# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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_shelx
_database_code_depnum_ccdc_archive 'CCDC 1477277'
_audit_update_record             
;
2016-04-29 deposited with the CCDC.
2016-08-08 downloaded from the CCDC.
;

_audit_creation_date             2016-04-26T12:10:03-00:00
_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 H16 Co Dy N8 O5'
_chemical_formula_sum            'C16 H16 Co Dy N8 O5'
_chemical_formula_weight         621.8

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

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/m'
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_Int_Tables_number      11
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, z'

_cell_length_a                   6.8970(5)
_cell_length_b                   15.6685(9)
_cell_length_c                   9.6096(6)
_cell_angle_alpha                90
_cell_angle_beta                 102.131(7)
_cell_angle_gamma                90
_cell_volume                     1015.28(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9618
_cell_measurement_theta_min      3.021
_cell_measurement_theta_max      27.481
_cell_measurement_wavelength     0.71075

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

_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.095
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.027
_exptl_crystal_density_diffrn    2.034
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             602

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

_exptl_absorpt_coefficient_mu    4.516
_exptl_absorpt_correction_type   multi-scan
_shelx_estimated_absorpt_T_min   0.674
_shelx_estimated_absorpt_T_max   0.888
_exptl_absorpt_correction_T_min  0.7012
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'

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

_diffrn_ambient_temperature      100(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  0.0855
_diffrn_reflns_av_unetI/netI     0.0723
_diffrn_reflns_number            9618
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         3.021
_diffrn_reflns_theta_max         27.481
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_reflns_Friedel_coverage         0
_reflns_number_total             2407
_reflns_number_gt                2117
_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)+(0.0373P)²+6.7117P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_number_reflns         2407
_refine_ls_number_parameters     185
_refine_ls_number_restraints     41
_refine_ls_number_constraints    0
_refine_ls_R_factor_all          0.0801
_refine_ls_R_factor_gt           0.0624
_refine_ls_wR_factor_ref         0.1119
_refine_ls_wR_factor_gt          0.1023
_refine_ls_goodness_of_fit_ref   1.21
_refine_ls_restrained_S_all      1.208
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_diff_density_max         2.934
_refine_diff_density_min         -2.729
_refine_diff_density_rms         0.289

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

_refine_special_details          
;
DFIX  0.95 0.01 O3 H3
DFIX  0.95 0.01 O2 H2A
DFIX  0.95 0.01 O2 H2B
DFIX  0.95 0.01 O1 H1
DELU  0.003 N2 C2
DELU  0.003 N3 C3
SIMU  0.005 N1 C1
ISOR  0.005 C4
ISOR  0.002 O3 C3 N4 C2
The hydrogen atoms were found independently from the electron density map, 
and refined isotropically, however the part of O-H distances were fixed by 
the DFIX command in order to stabilize their positions during 
the refinement procedure. 
The part of carbon and nitrogen atoms of cyanides, and the oxygen atom 
of one coordinated water molecule, reveal significant degree of structural disorder 
affecting the refinement procedure and the shape of their thermal ellipsoids. 
Thus, the restraints on their thermal ellipsoids (DELU, ISOR, SIMU) were applied.
;

#----------------------------------------------------------------------------#
#                   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
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
O O 0.0106 0.006 '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'

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
Dy1 Dy 0.32330(8) 0.25 0.71493(6) 0.00512(15) Uani 1 2 d S T P . .
Co1 Co 0.6804(3) 0.25 0.27089(15) 0.0078(3) Uani 1 2 d S T P . .
O1 O 0.5890(8) 0.3378(4) 0.7472(6) 0.0174(13) Uani 1 1 d . . . . .
O2 O 0.1946(10) 0.3913(4) 0.6993(9) 0.0331(17) Uani 1 1 d D . . . .
N2 N 1.0094(16) 0.25 0.5335(10) 0.018(2) Uani 1 2 d S TU P . .
N6 N 0.7997(12) 0.5794(5) 0.8120(10) 0.0266(18) Uani 1 1 d . . . . .
N1 N 0.3916(16) 0.25 0.4674(13) 0.022(2) Uani 1 2 d S TU P . .
N3 N 0.4034(16) 0.25 -0.0207(11) 0.018(2) Uani 1 2 d S TU P . .
N4 N 1.0083(13) 0.25 0.1082(9) 0.0045(18) Uani 1 2 d S TU P . .
N5 N 0.7066(11) 0.4440(4) 0.2795(8) 0.0187(16) Uani 1 1 d . . . . .
C6 C 0.6607(12) 0.4135(5) 0.7681(9) 0.0161(17) Uani 1 1 d . . . . .
C10 C 0.6966(13) 0.4521(5) 0.9044(9) 0.0159(18) Uani 1 1 d . . . . .
C9 C 0.7619(14) 0.5335(6) 0.9227(11) 0.025(2) Uani 1 1 d . . . . .
C7 C 0.7094(12) 0.4622(6) 0.6551(10) 0.0174(19) Uani 1 1 d . . . . .
C8 C 0.7778(13) 0.5440(6) 0.6821(11) 0.026(2) Uani 1 1 d . . . . .
C1 C 0.4889(19) 0.25 0.3895(14) 0.020(2) Uani 1 2 d S TU P . .
C4 C 0.8782(17) 0.25 0.1703(12) 0.010(2) Uani 1 2 d S TU P . .
C2 C 0.8784(16) 0.25 0.4382(11) 0.009(2) Uani 1 2 d S TU P . .
C3 C 0.4974(17) 0.25 0.0916(12) 0.012(2) Uani 1 2 d S TU P . .
C5 C 0.6920(12) 0.3714(5) 0.2743(8) 0.0138(17) Uani 1 1 d . . . . .
O3 O 0.0163(14) 0.25 0.8102(8) 0.021(2) Uani 1 2 d DS TU P . .
H8 H 0.804(14) 0.577(6) 0.606(10) 0.02(2) Uiso 1 1 d . . . . .
H10 H 0.678(13) 0.417(6) 0.985(10) 0.02(2) Uiso 1 1 d . . . . .
H7 H 0.713(12) 0.445(5) 0.571(9) 0.01(2) Uiso 1 1 d . . . . .
H9 H 0.775(15) 0.562(6) 1.003(11) 0.03(3) Uiso 1 1 d . . . . .
H2B H 0.237(14) 0.449(2) 0.704(11) 0.03(3) Uiso 1 1 d D . . . .
H2A H 0.058(4) 0.398(7) 0.699(12) 0.05(3) Uiso 1 1 d D . . . .
H3 H -0.015(14) 0.297(4) 0.862(8) 0.03(3) 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
Dy1 O1 2.260(5) . ?
Dy1 O1 2.260(5) 4_565 ?
Dy1 O2 2.378(6) . ?
Dy1 O2 2.378(6) 4_565 ?
Dy1 O3 2.477(9) . ?
Dy1 N2 2.478(10) 1_455 ?
Dy1 N3 2.483(10) 1_556 ?
Dy1 N1 2.520(11) . ?
Co1 C4 1.831(12) . ?
Co1 C2 1.878(11) . ?
Co1 C5 1.905(8) . ?
Co1 C5 1.905(8) 4_565 ?
Co1 C3 1.910(11) . ?
Co1 C1 1.918(14) . ?
O1 C6 1.284(10) . ?
O2 H2B 0.949(10) . ?
O2 H2A 0.948(10) . ?
N2 C2 1.143(14) . ?
N2 Dy1 2.478(10) 1_655 ?
N6 C8 1.345(13) . ?
N6 C9 1.354(13) . ?
N1 C1 1.105(16) . ?
N3 C3 1.136(14) . ?
N3 Dy1 2.483(10) 1_554 ?
N4 C4 1.177(14) . ?
N5 C5 1.142(10) . ?
C6 C10 1.416(11) . ?
C6 C7 1.423(12) . ?
C10 C9 1.352(13) . ?
C10 H10 0.98(9) . ?
C9 H9 0.89(10) . ?
C7 C8 1.371(13) . ?
C7 H7 0.86(9) . ?
C8 H8 0.94(9) . ?
O3 H3 0.948(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 Dy1 O1 75.0(3) . 4_565 ?
O1 Dy1 O2 73.9(2) . . ?
O1 Dy1 O2 148.9(2) 4_565 . ?
O1 Dy1 O2 148.9(2) . 4_565 ?
O1 Dy1 O2 73.9(2) 4_565 4_565 ?
O2 Dy1 O2 137.2(3) . 4_565 ?
O1 Dy1 O3 132.88(18) . . ?
O1 Dy1 O3 132.88(19) 4_565 . ?
O2 Dy1 O3 71.74(18) . . ?
O2 Dy1 O3 71.74(18) 4_565 . ?
O1 Dy1 N2 131.3(2) . 1_455 ?
O1 Dy1 N2 131.3(2) 4_565 1_455 ?
O2 Dy1 N2 72.33(18) . 1_455 ?
O2 Dy1 N2 72.33(18) 4_565 1_455 ?
O3 Dy1 N2 64.6(3) . 1_455 ?
O1 Dy1 N3 81.9(3) . 1_556 ?
O1 Dy1 N3 81.9(3) 4_565 1_556 ?
O2 Dy1 N3 93.7(2) . 1_556 ?
O2 Dy1 N3 93.7(2) 4_565 1_556 ?
O3 Dy1 N3 69.3(3) . 1_556 ?
N2 Dy1 N3 133.9(3) 1_455 1_556 ?
O1 Dy1 N1 79.8(3) . . ?
O1 Dy1 N1 79.8(2) 4_565 . ?
O2 Dy1 N1 94.7(2) . . ?
O2 Dy1 N1 94.7(2) 4_565 . ?
O3 Dy1 N1 133.8(3) . . ?
N2 Dy1 N1 69.2(3) 1_455 . ?
N3 Dy1 N1 156.9(4) 1_556 . ?
C4 Co1 C2 87.9(5) . . ?
C4 Co1 C5 88.6(2) . . ?
C2 Co1 C5 88.0(3) . . ?
C4 Co1 C5 88.6(2) . 4_565 ?
C2 Co1 C5 88.0(3) . 4_565 ?
C5 Co1 C5 175.2(5) . 4_565 ?
C4 Co1 C3 87.0(5) . . ?
C2 Co1 C3 175.0(5) . . ?
C5 Co1 C3 91.9(3) . . ?
C5 Co1 C3 91.9(3) 4_565 . ?
C4 Co1 C1 175.6(6) . . ?
C2 Co1 C1 87.6(5) . . ?
C5 Co1 C1 91.2(2) . . ?
C5 Co1 C1 91.2(2) 4_565 . ?
C3 Co1 C1 97.4(5) . . ?
C6 O1 Dy1 149.1(5) . . ?
Dy1 O2 H2B 141(6) . . ?
Dy1 O2 H2A 117(7) . . ?
H2B O2 H2A 101(9) . . ?
C2 N2 Dy1 171.9(10) . 1_655 ?
C8 N6 C9 120.5(8) . . ?
C1 N1 Dy1 154.1(11) . . ?
C3 N3 Dy1 158.7(10) . 1_554 ?
O1 C6 C10 121.6(8) . . ?
O1 C6 C7 121.4(8) . . ?
C10 C6 C7 117.0(8) . . ?
C9 C10 C6 120.8(9) . . ?
C9 C10 H10 122(5) . . ?
C6 C10 H10 117(5) . . ?
C10 C9 N6 120.9(9) . . ?
C10 C9 H9 125(7) . . ?
N6 C9 H9 114(7) . . ?
C8 C7 C6 118.9(9) . . ?
C8 C7 H7 114(6) . . ?
C6 C7 H7 127(6) . . ?
N6 C8 C7 121.9(9) . . ?
N6 C8 H8 119(5) . . ?
C7 C8 H8 119(5) . . ?
N1 C1 Co1 174.1(12) . . ?
N4 C4 Co1 178.6(10) . . ?
N2 C2 Co1 174.7(11) . . ?
N3 C3 Co1 173.6(11) . . ?
N5 C5 Co1 177.2(8) . . ?
Dy1 O3 H3 120(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
Dy1 O1 C6 C10 78.8(13) . . . . ?
Dy1 O1 C6 C7 -101.7(12) . . . . ?
O1 C6 C10 C9 -176.3(8) . . . . ?
C7 C6 C10 C9 4.2(12) . . . . ?
C6 C10 C9 N6 -1.8(13) . . . . ?
C8 N6 C9 C10 -1.8(14) . . . . ?
O1 C6 C7 C8 177.3(8) . . . . ?
C10 C6 C7 C8 -3.2(12) . . . . ?
C9 N6 C8 C7 2.8(14) . . . . ?
C6 C7 C8 N6 -0.1(13) . . . . ?


# END of CIF
_exptl_crystal_preparation       'Magnetic properties,Luminescent'
