# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# 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_Mn-1
_database_code_depnum_ccdc_archive 'CCDC 1840919'
loop_
_audit_author_name
_audit_author_address
'Goulven Cosquer'
;Tohoku University
Japan
;
_audit_update_record             
;
2018-05-02 deposited with the CCDC.	2019-07-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C26 H24 Mn N10 O6'
_chemical_formula_weight         627.49

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'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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, -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                   17.507(2)
_cell_length_b                   21.925(3)
_cell_length_c                   7.0181(9)
_cell_angle_alpha                90
_cell_angle_beta                 103.348(12)
_cell_angle_gamma                90
_cell_volume                     2621.1(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    2086
_cell_measurement_theta_min      3.0130
_cell_measurement_theta_max      30.4390

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.590
_exptl_crystal_F_000             1292
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    0.568
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.72878
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41p (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Rotating Anode'
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_detector       CCD
_diffrn_measurement_device       
;
Saturn724+ (4x4 bin mode)
;
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measurement_method       dtprofit.ref
_diffrn_reflns_number            5919
_diffrn_reflns_av_unetI/netI     0.0985
_diffrn_reflns_av_R_equivalents  0.0561
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         1.514
_diffrn_reflns_theta_max         30.680
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.840
_diffrn_measured_fraction_theta_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.840
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.840
_diffrn_reflns_point_group_measured_fraction_full 0.972
_reflns_number_total             3414
_reflns_number_gt                2152
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.1133P)²] 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         3414
_refine_ls_number_parameters     198
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1232
_refine_ls_R_factor_gt           0.0730
_refine_ls_wR_factor_ref         0.2047
_refine_ls_wR_factor_gt          0.1783
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_restrained_S_all      1.022
_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
Mn1 Mn 0.5000 0.22427(3) 0.7500 0.0221(2) Uani 1 2 d S T P . .
O3 O 0.54791(16) 0.21449(11) 0.4913(4) 0.0288(6) Uani 1 1 d . . . . .
H9 H 0.5329 0.1789 0.4143 0.035 Uiso 1 1 calc R U . . .
O1 O 0.56135(15) 0.31663(11) 0.8364(4) 0.0296(6) Uani 1 1 d . . . . .
O2 O 0.44076(14) -0.10247(12) 0.6458(4) 0.0281(6) Uani 1 1 d . . . . .
N6 N 0.5000 0.11838(19) 0.7500 0.0221(9) Uani 1 2 d S T P . .
N3 N 0.5000 0.54042(19) 0.7500 0.0233(9) Uani 1 2 d S T P . .
N4 N 0.38547(18) 0.18604(13) 0.5650(5) 0.0252(7) Uani 1 1 d . . . . .
N2 N 0.63430(17) 0.54532(14) 0.8254(5) 0.0254(7) Uani 1 1 d . . . . .
C11 C 0.4377(2) 0.08736(16) 0.6573(5) 0.0217(7) Uani 1 1 d . . . . .
C14 C 0.5000 -0.0774(2) 0.7500 0.0223(10) Uani 1 2 d S T P . .
C7 C 0.5000 0.3443(2) 0.7500 0.0216(10) Uani 1 2 d S T P . .
C13 C 0.5000 -0.0074(2) 0.7500 0.0229(10) Uani 1 2 d S T P . .
C6 C 0.5000 0.4136(2) 0.7500 0.0218(10) Uani 1 2 d S T P . .
C12 C 0.4339(2) 0.02399(16) 0.6542(5) 0.0221(7) Uani 1 1 d . . . . .
H8 H 0.3877 0.0031 0.5888 0.026 Uiso 1 1 calc R U . . .
C4 C 0.5665(2) 0.50832(16) 0.7902(5) 0.0227(7) Uani 1 1 d . . . . .
C5 C 0.5707(2) 0.44541(16) 0.7950(5) 0.0238(8) Uani 1 1 d . . . . .
H4 H 0.6197 0.4248 0.8276 0.029 Uiso 1 1 calc R U . . .
C8 C 0.3203(2) 0.20857(17) 0.4540(6) 0.0267(8) Uani 1 1 d . . . . .
H5 H 0.3106 0.2508 0.4298 0.032 Uiso 1 1 calc R U . . .
C9 C 0.2669(2) 0.16173(18) 0.3760(6) 0.0304(9) Uani 1 1 d . . . . .
H6 H 0.2161 0.1662 0.2927 0.036 Uiso 1 1 calc R U . . .
C3 C 0.6379(2) 0.60453(17) 0.7691(6) 0.0297(9) Uani 1 1 d . . . . .
H1 H 0.5957 0.6285 0.6971 0.036 Uiso 1 1 calc R U . . .
C2 C 0.7139(2) 0.62268(19) 0.8364(6) 0.0349(10) Uani 1 1 d . . . . .
H2 H 0.7355 0.6618 0.8233 0.042 Uiso 1 1 calc R U . . .
C10 C 0.3035(2) 0.10871(17) 0.4453(6) 0.0279(8) Uani 1 1 d . . . . .
H7 H 0.2832 0.0686 0.4193 0.034 Uiso 1 1 calc R U . . .
C1 C 0.7529(2) 0.57172(19) 0.9282(6) 0.0352(10) Uani 1 1 d . . . . .
H3 H 0.8073 0.5712 0.9887 0.042 Uiso 1 1 calc R U . . .
C15 C 0.5982(3) 0.2547(2) 0.4262(7) 0.0433(11) Uani 1 1 d . . . . .
H10 H 0.6102 0.2387 0.3060 0.065 Uiso 1 1 calc R U . . .
H11 H 0.5727 0.2946 0.3996 0.065 Uiso 1 1 calc R U . . .
H12 H 0.6469 0.2590 0.5273 0.065 Uiso 1 1 calc R U . . .
N5 N 0.62507(17) 0.12435(14) 0.9409(4) 0.0225(7) Uani 1 1 d . . . . .
N1 N 0.29383(18) 0.52391(16) 0.5773(5) 0.0344(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
Mn1 O3 2.179(3) . ?
Mn1 O3 2.179(3) 2_656 ?
Mn1 N4 2.282(3) 2_656 ?
Mn1 N4 2.282(3) . ?
Mn1 O1 2.307(3) . ?
Mn1 O1 2.307(3) 2_656 ?
Mn1 N6 2.322(4) . ?
Mn1 C7 2.631(5) . ?
O3 C15 1.394(5) . ?
O3 H9 0.9500 . ?
O1 C7 1.260(3) . ?
O2 C14 1.250(3) . ?
N6 C11 1.323(4) . ?
N6 C11 1.323(4) 2_656 ?
N3 C4 1.333(4) . ?
N3 C4 1.333(4) 2_656 ?
N4 C8 1.320(5) . ?
N4 N5 1.365(4) 2_656 ?
N2 C3 1.363(5) . ?
N2 N1 1.369(4) 2_656 ?
N2 C4 1.412(4) . ?
C11 C12 1.391(5) . ?
C11 N5 1.410(4) 2_656 ?
C14 O2 1.250(3) 2_656 ?
C14 C13 1.535(7) . ?
C7 O1 1.260(3) 2_656 ?
C7 C6 1.520(7) . ?
C13 C12 1.380(4) 2_656 ?
C13 C12 1.380(4) . ?
C6 C5 1.392(4) 2_656 ?
C6 C5 1.392(4) . ?
C12 H8 0.9500 . ?
C4 C5 1.381(5) . ?
C5 H4 0.9500 . ?
C8 C9 1.411(5) . ?
C8 H5 0.9500 . ?
C9 C10 1.362(5) . ?
C9 H6 0.9500 . ?
C3 C2 1.365(6) . ?
C3 H1 0.9500 . ?
C2 C1 1.388(6) . ?
C2 H2 0.9500 . ?
C10 N5 1.363(5) 2_656 ?
C10 H7 0.9500 . ?
C1 N1 1.325(5) 2_656 ?
C1 H3 0.9500 . ?
C15 H10 0.9800 . ?
C15 H11 0.9800 . ?
C15 H12 0.9800 . ?
N5 C10 1.363(5) 2_656 ?
N5 N4 1.365(4) 2_656 ?
N5 C11 1.410(4) 2_656 ?
N1 C1 1.324(5) 2_656 ?
N1 N2 1.369(4) 2_656 ?

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
O3 Mn1 O3 168.71(14) . 2_656 ?
O3 Mn1 N4 88.93(11) . 2_656 ?
O3 Mn1 N4 86.93(11) 2_656 2_656 ?
O3 Mn1 N4 86.93(11) . . ?
O3 Mn1 N4 88.93(11) 2_656 . ?
N4 Mn1 N4 136.90(15) 2_656 . ?
O3 Mn1 O1 93.44(9) . . ?
O3 Mn1 O1 96.47(10) 2_656 . ?
N4 Mn1 O1 83.00(10) 2_656 . ?
N4 Mn1 O1 140.06(10) . . ?
O3 Mn1 O1 96.47(10) . 2_656 ?
O3 Mn1 O1 93.44(9) 2_656 2_656 ?
N4 Mn1 O1 140.06(10) 2_656 2_656 ?
N4 Mn1 O1 83.00(10) . 2_656 ?
O1 Mn1 O1 57.24(13) . 2_656 ?
O3 Mn1 N6 84.36(7) . . ?
O3 Mn1 N6 84.36(7) 2_656 . ?
N4 Mn1 N6 68.45(8) 2_656 . ?
N4 Mn1 N6 68.45(8) . . ?
O1 Mn1 N6 151.38(7) . . ?
O1 Mn1 N6 151.38(7) 2_656 . ?
O3 Mn1 C7 95.64(7) . . ?
O3 Mn1 C7 95.64(7) 2_656 . ?
N4 Mn1 C7 111.55(8) 2_656 . ?
N4 Mn1 C7 111.55(8) . . ?
O1 Mn1 C7 28.62(7) . . ?
O1 Mn1 C7 28.62(7) 2_656 . ?
N6 Mn1 C7 180.0 . . ?
C15 O3 Mn1 127.1(2) . . ?
C15 O3 H9 116.4 . . ?
Mn1 O3 H9 116.4 . . ?
C7 O1 Mn1 90.1(2) . . ?
C11 N6 C11 118.1(4) . 2_656 ?
C11 N6 Mn1 121.0(2) . . ?
C11 N6 Mn1 121.0(2) 2_656 . ?
C4 N3 C4 116.3(4) . 2_656 ?
C8 N4 N5 105.1(3) . 2_656 ?
C8 N4 Mn1 136.4(3) . . ?
N5 N4 Mn1 118.4(2) 2_656 . ?
C3 N2 N1 111.9(3) . 2_656 ?
C3 N2 C4 126.1(3) . . ?
N1 N2 C4 122.0(3) 2_656 . ?
N6 C11 C12 123.5(3) . . ?
N6 C11 N5 113.9(3) . 2_656 ?
C12 C11 N5 122.5(3) . 2_656 ?
O2 C14 O2 127.8(5) . 2_656 ?
O2 C14 C13 116.1(2) . . ?
O2 C14 C13 116.1(2) 2_656 . ?
O1 C7 O1 122.5(5) 2_656 . ?
O1 C7 C6 118.8(2) 2_656 . ?
O1 C7 C6 118.8(2) . . ?
O1 C7 Mn1 61.2(2) 2_656 . ?
O1 C7 Mn1 61.2(2) . . ?
C6 C7 Mn1 180.0 . . ?
C12 C13 C12 120.3(5) 2_656 . ?
C12 C13 C14 119.9(2) 2_656 . ?
C12 C13 C14 119.9(2) . . ?
C5 C6 C5 119.9(5) 2_656 . ?
C5 C6 C7 120.1(2) 2_656 . ?
C5 C6 C7 120.1(2) . . ?
C13 C12 C11 117.3(3) . . ?
C13 C12 H8 121.4 . . ?
C11 C12 H8 121.4 . . ?
N3 C4 C5 124.9(3) . . ?
N3 C4 N2 113.0(3) . . ?
C5 C4 N2 122.1(3) . . ?
C4 C5 C6 117.1(3) . . ?
C4 C5 H4 121.5 . . ?
C6 C5 H4 121.5 . . ?
N4 C8 C9 111.2(3) . . ?
N4 C8 H5 124.4 . . ?
C9 C8 H5 124.4 . . ?
C10 C9 C8 105.5(3) . . ?
C10 C9 H6 127.2 . . ?
C8 C9 H6 127.2 . . ?
N2 C3 C2 106.5(3) . . ?
N2 C3 H1 126.8 . . ?
C2 C3 H1 126.8 . . ?
C3 C2 C1 105.2(4) . . ?
C3 C2 H2 127.4 . . ?
C1 C2 H2 127.4 . . ?
C9 C10 N5 106.7(3) . 2_656 ?
C9 C10 H7 126.6 . . ?
N5 C10 H7 126.7 2_656 . ?
N1 C1 C2 112.9(4) 2_656 . ?
N1 C1 H3 123.6 2_656 . ?
C2 C1 H3 123.6 . . ?
O3 C15 H10 109.5 . . ?
O3 C15 H11 109.5 . . ?
H10 C15 H11 109.5 . . ?
O3 C15 H12 109.5 . . ?
H10 C15 H12 109.5 . . ?
H11 C15 H12 109.5 . . ?
C10 N5 N4 111.5(3) 2_656 2_656 ?
C10 N5 C11 130.3(3) 2_656 2_656 ?
N4 N5 C11 118.1(3) 2_656 2_656 ?
C1 N1 N2 103.5(3) 2_656 2_656 ?

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
C11 N6 C11 C12 0.8(3) 2_656 . . . ?
Mn1 N6 C11 C12 -179.2(3) . . . . ?
C11 N6 C11 N5 -178.6(3) 2_656 . . 2_656 ?
Mn1 N6 C11 N5 1.4(3) . . . 2_656 ?
Mn1 O1 C7 O1 0.002(1) . . . 2_656 ?
Mn1 O1 C7 C6 180.000(0) . . . . ?
O2 C14 C13 C12 -173.8(2) . . . 2_656 ?
O2 C14 C13 C12 6.2(2) 2_656 . . 2_656 ?
O2 C14 C13 C12 6.2(2) . . . . ?
O2 C14 C13 C12 -173.8(2) 2_656 . . . ?
O1 C7 C6 C5 17.5(2) 2_656 . . 2_656 ?
O1 C7 C6 C5 -162.5(2) . . . 2_656 ?
O1 C7 C6 C5 -162.5(2) 2_656 . . . ?
O1 C7 C6 C5 17.5(2) . . . . ?
C12 C13 C12 C11 0.7(2) 2_656 . . . ?
C14 C13 C12 C11 -179.3(2) . . . . ?
N6 C11 C12 C13 -1.6(5) . . . . ?
N5 C11 C12 C13 177.8(3) 2_656 . . . ?
C4 N3 C4 C5 -0.8(3) 2_656 . . . ?
C4 N3 C4 N2 178.2(3) 2_656 . . . ?
C3 N2 C4 N3 -19.9(5) . . . . ?
N1 N2 C4 N3 160.6(3) 2_656 . . . ?
C3 N2 C4 C5 159.1(4) . . . . ?
N1 N2 C4 C5 -20.3(5) 2_656 . . . ?
N3 C4 C5 C6 1.5(5) . . . . ?
N2 C4 C5 C6 -177.4(3) . . . . ?
C5 C6 C5 C4 -0.7(2) 2_656 . . . ?
C7 C6 C5 C4 179.3(2) . . . . ?
N5 N4 C8 C9 0.2(4) 2_656 . . . ?
Mn1 N4 C8 C9 -178.7(3) . . . . ?
N4 C8 C9 C10 -0.3(5) . . . . ?
N1 N2 C3 C2 -1.7(5) 2_656 . . . ?
C4 N2 C3 C2 178.8(4) . . . . ?
N2 C3 C2 C1 1.2(5) . . . . ?
C8 C9 C10 N5 0.2(4) . . . 2_656 ?
C3 C2 C1 N1 -0.3(5) . . . 2_656 ?

_refine_diff_density_max         1.350
_refine_diff_density_min         -0.637
_refine_diff_density_rms         0.114

_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: water,MeOH'
_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_Fe-2
_database_code_depnum_ccdc_archive 'CCDC 1840920'
loop_
_audit_author_name
_audit_author_address
'Goulven Cosquer'
;Tohoku University
Japan
;
_audit_update_record             
;
2018-05-02 deposited with the CCDC.	2019-07-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C26 H24 Fe1 N10 O6'
_chemical_formula_weight         628.40

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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   C2/c

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

_cell_length_a                   17.4762(9)
_cell_length_b                   21.7676(11)
_cell_length_c                   7.0315(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 103.085(5)
_cell_angle_gamma                90.00
_cell_volume                     2605.4(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    4016
_cell_measurement_theta_min      3.4870
_cell_measurement_theta_max      30.5940

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.602
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1296
_exptl_absorpt_coefficient_mu    0.644
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.59032
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.675
_oxdiff_exptl_absorpt_empirical_full_max 1.797
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_diffrn_ambient_temperature      293(2)
_diffrn_source_power             2.0000
_diffrn_source_voltage           50.0000
_diffrn_source_current           40.0000
_diffrn_radiation_wavelength     0.710747
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_detector       CCD
_diffrn_measurement_device       
;
Saturn724+ (4x4 bin mode)
;
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measurement_method       dtprofit.ref
_diffrn_standards_number         5768
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5691
_diffrn_reflns_av_R_equivalents  0.0181
_diffrn_reflns_av_sigmaI/netI    0.0326
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_theta_min         3.51
_diffrn_reflns_theta_max         30.61
_reflns_number_total             3461
_reflns_number_gt                3010
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Crystal Clear'
_computing_cell_refinement       CrystAlisPro
_computing_data_reduction        CrystAlisPro
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0573P)²+1.3576P] 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         3461
_refine_ls_number_parameters     246
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0435
_refine_ls_R_factor_gt           0.0358
_refine_ls_wR_factor_ref         0.0969
_refine_ls_wR_factor_gt          0.0930
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_restrained_S_all      1.035
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
N4 N 0.61257(7) 0.18764(5) 0.93168(19) 0.0156(2) Uani 1 1 d . . .
N2 N 0.63492(7) 0.54441(5) 0.82069(18) 0.0152(2) Uani 1 1 d . . .
N5 N 0.62424(7) 0.12563(5) 0.94142(18) 0.0138(2) Uani 1 1 d . . .
N1 N 0.70621(7) 0.52331(6) 0.9215(2) 0.0222(3) Uani 1 1 d . . .
N3 N 0.5000 0.53909(8) 0.7500 0.0149(3) Uani 1 2 d S . .
N6 N 0.5000 0.11943(7) 0.7500 0.0129(3) Uani 1 2 d S . .
C11 C 0.56249(7) 0.08772(6) 0.8432(2) 0.0129(3) Uani 1 1 d . . .
C12 C 0.56631(8) 0.02410(6) 0.8467(2) 0.0142(3) Uani 1 1 d . . .
C4 C 0.56669(8) 0.50718(6) 0.7877(2) 0.0142(3) Uani 1 1 d . . .
C1 C 0.75348(9) 0.57158(7) 0.9265(3) 0.0228(3) Uani 1 1 d . . .
C14 C 0.5000 -0.07842(9) 0.7500 0.0141(4) Uani 1 2 d S . .
C3 C 0.63840(8) 0.60399(6) 0.7621(2) 0.0178(3) Uani 1 1 d . . .
C5 C 0.57108(8) 0.44309(6) 0.7925(2) 0.0151(3) Uani 1 1 d . . .
C13 C 0.5000 -0.00802(9) 0.7500 0.0131(4) Uani 1 2 d S . .
C9 C 0.72999(8) 0.16519(7) 1.1297(2) 0.0197(3) Uani 1 1 d . . .
C2 C 0.71453(9) 0.62276(7) 0.8284(2) 0.0204(3) Uani 1 1 d . . .
C10 C 0.69487(8) 0.11106(7) 1.0608(2) 0.0178(3) Uani 1 1 d . . .
C8 C 0.67667(8) 0.21148(7) 1.0455(2) 0.0173(3) Uani 1 1 d . . .
Fe1 Fe 0.5000 0.221688(12) 0.7500 0.01318(10) Uani 1 2 d S . .
O1 O 0.43974(6) 0.31319(5) 0.65801(16) 0.0197(2) Uani 1 1 d . . .
C6 C 0.5000 0.41108(9) 0.7500 0.0141(4) Uani 1 2 d S . .
C7 C 0.5000 0.34130(9) 0.7500 0.0150(4) Uani 1 2 d S . .
O2 O 0.55933(6) -0.10401(5) 0.85421(16) 0.0185(2) Uani 1 1 d . . .
O3 O 0.45288(7) 0.21623(5) 1.00415(18) 0.0204(2) Uani 1 1 d . . .
C15 C 0.40605(12) 0.26008(9) 1.0745(3) 0.0304(4) Uani 1 1 d . . .
H2 H 0.7364(10) 0.6630(8) 0.811(3) 0.017(4) Uiso 1 1 d . . .
H8 H 0.6098(11) 0.0031(9) 0.911(3) 0.021(5) Uiso 1 1 d . . .
H1 H 0.5955(11) 0.6227(8) 0.692(3) 0.022(5) Uiso 1 1 d . . .
H5 H 0.6813(11) 0.2551(9) 1.055(3) 0.021(5) Uiso 1 1 d . . .
H4 H 0.6187(11) 0.4221(8) 0.821(3) 0.021(5) Uiso 1 1 d . . .
H6 H 0.7793(13) 0.1706(9) 1.213(3) 0.033(6) Uiso 1 1 d . . .
H3 H 0.8067(12) 0.5686(9) 0.987(3) 0.028(5) Uiso 1 1 d . . .
H7 H 0.7110(12) 0.0694(9) 1.083(3) 0.030(5) Uiso 1 1 d . . .
H10 H 0.4207(13) 0.2607(10) 1.220(3) 0.035(6) Uiso 1 1 d . . .
H9 H 0.4461(14) 0.1859(11) 1.053(4) 0.040(7) Uiso 1 1 d . . .
H11 H 0.4123(14) 0.3002(12) 1.024(4) 0.048(7) Uiso 1 1 d . . .
H12 H 0.3452(17) 0.2489(13) 1.025(4) 0.061(8) Uiso 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N4 C8 1.3263(18) . ?
N4 N5 1.3647(15) . ?
N4 Fe1 2.2166(12) . ?
N2 N1 1.3659(16) . ?
N2 C3 1.3664(18) . ?
N2 C4 1.4166(17) . ?
N5 C10 1.3636(17) . ?
N5 C11 1.4089(16) . ?
N1 C1 1.332(2) . ?
N3 C4 1.3309(16) 2_656 ?
N3 C4 1.3309(16) . ?
N6 C11 1.3322(15) 2_656 ?
N6 C11 1.3322(15) . ?
N6 Fe1 2.2260(17) . ?
C11 C12 1.3864(19) . ?
C12 C13 1.3919(16) . ?
C4 C5 1.3972(19) . ?
C1 C2 1.403(2) . ?
C14 O2 1.2563(13) 2_656 ?
C14 O2 1.2563(13) . ?
C14 C13 1.533(3) . ?
C3 C2 1.369(2) . ?
C5 C6 1.3964(17) . ?
C13 C12 1.3919(16) 2_656 ?
C9 C10 1.366(2) . ?
C9 C8 1.409(2) . ?
Fe1 O3 2.1336(12) . ?
Fe1 O3 2.1336(12) 2_656 ?
Fe1 N4 2.2166(12) 2_656 ?
Fe1 O1 2.2773(11) 2_656 ?
Fe1 O1 2.2773(10) . ?
O1 C7 1.2624(13) . ?
C6 C5 1.3964(17) 2_656 ?
C6 C7 1.519(3) . ?
C7 O1 1.2623(13) 2_656 ?
O3 C15 1.417(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C8 N4 N5 105.09(11) . . ?
C8 N4 Fe1 137.33(10) . . ?
N5 N4 Fe1 117.57(8) . . ?
N1 N2 C3 112.21(11) . . ?
N1 N2 C4 121.84(12) . . ?
C3 N2 C4 125.94(12) . . ?
C10 N5 N4 111.41(11) . . ?
C10 N5 C11 130.67(12) . . ?
N4 N5 C11 117.74(11) . . ?
C1 N1 N2 103.63(12) . . ?
C4 N3 C4 117.09(17) 2_656 . ?
C11 N6 C11 117.59(16) 2_656 . ?
C11 N6 Fe1 121.21(8) 2_656 . ?
C11 N6 Fe1 121.21(8) . . ?
N6 C11 C12 123.85(13) . . ?
N6 C11 N5 112.91(12) . . ?
C12 C11 N5 123.22(12) . . ?
C11 C12 C13 117.49(13) . . ?
N3 C4 C5 124.51(13) . . ?
N3 C4 N2 113.63(12) . . ?
C5 C4 N2 121.85(12) . . ?
N1 C1 C2 112.61(13) . . ?
O2 C14 O2 127.37(18) 2_656 . ?
O2 C14 C13 116.32(9) 2_656 . ?
O2 C14 C13 116.32(9) . . ?
N2 C3 C2 106.67(12) . . ?
C6 C5 C4 116.87(13) . . ?
C12 C13 C12 119.70(17) . 2_656 ?
C12 C13 C14 120.15(9) . . ?
C12 C13 C14 120.15(9) 2_656 . ?
C10 C9 C8 105.46(12) . . ?
C3 C2 C1 104.87(13) . . ?
N5 C10 C9 106.82(13) . . ?
N4 C8 C9 111.21(13) . . ?
O3 Fe1 O3 173.62(6) . 2_656 ?
O3 Fe1 N4 90.21(5) . 2_656 ?
O3 Fe1 N4 87.66(5) 2_656 2_656 ?
O3 Fe1 N4 87.66(5) . . ?
O3 Fe1 N4 90.21(5) 2_656 . ?
N4 Fe1 N4 140.94(6) 2_656 . ?
O3 Fe1 N6 86.81(3) . . ?
O3 Fe1 N6 86.81(3) 2_656 . ?
N4 Fe1 N6 70.47(3) 2_656 . ?
N4 Fe1 N6 70.47(3) . . ?
O3 Fe1 O1 92.99(4) . 2_656 ?
O3 Fe1 O1 92.59(4) 2_656 2_656 ?
N4 Fe1 O1 138.52(4) 2_656 2_656 ?
N4 Fe1 O1 80.54(4) . 2_656 ?
N6 Fe1 O1 151.00(3) . 2_656 ?
O3 Fe1 O1 92.59(4) . . ?
O3 Fe1 O1 92.99(4) 2_656 . ?
N4 Fe1 O1 80.54(4) 2_656 . ?
N4 Fe1 O1 138.52(4) . . ?
N6 Fe1 O1 151.00(3) . . ?
O1 Fe1 O1 58.00(5) 2_656 . ?
C7 O1 Fe1 89.99(9) . . ?
C5 C6 C5 120.12(18) . 2_656 ?
C5 C6 C7 119.94(9) . . ?
C5 C6 C7 119.94(9) 2_656 . ?
O1 C7 O1 122.01(18) 2_656 . ?
O1 C7 C6 118.99(9) 2_656 . ?
O1 C7 C6 118.99(9) . . ?
C15 O3 Fe1 128.15(11) . . ?

_diffrn_measured_fraction_theta_max 0.8626
_diffrn_reflns_theta_full        30.5456
_diffrn_measured_fraction_theta_full 0.8626
_refine_diff_density_max         0.433
_refine_diff_density_min         -0.360
_refine_diff_density_rms         0.065
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: water,MeOH'
_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_Co-3
_database_code_depnum_ccdc_archive 'CCDC 1840921'
loop_
_audit_author_name
_audit_author_address
'Goulven Cosquer'
;Tohoku University
Japan
;
_audit_update_record             
;
2018-05-02 deposited with the CCDC.	2019-07-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C26 H24 Co1 N10 O6'
_chemical_formula_weight         631.48

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'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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, -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                   17.5740(12)
_cell_length_b                   21.7514(13)
_cell_length_c                   7.0063(5)
_cell_angle_alpha                90
_cell_angle_beta                 103.552(7)
_cell_angle_gamma                90
_cell_volume                     2603.7(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    4027
_cell_measurement_theta_min      3.5070
_cell_measurement_theta_max      30.6840

_exptl_crystal_description       needle
_exptl_crystal_colour            pink
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.611
_exptl_crystal_F_000             1300
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    0.724
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.710747
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_detector       CCD
_diffrn_measurement_device       
;
Saturn724+ (4x4 bin mode)
;
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measurement_method       dtprofit.ref
_diffrn_reflns_number            7384
_diffrn_reflns_av_unetI/netI     0.0368
_diffrn_reflns_av_R_equivalents  0.0279
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         1.872
_diffrn_reflns_theta_max         30.780
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.838
_diffrn_measured_fraction_theta_full 0.958
_diffrn_reflns_Laue_measured_fraction_max 0.838
_diffrn_reflns_Laue_measured_fraction_full 0.958
_diffrn_reflns_point_group_measured_fraction_max 0.838
_diffrn_reflns_point_group_measured_fraction_full 0.958
_reflns_number_total             3419
_reflns_number_gt                2829
_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       'Crystal Clear'
_computing_cell_refinement       CrystAlisPro
_computing_data_reduction        CrystAlisPro
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0632P)²+3.3084P] 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         3419
_refine_ls_number_parameters     198
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0568
_refine_ls_R_factor_gt           0.0426
_refine_ls_wR_factor_ref         0.1193
_refine_ls_wR_factor_gt          0.1114
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_restrained_S_all      1.052
_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
Co1 Co 0.5000 0.22095(2) 0.7500 0.01760(13) Uani 1 2 d S T P . .
O2 O 0.44155(8) -0.10269(6) 0.6421(2) 0.0246(3) Uani 1 1 d . . . . .
O1 O 0.56044(10) 0.31181(7) 0.8361(2) 0.0316(4) Uani 1 1 d . . . . .
N6 N 0.5000 0.12026(10) 0.7500 0.0172(4) Uani 1 2 d S T P . .
O3 O 0.45704(9) 0.21581(6) 1.0080(2) 0.0248(3) Uani 1 1 d . . . . .
H9 H 0.4757 0.1826 1.0943 0.030 Uiso 1 1 calc R U . . .
N3 N 0.5000 0.53731(10) 0.7500 0.0204(5) Uani 1 2 d S T P . .
N4 N 0.38782(10) 0.18877(7) 0.5708(3) 0.0211(3) Uani 1 1 d . . . . .
N2 N 0.63437(10) 0.54299(7) 0.8192(3) 0.0227(4) Uani 1 1 d . . . . .
C11 C 0.43751(10) 0.08865(8) 0.6569(3) 0.0168(4) Uani 1 1 d . . . . .
C14 C 0.5000 -0.07726(11) 0.7500 0.0184(5) Uani 1 2 d S T P . .
C7 C 0.5000 0.33931(12) 0.7500 0.0233(6) Uani 1 2 d S T P . .
C12 C 0.43355(11) 0.02513(8) 0.6533(3) 0.0185(4) Uani 1 1 d . . . . .
H8 H 0.3874 0.0042 0.5875 0.022 Uiso 1 1 calc R U . . .
C13 C 0.5000 -0.00684(11) 0.7500 0.0177(5) Uani 1 2 d S T P . .
C4 C 0.56656(11) 0.50538(9) 0.7869(3) 0.0207(4) Uani 1 1 d . . . . .
C6 C 0.5000 0.40953(12) 0.7500 0.0211(5) Uani 1 2 d S T P . .
C9 C 0.27046(12) 0.16705(9) 0.3705(3) 0.0270(5) Uani 1 1 d . . . . .
H6 H 0.2206 0.1728 0.2837 0.032 Uiso 1 1 calc R U . . .
C8 C 0.32412(12) 0.21293(9) 0.4570(3) 0.0231(4) Uani 1 1 d . . . . .
H5 H 0.3156 0.2558 0.4361 0.028 Uiso 1 1 calc R U . . .
C5 C 0.57099(12) 0.44168(9) 0.7913(3) 0.0221(4) Uani 1 1 d . . . . .
H4 H 0.6199 0.4209 0.8210 0.027 Uiso 1 1 calc R U . . .
C10 C 0.30518(12) 0.11257(9) 0.4377(3) 0.0242(4) Uani 1 1 d . . . . .
H7 H 0.2843 0.0726 0.4063 0.029 Uiso 1 1 calc R U . . .
C2 C 0.71259(13) 0.62223(10) 0.8312(4) 0.0310(5) Uani 1 1 d . . . . .
H2 H 0.7333 0.6620 0.8193 0.037 Uiso 1 1 calc R U . . .
C3 C 0.63655(13) 0.60342(9) 0.7698(4) 0.0280(5) Uani 1 1 d . . . . .
H3 H 0.5934 0.6279 0.7049 0.034 Uiso 1 1 calc R U . . .
C1 C 0.75295(13) 0.57026(10) 0.9150(4) 0.0340(5) Uani 1 1 d . . . . .
H1 H 0.8077 0.5696 0.9711 0.041 Uiso 1 1 calc R U . . .
C15 C 0.40394(16) 0.25620(12) 1.0656(4) 0.0394(6) Uani 1 1 d . . . . .
H12 H 0.3945 0.2427 1.1915 0.059 Uiso 1 1 calc R U . . .
H10 H 0.4259 0.2978 1.0796 0.059 Uiso 1 1 calc R U . . .
H11 H 0.3544 0.2562 0.9659 0.059 Uiso 1 1 calc R U . . .
N5 N 0.62417(9) 0.12680(7) 0.9412(2) 0.0186(3) Uani 1 1 d . . . . .
N1 N 0.29332(11) 0.52148(9) 0.5917(3) 0.0333(5) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 O3 2.1186(15) 2_656 ?
Co1 O3 2.1186(15) . ?
Co1 N4 2.1892(17) 2_656 ?
Co1 N4 2.1892(17) . ?
Co1 N6 2.190(2) . ?
Co1 O1 2.2578(15) . ?
Co1 O1 2.2578(15) 2_656 ?
O2 C14 1.2525(18) . ?
O1 C7 1.245(2) . ?
N6 C11 1.330(2) 2_656 ?
N6 C11 1.330(2) . ?
O3 C15 1.408(3) . ?
O3 H9 0.9500 . ?
N3 C4 1.333(2) . ?
N3 C4 1.333(2) 2_656 ?
N4 C8 1.322(3) . ?
N4 N5 1.364(2) 2_656 ?
N2 N1 1.361(2) 2_656 ?
N2 C3 1.362(2) . ?
N2 C4 1.419(2) . ?
C11 C12 1.383(2) . ?
C11 N5 1.410(2) 2_656 ?
C14 O2 1.2525(18) 2_656 ?
C14 C13 1.532(3) . ?
C7 O1 1.245(2) 2_656 ?
C7 C6 1.527(4) . ?
C12 C13 1.391(2) . ?
C12 H8 0.9500 . ?
C13 C12 1.391(2) 2_656 ?
C4 C5 1.388(3) . ?
C6 C5 1.400(2) . ?
C6 C5 1.400(2) 2_656 ?
C9 C10 1.365(3) . ?
C9 C8 1.409(3) . ?
C9 H6 0.9500 . ?
C8 H5 0.9500 . ?
C5 H4 0.9500 . ?
C10 N5 1.365(3) 2_656 ?
C10 H7 0.9500 . ?
C2 C3 1.367(3) . ?
C2 C1 1.389(3) . ?
C2 H2 0.9500 . ?
C3 H3 0.9500 . ?
C1 N1 1.331(3) 2_656 ?
C1 H1 0.9500 . ?
C15 H12 0.9800 . ?
C15 H10 0.9800 . ?
C15 H11 0.9800 . ?
N5 N4 1.364(2) 2_656 ?
N5 C10 1.365(3) 2_656 ?
N5 C11 1.410(2) 2_656 ?
N1 C1 1.331(3) 2_656 ?
N1 N2 1.361(2) 2_656 ?

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
O3 Co1 O3 173.95(7) 2_656 . ?
O3 Co1 N4 91.12(6) 2_656 2_656 ?
O3 Co1 N4 86.95(6) . 2_656 ?
O3 Co1 N4 86.95(6) 2_656 . ?
O3 Co1 N4 91.11(6) . . ?
N4 Co1 N4 142.71(8) 2_656 . ?
O3 Co1 N6 86.98(4) 2_656 . ?
O3 Co1 N6 86.98(4) . . ?
N4 Co1 N6 71.36(4) 2_656 . ?
N4 Co1 N6 71.36(4) . . ?
O3 Co1 O1 92.00(6) 2_656 . ?
O3 Co1 O1 93.30(6) . . ?
N4 Co1 O1 79.78(6) 2_656 . ?
N4 Co1 O1 137.49(6) . . ?
N6 Co1 O1 151.08(4) . . ?
O3 Co1 O1 93.30(6) 2_656 2_656 ?
O3 Co1 O1 91.99(6) . 2_656 ?
N4 Co1 O1 137.49(6) 2_656 2_656 ?
N4 Co1 O1 79.78(6) . 2_656 ?
N6 Co1 O1 151.08(4) . 2_656 ?
O1 Co1 O1 57.83(8) . 2_656 ?
C7 O1 Co1 89.80(14) . . ?
C11 N6 C11 117.7(2) 2_656 . ?
C11 N6 Co1 121.14(11) 2_656 . ?
C11 N6 Co1 121.13(11) . . ?
C15 O3 Co1 127.19(14) . . ?
C15 O3 H9 116.4 . . ?
Co1 O3 H9 116.4 . . ?
C4 N3 C4 117.2(2) . 2_656 ?
C8 N4 N5 105.01(16) . 2_656 ?
C8 N4 Co1 137.78(13) . . ?
N5 N4 Co1 117.17(12) 2_656 . ?
N1 N2 C3 111.68(17) 2_656 . ?
N1 N2 C4 122.27(16) 2_656 . ?
C3 N2 C4 126.04(17) . . ?
N6 C11 C12 123.89(18) . . ?
N6 C11 N5 112.77(16) . 2_656 ?
C12 C11 N5 123.32(17) . 2_656 ?
O2 C14 O2 127.6(2) . 2_656 ?
O2 C14 C13 116.20(12) . . ?
O2 C14 C13 116.20(12) 2_656 . ?
O1 C7 O1 122.6(3) . 2_656 ?
O1 C7 C6 118.72(13) . . ?
O1 C7 C6 118.72(13) 2_656 . ?
C11 C12 C13 117.21(18) . . ?
C11 C12 H8 121.4 . . ?
C13 C12 H8 121.4 . . ?
C12 C13 C12 120.0(2) . 2_656 ?
C12 C13 C14 119.98(11) . . ?
C12 C13 C14 119.99(11) 2_656 . ?
N3 C4 C5 124.53(19) . . ?
N3 C4 N2 113.36(17) . . ?
C5 C4 N2 122.10(18) . . ?
C5 C6 C5 120.1(2) . 2_656 ?
C5 C6 C7 119.97(12) . . ?
C5 C6 C7 119.97(12) 2_656 . ?
C10 C9 C8 105.46(18) . . ?
C10 C9 H6 127.3 . . ?
C8 C9 H6 127.3 . . ?
N4 C8 C9 111.40(17) . . ?
N4 C8 H5 124.3 . . ?
C9 C8 H5 124.3 . . ?
C4 C5 C6 116.84(19) . . ?
C4 C5 H4 121.6 . . ?
C6 C5 H4 121.6 . . ?
C9 C10 N5 106.57(17) . 2_656 ?
C9 C10 H7 126.7 . . ?
N5 C10 H7 126.7 2_656 . ?
C3 C2 C1 104.71(19) . . ?
C3 C2 H2 127.6 . . ?
C1 C2 H2 127.6 . . ?
N2 C3 C2 107.01(19) . . ?
N2 C3 H3 126.5 . . ?
C2 C3 H3 126.5 . . ?
N1 C1 C2 112.7(2) 2_656 . ?
N1 C1 H1 123.6 2_656 . ?
C2 C1 H1 123.6 . . ?
O3 C15 H12 109.5 . . ?
O3 C15 H10 109.5 . . ?
H12 C15 H10 109.5 . . ?
O3 C15 H11 109.5 . . ?
H12 C15 H11 109.5 . . ?
H10 C15 H11 109.5 . . ?
N4 N5 C10 111.56(15) 2_656 2_656 ?
N4 N5 C11 117.50(15) 2_656 2_656 ?
C10 N5 C11 130.77(16) 2_656 2_656 ?
C1 N1 N2 103.85(17) 2_656 2_656 ?

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
C11 N6 C11 C12 0.74(14) 2_656 . . . ?
Co1 N6 C11 C12 -179.26(14) . . . . ?
C11 N6 C11 N5 -178.19(18) 2_656 . . 2_656 ?
Co1 N6 C11 N5 1.81(18) . . . 2_656 ?
Co1 O1 C7 O1 0.002(1) . . . 2_656 ?
Co1 O1 C7 C6 180.000(0) . . . . ?
N6 C11 C12 C13 -1.4(3) . . . . ?
N5 C11 C12 C13 177.40(15) 2_656 . . . ?
C11 C12 C13 C12 0.65(12) . . . 2_656 ?
C11 C12 C13 C14 -179.35(12) . . . . ?
O2 C14 C13 C12 7.72(12) . . . . ?
O2 C14 C13 C12 -172.28(12) 2_656 . . . ?
O2 C14 C13 C12 -172.28(12) . . . 2_656 ?
O2 C14 C13 C12 7.72(12) 2_656 . . 2_656 ?
C4 N3 C4 C5 -0.70(15) 2_656 . . . ?
C4 N3 C4 N2 178.38(19) 2_656 . . . ?
N1 N2 C4 N3 162.31(18) 2_656 . . . ?
C3 N2 C4 N3 -17.0(3) . . . . ?
N1 N2 C4 C5 -18.6(3) 2_656 . . . ?
C3 N2 C4 C5 162.1(2) . . . . ?
O1 C7 C6 C5 19.08(13) . . . . ?
O1 C7 C6 C5 -160.93(13) 2_656 . . . ?
O1 C7 C6 C5 -160.92(13) . . . 2_656 ?
O1 C7 C6 C5 19.08(13) 2_656 . . 2_656 ?
N5 N4 C8 C9 0.0(2) 2_656 . . . ?
Co1 N4 C8 C9 177.38(16) . . . . ?
C10 C9 C8 N4 -0.2(3) . . . . ?
N3 C4 C5 C6 1.3(3) . . . . ?
N2 C4 C5 C6 -177.67(16) . . . . ?
C5 C6 C5 C4 -0.61(13) 2_656 . . . ?
C7 C6 C5 C4 179.40(13) . . . . ?
C8 C9 C10 N5 0.3(3) . . . 2_656 ?
N1 N2 C3 C2 -0.9(3) 2_656 . . . ?
C4 N2 C3 C2 178.5(2) . . . . ?
C1 C2 C3 N2 0.5(3) . . . . ?
C3 C2 C1 N1 0.1(3) . . . 2_656 ?

_refine_diff_density_max         0.509
_refine_diff_density_min         -0.636
_refine_diff_density_rms         0.069



_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: water,MeOH'
_exptl_crystal_preparation       'Magnetic properties'
