# Electronic Supplementary Material (ESI) for Dalton Transactions.
# 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_complex1
_database_code_depnum_ccdc_archive 'CCDC 1014970'
_audit_update_record             
;
2014-12-24 deposited with the CCDC.
2015-01-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H11 Fe3 N9 O18, 0.075(O4), 6.201(O)'
_chemical_formula_sum            'C12 H11 Fe3 N9 O24.50'
_chemical_formula_weight         840.89

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'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           86
_space_group_name_H-M_alt        'P 42/n'
_space_group_name_Hall           '-P 4bc'

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

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

_cell_length_a                   14.300(4)
_cell_length_b                   14.300(4)
_cell_length_c                   14.983(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3063.9(19)
_cell_formula_units_Z            4
_cell_measurement_temperature    307(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            BROWN
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.823
_exptl_crystal_F_000             1680.1
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.29
_exptl_absorpt_coefficient_mu    1.513
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6225
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      307(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            10492
_diffrn_reflns_av_unetI/netI     0.0191
_diffrn_reflns_av_R_equivalents  0.0249
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_theta_min         2.430
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             2687
_reflns_number_gt                2136
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker Apex II'
_computing_cell_refinement       'Bruker Apex II'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS-2014/6 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics    'Mercury 3.3'
_computing_publication_material  'Shelxl 2014'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0865P)²+5.5257P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2687
_refine_ls_number_parameters     223
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0646
_refine_ls_R_factor_gt           0.0521
_refine_ls_wR_factor_ref         0.1593
_refine_ls_wR_factor_gt          0.1511
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_restrained_S_all      1.049
_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_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
Fe2 Fe 0.57600(4) 0.34619(4) 0.25424(4) 0.0367(2) Uani 1 1 d . . . . .
Fe1 Fe 0.2500 0.2500 0.05939(8) 0.0567(3) Uani 1 2 d S T P . .
O1 O 0.2756(3) 0.4784(3) -0.0111(3) 0.0831(14) Uani 1 1 d . . . . .
O2 O 0.5243(3) 0.5624(2) 0.1548(3) 0.0691(11) Uani 1 1 d . . . . .
O3 O 0.3500(2) 0.1990(2) 0.1552(3) 0.0567(9) Uani 1 1 d . . . . .
O4 O 0.4790(2) 0.2369(2) 0.2305(2) 0.0479(8) Uani 1 1 d . . . . .
O5 O 0.6792(2) 0.2816(2) 0.33890(18) 0.0487(8) Uani 1 1 d . . . . .
O7 O 0.6037(2) 0.3107(2) 0.02652(19) 0.0520(8) Uani 1 1 d . . . . .
O11 O 0.6544(3) 0.4702(3) 0.2531(3) 0.0689(11) Uani 1 1 d . . . . .
H11A H 0.6746 0.4840 0.3067 0.103 Uiso 1 1 d R U . . .
H11B H 0.6204 0.5169 0.2343 0.103 Uiso 1 1 d R U . . .
N2 N 0.3413(2) 0.3678(2) 0.0797(2) 0.0429(9) Uani 1 1 d . . . . .
O15A O 0.1567(6) 0.3372(6) -0.0260(6) 0.067(2) Uiso 0.4835 1 d . . P . .
O15B O 0.1931(5) 0.3061(5) -0.0557(5) 0.0651(19) Uiso 0.5165 1 d . . P . .
O33 O 0.4949(3) 0.3865(3) 0.3679(2) 0.0717(11) Uani 1 1 d . . . . .
H33A H 0.5190 0.3637 0.4158 0.108 Uiso 1 1 d R U . . .
H33B H 0.4388 0.3655 0.3625 0.108 Uiso 1 1 d R U . . .
N1 N 0.4009(3) 0.5186(3) 0.0715(3) 0.0487(10) Uani 1 1 d . . . . .
H1 H 0.3992 0.5738 0.0486 0.058 Uiso 1 1 calc R U . . .
N3 N 0.4724(2) 0.4123(2) 0.1672(2) 0.0353(8) Uani 1 1 d . . . . .
N4 N 0.7500 0.2500 0.0277(3) 0.0607(17) Uani 1 2 d S T P . .
H4 H 0.7500 0.2500 -0.0297 0.073 Uiso 1 2 calc R U P . .
N5 N 0.6743(2) 0.2847(2) 0.1611(2) 0.0315(7) Uani 1 1 d . . . . .
C1 C 0.4082(3) 0.3529(3) 0.1381(3) 0.0356(9) Uani 1 1 d . . . . .
C2 C 0.3355(3) 0.4553(3) 0.0433(3) 0.0512(11) Uani 1 1 d . . . . .
C3 C 0.4684(3) 0.5005(3) 0.1329(3) 0.0445(10) Uani 1 1 d . . . . .
C4 C 0.4130(3) 0.2543(3) 0.1786(3) 0.0402(10) Uani 1 1 d . . . . .
C9 C 0.7500 0.2500 0.3008(3) 0.0376(13) Uani 1 2 d S T P . .
C10 C 0.7500 0.2500 0.1987(3) 0.0280(11) Uani 1 2 d S T P . .
C11 C 0.6718(3) 0.2836(3) 0.0688(3) 0.0393(10) Uani 1 1 d . . . . .
O20 O 0.0195(3) 0.2483(4) 0.8965(3) 0.0939(14) Uani 1 1 d . . . . .
O21A O 0.8499(12) 0.4587(14) 0.1693(13) 0.201(6) Uiso 0.5928 1 d . . P . .
O21B O 0.817(5) 0.534(5) 0.192(5) 0.45(3) Uiso 0.4072 1 d . . P . .
O22A O 0.9356(15) 0.4164(16) 0.0227(16) 0.237(9) Uiso 0.6152 1 d . . P . .
O22B O 0.911(3) 0.461(3) 0.063(3) 0.246(15) Uiso 0.3848 1 d . . P . .
O23A O 0.2500 0.2500 0.7500 0.32(7) Uiso 0.4013 4 d S . P . .
O23B O 0.309(9) 0.291(9) 0.757(6) 0.24(4) Uiso 0.1497 1 d . . P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe2 O11 2.098(4) . ?
Fe2 O4 2.121(3) . ?
Fe2 O33 2.140(4) . ?
Fe2 O5 2.154(3) . ?
Fe2 N5 2.167(3) . ?
Fe2 N3 2.189(3) . ?
Fe1 O15B 2.069(7) 3 ?
Fe1 O15B 2.069(7) . ?
Fe1 N2 2.153(3) . ?
Fe1 N2 2.153(3) 3 ?
Fe1 O3 2.154(4) 3 ?
Fe1 O3 2.154(4) . ?
Fe1 O15A 2.230(8) 3 ?
Fe1 O15A 2.230(8) . ?
O1 C2 1.227(6) . ?
O2 C3 1.236(5) . ?
O3 C4 1.249(5) . ?
O4 C4 1.247(5) . ?
O5 C9 1.247(4) . ?
O7 C11 1.225(5) . ?
O11 H11A 0.8749 . ?
O11 H11B 0.8742 . ?
N2 C1 1.314(5) . ?
N2 C2 1.367(6) . ?
O15A O15B 0.817(9) . ?
O33 H33A 0.8599 . ?
O33 H33B 0.8592 . ?
N1 C3 1.358(6) . ?
N1 C2 1.368(6) . ?
N1 H1 0.8600 . ?
N3 C1 1.324(5) . ?
N3 C3 1.363(5) . ?
N4 C11 1.363(5) 3_655 ?
N4 C11 1.363(5) . ?
N4 H4 0.8600 . ?
N5 C10 1.317(4) . ?
N5 C11 1.383(5) . ?
C1 C4 1.537(6) . ?
C9 O5 1.247(4) 3_655 ?
C9 C10 1.531(7) . ?
C10 N5 1.317(4) 3_655 ?
O21A O21B 1.22(6) . ?
O22A O22B 0.95(4) . ?
O23A O23B 1.04(11) . ?
O23A O23B 1.04(11) 3 ?
O23A O23B 1.04(11) 8_657 ?
O23A O23B 1.04(11) 6_567 ?
O23B O23B 1.47(15) 8_657 ?
O23B O23B 1.47(15) 6_567 ?

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
O11 Fe2 O4 166.30(13) . . ?
O11 Fe2 O33 93.93(17) . . ?
O4 Fe2 O33 88.70(15) . . ?
O11 Fe2 O5 90.04(14) . . ?
O4 Fe2 O5 103.36(13) . . ?
O33 Fe2 O5 91.04(13) . . ?
O11 Fe2 N5 89.48(15) . . ?
O4 Fe2 N5 91.00(12) . . ?
O33 Fe2 N5 166.76(14) . . ?
O5 Fe2 N5 76.15(12) . . ?
O11 Fe2 N3 89.53(13) . . ?
O4 Fe2 N3 77.03(12) . . ?
O33 Fe2 N3 89.50(13) . . ?
O5 Fe2 N3 179.33(12) . . ?
N5 Fe2 N3 103.33(12) . . ?
O15B Fe1 O15B 67.1(5) 3 . ?
O15B Fe1 N2 100.5(2) 3 . ?
O15B Fe1 N2 93.0(2) . . ?
O15B Fe1 N2 93.0(2) 3 3 ?
O15B Fe1 N2 100.5(2) . 3 ?
N2 Fe1 N2 163.8(2) . 3 ?
O15B Fe1 O3 161.5(2) 3 3 ?
O15B Fe1 O3 99.4(2) . 3 ?
N2 Fe1 O3 92.49(13) . 3 ?
N2 Fe1 O3 76.60(12) 3 3 ?
O15B Fe1 O3 99.4(2) 3 . ?
O15B Fe1 O3 161.5(2) . . ?
N2 Fe1 O3 76.60(12) . . ?
N2 Fe1 O3 92.49(13) 3 . ?
O3 Fe1 O3 96.4(2) 3 . ?
O15B Fe1 O15A 21.5(2) 3 3 ?
O15B Fe1 O15A 88.5(4) . 3 ?
N2 Fe1 O15A 99.0(2) . 3 ?
N2 Fe1 O15A 90.4(2) 3 3 ?
O3 Fe1 O15A 165.7(2) 3 3 ?
O3 Fe1 O15A 78.2(2) . 3 ?
O15B Fe1 O15A 88.5(4) 3 . ?
O15B Fe1 O15A 21.5(2) . . ?
N2 Fe1 O15A 90.4(2) . . ?
N2 Fe1 O15A 99.0(2) 3 . ?
O3 Fe1 O15A 78.2(2) 3 . ?
O3 Fe1 O15A 165.7(2) . . ?
O15A Fe1 O15A 110.0(5) 3 . ?
C4 O3 Fe1 116.9(3) . . ?
C4 O4 Fe2 116.9(3) . . ?
C9 O5 Fe2 116.2(3) . . ?
Fe2 O11 H11A 111.1 . . ?
Fe2 O11 H11B 110.6 . . ?
H11A O11 H11B 107.9 . . ?
C1 N2 C2 117.3(4) . . ?
C1 N2 Fe1 114.1(3) . . ?
C2 N2 Fe1 128.5(3) . . ?
O15B O15A Fe1 68.1(8) . . ?
O15A O15B Fe1 90.4(9) . . ?
Fe2 O33 H33A 110.1 . . ?
Fe2 O33 H33B 109.6 . . ?
H33A O33 H33B 108.8 . . ?
C3 N1 C2 124.7(4) . . ?
C3 N1 H1 117.7 . . ?
C2 N1 H1 117.7 . . ?
C1 N3 C3 116.1(3) . . ?
C1 N3 Fe2 112.8(3) . . ?
C3 N3 Fe2 130.8(3) . . ?
C11 N4 C11 126.3(5) 3_655 . ?
C11 N4 H4 116.9 3_655 . ?
C11 N4 H4 116.9 . . ?
C10 N5 C11 116.3(3) . . ?
C10 N5 Fe2 114.3(3) . . ?
C11 N5 Fe2 129.2(3) . . ?
N2 C1 N3 128.3(4) . . ?
N2 C1 C4 116.3(3) . . ?
N3 C1 C4 115.4(3) . . ?
O1 C2 N2 123.6(4) . . ?
O1 C2 N1 120.3(4) . . ?
N2 C2 N1 116.1(4) . . ?
O2 C3 N1 120.2(4) . . ?
O2 C3 N3 122.3(4) . . ?
N1 C3 N3 117.5(4) . . ?
O4 C4 O3 126.4(4) . . ?
O4 C4 C1 117.6(3) . . ?
O3 C4 C1 116.0(4) . . ?
O5 C9 O5 125.5(5) 3_655 . ?
O5 C9 C10 117.2(2) 3_655 . ?
O5 C9 C10 117.2(2) . . ?
N5 C10 N5 129.5(5) . 3_655 ?
N5 C10 C9 115.3(2) . . ?
N5 C10 C9 115.3(2) 3_655 . ?
O7 C11 N4 121.9(4) . . ?
O7 C11 N5 122.3(4) . . ?
N4 C11 N5 115.8(4) . . ?
O23B O23A O23B 168(9) . 3 ?
O23B O23A O23B 90.6(10) . 8_657 ?
O23B O23A O23B 90.6(10) 3 8_657 ?
O23B O23A O23B 90.6(10) . 6_567 ?
O23B O23A O23B 90.6(10) 3 6_567 ?
O23B O23A O23B 168(9) 8_657 6_567 ?
O23A O23B O23B 44.7(5) . 8_657 ?
O23A O23B O23B 44.7(5) . 6_567 ?
O23B O23B O23B 89(2) 8_657 6_567 ?

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
C2 N2 C1 N3 -0.2(7) . . . . ?
Fe1 N2 C1 N3 -177.2(3) . . . . ?
C2 N2 C1 C4 179.6(4) . . . . ?
Fe1 N2 C1 C4 2.6(5) . . . . ?
C3 N3 C1 N2 0.7(6) . . . . ?
Fe2 N3 C1 N2 -174.0(3) . . . . ?
C3 N3 C1 C4 -179.1(4) . . . . ?
Fe2 N3 C1 C4 6.2(4) . . . . ?
C1 N2 C2 O1 -179.1(5) . . . . ?
Fe1 N2 C2 O1 -2.6(8) . . . . ?
C1 N2 C2 N1 0.4(6) . . . . ?
Fe1 N2 C2 N1 176.9(3) . . . . ?
C3 N1 C2 O1 178.3(5) . . . . ?
C3 N1 C2 N2 -1.2(7) . . . . ?
C2 N1 C3 O2 -179.5(5) . . . . ?
C2 N1 C3 N3 1.7(7) . . . . ?
C1 N3 C3 O2 179.9(4) . . . . ?
Fe2 N3 C3 O2 -6.6(7) . . . . ?
C1 N3 C3 N1 -1.4(6) . . . . ?
Fe2 N3 C3 N1 172.1(3) . . . . ?
Fe2 O4 C4 O3 178.9(4) . . . . ?
Fe2 O4 C4 C1 -0.7(5) . . . . ?
Fe1 O3 C4 O4 -177.2(3) . . . . ?
Fe1 O3 C4 C1 2.3(5) . . . . ?
N2 C1 C4 O4 176.2(4) . . . . ?
N3 C1 C4 O4 -4.0(6) . . . . ?
N2 C1 C4 O3 -3.4(6) . . . . ?
N3 C1 C4 O3 176.4(4) . . . . ?
Fe2 O5 C9 O5 172.8(3) . . . 3_655 ?
Fe2 O5 C9 C10 -7.2(3) . . . . ?
C11 N5 C10 N5 1.4(3) . . . 3_655 ?
Fe2 N5 C10 N5 -173.8(2) . . . 3_655 ?
C11 N5 C10 C9 -178.6(3) . . . . ?
Fe2 N5 C10 C9 6.2(2) . . . . ?
O5 C9 C10 N5 -179.4(2) 3_655 . . . ?
O5 C9 C10 N5 0.6(2) . . . . ?
O5 C9 C10 N5 0.6(2) 3_655 . . 3_655 ?
O5 C9 C10 N5 -179.4(2) . . . 3_655 ?
C11 N4 C11 O7 -178.5(5) 3_655 . . . ?
C11 N4 C11 N5 1.3(2) 3_655 . . . ?
C10 N5 C11 O7 177.2(4) . . . . ?
Fe2 N5 C11 O7 -8.4(6) . . . . ?
C10 N5 C11 N4 -2.6(5) . . . . ?
Fe2 N5 C11 N4 171.7(2) . . . . ?
O23B O23A O23B O23B -96(5) 3 . . 8_657 ?
O23B O23A O23B O23B 168(9) 6_567 . . 8_657 ?
O23B O23A O23B O23B 96(5) 3 . . 6_567 ?
O23B O23A O23B O23B -168(9) 8_657 . . 6_567 ?

_refine_diff_density_max         1.293
_refine_diff_density_min         -0.517
_refine_diff_density_rms         0.093
#
_vrf_PLAT430_complex1            
;
PROBLEM: Short Inter D...A Contact  O21A   ..  O22B    ..       1.82 Ang.   
RESPONSE: Thermal parameters associated with the lattice occluded solvent
molecules Ox(x= 21A,21B,22A,22B,23A,23B) are relatively higher and H-atoms 
associated with these solvent molecules could not be located in the difference 
fourier map. Therefore it appears as short contact.
;
# 
#
_vrf_PLAT201_complex1            
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) .......          1 Report 
RESPONSE: We do not refine the disodered oxygen atom O15 
anisotropically.
;
#
_vrf_PLAT306_complex1            
;
PROBLEM:  Isolated Oxygen Atom (H-atoms Missing ?) .......        O20 Check 
RESPONSE: We are not able to locate H-atoms associated with the 
lattice occluded solvent O20.
;
# 
_shelxl_version_number           2014/6

####################################################################### 
# 
# 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_Complex2
_database_code_depnum_ccdc_archive 'CCDC 1014971'
_audit_update_record             
;
2014-12-24 deposited with the CCDC.
2015-01-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H15 Co3 N9 O18, 6.5(O)'
_chemical_formula_sum            'C12 H15 Co3 N9 O24.50'
_chemical_formula_weight         854.10

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

_space_group_crystal_system      tetragonal
_space_group_IT_number           86
_space_group_name_H-M_alt        'P 42/n'
_space_group_name_Hall           '-P 4bc'

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

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

_cell_length_a                   14.2040(9)
_cell_length_b                   14.2040(9)
_cell_length_c                   15.0369(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3033.7(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    307(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            PINK
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.870
_exptl_crystal_F_000             1708.0
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.29
_exptl_absorpt_coefficient_mu    1.734
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  0.5831
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      307(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            27274
_diffrn_reflns_av_unetI/netI     0.0459
_diffrn_reflns_av_R_equivalents  0.0522
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.439
_diffrn_reflns_theta_max         29.684
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             4264
_reflns_number_gt                2477
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker Apex II'
_computing_cell_refinement       'Bruker Apex II'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS-2014/6 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics    'Mercury 3.3'
_computing_publication_material  'Shelxl 2014'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1108P)²+1.9700P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4264
_refine_ls_number_parameters     226
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1070
_refine_ls_R_factor_gt           0.0572
_refine_ls_wR_factor_ref         0.1943
_refine_ls_wR_factor_gt          0.1681
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_restrained_S_all      0.997
_refine_ls_shift/su_max          0.028
_refine_ls_shift/su_mean         0.001

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.7500 -0.2500 0.43077(5) 0.0444(2) Uani 1 2 d S T P . .
Co2 Co 0.65418(4) 0.07779(3) 0.24793(3) 0.03273(19) Uani 1 1 d . . . . .
O1 O 0.6882(2) 0.10316(19) 0.47346(16) 0.0471(7) Uani 1 1 d . . . . .
O2 O 0.7175(2) 0.17889(18) 0.16267(15) 0.0435(7) Uani 1 1 d . . . . .
O3 O 0.5325(3) 0.1594(3) 0.2470(2) 0.0612(9) Uani 1 1 d . . . . .
H3A H 0.5229 0.1902 0.1942 0.092 Uiso 1 1 d R U . . .
H3B H 0.4792 0.1248 0.2566 0.092 Uiso 1 1 d R U . . .
O4 O 0.6175(2) -0.0012(2) 0.13628(19) 0.0586(8) Uani 1 1 d . . . . .
H4A H 0.6240 -0.0656 0.1450 0.088 Uiso 1 1 d R U . . .
H4B H 0.5556 0.0070 0.1183 0.088 Uiso 1 1 d R U . . .
O5 O 0.76640(19) -0.01741(19) 0.26857(19) 0.0416(7) Uani 1 1 d . . . . .
O6 O 0.80353(18) -0.15116(19) 0.3380(2) 0.0488(7) Uani 1 1 d . . . . .
O7 O 0.8175(3) -0.1743(4) 0.5296(3) 0.122(2) Uani 1 1 d . . . . .
H7A H 0.8943 -0.1716 0.5315 0.184 Uiso 1 1 d R U . . .
H7B H 0.8056 -0.0987 0.5357 0.184 Uiso 1 1 d R U . . .
O8 O 0.4404(2) 0.0302(2) 0.3475(2) 0.0648(9) Uani 1 1 d . . . . .
O9 O 0.5234(3) -0.2258(2) 0.5055(3) 0.0764(12) Uani 1 1 d . . . . .
N1 N 0.6345(2) -0.1590(2) 0.4156(2) 0.0377(7) Uani 1 1 d . . . . .
N2 N 0.59065(19) -0.02413(19) 0.33205(19) 0.0316(6) Uani 1 1 d . . . . .
N3 N 0.4832(2) -0.0967(2) 0.4267(2) 0.0437(8) Uani 1 1 d . . . . .
H3 H 0.4280 -0.0984 0.4501 0.052 Uiso 1 1 calc R U . . .
N4 N 0.7152(2) 0.17396(19) 0.33960(17) 0.0290(6) Uani 1 1 d . . . . .
N5 N 0.7500 0.2500 0.4729(3) 0.0573(15) Uani 1 2 d S T P . .
H5 H 0.7500 0.2500 0.5301 0.069 Uiso 1 2 calc R U P . .
C1 C 0.7500 0.2500 0.2001(3) 0.0322(10) Uani 1 2 d S T P . .
C2 C 0.7500 0.2500 0.3023(3) 0.0257(9) Uani 1 2 d S T P . .
C3 C 0.5014(3) -0.0269(3) 0.3670(3) 0.0396(8) Uani 1 1 d . . . . .
C4 C 0.5459(3) -0.1642(3) 0.4522(3) 0.0457(10) Uani 1 1 d . . . . .
C5 C 0.7482(2) -0.0854(3) 0.3175(3) 0.0359(8) Uani 1 1 d . . . . .
C6 C 0.6499(2) -0.0904(2) 0.3584(2) 0.0308(7) Uani 1 1 d . . . . .
C7 C 0.7158(3) 0.1714(3) 0.4310(2) 0.0356(8) Uani 1 1 d . . . . .
O11 O 0.7448(3) 0.9787(3) 0.6035(3) 0.0997(14) Uani 1 1 d . . . . .
O12A O 0.6393(14) 0.0458(14) 0.8318(16) 0.210(7) Uiso 0.5591 1 d . . P . .
O12B O 0.692(12) -0.014(12) 0.777(8) 0.85(11) Uiso 0.4409 1 d . . P . .
O13A O 0.5690(14) 0.0771(14) 0.9732(16) 0.233(7) Uiso 0.5802 1 d . . P . .
O13B O 0.598(3) 0.042(3) 0.899(4) 0.294(15) Uiso 0.4198 1 d . . P . .
O14A O 0.2500 0.2500 0.2500 0.41(5) Uiso 0.6022 4 d S . P . .
O14B O 0.313(7) 0.319(7) 0.213(7) 0.20(3) Uiso 0.0994 1 d . . P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 O7 2.069(4) . ?
Co1 O7 2.069(4) 3_645 ?
Co1 N1 2.101(3) . ?
Co1 N1 2.101(3) 3_645 ?
Co1 O6 2.121(3) 3_645 ?
Co1 O6 2.121(3) . ?
Co2 O3 2.081(3) . ?
Co2 O4 2.086(3) . ?
Co2 O5 2.113(3) . ?
Co2 N2 2.124(3) . ?
Co2 O2 2.125(2) . ?
Co2 N4 2.125(3) . ?
O1 C7 1.225(4) . ?
O2 C1 1.245(3) . ?
O3 H3A 0.9168 . ?
O3 H3B 0.9144 . ?
O4 H4A 0.9273 . ?
O4 H4B 0.9284 . ?
O5 C5 1.241(5) . ?
O6 C5 1.259(4) . ?
O7 H7A 1.0932 . ?
O7 H7B 1.0913 . ?
O8 C3 1.222(4) . ?
O9 C4 1.229(5) . ?
N1 C6 1.319(4) . ?
N1 C4 1.374(5) . ?
N2 C6 1.323(4) . ?
N2 C3 1.373(5) . ?
N3 C3 1.363(5) . ?
N3 C4 1.364(5) . ?
N3 H3 0.8600 . ?
N4 C2 1.313(3) . ?
N4 C7 1.375(4) . ?
N5 C7 1.370(4) . ?
N5 C7 1.370(4) 3_655 ?
N5 H5 0.8600 . ?
C1 O2 1.245(3) 3_655 ?
C1 C2 1.538(6) . ?
C2 N4 1.313(3) 3_655 ?
C5 C6 1.527(5) . ?
O12A O13B 1.17(5) . ?
O12A O12B 1.40(17) . ?
O13A O13B 1.29(5) . ?
O14A O14B 1.43(11) . ?
O14A O14B 1.43(11) 3 ?
O14A O14B 1.43(11) 8_656 ?
O14A O14B 1.43(11) 6_566 ?

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
O7 Co1 O7 88.2(4) . 3_645 ?
O7 Co1 N1 96.89(14) . . ?
O7 Co1 N1 92.04(14) 3_645 . ?
O7 Co1 N1 92.04(14) . 3_645 ?
O7 Co1 N1 96.89(14) 3_645 3_645 ?
N1 Co1 N1 167.57(17) . 3_645 ?
O7 Co1 O6 169.29(14) . 3_645 ?
O7 Co1 O6 87.9(2) 3_645 3_645 ?
N1 Co1 O6 93.20(11) . 3_645 ?
N1 Co1 O6 78.56(11) 3_645 3_645 ?
O7 Co1 O6 87.9(2) . . ?
O7 Co1 O6 169.29(14) 3_645 . ?
N1 Co1 O6 78.56(11) . . ?
N1 Co1 O6 93.20(11) 3_645 . ?
O6 Co1 O6 97.69(17) 3_645 . ?
O3 Co2 O4 94.99(14) . . ?
O3 Co2 O5 169.70(12) . . ?
O4 Co2 O5 87.82(13) . . ?
O3 Co2 N2 91.78(12) . . ?
O4 Co2 N2 90.37(11) . . ?
O5 Co2 N2 78.28(10) . . ?
O3 Co2 O2 88.32(13) . . ?
O4 Co2 O2 89.06(11) . . ?
O5 Co2 O2 101.66(11) . . ?
N2 Co2 O2 179.43(10) . . ?
O3 Co2 N4 89.15(13) . . ?
O4 Co2 N4 165.88(12) . . ?
O5 Co2 N4 90.49(11) . . ?
N2 Co2 N4 103.01(11) . . ?
O2 Co2 N4 77.55(10) . . ?
C1 O2 Co2 115.6(2) . . ?
Co2 O3 H3A 113.3 . . ?
Co2 O3 H3B 112.8 . . ?
H3A O3 H3B 105.6 . . ?
Co2 O4 H4A 113.1 . . ?
Co2 O4 H4B 113.8 . . ?
H4A O4 H4B 104.9 . . ?
C5 O5 Co2 115.3(2) . . ?
C5 O6 Co1 115.3(2) . . ?
Co1 O7 H7A 120.0 . . ?
Co1 O7 H7B 120.0 . . ?
H7A O7 H7B 96.7 . . ?
C6 N1 C4 116.9(3) . . ?
C6 N1 Co1 113.3(2) . . ?
C4 N1 Co1 129.7(3) . . ?
C6 N2 C3 116.9(3) . . ?
C6 N2 Co2 113.2(2) . . ?
C3 N2 Co2 129.8(2) . . ?
C3 N3 C4 124.9(3) . . ?
C3 N3 H3 117.5 . . ?
C4 N3 H3 117.5 . . ?
C2 N4 C7 116.5(3) . . ?
C2 N4 Co2 113.9(2) . . ?
C7 N4 Co2 129.3(2) . . ?
C7 N5 C7 125.3(4) . 3_655 ?
C7 N5 H5 117.3 . . ?
C7 N5 H5 117.3 3_655 . ?
O2 C1 O2 126.3(4) 3_655 . ?
O2 C1 C2 116.9(2) 3_655 . ?
O2 C1 C2 116.9(2) . . ?
N4 C2 N4 129.5(4) . 3_655 ?
N4 C2 C1 115.25(19) . . ?
N4 C2 C1 115.25(19) 3_655 . ?
O8 C3 N3 120.4(3) . . ?
O8 C3 N2 122.9(3) . . ?
N3 C3 N2 116.6(3) . . ?
O9 C4 N3 120.9(4) . . ?
O9 C4 N1 122.5(4) . . ?
N3 C4 N1 116.6(3) . . ?
O5 C5 O6 126.3(3) . . ?
O5 C5 C6 117.8(3) . . ?
O6 C5 C6 116.0(3) . . ?
N1 C6 N2 128.0(3) . . ?
N1 C6 C5 116.7(3) . . ?
N2 C6 C5 115.3(3) . . ?
O1 C7 N5 121.3(3) . . ?
O1 C7 N4 122.6(3) . . ?
N5 C7 N4 116.1(3) . . ?
O13B O12A O12B 139(7) . . ?
O12A O13B O13A 153(4) . . ?
O14B O14A O14B 135(8) . 3 ?
O14B O14A O14B 99(3) . 8_656 ?
O14B O14A O14B 99(3) 3 8_656 ?
O14B O14A O14B 99(3) . 6_566 ?
O14B O14A O14B 99(3) 3 6_566 ?
O14B O14A O14B 135(8) 8_656 6_566 ?

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
Co2 O2 C1 O2 -173.4(2) . . . 3_655 ?
Co2 O2 C1 C2 6.6(2) . . . . ?
C7 N4 C2 N4 -1.1(2) . . . 3_655 ?
Co2 N4 C2 N4 173.5(2) . . . 3_655 ?
C7 N4 C2 C1 178.9(2) . . . . ?
Co2 N4 C2 C1 -6.5(2) . . . . ?
O2 C1 C2 N4 180.00(19) 3_655 . . . ?
O2 C1 C2 N4 0.00(19) . . . . ?
O2 C1 C2 N4 0.00(19) 3_655 . . 3_655 ?
O2 C1 C2 N4 180.00(19) . . . 3_655 ?
C4 N3 C3 O8 179.4(4) . . . . ?
C4 N3 C3 N2 -1.6(6) . . . . ?
C6 N2 C3 O8 -179.8(4) . . . . ?
Co2 N2 C3 O8 5.6(6) . . . . ?
C6 N2 C3 N3 1.2(5) . . . . ?
Co2 N2 C3 N3 -173.4(3) . . . . ?
C3 N3 C4 O9 -178.7(4) . . . . ?
C3 N3 C4 N1 1.5(6) . . . . ?
C6 N1 C4 O9 179.2(4) . . . . ?
Co1 N1 C4 O9 3.4(7) . . . . ?
C6 N1 C4 N3 -1.0(6) . . . . ?
Co1 N1 C4 N3 -176.9(3) . . . . ?
Co2 O5 C5 O6 178.9(3) . . . . ?
Co2 O5 C5 C6 -1.8(4) . . . . ?
Co1 O6 C5 O5 175.9(3) . . . . ?
Co1 O6 C5 C6 -3.5(4) . . . . ?
C4 N1 C6 N2 0.9(6) . . . . ?
Co1 N1 C6 N2 177.4(3) . . . . ?
C4 N1 C6 C5 -179.6(3) . . . . ?
Co1 N1 C6 C5 -3.1(4) . . . . ?
C3 N2 C6 N1 -1.0(5) . . . . ?
Co2 N2 C6 N1 174.5(3) . . . . ?
C3 N2 C6 C5 179.5(3) . . . . ?
Co2 N2 C6 C5 -5.0(4) . . . . ?
O5 C5 C6 N1 -174.8(3) . . . . ?
O6 C5 C6 N1 4.5(5) . . . . ?
O5 C5 C6 N2 4.7(5) . . . . ?
O6 C5 C6 N2 -175.9(3) . . . . ?
C7 N5 C7 O1 178.5(4) 3_655 . . . ?
C7 N5 C7 N4 -1.0(2) 3_655 . . . ?
C2 N4 C7 O1 -177.5(3) . . . . ?
Co2 N4 C7 O1 8.9(6) . . . . ?
C2 N4 C7 N5 2.0(4) . . . . ?
Co2 N4 C7 N5 -171.58(19) . . . . ?
O12B O12A O13B O13A 144(11) . . . . ?

_refine_diff_density_max         1.072
_refine_diff_density_min         -0.637
_refine_diff_density_rms         0.110
#
_vrf_PLAT430_Complex2            
;
PROBLEM: Short Inter D...A Contact  O12A   ..  O13B    ..       1.17 Ang.   
RESPONSE: Thermal parameters associated with the lattice occluded solvent
molecules Ox(x= 11,12A,12B,13A,13B,14A,14B) are relatively higher and H-atoms 
associated with these solvent molecules could not be located in the difference 
fourier map. Therefore it appears as short contact.
;
# 
#
_vrf_PLAT355_Complex2            
;
PROBLEM:  Long    O-H (X0.82,N0.98A) O7     -   H7A    ...       1.09 Ang.  
RESPONSE: High thermal parameter associated with metal coordinated O7 
molecule corresponds to the longer O-H distance.
;
#
_vrf_PLAT306_Complex2            
;
PROBLEM:   Isolated Oxygen Atom (H-atoms Missing ?) .......        O11 Check  
RESPONSE: We are not able to locate H-atoms associated with the 
lattice occluded solvent O11.
;
# 
_shelxl_version_number           2014/6

