24(11) . . ?
N7 Ni1 Gd1 137.00(13) . . ?
O2 Ni1 Gd1 42.45(9) . . ?
O1 Ni1 Gd1 42.07(9) . . ?
C22 O1 Ni1 125.8(3) . . ?
C22 O1 Gd1 127.9(2) . . ?
Ni1 O1 Gd1 106.31(12) . . ?
C12 O2 Ni1 126.8(3) . . ?
C12 O2 Gd1 127.2(3) . . ?
Ni1 O2 Gd1 105.98(12) . . ?
C21 O3 C23 115.0(3) . . ?
C21 O3 Gd1 115.9(2) . . ?
C23 O3 Gd1 128.1(2) . . ?
C7 O4 C24 116.0(3) . . ?
C7 O4 Gd1 118.9(2) . . ?
C24 O4 Gd1 123.8(2) . . ?

_refine_diff_density_max         1.519
_refine_diff_density_min         -1.160
_refine_diff_density_rms         0.118

_shelxl_version_number           2014/6


_exptl_crystal_preparation       'Magnetic properties'
