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

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
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data_shelx_Complex1_Co2Gd_squeezed
_database_code_depnum_ccdc_archive 'CCDC 1429323'
_audit_update_record             
;
2016-04-23 deposited with the CCDC.
2016-04-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C28 H42 Co2 Gd N4 O13, N O3, 4(H2 O), 3(H4 C O)'
_chemical_formula_sum            'C31 H62 Co2 Gd N5 O23'
_chemical_formula_weight         1147.94

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'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Gd Gd -0.1653 3.9035 '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'

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

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   25.139(5)
_cell_length_b                   11.924(5)
_cell_length_c                   16.545(5)
_cell_angle_alpha                90
_cell_angle_beta                 116.956(5)
_cell_angle_gamma                90
_cell_volume                     4421(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    9110
_cell_measurement_theta_min      2.526
_cell_measurement_theta_max      28.356

_exptl_crystal_description       blocks
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.722
_exptl_crystal_F_000             2020
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_exptl_absorpt_coefficient_mu    2.294
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   PSI-SCAN
_exptl_absorpt_correction_T_min  0.700
_exptl_absorpt_correction_T_max  0.760
_exptl_absorpt_process_details   'North et al, 1968'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker SMART APEX'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            19398
_diffrn_reflns_av_unetI/netI     0.0378
_diffrn_reflns_av_R_equivalents  0.0414
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.124
_diffrn_reflns_theta_max         28.366
_diffrn_reflns_theta_full        25.240
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             5518
_reflns_number_gt                4740
_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       'Bruker APEX'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'DIAMOND 3.1 d'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_refine_special_details          SQUEEZE
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0555P)²+8.0089P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5518
_refine_ls_number_parameters     297
_refine_ls_number_restraints     38
_refine_ls_R_factor_all          0.0455
_refine_ls_R_factor_gt           0.0365
_refine_ls_wR_factor_ref         0.1036
_refine_ls_wR_factor_gt          0.0998
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_restrained_S_all      1.105
_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
Gd1 Gd 0.5000 0.75663(2) 0.7500 0.02512(8) Uani 1 2 d S T P . .
Co1 Co 0.38946(2) 0.93644(4) 0.70880(3) 0.03124(12) Uani 1 1 d . . . . .
O2 O 0.41063(10) 0.8399(2) 0.63848(16) 0.0303(5) Uani 1 1 d . . . . .
O3 O 0.46609(11) 0.9104(2) 0.80678(17) 0.0350(6) Uani 1 1 d . . . . .
O5 O 0.35324(11) 0.8180(2) 0.74548(17) 0.0353(6) Uani 1 1 d . . . . .
O1 O 0.45202(11) 0.6883(2) 0.57666(18) 0.0380(6) Uani 1 1 d . . . . .
O4 O 0.42158(11) 0.6830(2) 0.7751(2) 0.0449(7) Uani 1 1 d . . . . .
O7 O 0.5000 0.5557(3) 0.7500 0.0633(13) Uani 1 2 d S T P . .
N1 N 0.31292(14) 0.9708(3) 0.6176(2) 0.0406(7) Uani 1 1 d . . . . .
O6 O 0.42449(18) 1.0571(3) 0.6700(3) 0.0659(10) Uani 1 1 d D . . . .
C7 C 0.37286(14) 0.8032(3) 0.5572(2) 0.0271(6) Uani 1 1 d . . . . .
C2 C 0.39425(16) 0.7192(3) 0.5198(2) 0.0319(7) Uani 1 1 d . . . . .
N2 N 0.37208(16) 1.0300(3) 0.7869(3) 0.0481(9) Uani 1 1 d . . . . .
C6 C 0.31401(15) 0.8419(3) 0.5070(2) 0.0321(7) Uani 1 1 d . . . . .
C8 C 0.28740(17) 0.9260(3) 0.5397(3) 0.0398(9) Uani 1 1 d . . . . .
H8 H 0.2488 0.9491 0.5009 0.048 Uiso 1 1 calc R U . . .
C12 C 0.46702(19) 0.9490(4) 0.8887(3) 0.0461(10) Uani 1 1 d . . . . .
H12A H 0.5076 0.9656 0.9333 0.055 Uiso 0.51(5) 1 calc R U P A 1
H12B H 0.4508 0.8924 0.9135 0.055 Uiso 0.51(5) 1 calc R U P A 1
H12C H 0.4948 1.0111 0.9120 0.055 Uiso 0.49(5) 1 calc R U P A 2
H12D H 0.4816 0.8892 0.9332 0.055 Uiso 0.49(5) 1 calc R U P A 2
C3 C 0.35919(18) 0.6767(3) 0.4346(3) 0.0408(9) Uani 1 1 d . . . . .
H3 H 0.3744 0.6227 0.4102 0.049 Uiso 1 1 calc R U . . .
C5 C 0.27875(17) 0.7961(4) 0.4201(3) 0.0421(9) Uani 1 1 d . . . . .
H5 H 0.2399 0.8218 0.3861 0.051 Uiso 1 1 calc R U . . .
C4 C 0.30065(19) 0.7148(4) 0.3850(3) 0.0452(10) Uani 1 1 d . . . . .
H4 H 0.2765 0.6848 0.3281 0.054 Uiso 1 1 calc R U . . .
C13 C 0.37533(17) 0.7222(4) 0.7747(3) 0.0388(9) Uani 1 1 d . . . . .
C1 C 0.4761(2) 0.6012(4) 0.5413(3) 0.0600(13) Uani 1 1 d . . . . .
H1A H 0.5163 0.5847 0.5849 0.090 Uiso 1 1 calc R U . . .
H1B H 0.4521 0.5348 0.5296 0.090 Uiso 1 1 calc R U . . .
H1C H 0.4757 0.6265 0.4859 0.090 Uiso 1 1 calc R U . . .
C14 C 0.34163(19) 0.6501(4) 0.8110(3) 0.0541(12) Uani 1 1 d . . . . .
H14A H 0.3073 0.6903 0.8066 0.081 Uiso 1 1 calc R U . . .
H14B H 0.3290 0.5823 0.7761 0.081 Uiso 1 1 calc R U . . .
H14C H 0.3671 0.6319 0.8733 0.081 Uiso 1 1 calc R U . . .
C9 C 0.2821(2) 1.0539(4) 0.6478(4) 0.0583(12) Uani 1 1 d . . . . .
H9A H 0.2532 1.0167 0.6623 0.070 Uiso 0.51(5) 1 calc R U P A 1
H9B H 0.2612 1.1079 0.5999 0.070 Uiso 0.51(5) 1 calc R U P A 1
H9C H 0.2396 1.0391 0.6198 0.070 Uiso 0.49(5) 1 calc R U P A 2
H9D H 0.2885 1.1292 0.6315 0.070 Uiso 0.49(5) 1 calc R U P A 2
C2A C 0.3299(5) 1.1148(10) 0.7335(8) 0.071(3) Uani 0.5 1 d . . P B 1
H2A1 H 0.3496 1.1730 0.7161 0.085 Uiso 0.5 1 calc R U P B 1
H2A2 H 0.3114 1.1488 0.7677 0.085 Uiso 0.5 1 calc R U P B 1
C1B C 0.4274(5) 1.0587(10) 0.8642(7) 0.066(3) Uani 0.5 1 d . . P B 1
H1B1 H 0.4204 1.0815 0.9147 0.079 Uiso 0.5 1 calc R U P B 1
H1B2 H 0.4471 1.1196 0.8494 0.079 Uiso 0.5 1 calc R U P B 1
C1A C 0.4063(4) 0.9870(9) 0.8778(6) 0.053(2) Uani 0.5 1 d . . P B 2
H1A1 H 0.3855 0.9244 0.8881 0.064 Uiso 0.5 1 calc R U P B 2
H1A2 H 0.4113 1.0451 0.9218 0.064 Uiso 0.5 1 calc R U P B 2
C2B C 0.3083(4) 1.0424(9) 0.7481(6) 0.051(2) Uani 0.5 1 d . . P B 2
H2B1 H 0.2987 1.1082 0.7734 0.061 Uiso 0.5 1 calc R U P B 2
H2B2 H 0.2913 0.9774 0.7630 0.061 Uiso 0.5 1 calc R U P B 2
N1N N 0.3069(5) 0.8879(9) 0.9150(7) 0.094(3) Uani 0.5 1 d D U P C 1
O1N O 0.2766(4) 0.9338(8) 0.8414(6) 0.091(3) Uani 0.5 1 d D U P C 1
O2N O 0.3627(5) 0.9048(9) 0.9569(7) 0.105(3) Uani 0.5 1 d D U P C 1
O3N O 0.2779(6) 0.8236(9) 0.9458(7) 0.129(4) Uani 0.5 1 d D U P C 1
O3A O 0.3232(14) 0.8299(17) 0.9955(15) 0.129(4) Uani 0.3 1 d . U P D 2
O3B O 0.2319(11) 0.8811(18) 0.8486(16) 0.100(6) Uiso 0.25 1 d . . P E 2
O2A O 0.3730(15) 0.833(3) 1.020(2) 0.114(9) Uiso 0.2 1 d . . P F 3
O1A O 0.1948(12) 0.908(2) 0.8080(18) 0.117(7) Uiso 0.25 1 d . . P G 3
H1W H 0.403(5) 1.060(12) 0.6044(15) 0.26(6) Uiso 1 1 d D . . . .
H2W H 0.4658(18) 1.079(8) 0.711(6) 0.20(5) Uiso 1 1 d D . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Gd1 O4 2.360(3) . ?
Gd1 O4 2.360(3) 2_656 ?
Gd1 O2 2.383(2) . ?
Gd1 O2 2.383(2) 2_656 ?
Gd1 O3 2.386(3) 2_656 ?
Gd1 O3 2.386(3) . ?
Gd1 O7 2.396(4) . ?
Gd1 O1 2.685(3) 2_656 ?
Gd1 O1 2.685(3) . ?
Gd1 Co1 3.3267(9) 2_656 ?
Gd1 Co1 3.3267(8) . ?
Co1 O2 1.877(2) . ?
Co1 N1 1.875(3) . ?
Co1 O3 1.899(3) . ?
Co1 N2 1.901(3) . ?
Co1 O5 1.922(3) . ?
Co1 O6 1.941(4) . ?
O2 C7 1.320(4) . ?
O3 C12 1.422(5) . ?
O5 C13 1.267(5) . ?
O1 C2 1.375(4) . ?
O1 C1 1.452(4) . ?
O4 C13 1.250(5) . ?
N1 C8 1.269(5) . ?
N1 C9 1.476(5) . ?
O6 H1W 0.97(2) . ?
O6 H2W 0.98(2) . ?
C7 C2 1.406(5) . ?
C7 C6 1.406(5) . ?
C2 C3 1.377(5) . ?
N2 C1B 1.441(11) . ?
N2 C1A 1.447(11) . ?
N2 C2B 1.439(9) . ?
N2 C2A 1.442(11) . ?
C6 C5 1.413(5) . ?
C6 C8 1.440(5) . ?
C8 H8 0.9300 . ?
C12 C1A 1.523(10) . ?
C12 C1B 1.581(11) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C12 H12C 0.9700 . ?
C12 H12D 0.9700 . ?
C3 C4 1.397(6) . ?
C3 H3 0.9300 . ?
C5 C4 1.367(7) . ?
C5 H5 0.9300 . ?
C4 H4 0.9300 . ?
C13 C14 1.509(6) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C9 C2B 1.489(11) . ?
C9 C2A 1.560(13) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 H9C 0.9700 . ?
C9 H9D 0.9700 . ?
C2A H2A1 0.9700 . ?
C2A H2A2 0.9700 . ?
C1B H1B1 0.9700 . ?
C1B H1B2 0.9700 . ?
C1A H1A1 0.9700 . ?
C1A H1A2 0.9700 . ?
C2B H2B1 0.9700 . ?
C2B H2B2 0.9700 . ?
N1N O2N 1.267(11) . ?
N1N O1N 1.234(11) . ?
N1N O3N 1.311(12) . ?

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
O4 Gd1 O4 136.34(14) . 2_656 ?
O4 Gd1 O2 73.83(9) . . ?
O4 Gd1 O2 126.04(10) 2_656 . ?
O4 Gd1 O2 126.04(10) . 2_656 ?
O4 Gd1 O2 73.83(9) 2_656 2_656 ?
O2 Gd1 O2 130.77(12) . 2_656 ?
O4 Gd1 O3 146.16(9) . 2_656 ?
O4 Gd1 O3 74.96(10) 2_656 2_656 ?
O2 Gd1 O3 75.81(8) . 2_656 ?
O2 Gd1 O3 66.74(8) 2_656 2_656 ?
O4 Gd1 O3 74.96(10) . . ?
O4 Gd1 O3 146.16(9) 2_656 . ?
O2 Gd1 O3 66.75(8) . . ?
O2 Gd1 O3 75.81(8) 2_656 . ?
O3 Gd1 O3 79.63(13) 2_656 . ?
O4 Gd1 O7 68.17(7) . . ?
O4 Gd1 O7 68.17(7) 2_656 . ?
O2 Gd1 O7 114.62(6) . . ?
O2 Gd1 O7 114.62(6) 2_656 . ?
O3 Gd1 O7 140.19(7) 2_656 . ?
O3 Gd1 O7 140.19(7) . . ?
O4 Gd1 O1 72.90(9) . 2_656 ?
O4 Gd1 O1 93.92(10) 2_656 2_656 ?
O2 Gd1 O1 139.71(8) . 2_656 ?
O2 Gd1 O1 59.34(8) 2_656 2_656 ?
O3 Gd1 O1 125.87(8) 2_656 2_656 ?
O3 Gd1 O1 83.12(9) . 2_656 ?
O7 Gd1 O1 72.33(6) . 2_656 ?
O4 Gd1 O1 93.92(10) . . ?
O4 Gd1 O1 72.90(9) 2_656 . ?
O2 Gd1 O1 59.34(8) . . ?
O2 Gd1 O1 139.71(8) 2_656 . ?
O3 Gd1 O1 83.12(9) 2_656 . ?
O3 Gd1 O1 125.87(8) . . ?
O7 Gd1 O1 72.33(6) . . ?
O1 Gd1 O1 144.67(12) 2_656 . ?
O4 Gd1 Co1 152.92(8) . 2_656 ?
O4 Gd1 Co1 65.73(7) 2_656 2_656 ?
O2 Gd1 Co1 107.28(6) . 2_656 ?
O2 Gd1 Co1 33.50(6) 2_656 2_656 ?
O3 Gd1 Co1 34.04(6) 2_656 2_656 ?
O3 Gd1 Co1 80.71(7) . 2_656 ?
O7 Gd1 Co1 130.130(16) . 2_656 ?
O1 Gd1 Co1 92.73(5) 2_656 2_656 ?
O1 Gd1 Co1 110.09(6) . 2_656 ?
O4 Gd1 Co1 65.73(7) . . ?
O4 Gd1 Co1 152.92(8) 2_656 . ?
O2 Gd1 Co1 33.50(6) . . ?
O2 Gd1 Co1 107.28(6) 2_656 . ?
O3 Gd1 Co1 80.71(6) 2_656 . ?
O3 Gd1 Co1 34.04(6) . . ?
O7 Gd1 Co1 130.129(16) . . ?
O1 Gd1 Co1 110.09(6) 2_656 . ?
O1 Gd1 Co1 92.73(5) . . ?
Co1 Gd1 Co1 99.74(3) 2_656 . ?
O2 Co1 N1 96.41(13) . . ?
O2 Co1 O3 88.03(10) . . ?
N1 Co1 O3 175.52(13) . . ?
O2 Co1 N2 176.26(14) . . ?
N1 Co1 N2 87.14(15) . . ?
O3 Co1 N2 88.44(13) . . ?
O2 Co1 O5 93.04(11) . . ?
N1 Co1 O5 87.39(13) . . ?
O3 Co1 O5 93.02(11) . . ?
N2 Co1 O5 85.91(15) . . ?
O2 Co1 O6 87.21(14) . . ?
N1 Co1 O6 91.49(17) . . ?
O3 Co1 O6 88.09(16) . . ?
N2 Co1 O6 93.91(17) . . ?
O5 Co1 O6 178.87(15) . . ?
O2 Co1 Gd1 44.48(7) . . ?
N1 Co1 Gd1 139.76(10) . . ?
O3 Co1 Gd1 44.72(7) . . ?
N2 Co1 Gd1 131.81(11) . . ?
O5 Co1 Gd1 86.16(8) . . ?
O6 Co1 Gd1 94.78(11) . . ?
C7 O2 Co1 124.0(2) . . ?
C7 O2 Gd1 129.8(2) . . ?
Co1 O2 Gd1 102.02(10) . . ?
C12 O3 Co1 109.4(2) . . ?
C12 O3 Gd1 140.3(3) . . ?
Co1 O3 Gd1 101.24(10) . . ?
C13 O5 Co1 126.5(2) . . ?
C2 O1 C1 114.8(3) . . ?
C2 O1 Gd1 118.2(2) . . ?
C1 O1 Gd1 125.5(2) . . ?
C13 O4 Gd1 135.2(3) . . ?
C8 N1 C9 121.7(3) . . ?
C8 N1 Co1 126.0(3) . . ?
C9 N1 Co1 112.3(3) . . ?
Co1 O6 H1W 107(8) . . ?
Co1 O6 H2W 118(6) . . ?
H1W O6 H2W 129(10) . . ?
O2 C7 C2 116.3(3) . . ?
O2 C7 C6 124.8(3) . . ?
C2 C7 C6 118.9(3) . . ?
O1 C2 C7 112.7(3) . . ?
O1 C2 C3 126.1(3) . . ?
C7 C2 C3 121.2(3) . . ?
C1A N2 C2B 121.1(6) . . ?
C1B N2 C2A 121.6(8) . . ?
C1B N2 Co1 108.4(4) . . ?
C1A N2 Co1 106.7(4) . . ?
C2B N2 Co1 108.1(4) . . ?
C2A N2 Co1 109.1(5) . . ?
C7 C6 C5 118.7(4) . . ?
C7 C6 C8 123.4(3) . . ?
C5 C6 C8 117.9(3) . . ?
N1 C8 C6 124.6(3) . . ?
N1 C8 H8 117.7 . . ?
C6 C8 H8 117.7 . . ?
O3 C12 C1A 113.7(5) . . ?
O3 C12 C1B 106.7(5) . . ?
O3 C12 H12A 110.4 . . ?
C1B C12 H12A 110.4 . . ?
O3 C12 H12B 110.4 . . ?
C1B C12 H12B 110.4 . . ?
H12A C12 H12B 108.6 . . ?
O3 C12 H12C 108.8 . . ?
C1A C12 H12C 108.8 . . ?
O3 C12 H12D 108.8 . . ?
C1A C12 H12D 108.8 . . ?
H12C C12 H12D 107.7 . . ?
C2 C3 C4 119.8(4) . . ?
C2 C3 H3 120.1 . . ?
C4 C3 H3 120.1 . . ?
C4 C5 C6 121.2(4) . . ?
C4 C5 H5 119.4 . . ?
C6 C5 H5 119.4 . . ?
C5 C4 C3 120.1(4) . . ?
C5 C4 H4 120.0 . . ?
C3 C4 H4 120.0 . . ?
O4 C13 O5 125.8(4) . . ?
O4 C13 C14 118.3(4) . . ?
O5 C13 C14 115.9(4) . . ?
O1 C1 H1A 109.5 . . ?
O1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
O1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N1 C9 C2B 106.3(5) . . ?
N1 C9 C2A 108.3(5) . . ?
N1 C9 H9A 110.0 . . ?
C2A C9 H9A 110.0 . . ?
N1 C9 H9B 110.0 . . ?
C2A C9 H9B 110.0 . . ?
H9A C9 H9B 108.4 . . ?
N1 C9 H9C 110.5 . . ?
C2B C9 H9C 110.5 . . ?
N1 C9 H9D 110.5 . . ?
C2B C9 H9D 110.5 . . ?
H9C C9 H9D 108.7 . . ?
N2 C2A C9 106.2(7) . . ?
N2 C2A H2A1 110.5 . . ?
C9 C2A H2A1 110.5 . . ?
N2 C2A H2A2 110.5 . . ?
C9 C2A H2A2 110.5 . . ?
H2A1 C2A H2A2 108.7 . . ?
N2 C1B C12 105.9(7) . . ?
N2 C1B H1B1 110.6 . . ?
C12 C1B H1B1 110.6 . . ?
N2 C1B H1B2 110.6 . . ?
C12 C1B H1B2 110.6 . . ?
H1B1 C1B H1B2 108.7 . . ?
N2 C1A C12 108.7(6) . . ?
N2 C1A H1A1 110.0 . . ?
C12 C1A H1A1 110.0 . . ?
N2 C1A H1A2 110.0 . . ?
C12 C1A H1A2 110.0 . . ?
H1A1 C1A H1A2 108.3 . . ?
N2 C2B C9 110.3(6) . . ?
N2 C2B H2B1 109.6 . . ?
C9 C2B H2B1 109.6 . . ?
N2 C2B H2B2 109.6 . . ?
C9 C2B H2B2 109.6 . . ?
H2B1 C2B H2B2 108.1 . . ?
O2N N1N O1N 120.4(11) . . ?
O2N N1N O3N 123.6(11) . . ?
O1N N1N O3N 116.0(11) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 Co1 O2 C7 -10.0(3) . . . . ?
O3 Co1 O2 C7 170.6(3) . . . . ?
O5 Co1 O2 C7 77.7(3) . . . . ?
O6 Co1 O2 C7 -101.2(3) . . . . ?
Gd1 Co1 O2 C7 159.1(3) . . . . ?
N1 Co1 O2 Gd1 -169.10(13) . . . . ?
O3 Co1 O2 Gd1 11.53(11) . . . . ?
O5 Co1 O2 Gd1 -81.38(11) . . . . ?
O6 Co1 O2 Gd1 99.72(16) . . . . ?
O2 Co1 O3 C12 -166.0(3) . . . . ?
N2 Co1 O3 C12 12.8(3) . . . . ?
O5 Co1 O3 C12 -73.0(3) . . . . ?
O6 Co1 O3 C12 106.8(3) . . . . ?
Gd1 Co1 O3 C12 -154.5(3) . . . . ?
O2 Co1 O3 Gd1 -11.48(11) . . . . ?
N2 Co1 O3 Gd1 167.28(15) . . . . ?
O5 Co1 O3 Gd1 81.46(12) . . . . ?
O6 Co1 O3 Gd1 -98.76(15) . . . . ?
O2 Co1 N1 C8 6.7(4) . . . . ?
N2 Co1 N1 C8 -172.1(4) . . . . ?
O5 Co1 N1 C8 -86.1(4) . . . . ?
O6 Co1 N1 C8 94.1(4) . . . . ?
Gd1 Co1 N1 C8 -5.1(5) . . . . ?
O2 Co1 N1 C9 -176.7(3) . . . . ?
N2 Co1 N1 C9 4.4(3) . . . . ?
O5 Co1 N1 C9 90.5(3) . . . . ?
O6 Co1 N1 C9 -89.4(3) . . . . ?
Gd1 Co1 N1 C9 171.4(3) . . . . ?
Co1 O2 C7 C2 -171.2(2) . . . . ?
Gd1 O2 C7 C2 -18.3(4) . . . . ?
Co1 O2 C7 C6 8.7(5) . . . . ?
Gd1 O2 C7 C6 161.7(2) . . . . ?
C1 O1 C2 C7 179.6(4) . . . . ?
Gd1 O1 C2 C7 12.7(4) . . . . ?
C1 O1 C2 C3 -1.0(6) . . . . ?
Gd1 O1 C2 C3 -167.9(3) . . . . ?
O2 C7 C2 O1 0.9(5) . . . . ?
C6 C7 C2 O1 -179.1(3) . . . . ?
O2 C7 C2 C3 -178.5(3) . . . . ?
C6 C7 C2 C3 1.5(5) . . . . ?
O2 C7 C6 C5 179.1(3) . . . . ?
C2 C7 C6 C5 -0.9(5) . . . . ?
O2 C7 C6 C8 -1.1(5) . . . . ?
C2 C7 C6 C8 178.8(3) . . . . ?
C9 N1 C8 C6 -177.9(4) . . . . ?
Co1 N1 C8 C6 -1.6(6) . . . . ?
C7 C6 C8 N1 -2.8(6) . . . . ?
C5 C6 C8 N1 177.0(4) . . . . ?
Co1 O3 C12 C1A 6.6(6) . . . . ?
Gd1 O3 C12 C1A -132.0(6) . . . . ?
Co1 O3 C12 C1B -36.4(6) . . . . ?
Gd1 O3 C12 C1B -174.9(5) . . . . ?
O1 C2 C3 C4 178.8(4) . . . . ?
C7 C2 C3 C4 -1.9(6) . . . . ?
C7 C6 C5 C4 0.7(6) . . . . ?
C8 C6 C5 C4 -179.1(4) . . . . ?
C6 C5 C4 C3 -1.1(7) . . . . ?
C2 C3 C4 C5 1.6(6) . . . . ?
Gd1 O4 C13 O5 11.5(7) . . . . ?
Gd1 O4 C13 C14 -169.2(3) . . . . ?
Co1 O5 C13 O4 -8.7(6) . . . . ?
Co1 O5 C13 C14 171.9(3) . . . . ?
C8 N1 C9 C2B 150.5(6) . . . . ?
Co1 N1 C9 C2B -26.2(6) . . . . ?
C8 N1 C9 C2A -165.1(7) . . . . ?
Co1 N1 C9 C2A 18.2(7) . . . . ?
C1B N2 C2A C9 170.3(7) . . . . ?
Co1 N2 C2A C9 43.1(9) . . . . ?
N1 C9 C2A N2 -39.4(9) . . . . ?
C2A N2 C1B C12 -166.5(7) . . . . ?
Co1 N2 C1B C12 -39.1(9) . . . . ?
O3 C12 C1B N2 49.9(9) . . . . ?
C2B N2 C1A C12 162.2(6) . . . . ?
Co1 N2 C1A C12 38.2(8) . . . . ?
O3 C12 C1A N2 -30.1(9) . . . . ?
C1A N2 C2B C9 -162.8(7) . . . . ?
Co1 N2 C2B C9 -39.4(8) . . . . ?
N1 C9 C2B N2 42.5(8) . . . . ?

_refine_diff_density_max         1.428
_refine_diff_density_min         -0.568
_refine_diff_density_rms         0.119


_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_solvent_exptl_crystal_recrystallization_method 'MeOH, H2O'
_chemical_properties_physical    Heat-sensitive
_exptl_crystal_preparation       'Magnetic properties,Luminescent'
####################################################################### 
# 
# 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_Complex2_Co2Tb_squeezed
_database_code_depnum_ccdc_archive 'CCDC 1429324'
_audit_update_record             
;
2016-04-23 deposited with the CCDC.
2016-04-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C28 H42 Co2 N4 O13 Tb, N O3, 8(H2 O)'
_chemical_formula_sum            'C28 H58 Co2 N5 O24 Tb'
_chemical_formula_weight         1125.14

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'
Co Co 0.3494 0.9721 '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'
Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   25.196(5)
_cell_length_b                   11.877(5)
_cell_length_c                   16.580(5)
_cell_angle_alpha                90
_cell_angle_beta                 117.333(5)
_cell_angle_gamma                90
_cell_volume                     4408(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    2604
_cell_measurement_theta_min      2.614
_cell_measurement_theta_max      22.556

_exptl_crystal_description       blocks
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.695
_exptl_crystal_F_000             2008
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.11
_exptl_absorpt_coefficient_mu    2.400
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_correction_T_min  0.736
_exptl_absorpt_correction_T_max  0.768
_exptl_absorpt_process_details   'North et al, 1968'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker SMART APEX'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            13591
_diffrn_reflns_av_unetI/netI     0.0754
_diffrn_reflns_av_R_equivalents  0.0612
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.820
_diffrn_reflns_theta_max         28.344
_diffrn_reflns_theta_full        25.240
_diffrn_measured_fraction_theta_max 0.929
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.929
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.929
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             5119
_reflns_number_gt                3665
_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       'Bruker APEX'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_refine_special_details          
'The H2W-O6 distance was restricted using DFIX restraint. The ADPs were restricted to resonable values using EADP (for C13 C14 C2B C9 N1 C9 C1B C12 O3 C12) and ISOR (for N1N C1B O1B O2N O3A) restraints. SADI and RIGU restraints are used mandatorily for the mutually intertwined nitrate counter anion and water molecules. H atoms were not located for the ligand and hence fixed using HFIX command. Unassigned solvent molecules are squeezed out using SQUEEZE program in PLATON. Solvent accessible void volume (698 cA) contains 247 electrons, which could be assinged to approximately six water molecules per formula unit.'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0771P)²+19.7967P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5119
_refine_ls_number_parameters     250
_refine_ls_number_restraints     43
_refine_ls_R_factor_all          0.0915
_refine_ls_R_factor_gt           0.0601
_refine_ls_wR_factor_ref         0.1873
_refine_ls_wR_factor_gt          0.1444
_refine_ls_goodness_of_fit_ref   1.140
_refine_ls_restrained_S_all      1.137
_refine_ls_shift/su_max          0.020
_refine_ls_shift/su_mean         0.001

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
Tb1 Tb 0.5000 0.74178(4) 0.2500 0.03825(18) Uani 1 2 d S T P . .
Co1 Co 0.61055(5) 0.56227(8) 0.29165(7) 0.0441(3) Uani 1 1 d . . . . .
O3 O 0.5336(3) 0.5887(5) 0.1942(4) 0.0552(7) Uani 1 1 d . . . . .
O2 O 0.5894(2) 0.6602(4) 0.3618(3) 0.0434(11) Uani 1 1 d . . . . .
O4 O 0.6463(2) 0.6819(5) 0.2540(4) 0.0502(13) Uani 1 1 d . . . . .
O1 O 0.5483(2) 0.8119(5) 0.4243(4) 0.0532(14) Uani 1 1 d . . . . .
O5 O 0.5770(2) 0.8158(5) 0.2253(4) 0.0601(15) Uani 1 1 d . . . . .
N1 N 0.6874(3) 0.5280(6) 0.3832(5) 0.0552(7) Uani 1 1 d . . . . .
O6 O 0.5757(4) 0.4407(6) 0.3316(6) 0.078(2) Uani 1 1 d D . . . .
N2 N 0.6278(3) 0.4678(6) 0.2130(5) 0.0626(19) Uani 1 1 d . . . . .
C6 C 0.6859(3) 0.6578(6) 0.4935(5) 0.0462(18) Uani 1 1 d . . . . .
C7 C 0.6272(3) 0.6974(6) 0.4428(5) 0.0398(16) Uani 1 1 d . . . . .
C8 C 0.7131(4) 0.5744(7) 0.4608(6) 0.052(2) Uani 1 1 d . . . . .
H8 H 0.7531 0.5528 0.5002 0.062 Uiso 1 1 calc R U . . .
C2 C 0.6062(4) 0.7808(7) 0.4811(6) 0.0459(18) Uani 1 1 d . . . . .
C5 C 0.7214(4) 0.7049(8) 0.5803(5) 0.052(2) Uani 1 1 d . . . . .
H5 H 0.7614 0.6799 0.6147 0.062 Uiso 1 1 calc R U . . .
C12 C 0.5321(4) 0.5502(7) 0.1100(6) 0.0552(7) Uani 1 1 d . . . . .
H12A H 0.5473 0.6096 0.0842 0.066 Uiso 0.50(8) 1 calc R U P A 1
H12B H 0.4906 0.5317 0.0651 0.066 Uiso 0.50(8) 1 calc R U P A 1
H12C H 0.5038 0.4864 0.0861 0.066 Uiso 0.50(8) 1 calc R U P A 2
H12D H 0.5168 0.6118 0.0649 0.066 Uiso 0.50(8) 1 calc R U P A 2
C13 C 0.6242(4) 0.7766(8) 0.2265(6) 0.0552(7) Uani 1 1 d . . . . .
C4 C 0.6996(4) 0.7848(8) 0.6157(6) 0.061(2) Uani 1 1 d . . . . .
H4 H 0.7240 0.8142 0.6746 0.073 Uiso 1 1 calc R U . . .
C3 C 0.6414(4) 0.8236(7) 0.5655(6) 0.058(2) Uani 1 1 d . . . . .
H3 H 0.6261 0.8798 0.5900 0.070 Uiso 1 1 calc R U . . .
C1 C 0.5244(4) 0.8992(8) 0.4585(7) 0.075(3) Uani 1 1 d . . . . .
H1A H 0.4832 0.9156 0.4136 0.112 Uiso 1 1 calc R U . . .
H1B H 0.5250 0.8740 0.5152 0.112 Uiso 1 1 calc R U . . .
H1C H 0.5487 0.9673 0.4699 0.112 Uiso 1 1 calc R U . . .
C9 C 0.7181(4) 0.4447(7) 0.3522(6) 0.0552(7) Uani 1 1 d . . . . .
H9A H 0.7392 0.3886 0.4007 0.066 Uiso 0.50(8) 1 calc R U P A 1
H9B H 0.7481 0.4835 0.3392 0.066 Uiso 0.50(8) 1 calc R U P A 1
H9C H 0.7115 0.3675 0.3682 0.066 Uiso 0.50(8) 1 calc R U P A 2
H9D H 0.7617 0.4596 0.3816 0.066 Uiso 0.50(8) 1 calc R U P A 2
O7 O 0.5000 0.9424(7) 0.2500 0.089(3) Uani 1 2 d S T P . .
C14 C 0.6565(4) 0.8516(7) 0.1891(6) 0.0552(7) Uani 1 1 d . . . . .
H14A H 0.6920 0.8124 0.1935 0.083 Uiso 1 1 calc R U . . .
H14B H 0.6298 0.8692 0.1254 0.083 Uiso 1 1 calc R U . . .
H14C H 0.6687 0.9215 0.2243 0.083 Uiso 1 1 calc R U . . .
C1B C 0.5739(7) 0.4395(15) 0.1339(12) 0.0552(7) Uani 0.5 1 d . U P B 1
H1B1 H 0.5540 0.3744 0.1461 0.066 Uiso 0.5 1 calc R U P B 1
H1B2 H 0.5823 0.4201 0.0828 0.066 Uiso 0.5 1 calc R U P B 1
C2B C 0.6721(8) 0.3853(16) 0.2664(12) 0.0552(7) Uani 0.5 1 d . . P B 1
H2B1 H 0.6918 0.3545 0.2314 0.066 Uiso 0.5 1 calc R U P B 1
H2B2 H 0.6532 0.3224 0.2829 0.066 Uiso 0.5 1 calc R U P B 1
C2A C 0.6925(7) 0.4567(17) 0.2517(11) 0.058(4) Uani 0.5 1 d . . P B 2
H2A1 H 0.7094 0.5240 0.2368 0.070 Uiso 0.5 1 calc R U P B 2
H2A2 H 0.7026 0.3897 0.2259 0.070 Uiso 0.5 1 calc R U P B 2
C1A C 0.5928(8) 0.5129(14) 0.1206(12) 0.055(4) Uiso 0.5 1 d . . P B 2
H1A1 H 0.5876 0.4542 0.0752 0.065 Uiso 0.5 1 calc R U P B 2
H1A2 H 0.6139 0.5776 0.1108 0.065 Uiso 0.5 1 calc R U P B 2
N1N N 0.6939(8) 0.6137(16) 0.0857(12) 0.111(6) Uani 0.5 1 d D U P C 1
O1N O 0.7259(8) 0.5663(14) 0.1614(11) 0.110(5) Uani 0.5 1 d D U P C 1
O3N O 0.6382(8) 0.5957(15) 0.0448(11) 0.110(5) Uani 0.5 1 d D U P C 1
O2N O 0.7199(10) 0.6749(15) 0.0513(14) 0.122(6) Uani 0.5 1 d D U P C 1
O2B O 0.676(2) 0.667(3) 0.010(3) 0.130(13) Uiso 0.3 1 d . . P D 2
O1A O 0.7920(18) 0.598(3) 0.175(3) 0.125(12) Uiso 0.3 1 d . . P E 2
O1B O 0.763(3) 0.641(6) 0.135(5) 0.15(2) Uiso 0.2 1 d . . P F 3
O3A O 0.635(2) 0.678(4) -0.008(4) 0.111(15) Uiso 0.2 1 d . . P G 3
H1W H 0.534(3) 0.473(6) 0.323(5) 0.037(18) Uiso 1 1 d . . . . .
H2W H 0.595(11) 0.45(2) 0.396(2) 0.35(15) Uiso 1 1 d D . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tb1 O5 2.332(5) . ?
Tb1 O5 2.332(5) 2_655 ?
Tb1 O2 2.370(5) 2_655 ?
Tb1 O2 2.370(5) . ?
Tb1 O3 2.366(5) 2_655 ?
Tb1 O3 2.366(5) . ?
Tb1 O7 2.383(8) . ?
Tb1 O1 2.701(5) . ?
Tb1 O1 2.701(5) 2_655 ?
Tb1 Co1 3.3188(12) . ?
Tb1 Co1 3.3189(12) 2_655 ?
Co1 O3 1.895(6) . ?
Co1 N1 1.877(7) . ?
Co1 O2 1.887(5) . ?
Co1 N2 1.916(7) . ?
Co1 O4 1.933(5) . ?
Co1 O6 1.957(7) . ?
O3 C12 1.451(9) . ?
O2 C7 1.316(8) . ?
O4 C13 1.245(10) . ?
O1 C2 1.376(10) . ?
O1 C1 1.439(9) . ?
O5 C13 1.268(10) . ?
N1 C8 1.271(10) . ?
N1 C9 1.484(10) . ?
O6 H1W 1.08(7) . ?
O6 H2W 0.96(2) . ?
N2 C1B 1.430(18) . ?
N2 C2B 1.443(19) . ?
N2 C1A 1.474(19) . ?
N2 C2A 1.458(17) . ?
C6 C7 1.405(10) . ?
C6 C5 1.415(11) . ?
C6 C8 1.443(11) . ?
C7 C2 1.405(11) . ?
C8 H8 0.9500 . ?
C2 C3 1.364(11) . ?
C5 C4 1.358(13) . ?
C5 H5 0.9500 . ?
C12 C1A 1.523(18) . ?
C12 C1B 1.616(18) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C12 H12C 0.9900 . ?
C12 H12D 0.9900 . ?
C13 C14 1.519(12) . ?
C4 C3 1.391(13) . ?
C4 H4 0.9500 . ?
C3 H3 0.9500 . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C9 C2A 1.493(19) . ?
C9 C2B 1.534(19) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C9 H9C 0.9900 . ?
C9 H9D 0.9900 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C1B H1B1 0.9900 . ?
C1B H1B2 0.9900 . ?
C2B H2B1 0.9900 . ?
C2B H2B2 0.9900 . ?
C2A H2A1 0.9900 . ?
C2A H2A2 0.9900 . ?
C1A H1A1 0.9900 . ?
C1A H1A2 0.9900 . ?
N1N O1N 1.269(16) . ?
N1N O3N 1.266(16) . ?
N1N O2N 1.275(16) . ?

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
O5 Tb1 O5 135.7(3) . 2_655 ?
O5 Tb1 O2 125.9(2) . 2_655 ?
O5 Tb1 O2 73.89(19) 2_655 2_655 ?
O5 Tb1 O2 73.89(19) . . ?
O5 Tb1 O2 125.9(2) 2_655 . ?
O2 Tb1 O2 131.8(2) 2_655 . ?
O5 Tb1 O3 146.6(2) . 2_655 ?
O5 Tb1 O3 75.2(2) 2_655 2_655 ?
O2 Tb1 O3 67.02(19) 2_655 2_655 ?
O2 Tb1 O3 76.26(18) . 2_655 ?
O5 Tb1 O3 75.2(2) . . ?
O5 Tb1 O3 146.6(2) 2_655 . ?
O2 Tb1 O3 76.26(18) 2_655 . ?
O2 Tb1 O3 67.02(18) . . ?
O3 Tb1 O3 79.6(3) 2_655 . ?
O5 Tb1 O7 67.85(14) . . ?
O5 Tb1 O7 67.85(15) 2_655 . ?
O2 Tb1 O7 114.12(12) 2_655 . ?
O2 Tb1 O7 114.12(12) . . ?
O3 Tb1 O7 140.18(14) 2_655 . ?
O3 Tb1 O7 140.18(14) . . ?
O5 Tb1 O1 94.0(2) . . ?
O5 Tb1 O1 72.45(18) 2_655 . ?
O2 Tb1 O1 139.69(16) 2_655 . ?
O2 Tb1 O1 59.30(16) . . ?
O3 Tb1 O1 83.37(19) 2_655 . ?
O3 Tb1 O1 126.09(18) . . ?
O7 Tb1 O1 72.04(13) . . ?
O5 Tb1 O1 72.45(18) . 2_655 ?
O5 Tb1 O1 94.0(2) 2_655 2_655 ?
O2 Tb1 O1 59.30(16) 2_655 2_655 ?
O2 Tb1 O1 139.69(16) . 2_655 ?
O3 Tb1 O1 126.09(18) 2_655 2_655 ?
O3 Tb1 O1 83.37(19) . 2_655 ?
O7 Tb1 O1 72.04(13) . 2_655 ?
O1 Tb1 O1 144.1(3) . 2_655 ?
O5 Tb1 Co1 65.92(14) . . ?
O5 Tb1 Co1 153.19(16) 2_655 . ?
O2 Tb1 Co1 107.80(12) 2_655 . ?
O2 Tb1 Co1 33.81(12) . . ?
O3 Tb1 Co1 80.93(14) 2_655 . ?
O3 Tb1 Co1 33.99(14) . . ?
O7 Tb1 Co1 129.97(2) . . ?
O1 Tb1 Co1 93.02(12) . . ?
O1 Tb1 Co1 110.08(12) 2_655 . ?
O5 Tb1 Co1 153.19(16) . 2_655 ?
O5 Tb1 Co1 65.92(14) 2_655 2_655 ?
O2 Tb1 Co1 33.81(12) 2_655 2_655 ?
O2 Tb1 Co1 107.80(12) . 2_655 ?
O3 Tb1 Co1 33.98(14) 2_655 2_655 ?
O3 Tb1 Co1 80.93(14) . 2_655 ?
O7 Tb1 Co1 129.97(2) . 2_655 ?
O1 Tb1 Co1 110.08(12) . 2_655 ?
O1 Tb1 Co1 93.03(12) 2_655 2_655 ?
Co1 Tb1 Co1 100.06(5) . 2_655 ?
O3 Co1 N1 175.9(3) . . ?
O3 Co1 O2 87.5(2) . . ?
N1 Co1 O2 96.6(3) . . ?
O3 Co1 N2 88.8(3) . . ?
N1 Co1 N2 87.2(3) . . ?
O2 Co1 N2 176.0(3) . . ?
O3 Co1 O4 92.8(2) . . ?
N1 Co1 O4 87.7(3) . . ?
O2 Co1 O4 92.9(2) . . ?
N2 Co1 O4 85.7(3) . . ?
O3 Co1 O6 88.2(3) . . ?
N1 Co1 O6 91.3(3) . . ?
O2 Co1 O6 87.0(3) . . ?
N2 Co1 O6 94.3(3) . . ?
O4 Co1 O6 179.0(3) . . ?
O3 Co1 Tb1 44.28(17) . . ?
N1 Co1 Tb1 139.8(2) . . ?
O2 Co1 Tb1 44.33(16) . . ?
N2 Co1 Tb1 131.8(2) . . ?
O4 Co1 Tb1 86.09(16) . . ?
O6 Co1 Tb1 94.6(2) . . ?
C12 O3 Co1 109.5(5) . . ?
C12 O3 Tb1 139.6(5) . . ?
Co1 O3 Tb1 101.7(2) . . ?
C7 O2 Co1 124.0(5) . . ?
C7 O2 Tb1 130.1(4) . . ?
Co1 O2 Tb1 101.9(2) . . ?
C13 O4 Co1 125.8(5) . . ?
C2 O1 C1 115.3(6) . . ?
C2 O1 Tb1 117.7(4) . . ?
C1 O1 Tb1 125.4(5) . . ?
C13 O5 Tb1 135.1(5) . . ?
C8 N1 C9 122.4(7) . . ?
C8 N1 Co1 125.5(6) . . ?
C9 N1 Co1 111.9(5) . . ?
Co1 O6 H1W 105(4) . . ?
Co1 O6 H2W 104(10) . . ?
H1W O6 H2W 95(10) . . ?
C1B N2 C2B 123.0(11) . . ?
C1A N2 C2A 120.3(11) . . ?
C1B N2 Co1 110.2(8) . . ?
C2B N2 Co1 109.5(8) . . ?
C1A N2 Co1 106.2(8) . . ?
C2A N2 Co1 108.1(8) . . ?
C7 C6 C5 118.4(7) . . ?
C7 C6 C8 123.8(7) . . ?
C5 C6 C8 117.8(8) . . ?
O2 C7 C6 124.6(7) . . ?
O2 C7 C2 116.9(7) . . ?
C6 C7 C2 118.5(7) . . ?
N1 C8 C6 124.7(8) . . ?
N1 C8 H8 117.7 . . ?
C6 C8 H8 117.7 . . ?
O1 C2 C3 126.0(7) . . ?
O1 C2 C7 112.4(7) . . ?
C3 C2 C7 121.6(8) . . ?
C4 C5 C6 121.7(8) . . ?
C4 C5 H5 119.2 . . ?
C6 C5 H5 119.2 . . ?
C1A C12 O3 113.5(9) . . ?
O3 C12 C1B 107.1(8) . . ?
O3 C12 H12A 110.3 . . ?
C1B C12 H12A 110.3 . . ?
O3 C12 H12B 110.3 . . ?
C1B C12 H12B 110.3 . . ?
H12A C12 H12B 108.5 . . ?
C1A C12 H12C 108.9 . . ?
O3 C12 H12C 108.9 . . ?
C1A C12 H12D 108.9 . . ?
O3 C12 H12D 108.9 . . ?
H12C C12 H12D 107.7 . . ?
O5 C13 O4 126.6(8) . . ?
O5 C13 C14 116.9(8) . . ?
O4 C13 C14 116.4(7) . . ?
C5 C4 C3 119.8(8) . . ?
C5 C4 H4 120.1 . . ?
C3 C4 H4 120.1 . . ?
C2 C3 C4 120.0(8) . . ?
C2 C3 H3 120.0 . . ?
C4 C3 H3 120.0 . . ?
O1 C1 H1A 109.5 . . ?
O1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
O1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N1 C9 C2A 107.2(9) . . ?
N1 C9 C2B 109.6(9) . . ?
N1 C9 H9A 109.7 . . ?
C2B C9 H9A 109.7 . . ?
N1 C9 H9B 109.7 . . ?
C2B C9 H9B 109.7 . . ?
H9A C9 H9B 108.2 . . ?
N1 C9 H9C 110.3 . . ?
C2A C9 H9C 110.3 . . ?
N1 C9 H9D 110.3 . . ?
C2A C9 H9D 110.3 . . ?
H9C C9 H9D 108.5 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N2 C1B C12 105.7(11) . . ?
N2 C1B H1B1 110.6 . . ?
C12 C1B H1B1 110.6 . . ?
N2 C1B H1B2 110.6 . . ?
C12 C1B H1B2 110.6 . . ?
H1B1 C1B H1B2 108.7 . . ?
N2 C2B C9 107.4(12) . . ?
N2 C2B H2B1 110.2 . . ?
C9 C2B H2B1 110.2 . . ?
N2 C2B H2B2 110.2 . . ?
C9 C2B H2B2 110.2 . . ?
H2B1 C2B H2B2 108.5 . . ?
N2 C2A C9 108.8(11) . . ?
N2 C2A H2A1 109.9 . . ?
C9 C2A H2A1 109.9 . . ?
N2 C2A H2A2 109.9 . . ?
C9 C2A H2A2 109.9 . . ?
H2A1 C2A H2A2 108.3 . . ?
N2 C1A C12 108.4(11) . . ?
N2 C1A H1A1 110.0 . . ?
C12 C1A H1A1 110.0 . . ?
N2 C1A H1A2 110.0 . . ?
C12 C1A H1A2 110.0 . . ?
H1A1 C1A H1A2 108.4 . . ?
O1N N1N O3N 120.0(13) . . ?
O1N N1N O2N 118.2(13) . . ?
O3N N1N O2N 121.8(13) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2 Co1 O3 C12 165.3(5) . . . . ?
N2 Co1 O3 C12 -13.2(5) . . . . ?
O4 Co1 O3 C12 72.5(5) . . . . ?
O6 Co1 O3 C12 -107.6(5) . . . . ?
Tb1 Co1 O3 C12 154.0(6) . . . . ?
O2 Co1 O3 Tb1 11.3(2) . . . . ?
N2 Co1 O3 Tb1 -167.2(3) . . . . ?
O4 Co1 O3 Tb1 -81.5(2) . . . . ?
O6 Co1 O3 Tb1 98.4(3) . . . . ?
O3 Co1 O2 C7 -170.6(5) . . . . ?
N1 Co1 O2 C7 10.0(6) . . . . ?
O4 Co1 O2 C7 -78.0(5) . . . . ?
O6 Co1 O2 C7 101.0(6) . . . . ?
Tb1 Co1 O2 C7 -159.3(6) . . . . ?
O3 Co1 O2 Tb1 -11.3(2) . . . . ?
N1 Co1 O2 Tb1 169.3(3) . . . . ?
O4 Co1 O2 Tb1 81.3(2) . . . . ?
O6 Co1 O2 Tb1 -99.6(3) . . . . ?
O2 Co1 N1 C8 -7.3(7) . . . . ?
N2 Co1 N1 C8 171.3(7) . . . . ?
O4 Co1 N1 C8 85.4(7) . . . . ?
O6 Co1 N1 C8 -94.5(7) . . . . ?
Tb1 Co1 N1 C8 4.3(9) . . . . ?
O2 Co1 N1 C9 177.4(5) . . . . ?
N2 Co1 N1 C9 -4.1(6) . . . . ?
O4 Co1 N1 C9 -89.9(5) . . . . ?
O6 Co1 N1 C9 90.2(6) . . . . ?
Tb1 Co1 N1 C9 -171.1(4) . . . . ?
Co1 O2 C7 C6 -9.3(10) . . . . ?
Tb1 O2 C7 C6 -162.5(5) . . . . ?
Co1 O2 C7 C2 172.1(5) . . . . ?
Tb1 O2 C7 C2 18.9(9) . . . . ?
C5 C6 C7 O2 -179.3(7) . . . . ?
C8 C6 C7 O2 3.0(11) . . . . ?
C5 C6 C7 C2 -0.7(11) . . . . ?
C8 C6 C7 C2 -178.5(7) . . . . ?
C9 N1 C8 C6 178.4(7) . . . . ?
Co1 N1 C8 C6 3.5(12) . . . . ?
C7 C6 C8 N1 0.2(12) . . . . ?
C5 C6 C8 N1 -177.5(8) . . . . ?
C1 O1 C2 C3 1.2(12) . . . . ?
Tb1 O1 C2 C3 167.7(7) . . . . ?
C1 O1 C2 C7 -178.5(7) . . . . ?
Tb1 O1 C2 C7 -12.1(8) . . . . ?
O2 C7 C2 O1 -1.5(10) . . . . ?
C6 C7 C2 O1 179.8(6) . . . . ?
O2 C7 C2 C3 178.7(7) . . . . ?
C6 C7 C2 C3 0.0(12) . . . . ?
C7 C6 C5 C4 1.3(12) . . . . ?
C8 C6 C5 C4 179.1(8) . . . . ?
Co1 O3 C12 C1A -6.7(10) . . . . ?
Tb1 O3 C12 C1A 131.8(9) . . . . ?
Co1 O3 C12 C1B 35.0(9) . . . . ?
Tb1 O3 C12 C1B 173.5(8) . . . . ?
Tb1 O5 C13 O4 -9.8(15) . . . . ?
Tb1 O5 C13 C14 169.1(6) . . . . ?
Co1 O4 C13 O5 6.6(13) . . . . ?
Co1 O4 C13 C14 -172.4(5) . . . . ?
C6 C5 C4 C3 -1.1(13) . . . . ?
O1 C2 C3 C4 -179.6(8) . . . . ?
C7 C2 C3 C4 0.2(13) . . . . ?
C5 C4 C3 C2 0.4(13) . . . . ?
C8 N1 C9 C2A -148.7(11) . . . . ?
Co1 N1 C9 C2A 26.8(11) . . . . ?
C8 N1 C9 C2B 167.4(10) . . . . ?
Co1 N1 C9 C2B -17.1(11) . . . . ?
C2B N2 C1B C12 167.7(11) . . . . ?
Co1 N2 C1B C12 36.1(12) . . . . ?
O3 C12 C1B N2 -46.7(12) . . . . ?
C1B N2 C2B C9 -171.7(11) . . . . ?
Co1 N2 C2B C9 -39.9(13) . . . . ?
N1 C9 C2B N2 36.8(14) . . . . ?
C1A N2 C2A C9 162.3(12) . . . . ?
Co1 N2 C2A C9 40.1(15) . . . . ?
N1 C9 C2A N2 -43.2(15) . . . . ?
C2A N2 C1A C12 -161.8(11) . . . . ?
Co1 N2 C1A C12 -38.8(12) . . . . ?
O3 C12 C1A N2 30.5(14) . . . . ?

_refine_diff_density_max         1.388
_refine_diff_density_min         -1.754
_refine_diff_density_rms         0.180


####################################################################### 
# 
# 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_Complex3_Co2Ho_squeezed
_database_code_depnum_ccdc_archive 'CCDC 1429325'
_audit_update_record             
;
2016-04-23 deposited with the CCDC.
2016-04-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C28 H42 Co2 Ho N4 O13, N O3, 2(H2 O), 4(C H4 O)'
_chemical_formula_sum            'C32 H62 Co2 Ho N5 O22'
_chemical_formula_weight         1151.65

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'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ho Ho -0.2175 4.6783 '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'

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

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   25.251(5)
_cell_length_b                   11.921(5)
_cell_length_c                   16.799(5)
_cell_angle_alpha                90
_cell_angle_beta                 117.387(5)
_cell_angle_gamma                90
_cell_volume                     4490(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9480
_cell_measurement_theta_min      2.489
_cell_measurement_theta_max      28.294

_exptl_crystal_description       blocks
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.703
_exptl_crystal_F_000             2016
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.07
_exptl_absorpt_coefficient_mu    2.543
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_correction_T_min  0.894
_exptl_absorpt_correction_T_max  0.930
_exptl_absorpt_process_details   'North et al, 1968'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker SMART APEX'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            19343
_diffrn_reflns_av_unetI/netI     0.0399
_diffrn_reflns_av_R_equivalents  0.0387
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.113
_diffrn_reflns_theta_max         28.399
_diffrn_reflns_theta_full        25.240
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             5623
_reflns_number_gt                4765
_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       'Bruker APEX'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'DIAMOND 3.1 d'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_refine_special_details          
'The ADPs were restricted to resonable values using EADP (for C1A C9 C1A N2) and ISOR (for C1B C1A) restraints. SADI and RIGU restraints are used mandatorily for the mutually intertwined nitrate counter anion and water molecules. H atoms were not located for the ligand and hence fixed using HFIX command. Solvent accessible void volume (743 cA) contains 286 electrons, which could be assinged to four MeOH per formula unit.'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0494P)²+3.6889P] 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         5623
_refine_ls_number_parameters     277
_refine_ls_number_restraints     37
_refine_ls_R_factor_all          0.0430
_refine_ls_R_factor_gt           0.0350
_refine_ls_wR_factor_ref         0.0970
_refine_ls_wR_factor_gt          0.0933
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_restrained_S_all      1.043
_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
Ho1 Ho 0.5000 0.74103(2) 0.2500 0.04211(8) Uani 1 2 d S T P . .
Co1 Co 0.61008(2) 0.56507(4) 0.29097(3) 0.04742(12) Uani 1 1 d . . . . .
O2 O 0.58866(10) 0.6612(2) 0.35975(14) 0.0473(5) Uani 1 1 d . . . . .
O3 O 0.53332(10) 0.5896(2) 0.19489(15) 0.0485(5) Uani 1 1 d . . . . .
O4 O 0.64543(11) 0.6845(3) 0.25513(17) 0.0564(6) Uani 1 1 d . . . . .
O1 O 0.54823(12) 0.8117(3) 0.42200(18) 0.0659(7) Uani 1 1 d . . . . .
O5 O 0.57521(12) 0.8155(3) 0.2239(2) 0.0715(8) Uani 1 1 d . . . . .
N1 N 0.68718(14) 0.5309(3) 0.3808(2) 0.0620(8) Uani 1 1 d . . . . .
O6 O 0.57605(16) 0.4431(3) 0.3309(3) 0.0880(10) Uani 1 1 d . . . . .
C7 C 0.62687(14) 0.6970(3) 0.4410(2) 0.0451(7) Uani 1 1 d . . . . .
C6 C 0.68532(15) 0.6574(3) 0.4908(2) 0.0526(8) Uani 1 1 d . . . . .
N2 N 0.62714(16) 0.4720(4) 0.2135(3) 0.0784(8) Uani 1 1 d . . . . .
C8 C 0.71182(17) 0.5752(4) 0.4578(3) 0.0612(10) Uani 1 1 d . . . . .
H8 H 0.7513 0.5519 0.4973 0.073 Uiso 1 1 calc R U . . .
C2 C 0.60509(16) 0.7796(3) 0.4788(2) 0.0516(8) Uani 1 1 d . . . . .
C12 C 0.53275(19) 0.5536(5) 0.1136(3) 0.0720(12) Uani 1 1 d . . . . .
H12A H 0.5493 0.6126 0.0901 0.086 Uiso 0.61(5) 1 calc R U P A 1
H12B H 0.4915 0.5369 0.0678 0.086 Uiso 0.61(5) 1 calc R U P A 1
H12C H 0.5200 0.6171 0.0709 0.086 Uiso 0.39(5) 1 calc R U P A 2
H12D H 0.5028 0.4932 0.0870 0.086 Uiso 0.39(5) 1 calc R U P A 2
C13 C 0.62268(17) 0.7790(4) 0.2264(3) 0.0613(10) Uani 1 1 d . . . . .
C3 C 0.6404(2) 0.8203(4) 0.5633(3) 0.0682(11) Uani 1 1 d . . . . .
H3 H 0.6253 0.8753 0.5884 0.082 Uiso 1 1 calc R U . . .
C5 C 0.72030(18) 0.7016(4) 0.5768(3) 0.0656(11) Uani 1 1 d . . . . .
H5 H 0.7600 0.6756 0.6111 0.079 Uiso 1 1 calc R U . . .
C4 C 0.6984(2) 0.7809(4) 0.6122(3) 0.0740(13) Uani 1 1 d . . . . .
H4 H 0.7229 0.8094 0.6706 0.089 Uiso 1 1 calc R U . . .
C1 C 0.5246(2) 0.8968(5) 0.4571(4) 0.108(2) Uani 1 1 d . . . . .
H1A H 0.4838 0.9152 0.4125 0.163 Uiso 1 1 calc R U . . .
H1B H 0.5243 0.8693 0.5118 0.163 Uiso 1 1 calc R U . . .
H1C H 0.5495 0.9642 0.4709 0.163 Uiso 1 1 calc R U . . .
C14 C 0.6554(2) 0.8542(5) 0.1915(4) 0.0891(16) Uani 1 1 d . . . . .
H14A H 0.6913 0.8160 0.1973 0.134 Uiso 1 1 calc R U . . .
H14B H 0.6294 0.8716 0.1283 0.134 Uiso 1 1 calc R U . . .
H14C H 0.6666 0.9240 0.2263 0.134 Uiso 1 1 calc R U . . .
C9 C 0.7175(2) 0.4490(5) 0.3499(3) 0.0784(8) Uani 1 1 d . . . . .
H9A H 0.7395 0.3937 0.3979 0.094 Uiso 0.61(5) 1 calc R U P A 1
H9B H 0.7465 0.4879 0.3352 0.094 Uiso 0.61(5) 1 calc R U P A 1
H9C H 0.7606 0.4664 0.3763 0.094 Uiso 0.39(5) 1 calc R U P A 2
H9D H 0.7129 0.3723 0.3685 0.094 Uiso 0.39(5) 1 calc R U P A 2
O7 O 0.5000 0.9410(4) 0.2500 0.116(2) Uani 1 2 d S T P . .
C2A C 0.5721(5) 0.4452(11) 0.1367(8) 0.088(3) Uani 0.5 1 d . . P B 1
H2A1 H 0.5793 0.4236 0.0856 0.105 Uiso 0.5 1 calc R U P B 1
H2A2 H 0.5520 0.3822 0.1503 0.105 Uiso 0.5 1 calc R U P B 1
C1B C 0.6699(5) 0.3882(9) 0.2655(8) 0.097(4) Uani 0.5 1 d . U P B 1
H1B1 H 0.6885 0.3546 0.2305 0.117 Uiso 0.5 1 calc R U P B 1
H1B2 H 0.6503 0.3278 0.2830 0.117 Uiso 0.5 1 calc R U P B 1
C1A C 0.6898(4) 0.4565(11) 0.2514(7) 0.0784(8) Uani 0.5 1 d . U P B 2
H1A1 H 0.6982 0.3868 0.2271 0.094 Uiso 0.5 1 calc R U P B 2
H1A2 H 0.7076 0.5200 0.2341 0.094 Uiso 0.5 1 calc R U P B 2
C2B C 0.5917(5) 0.5113(12) 0.1249(7) 0.085(3) Uani 0.5 1 d . . P B 2
H2B1 H 0.6129 0.5724 0.1116 0.102 Uiso 0.5 1 calc R U P B 2
H2B2 H 0.5851 0.4495 0.0819 0.102 Uiso 0.5 1 calc R U P B 2
N1N N 0.6945(5) 0.6131(10) 0.0878(8) 0.120(3) Uani 0.5 1 d D U P C 1
O1N O 0.6406(5) 0.5942(10) 0.0496(7) 0.138(3) Uani 0.5 1 d D U P C 1
O2N O 0.7246(5) 0.5690(10) 0.1603(7) 0.135(3) Uani 0.5 1 d D U P C 1
O3N O 0.7205(7) 0.6691(13) 0.0552(10) 0.168(5) Uani 0.5 1 d D U P C 1
O1A O 0.6787(16) 0.667(3) 0.014(2) 0.195(12) Uiso 0.3 1 d . . P D 2
O2B O 0.7584(15) 0.625(3) 0.137(3) 0.218(13) Uiso 0.3 1 d . . P E 2
O1B O 0.6350(12) 0.670(3) -0.0016(18) 0.159(12) Uiso 0.2 1 d D . P F 3
O2A O 0.7924(15) 0.589(3) 0.182(2) 0.144(10) Uiso 0.2 1 d . . P G 3


_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
Ho1 O5 2.314(3) . ?
Ho1 O5 2.314(3) 2_655 ?
Ho1 O2 2.349(2) 2_655 ?
Ho1 O2 2.349(2) . ?
Ho1 O3 2.354(2) . ?
Ho1 O3 2.354(2) 2_655 ?
Ho1 O7 2.384(5) . ?
Ho1 O1 2.703(3) . ?
Ho1 O1 2.703(3) 2_655 ?
Ho1 Co1 3.2923(8) . ?
Ho1 Co1 3.2924(8) 2_655 ?
Co1 O2 1.875(2) . ?
Co1 N1 1.879(3) . ?
Co1 O3 1.889(2) . ?
Co1 N2 1.904(4) . ?
Co1 O4 1.919(3) . ?
Co1 O6 1.958(4) . ?
O2 C7 1.328(4) . ?
O3 C12 1.425(4) . ?
O4 C13 1.256(5) . ?
O1 C2 1.363(5) . ?
O1 C1 1.435(5) . ?
O5 C13 1.257(5) . ?
N1 C8 1.265(5) . ?
N1 C9 1.475(5) . ?
C7 C2 1.414(5) . ?
C7 C6 1.401(5) . ?
C6 C8 1.434(6) . ?
C6 C5 1.405(5) . ?
N2 C1A 1.420(9) . ?
N2 C1B 1.435(11) . ?
N2 C2A 1.432(11) . ?
N2 C2B 1.417(12) . ?
C8 H8 0.9500 . ?
C2 C3 1.371(5) . ?
C12 C2B 1.498(11) . ?
C12 C2A 1.565(13) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C12 H12C 0.9900 . ?
C12 H12D 0.9900 . ?
C13 C14 1.508(6) . ?
C3 C4 1.391(7) . ?
C3 H3 0.9500 . ?
C5 C4 1.362(8) . ?
C5 H5 0.9500 . ?
C4 H4 0.9500 . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C9 C1A 1.474(11) . ?
C9 C1B 1.554(13) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C9 H9C 0.9900 . ?
C9 H9D 0.9900 . ?
C2A H2A1 0.9900 . ?
C2A H2A2 0.9900 . ?
C1B H1B1 0.9900 . ?
C1B H1B2 0.9900 . ?
C1A H1A1 0.9900 . ?
C1A H1A2 0.9900 . ?
C2B H2B1 0.9900 . ?
C2B H2B2 0.9900 . ?
N1N O3N 1.227(13) . ?
N1N O2N 1.220(11) . ?
N1N O1N 1.230(12) . ?
O1N O3N 2.169(16) . ?

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
O5 Ho1 O5 134.87(17) . 2_655 ?
O5 Ho1 O2 125.14(10) . 2_655 ?
O5 Ho1 O2 74.64(9) 2_655 2_655 ?
O5 Ho1 O2 74.64(9) . . ?
O5 Ho1 O2 125.14(10) 2_655 . ?
O2 Ho1 O2 132.23(12) 2_655 . ?
O5 Ho1 O3 75.32(10) . . ?
O5 Ho1 O3 147.35(9) 2_655 . ?
O2 Ho1 O3 76.40(8) 2_655 . ?
O2 Ho1 O3 67.30(8) . . ?
O5 Ho1 O3 147.35(9) . 2_655 ?
O5 Ho1 O3 75.32(11) 2_655 2_655 ?
O2 Ho1 O3 67.30(8) 2_655 2_655 ?
O2 Ho1 O3 76.40(8) . 2_655 ?
O3 Ho1 O3 79.85(12) . 2_655 ?
O5 Ho1 O7 67.44(8) . . ?
O5 Ho1 O7 67.44(8) 2_655 . ?
O2 Ho1 O7 113.88(6) 2_655 . ?
O2 Ho1 O7 113.88(6) . . ?
O3 Ho1 O7 140.07(6) . . ?
O3 Ho1 O7 140.07(6) 2_655 . ?
O5 Ho1 O1 94.45(11) . . ?
O5 Ho1 O1 71.53(9) 2_655 . ?
O2 Ho1 O1 139.76(8) 2_655 . ?
O2 Ho1 O1 59.28(8) . . ?
O3 Ho1 O1 126.36(8) . . ?
O3 Ho1 O1 83.42(10) 2_655 . ?
O7 Ho1 O1 71.83(7) . . ?
O5 Ho1 O1 71.53(9) . 2_655 ?
O5 Ho1 O1 94.45(11) 2_655 2_655 ?
O2 Ho1 O1 59.28(8) 2_655 2_655 ?
O2 Ho1 O1 139.76(8) . 2_655 ?
O3 Ho1 O1 83.42(10) . 2_655 ?
O3 Ho1 O1 126.36(8) 2_655 2_655 ?
O7 Ho1 O1 71.83(7) . 2_655 ?
O1 Ho1 O1 143.66(14) . 2_655 ?
O5 Ho1 Co1 66.20(8) . . ?
O5 Ho1 Co1 153.18(9) 2_655 . ?
O2 Ho1 Co1 108.32(7) 2_655 . ?
O2 Ho1 Co1 33.88(5) . . ?
O3 Ho1 Co1 34.25(5) . . ?
O3 Ho1 Co1 81.34(6) 2_655 . ?
O7 Ho1 Co1 129.576(16) . . ?
O1 Ho1 Co1 93.05(6) . . ?
O1 Ho1 Co1 110.12(7) 2_655 . ?
O5 Ho1 Co1 153.18(9) . 2_655 ?
O5 Ho1 Co1 66.20(8) 2_655 2_655 ?
O2 Ho1 Co1 33.88(5) 2_655 2_655 ?
O2 Ho1 Co1 108.32(7) . 2_655 ?
O3 Ho1 Co1 81.34(6) . 2_655 ?
O3 Ho1 Co1 34.25(5) 2_655 2_655 ?
O7 Ho1 Co1 129.576(17) . 2_655 ?
O1 Ho1 Co1 110.12(7) . 2_655 ?
O1 Ho1 Co1 93.05(6) 2_655 2_655 ?
Co1 Ho1 Co1 100.85(3) . 2_655 ?
O2 Co1 N1 97.11(13) . . ?
O2 Co1 O3 87.61(10) . . ?
N1 Co1 O3 175.19(13) . . ?
O2 Co1 N2 175.79(14) . . ?
N1 Co1 N2 86.90(15) . . ?
O3 Co1 N2 88.39(13) . . ?
O2 Co1 O4 92.71(12) . . ?
N1 Co1 O4 87.30(14) . . ?
O3 Co1 O4 93.41(11) . . ?
N2 Co1 O4 86.18(17) . . ?
O2 Co1 O6 86.93(14) . . ?
N1 Co1 O6 91.14(15) . . ?
O3 Co1 O6 88.20(13) . . ?
N2 Co1 O6 94.29(18) . . ?
O4 Co1 O6 178.34(14) . . ?
O2 Co1 Ho1 44.30(7) . . ?
N1 Co1 Ho1 140.29(11) . . ?
O3 Co1 Ho1 44.52(7) . . ?
N2 Co1 Ho1 131.52(12) . . ?
O4 Co1 Ho1 86.07(9) . . ?
O6 Co1 Ho1 94.79(11) . . ?
C7 O2 Co1 123.4(2) . . ?
C7 O2 Ho1 131.0(2) . . ?
Co1 O2 Ho1 101.82(9) . . ?
C12 O3 Co1 109.0(2) . . ?
C12 O3 Ho1 139.5(3) . . ?
Co1 O3 Ho1 101.22(9) . . ?
C13 O4 Co1 126.1(2) . . ?
C2 O1 C1 114.5(3) . . ?
C2 O1 Ho1 118.2(2) . . ?
C1 O1 Ho1 126.3(3) . . ?
C13 O5 Ho1 135.5(3) . . ?
C8 N1 C9 123.0(3) . . ?
C8 N1 Co1 124.9(3) . . ?
C9 N1 Co1 112.0(3) . . ?
O2 C7 C2 115.9(3) . . ?
O2 C7 C6 125.0(3) . . ?
C2 C7 C6 119.1(3) . . ?
C7 C6 C8 123.4(3) . . ?
C7 C6 C5 118.6(4) . . ?
C8 C6 C5 118.0(4) . . ?
C1B N2 C2A 122.6(8) . . ?
C1A N2 C2B 123.3(7) . . ?
C1A N2 Co1 109.0(4) . . ?
C1B N2 Co1 109.4(5) . . ?
C2A N2 Co1 108.4(4) . . ?
C2B N2 Co1 107.1(5) . . ?
N1 C8 C6 125.6(3) . . ?
N1 C8 H8 117.2 . . ?
C6 C8 H8 117.2 . . ?
C3 C2 C7 120.6(4) . . ?
C3 C2 O1 126.8(4) . . ?
C7 C2 O1 112.5(3) . . ?
O3 C12 C2B 114.1(5) . . ?
O3 C12 C2A 106.6(5) . . ?
O3 C12 H12A 110.4 . . ?
C2A C12 H12A 110.4 . . ?
O3 C12 H12B 110.4 . . ?
C2A C12 H12B 110.4 . . ?
H12A C12 H12B 108.6 . . ?
O3 C12 H12C 108.7 . . ?
C2B C12 H12C 108.7 . . ?
O3 C12 H12D 108.7 . . ?
C2B C12 H12D 108.7 . . ?
H12C C12 H12D 107.6 . . ?
O5 C13 O4 125.7(4) . . ?
O5 C13 C14 117.7(4) . . ?
O4 C13 C14 116.6(4) . . ?
C2 C3 C4 119.9(4) . . ?
C2 C3 H3 120.0 . . ?
C4 C3 H3 120.0 . . ?
C4 C5 C6 121.3(4) . . ?
C4 C5 H5 119.3 . . ?
C6 C5 H5 119.3 . . ?
C5 C4 C3 120.3(4) . . ?
C5 C4 H4 119.8 . . ?
C3 C4 H4 119.8 . . ?
O1 C1 H1A 109.5 . . ?
O1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
O1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C1A C9 N1 107.4(5) . . ?
N1 C9 C1B 108.7(4) . . ?
N1 C9 H9A 110.0 . . ?
C1B C9 H9A 110.0 . . ?
N1 C9 H9B 110.0 . . ?
C1B C9 H9B 110.0 . . ?
H9A C9 H9B 108.3 . . ?
C1A C9 H9C 110.2 . . ?
N1 C9 H9C 110.2 . . ?
C1A C9 H9D 110.2 . . ?
N1 C9 H9D 110.2 . . ?
H9C C9 H9D 108.5 . . ?
C12 C2A N2 106.3(7) . . ?
C12 C2A H2A1 110.5 . . ?
N2 C2A H2A1 110.5 . . ?
C12 C2A H2A2 110.5 . . ?
N2 C2A H2A2 110.5 . . ?
H2A1 C2A H2A2 108.7 . . ?
N2 C1B C9 106.3(7) . . ?
N2 C1B H1B1 110.5 . . ?
C9 C1B H1B1 110.5 . . ?
N2 C1B H1B2 110.5 . . ?
C9 C1B H1B2 110.5 . . ?
H1B1 C1B H1B2 108.7 . . ?
C9 C1A N2 111.5(7) . . ?
C9 C1A H1A1 109.3 . . ?
N2 C1A H1A1 109.3 . . ?
C9 C1A H1A2 109.3 . . ?
N2 C1A H1A2 109.3 . . ?
H1A1 C1A H1A2 108.0 . . ?
C12 C2B N2 110.8(7) . . ?
C12 C2B H2B1 109.5 . . ?
N2 C2B H2B1 109.5 . . ?
C12 C2B H2B2 109.5 . . ?
N2 C2B H2B2 109.5 . . ?
H2B1 C2B H2B2 108.1 . . ?
O3N N1N O2N 117.7(12) . . ?
O3N N1N O1N 123.9(12) . . ?
O2N N1N O1N 118.2(11) . . ?
N1N O1N O3N 28.0(6) . . ?
N1N O3N O1N 28.1(6) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 Co1 O2 C7 9.0(3) . . . . ?
O3 Co1 O2 C7 -171.9(3) . . . . ?
O4 Co1 O2 C7 -78.6(3) . . . . ?
O6 Co1 O2 C7 99.7(3) . . . . ?
Ho1 Co1 O2 C7 -160.2(3) . . . . ?
N1 Co1 O2 Ho1 169.17(13) . . . . ?
O3 Co1 O2 Ho1 -11.74(11) . . . . ?
O4 Co1 O2 Ho1 81.56(11) . . . . ?
O6 Co1 O2 Ho1 -100.06(13) . . . . ?
O2 Co1 O3 C12 164.4(3) . . . . ?
N2 Co1 O3 C12 -14.3(3) . . . . ?
O4 Co1 O3 C12 71.8(3) . . . . ?
O6 Co1 O3 C12 -108.6(3) . . . . ?
Ho1 Co1 O3 C12 152.7(3) . . . . ?
O2 Co1 O3 Ho1 11.69(11) . . . . ?
N2 Co1 O3 Ho1 -166.96(16) . . . . ?
O4 Co1 O3 Ho1 -80.88(12) . . . . ?
O6 Co1 O3 Ho1 98.69(14) . . . . ?
O2 Co1 N1 C8 -5.3(4) . . . . ?
N2 Co1 N1 C8 173.4(4) . . . . ?
O4 Co1 N1 C8 87.1(4) . . . . ?
O6 Co1 N1 C8 -92.4(4) . . . . ?
Ho1 Co1 N1 C8 6.5(5) . . . . ?
O2 Co1 N1 C9 177.2(3) . . . . ?
N2 Co1 N1 C9 -4.1(4) . . . . ?
O4 Co1 N1 C9 -90.4(3) . . . . ?
O6 Co1 N1 C9 90.1(3) . . . . ?
Ho1 Co1 N1 C9 -171.0(3) . . . . ?
Co1 O2 C7 C2 172.6(3) . . . . ?
Ho1 O2 C7 C2 18.6(5) . . . . ?
Co1 O2 C7 C6 -8.7(5) . . . . ?
Ho1 O2 C7 C6 -162.6(3) . . . . ?
O2 C7 C6 C8 2.3(6) . . . . ?
C2 C7 C6 C8 -179.0(4) . . . . ?
O2 C7 C6 C5 -178.7(3) . . . . ?
C2 C7 C6 C5 0.0(5) . . . . ?
C9 N1 C8 C6 178.2(4) . . . . ?
Co1 N1 C8 C6 0.9(6) . . . . ?
C7 C6 C8 N1 2.0(7) . . . . ?
C5 C6 C8 N1 -177.0(4) . . . . ?
O2 C7 C2 C3 178.4(3) . . . . ?
C6 C7 C2 C3 -0.4(6) . . . . ?
O2 C7 C2 O1 -2.7(5) . . . . ?
C6 C7 C2 O1 178.5(3) . . . . ?
C1 O1 C2 C3 -0.2(7) . . . . ?
Ho1 O1 C2 C3 168.9(3) . . . . ?
C1 O1 C2 C7 -179.1(4) . . . . ?
Ho1 O1 C2 C7 -9.9(4) . . . . ?
Co1 O3 C12 C2B -2.1(8) . . . . ?
Ho1 O3 C12 C2B 134.0(7) . . . . ?
Co1 O3 C12 C2A 37.6(6) . . . . ?
Ho1 O3 C12 C2A 173.7(5) . . . . ?
Ho1 O5 C13 O4 -7.8(7) . . . . ?
Ho1 O5 C13 C14 171.8(3) . . . . ?
Co1 O4 C13 O5 7.0(6) . . . . ?
Co1 O4 C13 C14 -172.6(3) . . . . ?
C7 C2 C3 C4 0.5(7) . . . . ?
O1 C2 C3 C4 -178.2(4) . . . . ?
C7 C6 C5 C4 0.3(6) . . . . ?
C8 C6 C5 C4 179.3(4) . . . . ?
C6 C5 C4 C3 -0.1(8) . . . . ?
C2 C3 C4 C5 -0.3(7) . . . . ?
C8 N1 C9 C1A -153.7(7) . . . . ?
Co1 N1 C9 C1A 23.9(7) . . . . ?
C8 N1 C9 C1B 164.1(6) . . . . ?
Co1 N1 C9 C1B -18.3(7) . . . . ?
O3 C12 C2A N2 -50.2(9) . . . . ?
C1B N2 C2A C12 167.0(7) . . . . ?
Co1 N2 C2A C12 38.0(9) . . . . ?
C2A N2 C1B C9 -171.2(7) . . . . ?
Co1 N2 C1B C9 -42.7(9) . . . . ?
N1 C9 C1B N2 39.3(10) . . . . ?
N1 C9 C1A N2 -38.9(10) . . . . ?
C2B N2 C1A C9 162.6(9) . . . . ?
Co1 N2 C1A C9 35.9(10) . . . . ?
O3 C12 C2B N2 24.8(12) . . . . ?
C1A N2 C2B C12 -161.9(8) . . . . ?
Co1 N2 C2B C12 -34.4(10) . . . . ?
O2N N1N O1N O3N -176(2) . . . . ?
O2N N1N O3N O1N 176(2) . . . . ?

_refine_diff_density_max         1.032
_refine_diff_density_min         -0.457
_refine_diff_density_rms         0.089


####################################################################### 
# 
# 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_Complex4_Co2Er_squeezed
_database_code_depnum_ccdc_archive 'CCDC 1429326'
_audit_update_record             
;
2016-04-23 deposited with the CCDC.
2016-04-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C28 H42 Co2 Er N4 O13, N O3, 5(H2 O), 3(C H4 O)'
_chemical_formula_sum            'C31 H64 Co2 Er N5 O24'
_chemical_formula_weight         1175.98

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   25.231(5)
_cell_length_b                   11.986(5)
_cell_length_c                   16.814(5)
_cell_angle_alpha                90
_cell_angle_beta                 116.896(5)
_cell_angle_gamma                90
_cell_volume                     4535(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9044
_cell_measurement_theta_min      2.491
_cell_measurement_theta_max      28.371

_exptl_crystal_description       blocks
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.723
_exptl_crystal_F_000             2044
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_exptl_absorpt_coefficient_mu    2.624
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_correction_T_min  0.714
_exptl_absorpt_correction_T_max  0.790
_exptl_absorpt_process_details   'North et al, 1968'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker SMART APEX'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            19412
_diffrn_reflns_av_unetI/netI     0.0525
_diffrn_reflns_av_R_equivalents  0.0594
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.107
_diffrn_reflns_theta_max         28.443
_diffrn_reflns_theta_full        25.240
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             5714
_reflns_number_gt                4708
_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       'Bruker APEX'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'DIAMOND 3.1 d'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_refine_special_details          
'The ADPs were restricted to resonable values using EADP (for C1B C12) restraint. SADI and RIGU restraints are used mandatorily for the mutually intertwined nitrate counter anion and water molecules. H atoms were not located for the ligand and hence fixed using HFIX command. Unassigned solvent molecules are squeezed out using SQUEEZE program in PLATON. Solvent accessible void volume (853 cA) contains 336 electrons, which could be assinged to three water molecules and three methanol molecules per formula unit.'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0750P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5714
_refine_ls_number_parameters     296
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.0542
_refine_ls_R_factor_gt           0.0432
_refine_ls_wR_factor_ref         0.1194
_refine_ls_wR_factor_gt          0.1119
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_restrained_S_all      1.008
_refine_ls_shift/su_max          0.022
_refine_ls_shift/su_mean         0.002

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
Er1 Er 0.5000 0.24166(2) 0.2500 0.03976(10) Uani 1 2 d S T P . .
Co1 Co 0.60956(2) 0.06603(4) 0.29014(3) 0.04431(14) Uani 1 1 d . . . . .
O2 O 0.58782(10) 0.1620(2) 0.35886(16) 0.0449(6) Uani 1 1 d . . . . .
O3 O 0.53325(10) 0.0929(2) 0.19444(16) 0.0442(6) Uani 1 1 d . . . . .
O5 O 0.64569(12) 0.1860(3) 0.25561(19) 0.0542(7) Uani 1 1 d . . . . .
O1 O 0.54653(12) 0.3112(3) 0.42164(19) 0.0570(7) Uani 1 1 d . . . . .
O6 O 0.57611(12) 0.3157(3) 0.2256(2) 0.0649(8) Uani 1 1 d . . . . .
N1 N 0.68631(14) 0.0323(3) 0.3793(2) 0.0571(9) Uani 1 1 d . . . . .
O4 O 0.57631(19) -0.0560(4) 0.3301(3) 0.0842(11) Uani 1 1 d . . . . .
C7 C 0.62537(15) 0.1966(3) 0.4400(2) 0.0425(8) Uani 1 1 d . . . . .
C8 C 0.71099(18) 0.0769(4) 0.4566(3) 0.0576(10) Uani 1 1 d . . . . .
H8 H 0.7505 0.0549 0.4954 0.069 Uiso 1 1 calc R U . . .
N2 N 0.62611(16) -0.0274(4) 0.2123(3) 0.0658(10) Uani 1 1 d . . . . .
C6 C 0.68374(16) 0.1578(3) 0.4895(2) 0.0493(9) Uani 1 1 d . . . . .
C2 C 0.60363(18) 0.2784(3) 0.4776(3) 0.0470(8) Uani 1 1 d . . . . .
C12 C 0.5327(2) 0.0564(5) 0.1129(3) 0.0658(12) Uani 1 1 d . . . . .
H12A H 0.5202 0.1196 0.0704 0.079 Uiso 0.703(11) 1 calc R U P A 1
H12B H 0.5025 -0.0032 0.0866 0.079 Uiso 0.703(11) 1 calc R U P A 1
H12C H 0.5494 0.1148 0.0892 0.079 Uiso 0.297(11) 1 calc R U P A 2
H12D H 0.4915 0.0405 0.0676 0.079 Uiso 0.297(11) 1 calc R U P A 2
C13 C 0.6230(2) 0.2810(5) 0.2281(3) 0.0586(11) Uani 1 1 d . . . . .
C5 C 0.71848(19) 0.2006(5) 0.5754(3) 0.0623(11) Uani 1 1 d . . . . .
H5 H 0.7579 0.1742 0.6092 0.075 Uiso 1 1 calc R U . . .
C3 C 0.6383(2) 0.3189(4) 0.5618(3) 0.0631(11) Uani 1 1 d . . . . .
H3 H 0.6229 0.3736 0.5868 0.076 Uiso 1 1 calc R U . . .
C4 C 0.6967(2) 0.2790(5) 0.6111(3) 0.0696(13) Uani 1 1 d . . . . .
H4 H 0.7208 0.3069 0.6693 0.084 Uiso 1 1 calc R U . . .
C1 C 0.5226(2) 0.3961(5) 0.4562(4) 0.0898(19) Uani 1 1 d . . . . .
H1A H 0.4819 0.4139 0.4118 0.135 Uiso 1 1 calc R U . . .
H1B H 0.5221 0.3692 0.5109 0.135 Uiso 1 1 calc R U . . .
H1C H 0.5473 0.4633 0.4695 0.135 Uiso 1 1 calc R U . . .
C9 C 0.7164(2) -0.0502(5) 0.3487(4) 0.0797(15) Uani 1 1 d . . . . .
H9A H 0.7104 -0.1264 0.3659 0.096 Uiso 0.703(11) 1 calc R U P A 1
H9B H 0.7596 -0.0349 0.3760 0.096 Uiso 0.703(11) 1 calc R U P A 1
H9C H 0.7474 -0.0127 0.3377 0.096 Uiso 0.297(11) 1 calc R U P A 2
H9D H 0.7359 -0.1073 0.3955 0.096 Uiso 0.297(11) 1 calc R U P A 2
C14 C 0.6566(2) 0.3552(5) 0.1943(4) 0.0791(15) Uani 1 1 d . . . . .
H14A H 0.6925 0.3166 0.2005 0.119 Uiso 1 1 calc R U . . .
H14B H 0.6314 0.3728 0.1313 0.119 Uiso 1 1 calc R U . . .
H14C H 0.6678 0.4244 0.2291 0.119 Uiso 1 1 calc R U . . .
C1A C 0.5910(4) 0.0133(8) 0.1229(5) 0.077(3) Uani 0.703(11) 1 d . . P A 1
H1A1 H 0.5841 -0.0477 0.0796 0.092 Uiso 0.703(11) 1 calc R U P A 1
H1A2 H 0.6127 0.0738 0.1100 0.092 Uiso 0.703(11) 1 calc R U P A 1
C2A C 0.6901(3) -0.0411(10) 0.2496(6) 0.081(3) Uani 0.703(11) 1 d . . P A 1
H2A1 H 0.7075 0.0238 0.2333 0.097 Uiso 0.703(11) 1 calc R U P A 1
H2A2 H 0.6993 -0.1091 0.2248 0.097 Uiso 0.703(11) 1 calc R U P A 1
C1B C 0.5719(8) -0.0535(19) 0.1350(10) 0.0658(12) Uani 0.297(11) 1 d . . P A 2
H1B1 H 0.5798 -0.0740 0.0844 0.079 Uiso 0.297(11) 1 calc R U P A 2
H1B2 H 0.5513 -0.1164 0.1474 0.079 Uiso 0.297(11) 1 calc R U P A 2
C2B C 0.6732(8) -0.1044(16) 0.2661(15) 0.074(6) Uani 0.297(11) 1 d . . P A 2
H2B1 H 0.6558 -0.1701 0.2813 0.089 Uiso 0.297(11) 1 calc R U P A 2
H2B2 H 0.6937 -0.1306 0.2315 0.089 Uiso 0.297(11) 1 calc R U P A 2
O1N O 0.5275(7) -0.2265(11) 0.1562(12) 0.139(5) Uani 0.5 1 d D U P B 1
O2N O 0.5546(6) -0.4042(7) 0.1878(7) 0.103(3) Uani 0.5 1 d D U P B 1
N1N N 0.5635(6) -0.3016(8) 0.2015(8) 0.101(3) Uani 0.5 1 d D U P B 1
O3N O 0.6154(6) -0.2675(8) 0.2546(11) 0.137(5) Uani 0.5 1 d D U P B 1
O1A O 0.546(3) -0.268(4) 0.224(5) 0.26(3) Uiso 0.3 1 d . . P C 2
O2A O 0.5952(17) -0.413(3) 0.246(3) 0.226(15) Uiso 0.3 1 d . . P D 2
O1B O 0.516(2) -0.259(4) 0.182(4) 0.121(14) Uiso 0.2 1 d . . P E 3
O2B O 0.513(2) -0.365(5) 0.163(3) 0.20(2) Uiso 0.2 1 d . . P E 3
O7 O 0.5000 0.4381(5) 0.2500 0.094(2) Uani 1 2 d S T P . .
H1W H 0.557(5) -0.112(12) 0.313(9) 0.30(8) Uiso 1 1 d . . . . .
H2W H 0.541(2) -0.014(4) 0.334(3) 0.074(15) Uiso 1 1 d . . . . .
H3W H 0.527(4) 0.464(7) 0.254(8) 0.18(4) Uiso 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Er1 O6 2.314(3) 2_655 ?
Er1 O6 2.314(3) . ?
Er1 O3 2.338(3) 2_655 ?
Er1 O3 2.338(3) . ?
Er1 O2 2.346(2) . ?
Er1 O2 2.346(2) 2_655 ?
Er1 O7 2.355(6) . ?
Er1 O1 2.709(3) 2_655 ?
Er1 O1 2.709(3) . ?
Er1 Co1 3.2925(9) . ?
Er1 Co1 3.2925(9) 2_655 ?
Co1 O2 1.879(2) . ?
Co1 N1 1.880(3) . ?
Co1 O3 1.897(2) . ?
Co1 N2 1.908(3) . ?
Co1 O4 1.950(4) . ?
Co1 O5 1.927(3) . ?
O2 C7 1.327(4) . ?
O3 C12 1.433(5) . ?
O5 C13 1.265(6) . ?
O1 C2 1.374(5) . ?
O1 C1 1.434(5) . ?
O6 C13 1.236(6) . ?
N1 C8 1.276(6) . ?
N1 C9 1.474(6) . ?
O4 H1W 0.80(14) . ?
O4 H2W 1.06(6) . ?
C7 C2 1.407(6) . ?
C7 C6 1.403(5) . ?
C8 C6 1.436(6) . ?
C8 H8 0.9500 . ?
N2 C2A 1.452(8) . ?
N2 C1A 1.441(9) . ?
N2 C1B 1.432(16) . ?
N2 C2B 1.452(18) . ?
C6 C5 1.405(6) . ?
C2 C3 1.373(6) . ?
C12 C1B 1.586(19) . ?
C12 C1A 1.496(8) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C12 H12C 0.9900 . ?
C12 H12D 0.9900 . ?
C13 C14 1.507(6) . ?
C5 C4 1.358(8) . ?
C5 H5 0.9500 . ?
C3 C4 1.407(7) . ?
C3 H3 0.9500 . ?
C4 H4 0.9500 . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C9 C2B 1.47(2) . ?
C9 C2A 1.493(10) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C9 H9C 0.9900 . ?
C9 H9D 0.9900 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C1A H1A1 0.9900 . ?
C1A H1A2 0.9900 . ?
C2A H2A1 0.9900 . ?
C2A H2A2 0.9900 . ?
C1B H1B1 0.9900 . ?
C1B H1B2 0.9900 . ?
C2B H2B1 0.9900 . ?
C2B H2B2 0.9900 . ?
O1N N1N 1.261(13) . ?
O2N N1N 1.252(11) . ?
N1N O3N 1.273(13) . ?
O1B O2B 1.30(6) . ?
O7 H3W 0.73(8) . ?

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
O6 Er1 O6 134.91(17) 2_655 . ?
O6 Er1 O3 75.24(11) 2_655 2_655 ?
O6 Er1 O3 147.11(10) . 2_655 ?
O6 Er1 O3 147.12(10) 2_655 . ?
O6 Er1 O3 75.24(11) . . ?
O3 Er1 O3 80.58(13) 2_655 . ?
O6 Er1 O2 125.77(11) 2_655 . ?
O6 Er1 O2 74.21(10) . . ?
O3 Er1 O2 76.14(9) 2_655 . ?
O3 Er1 O2 67.55(9) . . ?
O6 Er1 O2 74.21(10) 2_655 2_655 ?
O6 Er1 O2 125.77(11) . 2_655 ?
O3 Er1 O2 67.55(9) 2_655 2_655 ?
O3 Er1 O2 76.14(9) . 2_655 ?
O2 Er1 O2 131.93(13) . 2_655 ?
O6 Er1 O7 67.45(8) 2_655 . ?
O6 Er1 O7 67.45(8) . . ?
O3 Er1 O7 139.71(7) 2_655 . ?
O3 Er1 O7 139.71(7) . . ?
O2 Er1 O7 114.04(6) . . ?
O2 Er1 O7 114.03(6) 2_655 . ?
O6 Er1 O1 94.37(11) 2_655 2_655 ?
O6 Er1 O1 71.80(10) . 2_655 ?
O3 Er1 O1 126.85(9) 2_655 2_655 ?
O3 Er1 O1 82.53(10) . 2_655 ?
O2 Er1 O1 139.27(9) . 2_655 ?
O2 Er1 O1 59.53(8) 2_655 2_655 ?
O7 Er1 O1 72.07(7) . 2_655 ?
O6 Er1 O1 71.80(10) 2_655 . ?
O6 Er1 O1 94.37(11) . . ?
O3 Er1 O1 82.53(10) 2_655 . ?
O3 Er1 O1 126.85(9) . . ?
O2 Er1 O1 59.53(8) . . ?
O2 Er1 O1 139.28(9) 2_655 . ?
O7 Er1 O1 72.07(7) . . ?
O1 Er1 O1 144.14(14) 2_655 . ?
O6 Er1 Co1 153.62(9) 2_655 . ?
O6 Er1 Co1 66.07(8) . . ?
O3 Er1 Co1 81.38(6) 2_655 . ?
O3 Er1 Co1 34.36(6) . . ?
O2 Er1 Co1 33.96(6) . . ?
O2 Er1 Co1 107.97(7) 2_655 . ?
O7 Er1 Co1 129.746(16) . . ?
O1 Er1 Co1 109.53(7) 2_655 . ?
O1 Er1 Co1 93.40(6) . . ?
O6 Er1 Co1 66.07(8) 2_655 2_655 ?
O6 Er1 Co1 153.62(9) . 2_655 ?
O3 Er1 Co1 34.36(6) 2_655 2_655 ?
O3 Er1 Co1 81.38(6) . 2_655 ?
O2 Er1 Co1 107.97(7) . 2_655 ?
O2 Er1 Co1 33.96(6) 2_655 2_655 ?
O7 Er1 Co1 129.746(16) . 2_655 ?
O1 Er1 Co1 93.40(6) 2_655 2_655 ?
O1 Er1 Co1 109.53(7) . 2_655 ?
Co1 Er1 Co1 100.51(3) . 2_655 ?
O2 Co1 N1 97.07(13) . . ?
O2 Co1 O3 87.20(11) . . ?
N1 Co1 O3 175.73(13) . . ?
O2 Co1 N2 175.44(14) . . ?
N1 Co1 N2 87.41(16) . . ?
O3 Co1 N2 88.32(14) . . ?
O2 Co1 O4 87.49(16) . . ?
N1 Co1 O4 90.70(18) . . ?
O3 Co1 O4 89.42(16) . . ?
N2 Co1 O4 93.3(2) . . ?
O2 Co1 O5 92.20(13) . . ?
N1 Co1 O5 86.78(15) . . ?
O3 Co1 O5 93.14(12) . . ?
N2 Co1 O5 87.19(17) . . ?
O4 Co1 O5 177.40(17) . . ?
O2 Co1 Er1 44.22(7) . . ?
N1 Co1 Er1 140.12(11) . . ?
O3 Co1 Er1 44.08(8) . . ?
N2 Co1 Er1 131.23(12) . . ?
O4 Co1 Er1 95.62(13) . . ?
O5 Co1 Er1 85.93(9) . . ?
C7 O2 Co1 123.5(2) . . ?
C7 O2 Er1 131.1(2) . . ?
Co1 O2 Er1 101.82(10) . . ?
C12 O3 Co1 109.1(2) . . ?
C12 O3 Er1 139.9(3) . . ?
Co1 O3 Er1 101.56(10) . . ?
C13 O5 Co1 125.7(3) . . ?
C2 O1 C1 115.4(3) . . ?
C2 O1 Er1 117.2(2) . . ?
C1 O1 Er1 126.2(3) . . ?
C13 O6 Er1 136.3(3) . . ?
C8 N1 C9 123.1(4) . . ?
C8 N1 Co1 125.0(3) . . ?
C9 N1 Co1 111.9(3) . . ?
Co1 O4 H1W 142(10) . . ?
Co1 O4 H2W 100(3) . . ?
H1W O4 H2W 91(10) . . ?
O2 C7 C2 116.0(3) . . ?
O2 C7 C6 125.2(4) . . ?
C2 C7 C6 118.9(3) . . ?
N1 C8 C6 125.2(4) . . ?
N1 C8 H8 117.4 . . ?
C6 C8 H8 117.4 . . ?
C2A N2 C1A 121.8(6) . . ?
C1B N2 C2B 127.2(13) . . ?
C2A N2 Co1 108.4(4) . . ?
C1A N2 Co1 107.1(4) . . ?
C1B N2 Co1 109.5(7) . . ?
C2B N2 Co1 108.4(9) . . ?
C5 C6 C7 119.2(4) . . ?
C5 C6 C8 117.3(4) . . ?
C7 C6 C8 123.5(4) . . ?
C7 C2 O1 113.1(3) . . ?
C7 C2 C3 120.9(4) . . ?
O1 C2 C3 125.9(4) . . ?
O3 C12 C1B 107.1(7) . . ?
O3 C12 C1A 114.5(4) . . ?
O3 C12 H12A 108.6 . . ?
C1A C12 H12A 108.6 . . ?
O3 C12 H12B 108.6 . . ?
C1A C12 H12B 108.6 . . ?
H12A C12 H12B 107.6 . . ?
O3 C12 H12C 110.3 . . ?
C1B C12 H12C 110.3 . . ?
O3 C12 H12D 110.3 . . ?
C1B C12 H12D 110.3 . . ?
H12C C12 H12D 108.6 . . ?
O6 C13 O5 125.7(4) . . ?
O6 C13 C14 118.8(5) . . ?
O5 C13 C14 115.4(4) . . ?
C4 C5 C6 121.2(4) . . ?
C4 C5 H5 119.4 . . ?
C6 C5 H5 119.4 . . ?
C4 C3 C2 119.7(4) . . ?
C4 C3 H3 120.1 . . ?
C2 C3 H3 120.1 . . ?
C5 C4 C3 120.0(4) . . ?
C5 C4 H4 120.0 . . ?
C3 C4 H4 120.0 . . ?
O1 C1 H1A 109.5 . . ?
O1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
O1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C2B C9 N1 110.3(7) . . ?
N1 C9 C2A 107.5(4) . . ?
N1 C9 H9A 110.2 . . ?
C2A C9 H9A 110.2 . . ?
N1 C9 H9B 110.2 . . ?
C2A C9 H9B 110.2 . . ?
H9A C9 H9B 108.5 . . ?
C2B C9 H9C 109.6 . . ?
N1 C9 H9C 109.6 . . ?
C2B C9 H9D 109.6 . . ?
N1 C9 H9D 109.6 . . ?
H9C C9 H9D 108.1 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N2 C1A C12 110.1(5) . . ?
N2 C1A H1A1 109.6 . . ?
C12 C1A H1A1 109.6 . . ?
N2 C1A H1A2 109.6 . . ?
C12 C1A H1A2 109.6 . . ?
H1A1 C1A H1A2 108.2 . . ?
N2 C2A C9 109.7(6) . . ?
N2 C2A H2A1 109.7 . . ?
C9 C2A H2A1 109.7 . . ?
N2 C2A H2A2 109.7 . . ?
C9 C2A H2A2 109.7 . . ?
H2A1 C2A H2A2 108.2 . . ?
C12 C1B N2 105.7(12) . . ?
C12 C1B H1B1 110.6 . . ?
N2 C1B H1B1 110.6 . . ?
C12 C1B H1B2 110.6 . . ?
N2 C1B H1B2 110.6 . . ?
H1B1 C1B H1B2 108.7 . . ?
C9 C2B N2 110.9(11) . . ?
C9 C2B H2B1 109.5 . . ?
N2 C2B H2B1 109.5 . . ?
C9 C2B H2B2 109.5 . . ?
N2 C2B H2B2 109.5 . . ?
H2B1 C2B H2B2 108.1 . . ?
O1N N1N O3N 115.3(10) . . ?
O1N N1N O2N 124.6(11) . . ?
O3N N1N O2N 119.1(10) . . ?
Er1 O7 H3W 115(7) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 Co1 O2 C7 8.1(3) . . . . ?
O3 Co1 O2 C7 -172.0(3) . . . . ?
O4 Co1 O2 C7 98.5(3) . . . . ?
O5 Co1 O2 C7 -78.9(3) . . . . ?
Er1 Co1 O2 C7 -160.8(3) . . . . ?
N1 Co1 O2 Er1 168.90(14) . . . . ?
O3 Co1 O2 Er1 -11.16(12) . . . . ?
O4 Co1 O2 Er1 -100.70(16) . . . . ?
O5 Co1 O2 Er1 81.88(12) . . . . ?
O2 Co1 O3 C12 165.0(3) . . . . ?
N2 Co1 O3 C12 -14.2(3) . . . . ?
O4 Co1 O3 C12 -107.5(3) . . . . ?
O5 Co1 O3 C12 72.9(3) . . . . ?
Er1 Co1 O3 C12 153.8(3) . . . . ?
O2 Co1 O3 Er1 11.19(12) . . . . ?
N2 Co1 O3 Er1 -167.95(16) . . . . ?
O4 Co1 O3 Er1 98.70(17) . . . . ?
O5 Co1 O3 Er1 -80.86(13) . . . . ?
O2 Co1 N1 C8 -5.5(4) . . . . ?
N2 Co1 N1 C8 173.6(4) . . . . ?
O4 Co1 N1 C8 -93.1(4) . . . . ?
O5 Co1 N1 C8 86.3(4) . . . . ?
Er1 Co1 N1 C8 6.5(5) . . . . ?
O2 Co1 N1 C9 176.5(3) . . . . ?
N2 Co1 N1 C9 -4.4(4) . . . . ?
O4 Co1 N1 C9 88.9(4) . . . . ?
O5 Co1 N1 C9 -91.7(3) . . . . ?
Er1 Co1 N1 C9 -171.4(3) . . . . ?
Co1 O2 C7 C2 172.7(3) . . . . ?
Er1 O2 C7 C2 17.9(5) . . . . ?
Co1 O2 C7 C6 -7.5(5) . . . . ?
Er1 O2 C7 C6 -162.2(3) . . . . ?
C9 N1 C8 C6 179.8(4) . . . . ?
Co1 N1 C8 C6 2.0(7) . . . . ?
O2 C7 C6 C5 -179.0(4) . . . . ?
C2 C7 C6 C5 0.8(6) . . . . ?
O2 C7 C6 C8 2.0(6) . . . . ?
C2 C7 C6 C8 -178.1(4) . . . . ?
N1 C8 C6 C5 -177.9(5) . . . . ?
N1 C8 C6 C7 1.0(7) . . . . ?
O2 C7 C2 O1 -1.7(5) . . . . ?
C6 C7 C2 O1 178.5(3) . . . . ?
O2 C7 C2 C3 178.8(4) . . . . ?
C6 C7 C2 C3 -1.0(6) . . . . ?
C1 O1 C2 C7 -178.9(4) . . . . ?
Er1 O1 C2 C7 -10.7(4) . . . . ?
C1 O1 C2 C3 0.5(7) . . . . ?
Er1 O1 C2 C3 168.8(4) . . . . ?
Co1 O3 C12 C1B 37.0(9) . . . . ?
Er1 O3 C12 C1B 174.7(9) . . . . ?
Co1 O3 C12 C1A -2.8(7) . . . . ?
Er1 O3 C12 C1A 135.0(5) . . . . ?
Er1 O6 C13 O5 -7.3(8) . . . . ?
Er1 O6 C13 C14 171.5(4) . . . . ?
Co1 O5 C13 O6 6.2(7) . . . . ?
Co1 O5 C13 C14 -172.6(3) . . . . ?
C7 C6 C5 C4 -0.3(7) . . . . ?
C8 C6 C5 C4 178.7(5) . . . . ?
C7 C2 C3 C4 0.7(7) . . . . ?
O1 C2 C3 C4 -178.7(4) . . . . ?
C6 C5 C4 C3 0.0(8) . . . . ?
C2 C3 C4 C5 -0.2(8) . . . . ?
C8 N1 C9 C2B 167.5(11) . . . . ?
Co1 N1 C9 C2B -14.5(12) . . . . ?
C8 N1 C9 C2A -152.1(6) . . . . ?
Co1 N1 C9 C2A 25.9(7) . . . . ?
C2A N2 C1A C12 -160.2(6) . . . . ?
Co1 N2 C1A C12 -34.8(8) . . . . ?
O3 C12 C1A N2 25.4(9) . . . . ?
C1A N2 C2A C9 162.8(6) . . . . ?
Co1 N2 C2A C9 38.0(9) . . . . ?
N1 C9 C2A N2 -41.4(9) . . . . ?
O3 C12 C1B N2 -48.8(14) . . . . ?
C2B N2 C1B C12 170.7(12) . . . . ?
Co1 N2 C1B C12 37.1(14) . . . . ?
N1 C9 C2B N2 32.8(18) . . . . ?
C1B N2 C2B C9 -169.8(11) . . . . ?
Co1 N2 C2B C9 -35.7(17) . . . . ?

_refine_diff_density_max         1.912
_refine_diff_density_min         -1.617
_refine_diff_density_rms         0.128



#=====END=====

