# 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_x_sq
_database_code_depnum_ccdc_archive 'CCDC 1584072'
_audit_update_record             
;
2017-11-06 deposited with the CCDC.
2018-01-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C79 H99 Co3 N7 O25'
_chemical_formula_weight         1723.44

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'
O O 0.0106 0.0060 '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'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           52
_space_group_name_H-M_alt        'P n n a'
_space_group_name_Hall           '-P 2a 2bc'

_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+1/2, -y, z'
'-x+1/2, y+1/2, -z+1/2'
'x, -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                   26.0789(5)
_cell_length_b                   22.3894(5)
_cell_length_c                   13.9388(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     8138.7(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    10240
_cell_measurement_theta_min      2.3930
_cell_measurement_theta_max      28.8938

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.407
_exptl_crystal_F_000             3612
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.81
_exptl_crystal_size_mid          0.75
_exptl_crystal_size_min          0.67
_exptl_absorpt_coefficient_mu    0.686
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.88738
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.2083
_diffrn_reflns_number            24301
_diffrn_reflns_av_unetI/netI     0.0477
_diffrn_reflns_av_R_equivalents  0.0295
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.398
_diffrn_reflns_theta_max         28.957
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.880
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.880
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.880
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             9498
_reflns_number_gt                6048
_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.
 
 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.
;

_computing_data_collection       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
;
_computing_cell_refinement       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
;
_computing_data_reduction        
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
;
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_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)+(0.0550P)²+4.0000P] 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         9498
_refine_ls_number_parameters     339
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0739
_refine_ls_R_factor_gt           0.0469
_refine_ls_wR_factor_ref         0.1221
_refine_ls_wR_factor_gt          0.1143
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_restrained_S_all      1.009
_refine_ls_shift/su_max          0.001
_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 0.09447(2) 0.40992(2) 0.27329(2) 0.02529(9) Uani 1 1 d . . . . .
Co2 Co 0.09461(2) 0.250000 0.250000 0.02051(10) Uani 1 2 d S T P . .
O1 O 0.15900(7) 0.38776(8) 0.20613(15) 0.0439(5) Uani 1 1 d . . . . .
O2 O 0.15138(7) 0.29048(9) 0.17325(15) 0.0515(6) Uani 1 1 d . . . . .
O3 O 0.53163(7) 0.38806(9) -0.20234(17) 0.0591(6) Uani 1 1 d . . . . .
O4 O 0.53831(7) 0.29077(9) -0.17186(14) 0.0493(5) Uani 1 1 d . . . . .
O5 O 0.10309(10) 0.49693(10) 0.24733(17) 0.0656(7) Uani 1 1 d . . . . .
O6 O 0.02997(14) 0.50105(13) 0.3203(3) 0.1147(12) Uani 1 1 d . . . . .
O7 O 0.10831(9) 0.40476(8) 0.41953(13) 0.0499(5) Uani 1 1 d . . . . .
O8 O 0.09231(7) 0.32061(8) 0.35214(12) 0.0373(4) Uani 1 1 d . . . . .
C1 C 0.17389(10) 0.33929(13) 0.17039(19) 0.0359(6) Uani 1 1 d . . . . .
C2 C 0.22436(10) 0.34057(13) 0.1183(2) 0.0426(7) Uani 1 1 d . . . . .
C3 C 0.24913(11) 0.39389(13) 0.0991(2) 0.0545(9) Uani 1 1 d . . . . .
H3A H 0.234471 0.429799 0.118425 0.065 Uiso 1 1 calc R U . . .
C4 C 0.29552(12) 0.39397(14) 0.0515(3) 0.0638(10) Uani 1 1 d . . . . .
H4A H 0.311702 0.430141 0.038922 0.077 Uiso 1 1 calc R U . . .
C5 C 0.31832(11) 0.34162(14) 0.0223(2) 0.0530(8) Uani 1 1 d . . . . .
C6 C 0.29330(12) 0.28847(15) 0.0413(3) 0.0699(11) Uani 1 1 d . . . . .
H6A H 0.307995 0.252664 0.021581 0.084 Uiso 1 1 calc R U . . .
C7 C 0.24704(12) 0.28764(14) 0.0887(3) 0.0624(10) Uani 1 1 d . . . . .
H7A H 0.230903 0.251405 0.101033 0.075 Uiso 1 1 calc R U . . .
C8 C 0.36948(11) 0.34169(14) -0.0264(2) 0.0521(8) Uani 1 1 d . . . . .
C9 C 0.38627(15) 0.38843(18) -0.0777(4) 0.116(2) Uani 1 1 d . . . . .
H9A H 0.365652 0.422207 -0.082207 0.139 Uiso 1 1 calc R U . . .
C10 C 0.43338(15) 0.38822(18) -0.1244(4) 0.116(2) Uani 1 1 d . . . . .
H10A H 0.443249 0.421281 -0.160339 0.139 Uiso 1 1 calc R U . . .
C11 C 0.46521(10) 0.34022(13) -0.1182(2) 0.0449(7) Uani 1 1 d . . . . .
C12 C 0.44914(13) 0.29346(15) -0.0656(3) 0.0812(14) Uani 1 1 d . . . . .
H12A H 0.469961 0.259921 -0.060003 0.097 Uiso 1 1 calc R U . . .
C13 C 0.40213(14) 0.29448(17) -0.0195(3) 0.0912(16) Uani 1 1 d . . . . .
H13A H 0.392518 0.261736 0.017362 0.109 Uiso 1 1 calc R U . . .
C14 C 0.51614(10) 0.33941(12) -0.1682(2) 0.0381(7) Uani 1 1 d . . . . .
C15 C 0.06656(17) 0.52484(16) 0.2788(3) 0.0664(10) Uani 1 1 d . . . . .
C16 C 0.06715(15) 0.59296(14) 0.2692(3) 0.0626(9) Uani 1 1 d . . . . .
C17 C 0.02444(17) 0.62584(17) 0.2910(4) 0.1008(16) Uani 1 1 d . . . . .
H17A H -0.005187 0.606893 0.312289 0.121 Uiso 1 1 calc R U . . .
C18 C 0.02545(16) 0.68712(17) 0.2813(4) 0.0966(16) Uani 1 1 d . . . . .
H18A H -0.004245 0.708999 0.292746 0.116 Uiso 1 1 calc R U . . .
C19 C 0.07004(16) 0.71676(14) 0.2547(3) 0.0643(10) Uani 1 1 d . . . . .
C20 C 0.11176(18) 0.68341(17) 0.2365(3) 0.0834(13) Uani 1 1 d . . . . .
H20A H 0.142243 0.702151 0.219392 0.100 Uiso 1 1 calc R U . . .
C21 C 0.11026(15) 0.62029(16) 0.2429(3) 0.0712(11) Uani 1 1 d . . . . .
H21A H 0.139361 0.597960 0.228695 0.085 Uiso 1 1 calc R U . . .
C22 C 0.10297(9) 0.34918(11) 0.42564(17) 0.0296(5) Uani 1 1 d . . . . .
C23 C 0.10716(10) 0.31913(11) 0.52105(18) 0.0332(6) Uani 1 1 d . . . . .
C24 C 0.11981(15) 0.35115(14) 0.6016(2) 0.0586(9) Uani 1 1 d . . . . .
H24A H 0.126785 0.391739 0.596005 0.070 Uiso 1 1 calc R U . . .
C25 C 0.12242(15) 0.32447(13) 0.6906(2) 0.0597(9) Uani 1 1 d . . . . .
H25A H 0.131628 0.347127 0.743759 0.072 Uiso 1 1 calc R U . . .
C26 C 0.11147(12) 0.26425(12) 0.70178(18) 0.0408(7) Uani 1 1 d . . . . .
C27 C 0.09874(14) 0.23233(13) 0.62024(19) 0.0525(8) Uani 1 1 d . . . . .
H27A H 0.091474 0.191796 0.625522 0.063 Uiso 1 1 calc R U . . .
C28 C 0.09654(12) 0.25932(12) 0.53084(18) 0.0460(7) Uani 1 1 d . . . . .
H28A H 0.087836 0.236815 0.477173 0.055 Uiso 1 1 calc R U . . .


_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 1.9755(18) 6 ?
Co1 O1 1.9886(18) . ?
Co1 O5 1.994(2) . ?
Co1 O7 2.0733(18) . ?
Co1 O8 2.2825(17) . ?
Co2 O2 2.0391(18) . ?
Co2 O2 2.0391(18) 4 ?
Co2 O4 2.0434(18) 6 ?
Co2 O4 2.0434(18) 7_566 ?
Co2 O8 2.1283(17) . ?
Co2 O8 2.1283(16) 4 ?
O1 C1 1.256(3) . ?
O2 C1 1.241(3) . ?
O3 C14 1.256(3) . ?
O4 C14 1.234(3) . ?
O5 C15 1.221(4) . ?
O6 C15 1.237(4) . ?
O7 C22 1.255(3) . ?
O8 C22 1.239(3) . ?
C1 C2 1.504(3) . ?
C2 C3 1.383(4) . ?
C2 C7 1.387(4) . ?
C3 C4 1.380(4) . ?
C3 H3A 0.9300 . ?
C4 C5 1.376(4) . ?
C4 H4A 0.9300 . ?
C5 C6 1.382(4) . ?
C5 C8 1.497(4) . ?
C6 C7 1.376(4) . ?
C6 H6A 0.9300 . ?
C7 H7A 0.9300 . ?
C8 C9 1.341(5) . ?
C8 C13 1.361(4) . ?
C9 C10 1.391(4) . ?
C9 H9A 0.9300 . ?
C10 C11 1.361(4) . ?
C10 H10A 0.9300 . ?
C11 C12 1.346(4) . ?
C11 C14 1.500(3) . ?
C12 C13 1.384(4) . ?
C12 H12A 0.9300 . ?
C13 H13A 0.9300 . ?
C15 C16 1.531(5) . ?
C16 C21 1.332(5) . ?
C16 C17 1.369(5) . ?
C17 C18 1.379(5) . ?
C17 H17A 0.9300 . ?
C18 C19 1.390(5) . ?
C18 H18A 0.9300 . ?
C19 C20 1.344(5) . ?
C19 C19 1.494(6) 4_565 ?
C20 C21 1.417(5) . ?
C20 H20A 0.9300 . ?
C21 H21A 0.9300 . ?
C22 C23 1.494(3) . ?
C23 C24 1.372(4) . ?
C23 C28 1.374(4) . ?
C24 C25 1.378(4) . ?
C24 H24A 0.9300 . ?
C25 C26 1.387(4) . ?
C25 H25A 0.9300 . ?
C26 C27 1.383(4) . ?
C26 C26 1.488(5) 4_556 ?
C27 C28 1.386(4) . ?
C27 H27A 0.9300 . ?
C28 H28A 0.9300 . ?

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 O1 113.86(9) 6 . ?
O3 Co1 O5 104.16(9) 6 . ?
O1 Co1 O5 93.61(9) . . ?
O3 Co1 O7 128.51(10) 6 . ?
O1 Co1 O7 107.56(9) . . ?
O5 Co1 O7 102.32(9) . . ?
O3 Co1 O8 90.20(8) 6 . ?
O1 Co1 O8 91.66(7) . . ?
O5 Co1 O8 161.09(8) . . ?
O7 Co1 O8 58.80(7) . . ?
O2 Co2 O2 86.89(13) . 4 ?
O2 Co2 O4 92.49(9) . 6 ?
O2 Co2 O4 179.34(9) 4 6 ?
O2 Co2 O4 179.34(9) . 7_566 ?
O2 Co2 O4 92.49(9) 4 7_566 ?
O4 Co2 O4 88.13(13) 6 7_566 ?
O2 Co2 O8 92.37(7) . . ?
O2 Co2 O8 89.98(7) 4 . ?
O4 Co2 O8 90.26(7) 6 . ?
O4 Co2 O8 87.42(7) 7_566 . ?
O2 Co2 O8 89.99(7) . 4 ?
O2 Co2 O8 92.37(7) 4 4 ?
O4 Co2 O8 87.42(7) 6 4 ?
O4 Co2 O8 90.25(7) 7_566 4 ?
O8 Co2 O8 176.76(10) . 4 ?
C1 O1 Co1 131.62(17) . . ?
C1 O2 Co2 138.73(18) . . ?
C14 O3 Co1 132.19(17) . 6_655 ?
C14 O4 Co2 138.85(17) . 6_655 ?
C15 O5 Co1 110.3(2) . . ?
C22 O7 Co1 95.90(15) . . ?
C22 O8 Co2 158.43(18) . . ?
C22 O8 Co1 86.57(15) . . ?
Co2 O8 Co1 109.15(7) . . ?
O2 C1 O1 127.0(2) . . ?
O2 C1 C2 116.5(2) . . ?
O1 C1 C2 116.5(2) . . ?
C3 C2 C7 118.7(3) . . ?
C3 C2 C1 121.2(3) . . ?
C7 C2 C1 120.0(2) . . ?
C4 C3 C2 120.2(3) . . ?
C4 C3 H3A 119.9 . . ?
C2 C3 H3A 119.9 . . ?
C5 C4 C3 121.3(3) . . ?
C5 C4 H4A 119.3 . . ?
C3 C4 H4A 119.3 . . ?
C4 C5 C6 118.2(3) . . ?
C4 C5 C8 121.2(3) . . ?
C6 C5 C8 120.5(3) . . ?
C7 C6 C5 121.1(3) . . ?
C7 C6 H6A 119.4 . . ?
C5 C6 H6A 119.4 . . ?
C6 C7 C2 120.3(3) . . ?
C6 C7 H7A 119.8 . . ?
C2 C7 H7A 119.8 . . ?
C9 C8 C13 116.1(3) . . ?
C9 C8 C5 122.3(3) . . ?
C13 C8 C5 121.7(3) . . ?
C8 C9 C10 122.4(3) . . ?
C8 C9 H9A 118.8 . . ?
C10 C9 H9A 118.8 . . ?
C11 C10 C9 120.8(3) . . ?
C11 C10 H10A 119.6 . . ?
C9 C10 H10A 119.6 . . ?
C12 C11 C10 117.3(3) . . ?
C12 C11 C14 121.3(3) . . ?
C10 C11 C14 121.4(3) . . ?
C11 C12 C13 121.1(3) . . ?
C11 C12 H12A 119.5 . . ?
C13 C12 H12A 119.5 . . ?
C8 C13 C12 122.3(3) . . ?
C8 C13 H13A 118.8 . . ?
C12 C13 H13A 118.8 . . ?
O4 C14 O3 126.8(2) . . ?
O4 C14 C11 116.4(2) . . ?
O3 C14 C11 116.8(2) . . ?
O5 C15 O6 123.4(4) . . ?
O5 C15 C16 118.1(3) . . ?
O6 C15 C16 118.5(4) . . ?
C21 C16 C17 120.1(3) . . ?
C21 C16 C15 119.4(3) . . ?
C17 C16 C15 120.5(3) . . ?
C16 C17 C18 119.9(4) . . ?
C16 C17 H17A 120.1 . . ?
C18 C17 H17A 120.1 . . ?
C17 C18 C19 121.2(4) . . ?
C17 C18 H18A 119.4 . . ?
C19 C18 H18A 119.4 . . ?
C20 C19 C18 117.6(3) . . ?
C20 C19 C19 122.5(3) . 4_565 ?
C18 C19 C19 119.9(2) . 4_565 ?
C19 C20 C21 121.4(4) . . ?
C19 C20 H20A 119.3 . . ?
C21 C20 H20A 119.3 . . ?
C16 C21 C20 119.9(4) . . ?
C16 C21 H21A 120.0 . . ?
C20 C21 H21A 120.0 . . ?
O8 C22 O7 118.7(2) . . ?
O8 C22 C23 121.3(2) . . ?
O7 C22 C23 119.9(2) . . ?
C24 C23 C28 118.4(2) . . ?
C24 C23 C22 120.7(2) . . ?
C28 C23 C22 120.8(2) . . ?
C23 C24 C25 121.4(3) . . ?
C23 C24 H24A 119.3 . . ?
C25 C24 H24A 119.3 . . ?
C24 C25 C26 120.8(3) . . ?
C24 C25 H25A 119.6 . . ?
C26 C25 H25A 119.6 . . ?
C27 C26 C25 117.3(2) . . ?
C27 C26 C26 121.4(3) . 4_556 ?
C25 C26 C26 121.2(3) . 4_556 ?
C26 C27 C28 121.6(3) . . ?
C26 C27 H27A 119.2 . . ?
C28 C27 H27A 119.2 . . ?
C23 C28 C27 120.4(2) . . ?
C23 C28 H28A 119.8 . . ?
C27 C28 H28A 119.8 . . ?

_refine_diff_density_max         0.565
_refine_diff_density_min         -0.373
_refine_diff_density_rms         0.058



####################################################################### 
# 
# 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_x_sq_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1584073'
_audit_update_record             
;
2017-11-06 deposited with the CCDC.
2018-01-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C77 H96 Co2 Mg N6 O25'
_chemical_formula_weight         1647.76

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'
O O 0.0106 0.0060 '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'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mg Mg 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           52
_space_group_name_H-M_alt        'P n n a'
_space_group_name_Hall           '-P 2a 2bc'

_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+1/2, -y, z'
'x, -y+1/2, -z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z'
'-x, y-1/2, z-1/2'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   26.0566(7)
_cell_length_b                   22.3986(6)
_cell_length_c                   13.8669(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     8093.2(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    11676
_cell_measurement_theta_min      3.8180
_cell_measurement_theta_max      29.3350

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.352
_exptl_crystal_F_000             3464
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_exptl_absorpt_coefficient_mu    0.497
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.83931
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3503
_diffrn_reflns_number            29346
_diffrn_reflns_av_unetI/netI     0.0276
_diffrn_reflns_av_R_equivalents  0.0273
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.451
_diffrn_reflns_theta_max         29.354
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.871
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.871
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.871
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             9698
_reflns_number_gt                7648
_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.
 
 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.
;

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_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)+(0.0700P)²+7.0000P] 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         9698
_refine_ls_number_parameters     339
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0613
_refine_ls_R_factor_gt           0.0497
_refine_ls_wR_factor_ref         0.1455
_refine_ls_wR_factor_gt          0.1363
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_restrained_S_all      1.018
_refine_ls_shift/su_max          0.002
_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 0.09392(2) 0.41065(2) 0.27299(2) 0.02227(9) Uani 1 1 d . . . . .
Mg1 Mg 0.09439(3) 0.250000 0.250000 0.01544(17) Uani 1 2 d S T P . .
O1 O 0.15844(5) 0.39074(6) 0.20498(12) 0.0317(3) Uani 1 1 d . . . . .
O2 O 0.15021(6) 0.29287(7) 0.17554(11) 0.0331(3) Uani 1 1 d . . . . .
O3 O 0.53048(6) 0.38969(7) -0.20443(17) 0.0542(5) Uani 1 1 d . . . . .
O4 O 0.53862(6) 0.29223(7) -0.17352(11) 0.0344(4) Uani 1 1 d . . . . .
O5 O 0.09907(8) 0.49750(8) 0.24851(14) 0.0510(5) Uani 1 1 d . . . . .
O6 O 0.02754(11) 0.50172(10) 0.3259(2) 0.0867(8) Uani 1 1 d . . . . .
O7 O 0.10745(7) 0.40427(6) 0.41831(11) 0.0373(4) Uani 1 1 d . . . . .
O8 O 0.09317(5) 0.31858(6) 0.34988(9) 0.0230(3) Uani 1 1 d . . . . .
C1 C 0.17303(8) 0.34149(9) 0.16980(15) 0.0287(4) Uani 1 1 d . . . . .
C2 C 0.22289(8) 0.34193(10) 0.11563(17) 0.0335(5) Uani 1 1 d . . . . .
C3 C 0.24822(9) 0.39527(10) 0.0958(2) 0.0440(6) Uani 1 1 d . . . . .
H3A H 0.233889 0.431295 0.115495 0.053 Uiso 1 1 calc R U . . .
C4 C 0.29465(9) 0.39507(11) 0.0471(2) 0.0502(7) Uani 1 1 d . . . . .
H4A H 0.311057 0.431053 0.034055 0.060 Uiso 1 1 calc R U . . .
C5 C 0.31691(9) 0.34215(11) 0.0175(2) 0.0447(6) Uani 1 1 d . . . . .
C6 C 0.29101(10) 0.28899(11) 0.0363(2) 0.0551(8) Uani 1 1 d . . . . .
H6A H 0.305329 0.252929 0.016707 0.066 Uiso 1 1 calc R U . . .
C7 C 0.24430(10) 0.28914(11) 0.0836(2) 0.0480(7) Uani 1 1 d . . . . .
H7A H 0.227116 0.253317 0.093880 0.058 Uiso 1 1 calc R U . . .
C8 C 0.36788(9) 0.34137(11) -0.0316(2) 0.0464(7) Uani 1 1 d . . . . .
C9 C 0.38316(12) 0.38858(14) -0.0891(4) 0.0901(16) Uani 1 1 d . . . . .
H9A H 0.361396 0.421103 -0.097211 0.108 Uiso 1 1 calc R U . . .
C10 C 0.43036(12) 0.38812(14) -0.1349(3) 0.0880(15) Uani 1 1 d . . . . .
H10A H 0.439756 0.419804 -0.174496 0.106 Uiso 1 1 calc R U . . .
C11 C 0.46366(9) 0.34052(10) -0.1219(2) 0.0421(6) Uani 1 1 d . . . . .
C12 C 0.44817(10) 0.29346(11) -0.0680(2) 0.0543(8) Uani 1 1 d . . . . .
H12A H 0.469586 0.260477 -0.061662 0.065 Uiso 1 1 calc R U . . .
C13 C 0.40087(10) 0.29366(12) -0.0222(3) 0.0596(9) Uani 1 1 d . . . . .
H13A H 0.391293 0.261134 0.015424 0.071 Uiso 1 1 calc R U . . .
C14 C 0.51543(8) 0.34029(10) -0.17051(18) 0.0336(5) Uani 1 1 d . . . . .
C15 C 0.06367(12) 0.52577(12) 0.2830(2) 0.0540(7) Uani 1 1 d . . . . .
C16 C 0.06417(12) 0.59319(12) 0.2725(2) 0.0519(7) Uani 1 1 d . . . . .
C17 C 0.02211(14) 0.62626(14) 0.2980(3) 0.0757(11) Uani 1 1 d . . . . .
H17A H -0.006914 0.607319 0.322210 0.091 Uiso 1 1 calc R U . . .
C18 C 0.02253(14) 0.68736(14) 0.2878(3) 0.0750(11) Uani 1 1 d . . . . .
H18A H -0.006673 0.709421 0.302560 0.090 Uiso 1 1 calc R U . . .
C19 C 0.06783(14) 0.71698(11) 0.2546(2) 0.0577(8) Uani 1 1 d . . . . .
C20 C 0.10849(14) 0.68299(14) 0.2319(3) 0.0639(9) Uani 1 1 d . . . . .
H20A H 0.138377 0.701394 0.210469 0.077 Uiso 1 1 calc R U . . .
C21 C 0.10730(13) 0.62031(13) 0.2397(3) 0.0582(8) Uani 1 1 d . . . . .
H21A H 0.135814 0.597737 0.222420 0.070 Uiso 1 1 calc R U . . .
C22 C 0.10297(8) 0.34818(9) 0.42410(14) 0.0247(4) Uani 1 1 d . . . . .
C23 C 0.10809(9) 0.31852(9) 0.52001(14) 0.0282(4) Uani 1 1 d . . . . .
C24 C 0.12275(11) 0.35150(10) 0.60074(16) 0.0416(6) Uani 1 1 d . . . . .
H24A H 0.130366 0.391875 0.594414 0.050 Uiso 1 1 calc R U . . .
C25 C 0.12600(12) 0.32443(10) 0.69018(16) 0.0438(6) Uani 1 1 d . . . . .
H25A H 0.136307 0.346677 0.743390 0.053 Uiso 1 1 calc R U . . .
C26 C 0.11403(10) 0.26429(10) 0.70144(15) 0.0354(5) Uani 1 1 d . . . . .
C27 C 0.10039(10) 0.23150(10) 0.61986(15) 0.0363(5) Uani 1 1 d . . . . .
H27A H 0.092904 0.191080 0.625898 0.044 Uiso 1 1 calc R U . . .
C28 C 0.09784(9) 0.25833(10) 0.52995(15) 0.0326(5) Uani 1 1 d . . . . .
H28A H 0.089202 0.235718 0.476088 0.039 Uiso 1 1 calc R U . . .


_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 1.9637(16) 6 ?
Co1 O1 1.9787(14) . ?
Co1 O5 1.9793(18) . ?
Co1 O7 2.0506(15) . ?
Co1 O8 2.3216(14) . ?
Mg1 O2 2.0257(15) 3 ?
Mg1 O2 2.0258(15) . ?
Mg1 O4 2.0325(15) 8_566 ?
Mg1 O4 2.0325(15) 6 ?
Mg1 O8 2.0686(13) . ?
Mg1 O8 2.0686(13) 3 ?
O1 C1 1.265(3) . ?
O2 C1 1.243(2) . ?
O3 C14 1.265(3) . ?
O4 C14 1.235(2) . ?
O5 C15 1.217(4) . ?
O6 C15 1.237(4) . ?
O7 C22 1.264(2) . ?
O8 C22 1.251(2) . ?
C1 C2 1.501(3) . ?
C2 C7 1.381(3) . ?
C2 C3 1.392(3) . ?
C3 C4 1.386(3) . ?
C3 H3A 0.9300 . ?
C4 C5 1.382(3) . ?
C4 H4A 0.9300 . ?
C5 C6 1.393(3) . ?
C5 C8 1.493(3) . ?
C6 C7 1.383(3) . ?
C6 H6A 0.9300 . ?
C7 H7A 0.9300 . ?
C8 C13 1.378(3) . ?
C8 C9 1.383(4) . ?
C9 C10 1.384(4) . ?
C9 H9A 0.9300 . ?
C10 C11 1.387(3) . ?
C10 H10A 0.9300 . ?
C11 C12 1.353(3) . ?
C11 C14 1.508(3) . ?
C12 C13 1.387(3) . ?
C12 H12A 0.9300 . ?
C13 H13A 0.9300 . ?
C15 C16 1.517(4) . ?
C16 C21 1.356(4) . ?
C16 C17 1.369(4) . ?
C17 C18 1.376(4) . ?
C17 H17A 0.9300 . ?
C18 C19 1.430(5) . ?
C18 H18A 0.9300 . ?
C19 C20 1.342(5) . ?
C19 C19 1.485(5) 3_565 ?
C20 C21 1.408(4) . ?
C20 H20A 0.9300 . ?
C21 H21A 0.9300 . ?
C22 C23 1.493(3) . ?
C23 C28 1.381(3) . ?
C23 C24 1.395(3) . ?
C24 C25 1.383(3) . ?
C24 H24A 0.9300 . ?
C25 C26 1.391(3) . ?
C25 H25A 0.9300 . ?
C26 C27 1.395(3) . ?
C26 C26 1.491(4) 3_556 ?
C27 C28 1.386(3) . ?
C27 H27A 0.9300 . ?
C28 H28A 0.9300 . ?

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 O1 115.50(9) 6 . ?
O3 Co1 O5 102.06(8) 6 . ?
O1 Co1 O5 94.70(8) . . ?
O3 Co1 O7 127.15(9) 6 . ?
O1 Co1 O7 107.85(7) . . ?
O5 Co1 O7 103.03(7) . . ?
O3 Co1 O8 90.17(6) 6 . ?
O1 Co1 O8 91.48(5) . . ?
O5 Co1 O8 162.25(7) . . ?
O7 Co1 O8 59.22(5) . . ?
O2 Mg1 O2 88.23(10) 3 . ?
O2 Mg1 O4 91.54(7) 3 8_566 ?
O2 Mg1 O4 179.13(6) . 8_566 ?
O2 Mg1 O4 179.13(6) 3 6 ?
O2 Mg1 O4 91.53(7) . 6 ?
O4 Mg1 O4 88.71(10) 8_566 6 ?
O2 Mg1 O8 91.25(6) 3 . ?
O2 Mg1 O8 90.02(6) . . ?
O4 Mg1 O8 89.15(6) 8_566 . ?
O4 Mg1 O8 89.59(6) 6 . ?
O2 Mg1 O8 90.02(6) 3 3 ?
O2 Mg1 O8 91.25(6) . 3 ?
O4 Mg1 O8 89.58(6) 8_566 3 ?
O4 Mg1 O8 89.15(6) 6 3 ?
O8 Mg1 O8 178.23(8) . 3 ?
C1 O1 Co1 129.48(13) . . ?
C1 O2 Mg1 142.30(14) . . ?
C14 O3 Co1 130.56(14) . 6_655 ?
C14 O4 Mg1 140.62(15) . 6_655 ?
C15 O5 Co1 113.11(19) . . ?
C22 O7 Co1 96.65(12) . . ?
C22 O8 Mg1 160.31(14) . . ?
C22 O8 Co1 84.57(11) . . ?
Mg1 O8 Co1 110.61(6) . . ?
O2 C1 O1 126.55(18) . . ?
O2 C1 C2 116.86(19) . . ?
O1 C1 C2 116.58(18) . . ?
C7 C2 C3 118.7(2) . . ?
C7 C2 C1 120.35(19) . . ?
C3 C2 C1 121.0(2) . . ?
C4 C3 C2 120.5(2) . . ?
C4 C3 H3A 119.8 . . ?
C2 C3 H3A 119.8 . . ?
C5 C4 C3 120.9(2) . . ?
C5 C4 H4A 119.5 . . ?
C3 C4 H4A 119.5 . . ?
C4 C5 C6 118.3(2) . . ?
C4 C5 C8 121.3(2) . . ?
C6 C5 C8 120.4(2) . . ?
C7 C6 C5 120.8(2) . . ?
C7 C6 H6A 119.6 . . ?
C5 C6 H6A 119.6 . . ?
C2 C7 C6 120.7(2) . . ?
C2 C7 H7A 119.6 . . ?
C6 C7 H7A 119.6 . . ?
C13 C8 C9 117.9(2) . . ?
C13 C8 C5 121.4(2) . . ?
C9 C8 C5 120.7(2) . . ?
C8 C9 C10 121.0(3) . . ?
C8 C9 H9A 119.5 . . ?
C10 C9 H9A 119.5 . . ?
C9 C10 C11 120.1(3) . . ?
C9 C10 H10A 119.9 . . ?
C11 C10 H10A 119.9 . . ?
C12 C11 C10 119.0(2) . . ?
C12 C11 C14 120.7(2) . . ?
C10 C11 C14 120.3(2) . . ?
C11 C12 C13 121.0(2) . . ?
C11 C12 H12A 119.5 . . ?
C13 C12 H12A 119.5 . . ?
C8 C13 C12 120.9(2) . . ?
C8 C13 H13A 119.5 . . ?
C12 C13 H13A 119.5 . . ?
O4 C14 O3 126.75(19) . . ?
O4 C14 C11 117.10(19) . . ?
O3 C14 C11 116.15(18) . . ?
O5 C15 O6 122.6(3) . . ?
O5 C15 C16 118.3(3) . . ?
O6 C15 C16 119.1(3) . . ?
C21 C16 C17 120.5(3) . . ?
C21 C16 C15 119.0(3) . . ?
C17 C16 C15 120.5(3) . . ?
C16 C17 C18 120.4(3) . . ?
C16 C17 H17A 119.8 . . ?
C18 C17 H17A 119.8 . . ?
C17 C18 C19 120.1(3) . . ?
C17 C18 H18A 120.0 . . ?
C19 C18 H18A 120.0 . . ?
C20 C19 C18 117.6(3) . . ?
C20 C19 C19 123.0(2) . 3_565 ?
C18 C19 C19 119.3(2) . 3_565 ?
C19 C20 C21 122.0(3) . . ?
C19 C20 H20A 119.0 . . ?
C21 C20 H20A 119.0 . . ?
C16 C21 C20 119.4(3) . . ?
C16 C21 H21A 120.3 . . ?
C20 C21 H21A 120.3 . . ?
O8 C22 O7 119.56(18) . . ?
O8 C22 C23 121.03(18) . . ?
O7 C22 C23 119.39(17) . . ?
C28 C23 C24 119.33(19) . . ?
C28 C23 C22 120.40(18) . . ?
C24 C23 C22 120.26(19) . . ?
C25 C24 C23 120.3(2) . . ?
C25 C24 H24A 119.9 . . ?
C23 C24 H24A 119.9 . . ?
C24 C25 C26 120.8(2) . . ?
C24 C25 H25A 119.6 . . ?
C26 C25 H25A 119.6 . . ?
C25 C26 C27 118.4(2) . . ?
C25 C26 C26 121.1(2) . 3_556 ?
C27 C26 C26 120.4(2) . 3_556 ?
C28 C27 C26 120.9(2) . . ?
C28 C27 H27A 119.5 . . ?
C26 C27 H27A 119.5 . . ?
C23 C28 C27 120.25(19) . . ?
C23 C28 H28A 119.9 . . ?
C27 C28 H28A 119.9 . . ?

_refine_diff_density_max         0.811
_refine_diff_density_min         -0.437
_refine_diff_density_rms         0.063



