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

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

data_shelx
_database_code_depnum_ccdc_archive 'CCDC 1869008'
_audit_update_record             
;
2018-09-21 deposited with the CCDC.
2018-11-02 downloaded from the CCDC.
;
_audit_creation_date             2018-09-20
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.25(C84 H52 Co2 Cu2.3 N12 O28), 3.25(O)'
_chemical_formula_sum            'C21 H11 Co0.50 Cu0.58 N3 O10.25'
_chemical_formula_weight         535.41
_chemical_melting_point          ?
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'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 '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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           87
_space_group_name_H-M_alt        'I 4/m'
_space_group_name_Hall           '-I 4'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-x, -y, -z'
'x, y, -z'
'y, -x, -z'
'-y, x, -z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'

_cell_length_a                   15.440(5)
_cell_length_b                   15.440(5)
_cell_length_c                   26.265(5)
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 90.000(5)
_cell_angle_gamma                90.000(5)
_cell_volume                     6261(4)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    5400
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.5910
_cell_measurement_theta_min      3.0570
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.719
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.96911
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.136
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2162
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.17
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0603
_diffrn_reflns_av_unetI/netI     0.0289
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            29481
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.348
_diffrn_reflns_theta_min         3.050
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 15.9853
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2558
_reflns_number_total             2954
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         1.290
_refine_diff_density_min         -0.599
_refine_diff_density_rms         0.091
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.128
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     194
_refine_ls_number_reflns         2954
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0759
_refine_ls_R_factor_gt           0.0690
_refine_ls_restrained_S_all      1.128
_refine_ls_shift/su_max          0.074
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0936P)²+33.9488P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2044
_refine_ls_wR_factor_ref         0.2086
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C11(H11)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.3888(3) 0.3195(3) 0.41608(15) 0.0309(9) Uani 1 1 d . . . . .
C2 C 0.4101(3) 0.2724(3) 0.36772(15) 0.0297(9) Uani 1 1 d . . . . .
C3 C 0.4958(3) 0.2548(3) 0.35579(18) 0.0389(10) Uani 1 1 d . . . . .
C4 C 0.5168(3) 0.2091(3) 0.31208(18) 0.0399(11) Uani 1 1 d . . . . .
C5 C 0.4519(3) 0.1789(3) 0.27994(15) 0.0311(9) Uani 1 1 d . . . . .
C6 C 0.3670(3) 0.1991(4) 0.29126(19) 0.0441(12) Uani 1 1 d . . . . .
C7 C 0.3463(3) 0.2453(3) 0.33465(19) 0.0436(12) Uani 1 1 d . . . . .
C8 C 0.4679(3) 0.1477(3) 0.19112(17) 0.0393(11) Uani 1 1 d . . . . .
C9 C 0.4864(3) 0.0742(3) 0.15513(16) 0.0378(10) Uani 1 1 d . . . . .
C10 C 0.4870(5) 0.0762(4) 0.1030(2) 0.069(2) Uani 1 1 d . . . . .
C11 C 0.500000 0.000000 0.0770(3) 0.087(4) Uani 1 2 d S T P . .
H11 H 0.500000 -0.000001 0.041633 0.105 Uiso 1 2 calc RS T P . .
Co1 Co 0.500000 0.000000 0.250000 0.0242(3) Uani 1 4 d S T P . .
Cu1 Cu 0.56676(8) 0.35189(8) 0.500000 0.0303(5) Uani 0.576(4) 2 d S T P . .
N1 N 0.4735(2) 0.1226(2) 0.23914(13) 0.0310(8) Uani 1 1 d . . . . .
N2 N 0.500000 0.000000 0.17958(18) 0.0289(10) Uani 1 2 d S T P . .
O1 O 0.500000 0.500000 0.500000 0.0242(15) Uiso 1 8 d S T P . .
O2 O 0.4129(6) 0.1881(6) 0.000000 0.108(3) Uani 1 2 d S T P . .
O3 O 0.3116(2) 0.3298(2) 0.42930(13) 0.0434(8) Uani 1 1 d . . . . .
O4 O 0.4479(3) 0.2209(2) 0.17474(14) 0.0633(12) Uani 1 1 d . . . . .
O5 O 0.4502(2) 0.3493(2) 0.44220(12) 0.0403(8) Uani 1 1 d . . . . .
O7 O 0.3436(3) 0.2580(4) 0.08931(19) 0.0825(14) Uani 1 1 d . . . . .
O10 O 0.5453(6) 0.1997(5) 0.500000 0.070(2) Uani 1 2 d S T P . .
H10A H 0.506(5) 0.180(5) 0.500000 0.03(2) Uiso 1 2 d S T P . .
H3 H 0.547(4) 0.269(4) 0.376(2) 0.054(15) Uiso 1 1 d . . . . .
H4 H 0.573(3) 0.200(3) 0.3036(17) 0.029(11) Uiso 1 1 d . . . . .
H6 H 0.328(4) 0.181(4) 0.274(2) 0.066(19) Uiso 1 1 d . . . . .
H7 H 0.290(4) 0.263(4) 0.343(2) 0.053(16) Uiso 1 1 d . . . . .
H10 H 0.476(5) 0.114(5) 0.087(3) 0.09(3) Uiso 1 1 d . . . . .
H10B H 0.586(10) 0.173(10) 0.500000 0.14(7) Uiso 1 2 d S T P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.500(6) . ?
C1 O3 1.253(5) . ?
C1 O5 1.257(5) . ?
C2 C3 1.386(6) . ?
C2 C7 1.378(6) . ?
C3 C4 1.386(6) . ?
C4 C5 1.391(6) . ?
C5 C6 1.380(7) . ?
C5 N1 1.419(5) . ?
C6 C7 1.382(7) . ?
C8 C9 1.505(6) . ?
C8 N1 1.322(6) . ?
C8 O4 1.248(6) . ?
C9 C10 1.369(7) . ?
C9 N2 1.330(5) . ?
C10 C11 1.374(7) . ?
Co1 N1 1.958(4) 15 ?
Co1 N1 1.958(4) 16_545 ?
Co1 N1 1.958(4) . ?
Co1 N1 1.958(4) 2_655 ?
Co1 N2 1.850(5) . ?
Co1 N2 1.850(5) 15 ?
Cu1 O5 2.355(3) . ?
Cu1 O5 2.355(3) 10_556 ?
Cu1 O10 2.373(7) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 C1 C2 120.3(4) . . ?
O3 C1 O5 121.3(4) . . ?
O5 C1 C2 118.4(4) . . ?
C3 C2 C1 119.6(4) . . ?
C7 C2 C1 121.6(4) . . ?
C7 C2 C3 118.7(4) . . ?
C4 C3 C2 120.7(4) . . ?
C3 C4 C5 120.3(4) . . ?
C4 C5 N1 119.6(4) . . ?
C6 C5 C4 118.5(4) . . ?
C6 C5 N1 121.6(4) . . ?
C5 C6 C7 120.9(4) . . ?
C2 C7 C6 120.7(4) . . ?
N1 C8 C9 111.4(4) . . ?
O4 C8 C9 120.9(4) . . ?
O4 C8 N1 127.6(4) . . ?
C10 C9 C8 127.8(4) . . ?
N2 C9 C8 112.1(4) . . ?
N2 C9 C10 120.0(5) . . ?
C9 C10 C11 118.6(5) . . ?
C10 C11 C10 120.5(7) . 2_655 ?
N1 Co1 N1 91.22(3) . 16_545 ?
N1 Co1 N1 91.22(3) . 15 ?
N1 Co1 N1 163.2(2) . 2_655 ?
N1 Co1 N1 163.2(2) 15 16_545 ?
N1 Co1 N1 91.22(3) 15 2_655 ?
N1 Co1 N1 91.22(3) 16_545 2_655 ?
N2 Co1 N1 98.38(10) . 15 ?
N2 Co1 N1 81.62(10) . . ?
N2 Co1 N1 98.38(10) 15 2_655 ?
N2 Co1 N1 81.62(10) 15 15 ?
N2 Co1 N1 98.38(10) . 16_545 ?
N2 Co1 N1 81.62(10) . 2_655 ?
N2 Co1 N1 98.38(10) 15 . ?
N2 Co1 N1 81.62(10) 15 16_545 ?
N2 Co1 N2 180.0 . 15 ?
O5 Cu1 O5 80.29(16) . 10_556 ?
O5 Cu1 O10 82.90(19) 10_556 . ?
O5 Cu1 O10 82.90(19) . . ?
C5 N1 Co1 122.1(3) . . ?
C8 N1 C5 121.7(4) . . ?
C8 N1 Co1 115.9(3) . . ?
C9 N2 C9 122.3(5) 2_655 . ?
C9 N2 Co1 118.9(3) . . ?
C9 N2 Co1 118.9(3) 2_655 . ?
C1 O5 Cu1 159.1(3) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
