# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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_GdCr
_database_code_depnum_ccdc_archive 'CCDC 1586426'
_audit_update_record             
;
2017-11-19 deposited with the CCDC.
2018-01-10 downloaded from the CCDC.
;

_audit_creation_date             2017-04-02T22:22:38-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.3
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_formula_moiety         'C16 H20 Cr Gd N8 O7'
_chemical_formula_sum            'C16 H20 Cr Gd N8 O7'
_chemical_formula_weight         645.65

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_Int_Tables_number      15
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                   15.8663(5)
_cell_length_b                   9.3487(3)
_cell_length_c                   18.1863(6)
_cell_angle_alpha                90
_cell_angle_beta                 116.0730(10)
_cell_angle_gamma                90
_cell_volume                     2423.04(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    11075
_cell_measurement_theta_min      3.143
_cell_measurement_theta_max      27.449
_cell_measurement_wavelength     0.71075

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_exptl_crystal_density_diffrn    1.77
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1264

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    3.213
_exptl_absorpt_correction_type   multi-scan
_shelx_estimated_absorpt_T_min   0.467
_shelx_estimated_absorpt_T_max   0.783
_exptl_absorpt_correction_T_min  0.6692
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_radiation_probe          x-ray
_diffrn_standards_number         0
_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       ω
_diffrn_reflns_av_R_equivalents  0.0291
_diffrn_reflns_av_unetI/netI     0.0232
_diffrn_reflns_number            11075
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         3.143
_diffrn_reflns_theta_max         27.449
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.99
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.99
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.99
_reflns_Friedel_coverage         0
_reflns_number_total             2736
_reflns_number_gt                2613
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION                                       #
#----------------------------------------------------------------------------#

_atom_sites_solution_hydrogens   difmap

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0374P)²+17.7610P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_extinction_method     none
_refine_ls_number_reflns         2736
_refine_ls_number_parameters     187
_refine_ls_number_restraints     6
_refine_ls_number_constraints    0
_refine_ls_R_factor_all          0.0232
_refine_ls_R_factor_gt           0.0194
_refine_ls_wR_factor_ref         0.092
_refine_ls_wR_factor_gt          0.0484
_refine_ls_goodness_of_fit_ref   1.388
_refine_ls_restrained_S_all      1.387
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_diff_density_max         1.23
_refine_diff_density_min         -1.609
_refine_diff_density_rms         0.224

#----------------------------------------------------------------------------#
#                   CONSTRAINTS AND RESTRAINTS                               #
#----------------------------------------------------------------------------#

_refine_special_details          
;
The following restraints have been applied:
DFIX  0.95 O2 H2A
DFIX  0.95 O2 H2B
DFIX  0.95 O3 H3A
DFIX  0.95 O3 H3B
DFIX  0.95 O4 H4A
DFIX  0.9 N4 H4N
The O-H distances between O atoms of water molecules and their hydrogen atoms were
fixed in order to ensure the proper geometry.
The N-H distance was fixed for the H atom attached to N atom of 3-pyridone ligand, to ensure
the proper geometry.
;

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Gd Gd -0.1653 3.9035 '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'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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
Gd1 Gd 0.5 0.40610(3) 0.25 0.00733(11) Uani 1 2 d S T P . .
Cr1 Cr 0.75 0.75 0.5 0.00818(19) Uani 1 2 d S . P . .
O3 O 0.5612(2) 0.1924(4) 0.2133(2) 0.0171(6) Uani 1 1 d D . . . .
O2 O 0.3813(2) 0.3332(3) 0.1182(2) 0.0186(7) Uani 1 1 d D . . . .
O4 O 0.5 0.9283(5) 0.25 0.0309(12) Uani 1 2 d DS T P . .
O1 O 0.6147(2) 0.4715(3) 0.21023(19) 0.0133(6) Uani 1 1 d . . . . .
N3 N 0.6952(4) 1.0707(5) 0.4334(3) 0.0288(10) Uani 1 1 d . . . . .
N2 N 0.8898(3) 0.7147(5) 0.4156(2) 0.0200(8) Uani 1 1 d . . . . .
N1 N 0.5806(3) 0.6214(4) 0.3385(2) 0.0127(7) Uani 1 1 d . . . . .
N4 N 0.7287(3) 0.7958(4) 0.2017(2) 0.0148(7) Uani 1 1 d D . . . .
C2 C 0.8414(3) 0.7308(5) 0.4470(3) 0.0133(8) Uani 1 1 d . . . . .
C3 C 0.7162(3) 0.9559(5) 0.4566(3) 0.0156(8) Uani 1 1 d . . . . .
C1 C 0.6404(3) 0.6732(4) 0.3944(3) 0.0118(8) Uani 1 1 d . . . . .
C5 C 0.6327(3) 0.5880(4) 0.1813(3) 0.0106(8) Uani 1 1 d . . . . .
C8 C 0.6780(3) 0.8439(5) 0.1249(3) 0.0199(9) Uani 1 1 d . . . . .
C7 C 0.6017(3) 0.7626(6) 0.0731(3) 0.0204(10) Uani 1 1 d . . . . .
C6 C 0.5794(3) 0.6384(5) 0.1005(3) 0.0170(9) Uani 1 1 d . . . . .
C4 C 0.7099(3) 0.6753(5) 0.2305(3) 0.0128(8) Uani 1 1 d . . . . .
H2A H 0.347(4) 0.394(5) 0.075(2) 0.015 Uiso 1 1 d D U . . .
H2B H 0.351(4) 0.244(3) 0.103(3) 0.015 Uiso 1 1 d D U . . .
H3A H 0.570(4) 0.193(6) 0.166(2) 0.015 Uiso 1 1 d D U . . .
H3B H 0.544(4) 0.100(3) 0.222(4) 0.015 Uiso 1 1 d D U . . .
H8 H 0.699(4) 0.930(6) 0.109(4) 0.019(14) Uiso 1 1 d . . . . .
H4 H 0.746(5) 0.651(7) 0.284(4) 0.029(16) Uiso 1 1 d . . . . .
H6 H 0.528(4) 0.583(6) 0.066(4) 0.019(15) Uiso 1 1 d . . . . .
H4A H 0.543(3) 0.862(5) 0.286(3) 0.022 Uiso 1 1 d D U . . .
H7 H 0.567(5) 0.796(8) 0.018(4) 0.037(18) Uiso 1 1 d . . . . .
H4N H 0.776(3) 0.852(6) 0.233(3) 0.025(15) Uiso 1 1 d D . . . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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 O1 2.317(3) 2_655 ?
Gd1 O1 2.317(3) . ?
Gd1 O2 2.406(3) . ?
Gd1 O2 2.406(3) 2_655 ?
Gd1 O3 2.439(3) 2_655 ?
Gd1 O3 2.439(3) . ?
Gd1 N1 2.544(4) . ?
Gd1 N1 2.544(4) 2_655 ?
Cr1 C3 2.060(5) . ?
Cr1 C3 2.060(5) 7_666 ?
Cr1 C1 2.072(4) . ?
Cr1 C1 2.072(4) 7_666 ?
Cr1 C2 2.072(5) 7_666 ?
Cr1 C2 2.072(5) . ?
O3 H3A 0.93(2) . ?
O3 H3B 0.94(2) . ?
O2 H2A 0.93(2) . ?
O2 H2B 0.94(2) . ?
O4 H4A 0.94(2) . ?
O1 C5 1.293(5) . ?
N3 C3 1.148(7) . ?
N2 C2 1.151(6) . ?
N1 C1 1.148(6) . ?
N4 C4 1.330(6) . ?
N4 C8 1.345(6) . ?
N4 H4N 0.89(2) . ?
C5 C4 1.416(6) . ?
C5 C6 1.417(6) . ?
C8 C7 1.389(7) . ?
C8 H8 0.96(6) . ?
C7 C6 1.370(7) . ?
C7 H7 0.96(7) . ?
C6 H6 0.94(6) . ?
C4 H4 0.92(7) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Gd1 O1 149.39(15) 2_655 . ?
O1 Gd1 O2 90.43(12) 2_655 . ?
O1 Gd1 O2 98.17(11) . . ?
O1 Gd1 O2 98.16(11) 2_655 2_655 ?
O1 Gd1 O2 90.43(12) . 2_655 ?
O2 Gd1 O2 147.09(16) . 2_655 ?
O1 Gd1 O3 70.67(11) 2_655 2_655 ?
O1 Gd1 O3 139.77(11) . 2_655 ?
O2 Gd1 O3 79.01(11) . 2_655 ?
O2 Gd1 O3 74.13(11) 2_655 2_655 ?
O1 Gd1 O3 139.77(11) 2_655 . ?
O1 Gd1 O3 70.67(11) . . ?
O2 Gd1 O3 74.13(11) . . ?
O2 Gd1 O3 79.01(11) 2_655 . ?
O3 Gd1 O3 70.01(15) 2_655 . ?
O1 Gd1 N1 80.74(11) 2_655 . ?
O1 Gd1 N1 75.11(11) . . ?
O2 Gd1 N1 144.14(11) . . ?
O2 Gd1 N1 68.76(11) 2_655 . ?
O3 Gd1 N1 128.67(11) 2_655 . ?
O3 Gd1 N1 132.18(11) . . ?
O1 Gd1 N1 75.11(11) 2_655 2_655 ?
O1 Gd1 N1 80.74(11) . 2_655 ?
O2 Gd1 N1 68.76(11) . 2_655 ?
O2 Gd1 N1 144.14(11) 2_655 2_655 ?
O3 Gd1 N1 132.18(11) 2_655 2_655 ?
O3 Gd1 N1 128.67(11) . 2_655 ?
N1 Gd1 N1 75.38(17) . 2_655 ?
C3 Cr1 C3 180 . 7_666 ?
C3 Cr1 C1 89.85(17) . . ?
C3 Cr1 C1 90.15(17) 7_666 . ?
C3 Cr1 C1 90.15(17) . 7_666 ?
C3 Cr1 C1 89.85(17) 7_666 7_666 ?
C1 Cr1 C1 180 . 7_666 ?
C3 Cr1 C2 88.82(18) . 7_666 ?
C3 Cr1 C2 91.18(18) 7_666 7_666 ?
C1 Cr1 C2 89.30(16) . 7_666 ?
C1 Cr1 C2 90.70(16) 7_666 7_666 ?
C3 Cr1 C2 91.18(18) . . ?
C3 Cr1 C2 88.82(18) 7_666 . ?
C1 Cr1 C2 90.70(16) . . ?
C1 Cr1 C2 89.30(16) 7_666 . ?
C2 Cr1 C2 180 7_666 . ?
Gd1 O3 H3A 119(3) . . ?
Gd1 O3 H3B 121(4) . . ?
H3A O3 H3B 111(5) . . ?
Gd1 O2 H2A 126(3) . . ?
Gd1 O2 H2B 128(3) . . ?
H2A O2 H2B 105(5) . . ?
C5 O1 Gd1 133.8(3) . . ?
C1 N1 Gd1 152.1(3) . . ?
C4 N4 C8 123.8(4) . . ?
C4 N4 H4N 122(4) . . ?
C8 N4 H4N 114(4) . . ?
N2 C2 Cr1 176.8(4) . . ?
N3 C3 Cr1 177.8(5) . . ?
N1 C1 Cr1 175.2(4) . . ?
O1 C5 C4 120.8(4) . . ?
O1 C5 C6 124.4(4) . . ?
C4 C5 C6 114.8(4) . . ?
N4 C8 C7 117.8(4) . . ?
N4 C8 H8 118(4) . . ?
C7 C8 H8 125(4) . . ?
C6 C7 C8 120.3(4) . . ?
C6 C7 H7 122(4) . . ?
C8 C7 H7 117(4) . . ?
C7 C6 C5 121.8(4) . . ?
C7 C6 H6 121(4) . . ?
C5 C6 H6 118(4) . . ?
N4 C4 C5 121.4(4) . . ?
N4 C4 H4 119(4) . . ?
C5 C4 H4 119(4) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Gd1 O1 C5 C4 107.0(4) . . . . ?
Gd1 O1 C5 C6 -73.4(6) . . . . ?
C4 N4 C8 C7 0.1(7) . . . . ?
N4 C8 C7 C6 0.4(8) . . . . ?
C8 C7 C6 C5 -0.3(8) . . . . ?
O1 C5 C6 C7 -180.0(4) . . . . ?
C4 C5 C6 C7 -0.4(7) . . . . ?
C8 N4 C4 C5 -0.8(7) . . . . ?
O1 C5 C4 N4 -179.5(4) . . . . ?
C6 C5 C4 N4 0.9(6) . . . . ?



# END of CIF
_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_TbCr
_database_code_depnum_ccdc_archive 'CCDC 1586427'
_audit_update_record             
;
2017-11-19 deposited with the CCDC.
2018-01-10 downloaded from the CCDC.
;

_audit_creation_date             2017-10-26T10:30:30-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.3
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_formula_moiety         'C16 H20 Cr N8 O7 Tb'
_chemical_formula_sum            'C16 H20 Cr N8 O7 Tb'
_chemical_formula_weight         647.32

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_Int_Tables_number      15
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                   15.8439(18)
_cell_length_b                   9.3305(11)
_cell_length_c                   18.178(2)
_cell_angle_alpha                90
_cell_angle_beta                 116.069(3)
_cell_angle_gamma                90
_cell_volume                     2413.9(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    11183
_cell_measurement_theta_min      3.147
_cell_measurement_theta_max      27.435
_cell_measurement_wavelength     0.71075

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_exptl_crystal_density_diffrn    1.781
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1268

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    3.407
_exptl_absorpt_correction_type   multi-scan
_shelx_estimated_absorpt_T_min   0.560
_shelx_estimated_absorpt_T_max   0.815
_exptl_absorpt_correction_T_min  0.5493
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_radiation_probe          x-ray
_diffrn_standards_number         0
_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       ω
_diffrn_reflns_av_R_equivalents  0.0757
_diffrn_reflns_av_unetI/netI     0.0661
_diffrn_reflns_number            11183
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         3.147
_diffrn_reflns_theta_max         27.435
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.996
_reflns_Friedel_coverage         0
_reflns_number_total             2739
_reflns_number_gt                2291
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION                                       #
#----------------------------------------------------------------------------#

_atom_sites_solution_hydrogens   difmap

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+104.0435P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_extinction_method     none
_refine_ls_number_reflns         2739
_refine_ls_number_parameters     182
_refine_ls_number_restraints     8
_refine_ls_number_constraints    0
_refine_ls_R_factor_all          0.0771
_refine_ls_R_factor_gt           0.0504
_refine_ls_wR_factor_ref         0.1496
_refine_ls_wR_factor_gt          0.1
_refine_ls_goodness_of_fit_ref   1.301
_refine_ls_restrained_S_all      1.3
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_diff_density_max         2.332
_refine_diff_density_min         -4.24
_refine_diff_density_rms         0.399

#----------------------------------------------------------------------------#
#                   CONSTRAINTS AND RESTRAINTS                               #
#----------------------------------------------------------------------------#

_refine_special_details          
;
The following restraints have been applied:
DFIX  0.95 O2 H2A
DFIX  0.95 O2 H2B
DFIX  0.95 O3 H3A
DFIX  0.95 O3 H3B
DFIX  0.95 O4 H4A
DFIX  0.9 N4 H4N
DFIX  2.42 0.05 N1 H4A
DELU  0.005 C1 N1
The O-H distances between O atoms of water molecules and their hydrogen atoms were
fixed in order to ensure the proper geometry. For H4A atom, its position was additionally
controlled by the relative position to the N1 atom of the cyanides.
The N-H distance was fixed for the H atom attached to N atom of 3-pyridone ligand, to ensure
the proper geometry.
In addition, a single DELU restraint was applied for the C1-N1 atoms of cyanides to 
ensure the convergence of the refinement process which was unstable due to the 
instability of the thermal ellipsoid on N1 atom.
;

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Tb Tb -0.1723 4.1537 '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'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Tb1 Tb 0.5 0.40631(7) 0.25 0.01218(18) Uani 1 2 d S T P . .
Cr1 Cr 0.75 0.75 0.5 0.0104(4) Uani 1 2 d S . P . .
O3 O 0.5617(5) 0.1940(7) 0.2140(4) 0.0162(13) Uani 1 1 d D . . . .
O2 O 0.3823(5) 0.3346(7) 0.1196(4) 0.0219(15) Uani 1 1 d D . . . .
O4 O 0.5 0.9294(13) 0.25 0.038(3) Uani 1 2 d DS T P . .
O1 O 0.6130(4) 0.4703(7) 0.2101(4) 0.0153(13) Uani 1 1 d . . . . .
N3 N 0.6956(7) 1.0724(10) 0.4336(5) 0.033(2) Uani 1 1 d . . . . .
N2 N 0.8896(6) 0.7149(10) 0.4150(5) 0.0220(18) Uani 1 1 d . . . . .
N1 N 0.5798(5) 0.6207(9) 0.3382(4) 0.0184(17) Uani 1 1 d D U . . .
N4 N 0.7289(5) 0.7946(9) 0.2007(5) 0.0189(17) Uani 1 1 d D . . . .
C2 C 0.8412(6) 0.7299(10) 0.4451(5) 0.0180(19) Uani 1 1 d . . . . .
C3 C 0.7168(6) 0.9577(11) 0.4575(5) 0.0179(19) Uani 1 1 d . . . . .
C1 C 0.6395(6) 0.6713(10) 0.3933(5) 0.0143(17) Uani 1 1 d . U . . .
C5 C 0.6332(6) 0.5895(10) 0.1813(5) 0.0133(17) Uani 1 1 d . . . . .
C8 C 0.6778(6) 0.8408(11) 0.1246(6) 0.019(2) Uani 1 1 d . . . . .
C7 C 0.6014(7) 0.7630(12) 0.0724(6) 0.023(2) Uani 1 1 d . . . . .
C6 C 0.5791(7) 0.6366(11) 0.1010(6) 0.022(2) Uani 1 1 d . . . . .
C4 C 0.7090(7) 0.6730(10) 0.2299(6) 0.0167(18) Uani 1 1 d . . . . .
H2A H 0.333(5) 0.387(10) 0.078(4) 0.02 Uiso 1 1 d D U . . .
H2B H 0.354(7) 0.244(5) 0.103(6) 0.02 Uiso 1 1 d D U . . .
H3A H 0.567(7) 0.193(11) 0.164(3) 0.02 Uiso 1 1 d D U . . .
H3B H 0.549(7) 0.096(4) 0.219(6) 0.02 Uiso 1 1 d D U . . .
H8 H 0.697(7) 0.931(12) 0.114(6) 0.02 Uiso 1 1 d . U . . .
H4 H 0.748(7) 0.641(11) 0.283(6) 0.02 Uiso 1 1 d . U . . .
H6 H 0.524(7) 0.582(12) 0.065(6) 0.02 Uiso 1 1 d . U . . .
H4A H 0.546(5) 0.870(6) 0.291(4) 0.02 Uiso 1 1 d D U . . .
H7 H 0.563(7) 0.799(11) 0.017(7) 0.02 Uiso 1 1 d . U . . .
H4N H 0.781(4) 0.847(9) 0.231(5) 0.02 Uiso 1 1 d D U . . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tb1 O1 2.287(6) 2_655 ?
Tb1 O1 2.287(6) . ?
Tb1 O2 2.378(6) . ?
Tb1 O2 2.378(6) 2_655 ?
Tb1 O3 2.422(6) 2_655 ?
Tb1 O3 2.422(6) . ?
Tb1 N1 2.528(8) . ?
Tb1 N1 2.528(8) 2_655 ?
Cr1 C3 2.067(10) . ?
Cr1 C3 2.067(10) 7_666 ?
Cr1 C1 2.093(9) . ?
Cr1 C1 2.094(9) 7_666 ?
Cr1 C2 2.096(9) . ?
Cr1 C2 2.096(9) 7_666 ?
O3 H3A 0.95(2) . ?
O3 H3B 0.95(2) . ?
O2 H2A 0.95(2) . ?
O2 H2B 0.94(2) . ?
O4 H4A 0.95(2) . ?
O1 C5 1.328(11) . ?
N3 C3 1.148(13) . ?
N2 C2 1.129(12) . ?
N1 C1 1.135(11) . ?
N4 C8 1.330(12) . ?
N4 C4 1.347(12) . ?
N4 H4N 0.90(2) . ?
C5 C4 1.377(12) . ?
C5 C6 1.399(13) . ?
C8 C7 1.372(13) . ?
C8 H8 0.95(11) . ?
C7 C6 1.395(14) . ?
C7 H7 0.98(11) . ?
C6 H6 0.97(10) . ?
C4 H4 0.94(10) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Tb1 O1 149.7(3) 2_655 . ?
O1 Tb1 O2 90.5(2) 2_655 . ?
O1 Tb1 O2 97.9(2) . . ?
O1 Tb1 O2 97.9(2) 2_655 2_655 ?
O1 Tb1 O2 90.5(2) . 2_655 ?
O2 Tb1 O2 147.3(3) . 2_655 ?
O1 Tb1 O3 70.3(2) 2_655 2_655 ?
O1 Tb1 O3 139.8(2) . 2_655 ?
O2 Tb1 O3 78.8(2) . 2_655 ?
O2 Tb1 O3 74.6(2) 2_655 2_655 ?
O1 Tb1 O3 139.8(2) 2_655 . ?
O1 Tb1 O3 70.3(2) . . ?
O2 Tb1 O3 74.6(2) . . ?
O2 Tb1 O3 78.8(2) 2_655 . ?
O3 Tb1 O3 70.3(3) 2_655 . ?
O1 Tb1 N1 80.5(2) 2_655 . ?
O1 Tb1 N1 75.6(2) . . ?
O2 Tb1 N1 144.0(2) . . ?
O2 Tb1 N1 68.7(2) 2_655 . ?
O3 Tb1 N1 128.7(2) 2_655 . ?
O3 Tb1 N1 132.1(2) . . ?
O1 Tb1 N1 75.6(2) 2_655 2_655 ?
O1 Tb1 N1 80.5(2) . 2_655 ?
O2 Tb1 N1 68.7(2) . 2_655 ?
O2 Tb1 N1 144.0(2) 2_655 2_655 ?
O3 Tb1 N1 132.0(2) 2_655 2_655 ?
O3 Tb1 N1 128.7(2) . 2_655 ?
N1 Tb1 N1 75.3(3) . 2_655 ?
C3 Cr1 C3 180.00(19) . 7_666 ?
C3 Cr1 C1 90.6(4) . . ?
C3 Cr1 C1 89.4(4) 7_666 . ?
C3 Cr1 C1 89.4(4) . 7_666 ?
C3 Cr1 C1 90.6(4) 7_666 7_666 ?
C1 Cr1 C1 180.0(4) . 7_666 ?
C3 Cr1 C2 91.2(4) . . ?
C3 Cr1 C2 88.8(4) 7_666 . ?
C1 Cr1 C2 89.9(3) . . ?
C1 Cr1 C2 90.1(3) 7_666 . ?
C3 Cr1 C2 88.8(4) . 7_666 ?
C3 Cr1 C2 91.2(4) 7_666 7_666 ?
C1 Cr1 C2 90.1(3) . 7_666 ?
C1 Cr1 C2 89.9(3) 7_666 7_666 ?
C2 Cr1 C2 180 . 7_666 ?
Tb1 O3 H3A 119(6) . . ?
Tb1 O3 H3B 129(6) . . ?
H3A O3 H3B 102(9) . . ?
Tb1 O2 H2A 131(6) . . ?
Tb1 O2 H2B 129(6) . . ?
H2A O2 H2B 96(9) . . ?
C5 O1 Tb1 134.7(5) . . ?
C1 N1 Tb1 151.6(7) . . ?
C8 N4 C4 122.8(8) . . ?
C8 N4 H4N 115(7) . . ?
C4 N4 H4N 122(7) . . ?
N2 C2 Cr1 178.0(9) . . ?
N3 C3 Cr1 177.9(9) . . ?
N1 C1 Cr1 175.5(8) . . ?
O1 C5 C4 121.0(8) . . ?
O1 C5 C6 122.0(8) . . ?
C4 C5 C6 117.0(9) . . ?
N4 C8 C7 119.8(9) . . ?
N4 C8 H8 114(6) . . ?
C7 C8 H8 126(6) . . ?
C8 C7 C6 118.7(9) . . ?
C8 C7 H7 119(6) . . ?
C6 C7 H7 122(6) . . ?
C7 C6 C5 120.9(9) . . ?
C7 C6 H6 119(6) . . ?
C5 C6 H6 120(6) . . ?
N4 C4 C5 120.8(9) . . ?
N4 C4 H4 121(6) . . ?
C5 C4 H4 118(6) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Tb1 O1 C5 C4 105.7(9) . . . . ?
Tb1 O1 C5 C6 -73.9(11) . . . . ?
C4 N4 C8 C7 -0.2(15) . . . . ?
N4 C8 C7 C6 0.2(15) . . . . ?
C8 C7 C6 C5 0.0(15) . . . . ?
O1 C5 C6 C7 179.4(8) . . . . ?
C4 C5 C6 C7 -0.2(13) . . . . ?
C8 N4 C4 C5 0.0(14) . . . . ?
O1 C5 C4 N4 -179.4(8) . . . . ?
C6 C5 C4 N4 0.2(13) . . . . ?



# END of CIF
_exptl_crystal_preparation       'Magnetic properties'
