# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1040740'
_audit_update_record             
;
2014-12-22 deposited with the CCDC.
2015-04-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C21 H15 Co Dy N3 O15'
_chemical_formula_sum            'C21 H15 Co Dy N3 O15'
_chemical_melting_point          ?

_exptl_crystal_description       stick
_exptl_crystal_colour            purple

_diffrn_ambient_temperature      296(2)
_chemical_formula_weight         770.79

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'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   'P 3'
_symmetry_int_tables_number      143
_chemical_absolute_configuration ?
_symmetry_space_group_name_Hall  P3

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'

_cell_length_a                   13.1350(10)
_cell_length_b                   13.1350(10)
_cell_length_c                   5.8794(12)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     878.5(2)
_cell_formula_units_Z            1
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    3770
_cell_measurement_theta_min      3.11
_cell_measurement_theta_max      29.01
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.457
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             375
_exptl_absorpt_coefficient_mu    2.642
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6772
_exptl_absorpt_correction_T_max  0.8165
_exptl_absorpt_process_details   'SADABS(Bruker, 2000)'

_exptl_special_details           
; 
 ? 
;
_diffrn_radiation_probe          ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6913
_diffrn_reflns_av_R_equivalents  0.0345
_diffrn_reflns_av_sigmaI/netI    0.0470
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_theta_min         1.79
_diffrn_reflns_theta_max         25.99
_reflns_number_total             2099
_reflns_number_gt                2097
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0285P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.043(13)
_refine_ls_number_reflns         2099
_refine_ls_number_parameters     124
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0228
_refine_ls_R_factor_gt           0.0227
_refine_ls_wR_factor_ref         0.0570
_refine_ls_wR_factor_gt          0.0570
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_restrained_S_all      1.001
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy1 Dy 0.6667 0.3333 1.1094 0.02528(9) Uani 1 3 d S . .
Co1 Co 1.0000 1.0000 0.90702(16) 0.0310(2) Uani 1 3 d S . .
C1 C 0.9144(4) 0.7639(4) 0.8477(7) 0.0335(9) Uani 1 1 d . . .
C2 C 0.8993(4) 0.6580(4) 0.7703(7) 0.0358(10) Uani 1 1 d . . .
C3 C 0.9611(5) 0.6587(4) 0.5770(8) 0.0456(12) Uani 1 1 d . . .
H3 H 0.9533 0.5888 0.5217 0.055 Uiso 1 1 calc R . .
C4 C 1.0336(5) 0.7633(5) 0.4680(8) 0.0466(12) Uani 1 1 d . . .
H4 H 1.0730 0.7645 0.3357 0.056 Uiso 1 1 calc R . .
C5 C 1.0470(4) 0.8673(4) 0.5596(8) 0.0386(10) Uani 1 1 d . . .
H5 H 1.0987 0.9384 0.4903 0.046 Uiso 1 1 calc R . .
C6 C 0.8509(4) 0.7769(4) 1.0571(8) 0.0343(10) Uani 1 1 d . . .
C7 C 0.8192(4) 0.5447(4) 0.8902(8) 0.0393(11) Uani 1 1 d . . .
N1 N 0.9884(3) 0.8680(3) 0.7421(6) 0.0327(8) Uani 1 1 d . . .
O1 O 0.8809(3) 0.8856(3) 1.0942(5) 0.0380(7) Uani 1 1 d . . .
O2 O 0.7811(3) 0.6924(3) 1.1626(6) 0.0550(10) Uani 1 1 d . . .
O3 O 0.7132(3) 0.4807(3) 0.8232(6) 0.0451(8) Uani 1 1 d . . .
O4 O 0.8602(3) 0.5116(3) 1.0518(6) 0.0464(8) Uani 1 1 d . . .
O5 O 0.7984(4) 0.3290(4) 1.3702(6) 0.0497(9) Uani 1 1 d . . .
H5A H 0.7629 0.2675 1.4515 0.075 Uiso 1 1 d R . .
H5B H 0.8544 0.3283 1.2991 0.075 Uiso 1 1 d R . .


_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
Dy1 O5 2.334(3) . ?
Dy1 O5 2.334(3) 3_665 ?
Dy1 O5 2.334(3) 2_655 ?
Dy1 O3 2.402(3) 3_665 ?
Dy1 O3 2.402(3) 2_655 ?
Dy1 O3 2.402(3) . ?
Dy1 O4 2.472(3) 3_665 ?
Dy1 O4 2.472(3) . ?
Dy1 O4 2.472(3) 2_655 ?
Dy1 C7 2.797(5) 3_665 ?
Dy1 C7 2.797(5) 2_655 ?
Co1 O1 1.888(3) 2_765 ?
Co1 O1 1.888(3) 3_675 ?
Co1 O1 1.888(3) . ?
Co1 N1 1.925(4) . ?
Co1 N1 1.925(4) 3_675 ?
Co1 N1 1.925(4) 2_765 ?
C1 N1 1.367(6) . ?
C1 C2 1.381(6) . ?
C1 C6 1.543(6) . ?
C2 C3 1.393(6) . ?
C2 C7 1.501(7) . ?
C3 C4 1.376(7) . ?
C3 H3 0.9300 . ?
C4 C5 1.396(7) . ?
C4 H4 0.9300 . ?
C5 N1 1.323(6) . ?
C5 H5 0.9300 . ?
C6 O2 1.200(6) . ?
C6 O1 1.296(5) . ?
C7 O4 1.271(6) . ?
C7 O3 1.276(6) . ?
O5 H5A 0.8500 . ?
O5 H5B 0.8500 . ?

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 Dy1 O5 81.52(15) . 3_665 ?
O5 Dy1 O5 81.52(15) . 2_655 ?
O5 Dy1 O5 81.52(15) 3_665 2_655 ?
O5 Dy1 O3 86.80(13) . 3_665 ?
O5 Dy1 O3 125.92(13) 3_665 3_665 ?
O5 Dy1 O3 148.20(13) 2_655 3_665 ?
O5 Dy1 O3 148.20(13) . 2_655 ?
O5 Dy1 O3 86.80(13) 3_665 2_655 ?
O5 Dy1 O3 125.92(13) 2_655 2_655 ?
O3 Dy1 O3 76.34(13) 3_665 2_655 ?
O5 Dy1 O3 125.92(13) . . ?
O5 Dy1 O3 148.20(13) 3_665 . ?
O5 Dy1 O3 86.80(13) 2_655 . ?
O3 Dy1 O3 76.34(13) 3_665 . ?
O3 Dy1 O3 76.34(13) 2_655 . ?
O5 Dy1 O4 75.22(13) . 3_665 ?
O5 Dy1 O4 71.88(13) 3_665 3_665 ?
O5 Dy1 O4 146.73(12) 2_655 3_665 ?
O3 Dy1 O4 54.10(11) 3_665 3_665 ?
O3 Dy1 O4 73.05(12) 2_655 3_665 ?
O3 Dy1 O4 126.17(12) . 3_665 ?
O5 Dy1 O4 71.88(13) . . ?
O5 Dy1 O4 146.73(12) 3_665 . ?
O5 Dy1 O4 75.22(13) 2_655 . ?
O3 Dy1 O4 73.05(12) 3_665 . ?
O3 Dy1 O4 126.17(12) 2_655 . ?
O3 Dy1 O4 54.10(11) . . ?
O4 Dy1 O4 118.16(4) 3_665 . ?
O5 Dy1 O4 146.73(12) . 2_655 ?
O5 Dy1 O4 75.22(13) 3_665 2_655 ?
O5 Dy1 O4 71.88(13) 2_655 2_655 ?
O3 Dy1 O4 126.17(12) 3_665 2_655 ?
O3 Dy1 O4 54.10(11) 2_655 2_655 ?
O3 Dy1 O4 73.05(12) . 2_655 ?
O4 Dy1 O4 118.16(4) 3_665 2_655 ?
O4 Dy1 O4 118.16(4) . 2_655 ?
O5 Dy1 C7 79.14(14) . 3_665 ?
O5 Dy1 C7 98.92(15) 3_665 3_665 ?
O5 Dy1 C7 160.35(13) 2_655 3_665 ?
O3 Dy1 C7 27.08(13) 3_665 3_665 ?
O3 Dy1 C7 73.59(13) 2_655 3_665 ?
O3 Dy1 C7 101.79(13) . 3_665 ?
O4 Dy1 C7 27.04(13) 3_665 3_665 ?
O4 Dy1 C7 95.39(14) . 3_665 ?
O4 Dy1 C7 127.41(13) 2_655 3_665 ?
O5 Dy1 C7 160.35(13) . 2_655 ?
O5 Dy1 C7 79.14(14) 3_665 2_655 ?
O5 Dy1 C7 98.92(15) 2_655 2_655 ?
O3 Dy1 C7 101.79(13) 3_665 2_655 ?
O3 Dy1 C7 27.08(13) 2_655 2_655 ?
O3 Dy1 C7 73.59(13) . 2_655 ?
O4 Dy1 C7 95.39(14) 3_665 2_655 ?
O4 Dy1 C7 127.41(13) . 2_655 ?
O4 Dy1 C7 27.04(13) 2_655 2_655 ?
C7 Dy1 C7 100.45(13) 3_665 2_655 ?
O1 Co1 O1 89.47(14) 2_765 3_675 ?
O1 Co1 O1 89.47(14) 2_765 . ?
O1 Co1 O1 89.47(14) 3_675 . ?
O1 Co1 N1 88.28(15) 2_765 . ?
O1 Co1 N1 174.18(15) 3_675 . ?
O1 Co1 N1 85.15(14) . . ?
O1 Co1 N1 174.18(15) 2_765 3_675 ?
O1 Co1 N1 85.15(14) 3_675 3_675 ?
O1 Co1 N1 88.28(15) . 3_675 ?
N1 Co1 N1 96.87(15) . 3_675 ?
O1 Co1 N1 85.15(14) 2_765 2_765 ?
O1 Co1 N1 88.28(15) 3_675 2_765 ?
O1 Co1 N1 174.18(15) . 2_765 ?
N1 Co1 N1 96.87(15) . 2_765 ?
N1 Co1 N1 96.87(14) 3_675 2_765 ?
N1 C1 C2 122.0(4) . . ?
N1 C1 C6 113.9(4) . . ?
C2 C1 C6 124.1(4) . . ?
C1 C2 C3 118.2(4) . . ?
C1 C2 C7 121.4(4) . . ?
C3 C2 C7 120.5(4) . . ?
C4 C3 C2 119.8(4) . . ?
C4 C3 H3 120.1 . . ?
C2 C3 H3 120.1 . . ?
C3 C4 C5 118.9(4) . . ?
C3 C4 H4 120.6 . . ?
C5 C4 H4 120.6 . . ?
N1 C5 C4 122.0(4) . . ?
N1 C5 H5 119.0 . . ?
C4 C5 H5 119.0 . . ?
O2 C6 O1 127.1(4) . . ?
O2 C6 C1 121.0(4) . . ?
O1 C6 C1 111.9(4) . . ?
O4 C7 O3 121.0(5) . . ?
O4 C7 C2 118.9(4) . . ?
O3 C7 C2 120.1(4) . . ?
C5 N1 C1 119.1(4) . . ?
C5 N1 Co1 129.0(3) . . ?
C1 N1 Co1 111.6(3) . . ?
C6 O1 Co1 116.9(3) . . ?
C7 O3 Dy1 94.0(3) . . ?
C7 O4 Dy1 90.9(3) . . ?
Dy1 O5 H5A 109.3 . . ?
Dy1 O5 H5B 109.4 . . ?
H5A O5 H5B 109.5 . . ?

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 C1 C2 C3 -0.7(7) . . . . ?
C6 C1 C2 C3 179.1(4) . . . . ?
N1 C1 C2 C7 179.1(4) . . . . ?
C6 C1 C2 C7 -1.0(7) . . . . ?
C1 C2 C3 C4 -0.6(7) . . . . ?
C7 C2 C3 C4 179.5(5) . . . . ?
C2 C3 C4 C5 2.4(8) . . . . ?
C3 C4 C5 N1 -2.9(8) . . . . ?
N1 C1 C6 O2 178.0(4) . . . . ?
C2 C1 C6 O2 -1.9(7) . . . . ?
N1 C1 C6 O1 -0.4(5) . . . . ?
C2 C1 C6 O1 179.7(4) . . . . ?
C1 C2 C7 O4 -88.1(6) . . . . ?
C3 C2 C7 O4 91.7(6) . . . . ?
C1 C2 C7 O3 95.0(6) . . . . ?
C3 C2 C7 O3 -85.2(6) . . . . ?
C4 C5 N1 C1 1.6(7) . . . . ?
C4 C5 N1 Co1 175.8(4) . . . . ?
C2 C1 N1 C5 0.3(7) . . . . ?
C6 C1 N1 C5 -179.6(4) . . . . ?
C2 C1 N1 Co1 -174.9(4) . . . . ?
C6 C1 N1 Co1 5.2(4) . . . . ?
O1 Co1 N1 C5 -91.2(4) 2_765 . . . ?
O1 Co1 N1 C5 -158.4(13) 3_675 . . . ?
O1 Co1 N1 C5 179.2(4) . . . . ?
N1 Co1 N1 C5 91.5(3) 3_675 . . . ?
N1 Co1 N1 C5 -6.3(4) 2_765 . . . ?
O1 Co1 N1 C1 83.4(3) 2_765 . . . ?
O1 Co1 N1 C1 16.1(16) 3_675 . . . ?
O1 Co1 N1 C1 -6.2(3) . . . . ?
N1 Co1 N1 C1 -93.9(4) 3_675 . . . ?
N1 Co1 N1 C1 168.3(3) 2_765 . . . ?
O2 C6 O1 Co1 176.8(4) . . . . ?
C1 C6 O1 Co1 -4.9(5) . . . . ?
O1 Co1 O1 C6 -81.9(4) 2_765 . . . ?
O1 Co1 O1 C6 -171.4(3) 3_675 . . . ?
N1 Co1 O1 C6 6.4(3) . . . . ?
N1 Co1 O1 C6 103.5(3) 3_675 . . . ?
N1 Co1 O1 C6 -104.2(15) 2_765 . . . ?
O4 C7 O3 Dy1 3.3(5) . . . . ?
C2 C7 O3 Dy1 -179.8(4) . . . . ?
O5 Dy1 O3 C7 -4.9(4) . . . . ?
O5 Dy1 O3 C7 140.5(3) 3_665 . . . ?
O5 Dy1 O3 C7 72.2(3) 2_655 . . . ?
O3 Dy1 O3 C7 -80.6(4) 3_665 . . . ?
O3 Dy1 O3 C7 -159.6(3) 2_655 . . . ?
O4 Dy1 O3 C7 -102.9(3) 3_665 . . . ?
O4 Dy1 O3 C7 -1.8(3) . . . . ?
O4 Dy1 O3 C7 144.3(3) 2_655 . . . ?
C7 Dy1 O3 C7 -89.9(2) 3_665 . . . ?
C7 Dy1 O3 C7 172.5(3) 2_655 . . . ?
O3 C7 O4 Dy1 -3.2(5) . . . . ?
C2 C7 O4 Dy1 179.9(4) . . . . ?
O5 Dy1 O4 C7 179.2(3) . . . . ?
O5 Dy1 O4 C7 -142.2(3) 3_665 . . . ?
O5 Dy1 O4 C7 -95.1(3) 2_655 . . . ?
O3 Dy1 O4 C7 87.0(3) 3_665 . . . ?
O3 Dy1 O4 C7 28.9(3) 2_655 . . . ?
O3 Dy1 O4 C7 1.8(3) . . . . ?
O4 Dy1 O4 C7 117.8(3) 3_665 . . . ?
O4 Dy1 O4 C7 -35.5(3) 2_655 . . . ?
C7 Dy1 O4 C7 102.5(4) 3_665 . . . ?
C7 Dy1 O4 C7 -5.1(3) 2_655 . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O5 H5B O2 0.85 2.08 2.815(5) 143.9 3_665
O5 H5A O3 0.85 2.20 2.709(5) 118.6 3_666

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.99
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.228
_refine_diff_density_min         -0.393
_refine_diff_density_rms         0.070
# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.333 0.667 -0.060 355 241 ' '
_platon_squeeze_details          
;
;

####################################################################### 
# 
# 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_2
_database_code_depnum_ccdc_archive 'CCDC 1040741'

_audit_update_record             
;
2014-12-22 deposited with the CCDC.
2015-04-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C21 H15 Co Ho N3 O15'
_chemical_formula_sum            'C21 H15 Co Ho N3 O15'
_chemical_formula_weight         773.22

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

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   P3
_symmetry_space_group_name_Hall  P3

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'

_cell_length_a                   13.0601(3)
_cell_length_b                   13.0601(3)
_cell_length_c                   5.8637(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     866.15(5)
_cell_formula_units_Z            1
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    2497
_cell_measurement_theta_min      3.12
_cell_measurement_theta_max      29.69

_exptl_crystal_description       stick
_exptl_crystal_colour            purple
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.482
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             376
_exptl_absorpt_coefficient_mu    2.806
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3232
_exptl_absorpt_correction_T_max  0.7294
_exptl_absorpt_process_details   'SADABS(Bruker, 2000)'

_exptl_special_details           ?

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6602
_diffrn_reflns_av_R_equivalents  0.0370
_diffrn_reflns_av_sigmaI/netI    0.0723
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         1.80
_diffrn_reflns_theta_max         30.52
_reflns_number_total             3194
_reflns_number_gt                3141
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0061P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.067(10)
_refine_ls_number_reflns         3194
_refine_ls_number_parameters     124
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0297
_refine_ls_R_factor_gt           0.0291
_refine_ls_wR_factor_ref         0.0583
_refine_ls_wR_factor_gt          0.0581
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_restrained_S_all      1.000
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ho1 Ho 0.0000 0.0000 1.10937(2) 0.01735(7) Uani 1 3 d S . .
Co1 Co 0.3333 0.6667 0.90106(16) 0.01808(19) Uani 1 3 d S . .
C1 C 0.1818(3) 0.4317(3) 0.8398(7) 0.0202(8) Uani 1 1 d . . .
C2 C 0.0898(3) 0.3253(3) 0.7618(7) 0.0222(9) Uani 1 1 d . . .
C3 C 0.0286(4) 0.3257(4) 0.5679(7) 0.0262(9) Uani 1 1 d . . .
H3 H -0.0330 0.2554 0.5104 0.031 Uiso 1 1 calc R . .
C4 C 0.0611(4) 0.4334(4) 0.4605(7) 0.0269(9) Uani 1 1 d . . .
H4 H 0.0213 0.4360 0.3312 0.032 Uiso 1 1 calc R . .
C5 C 0.1532(3) 0.5351(3) 0.5500(7) 0.0221(8) Uani 1 1 d . . .
H5 H 0.1746 0.6068 0.4793 0.027 Uiso 1 1 calc R . .
C6 C 0.2567(4) 0.4444(3) 1.0510(7) 0.0235(9) Uani 1 1 d . . .
C7 C 0.0561(3) 0.2116(4) 0.8854(8) 0.0235(9) Uani 1 1 d . . .
N1 N 0.2131(3) 0.5349(3) 0.7351(6) 0.0161(6) Uani 1 1 d . . .
O1 O 0.3363(2) 0.5512(2) 1.0869(5) 0.0218(6) Uani 1 1 d . . .
O2 O 0.2426(2) 0.3577(2) 1.1567(5) 0.0319(8) Uani 1 1 d . . .
O3 O 0.1002(3) 0.1486(2) 0.8191(5) 0.0258(6) Uani 1 1 d . . .
O4 O -0.0170(2) 0.1793(2) 1.0478(5) 0.0270(6) Uani 1 1 d . . .
O5 O -0.1384(3) -0.0022(3) 1.3699(6) 0.0329(8) Uani 1 1 d . . .
H5A H -0.1655 -0.0628 1.4527 0.049 Uiso 1 1 d R . .
H5B H -0.1940 -0.0023 1.2973 0.049 Uiso 1 1 d R . .


_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 2.356(3) 3 ?
Ho1 O5 2.356(3) 2 ?
Ho1 O5 2.356(3) . ?
Ho1 O3 2.416(3) 2 ?
Ho1 O3 2.416(3) 3 ?
Ho1 O3 2.416(3) . ?
Ho1 O4 2.486(3) 2 ?
Ho1 O4 2.486(3) 3 ?
Ho1 O4 2.486(3) . ?
Ho1 C7 2.806(4) 2 ?
Ho1 C7 2.806(4) 3 ?
Co1 O1 1.876(3) 3_565 ?
Co1 O1 1.876(3) 2_665 ?
Co1 O1 1.876(3) . ?
Co1 N1 1.916(3) 3_565 ?
Co1 N1 1.916(3) . ?
Co1 N1 1.916(3) 2_665 ?
C1 N1 1.345(5) . ?
C1 C2 1.384(5) . ?
C1 C6 1.534(5) . ?
C2 C3 1.391(6) . ?
C2 C7 1.507(5) . ?
C3 C4 1.399(6) . ?
C3 H3 0.9300 . ?
C4 C5 1.374(6) . ?
C4 H4 0.9300 . ?
C5 N1 1.340(5) . ?
C5 H5 0.9300 . ?
C6 O2 1.222(5) . ?
C6 O1 1.273(4) . ?
C7 O4 1.262(5) . ?
C7 O3 1.279(5) . ?
O5 H5A 0.8415 . ?
O5 H5B 0.8416 . ?

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 82.48(12) 3 2 ?
O5 Ho1 O5 82.48(12) 3 . ?
O5 Ho1 O5 82.48(12) 2 . ?
O5 Ho1 O3 148.99(10) 3 2 ?
O5 Ho1 O3 124.83(10) 2 2 ?
O5 Ho1 O3 86.71(10) . 2 ?
O5 Ho1 O3 124.83(10) 3 3 ?
O5 Ho1 O3 86.71(10) 2 3 ?
O5 Ho1 O3 148.99(10) . 3 ?
O3 Ho1 O3 75.83(11) 2 3 ?
O5 Ho1 O3 86.71(10) 3 . ?
O5 Ho1 O3 148.99(10) 2 . ?
O5 Ho1 O3 124.83(10) . . ?
O3 Ho1 O3 75.83(11) 2 . ?
O3 Ho1 O3 75.83(11) 3 . ?
O5 Ho1 O4 147.76(11) 3 2 ?
O5 Ho1 O4 71.13(11) 2 2 ?
O5 Ho1 O4 76.14(11) . 2 ?
O3 Ho1 O4 53.77(9) 2 2 ?
O3 Ho1 O4 72.87(9) 3 2 ?
O3 Ho1 O4 125.34(10) . 2 ?
O5 Ho1 O4 71.13(10) 3 3 ?
O5 Ho1 O4 76.14(11) 2 3 ?
O5 Ho1 O4 147.76(11) . 3 ?
O3 Ho1 O4 125.34(10) 2 3 ?
O3 Ho1 O4 53.77(9) 3 3 ?
O3 Ho1 O4 72.87(9) . 3 ?
O4 Ho1 O4 117.93(3) 2 3 ?
O5 Ho1 O4 76.14(11) 3 . ?
O5 Ho1 O4 147.76(11) 2 . ?
O5 Ho1 O4 71.13(10) . . ?
O3 Ho1 O4 72.87(9) 2 . ?
O3 Ho1 O4 125.34(10) 3 . ?
O3 Ho1 O4 53.77(9) . . ?
O4 Ho1 O4 117.93(3) 2 . ?
O4 Ho1 O4 117.93(4) 3 . ?
O5 Ho1 C7 162.06(11) 3 2 ?
O5 Ho1 C7 97.83(12) 2 2 ?
O5 Ho1 C7 79.80(12) . 2 ?
O3 Ho1 C7 27.06(11) 2 2 ?
O3 Ho1 C7 72.99(11) 3 2 ?
O3 Ho1 C7 101.17(12) . 2 ?
O4 Ho1 C7 26.71(11) 2 2 ?
O4 Ho1 C7 126.50(10) 3 2 ?
O4 Ho1 C7 95.42(11) . 2 ?
O5 Ho1 C7 97.83(12) 3 3 ?
O5 Ho1 C7 79.80(12) 2 3 ?
O5 Ho1 C7 162.06(11) . 3 ?
O3 Ho1 C7 101.17(12) 2 3 ?
O3 Ho1 C7 27.06(11) 3 3 ?
O3 Ho1 C7 72.99(11) . 3 ?
O4 Ho1 C7 95.42(11) 2 3 ?
O4 Ho1 C7 26.71(11) 3 3 ?
O4 Ho1 C7 126.50(10) . 3 ?
C7 Ho1 C7 99.87(11) 2 3 ?
O1 Co1 O1 89.67(12) 3_565 2_665 ?
O1 Co1 O1 89.67(12) 3_565 . ?
O1 Co1 O1 89.67(12) 2_665 . ?
O1 Co1 N1 84.83(12) 3_565 3_565 ?
O1 Co1 N1 88.83(13) 2_665 3_565 ?
O1 Co1 N1 174.31(13) . 3_565 ?
O1 Co1 N1 88.83(13) 3_565 . ?
O1 Co1 N1 174.31(13) 2_665 . ?
O1 Co1 N1 84.83(12) . . ?
N1 Co1 N1 96.50(13) 3_565 . ?
O1 Co1 N1 174.31(13) 3_565 2_665 ?
O1 Co1 N1 84.83(12) 2_665 2_665 ?
O1 Co1 N1 88.83(13) . 2_665 ?
N1 Co1 N1 96.50(13) 3_565 2_665 ?
N1 Co1 N1 96.50(13) . 2_665 ?
N1 C1 C2 122.1(4) . . ?
N1 C1 C6 113.7(3) . . ?
C2 C1 C6 124.2(3) . . ?
C1 C2 C3 118.6(4) . . ?
C1 C2 C7 120.6(3) . . ?
C3 C2 C7 120.8(4) . . ?
C2 C3 C4 119.0(4) . . ?
C2 C3 H3 120.5 . . ?
C4 C3 H3 120.5 . . ?
C5 C4 C3 118.7(4) . . ?
C5 C4 H4 120.7 . . ?
C3 C4 H4 120.7 . . ?
N1 C5 C4 122.4(4) . . ?
N1 C5 H5 118.8 . . ?
C4 C5 H5 118.8 . . ?
O2 C6 O1 126.4(4) . . ?
O2 C6 C1 121.1(4) . . ?
O1 C6 C1 112.3(3) . . ?
O4 C7 O3 121.5(4) . . ?
O4 C7 C2 119.5(4) . . ?
O3 C7 C2 119.0(4) . . ?
C5 N1 C1 119.2(3) . . ?
C5 N1 Co1 128.8(3) . . ?
C1 N1 Co1 111.7(3) . . ?
C6 O1 Co1 116.8(3) . . ?
C7 O3 Ho1 93.7(2) . . ?
C7 O4 Ho1 90.9(2) . . ?
Ho1 O5 H5A 110.2 . . ?
Ho1 O5 H5B 109.2 . . ?
H5A O5 H5B 109.5 . . ?

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 C1 C2 C3 0.5(6) . . . . ?
C6 C1 C2 C3 180.0(4) . . . . ?
N1 C1 C2 C7 -179.1(4) . . . . ?
C6 C1 C2 C7 0.4(6) . . . . ?
C1 C2 C3 C4 -0.9(6) . . . . ?
C7 C2 C3 C4 178.8(4) . . . . ?
C2 C3 C4 C5 0.4(6) . . . . ?
C3 C4 C5 N1 0.4(6) . . . . ?
N1 C1 C6 O2 -176.2(4) . . . . ?
C2 C1 C6 O2 4.3(6) . . . . ?
N1 C1 C6 O1 -0.8(5) . . . . ?
C2 C1 C6 O1 179.7(4) . . . . ?
C1 C2 C7 O4 87.5(5) . . . . ?
C3 C2 C7 O4 -92.1(5) . . . . ?
C1 C2 C7 O3 -94.2(5) . . . . ?
C3 C2 C7 O3 86.2(5) . . . . ?
C4 C5 N1 C1 -0.7(6) . . . . ?
C4 C5 N1 Co1 -173.8(3) . . . . ?
C2 C1 N1 C5 0.3(6) . . . . ?
C6 C1 N1 C5 -179.2(4) . . . . ?
C2 C1 N1 Co1 174.5(3) . . . . ?
C6 C1 N1 Co1 -5.0(4) . . . . ?
O1 Co1 N1 C5 90.5(4) 3_565 . . . ?
O1 Co1 N1 C5 165.2(11) 2_665 . . . ?
O1 Co1 N1 C5 -179.7(4) . . . . ?
N1 Co1 N1 C5 5.8(4) 3_565 . . . ?
N1 Co1 N1 C5 -91.5(3) 2_665 . . . ?
O1 Co1 N1 C1 -83.0(3) 3_565 . . . ?
O1 Co1 N1 C1 -8.3(14) 2_665 . . . ?
O1 Co1 N1 C1 6.8(3) . . . . ?
N1 Co1 N1 C1 -167.7(3) 3_565 . . . ?
N1 Co1 N1 C1 95.0(3) 2_665 . . . ?
O2 C6 O1 Co1 -178.4(4) . . . . ?
C1 C6 O1 Co1 6.6(4) . . . . ?
O1 Co1 O1 C6 81.1(3) 3_565 . . . ?
O1 Co1 O1 C6 170.8(3) 2_665 . . . ?
N1 Co1 O1 C6 96.1(13) 3_565 . . . ?
N1 Co1 O1 C6 -7.7(3) . . . . ?
N1 Co1 O1 C6 -104.4(3) 2_665 . . . ?
O4 C7 O3 Ho1 -2.5(4) . . . . ?
C2 C7 O3 Ho1 179.3(3) . . . . ?
O5 Ho1 O3 C7 -73.9(2) 3 . . . ?
O5 Ho1 O3 C7 -143.4(2) 2 . . . ?
O5 Ho1 O3 C7 4.6(3) . . . . ?
O3 Ho1 O3 C7 80.3(3) 2 . . . ?
O3 Ho1 O3 C7 158.9(2) 3 . . . ?
O4 Ho1 O3 C7 102.4(2) 2 . . . ?
O4 Ho1 O3 C7 -145.1(3) 3 . . . ?
O4 Ho1 O3 C7 1.3(2) . . . . ?
C7 Ho1 O3 C7 89.87(18) 2 . . . ?
C7 Ho1 O3 C7 -173.1(3) 3 . . . ?
O3 C7 O4 Ho1 2.4(4) . . . . ?
C2 C7 O4 Ho1 -179.4(3) . . . . ?
O5 Ho1 O4 C7 94.8(3) 3 . . . ?
O5 Ho1 O4 C7 144.8(2) 2 . . . ?
O5 Ho1 O4 C7 -178.5(3) . . . . ?
O3 Ho1 O4 C7 -86.1(3) 2 . . . ?
O3 Ho1 O4 C7 -28.3(3) 3 . . . ?
O3 Ho1 O4 C7 -1.3(2) . . . . ?
O4 Ho1 O4 C7 -116.4(2) 2 . . . ?
O4 Ho1 O4 C7 35.4(3) 3 . . . ?
C7 Ho1 O4 C7 -101.2(3) 2 . . . ?
C7 Ho1 O4 C7 5.3(3) 3 . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O5 H5A O3 0.84 2.16 2.690(4) 121.0 2_556
O5 H5B O2 0.84 2.07 2.778(4) 142.0 2

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        30.52
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.750
_refine_diff_density_min         -0.704
_refine_diff_density_rms         0.085
# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.667 0.333 -0.081 338 248 ' '
_platon_squeeze_details          
;
;

####################################################################### 
# 
# 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_3
_database_code_depnum_ccdc_archive 'CCDC 1040742'
_audit_update_record             
;
2014-12-22 deposited with the CCDC.
2015-04-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C21 H15 Co Er N3 O15'
_chemical_formula_sum            'C21 H15 Co Er N3 O15'
_chemical_formula_weight         775.55

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'

_symmetry_cell_setting           Trigonal
_symmetry_space_group_name_H-M   P3
_symmetry_space_group_name_Hall  P3

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'

_cell_length_a                   13.0479(3)
_cell_length_b                   13.0479(3)
_cell_length_c                   5.8596(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     863.93(4)
_cell_formula_units_Z            1
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    3173
_cell_measurement_theta_min      3.12
_cell_measurement_theta_max      29.72

_exptl_crystal_description       stick
_exptl_crystal_colour            purple
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.491
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             377
_exptl_absorpt_coefficient_mu    2.952
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3437
_exptl_absorpt_correction_T_max  0.7183
_exptl_absorpt_process_details   'SADABS(Bruker, 2000)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6528
_diffrn_reflns_av_R_equivalents  0.0341
_diffrn_reflns_av_sigmaI/netI    0.0663
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         3.12
_diffrn_reflns_theta_max         30.50
_reflns_number_total             3003
_reflns_number_gt                2970
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0140P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.007(10)
_refine_ls_number_reflns         3003
_refine_ls_number_parameters     124
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0304
_refine_ls_R_factor_gt           0.0299
_refine_ls_wR_factor_ref         0.0609
_refine_ls_wR_factor_gt          0.0606
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_restrained_S_all      1.001
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Er1 Er 0.0000 0.0000 1.109370(11) 0.01852(8) Uani 1 3 d S . .
Co1 Co 0.3333 0.6667 0.90212(15) 0.0182(2) Uani 1 3 d S . .
C1 C 0.1828(3) 0.4318(3) 0.8404(6) 0.0180(8) Uani 1 1 d . . .
C2 C 0.0915(4) 0.3272(4) 0.7644(7) 0.0210(9) Uani 1 1 d . . .
C3 C 0.0305(4) 0.3266(4) 0.5676(7) 0.0291(10) Uani 1 1 d U . .
H3 H -0.0305 0.2559 0.5098 0.035 Uiso 1 1 calc R . .
C4 C 0.0617(4) 0.4315(4) 0.4617(7) 0.0289(10) Uani 1 1 d U . .
H4 H 0.0218 0.4335 0.3319 0.035 Uiso 1 1 calc R . .
C5 C 0.1537(4) 0.5342(4) 0.5508(7) 0.0221(8) Uani 1 1 d . . .
H5 H 0.1752 0.6059 0.4799 0.027 Uiso 1 1 calc R . .
C6 C 0.2569(4) 0.4433(4) 1.0498(7) 0.0249(9) Uani 1 1 d . . .
C7 C 0.0567(4) 0.2104(4) 0.8870(7) 0.0243(9) Uani 1 1 d . . .
N1 N 0.2128(3) 0.5334(3) 0.7371(5) 0.0176(7) Uani 1 1 d . . .
O1 O 0.3378(2) 0.5509(2) 1.0899(5) 0.0228(6) Uani 1 1 d . . .
O2 O 0.2425(3) 0.3574(3) 1.1588(5) 0.0320(7) Uani 1 1 d . . .
O3 O 0.1003(3) 0.1473(3) 0.8196(5) 0.0272(7) Uani 1 1 d . . .
O4 O -0.0160(3) 0.1774(3) 1.0495(5) 0.0286(7) Uani 1 1 d . . .
O5 O -0.1368(3) -0.0034(3) 1.3682(5) 0.0327(8) Uani 1 1 d . . .
H5A H -0.1640 -0.0640 1.4510 0.049 Uiso 1 1 d R . .
H5B H -0.1925 -0.0035 1.2956 0.049 Uiso 1 1 d R . .


_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 O5 2.327(3) 3 ?
Er1 O5 2.327(3) 2 ?
Er1 O5 2.327(3) . ?
Er1 O3 2.403(3) 3 ?
Er1 O3 2.403(3) 2 ?
Er1 O3 2.403(3) . ?
Er1 O4 2.451(3) 2 ?
Er1 O4 2.451(3) 3 ?
Er1 O4 2.451(3) . ?
Er1 C7 2.784(4) 2 ?
Er1 C7 2.784(4) 3 ?
Co1 O1 1.893(3) 3_565 ?
Co1 O1 1.893(3) 2_665 ?
Co1 O1 1.893(3) . ?
Co1 N1 1.923(3) 3_565 ?
Co1 N1 1.923(3) . ?
Co1 N1 1.923(3) 2_665 ?
C1 N1 1.325(5) . ?
C1 C2 1.362(6) . ?
C1 C6 1.523(5) . ?
C2 C3 1.399(6) . ?
C2 C7 1.534(6) . ?
C3 C4 1.366(6) . ?
C3 H3 0.9300 . ?
C4 C5 1.379(6) . ?
C4 H4 0.9300 . ?
C5 N1 1.340(5) . ?
C5 H5 0.9300 . ?
C6 O2 1.221(5) . ?
C6 O1 1.288(5) . ?
C7 O4 1.258(5) . ?
C7 O3 1.276(5) . ?
O5 H5A 0.8408 . ?
O5 H5B 0.8408 . ?

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 Er1 O5 82.09(13) 3 2 ?
O5 Er1 O5 82.09(13) 3 . ?
O5 Er1 O5 82.09(13) 2 . ?
O5 Er1 O3 125.58(11) 3 3 ?
O5 Er1 O3 87.00(10) 2 3 ?
O5 Er1 O3 148.52(11) . 3 ?
O5 Er1 O3 148.52(11) 3 2 ?
O5 Er1 O3 125.58(11) 2 2 ?
O5 Er1 O3 87.00(10) . 2 ?
O3 Er1 O3 75.57(11) 3 2 ?
O5 Er1 O3 87.00(10) 3 . ?
O5 Er1 O3 148.52(11) 2 . ?
O5 Er1 O3 125.58(11) . . ?
O3 Er1 O3 75.57(11) 3 . ?
O3 Er1 O3 75.57(11) 2 . ?
O5 Er1 O4 147.42(11) 3 2 ?
O5 Er1 O4 71.59(11) 2 2 ?
O5 Er1 O4 75.70(11) . 2 ?
O3 Er1 O4 72.84(10) 3 2 ?
O3 Er1 O4 54.07(9) 2 2 ?
O3 Er1 O4 125.35(10) . 2 ?
O5 Er1 O4 71.59(11) 3 3 ?
O5 Er1 O4 75.70(11) 2 3 ?
O5 Er1 O4 147.42(11) . 3 ?
O3 Er1 O4 54.07(9) 3 3 ?
O3 Er1 O4 125.35(10) 2 3 ?
O3 Er1 O4 72.84(10) . 3 ?
O4 Er1 O4 117.99(3) 2 3 ?
O5 Er1 O4 75.70(11) 3 . ?
O5 Er1 O4 147.42(10) 2 . ?
O5 Er1 O4 71.59(11) . . ?
O3 Er1 O4 125.35(10) 3 . ?
O3 Er1 O4 72.84(10) 2 . ?
O3 Er1 O4 54.07(9) . . ?
O4 Er1 O4 117.99(3) 2 . ?
O4 Er1 O4 117.99(3) 3 . ?
O5 Er1 C7 161.48(11) 3 2 ?
O5 Er1 C7 98.44(13) 2 2 ?
O5 Er1 C7 79.66(12) . 2 ?
O3 Er1 C7 72.84(12) 3 2 ?
O3 Er1 C7 27.22(11) 2 2 ?
O3 Er1 C7 101.06(12) . 2 ?
O4 Er1 C7 26.86(11) 2 2 ?
O4 Er1 C7 126.63(11) 3 2 ?
O4 Er1 C7 95.43(12) . 2 ?
O5 Er1 C7 98.44(13) 3 3 ?
O5 Er1 C7 79.66(12) 2 3 ?
O5 Er1 C7 161.48(11) . 3 ?
O3 Er1 C7 27.22(11) 3 3 ?
O3 Er1 C7 101.06(12) 2 3 ?
O3 Er1 C7 72.84(12) . 3 ?
O4 Er1 C7 95.43(12) 2 3 ?
O4 Er1 C7 26.86(11) 3 3 ?
O4 Er1 C7 126.63(11) . 3 ?
C7 Er1 C7 99.87(12) 2 3 ?
O1 Co1 O1 89.61(12) 3_565 2_665 ?
O1 Co1 O1 89.61(12) 3_565 . ?
O1 Co1 O1 89.61(12) 2_665 . ?
O1 Co1 N1 84.73(13) 3_565 3_565 ?
O1 Co1 N1 88.52(13) 2_665 3_565 ?
O1 Co1 N1 174.05(13) . 3_565 ?
O1 Co1 N1 88.52(13) 3_565 . ?
O1 Co1 N1 174.05(13) 2_665 . ?
O1 Co1 N1 84.73(13) . . ?
N1 Co1 N1 96.93(13) 3_565 . ?
O1 Co1 N1 174.05(14) 3_565 2_665 ?
O1 Co1 N1 84.73(13) 2_665 2_665 ?
O1 Co1 N1 88.52(13) . 2_665 ?
N1 Co1 N1 96.93(13) 3_565 2_665 ?
N1 Co1 N1 96.93(13) . 2_665 ?
N1 C1 C2 121.8(3) . . ?
N1 C1 C6 114.4(3) . . ?
C2 C1 C6 123.8(4) . . ?
C1 C2 C3 119.0(4) . . ?
C1 C2 C7 121.3(4) . . ?
C3 C2 C7 119.7(4) . . ?
C4 C3 C2 119.0(4) . . ?
C4 C3 H3 120.5 . . ?
C2 C3 H3 120.5 . . ?
C3 C4 C5 118.7(4) . . ?
C3 C4 H4 120.6 . . ?
C5 C4 H4 120.6 . . ?
N1 C5 C4 121.7(4) . . ?
N1 C5 H5 119.1 . . ?
C4 C5 H5 119.1 . . ?
O2 C6 O1 124.9(4) . . ?
O2 C6 C1 122.2(4) . . ?
O1 C6 C1 112.9(3) . . ?
O4 C7 O3 121.1(4) . . ?
O4 C7 C2 119.5(4) . . ?
O3 C7 C2 119.4(4) . . ?
C1 N1 C5 119.7(3) . . ?
C1 N1 Co1 112.0(3) . . ?
C5 N1 Co1 128.1(3) . . ?
C6 O1 Co1 115.3(3) . . ?
C7 O3 Er1 93.3(2) . . ?
C7 O4 Er1 91.5(2) . . ?
Er1 O5 H5A 110.6 . . ?
Er1 O5 H5B 108.9 . . ?
H5A O5 H5B 109.5 . . ?

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 C1 C2 C3 2.1(6) . . . . ?
C6 C1 C2 C3 -179.0(4) . . . . ?
N1 C1 C2 C7 -179.3(4) . . . . ?
C6 C1 C2 C7 -0.4(6) . . . . ?
C1 C2 C3 C4 -2.1(6) . . . . ?
C7 C2 C3 C4 179.3(4) . . . . ?
C2 C3 C4 C5 0.9(6) . . . . ?
C3 C4 C5 N1 0.3(6) . . . . ?
N1 C1 C6 O2 -177.6(4) . . . . ?
C2 C1 C6 O2 3.5(6) . . . . ?
N1 C1 C6 O1 -0.7(5) . . . . ?
C2 C1 C6 O1 -179.6(4) . . . . ?
C1 C2 C7 O4 87.8(5) . . . . ?
C3 C2 C7 O4 -93.7(5) . . . . ?
C1 C2 C7 O3 -93.5(5) . . . . ?
C3 C2 C7 O3 85.1(5) . . . . ?
C2 C1 N1 C5 -1.0(6) . . . . ?
C6 C1 N1 C5 -179.9(4) . . . . ?
C2 C1 N1 Co1 173.9(3) . . . . ?
C6 C1 N1 Co1 -5.1(4) . . . . ?
C4 C5 N1 C1 -0.3(6) . . . . ?
C4 C5 N1 Co1 -174.2(3) . . . . ?
O1 Co1 N1 C1 -83.0(3) 3_565 . . . ?
O1 Co1 N1 C1 -11.3(14) 2_665 . . . ?
O1 Co1 N1 C1 6.7(3) . . . . ?
N1 Co1 N1 C1 -167.5(3) 3_565 . . . ?
N1 Co1 N1 C1 94.6(3) 2_665 . . . ?
O1 Co1 N1 C5 91.3(3) 3_565 . . . ?
O1 Co1 N1 C5 163.0(11) 2_665 . . . ?
O1 Co1 N1 C5 -179.0(4) . . . . ?
N1 Co1 N1 C5 6.8(4) 3_565 . . . ?
N1 Co1 N1 C5 -91.1(3) 2_665 . . . ?
O2 C6 O1 Co1 -176.9(3) . . . . ?
C1 C6 O1 Co1 6.3(4) . . . . ?
O1 Co1 O1 C6 81.1(3) 3_565 . . . ?
O1 Co1 O1 C6 170.7(3) 2_665 . . . ?
N1 Co1 O1 C6 99.1(13) 3_565 . . . ?
N1 Co1 O1 C6 -7.4(3) . . . . ?
N1 Co1 O1 C6 -104.5(3) 2_665 . . . ?
O4 C7 O3 Er1 -2.6(4) . . . . ?
C2 C7 O3 Er1 178.7(3) . . . . ?
O5 Er1 O3 C7 -73.1(3) 3 . . . ?
O5 Er1 O3 C7 -142.6(3) 2 . . . ?
O5 Er1 O3 C7 5.0(3) . . . . ?
O3 Er1 O3 C7 159.0(3) 3 . . . ?
O3 Er1 O3 C7 80.5(3) 2 . . . ?
O4 Er1 O3 C7 102.7(3) 2 . . . ?
O4 Er1 O3 C7 -144.7(3) 3 . . . ?
O4 Er1 O3 C7 1.4(2) . . . . ?
C7 Er1 O3 C7 90.09(19) 2 . . . ?
C7 Er1 O3 C7 -172.9(3) 3 . . . ?
O3 C7 O4 Er1 2.5(4) . . . . ?
C2 C7 O4 Er1 -178.8(3) . . . . ?
O5 Er1 O4 C7 95.4(3) 3 . . . ?
O5 Er1 O4 C7 143.9(3) 2 . . . ?
O5 Er1 O4 C7 -178.3(3) . . . . ?
O3 Er1 O4 C7 -28.4(3) 3 . . . ?
O3 Er1 O4 C7 -85.8(3) 2 . . . ?
O3 Er1 O4 C7 -1.4(2) . . . . ?
O4 Er1 O4 C7 -116.5(2) 2 . . . ?
O4 Er1 O4 C7 35.7(3) 3 . . . ?
C7 Er1 O4 C7 -101.1(3) 2 . . . ?
C7 Er1 O4 C7 5.4(3) 3 . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O5 H5B O2 0.84 2.06 2.778(4) 142.5 2
O5 H5A O3 0.84 2.17 2.694(4) 120.3 2_556

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        30.50
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         1.060
_refine_diff_density_min         -0.479
_refine_diff_density_rms         0.103
# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.667 0.333 -0.081 337 56 ' '
_platon_squeeze_details          
;
;

####################################################################### 
# 
# 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_4
_database_code_depnum_ccdc_archive 'CCDC 1040743'
_audit_update_record             
;
2014-12-22 deposited with the CCDC.
2015-04-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C21 H15 Co N3 O15 Tm'
_chemical_formula_sum            'C21 H15 Co N3 O15 Tm'
_chemical_formula_weight         777.22

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'
Tm Tm -0.3139 5.2483 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Trigonal
_symmetry_space_group_name_H-M   P3
_symmetry_space_group_name_Hall  P3

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'

_cell_length_a                   13.0373(3)
_cell_length_b                   13.0373(3)
_cell_length_c                   5.8491(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     860.98(5)
_cell_formula_units_Z            1
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    2332
_cell_measurement_theta_min      3.12
_cell_measurement_theta_max      27.15

_exptl_crystal_description       stick
_exptl_crystal_colour            purple
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.499
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             378
_exptl_absorpt_coefficient_mu    3.102
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3558
_exptl_absorpt_correction_T_max  0.7894
_exptl_absorpt_process_details   'SADABS(Bruker, 2000)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6498
_diffrn_reflns_av_R_equivalents  0.0375
_diffrn_reflns_av_sigmaI/netI    0.0766
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_theta_min         3.13
_diffrn_reflns_theta_max         30.54
_reflns_number_total             3146
_reflns_number_gt                3102
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0136P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.007(10)
_refine_ls_number_reflns         3146
_refine_ls_number_parameters     124
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0336
_refine_ls_R_factor_gt           0.0329
_refine_ls_wR_factor_ref         0.0669
_refine_ls_wR_factor_gt          0.0666
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_restrained_S_all      1.002
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Tm1 Tm 1.0000 1.0000 -0.1094 0.01638(8) Uani 1 3 d S . .
Co1 Co 0.6667 0.3333 0.09869(15) 0.0161(2) Uani 1 3 d S . .
C1 C 0.8181(4) 0.5685(4) 0.1589(7) 0.0160(8) Uani 1 1 d . . .
C2 C 0.9093(4) 0.6731(4) 0.2342(7) 0.0182(9) Uani 1 1 d . . .
C3 C 0.9705(4) 0.6746(4) 0.4340(7) 0.0231(9) Uani 1 1 d . . .
H3 H 1.0305 0.7455 0.4937 0.028 Uiso 1 1 calc R . .
C4 C 0.9393(4) 0.5681(5) 0.5386(8) 0.0265(10) Uani 1 1 d . . .
H4 H 0.9801 0.5653 0.6666 0.032 Uiso 1 1 calc R . .
C5 C 0.8464(4) 0.4659(4) 0.4494(7) 0.0211(9) Uani 1 1 d . . .
H5 H 0.8244 0.3940 0.5208 0.025 Uiso 1 1 calc R . .
C6 C 0.7429(4) 0.5556(4) -0.0479(7) 0.0207(9) Uani 1 1 d . . .
C7 C 0.9436(4) 0.7898(4) 0.1124(8) 0.0224(10) Uani 1 1 d . . .
N1 N 0.7870(3) 0.4664(3) 0.2645(6) 0.0149(7) Uani 1 1 d . . .
O1 O 0.6618(3) 0.4490(3) -0.0882(5) 0.0196(6) Uani 1 1 d . . .
O2 O 0.7576(3) 0.6426(3) -0.1582(5) 0.0294(8) Uani 1 1 d . . .
O3 O 0.8998(3) 0.8527(3) 0.1794(5) 0.0241(7) Uani 1 1 d . . .
O4 O 1.0166(3) 0.8223(3) -0.0497(5) 0.0270(7) Uani 1 1 d . . .
O5 O 1.1364(3) 1.0041(3) -0.3669(6) 0.0323(8) Uani 1 1 d . . .
H5A H 1.1636 1.0647 -0.4497 0.048 Uiso 1 1 d R . .
H5B H 1.1921 1.0042 -0.2943 0.048 Uiso 1 1 d R . .


_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
Tm1 O5 2.311(3) 3_675 ?
Tm1 O5 2.311(3) . ?
Tm1 O5 2.311(3) 2_765 ?
Tm1 O3 2.395(3) 2_765 ?
Tm1 O3 2.395(3) . ?
Tm1 O3 2.395(3) 3_675 ?
Tm1 O4 2.457(3) 2_765 ?
Tm1 O4 2.457(3) . ?
Tm1 O4 2.457(3) 3_675 ?
Tm1 C7 2.778(5) 2_765 ?
Tm1 C7 2.778(5) 3_675 ?
Co1 O1 1.889(3) 3_665 ?
Co1 O1 1.889(3) 2_655 ?
Co1 O1 1.889(3) . ?
Co1 N1 1.921(3) 3_665 ?
Co1 N1 1.921(3) . ?
Co1 N1 1.921(3) 2_655 ?
C1 N1 1.333(5) . ?
C1 C2 1.359(6) . ?
C1 C6 1.512(6) . ?
C2 C3 1.410(6) . ?
C2 C7 1.530(6) . ?
C3 C4 1.379(7) . ?
C3 H3 0.9300 . ?
C4 C5 1.379(7) . ?
C4 H4 0.9300 . ?
C5 N1 1.332(5) . ?
C5 H5 0.9300 . ?
C6 O2 1.233(5) . ?
C6 O1 1.279(5) . ?
C7 O4 1.257(5) . ?
C7 O3 1.273(5) . ?
O5 H5A 0.8399 . ?
O5 H5B 0.8399 . ?

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 Tm1 O5 82.11(14) 3_675 . ?
O5 Tm1 O5 82.11(14) 3_675 2_765 ?
O5 Tm1 O5 82.11(14) . 2_765 ?
O5 Tm1 O3 148.35(11) 3_675 2_765 ?
O5 Tm1 O3 86.82(12) . 2_765 ?
O5 Tm1 O3 125.65(12) 2_765 2_765 ?
O5 Tm1 O3 86.82(12) 3_675 . ?
O5 Tm1 O3 125.65(12) . . ?
O5 Tm1 O3 148.35(12) 2_765 . ?
O3 Tm1 O3 75.78(12) 2_765 . ?
O5 Tm1 O3 125.65(12) 3_675 3_675 ?
O5 Tm1 O3 148.35(12) . 3_675 ?
O5 Tm1 O3 86.82(12) 2_765 3_675 ?
O3 Tm1 O3 75.78(12) 2_765 3_675 ?
O3 Tm1 O3 75.78(12) . 3_675 ?
O5 Tm1 O4 147.38(12) 3_675 2_765 ?
O5 Tm1 O4 75.57(13) . 2_765 ?
O5 Tm1 O4 71.61(12) 2_765 2_765 ?
O3 Tm1 O4 54.11(10) 2_765 2_765 ?
O3 Tm1 O4 125.56(11) . 2_765 ?
O3 Tm1 O4 72.80(11) 3_675 2_765 ?
O5 Tm1 O4 75.57(12) 3_675 . ?
O5 Tm1 O4 71.61(12) . . ?
O5 Tm1 O4 147.38(12) 2_765 . ?
O3 Tm1 O4 72.80(11) 2_765 . ?
O3 Tm1 O4 54.11(10) . . ?
O3 Tm1 O4 125.56(11) 3_675 . ?
O4 Tm1 O4 118.02(4) 2_765 . ?
O5 Tm1 O4 71.61(12) 3_675 3_675 ?
O5 Tm1 O4 147.38(12) . 3_675 ?
O5 Tm1 O4 75.57(13) 2_765 3_675 ?
O3 Tm1 O4 125.56(11) 2_765 3_675 ?
O3 Tm1 O4 72.80(11) . 3_675 ?
O3 Tm1 O4 54.11(10) 3_675 3_675 ?
O4 Tm1 O4 118.02(4) 2_765 3_675 ?
O4 Tm1 O4 118.02(4) . 3_675 ?
O5 Tm1 C7 161.32(12) 3_675 2_765 ?
O5 Tm1 C7 79.50(14) . 2_765 ?
O5 Tm1 C7 98.51(14) 2_765 2_765 ?
O3 Tm1 C7 27.22(12) 2_765 2_765 ?
O3 Tm1 C7 101.26(13) . 2_765 ?
O3 Tm1 C7 72.94(12) 3_675 2_765 ?
O4 Tm1 C7 26.90(12) 2_765 2_765 ?
O4 Tm1 C7 95.40(13) . 2_765 ?
O4 Tm1 C7 126.78(12) 3_675 2_765 ?
O5 Tm1 C7 98.51(14) 3_675 3_675 ?
O5 Tm1 C7 161.32(12) . 3_675 ?
O5 Tm1 C7 79.50(13) 2_765 3_675 ?
O3 Tm1 C7 101.26(13) 2_765 3_675 ?
O3 Tm1 C7 72.94(12) . 3_675 ?
O3 Tm1 C7 27.22(12) 3_675 3_675 ?
O4 Tm1 C7 95.40(13) 2_765 3_675 ?
O4 Tm1 C7 126.78(12) . 3_675 ?
O4 Tm1 C7 26.90(12) 3_675 3_675 ?
C7 Tm1 C7 99.96(12) 2_765 3_675 ?
O1 Co1 O1 89.88(13) 3_665 2_655 ?
O1 Co1 O1 89.88(13) 3_665 . ?
O1 Co1 O1 89.88(13) 2_655 . ?
O1 Co1 N1 84.80(13) 3_665 3_665 ?
O1 Co1 N1 88.37(14) 2_655 3_665 ?
O1 Co1 N1 174.40(14) . 3_665 ?
O1 Co1 N1 88.37(14) 3_665 . ?
O1 Co1 N1 174.40(14) 2_655 . ?
O1 Co1 N1 84.80(13) . . ?
N1 Co1 N1 96.76(14) 3_665 . ?
O1 Co1 N1 174.40(14) 3_665 2_655 ?
O1 Co1 N1 84.80(13) 2_655 2_655 ?
O1 Co1 N1 88.37(14) . 2_655 ?
N1 Co1 N1 96.76(14) 3_665 2_655 ?
N1 Co1 N1 96.76(14) . 2_655 ?
N1 C1 C2 121.9(4) . . ?
N1 C1 C6 113.7(4) . . ?
C2 C1 C6 124.4(4) . . ?
C1 C2 C3 119.2(4) . . ?
C1 C2 C7 121.4(4) . . ?
C3 C2 C7 119.4(4) . . ?
C4 C3 C2 118.3(4) . . ?
C4 C3 H3 120.8 . . ?
C2 C3 H3 120.8 . . ?
C3 C4 C5 118.7(4) . . ?
C3 C4 H4 120.7 . . ?
C5 C4 H4 120.7 . . ?
N1 C5 C4 122.3(4) . . ?
N1 C5 H5 118.9 . . ?
C4 C5 H5 118.9 . . ?
O2 C6 O1 124.5(4) . . ?
O2 C6 C1 121.4(4) . . ?
O1 C6 C1 114.0(4) . . ?
O4 C7 O3 121.5(4) . . ?
O4 C7 C2 118.9(4) . . ?
O3 C7 C2 119.6(4) . . ?
C5 N1 C1 119.6(4) . . ?
C5 N1 Co1 128.3(3) . . ?
C1 N1 Co1 111.8(3) . . ?
C6 O1 Co1 114.9(3) . . ?
C7 O3 Tm1 93.4(3) . . ?
C7 O4 Tm1 90.9(3) . . ?
Tm1 O5 H5A 110.8 . . ?
Tm1 O5 H5B 108.9 . . ?
H5A O5 H5B 109.4 . . ?

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 C1 C2 C3 -2.0(6) . . . . ?
C6 C1 C2 C3 177.9(4) . . . . ?
N1 C1 C2 C7 -179.7(4) . . . . ?
C6 C1 C2 C7 0.3(6) . . . . ?
C1 C2 C3 C4 3.4(6) . . . . ?
C7 C2 C3 C4 -178.9(4) . . . . ?
C2 C3 C4 C5 -2.9(7) . . . . ?
C3 C4 C5 N1 0.9(7) . . . . ?
N1 C1 C6 O2 177.0(4) . . . . ?
C2 C1 C6 O2 -3.0(7) . . . . ?
N1 C1 C6 O1 0.0(5) . . . . ?
C2 C1 C6 O1 -179.9(4) . . . . ?
C1 C2 C7 O4 -88.2(5) . . . . ?
C3 C2 C7 O4 94.2(5) . . . . ?
C1 C2 C7 O3 93.1(5) . . . . ?
C3 C2 C7 O3 -84.5(5) . . . . ?
C4 C5 N1 C1 0.6(6) . . . . ?
C4 C5 N1 Co1 173.3(3) . . . . ?
C2 C1 N1 C5 0.0(6) . . . . ?
C6 C1 N1 C5 -180.0(4) . . . . ?
C2 C1 N1 Co1 -173.9(3) . . . . ?
C6 C1 N1 Co1 6.2(4) . . . . ?
O1 Co1 N1 C5 -90.8(4) 3_665 . . . ?
O1 Co1 N1 C5 -162.7(12) 2_655 . . . ?
O1 Co1 N1 C5 179.1(4) . . . . ?
N1 Co1 N1 C5 -6.3(4) 3_665 . . . ?
N1 Co1 N1 C5 91.4(3) 2_655 . . . ?
O1 Co1 N1 C1 82.4(3) 3_665 . . . ?
O1 Co1 N1 C1 10.5(15) 2_655 . . . ?
O1 Co1 N1 C1 -7.7(3) . . . . ?
N1 Co1 N1 C1 166.9(3) 3_665 . . . ?
N1 Co1 N1 C1 -95.4(4) 2_655 . . . ?
O2 C6 O1 Co1 176.7(4) . . . . ?
C1 C6 O1 Co1 -6.5(5) . . . . ?
O1 Co1 O1 C6 -80.4(4) 3_665 . . . ?
O1 Co1 O1 C6 -170.3(3) 2_655 . . . ?
N1 Co1 O1 C6 -98.4(14) 3_665 . . . ?
N1 Co1 O1 C6 8.0(3) . . . . ?
N1 Co1 O1 C6 104.9(3) 2_655 . . . ?
O4 C7 O3 Tm1 2.6(5) . . . . ?
C2 C7 O3 Tm1 -178.7(3) . . . . ?
O5 Tm1 O3 C7 73.1(3) 3_675 . . . ?
O5 Tm1 O3 C7 -4.9(3) . . . . ?
O5 Tm1 O3 C7 142.4(3) 2_765 . . . ?
O3 Tm1 O3 C7 -80.3(3) 2_765 . . . ?
O3 Tm1 O3 C7 -158.9(3) 3_675 . . . ?
O4 Tm1 O3 C7 -102.7(3) 2_765 . . . ?
O4 Tm1 O3 C7 -1.4(3) . . . . ?
O4 Tm1 O3 C7 144.8(3) 3_675 . . . ?
C7 Tm1 O3 C7 -89.9(2) 2_765 . . . ?
C7 Tm1 O3 C7 173.0(3) 3_675 . . . ?
O3 C7 O4 Tm1 -2.5(5) . . . . ?
C2 C7 O4 Tm1 178.8(4) . . . . ?
O5 Tm1 O4 C7 -95.2(3) 3_675 . . . ?
O5 Tm1 O4 C7 178.4(3) . . . . ?
O5 Tm1 O4 C7 -143.5(3) 2_765 . . . ?
O3 Tm1 O4 C7 86.0(3) 2_765 . . . ?
O3 Tm1 O4 C7 1.4(3) . . . . ?
O3 Tm1 O4 C7 28.5(3) 3_675 . . . ?
O4 Tm1 O4 C7 116.8(2) 2_765 . . . ?
O4 Tm1 O4 C7 -35.6(3) 3_675 . . . ?
C7 Tm1 O4 C7 101.4(3) 2_765 . . . ?
C7 Tm1 O4 C7 -5.3(3) 3_675 . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O5 H5B O2 0.84 2.06 2.778(5) 142.7 2_765
O5 H5A O3 0.84 2.18 2.701(4) 120.1 2_764

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        30.54
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         1.035
_refine_diff_density_min         -0.505
_refine_diff_density_rms         0.114
# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.333 0.667 -0.001 335 61 ' '
_platon_squeeze_details          
;
;

