# Electronic Supplementary Material (ESI) for ChemComm.
# 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_a
_database_code_depnum_ccdc_archive 'CCDC 1031893'
_audit_update_record             
;
2014-10-31 deposited with the CCDC.
2015-02-18 downloaded from the CCDC.
;
_audit_creation_date             2014-10-22
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_shelxl_version_number           2013-2
_chemical_name_common            ?
_chemical_name_systematic        '[NaCo3(IA)6](NO3)'
_chemical_formula_moiety         '0.5(C72 H48 Co6 N24 Na2 O24), N1 O3, 0.25(O1)'
_chemical_formula_sum            'C36 H24 Co3 N13 Na O15.25'
_chemical_formula_weight         1082.46
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Co C N O H Na'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 -2.3653 3.6143 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.1353 0.1239 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      hexagonal
_space_group_IT_number           173
_space_group_name_H-M_alt        'P 63'
_space_group_name_Hall           'P 6c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'

_cell_length_a                   13.1191(3)
_cell_length_b                   13.1191(3)
_cell_length_c                   16.0140(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     2386.92(13)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    1807
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      70.8500
_cell_measurement_theta_min      3.8820
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    8.838
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84149
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.506
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             1090
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.2
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0413
_diffrn_reflns_av_unetI/netI     0.0452
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            5278
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.027
_diffrn_reflns_theta_min         2.759
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.0710
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega    0.00   28.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -99.0000   30.0000 28

#__ type_ start__ end____ width___ exp.time_
  2 omega  -27.00    3.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000   38.0000    0.0000 30

#__ type_ start__ end____ width___ exp.time_
  3 omega -117.00  -35.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  178.0000 -180.0000 82

#__ type_ start__ end____ width___ exp.time_
  4 omega  -41.00   27.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000   38.0000 -120.0000 68

#__ type_ start__ end____ width___ exp.time_
  5 omega   38.00  105.00   1.0000   19.0200
omega____ theta____ kappa____ phi______ frames
    -      109.8892 -111.0000  150.0000 67

#__ type_ start__ end____ width___ exp.time_
  6 omega   43.00   69.00   1.0000   19.0200
omega____ theta____ kappa____ phi______ frames
    -      109.8892  -25.0000    0.0000 26

#__ type_ start__ end____ width___ exp.time_
  7 omega   68.00  102.00   1.0000   19.0200
omega____ theta____ kappa____ phi______ frames
    -      109.8892  -50.0000 -150.0000 34

#__ type_ start__ end____ width___ exp.time_
  8 omega   42.00   93.00   1.0000   19.0200
omega____ theta____ kappa____ phi______ frames
    -      109.8892  -38.0000   90.0000 51

#__ type_ start__ end____ width___ exp.time_
  9 omega   40.00  115.00   1.0000   19.0200
omega____ theta____ kappa____ phi______ frames
    -      109.8892 -111.0000 -120.0000 75

#__ type_ start__ end____ width___ exp.time_
 10 omega   38.00   92.00   1.0000   19.0200
omega____ theta____ kappa____ phi______ frames
    -      109.8892  -25.0000   30.0000 54
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.1316295000
_diffrn_orient_matrix_UB_12      0.0413873000
_diffrn_orient_matrix_UB_13      0.0118010000
_diffrn_orient_matrix_UB_21      0.0302956000
_diffrn_orient_matrix_UB_22      0.1284624000
_diffrn_orient_matrix_UB_23      -0.0134615000
_diffrn_orient_matrix_UB_31      -0.0120164000
_diffrn_orient_matrix_UB_32      0.0132189000
_diffrn_orient_matrix_UB_33      0.0944538000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   'Enhance (Cu) X-ray Source'
_reflns_Friedel_coverage         0.922
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.987
_reflns_number_gt                1750
_reflns_number_total             1878
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    ?
_refine_diff_density_max         0.640
_refine_diff_density_min         -0.384
_refine_diff_density_rms         0.111
_refine_ls_abs_structure_details 
;
 Flack x determined using 219 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.025(10)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     209
_refine_ls_number_reflns         1878
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0496
_refine_ls_R_factor_gt           0.0454
_refine_ls_restrained_S_all      1.115
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.0706P)²]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1147
_refine_ls_wR_factor_ref         0.1185
_refine_special_details          
;
 Refined as a 2-component twin.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Others
 Fixed Sof: O6(0.08333)
3.a Aromatic/amide H refined with riding coordinates:
 C8(H8), C11(H11), C9(H9), C2(H2), C3(H3), C5(H5), C6(H6), C12(H12)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.47336(10) 0.51793(10) 0.27171(11) 0.0243(2) Uani 1 1 d . . . . .
Na1 Na 0.3333 0.6667 0.2704(4) 0.0229(7) Uani 1 3 d S T P . .
C7 C 0.5633(7) 0.6918(6) 0.1460(5) 0.0288(16) Uani 1 1 d . . . . .
O2 O 0.3812(7) 0.3739(6) 0.3752(3) 0.0464(16) Uani 1 1 d . . . . .
O3 O 0.4749(5) 0.6407(5) 0.1947(3) 0.0307(12) Uani 1 1 d . . . . .
C8 C 0.5518(9) 0.7663(9) 0.0787(5) 0.043(2) Uani 1 1 d . . . . .
H8 H 0.4855 0.7747 0.0777 0.052 Uiso 1 1 calc R . . . .
C1 C 0.3322(7) 0.4317(7) 0.3923(5) 0.0296(17) Uani 1 1 d . . . . .
O4 O 0.6501(6) 0.6813(7) 0.1509(4) 0.0513(17) Uani 1 1 d . . . . .
O1 O 0.3410(5) 0.5126(5) 0.3424(4) 0.0352(13) Uani 1 1 d . . . . .
C11 C 0.5453(9) 0.9026(8) -0.0856(5) 0.042(2) Uani 1 1 d . . . . .
H11 H 0.4683 0.8697 -0.0665 0.051 Uiso 1 1 calc R . . . .
C9 C 0.6323(8) 0.8185(8) 0.0225(5) 0.0431(18) Uani 1 1 d . . . . .
H9 H 0.6993 0.8120 0.0289 0.052 Uiso 1 1 calc R . . . .
C10 C 0.6319(9) 0.8871(8) -0.0507(5) 0.045(2) Uani 1 1 d . . . . .
N4 N 0.7275(8) 0.9474(8) -0.0969(5) 0.056(2) Uani 1 1 d . . . . .
C2 C 0.2686(8) 0.4088(8) 0.4716(5) 0.0365(18) Uani 1 1 d . . . . .
H2 H 0.2656 0.3501 0.5058 0.044 Uiso 1 1 calc R . . . .
C3 C 0.2154(7) 0.4654(7) 0.4978(5) 0.0331(18) Uani 1 1 d . . . . .
H3 H 0.2115 0.5188 0.4615 0.040 Uiso 1 1 calc R . . . .
C4 C 0.1621(8) 0.4494(8) 0.5802(5) 0.0359(18) Uani 1 1 d . . . . .
N2 N 0.1833(8) 0.3944(8) 0.6455(4) 0.053(2) Uani 1 1 d . . . . .
C5 C 0.0880(8) 0.4833(8) 0.6112(5) 0.0376(19) Uani 1 1 d . . . . .
H5 H 0.0590 0.5242 0.5814 0.045 Uiso 1 1 calc R . . . .
C6 C 0.1240(9) 0.3985(10) 0.7122(6) 0.051(2) Uani 1 1 d . . . . .
H6 H 0.1266 0.3698 0.7648 0.062 Uiso 1 1 calc R . . . .
C12 C 0.7002(9) 0.9977(9) -0.1560(6) 0.047(2) Uani 1 1 d . . . . .
H12 H 0.7532 1.0457 -0.1966 0.057 Uiso 1 1 calc R . . . .
N1 N 0.0613(6) 0.4487(7) 0.6933(4) 0.0362(16) Uani 1 1 d . . . . .
N3 N 0.5909(7) 0.9741(6) -0.1527(5) 0.0369(16) Uani 1 1 d . . . . .
N5 N 1.0000 1.0000 -0.0634(19) 0.107(8) Uani 1 3 d S T P . .
O6 O 1.0000 1.0000 0.192(5) 0.23(7) Uani 0.25 3 d S T P . .
O5 O 1.0968(10) 1.0146(11) -0.0673(14) 0.172(7) Uani 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
Co1 Na1 3.2814(8) . ?
Co1 O2 2.344(6) . ?
Co1 O3 2.020(5) . ?
Co1 C1 2.518(8) . ?
Co1 O1 2.045(6) . ?
Co1 N1 2.015(7) 5_554 ?
Co1 N3 2.030(7) 6_655 ?
Na1 Co1 3.2814(8) 3_565 ?
Na1 Co1 3.2814(8) 2_665 ?
Na1 O3 2.381(6) . ?
Na1 O3 2.381(6) 3_565 ?
Na1 O3 2.381(6) 2_665 ?
Na1 O1 2.373(7) 3_565 ?
Na1 O1 2.373(7) . ?
Na1 O1 2.373(7) 2_665 ?
C7 O3 1.275(10) . ?
C7 C8 1.512(11) . ?
C7 O4 1.217(10) . ?
O2 C1 1.245(10) . ?
C8 C9 1.292(12) . ?
C1 O1 1.286(10) . ?
C1 C2 1.466(11) . ?
C11 C10 1.371(13) . ?
C11 N3 1.352(11) . ?
C9 C10 1.480(11) . ?
C10 N4 1.323(12) . ?
N4 C12 1.303(12) . ?
C2 C3 1.316(11) . ?
C3 C4 1.458(10) . ?
C4 N2 1.376(11) . ?
C4 C5 1.350(12) . ?
N2 C6 1.338(11) . ?
C5 N1 1.378(10) . ?
C6 N1 1.321(11) . ?
C12 N3 1.308(12) . ?
N1 Co1 2.015(7) 6 ?
N3 Co1 2.030(7) 5_564 ?
N5 O5 1.187(11) 2_765 ?
N5 O5 1.187(11) 3_675 ?
N5 O5 1.187(11) . ?

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
O2 Co1 Na1 105.48(19) . . ?
O2 Co1 C1 29.4(2) . . ?
O3 Co1 Na1 46.18(18) . . ?
O3 Co1 O2 150.4(2) . . ?
O3 Co1 C1 122.5(3) . . ?
O3 Co1 O1 92.02(19) . . ?
O3 Co1 N3 110.5(3) . 6_655 ?
C1 Co1 Na1 76.5(2) . . ?
O1 Co1 Na1 46.02(18) . . ?
O1 Co1 O2 59.6(2) . . ?
O1 Co1 C1 30.5(2) . . ?
N1 Co1 Na1 127.0(2) 5_554 . ?
N1 Co1 O2 87.5(2) 5_554 . ?
N1 Co1 O3 103.3(3) 5_554 . ?
N1 Co1 C1 109.1(3) 5_554 . ?
N1 Co1 O1 122.9(3) 5_554 . ?
N1 Co1 N3 119.3(3) 5_554 6_655 ?
N3 Co1 Na1 112.7(2) 6_655 . ?
N3 Co1 O2 86.6(3) 6_655 . ?
N3 Co1 C1 93.1(3) 6_655 . ?
N3 Co1 O1 104.9(3) 6_655 . ?
Co1 Na1 Co1 119.997(3) 2_665 . ?
Co1 Na1 Co1 119.994(3) 3_565 2_665 ?
Co1 Na1 Co1 119.997(3) 3_565 . ?
O3 Na1 Co1 37.75(13) . . ?
O3 Na1 Co1 133.5(2) . 3_565 ?
O3 Na1 Co1 96.45(15) 2_665 3_565 ?
O3 Na1 Co1 96.45(15) 3_565 . ?
O3 Na1 Co1 133.5(2) 3_565 2_665 ?
O3 Na1 Co1 96.45(15) . 2_665 ?
O3 Na1 Co1 37.76(13) 3_565 3_565 ?
O3 Na1 Co1 37.76(13) 2_665 2_665 ?
O3 Na1 Co1 133.5(2) 2_665 . ?
O3 Na1 O3 96.4(2) 2_665 . ?
O3 Na1 O3 96.4(2) 2_665 3_565 ?
O3 Na1 O3 96.4(2) 3_565 . ?
O1 Na1 Co1 136.6(2) . 2_665 ?
O1 Na1 Co1 92.80(16) 2_665 . ?
O1 Na1 Co1 38.32(14) 3_565 3_565 ?
O1 Na1 Co1 136.6(2) 2_665 3_565 ?
O1 Na1 Co1 38.32(14) 2_665 2_665 ?
O1 Na1 Co1 92.80(16) 3_565 2_665 ?
O1 Na1 Co1 38.33(14) . . ?
O1 Na1 Co1 136.6(2) 3_565 . ?
O1 Na1 Co1 92.80(16) . 3_565 ?
O1 Na1 O3 75.95(15) . . ?
O1 Na1 O3 75.95(15) 2_665 2_665 ?
O1 Na1 O3 89.93(17) 3_565 2_665 ?
O1 Na1 O3 170.60(18) 2_665 3_565 ?
O1 Na1 O3 89.93(18) 2_665 . ?
O1 Na1 O3 170.60(18) . 2_665 ?
O1 Na1 O3 75.95(15) 3_565 3_565 ?
O1 Na1 O3 89.93(18) . 3_565 ?
O1 Na1 O3 170.60(18) 3_565 . ?
O1 Na1 O1 98.4(2) 3_565 2_665 ?
O1 Na1 O1 98.4(2) 3_565 . ?
O1 Na1 O1 98.4(2) 2_665 . ?
O3 C7 C8 114.7(7) . . ?
O4 C7 O3 123.9(7) . . ?
O4 C7 C8 121.4(8) . . ?
C1 O2 Co1 83.1(5) . . ?
Co1 O3 Na1 96.1(2) . . ?
C7 O3 Co1 115.9(5) . . ?
C7 O3 Na1 143.7(5) . . ?
C9 C8 C7 121.4(9) . . ?
O2 C1 Co1 67.5(4) . . ?
O2 C1 O1 120.4(7) . . ?
O2 C1 C2 118.6(7) . . ?
O1 C1 Co1 53.9(4) . . ?
O1 C1 C2 120.9(7) . . ?
C2 C1 Co1 166.4(6) . . ?
Co1 O1 Na1 95.7(2) . . ?
C1 O1 Co1 95.5(5) . . ?
C1 O1 Na1 168.5(5) . . ?
N3 C11 C10 108.3(9) . . ?
C8 C9 C10 128.6(9) . . ?
C11 C10 C9 131.9(9) . . ?
N4 C10 C11 107.0(8) . . ?
N4 C10 C9 121.1(8) . . ?
C12 N4 C10 106.9(8) . . ?
C3 C2 C1 124.6(8) . . ?
C2 C3 C4 123.9(8) . . ?
N2 C4 C3 123.7(7) . . ?
C5 C4 C3 131.2(8) . . ?
C5 C4 N2 105.1(7) . . ?
C6 N2 C4 108.2(7) . . ?
C4 C5 N1 110.4(8) . . ?
N1 C6 N2 110.9(8) . . ?
N4 C12 N3 113.4(9) . . ?
C5 N1 Co1 128.6(6) . 6 ?
C6 N1 Co1 126.1(6) . 6 ?
C6 N1 C5 105.3(7) . . ?
C11 N3 Co1 130.0(7) . 5_564 ?
C12 N3 Co1 125.3(6) . 5_564 ?
C12 N3 C11 104.4(8) . . ?
O5 N5 O5 119.7(4) 2_765 . ?
O5 N5 O5 119.7(4) . 3_675 ?
O5 N5 O5 119.7(4) 2_765 3_675 ?

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
Co1 O2 C1 O1 11.2(8) . . . . ?
Co1 O2 C1 C2 -166.5(7) . . . . ?
Co1 C1 O1 Na1 -167(3) . . . . ?
Co1 C1 C2 C3 65(3) . . . . ?
C7 C8 C9 C10 175.3(9) . . . . ?
O2 C1 O1 Co1 -12.8(9) . . . . ?
O2 C1 O1 Na1 180(2) . . . . ?
O2 C1 C2 C3 178.5(9) . . . . ?
O3 C7 C8 C9 -176.6(9) . . . . ?
C8 C7 O3 Co1 169.3(5) . . . . ?
C8 C7 O3 Na1 -41.5(12) . . . . ?
C8 C9 C10 C11 -9.4(18) . . . . ?
C8 C9 C10 N4 171.5(11) . . . . ?
C1 C2 C3 C4 -173.9(8) . . . . ?
O4 C7 O3 Co1 -9.3(10) . . . . ?
O4 C7 O3 Na1 139.8(8) . . . . ?
O4 C7 C8 C9 2.1(14) . . . . ?
O1 C1 C2 C3 0.8(13) . . . . ?
C11 C10 N4 C12 0.6(11) . . . . ?
C9 C10 N4 C12 179.9(9) . . . . ?
C10 C11 N3 Co1 -174.7(6) . . . 5_564 ?
C10 C11 N3 C12 0.4(11) . . . . ?
C10 N4 C12 N3 -0.4(13) . . . . ?
N4 C12 N3 Co1 175.4(7) . . . 5_564 ?
N4 C12 N3 C11 0.0(12) . . . . ?
C2 C1 O1 Co1 164.8(7) . . . . ?
C2 C1 O1 Na1 -3(3) . . . . ?
C2 C3 C4 N2 14.8(15) . . . . ?
C2 C3 C4 C5 -166.7(10) . . . . ?
C3 C4 N2 C6 177.9(9) . . . . ?
C3 C4 C5 N1 -179.7(9) . . . . ?
C4 N2 C6 N1 2.6(14) . . . . ?
C4 C5 N1 Co1 -179.7(7) . . . 6 ?
C4 C5 N1 C6 2.7(12) . . . . ?
N2 C4 C5 N1 -1.1(11) . . . . ?
N2 C6 N1 Co1 179.0(7) . . . 6 ?
N2 C6 N1 C5 -3.2(13) . . . . ?
C5 C4 N2 C6 -0.9(12) . . . . ?
N3 C11 C10 C9 -179.8(9) . . . . ?
N3 C11 C10 N4 -0.6(11) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_b
_database_code_depnum_ccdc_archive 'CCDC 1031894'
_audit_update_record             
;
2014-10-31 deposited with the CCDC.
2015-02-18 downloaded from the CCDC.
;
_audit_creation_date             2014-10-22
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_shelxl_version_number           2013-2
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         '0.5(C72 H54 Co6 N24 Na2 O24), N1 O3'
_chemical_formula_sum            'C36 H27 Co3 N13 Na O15'
_chemical_formula_weight         1081.48
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 -2.3653 3.6143 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.1353 0.1239 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      hexagonal
_space_group_IT_number           173
_space_group_name_H-M_alt        'P 63'
_space_group_name_Hall           'P 6c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'

_cell_length_a                   13.1177(4)
_cell_length_b                   13.1177(4)
_cell_length_c                   16.0050(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     2385.07(17)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    ?
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      ?
_cell_measurement_theta_min      ?
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    8.839
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.506
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             1092
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0261
_diffrn_reflns_av_unetI/netI     0.0355
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            4821
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         66.848
_diffrn_reflns_theta_min         3.891
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   ?
_reflns_Friedel_coverage         0.925
_reflns_Friedel_fraction_full    0.988
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                2071
_reflns_number_total             2197
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    ?
_refine_diff_density_max         0.913
_refine_diff_density_min         -0.302
_refine_diff_density_rms         0.118
_refine_ls_abs_structure_details 
;
 Flack x determined using 619 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.001(6)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     210
_refine_ls_number_reflns         2197
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0489
_refine_ls_R_factor_gt           0.0456
_refine_ls_restrained_S_all      1.123
_refine_ls_shift/su_max          0.097
_refine_ls_shift/su_mean         0.019
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.0831P)²]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1211
_refine_ls_wR_factor_ref         0.1240
_refine_special_details          
;
 Refined as a 2-component twin.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C9(H9), C3(H3), C2(H2), N2(H2A), C11(H11), C12(H12), N4(H4), C8(H8)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.04430(8) 0.52597(13) 0.09155(13) 0.0281(3) Uani 1 1 d . . . . .
Na1 Na 0.3333 0.6667 0.0931(4) 0.0240(8) Uani 1 3 d S T P . .
O3 O 0.1657(5) 0.5250(6) 0.1678(4) 0.0324(15) Uani 1 1 d . . . . .
O1 O 0.1720(6) 0.6588(7) 0.0202(5) 0.0404(16) Uani 1 1 d . . . . .
C7 C 0.1272(8) 0.4362(10) 0.2165(6) 0.036(2) Uani 1 1 d . . . . .
C1 C 0.0994(9) 0.6675(9) -0.0292(6) 0.036(2) Uani 1 1 d . . . . .
O4 O 0.0313(6) 0.3506(7) 0.2116(4) 0.0544(19) Uani 1 1 d . . . . .
O2 O -0.0074(7) 0.6187(8) -0.0128(4) 0.0494(19) Uani 1 1 d . . . . .
C9 C 0.1863(10) 0.3678(9) 0.3403(5) 0.050(2) Uani 1 1 d . . . . .
H9 H 0.1131 0.3006 0.3336 0.060 Uiso 1 1 calc R . . . .
C3 C 0.2509(8) 0.7856(8) -0.1352(5) 0.035(2) Uani 1 1 d . . . . .
H3 H 0.3085 0.7900 -0.0990 0.042 Uiso 1 1 calc R . . . .
C4 C 0.2877(8) 0.8386(9) -0.2186(6) 0.039(2) Uani 1 1 d . . . . .
C2 C 0.1410(9) 0.7321(9) -0.1087(6) 0.044(2) Uani 1 1 d . . . . .
H2 H 0.0854 0.7354 -0.1429 0.053 Uiso 1 1 calc R . . . .
C5 C 0.3957(9) 0.9139(10) -0.2496(6) 0.042(2) Uani 1 1 d . . . . .
N2 N 0.2114(8) 0.8180(10) -0.2828(4) 0.060(3) Uani 1 1 d . . . . .
H2A H 0.1360 0.7752 -0.2809 0.072 Uiso 1 1 calc R . . . .
N1 N 0.3868(7) 0.9390(7) -0.3303(5) 0.0404(19) Uani 1 1 d . . . . .
C11 C 0.3574(10) 0.4545(11) 0.4471(6) 0.048(3) Uani 1 1 d . . . . .
H11 H 0.4025 0.5308 0.4268 0.058 Uiso 1 1 calc R . . . .
N3 N 0.3830(8) 0.4088(9) 0.5162(5) 0.043(2) Uani 1 1 d . . . . .
C12 C 0.2967(10) 0.3001(10) 0.5186(7) 0.051(3) Uani 1 1 d . . . . .
H12 H 0.2914 0.2466 0.5589 0.062 Uiso 1 1 calc R . . . .
C6 C 0.2765(9) 0.8774(12) -0.3501(7) 0.059(3) Uani 1 1 d . . . . .
N4 N 0.2185(9) 0.2729(9) 0.4597(6) 0.063(3) Uani 1 1 d . . . . .
H4 H 0.1559 0.2058 0.4523 0.075 Uiso 1 1 calc R . . . .
C10 C 0.2546(9) 0.3688(11) 0.4136(6) 0.049(3) Uani 1 1 d . . . . .
C8 C 0.2153(12) 0.4491(10) 0.2838(6) 0.047(2) Uani 1 1 d . . . . .
H8 H 0.2901 0.5153 0.2844 0.056 Uiso 1 1 calc R . . . .
N5 N 0.0000 0.0000 0.425(2) 0.124(10) Uani 1 3 d S T P . .
O5 O -0.0124(15) 0.0832(12) 0.4393(17) 0.208(11) Uani 1 1 d . . . . .
H5 H 0.486(9) 0.935(8) -0.230(6) 0.04(3) 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
Co1 Na1 3.2840(9) . ?
Co1 O3 2.011(6) . ?
Co1 O1 2.056(7) . ?
Co1 O2 2.357(7) . ?
Co1 N1 2.017(8) 5_455 ?
Co1 N3 2.023(9) 6_554 ?
Na1 Co1 3.2840(9) 3_565 ?
Na1 Co1 3.2839(9) 2_665 ?
Na1 O3 2.373(7) . ?
Na1 O3 2.373(7) 3_565 ?
Na1 O3 2.373(7) 2_665 ?
Na1 O1 2.373(8) 2_665 ?
Na1 O1 2.373(8) 3_565 ?
Na1 O1 2.373(8) . ?
O3 C7 1.277(12) . ?
O1 C1 1.286(12) . ?
C7 O4 1.199(13) . ?
C7 C8 1.526(13) . ?
C1 O2 1.242(13) . ?
C1 C2 1.475(13) . ?
C9 C10 1.472(12) . ?
C9 C8 1.302(14) . ?
C3 C4 1.471(12) . ?
C3 C2 1.319(13) . ?
C4 C5 1.353(14) . ?
C4 N2 1.364(12) . ?
C5 N1 1.352(12) . ?
N2 C6 1.354(13) . ?
N1 Co1 2.017(8) 6_664 ?
N1 C6 1.296(14) . ?
C11 N3 1.378(13) . ?
C11 C10 1.361(16) . ?
N3 Co1 2.023(9) 5 ?
N3 C12 1.304(14) . ?
C12 N4 1.304(14) . ?
N4 C10 1.326(14) . ?
N5 O5 1.204(16) 3 ?
N5 O5 1.204(16) 2 ?
N5 O5 1.204(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
O3 Co1 Na1 45.9(2) . . ?
O3 Co1 O1 91.7(2) . . ?
O3 Co1 O2 150.0(3) . . ?
O3 Co1 N1 103.7(3) . 5_455 ?
O3 Co1 N3 110.5(4) . 6_554 ?
O1 Co1 Na1 46.0(2) . . ?
O1 Co1 O2 59.4(3) . . ?
O2 Co1 Na1 105.3(2) . . ?
N1 Co1 Na1 126.6(3) 5_455 . ?
N1 Co1 O1 122.5(4) 5_455 . ?
N1 Co1 O2 87.3(3) 5_455 . ?
N1 Co1 N3 119.7(4) 5_455 6_554 ?
N3 Co1 Na1 112.8(3) 6_554 . ?
N3 Co1 O1 104.8(4) 6_554 . ?
N3 Co1 O2 86.7(3) 6_554 . ?
Co1 Na1 Co1 119.993(4) . 3_565 ?
Co1 Na1 Co1 119.995(4) 3_565 2_665 ?
Co1 Na1 Co1 119.994(4) . 2_665 ?
O3 Na1 Co1 96.61(17) . 2_665 ?
O3 Na1 Co1 96.61(17) 2_665 3_565 ?
O3 Na1 Co1 37.47(15) . . ?
O3 Na1 Co1 133.6(2) 2_665 . ?
O3 Na1 Co1 133.6(2) 3_565 2_665 ?
O3 Na1 Co1 37.47(15) 3_565 3_565 ?
O3 Na1 Co1 96.61(17) 3_565 . ?
O3 Na1 Co1 133.6(2) . 3_565 ?
O3 Na1 Co1 37.47(15) 2_665 2_665 ?
O3 Na1 O3 96.9(3) 3_565 2_665 ?
O3 Na1 O3 96.9(3) 3_565 . ?
O3 Na1 O3 96.9(3) . 2_665 ?
O3 Na1 O1 170.6(2) 3_565 2_665 ?
O3 Na1 O1 75.91(17) 3_565 3_565 ?
O3 Na1 O1 170.6(2) . 3_565 ?
O3 Na1 O1 75.91(17) 2_665 2_665 ?
O3 Na1 O1 90.0(2) . 2_665 ?
O1 Na1 Co1 136.4(3) 2_665 3_565 ?
O1 Na1 Co1 136.4(3) . 2_665 ?
O1 Na1 Co1 92.7(2) . 3_565 ?
O1 Na1 Co1 136.3(3) 3_565 . ?
O1 Na1 Co1 38.55(17) 3_565 3_565 ?
O1 Na1 Co1 38.55(17) 2_665 2_665 ?
O1 Na1 Co1 92.7(2) 2_665 . ?
O1 Na1 Co1 92.7(2) 3_565 2_665 ?
O1 Na1 Co1 38.55(17) . . ?
O1 Na1 O3 90.0(2) 3_565 2_665 ?
O1 Na1 O3 90.0(2) . 3_565 ?
O1 Na1 O3 170.6(2) . 2_665 ?
O1 Na1 O3 75.91(17) . . ?
O1 Na1 O1 97.9(3) . 2_665 ?
O1 Na1 O1 97.9(3) 3_565 2_665 ?
O1 Na1 O1 97.9(3) . 3_565 ?
Co1 O3 Na1 96.7(3) . . ?
C7 O3 Co1 115.0(6) . . ?
C7 O3 Na1 144.1(6) . . ?
Co1 O1 Na1 95.4(3) . . ?
C1 O1 Co1 95.2(6) . . ?
C1 O1 Na1 169.2(7) . . ?
O3 C7 C8 113.4(9) . . ?
O4 C7 O3 124.4(9) . . ?
O4 C7 C8 122.1(10) . . ?
O1 C1 C2 120.2(9) . . ?
O2 C1 O1 121.3(9) . . ?
O2 C1 C2 118.4(9) . . ?
C1 O2 Co1 82.8(6) . . ?
C8 C9 C10 128.2(11) . . ?
C2 C3 C4 123.8(9) . . ?
C5 C4 C3 130.9(9) . . ?
C5 C4 N2 105.4(8) . . ?
N2 C4 C3 123.7(8) . . ?
C3 C2 C1 125.1(9) . . ?
N1 C5 C4 110.0(9) . . ?
C6 N2 C4 107.3(9) . . ?
C5 N1 Co1 127.6(8) . 6_664 ?
C6 N1 Co1 125.5(7) . 6_664 ?
C6 N1 C5 106.8(9) . . ?
C10 C11 N3 108.2(11) . . ?
C11 N3 Co1 130.0(8) . 5 ?
C12 N3 Co1 126.3(7) . 5 ?
C12 N3 C11 103.4(10) . . ?
N3 C12 N4 114.4(10) . . ?
N1 C6 N2 110.5(9) . . ?
C12 N4 C10 106.4(9) . . ?
C11 C10 C9 131.9(11) . . ?
N4 C10 C9 120.5(9) . . ?
N4 C10 C11 107.5(9) . . ?
C9 C8 C7 120.3(11) . . ?
O5 N5 O5 116.3(16) . 2 ?
O5 N5 O5 116.3(16) 2 3 ?
O5 N5 O5 116.3(16) . 3 ?

_olex2_submission_special_instructions 'No special instructions were received'
