# Electronic Supplementary Material (ESI) for Inorganic Chemistry Frontiers.
# This journal is © the Partner Organisations 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_LiCo
_database_code_depnum_ccdc_archive 'CCDC 1476207'
_audit_update_record             
;
2016-04-24 deposited with the CCDC.
2016-10-13 downloaded from the CCDC.
;
#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_formula_sum            'C112 H82 Co8 Li8 N16 O81'
_chemical_formula_weight         3474.90

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

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'I 2/a'
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_Int_Tables_number      15
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'

_cell_length_a                   21.3041(3)
_cell_length_b                   14.3738(2)
_cell_length_c                   21.3818(3)
_cell_angle_alpha                90
_cell_angle_beta                 92.286(10)
_cell_angle_gamma                90
_cell_volume                     6542.34(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    173.0(2)
_cell_measurement_reflns_used    8240
_cell_measurement_theta_min      2.532
_cell_measurement_theta_max      25.242

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

_exptl_crystal_density_diffrn    1.764
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3508
_exptl_crystal_description       Rod
_exptl_crystal_colour            Violet
_exptl_crystal_size_max          0.133
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.020
_exptl_special_details           
;
 ?
;
#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    1.112
_exptl_absorpt_correction_type   EMPIRICAL
_exptl_absorpt_process_details   
; 
 SADABS(Blessing, 1995) 
;
_exptl_absorpt_correction_T_min  0.82
_exptl_absorpt_correction_T_max  0.98

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

_diffrn_measurement_device_type  'Bruker SMART BREEZE'
_diffrn_measurement_method       CCD
_diffrn_ambient_temperature      173.0(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_probe          x-ray
_diffrn_reflns_av_R_equivalents  0.0999
_diffrn_reflns_number            73440
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         2.532
_diffrn_reflns_theta_max         28.449
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_reflns_number_total             8240
_reflns_number_gt                5128
_reflns_threshold_expression     'I > 2σ(I)'

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

_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'

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

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   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)+(0.0344P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_coef       0.000070(19)
_refine_ls_number_reflns         8240
_refine_ls_number_parameters     555
_refine_ls_number_restraints     3
_refine_ls_number_constraints    0
_refine_ls_R_factor_all          0.0739
_refine_ls_R_factor_gt           0.037
_refine_ls_wR_factor_ref         0.0832
_refine_ls_wR_factor_gt          0.0738
_refine_ls_goodness_of_fit_ref   0.869
_refine_ls_restrained_S_all      0.868
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.463
_refine_diff_density_min         -0.564
_refine_diff_density_rms         0.077

#----------------------------------------------------------------------------#
#                   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
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'
Li Li -0.0003 0.0001 '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'
Co Co 0.3494 0.9721 '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_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.24447(2) 0.50030(2) 0.24530(2) 0.01668(8) Uani 1 d . .
Co2 Co 0.00314(2) 0.75313(2) 0.00716(2) 0.01579(8) Uani 1 d . .
O1 O 0.16342(8) 0.44294(11) 0.23861(7) 0.0207(4) Uani 1 d . .
O2 O 0.06449(8) 0.46079(13) 0.26694(8) 0.0317(5) Uani 1 d . .
O3 O 0.31540(8) 0.57983(11) 0.26302(7) 0.0211(4) Uani 1 d . .
O4 O 0.34054(8) 0.71537(13) 0.30949(8) 0.0298(4) Uani 1 d . .
O5 O 0.23288(8) 0.55646(11) 0.16427(7) 0.0210(4) Uani 1 d . .
O6 O 0.26404(8) 0.54112(13) 0.06626(7) 0.0266(4) Uani 1 d . .
O7 O 0.26705(8) 0.42219(11) 0.31584(7) 0.0190(4) Uani 1 d . .
O8 O 0.31711(8) 0.28862(12) 0.33964(7) 0.0267(4) Uani 1 d . .
O9 O -0.00471(8) 0.78663(12) -0.07993(7) 0.0227(4) Uani 1 d . .
O10 O -0.03524(9) 0.72489(14) -0.17270(8) 0.0325(5) Uani 1 d . .
O11 O -0.00022(8) 0.69445(12) 0.08722(7) 0.0226(4) Uani 1 d . .
O12 O -0.03929(10) 0.57097(14) 0.13448(9) 0.0392(5) Uani 1 d . .
O13 O 0.08291(8) 0.69871(11) -0.00610(7) 0.0212(4) Uani 1 d . .
O14 O 0.18534(8) 0.72366(13) 0.01340(8) 0.0295(4) Uani 1 d . .
O15 O -0.06619(7) 0.83211(11) 0.02763(7) 0.0189(4) Uani 1 d . .
O16 O -0.08610(8) 0.96972(12) 0.07221(8) 0.0258(4) Uani 1 d . .
OW1 O 0.31659(9) 0.29148(15) 0.46979(10) 0.0291(5) Uani 1 d . .
OW2 O 0.46991(13) 0.70681(19) 0.30381(10) 0.0475(6) Uani 1 d . .
OW3 O -0.06977(10) 0.41506(15) 0.19828(10) 0.0397(5) Uani 1 d . .
OW4 O -0.21573(10) 0.94571(15) 0.06721(9) 0.0294(5) Uani 1 d . .
OW5 O 0.0612(3) 1.0980(5) 0.2217(3) 0.0281(17) Uani 0.25 d . .
N1 N 0.20206(9) 0.58902(13) 0.28907(8) 0.0170(4) Uani 1 d . .
N2 N 0.28553(9) 0.41032(13) 0.20143(8) 0.0158(4) Uani 1 d . .
N3 N -0.04254(9) 0.65096(14) -0.01892(9) 0.0180(4) Uani 1 d . .
N4 N 0.05056(9) 0.85190(13) 0.03663(8) 0.0157(4) Uani 1 d . .
Li1 Li 0.25 0.6324(4) 0 0.0212(13) Uani 1 d . .
Li2 Li -0.25 0.8687(5) 0 0.0271(15) Uani 1 d . .
Li3 Li 0.5051(2) 0.6385(4) 0.2390(2) 0.0329(12) Uani 1 d . .
C1 C 0.14064(12) 0.57741(17) 0.29637(11) 0.0195(5) Uani 1 d . .
C2 C 0.10777(13) 0.64290(18) 0.32864(11) 0.0260(6) Uani 1 d . .
H2 H 0.0649 0.6364 0.334 0.031 Uiso 1 calc . .
C3 C 0.14060(13) 0.71924(19) 0.35297(11) 0.0273(6) Uani 1 d . .
H3 H 0.1193 0.7643 0.3751 0.033 Uiso 1 calc . .
C4 C 0.20472(13) 0.72944(18) 0.34481(11) 0.0251(6) Uani 1 d . .
H4 H 0.2266 0.7804 0.3613 0.03 Uiso 1 calc . .
C5 C 0.23492(12) 0.66148(17) 0.31144(10) 0.0197(5) Uani 1 d . .
C6 C 0.11902(12) 0.48784(18) 0.26594(11) 0.0218(6) Uani 1 d . .
C7 C 0.30247(12) 0.65490(18) 0.29444(11) 0.0219(6) Uani 1 d . .
C8 C 0.28718(11) 0.41976(17) 0.13983(10) 0.0175(5) Uani 1 d . .
C9 C 0.31289(12) 0.34952(17) 0.10471(11) 0.0210(5) Uani 1 d . .
H9 H 0.3133 0.3536 0.0613 0.025 Uiso 1 calc . .
C10 C 0.33818(12) 0.27242(18) 0.13626(11) 0.0234(6) Uani 1 d . .
H10 H 0.3558 0.2245 0.1136 0.028 Uiso 1 calc . .
C11 C 0.33740(12) 0.26630(17) 0.20113(11) 0.0219(6) Uani 1 d . .
H11 H 0.3555 0.216 0.2224 0.026 Uiso 1 calc . .
C12 C 0.30899(11) 0.33733(17) 0.23284(10) 0.0176(5) Uani 1 d . .
C13 C 0.25979(11) 0.51215(17) 0.11977(11) 0.0204(5) Uani 1 d . .
C14 C 0.29840(11) 0.34657(17) 0.30194(10) 0.0187(5) Uani 1 d . .
C15 C -0.05770(11) 0.64266(18) -0.07960(11) 0.0208(6) Uani 1 d . .
C16 C -0.09225(12) 0.56606(19) -0.10002(12) 0.0297(7) Uani 1 d . .
H16 H -0.1041 0.5588 -0.1421 0.036 Uiso 1 calc . .
C17 C -0.10878(12) 0.5004(2) -0.05606(13) 0.0305(6) Uani 1 d . .
H17 H -0.1319 0.4484 -0.0689 0.037 Uiso 1 calc . .
C18 C -0.09158(12) 0.51094(18) 0.00612(13) 0.0266(6) Uani 1 d . .
H18 H -0.1027 0.4666 0.0354 0.032 Uiso 1 calc . .
C19 C -0.05756(11) 0.58853(17) 0.02413(11) 0.0203(5) Uani 1 d . .
C20 C -0.03188(12) 0.72306(19) -0.11544(11) 0.0245(6) Uani 1 d . .
C21 C -0.03140(12) 0.61672(19) 0.08748(12) 0.0242(6) Uani 1 d . .
C22 C 0.11270(11) 0.84323(17) 0.03811(10) 0.0185(5) Uani 1 d . .
C23 C 0.14973(12) 0.91446(18) 0.06204(11) 0.0230(6) Uani 1 d . .
H23 H 0.1933 0.9109 0.062 0.028 Uiso 1 calc . .
C24 C 0.12003(12) 0.99182(18) 0.08628(11) 0.0241(6) Uani 1 d . .
H24 H 0.1441 1.0407 0.1027 0.029 Uiso 1 calc . .
C25 C 0.05474(12) 0.99704(17) 0.08638(11) 0.0217(5) Uani 1 d . .
H25 H 0.0349 1.048 0.1037 0.026 Uiso 1 calc . .
C26 C 0.02041(11) 0.92463(17) 0.06014(10) 0.0176(5) Uani 1 d . .
C27 C 0.13047(12) 0.74915(18) 0.01342(11) 0.0209(5) Uani 1 d . .
C28 C -0.04956(11) 0.91128(17) 0.05419(10) 0.0187(5) Uani 1 d . .
H111 H 0.3500(13) 0.3050(19) 0.4826(12) 0.028(9) Uiso 1 d . .
H112 H 0.3176(15) 0.292(2) 0.4315(16) 0.053(11) Uiso 1 d . .
H211 H 0.483(2) 0.754(3) 0.331(2) 0.14(2) Uiso 1 d . .
H212 H 0.431(2) 0.689(3) 0.306(2) 0.12(2) Uiso 1 d . .
H311 H -0.065(3) 0.480(4) 0.176(3) 0.18(2) Uiso 1 d . .
H312 H -0.058(3) 0.442(5) 0.253(3) 0.22(3) Uiso 1 d . .
H411 H -0.1774(19) 0.960(3) 0.0689(17) 0.074(13) Uiso 1 d . .
H412 H -0.2292(15) 0.936(2) 0.1048(16) 0.052(10) Uiso 1 d . .
H511 H 0.033(3) 1.077(5) 0.243(4) 0.013(19) Uiso 0.25 d . .
H512 H 0.053(4) 1.1544(17) 0.216(4) 0.013(19) Uiso 0.25 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
Co1 N2 1.8395(19) . ?
Co1 N1 1.8400(19) . ?
Co1 O1 1.9136(17) . ?
Co1 O5 1.9183(15) . ?
Co1 O3 1.9205(17) . ?
Co1 O7 1.9260(16) . ?
Co2 N3 1.8360(19) . ?
Co2 N4 1.8393(19) . ?
Co2 O13 1.9023(17) . ?
Co2 O11 1.9123(16) . ?
Co2 O9 1.9243(16) . ?
Co2 O15 1.9270(16) . ?
O1 C6 1.303(3) . ?
O2 C6 1.226(3) . ?
O2 Li3 1.984(5) 6_565 ?
O3 C7 1.306(3) . ?
O4 C7 1.223(3) . ?
O5 C13 1.297(3) . ?
O6 C13 1.224(3) . ?
O6 Li1 1.945(4) . ?
O7 C14 1.316(3) . ?
O8 C14 1.215(3) . ?
O9 C20 1.308(3) . ?
O10 C20 1.224(3) . ?
O10 Li3 2.008(5) 2 ?
O11 C21 1.300(3) . ?
O12 C21 1.218(3) . ?
O13 C27 1.301(3) . ?
O14 C27 1.225(3) . ?
O14 Li1 1.932(4) . ?
O15 C28 1.314(3) . ?
O16 C28 1.218(3) . ?
OW1 Li2 1.932(4) 3_545 ?
OW2 Li3 1.879(5) . ?
OW3 Li3 1.945(5) 6_565 ?
OW4 Li2 1.934(4) . ?
N1 C5 1.333(3) . ?
N1 C1 1.335(3) . ?
N2 C8 1.326(3) . ?
N2 C12 1.332(3) . ?
N3 C15 1.330(3) . ?
N3 C19 1.333(3) . ?
N4 C22 1.329(3) . ?
N4 C26 1.336(3) . ?
Li1 O14 1.932(4) 2 ?
Li1 O6 1.945(4) 2 ?
Li2 OW1 1.932(4) 4_455 ?
Li2 OW1 1.932(4) 3_454 ?
Li2 OW4 1.934(4) 2_455 ?
Li3 OW3 1.945(5) 6_665 ?
Li3 O2 1.984(5) 6_665 ?
Li3 O10 2.009(5) 2 ?
C1 C2 1.375(3) . ?
C1 C6 1.506(3) . ?
C2 C3 1.391(4) . ?
C3 C4 1.392(4) . ?
C4 C5 1.383(3) . ?
C5 C7 1.501(4) . ?
C8 C9 1.384(3) . ?
C8 C13 1.506(3) . ?
C9 C10 1.394(3) . ?
C10 C11 1.391(3) . ?
C11 C12 1.379(3) . ?
C12 C14 1.510(3) . ?
C15 C16 1.385(3) . ?
C15 C20 1.503(4) . ?
C16 C17 1.387(4) . ?
C17 C18 1.373(4) . ?
C18 C19 1.377(3) . ?
C19 C21 1.500(3) . ?
C22 C23 1.379(3) . ?
C22 C27 1.506(3) . ?
C23 C24 1.390(3) . ?
C24 C25 1.393(3) . ?
C25 C26 1.378(3) . ?
C26 C28 1.503(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

N2 Co1 N1 178.95(9) . . ?
N2 Co1 O1 96.03(8) . . ?
N1 Co1 O1 82.92(8) . . ?
N2 Co1 O5 83.22(8) . . ?
N1 Co1 O5 96.87(8) . . ?
O1 Co1 O5 91.75(7) . . ?
N2 Co1 O3 97.62(8) . . ?
N1 Co1 O3 83.43(8) . . ?
O1 Co1 O3 166.35(7) . . ?
O5 Co1 O3 89.98(7) . . ?
N2 Co1 O7 83.13(7) . . ?
N1 Co1 O7 96.78(7) . . ?
O1 Co1 O7 90.21(7) . . ?
O5 Co1 O7 166.35(7) . . ?
O3 Co1 O7 91.29(7) . . ?
N3 Co2 N4 177.07(8) . . ?
N3 Co2 O13 95.26(8) . . ?
N4 Co2 O13 83.49(8) . . ?
N3 Co2 O11 83.15(8) . . ?
N4 Co2 O11 94.21(8) . . ?
O13 Co2 O11 91.01(7) . . ?
N3 Co2 O9 83.21(8) . . ?
N4 Co2 O9 99.42(8) . . ?
O13 Co2 O9 90.13(7) . . ?
O11 Co2 O9 166.36(7) . . ?
N3 Co2 O15 97.96(8) . . ?
N4 Co2 O15 83.28(8) . . ?
O13 Co2 O15 166.77(7) . . ?
O11 Co2 O15 90.01(7) . . ?
O9 Co2 O15 91.99(7) . . ?
C6 O1 Co1 114.97(15) . . ?
C6 O2 Li3 144.7(2) . 6_565 ?
C7 O3 Co1 114.37(16) . . ?
C13 O5 Co1 114.27(15) . . ?
C13 O6 Li1 153.5(2) . . ?
C14 O7 Co1 114.70(14) . . ?
C20 O9 Co2 113.96(15) . . ?
C20 O10 Li3 133.2(2) . 2 ?
C21 O11 Co2 114.85(15) . . ?
C27 O13 Co2 114.34(15) . . ?
C27 O14 Li1 152.8(2) . . ?
C28 O15 Co2 114.37(15) . . ?
C5 N1 C1 124.0(2) . . ?
C5 N1 Co1 117.56(17) . . ?
C1 N1 Co1 118.46(16) . . ?
C8 N2 C12 123.9(2) . . ?
C8 N2 Co1 117.81(16) . . ?
C12 N2 Co1 118.24(15) . . ?
C15 N3 C19 123.9(2) . . ?
C15 N3 Co2 118.24(17) . . ?
C19 N3 Co2 117.87(15) . . ?
C22 N4 C26 123.9(2) . . ?
C22 N4 Co2 117.97(16) . . ?
C26 N4 Co2 117.85(16) . . ?
O14 Li1 O14 94.4(3) 2 . ?
O14 Li1 O6 118.44(7) 2 . ?
O14 Li1 O6 116.09(7) . . ?
O14 Li1 O6 116.09(8) 2 2 ?
O14 Li1 O6 118.44(7) . 2 ?
O6 Li1 O6 95.2(3) . 2 ?
OW1 Li2 OW1 109.9(3) 4_455 3_454 ?
OW1 Li2 OW4 108.46(9) 4_455 2_455 ?
OW1 Li2 OW4 109.92(9) 3_454 2_455 ?
OW1 Li2 OW4 109.92(9) 4_455 . ?
OW1 Li2 OW4 108.46(9) 3_454 . ?
OW4 Li2 OW4 110.2(3) 2_455 . ?
OW2 Li3 OW3 101.1(2) . 6_665 ?
OW2 Li3 O2 115.0(2) . 6_665 ?
OW3 Li3 O2 110.6(3) 6_665 6_665 ?
OW2 Li3 O10 110.2(3) . 2 ?
OW3 Li3 O10 102.0(2) 6_665 2 ?
O2 Li3 O10 116.1(2) 6_665 2 ?
N1 C1 C2 119.6(2) . . ?
N1 C1 C6 109.9(2) . . ?
C2 C1 C6 130.5(2) . . ?
C1 C2 C3 118.0(2) . . ?
C2 C3 C4 121.2(2) . . ?
C5 C4 C3 118.0(2) . . ?
N1 C5 C4 119.2(2) . . ?
N1 C5 C7 111.0(2) . . ?
C4 C5 C7 129.7(2) . . ?
O2 C6 O1 123.8(2) . . ?
O2 C6 C1 122.5(2) . . ?
O1 C6 C1 113.7(2) . . ?
O4 C7 O3 124.8(2) . . ?
O4 C7 C5 121.6(2) . . ?
O3 C7 C5 113.6(2) . . ?
N2 C8 C9 119.4(2) . . ?
N2 C8 C13 110.4(2) . . ?
C9 C8 C13 130.2(2) . . ?
C8 C9 C10 118.1(2) . . ?
C11 C10 C9 120.9(2) . . ?
C12 C11 C10 117.8(2) . . ?
N2 C12 C11 119.9(2) . . ?
N2 C12 C14 110.9(2) . . ?
C11 C12 C14 129.2(2) . . ?
O6 C13 O5 124.7(2) . . ?
O6 C13 C8 121.6(2) . . ?
O5 C13 C8 113.7(2) . . ?
O8 C14 O7 124.9(2) . . ?
O8 C14 C12 122.1(2) . . ?
O7 C14 C12 113.0(2) . . ?
N3 C15 C16 119.0(2) . . ?
N3 C15 C20 110.4(2) . . ?
C16 C15 C20 130.6(2) . . ?
C15 C16 C17 118.2(2) . . ?
C18 C17 C16 121.1(3) . . ?
C17 C18 C19 118.5(3) . . ?
N3 C19 C18 119.4(2) . . ?
N3 C19 C21 110.5(2) . . ?
C18 C19 C21 130.1(2) . . ?
O10 C20 O9 124.9(3) . . ?
O10 C20 C15 121.2(2) . . ?
O9 C20 C15 113.8(2) . . ?
O12 C21 O11 123.7(2) . . ?
O12 C21 C19 122.7(2) . . ?
O11 C21 C19 113.6(2) . . ?
N4 C22 C23 119.6(2) . . ?
N4 C22 C27 109.9(2) . . ?
C23 C22 C27 130.5(2) . . ?
C22 C23 C24 118.1(2) . . ?
C23 C24 C25 120.9(2) . . ?
C26 C25 C24 118.2(2) . . ?
N4 C26 C25 119.3(2) . . ?
N4 C26 C28 111.0(2) . . ?
C25 C26 C28 129.7(2) . . ?
O14 C27 O13 124.4(2) . . ?
O14 C27 C22 121.5(2) . . ?
O13 C27 C22 114.2(2) . . ?
O16 C28 O15 124.7(2) . . ?
O16 C28 C26 121.9(2) . . ?
O15 C28 C26 113.3(2) . . ?
####################################################################### 
# 
# 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_NaCo
_database_code_depnum_ccdc_archive 'CCDC 1476208'
_audit_update_record             
;
2016-04-24 deposited with the CCDC.
2016-10-13 downloaded from the CCDC.
;
#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_formula_sum            'C14 H10 Co N2 Na O10'
_chemical_formula_weight         448.16

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

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_Int_Tables_number      14
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                   14.0209(10)
_cell_length_b                   9.5023(10)
_cell_length_c                   12.8892(10)
_cell_angle_alpha                90
_cell_angle_beta                 113.564(10)
_cell_angle_gamma                90
_cell_volume                     1574.1(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    173.0(2)
_cell_measurement_reflns_used    3002
_cell_measurement_theta_min      2.666
_cell_measurement_theta_max      25.242

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

_exptl_crystal_density_diffrn    1.891
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             904
_exptl_crystal_description       Rod
_exptl_crystal_colour            Violet
_exptl_crystal_size_max          0.137
_exptl_crystal_size_mid          0.026
_exptl_crystal_size_min          0.026
_exptl_special_details           
;
 ?
;

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

_exptl_absorpt_coefficient_mu    1.184
_exptl_absorpt_correction_type   EMPIRICAL
_exptl_absorpt_process_details   
; 
 SADABS(Blessing, 1995) 
;
_exptl_absorpt_correction_T_min  0.76
_exptl_absorpt_correction_T_max  0.97

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

_diffrn_measurement_device_type  'Bruker SMART BREEZE'
_diffrn_measurement_method       CCD
_diffrn_ambient_temperature      173.0(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_probe          x-ray
_diffrn_reflns_av_R_equivalents  0.073
_diffrn_reflns_number            38746
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.666
_diffrn_reflns_theta_max         28.389
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 1
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 1
_diffrn_reflns_point_group_measured_fraction_max 0.998
_reflns_number_total             3949
_reflns_number_gt                3002
_reflns_threshold_expression     'I > 2σ(I)'

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

_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'

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

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   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)+(0.0370P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_extinction_method     none
_refine_ls_number_reflns         3949
_refine_ls_number_parameters     269
_refine_ls_number_restraints     0
_refine_ls_number_constraints    0
_refine_ls_R_factor_all          0.0458
_refine_ls_R_factor_gt           0.0305
_refine_ls_wR_factor_ref         0.0736
_refine_ls_wR_factor_gt          0.0695
_refine_ls_goodness_of_fit_ref   0.966
_refine_ls_restrained_S_all      0.966
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.38
_refine_diff_density_min         -0.515
_refine_diff_density_rms         0.069

#----------------------------------------------------------------------------#
#                   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
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'
Na Na 0.0362 0.0249 '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'

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_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.75948(2) 0.04479(3) 0.23412(2) 0.01482(8) Uani 1 d . .
Na1 Na 0.76786(6) 0.46056(8) 0.31331(7) 0.02118(18) Uani 1 d . .
O1 O 0.81647(10) 0.22684(14) 0.28873(11) 0.0187(3) Uani 1 d . .
O2 O 0.96361(11) 0.33487(16) 0.39543(12) 0.0262(3) Uani 1 d . .
O3 O 0.73566(10) -0.15051(14) 0.19813(11) 0.0192(3) Uani 1 d . .
O4 O 0.82140(11) -0.35586(15) 0.22623(12) 0.0242(3) Uani 1 d . .
O5 O 0.76499(10) 0.41769(14) 0.59082(11) 0.0181(3) Uani 1 d . .
O6 O 0.66355(11) 0.35657(15) 0.41250(11) 0.0229(3) Uani 1 d . .
O7 O 0.72128(10) 0.01904(15) 0.35914(11) 0.0183(3) Uani 1 d . .
O8 O 0.58510(11) 0.03815(15) 0.40704(11) 0.0228(3) Uani 1 d . .
OW1 O 0.62317(14) 0.4657(2) 0.14692(15) 0.0293(4) Uani 1 d . .
OW2 O 0.82517(14) 0.6172(2) 0.46881(14) 0.0287(4) Uani 1 d . .
N1 N 0.89604(12) -0.01151(18) 0.30776(13) 0.0152(3) Uani 1 d . .
N2 N 0.62415(12) 0.39517(17) 0.66134(13) 0.0150(3) Uani 1 d . .
C1 C 0.96766(14) 0.0861(2) 0.36118(15) 0.0160(4) Uani 1 d . .
C2 C 1.07078(15) 0.0466(2) 0.41654(16) 0.0199(4) Uani 1 d . .
H2 H 1.1222 0.1125 0.4536 0.024 Uiso 1 calc . .
C3 C 1.09487(16) -0.0960(2) 0.41472(16) 0.0227(5) Uani 1 d . .
H3 H 1.1636 -0.1252 0.4508 0.027 Uiso 1 calc . .
C4 C 1.01836(16) -0.1942(2) 0.36033(16) 0.0212(4) Uani 1 d . .
H4 H 1.0345 -0.2891 0.3604 0.025 Uiso 1 calc . .
C5 C 0.91675(15) -0.1469(2) 0.30561(15) 0.0166(4) Uani 1 d . .
C6 C 0.91630(15) 0.2277(2) 0.35000(15) 0.0181(4) Uani 1 d . .
C7 C 0.81888(15) -0.2295(2) 0.23902(15) 0.0177(4) Uani 1 d . .
C8 C 0.59160(14) 0.3550(2) 0.55332(15) 0.0148(4) Uani 1 d . .
C9 C 0.49144(15) 0.3060(2) 0.49786(16) 0.0182(4) Uani 1 d . .
H9 H 0.4667 0.2789 0.4223 0.022 Uiso 1 calc . .
C10 C 0.42806(15) 0.2981(2) 0.55791(17) 0.0201(4) Uani 1 d . .
H10 H 0.3607 0.2635 0.5225 0.024 Uiso 1 calc . .
C11 C 0.46458(15) 0.3415(2) 0.67037(17) 0.0198(4) Uani 1 d . .
H11 H 0.4223 0.3371 0.7104 0.024 Uiso 1 calc . .
C12 C 0.56528(14) 0.3914(2) 0.72081(16) 0.0156(4) Uani 1 d . .
C13 C 0.67698(15) 0.3750(2) 0.51148(16) 0.0170(4) Uani 1 d . .
C14 C 0.62587(15) 0.0520(2) 0.33929(16) 0.0174(4) Uani 1 d . .
HW21 H 0.885(2) 0.633(3) 0.496(2) 0.045(9) Uiso 1 d . .
HW22 H 0.813(3) 0.570(4) 0.509(3) 0.064(12) Uiso 1 d . .
HW12 H 0.633(3) 0.479(3) 0.099(3) 0.059(12) Uiso 1 d . .
HW11 H 0.566(3) 0.476(3) 0.137(3) 0.056(10) Uiso 1 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
Co1 N2 1.8392(15) 4_565 ?
Co1 N1 1.8439(16) . ?
Co1 O7 1.9062(13) . ?
Co1 O3 1.9097(14) . ?
Co1 O5 1.9128(13) 4_565 ?
Co1 O1 1.9175(14) . ?
Na1 OW1 2.2889(18) . ?
Na1 O4 2.3538(17) 1_565 ?
Na1 OW2 2.3646(19) . ?
Na1 O1 2.3811(16) . ?
Na1 O6 2.4988(16) . ?
Na1 O2 2.7852(17) . ?
Na1 C6 2.943(2) . ?
O1 C6 1.304(2) . ?
O2 C6 1.228(2) . ?
O3 C7 1.308(2) . ?
O4 C7 1.215(2) . ?
O4 Na1 2.3538(16) 1_545 ?
O5 C13 1.313(2) . ?
O5 Co1 1.9128(13) 4_566 ?
O6 C13 1.225(2) . ?
O7 C14 1.296(2) . ?
O8 C14 1.227(2) . ?
N1 C5 1.322(3) . ?
N1 C1 1.338(2) . ?
N2 C12 1.333(2) . ?
N2 C8 1.336(2) . ?
N2 Co1 1.8391(15) 4_566 ?
C1 C2 1.384(3) . ?
C1 C6 1.506(3) . ?
C2 C3 1.398(3) . ?
C3 C4 1.383(3) . ?
C4 C5 1.388(3) . ?
C5 C7 1.514(3) . ?
C8 C9 1.378(3) . ?
C8 C13 1.509(3) . ?
C9 C10 1.394(3) . ?
C10 C11 1.393(3) . ?
C11 C12 1.381(3) . ?
C12 C14 1.518(3) 4_566 ?
C14 C12 1.518(3) 4_565 ?

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
N2 Co1 N1 178.79(7) 4_565 . ?
N2 Co1 O7 83.67(6) 4_565 . ?
N1 Co1 O7 96.46(6) . . ?
N2 Co1 O3 97.64(6) 4_565 . ?
N1 Co1 O3 83.56(7) . . ?
O7 Co1 O3 89.98(6) . . ?
N2 Co1 O5 83.18(6) 4_565 4_565 ?
N1 Co1 O5 96.70(6) . 4_565 ?
O7 Co1 O5 166.83(6) . 4_565 ?
O3 Co1 O5 90.98(6) . 4_565 ?
N2 Co1 O1 95.79(6) 4_565 . ?
N1 Co1 O1 83.01(6) . . ?
O7 Co1 O1 91.27(6) . . ?
O3 Co1 O1 166.57(6) . . ?
O5 Co1 O1 90.83(6) 4_565 . ?
OW1 Na1 O4 82.50(7) . 1_565 ?
OW1 Na1 OW2 130.87(7) . . ?
O4 Na1 OW2 82.68(6) 1_565 . ?
OW1 Na1 O1 95.10(7) . . ?
O4 Na1 O1 117.70(6) 1_565 . ?
OW2 Na1 O1 132.97(6) . . ?
OW1 Na1 O6 90.41(7) . . ?
O4 Na1 O6 154.23(6) 1_565 . ?
OW2 Na1 O6 83.42(6) . . ?
O1 Na1 O6 87.50(5) . . ?
OW1 Na1 O2 137.30(7) . . ?
O4 Na1 O2 92.60(5) 1_565 . ?
OW2 Na1 O2 89.92(6) . . ?
O1 Na1 O2 50.18(5) . . ?
O6 Na1 O2 108.99(5) . . ?
OW1 Na1 C6 118.13(7) . . ?
O4 Na1 C6 107.08(6) 1_565 . ?
OW2 Na1 C6 110.99(6) . . ?
O1 Na1 C6 25.67(5) . . ?
O6 Na1 C6 98.13(6) . . ?
O2 Na1 C6 24.56(5) . . ?
C6 O1 Co1 114.66(12) . . ?
C6 O1 Na1 102.03(12) . . ?
Co1 O1 Na1 142.27(7) . . ?
C6 O2 Na1 84.95(12) . . ?
C7 O3 Co1 114.73(12) . . ?
C7 O4 Na1 129.48(13) . 1_545 ?
C13 O5 Co1 114.93(12) . 4_566 ?
C13 O6 Na1 126.76(13) . . ?
C14 O7 Co1 114.75(12) . . ?
C5 N1 C1 124.03(17) . . ?
C5 N1 Co1 117.60(13) . . ?
C1 N1 Co1 118.36(14) . . ?
C12 N2 C8 124.04(16) . . ?
C12 N2 Co1 117.70(13) . 4_566 ?
C8 N2 Co1 118.24(13) . 4_566 ?
N1 C1 C2 119.45(19) . . ?
N1 C1 C6 109.79(16) . . ?
C2 C1 C6 130.75(18) . . ?
C1 C2 C3 117.62(19) . . ?
C4 C3 C2 121.25(19) . . ?
C3 C4 C5 118.02(19) . . ?
N1 C5 C4 119.60(18) . . ?
N1 C5 C7 111.05(16) . . ?
C4 C5 C7 129.35(19) . . ?
O2 C6 O1 122.59(19) . . ?
O2 C6 C1 123.28(17) . . ?
O1 C6 C1 114.13(17) . . ?
O2 C6 Na1 70.49(12) . . ?
O1 C6 Na1 52.30(10) . . ?
C1 C6 Na1 165.36(13) . . ?
O4 C7 O3 125.61(19) . . ?
O4 C7 C5 121.34(18) . . ?
O3 C7 C5 113.05(17) . . ?
N2 C8 C9 119.34(17) . . ?
N2 C8 C13 110.33(16) . . ?
C9 C8 C13 130.32(18) . . ?
C8 C9 C10 118.29(18) . . ?
C11 C10 C9 120.73(18) . . ?
C12 C11 C10 118.22(19) . . ?
N2 C12 C11 119.36(18) . . ?
N2 C12 C14 110.05(16) . 4_566 ?
C11 C12 C14 130.59(18) . 4_566 ?
O6 C13 O5 124.07(18) . . ?
O6 C13 C8 122.74(17) . . ?
O5 C13 C8 113.16(16) . . ?
O8 C14 O7 124.83(18) . . ?
O8 C14 C12 121.42(17) . 4_565 ?
O7 C14 C12 113.74(17) . 4_565 ?
####################################################################### 
# 
# 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_KCo
_database_code_depnum_ccdc_archive 'CCDC 1476209'
_audit_update_record             
;
2016-04-24 deposited with the CCDC.
2016-10-13 downloaded from the CCDC.
;
#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_formula_sum            'C14 H6 Co K N2 O8'
_chemical_formula_weight         428.24

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

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'

_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   'I 41/a'
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_Int_Tables_number      88
_cell_length_a                   6.9113(10)
_cell_length_b                   6.9113(10)
_cell_length_c                   28.4262(14)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1357.8(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    173.0(2)
_cell_measurement_reflns_used    605
_cell_measurement_theta_min      2.866
_cell_measurement_theta_max      25.242

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

_exptl_crystal_density_diffrn    2.095
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             856.0
_exptl_crystal_description       Octahedron
_exptl_crystal_colour            Violet
_exptl_crystal_size_max          0.106
_exptl_crystal_size_mid          0.046
_exptl_crystal_size_min          0.046
_exptl_special_details           
;
 ?
;


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

_exptl_absorpt_coefficient_mu    1.627
_exptl_absorpt_correction_type   EMPIRICAL
_exptl_absorpt_process_details   
; 
 SADABS(Blessing, 1995) 
;
_exptl_absorpt_correction_T_min  0.90
_exptl_absorpt_correction_T_max  0.94

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

_diffrn_measurement_device_type  'Bruker SMART BREEZE'
_diffrn_measurement_method       CCD
_diffrn_ambient_temperature      173.0(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_probe          x-ray
_diffrn_reflns_av_R_equivalents  0.1088
_diffrn_reflns_number            17071
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_theta_min         2.866
_diffrn_reflns_theta_max         28.44
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 1
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 1
_diffrn_reflns_point_group_measured_fraction_max 0.999
_reflns_number_total             853
_reflns_number_gt                605
_reflns_threshold_expression     'I > 2σ(I)'

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

_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'

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

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   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)+(0.0648P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_coef       0.0044(11)
_refine_ls_number_reflns         853
_refine_ls_number_parameters     61
_refine_ls_number_restraints     0
_refine_ls_number_constraints    0
_refine_ls_R_factor_all          0.0659
_refine_ls_R_factor_gt           0.0397
_refine_ls_wR_factor_ref         0.1115
_refine_ls_wR_factor_gt          0.1023
_refine_ls_goodness_of_fit_ref   0.99
_refine_ls_restrained_S_all      0.99
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.429
_refine_diff_density_min         -1.413
_refine_diff_density_rms         0.121

#----------------------------------------------------------------------------#
#                   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
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'
K K 0.2009 0.2494 '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'

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_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.5 0.75 0.125 0.0147(3) Uani 1 d . .
K1 K 0 0.25 0.125 0.0354(4) Uani 1 d . .
O1 O 0.2507(3) 0.6312(3) 0.11710(7) 0.0191(5) Uani 1 d . .
O2 O 0.0492(3) 0.5269(3) 0.06078(9) 0.0250(6) Uani 1 d . .
N1 N 0.5 0.75 0.06031(13) 0.0151(7) Uani 1 d . .
C1 C 0.3428(4) 0.6845(4) 0.03825(11) 0.0157(6) Uani 1 d . .
C2 C 0.3379(4) 0.6829(4) -0.01031(11) 0.0185(7) Uani 1 d . .
H2 H 0.2294 0.6382 -0.0263 0.022 Uiso 1 calc . .
C3 C 0.5 0.75 -0.03485(16) 0.0185(9) Uani 1 d . .
H3 H 0.5 0.75 -0.0676 0.022 Uiso 1 calc . .
C4 C 0.1979(4) 0.6092(4) 0.07344(11) 0.0184(7) Uani 1 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
Co1 N1 1.839(4) 15_565 ?
Co1 N1 1.839(4) . ?
Co1 O1 1.922(2) . ?
Co1 O1 1.922(2) 6_564 ?
Co1 O1 1.922(2) 15_565 ?
Co1 O1 1.922(2) 12_766 ?
K1 O2 2.667(2) . ?
K1 O2 2.667(2) 6_454 ?
K1 O2 2.667(2) 15 ?
K1 O2 2.667(2) 12_666 ?
K1 O1 3.161(2) 6_454 ?
K1 O1 3.161(2) . ?
K1 O1 3.161(2) 15 ?
K1 O1 3.161(2) 12_666 ?
K1 C4 3.191(3) 6_454 ?
K1 C4 3.191(3) 15 ?
K1 C4 3.191(3) 12_666 ?
K1 C4 3.191(3) . ?
O1 C4 1.303(4) . ?
O2 C4 1.229(4) . ?
N1 C1 1.334(3) . ?
N1 C1 1.334(3) 6_564 ?
C1 C2 1.381(4) . ?
C1 C4 1.508(4) . ?
C2 C3 1.399(4) . ?
C3 C2 1.399(4) 6_564 ?

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 Co1 N1 180 15_565 . ?
N1 Co1 O1 96.71(6) 15_565 . ?
N1 Co1 O1 83.29(6) . . ?
N1 Co1 O1 96.71(6) 15_565 6_564 ?
N1 Co1 O1 83.29(6) . 6_564 ?
O1 Co1 O1 166.58(12) . 6_564 ?
N1 Co1 O1 83.29(6) 15_565 15_565 ?
N1 Co1 O1 96.71(6) . 15_565 ?
O1 Co1 O1 90.783(14) . 15_565 ?
O1 Co1 O1 90.783(14) 6_564 15_565 ?
N1 Co1 O1 83.29(6) 15_565 12_766 ?
N1 Co1 O1 96.71(6) . 12_766 ?
O1 Co1 O1 90.783(14) . 12_766 ?
O1 Co1 O1 90.783(14) 6_564 12_766 ?
O1 Co1 O1 166.57(12) 15_565 12_766 ?
O2 K1 O2 93.59(10) . 6_454 ?
O2 K1 O2 117.95(6) . 15 ?
O2 K1 O2 117.95(6) 6_454 15 ?
O2 K1 O2 117.95(6) . 12_666 ?
O2 K1 O2 117.95(6) 6_454 12_666 ?
O2 K1 O2 93.59(10) 15 12_666 ?
O2 K1 O1 128.27(6) . 6_454 ?
O2 K1 O1 44.22(6) 6_454 6_454 ?
O2 K1 O1 109.62(6) 15 6_454 ?
O2 K1 O1 76.20(6) 12_666 6_454 ?
O2 K1 O1 44.22(6) . . ?
O2 K1 O1 128.27(6) 6_454 . ?
O2 K1 O1 76.20(6) 15 . ?
O2 K1 O1 109.62(6) 12_666 . ?
O1 K1 O1 171.85(7) 6_454 . ?
O2 K1 O1 109.62(6) . 15 ?
O2 K1 O1 76.20(6) 6_454 15 ?
O2 K1 O1 44.22(6) 15 15 ?
O2 K1 O1 128.27(6) 12_666 15 ?
O1 K1 O1 90.289(5) 6_454 15 ?
O1 K1 O1 90.289(5) . 15 ?
O2 K1 O1 76.20(6) . 12_666 ?
O2 K1 O1 109.62(6) 6_454 12_666 ?
O2 K1 O1 128.27(6) 15 12_666 ?
O2 K1 O1 44.22(6) 12_666 12_666 ?
O1 K1 O1 90.289(5) 6_454 12_666 ?
O1 K1 O1 90.290(5) . 12_666 ?
O1 K1 O1 171.85(7) 15 12_666 ?
O2 K1 C4 107.37(7) . 6_454 ?
O2 K1 C4 21.96(7) 6_454 6_454 ?
O2 K1 C4 121.53(7) 15 6_454 ?
O2 K1 C4 96.08(8) 12_666 6_454 ?
O1 K1 C4 23.66(6) 6_454 6_454 ?
O1 K1 C4 148.29(7) . 6_454 ?
O1 K1 C4 87.91(7) 15 6_454 ?
O1 K1 C4 95.84(7) 12_666 6_454 ?
O2 K1 C4 121.53(7) . 15 ?
O2 K1 C4 96.08(8) 6_454 15 ?
O2 K1 C4 21.96(7) 15 15 ?
O2 K1 C4 107.37(7) 12_666 15 ?
O1 K1 C4 95.84(7) 6_454 15 ?
O1 K1 C4 87.91(7) . 15 ?
O1 K1 C4 23.66(6) 15 15 ?
O1 K1 C4 148.29(7) 12_666 15 ?
C4 K1 C4 102.18(5) 6_454 15 ?
O2 K1 C4 96.08(8) . 12_666 ?
O2 K1 C4 121.53(7) 6_454 12_666 ?
O2 K1 C4 107.37(7) 15 12_666 ?
O2 K1 C4 21.96(7) 12_666 12_666 ?
O1 K1 C4 87.91(7) 6_454 12_666 ?
O1 K1 C4 95.84(7) . 12_666 ?
O1 K1 C4 148.29(7) 15 12_666 ?
O1 K1 C4 23.66(6) 12_666 12_666 ?
C4 K1 C4 102.18(5) 6_454 12_666 ?
C4 K1 C4 125.31(11) 15 12_666 ?
O2 K1 C4 21.96(7) . . ?
O2 K1 C4 107.37(7) 6_454 . ?
O2 K1 C4 96.08(8) 15 . ?
O2 K1 C4 121.53(7) 12_666 . ?
O1 K1 C4 148.28(7) 6_454 . ?
O1 K1 C4 23.66(6) . . ?
O1 K1 C4 95.84(7) 15 . ?
O1 K1 C4 87.91(7) 12_666 . ?
C4 K1 C4 125.31(11) 6_454 . ?
C4 K1 C4 102.18(5) 15 . ?
C4 K1 C4 102.18(5) 12_666 . ?
C4 O1 Co1 114.36(19) . . ?
C4 O1 K1 79.44(16) . . ?
Co1 O1 K1 147.04(10) . . ?
C4 O2 K1 103.8(2) . . ?
C1 N1 C1 123.9(4) . 6_564 ?
C1 N1 Co1 118.04(19) . . ?
C1 N1 Co1 118.04(19) 6_564 . ?
N1 C1 C2 119.5(3) . . ?
N1 C1 C4 110.3(3) . . ?
C2 C1 C4 130.1(3) . . ?
C1 C2 C3 118.4(3) . . ?
C2 C3 C2 120.2(4) 6_564 . ?
O2 C4 O1 124.6(3) . . ?
O2 C4 C1 121.4(3) . . ?
O1 C4 C1 113.9(3) . . ?
O2 C4 K1 54.26(17) . . ?
O1 C4 K1 76.90(17) . . ?
C1 C4 K1 149.07(19) . . ?
####################################################################### 
# 
# 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_H3OCo
_database_code_depnum_ccdc_archive 'CCDC 1476210'
_audit_update_record             
;
2016-04-24 deposited with the CCDC.
2016-10-13 downloaded from the CCDC.
;
#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_formula_sum            'C14 H8 Co N2 O9'
_chemical_formula_weight         407.15

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


loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y+3/4, x+1/4, z+1/4'
'-x+1/2, -y, z+1/2'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-y+5/4, x+3/4, z+3/4'
'-x+1, -y+1/2, z+1'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'y-3/4, -x-1/4, -z-1/4'
'x-1/2, y, -z-1/2'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'y-1/4, -x+1/4, -z+1/4'
'x, y+1/2, -z'
'-y-1/4, x-1/4, -z-1/4'

_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   'I 41/a'
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_Int_Tables_number      88
_cell_length_a                   7.0260(10)
_cell_length_b                   7.0260(10)
_cell_length_c                   27.891(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1376.8(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    173.0(2)
_cell_measurement_reflns_used    781
_cell_measurement_theta_min      2.921
_cell_measurement_theta_max      25.242

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

_exptl_crystal_density_diffrn    1.964
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             820
_exptl_crystal_description       Block
_exptl_crystal_colour            Violet
_exptl_crystal_size_max          0.048
_exptl_crystal_size_mid          0.025
_exptl_crystal_size_min          0.010
_exptl_special_details           
;
 ?
;


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

_exptl_absorpt_coefficient_mu    1.310
_exptl_absorpt_correction_type   EMPIRICAL
_exptl_absorpt_process_details   
; 
 SADABS(Blessing, 1995) 
;
_exptl_absorpt_correction_T_min  0.89
_exptl_absorpt_correction_T_max  0.95


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

_diffrn_measurement_device_type  'Bruker SMART BREEZE'
_diffrn_measurement_method       CCD
_diffrn_ambient_temperature      173.0(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_probe          x-ray
_diffrn_reflns_av_R_equivalents  0.0448
_diffrn_reflns_number            12176
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_theta_min         2.921
_diffrn_reflns_theta_max         28.387
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 1
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 1
_diffrn_reflns_point_group_measured_fraction_max 0.995
_reflns_number_total             864
_reflns_number_gt                781
_reflns_threshold_expression     'I > 2σ(I)'

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

_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'

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

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   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)+(0.0412P)²+0.8783P] where P=(Fo²+2Fc²)/3'
_refine_ls_extinction_method     none
_refine_ls_number_reflns         864
_refine_ls_number_parameters     64
_refine_ls_number_restraints     0
_refine_ls_number_constraints    0
_refine_ls_R_factor_all          0.029
_refine_ls_R_factor_gt           0.0262
_refine_ls_wR_factor_ref         0.0717
_refine_ls_wR_factor_gt          0.0706
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_restrained_S_all      1.088
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.346
_refine_diff_density_min         -0.281
_refine_diff_density_rms         0.055

#----------------------------------------------------------------------------#
#                   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
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'
Co Co 0.3494 0.9721 '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_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.5 0.75 0.125 0.02076(14) Uani 1 d . .
O1 O 0.25565(16) 0.63396(17) 0.11732(4) 0.0279(3) Uani 1 d . .
O2 O 0.05920(19) 0.5267(2) 0.06104(5) 0.0466(4) Uani 1 d . .
O3 O 0 0.25 0.125 0.0449(7) Uani 1 d . .
N1 N 0.5 0.75 0.05907(7) 0.0224(4) Uani 1 d . .
C1 C 0.3459(2) 0.6838(2) 0.03691(5) 0.0236(3) Uani 1 d . .
C2 C 0.3407(3) 0.6826(2) -0.01259(6) 0.0292(3) Uani 1 d . .
H2 H 0.2344 0.6383 -0.029 0.035 Uiso 1 calc . .
C3 C 0.5 0.75 -0.03708(8) 0.0317(5) Uani 1 d . .
H3 H 0.5 0.75 -0.0704 0.038 Uiso 1 calc . .
C4 C 0.2045(2) 0.6107(2) 0.07322(6) 0.0281(3) Uani 1 d . .
H31 H 0.011(5) 0.338(5) 0.1083(15) 0.028(9) Uiso 0.5 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
Co1 N1 1.8389(18) . ?
Co1 N1 1.8390(18) 14_565 ?
Co1 O1 1.9124(11) 7_564 ?
Co1 O1 1.9124(11) 14_565 ?
Co1 O1 1.9124(11) 12_766 ?
Co1 O1 1.9124(11) . ?
O1 C4 1.2919(19) . ?
O2 C4 1.227(2) . ?
N1 C1 1.3304(17) 7_564 ?
N1 C1 1.3305(17) . ?
C1 C2 1.381(2) . ?
C1 C4 1.509(2) . ?
C2 C3 1.394(2) . ?
C3 C2 1.394(2) 7_564 ?

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 Co1 N1 180 . 14_565 ?
N1 Co1 O1 83.57(3) . 7_564 ?
N1 Co1 O1 96.43(3) 14_565 7_564 ?
N1 Co1 O1 96.43(3) . 14_565 ?
N1 Co1 O1 83.57(3) 14_565 14_565 ?
O1 Co1 O1 90.719(7) 7_564 14_565 ?
N1 Co1 O1 96.43(3) . 12_766 ?
N1 Co1 O1 83.57(3) 14_565 12_766 ?
O1 Co1 O1 90.719(7) 7_564 12_766 ?
O1 Co1 O1 167.13(6) 14_565 12_766 ?
N1 Co1 O1 83.57(3) . . ?
N1 Co1 O1 96.43(3) 14_565 . ?
O1 Co1 O1 167.13(6) 7_564 . ?
O1 Co1 O1 90.718(7) 14_565 . ?
O1 Co1 O1 90.720(7) 12_766 . ?
C4 O1 Co1 114.23(10) . . ?
C1 N1 C1 124.64(19) 7_564 . ?
C1 N1 Co1 117.68(10) 7_564 . ?
C1 N1 Co1 117.68(10) . . ?
N1 C1 C2 119.23(15) . . ?
N1 C1 C4 110.06(14) . . ?
C2 C1 C4 130.63(14) . . ?
C1 C2 C3 117.78(16) . . ?
C2 C3 C2 121.3(2) . 7_564 ?
O2 C4 O1 123.78(15) . . ?
O2 C4 C1 121.72(15) . . ?
O1 C4 C1 114.37(13) . . ?

#===END
