# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1055583'
_audit_update_record             
;
2015-03-23 deposited with the CCDC.
2015-06-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C30 H42 Eu Fe7 N6 O42 P6, 2(H2 O)'
_chemical_formula_sum            'C30 H46 Eu Fe7 N6 O44 P6'
_chemical_melting_point          ?

_exptl_crystal_description       block
_exptl_crystal_colour            gold

_diffrn_ambient_temperature      296(2)
_chemical_formula_weight         1923.46

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'
Eu Eu -0.1578 3.6682 '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'
P P 0.1023 0.0942 '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'

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   'R -3'
_symmetry_int_tables_number      148
_chemical_absolute_configuration ?
_symmetry_space_group_name_HALL  '-R 3'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   15.3720(4)
_cell_length_b                   15.3720(4)
_cell_length_c                   22.8499(17)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     4676.0(4)
_cell_formula_units_Z            3
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    1346
_cell_measurement_theta_min      2.349
_cell_measurement_theta_max      23.511
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.049
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2864.9
_exptl_absorpt_coefficient_mu    2.836
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8049
_exptl_absorpt_correction_T_max  0.8950
_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  'multiwire proportional'
_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            9435
_diffrn_reflns_av_R_equivalents  0.0715
_diffrn_reflns_av_sigmaI/netI    0.0954
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         3.77
_diffrn_reflns_theta_max         28.29
_reflns_number_total             2577
_reflns_number_gt                1835
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker FRAMBO'
_computing_cell_refinement       'Bruker FRAMBO'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_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)+(0.0412P)²+62.4848P] 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_number_reflns         2577
_refine_ls_number_parameters     145
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0962
_refine_ls_R_factor_gt           0.0566
_refine_ls_wR_factor_ref         0.1222
_refine_ls_wR_factor_gt          0.1079
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_restrained_S_all      1.041
_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
Eu1 Eu 0.6667 0.3333 0.8333 0.01066(19) Uani 1 6 d S . .
Fe1 Fe 0.89916(7) 0.77569(7) 0.75564(4) 0.0247(3) Uani 1 1 d . . .
Fe2 Fe 0.6667 0.3333 0.63634(16) 0.0266(8) Uani 0.50 3 d SP . .
P1 P 0.75666(12) 0.54504(11) 0.72450(7) 0.0179(4) Uani 1 1 d . . .
N1 N 0.7308(4) 0.6988(4) 0.7627(2) 0.0218(11) Uani 1 1 d . . .
C1 C 0.6886(5) 0.6134(4) 0.7217(3) 0.0210(13) Uani 1 1 d . . .
H1A H 0.6914 0.6379 0.6823 0.025 Uiso 1 1 calc R . .
H1B H 0.6186 0.5682 0.7314 0.025 Uiso 1 1 calc R . .
C2 C 0.6994(5) 0.6617(5) 0.8234(3) 0.0293(15) Uani 1 1 d . . .
H2A H 0.6598 0.5889 0.8226 0.035 Uiso 1 1 calc R . .
H2B H 0.6566 0.6866 0.8379 0.035 Uiso 1 1 calc R . .
C3 C 0.7843(5) 0.6920(5) 0.8649(3) 0.0289(15) Uani 1 1 d . . .
C4 C 0.7030(5) 0.7761(5) 0.7463(3) 0.0297(16) Uani 1 1 d . . .
H4A H 0.6420 0.7621 0.7668 0.036 Uiso 1 1 calc R . .
H4B H 0.6896 0.7722 0.7046 0.036 Uiso 1 1 calc R . .
C5 C 0.7868(5) 0.8821(5) 0.7617(3) 0.0253(14) Uani 1 1 d . . .
O1 O 0.8663(3) 0.6272(3) 0.73566(18) 0.0212(9) Uani 1 1 d . . .
O2 O 0.7169(3) 0.4705(3) 0.77400(19) 0.0277(10) Uani 1 1 d . . .
O3 O 0.7440(4) 0.4977(3) 0.66456(19) 0.0307(11) Uani 1 1 d . . .
O4 O 0.8739(4) 0.7443(4) 0.8507(2) 0.0378(12) Uani 1 1 d . . .
O5 O 0.7600(4) 0.6613(4) 0.9186(2) 0.0426(13) Uani 1 1 d . . .
H5 H 0.6987 0.6292 0.9217 0.064 Uiso 1 1 calc R . .
O6 O 0.8733(4) 0.8968(3) 0.7719(2) 0.0327(11) Uani 1 1 d . . .
O7 O 0.7635(4) 0.9490(3) 0.7599(2) 0.0348(12) Uani 1 1 d . . .
O8 O 1.0000 0.0000 0.921(4) 0.66(8) Uani 1 3 d SD . .
H8A H 1.0182 0.0619 0.9237 0.789 Uiso 0.33 1 d PRD . .
H8B H 0.9558 -0.0264 0.8938 0.789 Uiso 0.33 1 d PRD . .


_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
Eu1 O2 2.292(4) 18_546 ?
Eu1 O2 2.292(4) 17_556 ?
Eu1 O2 2.292(4) 3_665 ?
Eu1 O2 2.292(4) 2_655 ?
Eu1 O2 2.292(4) 16_656 ?
Eu1 O2 2.292(4) . ?
Fe1 O7 2.102(5) 2_765 ?
Fe1 O6 2.121(5) . ?
Fe1 O1 2.127(4) . ?
Fe1 O3 2.141(5) 13_666 ?
Fe1 O4 2.218(5) . ?
Fe1 N1 2.250(5) . ?
Fe2 O3 2.283(5) 3_665 ?
Fe2 O3 2.283(5) . ?
Fe2 O3 2.283(5) 2_655 ?
P1 O2 1.505(4) . ?
P1 O3 1.517(5) . ?
P1 O1 1.540(4) . ?
P1 C1 1.817(6) . ?
N1 C1 1.473(8) . ?
N1 C2 1.486(8) . ?
N1 C4 1.498(8) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 C3 1.487(9) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 O4 1.240(8) . ?
C3 O5 1.302(8) . ?
C4 C5 1.529(9) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 O7 1.247(8) . ?
C5 O6 1.255(8) . ?
O3 Fe1 2.141(5) 13_666 ?
O5 H5 0.8200 . ?
O7 Fe1 2.102(5) 3_675 ?
O8 H8A 0.8500 . ?
O8 H8B 0.8501 . ?

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 Eu1 O2 88.57(16) 18_546 17_556 ?
O2 Eu1 O2 180.00(18) 18_546 3_665 ?
O2 Eu1 O2 91.43(16) 17_556 3_665 ?
O2 Eu1 O2 91.43(17) 18_546 2_655 ?
O2 Eu1 O2 179.998(1) 17_556 2_655 ?
O2 Eu1 O2 88.57(16) 3_665 2_655 ?
O2 Eu1 O2 88.57(17) 18_546 16_656 ?
O2 Eu1 O2 88.57(16) 17_556 16_656 ?
O2 Eu1 O2 91.43(16) 3_665 16_656 ?
O2 Eu1 O2 91.43(17) 2_655 16_656 ?
O2 Eu1 O2 91.43(17) 18_546 . ?
O2 Eu1 O2 91.43(17) 17_556 . ?
O2 Eu1 O2 88.57(17) 3_665 . ?
O2 Eu1 O2 88.57(16) 2_655 . ?
O2 Eu1 O2 179.998(1) 16_656 . ?
O7 Fe1 O6 114.28(19) 2_765 . ?
O7 Fe1 O1 87.08(17) 2_765 . ?
O6 Fe1 O1 158.64(18) . . ?
O7 Fe1 O3 89.79(19) 2_765 13_666 ?
O6 Fe1 O3 81.37(18) . 13_666 ?
O1 Fe1 O3 99.29(17) . 13_666 ?
O7 Fe1 O4 93.73(19) 2_765 . ?
O6 Fe1 O4 86.00(19) . . ?
O1 Fe1 O4 93.15(18) . . ?
O3 Fe1 O4 167.24(19) 13_666 . ?
O7 Fe1 N1 165.43(19) 2_765 . ?
O6 Fe1 N1 77.15(18) . . ?
O1 Fe1 N1 81.81(17) . . ?
O3 Fe1 N1 101.24(18) 13_666 . ?
O4 Fe1 N1 77.58(18) . . ?
O3 Fe2 O3 112.35(13) 3_665 . ?
O3 Fe2 O3 112.35(13) 3_665 2_655 ?
O3 Fe2 O3 112.35(12) . 2_655 ?
O2 P1 O3 114.0(3) . . ?
O2 P1 O1 111.2(3) . . ?
O3 P1 O1 111.6(3) . . ?
O2 P1 C1 109.5(3) . . ?
O3 P1 C1 105.8(3) . . ?
O1 P1 C1 104.0(3) . . ?
C1 N1 C2 109.7(5) . . ?
C1 N1 C4 112.0(5) . . ?
C2 N1 C4 111.8(5) . . ?
C1 N1 Fe1 107.5(4) . . ?
C2 N1 Fe1 109.7(4) . . ?
C4 N1 Fe1 106.0(4) . . ?
N1 C1 P1 111.6(4) . . ?
N1 C1 H1A 109.3 . . ?
P1 C1 H1A 109.3 . . ?
N1 C1 H1B 109.3 . . ?
P1 C1 H1B 109.3 . . ?
H1A C1 H1B 108.0 . . ?
N1 C2 C3 114.1(5) . . ?
N1 C2 H2A 108.7 . . ?
C3 C2 H2A 108.7 . . ?
N1 C2 H2B 108.7 . . ?
C3 C2 H2B 108.7 . . ?
H2A C2 H2B 107.6 . . ?
O4 C3 O5 120.3(6) . . ?
O4 C3 C2 123.6(6) . . ?
O5 C3 C2 116.1(6) . . ?
N1 C4 C5 111.4(5) . . ?
N1 C4 H4A 109.3 . . ?
C5 C4 H4A 109.3 . . ?
N1 C4 H4B 109.3 . . ?
C5 C4 H4B 109.3 . . ?
H4A C4 H4B 108.0 . . ?
O7 C5 O6 125.0(6) . . ?
O7 C5 C4 115.8(6) . . ?
O6 C5 C4 119.1(6) . . ?
P1 O1 Fe1 119.4(2) . . ?
P1 O2 Eu1 165.2(3) . . ?
P1 O3 Fe1 132.6(3) . 13_666 ?
P1 O3 Fe2 131.1(3) . . ?
Fe1 O3 Fe2 95.56(19) 13_666 . ?
C3 O4 Fe1 114.4(4) . . ?
C3 O5 H5 109.5 . . ?
C5 O6 Fe1 117.2(4) . . ?
C5 O7 Fe1 119.9(4) . 3_675 ?
H8A O8 H8B 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
O7 Fe1 N1 C1 -71.2(9) 2_765 . . . ?
O6 Fe1 N1 C1 145.7(4) . . . . ?
O1 Fe1 N1 C1 -30.6(3) . . . . ?
O3 Fe1 N1 C1 67.3(4) 13_666 . . . ?
O4 Fe1 N1 C1 -125.6(4) . . . . ?
O7 Fe1 N1 C2 48.0(9) 2_765 . . . ?
O6 Fe1 N1 C2 -95.1(4) . . . . ?
O1 Fe1 N1 C2 88.7(4) . . . . ?
O3 Fe1 N1 C2 -173.4(4) 13_666 . . . ?
O4 Fe1 N1 C2 -6.4(4) . . . . ?
O7 Fe1 N1 C4 168.8(7) 2_765 . . . ?
O6 Fe1 N1 C4 25.7(4) . . . . ?
O1 Fe1 N1 C4 -150.5(4) . . . . ?
O3 Fe1 N1 C4 -52.6(4) 13_666 . . . ?
O4 Fe1 N1 C4 114.4(4) . . . . ?
C2 N1 C1 P1 -76.2(5) . . . . ?
C4 N1 C1 P1 159.0(4) . . . . ?
Fe1 N1 C1 P1 43.0(4) . . . . ?
O2 P1 C1 N1 84.0(5) . . . . ?
O3 P1 C1 N1 -152.7(4) . . . . ?
O1 P1 C1 N1 -35.0(5) . . . . ?
C1 N1 C2 C3 123.5(6) . . . . ?
C4 N1 C2 C3 -111.6(6) . . . . ?
Fe1 N1 C2 C3 5.6(7) . . . . ?
N1 C2 C3 O4 0.4(10) . . . . ?
N1 C2 C3 O5 179.8(6) . . . . ?
C1 N1 C4 C5 -146.5(5) . . . . ?
C2 N1 C4 C5 89.9(6) . . . . ?
Fe1 N1 C4 C5 -29.5(6) . . . . ?
N1 C4 C5 O7 -167.1(6) . . . . ?
N1 C4 C5 O6 16.7(9) . . . . ?
O2 P1 O1 Fe1 -109.2(3) . . . . ?
O3 P1 O1 Fe1 122.3(3) . . . . ?
C1 P1 O1 Fe1 8.6(3) . . . . ?
O7 Fe1 O1 P1 -179.3(3) 2_765 . . . ?
O6 Fe1 O1 P1 0.0(6) . . . . ?
O3 Fe1 O1 P1 -90.0(3) 13_666 . . . ?
O4 Fe1 O1 P1 87.1(3) . . . . ?
N1 Fe1 O1 P1 10.1(3) . . . . ?
O3 P1 O2 Eu1 29.0(13) . . . . ?
O1 P1 O2 Eu1 -98.2(12) . . . . ?
C1 P1 O2 Eu1 147.4(11) . . . . ?
O2 Eu1 O2 P1 -165.3(11) 18_546 . . . ?
O2 Eu1 O2 P1 106.1(11) 17_556 . . . ?
O2 Eu1 O2 P1 14.7(11) 3_665 . . . ?
O2 Eu1 O2 P1 -73.9(11) 2_655 . . . ?
O2 Eu1 O2 P1 6(19) 16_656 . . . ?
O2 P1 O3 Fe1 171.7(3) . . . 13_666 ?
O1 P1 O3 Fe1 -61.3(4) . . . 13_666 ?
C1 P1 O3 Fe1 51.2(4) . . . 13_666 ?
O2 P1 O3 Fe2 4.3(5) . . . . ?
O1 P1 O3 Fe2 131.4(3) . . . . ?
C1 P1 O3 Fe2 -116.1(4) . . . . ?
O3 Fe2 O3 P1 -71.3(3) 3_665 . . . ?
O3 Fe2 O3 P1 56.5(4) 2_655 . . . ?
O3 Fe2 O3 Fe1 118.0(3) 3_665 . . 13_666 ?
O3 Fe2 O3 Fe1 -114.1(3) 2_655 . . 13_666 ?
O5 C3 O4 Fe1 174.2(5) . . . . ?
C2 C3 O4 Fe1 -6.5(9) . . . . ?
O7 Fe1 O4 C3 -161.1(5) 2_765 . . . ?
O6 Fe1 O4 C3 84.8(5) . . . . ?
O1 Fe1 O4 C3 -73.8(5) . . . . ?
O3 Fe1 O4 C3 93.2(9) 13_666 . . . ?
N1 Fe1 O4 C3 7.1(5) . . . . ?
O7 C5 O6 Fe1 -167.9(5) . . . . ?
C4 C5 O6 Fe1 7.9(8) . . . . ?
O7 Fe1 O6 C5 170.0(4) 2_765 . . . ?
O1 Fe1 O6 C5 -9.3(8) . . . . ?
O3 Fe1 O6 C5 84.1(5) 13_666 . . . ?
O4 Fe1 O6 C5 -97.7(5) . . . . ?
N1 Fe1 O6 C5 -19.6(4) . . . . ?
O6 C5 O7 Fe1 13.7(9) . . . 3_675 ?
C4 C5 O7 Fe1 -162.3(4) . . . 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 H5 O1 0.82 1.77 2.569(6) 164.6 18_546

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        28.29
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         1.189
_refine_diff_density_min         -1.001
_refine_diff_density_rms         0.180

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

data_1
_database_code_depnum_ccdc_archive 'CCDC 1055584'
_audit_update_record             
;
2015-03-23 deposited with the CCDC.
2015-06-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H42 Dy Fe7 N6 O42 P6, 2(H1.98 O)'
_chemical_formula_sum            'C30 H46 Dy Fe7 N6 O44 P6'
_chemical_formula_weight         1934.00

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'
Dy Dy -0.1892 4.4098 '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'
P P 0.1023 0.0942 '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'

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   'R -3'
_symmetry_space_group_name_HALL  '-R 3'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   15.2875(5)
_cell_length_b                   15.2875(5)
_cell_length_c                   22.7526(17)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     4605.1(4)
_cell_formula_units_Z            3
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    1656
_cell_measurement_theta_min      2.36
_cell_measurement_theta_max      27.86

_exptl_crystal_description       block
_exptl_crystal_colour            gold
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.092
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2874
_exptl_absorpt_coefficient_mu    3.076
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6389
_exptl_absorpt_correction_T_max  0.6727
_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  'multiwire proportional'
_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            7855
_diffrn_reflns_av_R_equivalents  0.0527
_diffrn_reflns_av_sigmaI/netI    0.0494
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         1.78
_diffrn_reflns_theta_max         25.99
_reflns_number_total             2019
_reflns_number_gt                1708
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker FRAMBO'
_computing_cell_refinement       'Bruker FRAMBO'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_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)+(0.0867P)²+89.0669P] 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_number_reflns         2019
_refine_ls_number_parameters     145
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0600
_refine_ls_R_factor_gt           0.0487
_refine_ls_wR_factor_ref         0.1551
_refine_ls_wR_factor_gt          0.1491
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_restrained_S_all      1.082
_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
Dy1 Dy 0.6667 0.3333 0.8333 0.0128(2) Uani 1 6 d S . .
Fe1 Fe 0.89904(8) 0.77519(8) 0.75554(5) 0.0235(3) Uani 1 1 d . . .
Fe2 Fe 0.6667 0.3333 0.63386(16) 0.0170(7) Uani 0.50 3 d SP . .
P1 P 0.75627(14) 0.54332(13) 0.72475(8) 0.0173(4) Uani 1 1 d . . .
N1 N 0.7293(5) 0.6973(5) 0.7627(3) 0.0224(13) Uani 1 1 d . . .
C1 C 0.6867(6) 0.6113(5) 0.7213(3) 0.0214(15) Uani 1 1 d . . .
H1A H 0.6898 0.6360 0.6816 0.026 Uiso 1 1 calc R . .
H1B H 0.6163 0.5657 0.7308 0.026 Uiso 1 1 calc R . .
C2 C 0.6991(6) 0.6615(6) 0.8239(3) 0.0273(17) Uani 1 1 d . . .
H2A H 0.6590 0.5884 0.8236 0.033 Uiso 1 1 calc R . .
H2B H 0.6564 0.6871 0.8384 0.033 Uiso 1 1 calc R . .
C3 C 0.7852(6) 0.6925(6) 0.8657(3) 0.0268(17) Uani 1 1 d . . .
C4 C 0.7021(6) 0.7736(6) 0.7462(4) 0.0276(17) Uani 1 1 d . . .
H4A H 0.6406 0.7595 0.7665 0.033 Uiso 1 1 calc R . .
H4B H 0.6887 0.7692 0.7043 0.033 Uiso 1 1 calc R . .
C5 C 0.7862(6) 0.8815(6) 0.7614(3) 0.0241(16) Uani 1 1 d . . .
O1 O 0.8671(4) 0.6268(4) 0.7350(2) 0.0207(10) Uani 1 1 d . . .
O2 O 0.7181(4) 0.4695(4) 0.7749(2) 0.0242(11) Uani 1 1 d . . .
O3 O 0.7432(4) 0.4951(4) 0.6650(2) 0.0283(12) Uani 1 1 d . . .
O4 O 0.8749(4) 0.7442(5) 0.8506(3) 0.0341(13) Uani 1 1 d . . .
O5 O 0.7611(5) 0.6633(5) 0.9198(2) 0.0357(14) Uani 1 1 d . . .
H5 H 0.7004 0.6411 0.9245 0.053 Uiso 1 1 calc R . .
O6 O 0.8728(4) 0.8969(4) 0.7719(2) 0.0297(13) Uani 1 1 d . . .
O7 O 0.7615(4) 0.9486(4) 0.7594(3) 0.0304(13) Uani 1 1 d . . .
O8 O 1.0000 0.0000 1.051(5) 0.62(17) Uani 1 3 d SD . .
H8A H 1.0182 0.0619 1.0543 0.743 Uiso 0.33 1 d PRD . .
H8B H 0.9558 -0.0264 1.0244 0.743 Uiso 0.33 1 d PRD . .


_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 O2 2.254(5) 18_546 ?
Dy1 O2 2.254(5) 17_556 ?
Dy1 O2 2.254(5) 3_665 ?
Dy1 O2 2.254(5) 2_655 ?
Dy1 O2 2.254(5) . ?
Dy1 O2 2.254(5) 16_656 ?
Fe1 O7 2.103(6) 2_765 ?
Fe1 O1 2.120(5) . ?
Fe1 O6 2.123(6) . ?
Fe1 O3 2.154(5) 13_666 ?
Fe1 O4 2.205(6) . ?
Fe1 N1 2.256(6) . ?
Fe2 O3 2.257(6) 3_665 ?
Fe2 O3 2.257(6) . ?
Fe2 O3 2.257(6) 2_655 ?
P1 O2 1.503(5) . ?
P1 O3 1.512(5) . ?
P1 O1 1.546(5) . ?
P1 C1 1.823(7) . ?
N1 C4 1.470(10) . ?
N1 C1 1.479(9) . ?
N1 C2 1.482(9) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 C3 1.496(11) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 O4 1.240(9) . ?
C3 O5 1.299(9) . ?
C4 C5 1.540(11) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 O6 1.246(10) . ?
C5 O7 1.259(9) . ?
O3 Fe1 2.154(5) 13_666 ?
O5 H5 0.8200 . ?
O7 Fe1 2.103(6) 3_675 ?
O8 H8A 0.8454 . ?
O8 H8B 0.8460 . ?

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 Dy1 O2 88.78(19) 18_546 17_556 ?
O2 Dy1 O2 180.0(2) 18_546 3_665 ?
O2 Dy1 O2 91.22(19) 17_556 3_665 ?
O2 Dy1 O2 91.22(19) 18_546 2_655 ?
O2 Dy1 O2 179.998(1) 17_556 2_655 ?
O2 Dy1 O2 88.78(19) 3_665 2_655 ?
O2 Dy1 O2 91.22(19) 18_546 . ?
O2 Dy1 O2 91.22(19) 17_556 . ?
O2 Dy1 O2 88.78(19) 3_665 . ?
O2 Dy1 O2 88.78(19) 2_655 . ?
O2 Dy1 O2 88.78(19) 18_546 16_656 ?
O2 Dy1 O2 88.78(19) 17_556 16_656 ?
O2 Dy1 O2 91.22(19) 3_665 16_656 ?
O2 Dy1 O2 91.22(19) 2_655 16_656 ?
O2 Dy1 O2 179.998(1) . 16_656 ?
O7 Fe1 O1 86.2(2) 2_765 . ?
O7 Fe1 O6 114.9(2) 2_765 . ?
O1 Fe1 O6 158.9(2) . . ?
O7 Fe1 O3 89.8(2) 2_765 13_666 ?
O1 Fe1 O3 99.9(2) . 13_666 ?
O6 Fe1 O3 80.6(2) . 13_666 ?
O7 Fe1 O4 93.5(2) 2_765 . ?
O1 Fe1 O4 93.5(2) . . ?
O6 Fe1 O4 86.1(2) . . ?
O3 Fe1 O4 166.4(2) 13_666 . ?
O7 Fe1 N1 165.0(2) 2_765 . ?
O1 Fe1 N1 82.1(2) . . ?
O6 Fe1 N1 77.2(2) . . ?
O3 Fe1 N1 101.5(2) 13_666 . ?
O4 Fe1 N1 77.9(2) . . ?
O3 Fe2 O3 110.64(16) 3_665 . ?
O3 Fe2 O3 110.64(16) 3_665 2_655 ?
O3 Fe2 O3 110.64(15) . 2_655 ?
O2 P1 O3 114.2(3) . . ?
O2 P1 O1 111.0(3) . . ?
O3 P1 O1 111.2(3) . . ?
O2 P1 C1 110.0(3) . . ?
O3 P1 C1 105.4(3) . . ?
O1 P1 C1 104.3(3) . . ?
C4 N1 C1 111.6(6) . . ?
C4 N1 C2 111.9(6) . . ?
C1 N1 C2 110.7(6) . . ?
C4 N1 Fe1 105.7(5) . . ?
C1 N1 Fe1 107.6(4) . . ?
C2 N1 Fe1 109.1(4) . . ?
N1 C1 P1 110.8(5) . . ?
N1 C1 H1A 109.5 . . ?
P1 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
P1 C1 H1B 109.5 . . ?
H1A C1 H1B 108.1 . . ?
N1 C2 C3 114.7(6) . . ?
N1 C2 H2A 108.6 . . ?
C3 C2 H2A 108.6 . . ?
N1 C2 H2B 108.6 . . ?
C3 C2 H2B 108.6 . . ?
H2A C2 H2B 107.6 . . ?
O4 C3 O5 121.0(7) . . ?
O4 C3 C2 122.9(7) . . ?
O5 C3 C2 116.1(7) . . ?
N1 C4 C5 112.1(6) . . ?
N1 C4 H4A 109.2 . . ?
C5 C4 H4A 109.2 . . ?
N1 C4 H4B 109.2 . . ?
C5 C4 H4B 109.2 . . ?
H4A C4 H4B 107.9 . . ?
O6 C5 O7 125.2(8) . . ?
O6 C5 C4 119.0(7) . . ?
O7 C5 C4 115.7(7) . . ?
P1 O1 Fe1 119.2(3) . . ?
P1 O2 Dy1 165.1(3) . . ?
P1 O3 Fe1 131.2(3) . 13_666 ?
P1 O3 Fe2 133.3(3) . . ?
Fe1 O3 Fe2 94.6(2) 13_666 . ?
C3 O4 Fe1 114.9(5) . . ?
C3 O5 H5 109.5 . . ?
C5 O6 Fe1 116.7(5) . . ?
C5 O7 Fe1 118.7(5) . 3_675 ?
H8A O8 H8B 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
O7 Fe1 N1 C4 170.9(8) 2_765 . . . ?
O1 Fe1 N1 C4 -149.8(5) . . . . ?
O6 Fe1 N1 C4 26.1(5) . . . . ?
O3 Fe1 N1 C4 -51.3(5) 13_666 . . . ?
O4 Fe1 N1 C4 114.8(5) . . . . ?
O7 Fe1 N1 C1 -69.7(10) 2_765 . . . ?
O1 Fe1 N1 C1 -30.5(4) . . . . ?
O6 Fe1 N1 C1 145.4(5) . . . . ?
O3 Fe1 N1 C1 68.0(4) 13_666 . . . ?
O4 Fe1 N1 C1 -125.9(5) . . . . ?
O7 Fe1 N1 C2 50.4(11) 2_765 . . . ?
O1 Fe1 N1 C2 89.6(5) . . . . ?
O6 Fe1 N1 C2 -94.4(5) . . . . ?
O3 Fe1 N1 C2 -171.8(5) 13_666 . . . ?
O4 Fe1 N1 C2 -5.7(5) . . . . ?
C4 N1 C1 P1 158.8(5) . . . . ?
C2 N1 C1 P1 -75.8(7) . . . . ?
Fe1 N1 C1 P1 43.3(5) . . . . ?
O2 P1 C1 N1 83.0(5) . . . . ?
O3 P1 C1 N1 -153.3(5) . . . . ?
O1 P1 C1 N1 -36.1(5) . . . . ?
C4 N1 C2 C3 -111.5(7) . . . . ?
C1 N1 C2 C3 123.3(7) . . . . ?
Fe1 N1 C2 C3 5.1(8) . . . . ?
N1 C2 C3 O4 0.1(11) . . . . ?
N1 C2 C3 O5 179.2(7) . . . . ?
C1 N1 C4 C5 -146.3(6) . . . . ?
C2 N1 C4 C5 88.9(8) . . . . ?
Fe1 N1 C4 C5 -29.7(7) . . . . ?
N1 C4 C5 O6 16.5(10) . . . . ?
N1 C4 C5 O7 -166.5(6) . . . . ?
O2 P1 O1 Fe1 -108.3(3) . . . . ?
O3 P1 O1 Fe1 123.3(3) . . . . ?
C1 P1 O1 Fe1 10.1(4) . . . . ?
O7 Fe1 O1 P1 179.6(3) 2_765 . . . ?
O6 Fe1 O1 P1 -2.0(8) . . . . ?
O3 Fe1 O1 P1 -91.3(3) 13_666 . . . ?
O4 Fe1 O1 P1 86.3(3) . . . . ?
N1 Fe1 O1 P1 9.1(3) . . . . ?
O3 P1 O2 Dy1 22.6(15) . . . . ?
O1 P1 O2 Dy1 -104.1(14) . . . . ?
C1 P1 O2 Dy1 141.0(13) . . . . ?
O2 Dy1 O2 P1 -159.5(13) 18_546 . . . ?
O2 Dy1 O2 P1 111.7(12) 17_556 . . . ?
O2 Dy1 O2 P1 20.5(13) 3_665 . . . ?
O2 Dy1 O2 P1 -68.3(12) 2_655 . . . ?
O2 Dy1 O2 P1 12(10) 16_656 . . . ?
O2 P1 O3 Fe1 172.5(4) . . . 13_666 ?
O1 P1 O3 Fe1 -60.8(5) . . . 13_666 ?
C1 P1 O3 Fe1 51.6(5) . . . 13_666 ?
O2 P1 O3 Fe2 5.8(6) . . . . ?
O1 P1 O3 Fe2 132.4(4) . . . . ?
C1 P1 O3 Fe2 -115.2(4) . . . . ?
O3 Fe2 O3 P1 -69.2(4) 3_665 . . . ?
O3 Fe2 O3 P1 53.7(5) 2_655 . . . ?
O3 Fe2 O3 Fe1 120.7(3) 3_665 . . 13_666 ?
O3 Fe2 O3 Fe1 -116.3(3) 2_655 . . 13_666 ?
O5 C3 O4 Fe1 175.4(6) . . . . ?
C2 C3 O4 Fe1 -5.5(10) . . . . ?
O7 Fe1 O4 C3 -161.3(6) 2_765 . . . ?
O1 Fe1 O4 C3 -74.9(6) . . . . ?
O6 Fe1 O4 C3 83.9(6) . . . . ?
O3 Fe1 O4 C3 95.2(11) 13_666 . . . ?
N1 Fe1 O4 C3 6.2(6) . . . . ?
O7 C5 O6 Fe1 -168.1(6) . . . . ?
C4 C5 O6 Fe1 8.6(9) . . . . ?
O7 Fe1 O6 C5 169.5(5) 2_765 . . . ?
O1 Fe1 O6 C5 -8.7(9) . . . . ?
O3 Fe1 O6 C5 84.2(5) 13_666 . . . ?
O4 Fe1 O6 C5 -98.4(6) . . . . ?
N1 Fe1 O6 C5 -20.0(5) . . . . ?
O6 C5 O7 Fe1 13.9(10) . . . 3_675 ?
C4 C5 O7 Fe1 -162.9(5) . . . 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 H5 O1 0.82 1.81 2.555(8) 149.5 18_546

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.99
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         1.711
_refine_diff_density_min         -1.204
_refine_diff_density_rms         0.230
####################################################################### 
# 
# 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 1055585'
_audit_update_record             
;
2015-03-23 deposited with the CCDC.
2015-06-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H42 Fe7 Ho N6 O42 P6, H4 O2'
_chemical_formula_sum            'C30 H46 Fe7 Ho N6 O44 P6'
_chemical_formula_weight         1936.43

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'
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'
P P 0.1023 0.0942 '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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   'R -3'
_symmetry_space_group_name_HALL  '-R 3'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   15.2935(4)
_cell_length_b                   15.2935(4)
_cell_length_c                   22.7749(12)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     4613.2(3)
_cell_formula_units_Z            3
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2596
_cell_measurement_theta_min      2.36
_cell_measurement_theta_max      27.35

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.091
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2877
_exptl_absorpt_coefficient_mu    3.142
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7441
_exptl_absorpt_correction_T_max  0.7872
_exptl_absorpt_process_details   'SADABS(Bruker, 2000)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(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  'multiwire proportional'
_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            8237
_diffrn_reflns_av_R_equivalents  0.0393
_diffrn_reflns_av_sigmaI/netI    0.0396
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         2.36
_diffrn_reflns_theta_max         25.99
_reflns_number_total             2021
_reflns_number_gt                1770
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker FRAMBO'
_computing_cell_refinement       'Bruker FRAMBO'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_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)+(0.0691P)²+144.6606P] 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_number_reflns         2021
_refine_ls_number_parameters     145
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0554
_refine_ls_R_factor_gt           0.0470
_refine_ls_wR_factor_ref         0.1398
_refine_ls_wR_factor_gt          0.1361
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_restrained_S_all      1.047
_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 1.0000 0.5000 0.0105(2) Uani 1 6 d S . .
Fe1 Fe 0.23263(8) 0.79057(8) 0.42216(5) 0.0236(3) Uani 1 1 d . . .
Fe2 Fe 0.0000 1.0000 0.29856(15) 0.0136(6) Uani 0.50 3 d SP . .
P1 P 0.09014(13) 0.88029(13) 0.39182(7) 0.0167(4) Uani 1 1 d . . .
C1 C 0.0208(5) 0.7433(5) 0.3882(3) 0.0196(14) Uani 1 1 d . . .
H1A H -0.0495 0.7186 0.3977 0.024 Uiso 1 1 calc R . .
H1B H 0.0240 0.7219 0.3485 0.024 Uiso 1 1 calc R . .
C2 C 0.0332(6) 0.7049(6) 0.4905(3) 0.0252(16) Uani 1 1 d . . .
H2A H -0.0068 0.7381 0.4904 0.030 Uiso 1 1 calc R . .
H2B H -0.0095 0.6367 0.5049 0.030 Uiso 1 1 calc R . .
C3 C 0.1184(6) 0.7591(6) 0.5321(3) 0.0262(16) Uani 1 1 d . . .
C4 C 0.0353(6) 0.5946(6) 0.4127(4) 0.0270(16) Uani 1 1 d . . .
H4A H 0.0223 0.5857 0.3708 0.032 Uiso 1 1 calc R . .
H4B H -0.0263 0.5473 0.4329 0.032 Uiso 1 1 calc R . .
C5 C 0.1185(5) 0.5711(5) 0.4280(3) 0.0227(15) Uani 1 1 d . . .
N1 N 0.0628(5) 0.6994(5) 0.4292(3) 0.0232(13) Uani 1 1 d . . .
O1 O 0.2007(4) 0.9071(4) 0.4020(2) 0.0210(10) Uani 1 1 d . . .
O2 O 0.0519(4) 0.9158(4) 0.4419(2) 0.0231(11) Uani 1 1 d . . .
O3 O 0.0769(4) 0.9149(4) 0.3317(2) 0.0283(12) Uani 1 1 d . . .
O4 O 0.2082(4) 0.7975(4) 0.5172(3) 0.0329(13) Uani 1 1 d . . .
O5 O 0.0949(4) 0.7648(5) 0.5866(2) 0.0358(14) Uani 1 1 d . . .
H5 H 0.0333 0.7335 0.5903 0.054 Uiso 1 1 calc R . .
O6 O 0.2060(4) 0.6427(4) 0.4386(2) 0.0287(12) Uani 1 1 d . . .
O7 O 0.0953(4) 0.4803(4) 0.4256(2) 0.0307(12) Uani 1 1 d . . .
O8 O 0.0000 1.0000 0.954(8) 0.6(2) Uani 1 3 d S . .
H8A H -0.0100 1.0063 0.9902 0.954 Uiso 0.33 1 d PR . .
H8B H 0.0129 0.9529 0.9504 0.954 Uiso 0.33 1 d PR . .


_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 O2 2.250(5) 12_666 ?
Ho1 O2 2.250(5) 3_465 ?
Ho1 O2 2.250(5) 11_456 ?
Ho1 O2 2.250(4) . ?
Ho1 O2 2.250(4) 10_576 ?
Ho1 O2 2.250(5) 2_675 ?
Fe1 O7 2.101(5) 3_565 ?
Fe1 O1 2.120(5) . ?
Fe1 O6 2.121(5) . ?
Fe1 O3 2.155(5) 16_565 ?
Fe1 O4 2.209(6) . ?
Fe1 N1 2.258(6) . ?
Fe2 O3 2.275(5) 2_675 ?
Fe2 O3 2.275(5) . ?
Fe2 O3 2.275(5) 3_465 ?
P1 O2 1.502(5) . ?
P1 O3 1.517(5) . ?
P1 O1 1.545(5) . ?
P1 C1 1.817(7) . ?
C1 N1 1.471(9) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 C3 1.483(11) . ?
C2 N1 1.483(9) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 O4 1.240(9) . ?
C3 O5 1.308(9) . ?
C4 N1 1.488(9) . ?
C4 C5 1.526(10) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 O7 1.251(9) . ?
C5 O6 1.258(9) . ?
O3 Fe1 2.155(5) 16_565 ?
O5 H5 0.8200 . ?
O7 Fe1 2.101(5) 2_665 ?
O8 H8A 0.8464 . ?
O8 H8B 0.8413 . ?

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 Ho1 O2 180.000(1) 12_666 3_465 ?
O2 Ho1 O2 88.91(19) 12_666 11_456 ?
O2 Ho1 O2 91.09(19) 3_465 11_456 ?
O2 Ho1 O2 91.09(19) 12_666 . ?
O2 Ho1 O2 88.91(19) 3_465 . ?
O2 Ho1 O2 91.09(19) 11_456 . ?
O2 Ho1 O2 88.91(19) 12_666 10_576 ?
O2 Ho1 O2 91.09(19) 3_465 10_576 ?
O2 Ho1 O2 88.91(19) 11_456 10_576 ?
O2 Ho1 O2 180.0(2) . 10_576 ?
O2 Ho1 O2 91.09(19) 12_666 2_675 ?
O2 Ho1 O2 88.91(19) 3_465 2_675 ?
O2 Ho1 O2 180.0(2) 11_456 2_675 ?
O2 Ho1 O2 88.91(19) . 2_675 ?
O2 Ho1 O2 91.09(19) 10_576 2_675 ?
O7 Fe1 O1 86.3(2) 3_565 . ?
O7 Fe1 O6 114.9(2) 3_565 . ?
O1 Fe1 O6 158.8(2) . . ?
O7 Fe1 O3 89.6(2) 3_565 16_565 ?
O1 Fe1 O3 100.00(19) . 16_565 ?
O6 Fe1 O3 80.6(2) . 16_565 ?
O7 Fe1 O4 93.9(2) 3_565 . ?
O1 Fe1 O4 93.2(2) . . ?
O6 Fe1 O4 86.1(2) . . ?
O3 Fe1 O4 166.5(2) 16_565 . ?
O7 Fe1 N1 165.0(2) 3_565 . ?
O1 Fe1 N1 81.8(2) . . ?
O6 Fe1 N1 77.3(2) . . ?
O3 Fe1 N1 101.3(2) 16_565 . ?
O4 Fe1 N1 77.9(2) . . ?
O3 Fe2 O3 109.56(15) 2_675 . ?
O3 Fe2 O3 109.56(15) 2_675 3_465 ?
O3 Fe2 O3 109.56(15) . 3_465 ?
O2 P1 O3 114.5(3) . . ?
O2 P1 O1 111.2(3) . . ?
O3 P1 O1 111.2(3) . . ?
O2 P1 C1 110.1(3) . . ?
O3 P1 C1 105.0(3) . . ?
O1 P1 C1 104.0(3) . . ?
N1 C1 P1 111.2(5) . . ?
N1 C1 H1A 109.4 . . ?
P1 C1 H1A 109.4 . . ?
N1 C1 H1B 109.4 . . ?
P1 C1 H1B 109.4 . . ?
H1A C1 H1B 108.0 . . ?
C3 C2 N1 115.1(6) . . ?
C3 C2 H2A 108.5 . . ?
N1 C2 H2A 108.5 . . ?
C3 C2 H2B 108.5 . . ?
N1 C2 H2B 108.5 . . ?
H2A C2 H2B 107.5 . . ?
O4 C3 O5 120.3(7) . . ?
O4 C3 C2 123.1(7) . . ?
O5 C3 C2 116.6(6) . . ?
N1 C4 C5 112.1(6) . . ?
N1 C4 H4A 109.2 . . ?
C5 C4 H4A 109.2 . . ?
N1 C4 H4B 109.2 . . ?
C5 C4 H4B 109.2 . . ?
H4A C4 H4B 107.9 . . ?
O7 C5 O6 124.2(7) . . ?
O7 C5 C4 116.4(6) . . ?
O6 C5 C4 119.2(6) . . ?
C1 N1 C2 110.9(6) . . ?
C1 N1 C4 112.2(6) . . ?
C2 N1 C4 111.7(6) . . ?
C1 N1 Fe1 107.6(4) . . ?
C2 N1 Fe1 108.7(4) . . ?
C4 N1 Fe1 105.4(4) . . ?
P1 O1 Fe1 119.4(3) . . ?
P1 O2 Ho1 165.1(3) . . ?
P1 O3 Fe1 131.7(3) . 16_565 ?
P1 O3 Fe2 134.1(3) . . ?
Fe1 O3 Fe2 93.4(2) 16_565 . ?
C3 O4 Fe1 114.7(5) . . ?
C3 O5 H5 109.5 . . ?
C5 O6 Fe1 116.6(5) . . ?
C5 O7 Fe1 119.8(5) . 2_665 ?
H8A O8 H8B 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
O2 P1 C1 N1 -83.2(5) . . . . ?
O3 P1 C1 N1 153.1(5) . . . . ?
O1 P1 C1 N1 36.1(5) . . . . ?
N1 C2 C3 O4 0.1(11) . . . . ?
N1 C2 C3 O5 -179.6(7) . . . . ?
N1 C4 C5 O7 167.5(6) . . . . ?
N1 C4 C5 O6 -16.8(10) . . . . ?
P1 C1 N1 C2 75.4(6) . . . . ?
P1 C1 N1 C4 -158.8(5) . . . . ?
P1 C1 N1 Fe1 -43.4(5) . . . . ?
C3 C2 N1 C1 -123.0(7) . . . . ?
C3 C2 N1 C4 111.1(7) . . . . ?
C3 C2 N1 Fe1 -4.8(8) . . . . ?
C5 C4 N1 C1 146.5(6) . . . . ?
C5 C4 N1 C2 -88.2(7) . . . . ?
C5 C4 N1 Fe1 29.8(7) . . . . ?
O7 Fe1 N1 C1 68.0(10) 3_565 . . . ?
O1 Fe1 N1 C1 30.4(4) . . . . ?
O6 Fe1 N1 C1 -145.8(5) . . . . ?
O3 Fe1 N1 C1 -68.2(4) 16_565 . . . ?
O4 Fe1 N1 C1 125.5(4) . . . . ?
O7 Fe1 N1 C2 -52.2(11) 3_565 . . . ?
O1 Fe1 N1 C2 -89.8(5) . . . . ?
O6 Fe1 N1 C2 94.0(5) . . . . ?
O3 Fe1 N1 C2 171.6(4) 16_565 . . . ?
O4 Fe1 N1 C2 5.3(4) . . . . ?
O7 Fe1 N1 C4 -172.2(8) 3_565 . . . ?
O1 Fe1 N1 C4 150.3(5) . . . . ?
O6 Fe1 N1 C4 -25.9(4) . . . . ?
O3 Fe1 N1 C4 51.6(5) 16_565 . . . ?
O4 Fe1 N1 C4 -114.6(5) . . . . ?
O2 P1 O1 Fe1 108.4(3) . . . . ?
O3 P1 O1 Fe1 -122.6(3) . . . . ?
C1 P1 O1 Fe1 -10.1(4) . . . . ?
O7 Fe1 O1 P1 -180.0(3) 3_565 . . . ?
O6 Fe1 O1 P1 1.2(7) . . . . ?
O3 Fe1 O1 P1 91.1(3) 16_565 . . . ?
O4 Fe1 O1 P1 -86.3(3) . . . . ?
N1 Fe1 O1 P1 -9.0(3) . . . . ?
O3 P1 O2 Ho1 -22.2(14) . . . . ?
O1 P1 O2 Ho1 105.0(13) . . . . ?
C1 P1 O2 Ho1 -140.2(12) . . . . ?
O2 Ho1 O2 P1 -112.2(12) 12_666 . . . ?
O2 Ho1 O2 P1 67.8(12) 3_465 . . . ?
O2 Ho1 O2 P1 158.9(12) 11_456 . . . ?
O2 Ho1 O2 P1 -157(100) 10_576 . . . ?
O2 Ho1 O2 P1 -21.1(12) 2_675 . . . ?
O2 P1 O3 Fe1 -172.3(4) . . . 16_565 ?
O1 P1 O3 Fe1 60.6(5) . . . 16_565 ?
C1 P1 O3 Fe1 -51.4(5) . . . 16_565 ?
O2 P1 O3 Fe2 -5.8(6) . . . . ?
O1 P1 O3 Fe2 -133.0(4) . . . . ?
C1 P1 O3 Fe2 115.1(4) . . . . ?
O3 Fe2 O3 P1 67.8(4) 2_675 . . . ?
O3 Fe2 O3 P1 -52.4(5) 3_465 . . . ?
O3 Fe2 O3 Fe1 -122.3(3) 2_675 . . 16_565 ?
O3 Fe2 O3 Fe1 117.5(3) 3_465 . . 16_565 ?
O5 C3 O4 Fe1 -175.3(6) . . . . ?
C2 C3 O4 Fe1 5.0(10) . . . . ?
O7 Fe1 O4 C3 161.6(6) 3_565 . . . ?
O1 Fe1 O4 C3 75.1(6) . . . . ?
O6 Fe1 O4 C3 -83.6(6) . . . . ?
O3 Fe1 O4 C3 -93.6(10) 16_565 . . . ?
N1 Fe1 O4 C3 -5.8(5) . . . . ?
O7 C5 O6 Fe1 167.1(6) . . . . ?
C4 C5 O6 Fe1 -8.2(9) . . . . ?
O7 Fe1 O6 C5 -169.3(5) 3_565 . . . ?
O1 Fe1 O6 C5 9.4(9) . . . . ?
O3 Fe1 O6 C5 -84.1(5) 16_565 . . . ?
O4 Fe1 O6 C5 98.2(5) . . . . ?
N1 Fe1 O6 C5 19.8(5) . . . . ?
O6 C5 O7 Fe1 -12.6(10) . . . 2_665 ?
C4 C5 O7 Fe1 162.9(5) . . . 2_665 ?

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
O8 H8A O8 0.85 1.28 2.1(3) 155.4 10_577
O5 H5 O1 0.82 1.77 2.559(7) 161.4 11_456

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.99
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         2.481
_refine_diff_density_min         -1.425
_refine_diff_density_rms         0.196
####################################################################### 
# 
# 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 1055586'
_audit_update_record             
;
2015-03-23 deposited with the CCDC.
2015-06-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H42 Fe7 N6 O42 P6 Y, 2(H2 O)'
_chemical_formula_sum            'C30 H46 Fe7 N6 O44 P6 Y'
_chemical_formula_weight         1860.41

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'
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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Y Y -2.7962 3.5667 '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'

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   'R -3'
_symmetry_space_group_name_HALL  '-R 3'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   15.3080(3)
_cell_length_b                   15.3080(3)
_cell_length_c                   22.7261(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     4612.0(2)
_cell_formula_units_Z            3
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1427
_cell_measurement_theta_min      2.36
_cell_measurement_theta_max      25.98

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.009
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2793
_exptl_absorpt_coefficient_mu    2.804
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6625
_exptl_absorpt_correction_T_max  0.7296
_exptl_absorpt_process_details   'SADABS(Bruker, 2000)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(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  'multiwire proportional'
_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            8116
_diffrn_reflns_av_R_equivalents  0.0550
_diffrn_reflns_av_sigmaI/netI    0.0558
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.36
_diffrn_reflns_theta_max         25.99
_reflns_number_total             2016
_reflns_number_gt                1520
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker FRAMBO'
_computing_cell_refinement       'Bruker FRAMBO'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_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)+(0.0808P)²+46.8069P] 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_number_reflns         2016
_refine_ls_number_parameters     145
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0682
_refine_ls_R_factor_gt           0.0448
_refine_ls_wR_factor_ref         0.1465
_refine_ls_wR_factor_gt          0.1380
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_restrained_S_all      1.008
_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
Y1 Y 0.0000 1.0000 0.5000 0.0118(3) Uani 1 6 d S . .
Fe1 Fe 0.23243(6) 0.79024(6) 0.42235(4) 0.0183(3) Uani 1 1 d . . .
Fe2 Fe 0.0000 1.0000 0.30104(14) 0.0219(7) Uani 0.50 3 d SP . .
P1 P 0.09025(10) 0.88027(10) 0.39152(6) 0.0134(3) Uani 1 1 d . . .
C1 C 0.0216(4) 0.7434(4) 0.3878(2) 0.0165(12) Uani 1 1 d . . .
H1A H -0.0489 0.7186 0.3969 0.020 Uiso 1 1 calc R . .
H1B H 0.0255 0.7223 0.3482 0.020 Uiso 1 1 calc R . .
C2 C 0.0331(4) 0.7053(5) 0.4904(3) 0.0208(13) Uani 1 1 d . . .
H2A H -0.0103 0.6374 0.5049 0.025 Uiso 1 1 calc R . .
H2B H -0.0061 0.7391 0.4898 0.025 Uiso 1 1 calc R . .
C3 C 0.1194(4) 0.7597(4) 0.5324(3) 0.0212(13) Uani 1 1 d . . .
C4 C 0.0355(4) 0.5949(4) 0.4130(3) 0.0227(13) Uani 1 1 d . . .
H4A H 0.0225 0.5862 0.3710 0.027 Uiso 1 1 calc R . .
H4B H -0.0260 0.5477 0.4332 0.027 Uiso 1 1 calc R . .
C5 C 0.1190(4) 0.5711(4) 0.4284(3) 0.0197(13) Uani 1 1 d . . .
N1 N 0.0633(4) 0.6991(3) 0.4298(2) 0.0180(10) Uani 1 1 d . . .
O1 O 0.2004(3) 0.9067(3) 0.40246(16) 0.0149(8) Uani 1 1 d . . .
O2 O 0.0513(3) 0.9160(3) 0.44168(18) 0.0210(9) Uani 1 1 d . . .
O3 O 0.0779(3) 0.9150(3) 0.33134(18) 0.0227(9) Uani 1 1 d . . .
O4 O 0.2081(3) 0.7969(3) 0.51751(19) 0.0252(10) Uani 1 1 d . . .
O5 O 0.0945(3) 0.7647(3) 0.58704(18) 0.0287(10) Uani 1 1 d . . .
H5 H 0.0339 0.7259 0.5916 0.043 Uiso 1 1 calc R . .
O6 O 0.2062(3) 0.6431(3) 0.43887(19) 0.0229(9) Uani 1 1 d . . .
O7 O 0.0954(3) 0.4800(3) 0.42543(19) 0.0249(10) Uani 1 1 d . . .
O8 O 0.0000 1.0000 0.928(3) 0.48(5) Uani 1 3 d S . .
H8A H -0.0100 1.0063 0.9644 0.727 Uiso 0.33 1 d PR . .
H8B H 0.0129 0.9529 0.9246 0.727 Uiso 0.33 1 d PR . .


_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
Y1 O2 2.244(4) 3_465 ?
Y1 O2 2.244(4) 12_666 ?
Y1 O2 2.244(4) 10_576 ?
Y1 O2 2.244(4) 11_456 ?
Y1 O2 2.244(4) . ?
Y1 O2 2.244(4) 2_675 ?
Fe1 O7 2.102(4) 3_565 ?
Fe1 O6 2.114(4) . ?
Fe1 O1 2.120(4) . ?
Fe1 O3 2.143(4) 16_565 ?
Fe1 O4 2.206(4) . ?
Fe1 N1 2.251(5) . ?
Fe2 O3 2.267(4) 2_675 ?
Fe2 O3 2.267(4) . ?
Fe2 O3 2.267(4) 3_465 ?
P1 O2 1.510(4) . ?
P1 O3 1.513(4) . ?
P1 O1 1.545(4) . ?
P1 C1 1.816(6) . ?
C1 N1 1.486(7) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 N1 1.471(7) . ?
C2 C3 1.499(8) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 O4 1.228(7) . ?
C3 O5 1.313(7) . ?
C4 N1 1.480(7) . ?
C4 C5 1.534(8) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 O7 1.256(7) . ?
C5 O6 1.258(7) . ?
O3 Fe1 2.143(4) 16_565 ?
O5 H5 0.8200 . ?
O7 Fe1 2.102(4) 2_665 ?
O8 H8A 0.8448 . ?
O8 H8B 0.8421 . ?

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 Y1 O2 180.000(1) 3_465 12_666 ?
O2 Y1 O2 91.32(15) 3_465 10_576 ?
O2 Y1 O2 88.68(15) 12_666 10_576 ?
O2 Y1 O2 91.32(15) 3_465 11_456 ?
O2 Y1 O2 88.68(15) 12_666 11_456 ?
O2 Y1 O2 88.68(15) 10_576 11_456 ?
O2 Y1 O2 88.68(15) 3_465 . ?
O2 Y1 O2 91.32(15) 12_666 . ?
O2 Y1 O2 180.00(17) 10_576 . ?
O2 Y1 O2 91.32(15) 11_456 . ?
O2 Y1 O2 88.68(15) 3_465 2_675 ?
O2 Y1 O2 91.32(15) 12_666 2_675 ?
O2 Y1 O2 91.32(15) 10_576 2_675 ?
O2 Y1 O2 180.000(1) 11_456 2_675 ?
O2 Y1 O2 88.68(15) . 2_675 ?
O7 Fe1 O6 115.00(16) 3_565 . ?
O7 Fe1 O1 86.14(15) 3_565 . ?
O6 Fe1 O1 158.86(15) . . ?
O7 Fe1 O3 89.65(16) 3_565 16_565 ?
O6 Fe1 O3 80.79(16) . 16_565 ?
O1 Fe1 O3 100.03(15) . 16_565 ?
O7 Fe1 O4 94.10(16) 3_565 . ?
O6 Fe1 O4 85.92(17) . . ?
O1 Fe1 O4 93.13(15) . . ?
O3 Fe1 O4 166.54(16) 16_565 . ?
O7 Fe1 N1 165.03(17) 3_565 . ?
O6 Fe1 N1 77.27(16) . . ?
O1 Fe1 N1 81.90(15) . . ?
O3 Fe1 N1 101.24(17) 16_565 . ?
O4 Fe1 N1 77.68(16) . . ?
O3 Fe2 O3 111.20(12) 2_675 . ?
O3 Fe2 O3 111.20(12) 2_675 3_465 ?
O3 Fe2 O3 111.20(12) . 3_465 ?
O2 P1 O3 114.4(2) . . ?
O2 P1 O1 111.1(2) . . ?
O3 P1 O1 111.4(2) . . ?
O2 P1 C1 110.3(2) . . ?
O3 P1 C1 105.2(2) . . ?
O1 P1 C1 103.6(2) . . ?
N1 C1 P1 111.3(4) . . ?
N1 C1 H1A 109.4 . . ?
P1 C1 H1A 109.4 . . ?
N1 C1 H1B 109.4 . . ?
P1 C1 H1B 109.4 . . ?
H1A C1 H1B 108.0 . . ?
N1 C2 C3 114.5(5) . . ?
N1 C2 H2A 108.6 . . ?
C3 C2 H2A 108.6 . . ?
N1 C2 H2B 108.6 . . ?
C3 C2 H2B 108.6 . . ?
H2A C2 H2B 107.6 . . ?
O4 C3 O5 121.3(5) . . ?
O4 C3 C2 123.0(5) . . ?
O5 C3 C2 115.7(5) . . ?
N1 C4 C5 111.9(5) . . ?
N1 C4 H4A 109.2 . . ?
C5 C4 H4A 109.2 . . ?
N1 C4 H4B 109.2 . . ?
C5 C4 H4B 109.2 . . ?
H4A C4 H4B 107.9 . . ?
O7 C5 O6 125.0(5) . . ?
O7 C5 C4 116.1(5) . . ?
O6 C5 C4 118.7(5) . . ?
C2 N1 C4 112.3(5) . . ?
C2 N1 C1 110.6(4) . . ?
C4 N1 C1 111.7(4) . . ?
C2 N1 Fe1 109.3(3) . . ?
C4 N1 Fe1 105.7(3) . . ?
C1 N1 Fe1 107.0(3) . . ?
P1 O1 Fe1 119.7(2) . . ?
P1 O2 Y1 165.5(3) . . ?
P1 O3 Fe1 132.1(2) . 16_565 ?
P1 O3 Fe2 132.1(3) . . ?
Fe1 O3 Fe2 94.82(17) 16_565 . ?
C3 O4 Fe1 114.9(4) . . ?
C3 O5 H5 109.5 . . ?
C5 O6 Fe1 116.9(4) . . ?
C5 O7 Fe1 119.4(4) . 2_665 ?
H8A O8 H8B 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
O2 P1 C1 N1 -82.9(4) . . . . ?
O3 P1 C1 N1 153.2(4) . . . . ?
O1 P1 C1 N1 36.1(4) . . . . ?
N1 C2 C3 O4 0.5(8) . . . . ?
N1 C2 C3 O5 -178.9(5) . . . . ?
N1 C4 C5 O7 167.9(5) . . . . ?
N1 C4 C5 O6 -16.9(8) . . . . ?
C3 C2 N1 C4 111.2(5) . . . . ?
C3 C2 N1 C1 -123.4(5) . . . . ?
C3 C2 N1 Fe1 -5.8(6) . . . . ?
C5 C4 N1 C2 -89.0(6) . . . . ?
C5 C4 N1 C1 146.1(5) . . . . ?
C5 C4 N1 Fe1 30.1(5) . . . . ?
P1 C1 N1 C2 75.0(5) . . . . ?
P1 C1 N1 C4 -159.2(4) . . . . ?
P1 C1 N1 Fe1 -44.0(4) . . . . ?
O7 Fe1 N1 C2 -51.6(8) 3_565 . . . ?
O6 Fe1 N1 C2 94.7(4) . . . . ?
O1 Fe1 N1 C2 -88.8(4) . . . . ?
O3 Fe1 N1 C2 172.5(3) 16_565 . . . ?
O4 Fe1 N1 C2 6.2(3) . . . . ?
O7 Fe1 N1 C4 -172.6(6) 3_565 . . . ?
O6 Fe1 N1 C4 -26.3(4) . . . . ?
O1 Fe1 N1 C4 150.1(4) . . . . ?
O3 Fe1 N1 C4 51.4(4) 16_565 . . . ?
O4 Fe1 N1 C4 -114.9(4) . . . . ?
O7 Fe1 N1 C1 68.2(8) 3_565 . . . ?
O6 Fe1 N1 C1 -145.5(4) . . . . ?
O1 Fe1 N1 C1 31.0(3) . . . . ?
O3 Fe1 N1 C1 -67.7(3) 16_565 . . . ?
O4 Fe1 N1 C1 126.0(3) . . . . ?
O2 P1 O1 Fe1 109.0(3) . . . . ?
O3 P1 O1 Fe1 -122.1(2) . . . . ?
C1 P1 O1 Fe1 -9.5(3) . . . . ?
O7 Fe1 O1 P1 179.1(3) 3_565 . . . ?
O6 Fe1 O1 P1 -0.3(6) . . . . ?
O3 Fe1 O1 P1 90.1(2) 16_565 . . . ?
O4 Fe1 O1 P1 -87.0(2) . . . . ?
N1 Fe1 O1 P1 -10.0(2) . . . . ?
O3 P1 O2 Y1 -23.8(11) . . . . ?
O1 P1 O2 Y1 103.5(10) . . . . ?
C1 P1 O2 Y1 -142.1(10) . . . . ?
O2 Y1 O2 P1 69.5(10) 3_465 . . . ?
O2 Y1 O2 P1 -110.5(10) 12_666 . . . ?
O2 Y1 O2 P1 -69(9) 10_576 . . . ?
O2 Y1 O2 P1 160.8(10) 11_456 . . . ?
O2 Y1 O2 P1 -19.2(10) 2_675 . . . ?
O2 P1 O3 Fe1 -171.6(3) . . . 16_565 ?
O1 P1 O3 Fe1 61.2(4) . . . 16_565 ?
C1 P1 O3 Fe1 -50.4(4) . . . 16_565 ?
O2 P1 O3 Fe2 -6.0(4) . . . . ?
O1 P1 O3 Fe2 -133.1(3) . . . . ?
C1 P1 O3 Fe2 115.2(3) . . . . ?
O3 Fe2 O3 P1 70.2(3) 2_675 . . . ?
O3 Fe2 O3 P1 -54.3(3) 3_465 . . . ?
O3 Fe2 O3 Fe1 -120.4(2) 2_675 . . 16_565 ?
O3 Fe2 O3 Fe1 115.1(2) 3_465 . . 16_565 ?
O5 C3 O4 Fe1 -175.3(4) . . . . ?
C2 C3 O4 Fe1 5.4(7) . . . . ?
O7 Fe1 O4 C3 160.9(4) 3_565 . . . ?
O6 Fe1 O4 C3 -84.3(4) . . . . ?
O1 Fe1 O4 C3 74.6(4) . . . . ?
O3 Fe1 O4 C3 -93.3(8) 16_565 . . . ?
N1 Fe1 O4 C3 -6.4(4) . . . . ?
O7 C5 O6 Fe1 166.4(5) . . . . ?
C4 C5 O6 Fe1 -8.4(7) . . . . ?
O7 Fe1 O6 C5 -169.0(4) 3_565 . . . ?
O1 Fe1 O6 C5 10.2(7) . . . . ?
O3 Fe1 O6 C5 -83.8(4) 16_565 . . . ?
O4 Fe1 O6 C5 98.3(4) . . . . ?
N1 Fe1 O6 C5 20.0(4) . . . . ?
O6 C5 O7 Fe1 -11.7(8) . . . 2_665 ?
C4 C5 O7 Fe1 163.3(4) . . . 2_665 ?

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 H5 O1 0.82 1.82 2.559(5) 148.9 11_456
O8 H8A O8 0.84 2.44 3.25(13) 160.0 10_577

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.99
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         1.052
_refine_diff_density_min         -0.825
_refine_diff_density_rms         0.146
