# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2014

data_publication_text
_journal_name_full               Dalton
_journal_coden_Cambridge         ?

_publ_contact_author_name        'Prof. Maria Laura Mercuri'
_publ_contact_author_address     
;
Dipartimento di Scienze Chimiche e Geologiche, 
Universita' degli Studi di Cagliari, Cagliari, Italy
;
_publ_contact_author_phone       '0039 070 6754486'
_publ_contact_author_fax         '0039 070 6754456'

_publ_contact_author_email       mercuri@unipr.it

_publ_section_title              
;
Halogen-Bonding in a New Family of tris(haloanilato)metallate(III)
Magnetic Molecular Building Blocks

;


#BEGIN

data_feca510

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 Cl6 O12 Fe 3-, 3(C6 H16 N 1+), 2(O H2)'
_chemical_formula_sum            'C36 H50 Cl6 Fe N3 O14'
_chemical_formula_weight         1019.36

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Pbcn

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

_cell_length_a                   26.340(6)
_cell_length_b                   16.510(4)
_cell_length_c                   10.564(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4594(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    16354
_cell_measurement_theta_min      1.46
_cell_measurement_theta_max      27.08

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.13
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.474
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2116
_exptl_absorpt_coefficient_mu    0.742
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.398
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   SADABS

_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  'Bruker Smart 1000 CCD'
_diffrn_measurement_method       'theta & omega scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        none
_diffrn_reflns_number            38219
_diffrn_reflns_av_R_equivalents  0.0587
_diffrn_reflns_av_sigmaI/netI    0.0303
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         1.46
_diffrn_reflns_theta_max         27.08
_reflns_number_total             5042
_reflns_number_gt                3690
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       Smart
_computing_cell_refinement       Saint
_computing_data_reduction        Saint
_computing_structure_solution    Sir2004
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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.
 One of the Et3NH+ molecules lies on a binary axis and is disordered in two
 equivalent positions. The H atoms of the water molecule could not be located
 from the difference fourier map.
 
;

_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)+(0.1130P)²+1.5737P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5042
_refine_ls_number_parameters     311
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0784
_refine_ls_R_factor_gt           0.0572
_refine_ls_wR_factor_ref         0.1735
_refine_ls_wR_factor_gt          0.1562
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_restrained_S_all      1.020
_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
Fe Fe 0.0000 0.22007(3) 0.2500 0.03392(19) Uani 1 2 d S . .
Cl22 Cl 0.07442(3) 0.45371(5) 0.01445(8) 0.0463(2) Uani 1 1 d . . .
Cl31 Cl -0.15939(3) 0.19725(8) -0.00870(9) 0.0661(3) Uani 1 1 d . . .
Cl61 Cl -0.10391(5) 0.03246(8) 0.51556(12) 0.0827(4) Uani 1 1 d . . .
O12 O 0.02786(7) 0.31309(12) 0.15011(19) 0.0376(5) Uani 1 1 d . . .
O21 O -0.06180(7) 0.20754(13) 0.1397(2) 0.0386(5) Uani 1 1 d . . .
O11 O -0.04028(8) 0.14145(13) 0.3530(2) 0.0425(5) Uani 1 1 d . . .
O32 O 0.03431(9) 0.59734(14) 0.1574(2) 0.0506(6) Uani 1 1 d . . .
N13 N -0.21803(11) 0.4448(2) 0.2420(3) 0.0499(7) Uani 1 1 d . . .
C22 C 0.03440(11) 0.45514(18) 0.1442(3) 0.0356(6) Uani 1 1 d . . .
C21 C -0.09729(10) 0.16338(17) 0.1852(3) 0.0334(6) Uani 1 1 d . . .
O51 O -0.19986(11) 0.0177(2) 0.3684(3) 0.0745(9) Uani 1 1 d . . .
O41 O -0.22290(9) 0.0876(2) 0.1489(3) 0.0667(8) Uani 1 1 d . . .
C12 C 0.01709(10) 0.38365(17) 0.1925(3) 0.0328(6) Uani 1 1 d . . .
C31 C -0.14380(11) 0.1518(2) 0.1329(3) 0.0404(7) Uani 1 1 d . . .
C11 C -0.08450(11) 0.12448(18) 0.3115(3) 0.0375(6) Uani 1 1 d . . .
C61 C -0.11889(13) 0.0757(2) 0.3717(3) 0.0511(8) Uani 1 1 d . . .
C32 C 0.01940(11) 0.53115(18) 0.1948(3) 0.0366(6) Uani 1 1 d . . .
C41 C -0.18076(11) 0.1011(2) 0.1909(3) 0.0461(8) Uani 1 1 d . . .
C51 C -0.16721(13) 0.0606(2) 0.3193(4) 0.0530(9) Uani 1 1 d . . .
C53 C -0.17348(15) 0.4972(3) 0.2122(4) 0.0681(11) Uani 1 1 d . . .
H53A H -0.1429 0.4647 0.2166 0.082 Uiso 1 1 calc R . .
H53B H -0.1767 0.5169 0.1261 0.082 Uiso 1 1 calc R . .
C33 C -0.21033(16) 0.3949(3) 0.3597(4) 0.0599(9) Uani 1 1 d . . .
H33A H -0.2430 0.3744 0.3877 0.072 Uiso 1 1 calc R . .
H33B H -0.1971 0.4295 0.4261 0.072 Uiso 1 1 calc R . .
C13 C -0.23433(18) 0.3981(3) 0.1292(4) 0.0758(12) Uani 1 1 d . . .
H13A H -0.2067 0.3631 0.1029 0.091 Uiso 1 1 calc R . .
H13B H -0.2412 0.4355 0.0606 0.091 Uiso 1 1 calc R . .
C43 C -0.17456(19) 0.3241(3) 0.3419(5) 0.0810(13) Uani 1 1 d . . .
H43A H -0.1896 0.2855 0.2854 0.122 Uiso 1 1 calc R . .
H43B H -0.1682 0.2989 0.4223 0.122 Uiso 1 1 calc R . .
H43C H -0.1431 0.3431 0.3068 0.122 Uiso 1 1 calc R . .
C63 C -0.16788(18) 0.5679(3) 0.2987(6) 0.0828(14) Uani 1 1 d . . .
H63A H -0.1984 0.5997 0.2967 0.124 Uiso 1 1 calc R . .
H63B H -0.1397 0.6004 0.2718 0.124 Uiso 1 1 calc R . .
H63C H -0.1620 0.5490 0.3834 0.124 Uiso 1 1 calc R . .
C23 C -0.2805(2) 0.3474(4) 0.1514(7) 0.113(2) Uani 1 1 d . . .
H23A H -0.2722 0.3033 0.2067 0.170 Uiso 1 1 calc R . .
H23B H -0.2925 0.3264 0.0721 0.170 Uiso 1 1 calc R . .
H23C H -0.3065 0.3800 0.1895 0.170 Uiso 1 1 calc R . .
O1W O -0.09634(15) 0.3651(2) 0.0708(4) 0.1022(12) Uani 1 1 d . . .
N14 N 0.0000 0.7594(3) 0.2500 0.0434(9) Uani 1 2 d S . .
C44 C 0.0832(8) 0.7530(11) 0.356(2) 0.075(8) Uani 0.50 1 d P A 1
H44A H 0.0872 0.6954 0.3493 0.112 Uiso 0.50 1 calc PR A 1
H44B H 0.1023 0.7726 0.4270 0.112 Uiso 0.50 1 calc PR A 1
H44C H 0.0954 0.7783 0.2798 0.112 Uiso 0.50 1 calc PR A 1
C34 C 0.0257(3) 0.7739(5) 0.3745(6) 0.0518(17) Uani 0.50 1 d P A 1
H34A H 0.0110 0.7397 0.4394 0.062 Uiso 0.50 1 calc PR A 1
H34B H 0.0218 0.8301 0.3998 0.062 Uiso 0.50 1 calc PR A 1
C14 C 0.0206(4) 0.8000(6) 0.1405(7) 0.066(2) Uani 0.50 1 d P A 2
H14A H 0.0001 0.7861 0.0675 0.079 Uiso 0.50 1 calc PR A 2
H14B H 0.0546 0.7796 0.1254 0.079 Uiso 0.50 1 calc PR A 2
C24 C 0.0231(5) 0.8900(7) 0.1507(11) 0.097(4) Uani 0.50 1 d P A 2
H24A H -0.0069 0.9097 0.1919 0.146 Uiso 0.50 1 calc PR A 2
H24B H 0.0255 0.9131 0.0675 0.146 Uiso 0.50 1 calc PR A 2
H24C H 0.0525 0.9051 0.1992 0.146 Uiso 0.50 1 calc PR A 2
C54 C -0.0570(3) 0.7780(4) 0.2730(8) 0.0521(17) Uani 0.50 1 d P A 3
H54A H -0.0617 0.8351 0.2912 0.062 Uiso 0.50 1 calc PR A 3
H54B H -0.0695 0.7470 0.3445 0.062 Uiso 0.50 1 calc PR A 3
C64 C -0.0866(8) 0.7541(17) 0.150(3) 0.104(11) Uani 0.50 1 d P A 3
H64A H -0.0731 0.7839 0.0793 0.157 Uiso 0.50 1 calc PR A 3
H64B H -0.1219 0.7668 0.1600 0.157 Uiso 0.50 1 calc PR A 3
H64C H -0.0827 0.6971 0.1346 0.157 Uiso 0.50 1 calc PR A 3
H14 H 0.0000 0.700(3) 0.2500 0.049(14) Uiso 1 2 d S . .
H13 H -0.2410(16) 0.474(2) 0.256(3) 0.046(10) Uiso 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe O11 1.999(2) . ?
Fe O11 1.999(2) 3 ?
Fe O12 2.003(2) 3 ?
Fe O12 2.003(2) . ?
Fe O21 2.013(2) . ?
Fe O21 2.013(2) 3 ?
Cl22 C22 1.729(3) . ?
Cl31 C31 1.724(3) . ?
Cl61 C61 1.725(4) . ?
O12 C12 1.280(3) . ?
O21 C21 1.279(3) . ?
O11 C11 1.275(3) . ?
O32 C32 1.227(4) . ?
N13 C13 1.482(5) . ?
N13 C53 1.492(5) . ?
N13 C33 1.506(5) . ?
N13 H13 0.79(4) . ?
C22 C12 1.365(4) . ?
C22 C32 1.420(4) . ?
C21 C31 1.357(4) . ?
C21 C11 1.519(4) . ?
O51 C51 1.229(4) . ?
O41 C41 1.216(4) . ?
C12 C12 1.512(6) 3 ?
C31 C41 1.423(5) . ?
C11 C61 1.368(4) . ?
C61 C51 1.410(5) . ?
C32 C32 1.551(6) 3 ?
C41 C51 1.553(5) . ?
C53 C63 1.489(7) . ?
C53 H53A 0.9700 . ?
C53 H53B 0.9700 . ?
C33 C43 1.512(6) . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C13 C23 1.495(8) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C43 H43A 0.9600 . ?
C43 H43B 0.9600 . ?
C43 H43C 0.9600 . ?
C63 H63A 0.9600 . ?
C63 H63B 0.9600 . ?
C63 H63C 0.9600 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
N14 C14 1.443(7) 3 ?
N14 C14 1.443(7) . ?
N14 C34 1.498(7) 3 ?
N14 C34 1.498(7) . ?
N14 C54 1.552(7) . ?
N14 C54 1.552(7) 3 ?
N14 H14 0.98(5) . ?
C44 C34 1.57(2) . ?
C44 H44A 0.9600 . ?
C44 H44B 0.9600 . ?
C44 H44C 0.9600 . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
C14 C24 1.490(14) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C54 C64 1.57(3) . ?
C54 H54A 0.9700 . ?
C54 H54B 0.9700 . ?
C64 H64A 0.9600 . ?
C64 H64B 0.9600 . ?
C64 H64C 0.9600 . ?

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 Fe O11 99.00(13) . 3 ?
O11 Fe O12 90.96(9) . 3 ?
O11 Fe O12 168.36(8) 3 3 ?
O11 Fe O12 168.36(8) . . ?
O11 Fe O12 90.96(9) 3 . ?
O12 Fe O12 79.85(11) 3 . ?
O11 Fe O21 79.58(8) . . ?
O11 Fe O21 92.72(9) 3 . ?
O12 Fe O21 95.03(9) 3 . ?
O12 Fe O21 94.02(8) . . ?
O11 Fe O21 92.72(9) . 3 ?
O11 Fe O21 79.58(8) 3 3 ?
O12 Fe O21 94.02(8) 3 3 ?
O12 Fe O21 95.02(9) . 3 ?
O21 Fe O21 168.20(13) . 3 ?
C12 O12 Fe 115.62(18) . . ?
C21 O21 Fe 115.60(18) . . ?
C11 O11 Fe 116.13(19) . . ?
C13 N13 C53 111.1(3) . . ?
C13 N13 C33 114.7(3) . . ?
C53 N13 C33 112.7(3) . . ?
C13 N13 H13 105(3) . . ?
C53 N13 H13 107(3) . . ?
C33 N13 H13 106(3) . . ?
C12 C22 C32 122.0(3) . . ?
C12 C22 Cl22 119.3(2) . . ?
C32 C22 Cl22 118.7(2) . . ?
O21 C21 C31 126.0(3) . . ?
O21 C21 C11 114.1(2) . . ?
C31 C21 C11 119.9(3) . . ?
O12 C12 C22 125.6(3) . . ?
O12 C12 C12 114.40(15) . 3 ?
C22 C12 C12 119.99(17) . 3 ?
C21 C31 C41 121.7(3) . . ?
C21 C31 Cl31 120.4(2) . . ?
C41 C31 Cl31 117.8(2) . . ?
O11 C11 C61 125.0(3) . . ?
O11 C11 C21 114.3(2) . . ?
C61 C11 C21 120.7(3) . . ?
C11 C61 C51 121.3(3) . . ?
C11 C61 Cl61 120.1(3) . . ?
C51 C61 Cl61 118.6(3) . . ?
O32 C32 C22 125.2(3) . . ?
O32 C32 C32 116.96(18) . 3 ?
C22 C32 C32 117.82(17) . 3 ?
O41 C41 C31 125.2(3) . . ?
O41 C41 C51 116.7(3) . . ?
C31 C41 C51 118.1(3) . . ?
O51 C51 C61 124.6(4) . . ?
O51 C51 C41 117.1(3) . . ?
C61 C51 C41 118.3(3) . . ?
C63 C53 N13 113.8(4) . . ?
C63 C53 H53A 108.8 . . ?
N13 C53 H53A 108.8 . . ?
C63 C53 H53B 108.8 . . ?
N13 C53 H53B 108.8 . . ?
H53A C53 H53B 107.7 . . ?
N13 C33 C43 113.8(3) . . ?
N13 C33 H33A 108.8 . . ?
C43 C33 H33A 108.8 . . ?
N13 C33 H33B 108.8 . . ?
C43 C33 H33B 108.8 . . ?
H33A C33 H33B 107.7 . . ?
N13 C13 C23 113.6(4) . . ?
N13 C13 H13A 108.8 . . ?
C23 C13 H13A 108.8 . . ?
N13 C13 H13B 108.8 . . ?
C23 C13 H13B 108.8 . . ?
H13A C13 H13B 107.7 . . ?
C33 C43 H43A 109.5 . . ?
C33 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C33 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C53 C63 H63A 109.5 . . ?
C53 C63 H63B 109.5 . . ?
H63A C63 H63B 109.5 . . ?
C53 C63 H63C 109.5 . . ?
H63A C63 H63C 109.5 . . ?
H63B C63 H63C 109.5 . . ?
C13 C23 H23A 109.5 . . ?
C13 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C13 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C14 N14 C14 124.6(8) 3 . ?
C14 N14 C34 117.3(5) 3 3 ?
C14 N14 C34 52.6(5) . 3 ?
C14 N14 C34 52.6(5) 3 . ?
C14 N14 C34 117.3(5) . . ?
C34 N14 C34 161.6(7) 3 . ?
C14 N14 C54 54.4(5) 3 . ?
C14 N14 C54 113.5(5) . . ?
C34 N14 C54 70.7(4) 3 . ?
C34 N14 C54 105.6(4) . . ?
C14 N14 C54 113.5(5) 3 3 ?
C14 N14 C54 54.4(5) . 3 ?
C34 N14 C54 105.6(4) 3 3 ?
C34 N14 C54 70.7(4) . 3 ?
C54 N14 C54 157.2(6) . 3 ?
C14 N14 H14 117.7(4) 3 . ?
C14 N14 H14 117.7(4) . . ?
C34 N14 H14 99.2(3) 3 . ?
C34 N14 H14 99.2(3) . . ?
C54 N14 H14 101.4(3) . . ?
C54 N14 H14 101.4(3) 3 . ?
N14 C34 C44 107.0(10) . . ?
N14 C34 H34A 110.3 . . ?
C44 C34 H34A 110.3 . . ?
N14 C34 H34B 110.3 . . ?
C44 C34 H34B 110.3 . . ?
H34A C34 H34B 108.6 . . ?
N14 C14 C24 115.0(8) . . ?
N14 C14 H14A 108.5 . . ?
C24 C14 H14A 108.5 . . ?
N14 C14 H14B 108.5 . . ?
C24 C14 H14B 108.5 . . ?
H14A C14 H14B 107.5 . . ?
C14 C24 H24A 109.5 . . ?
C14 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C14 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
N14 C54 C64 107.5(11) . . ?
N14 C54 H54A 110.2 . . ?
C64 C54 H54A 110.2 . . ?
N14 C54 H54B 110.2 . . ?
C64 C54 H54B 110.2 . . ?
H54A C54 H54B 108.5 . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        27.08
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         1.298
_refine_diff_density_min         -0.941
_refine_diff_density_rms         0.089
_database_code_depnum_ccdc_archive 'CCDC 941114'
data_publication_text
_journal_name_full               Dalton
_journal_coden_Cambridge         ?

_publ_contact_author_name        'Prof. Maria Laura Mercuri'
_publ_contact_author_address     
;
Dipartimento di Scienze Chimiche e Geologiche, 
Universita' degli Studi di Cagliari, Cagliari, Italy
;
_publ_contact_author_phone       '0039 070 6754486'
_publ_contact_author_fax         '0039 070 6754456'

_publ_contact_author_email       mercuri@unipr.it

_publ_section_title              
;
Halogen-Bonding in a New Family of tris(haloanilato)metallate(III)
Magnetic Molecular Building Blocks

;

#END
#BEGIN
data_cra308

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '(C18 O12 Cl6 Cr) 3-, (C18 H48 N3) 3+, H2 O'
_chemical_formula_sum            'C36 H50 Cl6 Cr N3 O13'
_chemical_formula_weight         997.49

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cr Cr 0.3209 0.6236 '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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P21/n

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

_cell_length_a                   16.154(3)
_cell_length_b                   10.575(2)
_cell_length_c                   26.682(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.092(3)
_cell_angle_gamma                90.00
_cell_volume                     4555.0(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    7028
_cell_measurement_theta_min      1.45
_cell_measurement_theta_max      27.58

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.455
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2068
_exptl_absorpt_coefficient_mu    0.665
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.800
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   SADABS

_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  'Bruker Smart 1000 CCD'
_diffrn_measurement_method       'theta & omega scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        none
_diffrn_reflns_number            53418
_diffrn_reflns_av_R_equivalents  0.1443
_diffrn_reflns_av_sigmaI/netI    0.1756
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_theta_min         1.45
_diffrn_reflns_theta_max         27.58
_reflns_number_total             10212
_reflns_number_gt                3600
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       Smart
_computing_cell_refinement       Saint
_computing_data_reduction        saint
_computing_structure_solution    Sir97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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.
 The H atoms of the crystallization water molecule were not included in the mode
 
;

_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)+(0.0467P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         10212
_refine_ls_number_parameters     541
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.2011
_refine_ls_R_factor_gt           0.0834
_refine_ls_wR_factor_ref         0.1743
_refine_ls_wR_factor_gt          0.1515
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_restrained_S_all      1.007
_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
Cr Cr 0.22388(6) 0.23282(9) 0.00949(3) 0.0412(3) Uani 1 1 d . . .
Cl61 Cl 0.44123(10) 0.47733(15) -0.07343(6) 0.0553(5) Uani 1 1 d . . .
Cl32 Cl 0.19944(11) 0.49841(16) 0.16415(6) 0.0618(5) Uani 1 1 d . . .
Cl31 Cl 0.47738(10) 0.01146(16) 0.07723(6) 0.0576(5) Uani 1 1 d . . .
Cl62 Cl 0.03392(12) -0.03187(17) 0.10819(7) 0.0691(6) Uani 1 1 d . . .
Cl63 Cl 0.22584(12) -0.00448(17) -0.15076(6) 0.0705(5) Uani 1 1 d . . .
Cl33 Cl 0.01206(12) 0.47395(18) -0.09052(8) 0.0822(6) Uani 1 1 d . . .
O21 O 0.3218(2) 0.1431(4) 0.03794(14) 0.0418(10) Uani 1 1 d . . .
O51 O 0.5974(3) 0.3463(4) -0.03626(17) 0.0607(13) Uani 1 1 d . . .
O11 O 0.3086(2) 0.3365(3) -0.02073(14) 0.0421(10) Uani 1 1 d . . .
O22 O 0.2156(2) 0.3418(4) 0.06979(14) 0.0418(10) Uani 1 1 d . . .
O13 O 0.2189(3) 0.1274(3) -0.05132(15) 0.0456(11) Uani 1 1 d . . .
O23 O 0.1343(2) 0.3233(4) -0.02673(15) 0.0487(11) Uani 1 1 d . . .
C21 C 0.3921(4) 0.1885(5) 0.0232(2) 0.0387(16) Uani 1 1 d . . .
C11 C 0.3839(4) 0.2978(6) -0.0124(2) 0.0421(16) Uani 1 1 d . . .
O12 O 0.1464(2) 0.1284(4) 0.04730(14) 0.0449(11) Uani 1 1 d . . .
N16 N 0.4350(4) 0.2480(5) -0.2230(2) 0.0592(15) Uani 1 1 d . . .
H16 H 0.4746 0.2670 -0.2452 0.071 Uiso 1 1 calc R . .
C41 C 0.5423(4) 0.1956(6) 0.0191(2) 0.0422(16) Uani 1 1 d . . .
C22 C 0.1682(4) 0.2985(5) 0.1032(2) 0.0392(15) Uani 1 1 d . . .
O42 O 0.0822(3) 0.3440(4) 0.22418(17) 0.0731(15) Uani 1 1 d . . .
C23 C 0.1228(4) 0.2870(6) -0.0740(2) 0.0414(15) Uani 1 1 d . . .
C13 C 0.1736(4) 0.1741(5) -0.0875(2) 0.0374(15) Uani 1 1 d . . .
O41 O 0.6128(3) 0.1621(4) 0.03114(16) 0.0606(13) Uani 1 1 d . . .
C43 C 0.0645(4) 0.3004(6) -0.1588(3) 0.0585(19) Uani 1 1 d . . .
C33 C 0.0698(4) 0.3451(6) -0.1079(2) 0.0527(18) Uani 1 1 d . . .
N14 N 0.5423(3) -0.2545(5) -0.21929(19) 0.0551(15) Uani 1 1 d . . .
H14 H 0.5071 -0.2407 -0.2462 0.066 Uiso 1 1 calc R . .
C31 C 0.4679(4) 0.1414(5) 0.0369(2) 0.0399(15) Uani 1 1 d . . .
C32 C 0.1526(4) 0.3543(5) 0.1484(2) 0.0423(16) Uani 1 1 d . . .
C12 C 0.1273(4) 0.1732(6) 0.0905(2) 0.0407(15) Uani 1 1 d . . .
N15 N 0.2296(3) -0.2621(4) 0.00617(18) 0.0445(13) Uani 1 1 d . . .
H15 H 0.2834 -0.2408 0.0016 0.053 Uiso 1 1 calc R . .
C63 C 0.1682(4) 0.1266(5) -0.1356(2) 0.0444(16) Uani 1 1 d . . .
C51 C 0.5331(4) 0.3049(6) -0.0194(2) 0.0473(17) Uani 1 1 d . . .
O53 O 0.1080(3) 0.1493(5) -0.21714(17) 0.0762(15) Uani 1 1 d . . .
C61 C 0.4524(4) 0.3478(5) -0.0321(2) 0.0410(16) Uani 1 1 d . . .
C55 C 0.2160(4) -0.3856(6) -0.0196(3) 0.069(2) Uani 1 1 d . . .
H55A H 0.1599 -0.4139 -0.0141 0.083 Uiso 1 1 calc R . .
H55B H 0.2537 -0.4477 -0.0047 0.083 Uiso 1 1 calc R . .
C42 C 0.0998(4) 0.2969(6) 0.1838(2) 0.0566(19) Uani 1 1 d . . .
C52 C 0.0597(4) 0.1690(6) 0.1704(2) 0.0520(18) Uani 1 1 d . . .
C14 C 0.5915(4) -0.1342(6) -0.2107(3) 0.064(2) Uani 1 1 d . . .
H14A H 0.6130 -0.1074 -0.2425 0.077 Uiso 1 1 calc R . .
H14B H 0.5542 -0.0687 -0.1998 0.077 Uiso 1 1 calc R . .
C62 C 0.0778(4) 0.1132(6) 0.1237(2) 0.0470(17) Uani 1 1 d . . .
C53 C 0.1158(4) 0.1833(6) -0.1724(2) 0.0501(18) Uani 1 1 d . . .
C46 C 0.5563(6) 0.2893(10) -0.1645(3) 0.126(4) Uani 1 1 d . . .
H46A H 0.5907 0.2875 -0.1931 0.188 Uiso 1 1 calc R . .
H46B H 0.5863 0.2550 -0.1359 0.188 Uiso 1 1 calc R . .
H46C H 0.5408 0.3751 -0.1576 0.188 Uiso 1 1 calc R . .
C34 C 0.4900(5) -0.2873(7) -0.1758(3) 0.076(2) Uani 1 1 d . . .
H34A H 0.5234 -0.2794 -0.1450 0.091 Uiso 1 1 calc R . .
H34B H 0.4726 -0.3748 -0.1789 0.091 Uiso 1 1 calc R . .
C16 C 0.3849(5) 0.3648(7) -0.2184(3) 0.079(2) Uani 1 1 d . . .
H16A H 0.3672 0.3927 -0.2517 0.094 Uiso 1 1 calc R . .
H16B H 0.4196 0.4306 -0.2035 0.094 Uiso 1 1 calc R . .
C44 C 0.4136(4) -0.2037(8) -0.1723(3) 0.090(3) Uani 1 1 d . . .
H44A H 0.4303 -0.1168 -0.1695 0.135 Uiso 1 1 calc R . .
H44B H 0.3837 -0.2270 -0.1432 0.135 Uiso 1 1 calc R . .
H44C H 0.3785 -0.2147 -0.2018 0.135 Uiso 1 1 calc R . .
C35 C 0.2206(4) -0.2753(7) 0.0630(2) 0.066(2) Uani 1 1 d . . .
H35A H 0.1626 -0.2883 0.0698 0.080 Uiso 1 1 calc R . .
H35B H 0.2509 -0.3496 0.0746 0.080 Uiso 1 1 calc R . .
C24 C 0.6627(5) -0.1446(8) -0.1729(3) 0.090(3) Uani 1 1 d . . .
H24A H 0.6439 -0.1834 -0.1428 0.134 Uiso 1 1 calc R . .
H24B H 0.6839 -0.0618 -0.1652 0.134 Uiso 1 1 calc R . .
H24C H 0.7058 -0.1954 -0.1865 0.134 Uiso 1 1 calc R . .
C36 C 0.4814(6) 0.2134(8) -0.1750(3) 0.096(3) Uani 1 1 d . . .
H36A H 0.4445 0.2232 -0.1474 0.115 Uiso 1 1 calc R . .
H36B H 0.4970 0.1250 -0.1766 0.115 Uiso 1 1 calc R . .
C26 C 0.3089(5) 0.3487(9) -0.1871(4) 0.134(4) Uani 1 1 d . . .
H26A H 0.2649 0.3117 -0.2073 0.202 Uiso 1 1 calc R . .
H26B H 0.2917 0.4298 -0.1751 0.202 Uiso 1 1 calc R . .
H26C H 0.3222 0.2944 -0.1591 0.202 Uiso 1 1 calc R . .
C45 C 0.2521(5) -0.1612(7) 0.0922(3) 0.073(2) Uani 1 1 d . . .
H45A H 0.3030 -0.1326 0.0787 0.109 Uiso 1 1 calc R . .
H45B H 0.2615 -0.1840 0.1268 0.109 Uiso 1 1 calc R . .
H45C H 0.2117 -0.0947 0.0897 0.109 Uiso 1 1 calc R . .
C65 C 0.2290(5) -0.3790(8) -0.0757(3) 0.087(3) Uani 1 1 d . . .
H65A H 0.1879 -0.3248 -0.0912 0.131 Uiso 1 1 calc R . .
H65B H 0.2242 -0.4623 -0.0899 0.131 Uiso 1 1 calc R . .
H65C H 0.2832 -0.3459 -0.0814 0.131 Uiso 1 1 calc R . .
C56 C 0.3892(6) 0.1340(8) -0.2449(4) 0.110(3) Uani 1 1 d . . .
H56A H 0.4280 0.0644 -0.2477 0.132 Uiso 1 1 calc R . .
H56B H 0.3471 0.1081 -0.2220 0.132 Uiso 1 1 calc R . .
C66 C 0.3493(7) 0.1593(10) -0.2951(4) 0.158(5) Uani 1 1 d . . .
H66A H 0.3070 0.2223 -0.2920 0.237 Uiso 1 1 calc R . .
H66B H 0.3250 0.0827 -0.3082 0.237 Uiso 1 1 calc R . .
H66C H 0.3902 0.1891 -0.3175 0.237 Uiso 1 1 calc R . .
C64 C 0.6511(5) -0.3383(8) -0.2758(3) 0.103(3) Uani 1 1 d . . .
H64A H 0.6191 -0.2998 -0.3027 0.155 Uiso 1 1 calc R . .
H64B H 0.6744 -0.4162 -0.2872 0.155 Uiso 1 1 calc R . .
H64C H 0.6949 -0.2822 -0.2650 0.155 Uiso 1 1 calc R . .
C15 C 0.1795(5) -0.1581(7) -0.0149(3) 0.082(3) Uani 1 1 d . . .
H15A H 0.1975 -0.1405 -0.0484 0.098 Uiso 1 1 calc R . .
H15B H 0.1901 -0.0831 0.0052 0.098 Uiso 1 1 calc R . .
C25 C 0.0862(6) -0.1824(9) -0.0175(3) 0.119(4) Uani 1 1 d . . .
H25A H 0.0582 -0.1098 -0.0316 0.178 Uiso 1 1 calc R . .
H25B H 0.0672 -0.1976 0.0156 0.178 Uiso 1 1 calc R . .
H25C H 0.0745 -0.2549 -0.0383 0.178 Uiso 1 1 calc R . .
C54 C 0.5953(5) -0.3649(7) -0.2320(3) 0.076(2) Uani 1 1 d . . .
H54A H 0.5601 -0.4367 -0.2403 0.091 Uiso 1 1 calc R . .
H54B H 0.6296 -0.3875 -0.2027 0.091 Uiso 1 1 calc R . .
O52 O 0.0157(3) 0.1206(4) 0.20146(18) 0.0775(16) Uani 1 1 d . . .
O43 O 0.0217(3) 0.3536(5) -0.19185(18) 0.0812(17) Uani 1 1 d . . .
O1W O 0.3743(4) 0.4327(6) 0.1000(2) 0.125(2) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cr O11 1.951(4) . ?
Cr O23 1.959(4) . ?
Cr O13 1.968(4) . ?
Cr O21 1.972(4) . ?
Cr O12 1.974(4) . ?
Cr O22 1.987(4) . ?
Cl61 C61 1.763(6) . ?
Cl32 C32 1.745(6) . ?
Cl31 C31 1.748(6) . ?
Cl62 C62 1.733(6) . ?
Cl63 C63 1.726(6) . ?
Cl33 C33 1.724(7) . ?
O21 C21 1.307(6) . ?
O51 C51 1.228(7) . ?
O11 C11 1.296(6) . ?
O22 C22 1.280(6) . ?
O13 C13 1.288(6) . ?
O23 C23 1.324(6) . ?
C21 C31 1.360(8) . ?
C21 C11 1.498(8) . ?
C11 C61 1.350(8) . ?
O12 C12 1.295(6) . ?
N16 C16 1.484(8) . ?
N16 C36 1.503(9) . ?
N16 C56 1.520(10) . ?
N16 H16 0.9100 . ?
C41 O41 1.223(7) . ?
C41 C31 1.428(8) . ?
C41 C51 1.551(8) . ?
C22 C32 1.376(8) . ?
C22 C12 1.514(8) . ?
O42 C42 1.230(7) . ?
C23 C33 1.369(8) . ?
C23 C13 1.500(8) . ?
C13 C63 1.378(8) . ?
C43 O43 1.236(7) . ?
C43 C33 1.437(9) . ?
C43 C53 1.541(9) . ?
N14 C54 1.495(8) . ?
N14 C34 1.500(8) . ?
N14 C14 1.513(8) . ?
N14 H14 0.9100 . ?
C32 C42 1.430(8) . ?
C12 C62 1.370(8) . ?
N15 C15 1.465(8) . ?
N15 C55 1.489(7) . ?
N15 C35 1.534(7) . ?
N15 H15 0.9100 . ?
C63 C53 1.407(8) . ?
C51 C61 1.410(8) . ?
O53 C53 1.250(7) . ?
C55 C65 1.521(9) . ?
C55 H55A 0.9700 . ?
C55 H55B 0.9700 . ?
C42 C52 1.537(9) . ?
C52 O52 1.224(7) . ?
C52 C62 1.419(8) . ?
C14 C24 1.507(9) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C46 C36 1.471(11) . ?
C46 H46A 0.9600 . ?
C46 H46B 0.9600 . ?
C46 H46C 0.9600 . ?
C34 C44 1.525(9) . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
C16 C26 1.520(9) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C44 H44A 0.9600 . ?
C44 H44B 0.9600 . ?
C44 H44C 0.9600 . ?
C35 C45 1.515(9) . ?
C35 H35A 0.9700 . ?
C35 H35B 0.9700 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C36 H36A 0.9700 . ?
C36 H36B 0.9700 . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C45 H45A 0.9600 . ?
C45 H45B 0.9600 . ?
C45 H45C 0.9600 . ?
C65 H65A 0.9600 . ?
C65 H65B 0.9600 . ?
C65 H65C 0.9600 . ?
C56 C66 1.491(11) . ?
C56 H56A 0.9700 . ?
C56 H56B 0.9700 . ?
C66 H66A 0.9600 . ?
C66 H66B 0.9600 . ?
C66 H66C 0.9600 . ?
C64 C54 1.528(10) . ?
C64 H64A 0.9600 . ?
C64 H64B 0.9600 . ?
C64 H64C 0.9600 . ?
C15 C25 1.528(10) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C54 H54A 0.9700 . ?
C54 H54B 0.9700 . ?

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 Cr O23 92.17(17) . . ?
O11 Cr O13 89.19(16) . . ?
O23 Cr O13 82.11(17) . . ?
O11 Cr O21 82.24(17) . . ?
O23 Cr O21 172.67(17) . . ?
O13 Cr O21 93.03(16) . . ?
O11 Cr O12 173.31(17) . . ?
O23 Cr O12 93.15(17) . . ?
O13 Cr O12 95.56(16) . . ?
O21 Cr O12 92.78(17) . . ?
O11 Cr O22 94.44(16) . . ?
O23 Cr O22 92.65(16) . . ?
O13 Cr O22 173.74(17) . . ?
O21 Cr O22 92.52(16) . . ?
O12 Cr O22 81.27(16) . . ?
C21 O21 Cr 113.6(4) . . ?
C11 O11 Cr 114.8(4) . . ?
C22 O22 Cr 114.5(4) . . ?
C13 O13 Cr 113.9(4) . . ?
C23 O23 Cr 113.8(4) . . ?
O21 C21 C31 124.6(6) . . ?
O21 C21 C11 114.6(6) . . ?
C31 C21 C11 120.7(6) . . ?
O11 C11 C61 125.9(6) . . ?
O11 C11 C21 114.4(6) . . ?
C61 C11 C21 119.6(6) . . ?
C12 O12 Cr 115.2(4) . . ?
C16 N16 C36 112.9(6) . . ?
C16 N16 C56 115.6(6) . . ?
C36 N16 C56 110.7(6) . . ?
C16 N16 H16 105.6 . . ?
C36 N16 H16 105.6 . . ?
C56 N16 H16 105.6 . . ?
O41 C41 C31 125.7(6) . . ?
O41 C41 C51 117.1(6) . . ?
C31 C41 C51 117.2(6) . . ?
O22 C22 C32 126.2(6) . . ?
O22 C22 C12 115.2(5) . . ?
C32 C22 C12 118.6(6) . . ?
O23 C23 C33 124.3(6) . . ?
O23 C23 C13 113.6(5) . . ?
C33 C23 C13 122.2(6) . . ?
O13 C13 C63 124.9(6) . . ?
O13 C13 C23 115.2(5) . . ?
C63 C13 C23 119.8(6) . . ?
O43 C43 C33 122.5(7) . . ?
O43 C43 C53 119.4(6) . . ?
C33 C43 C53 118.2(6) . . ?
C23 C33 C43 119.5(6) . . ?
C23 C33 Cl33 120.5(5) . . ?
C43 C33 Cl33 120.0(5) . . ?
C54 N14 C34 109.8(5) . . ?
C54 N14 C14 112.8(5) . . ?
C34 N14 C14 112.6(5) . . ?
C54 N14 H14 107.1 . . ?
C34 N14 H14 107.1 . . ?
C14 N14 H14 107.1 . . ?
C21 C31 C41 121.6(6) . . ?
C21 C31 Cl31 120.7(5) . . ?
C41 C31 Cl31 117.7(5) . . ?
C22 C32 C42 122.0(6) . . ?
C22 C32 Cl32 119.6(5) . . ?
C42 C32 Cl32 118.4(5) . . ?
O12 C12 C62 124.7(6) . . ?
O12 C12 C22 113.7(5) . . ?
C62 C12 C22 121.5(6) . . ?
C15 N15 C55 114.3(5) . . ?
C15 N15 C35 112.1(5) . . ?
C55 N15 C35 111.0(5) . . ?
C15 N15 H15 106.3 . . ?
C55 N15 H15 106.3 . . ?
C35 N15 H15 106.3 . . ?
C13 C63 C53 120.7(6) . . ?
C13 C63 Cl63 119.7(5) . . ?
C53 C63 Cl63 119.6(5) . . ?
O51 C51 C61 125.7(6) . . ?
O51 C51 C41 116.5(6) . . ?
C61 C51 C41 117.7(6) . . ?
C11 C61 C51 122.9(6) . . ?
C11 C61 Cl61 118.8(5) . . ?
C51 C61 Cl61 118.2(5) . . ?
N15 C55 C65 113.0(6) . . ?
N15 C55 H55A 109.0 . . ?
C65 C55 H55A 109.0 . . ?
N15 C55 H55B 109.0 . . ?
C65 C55 H55B 109.0 . . ?
H55A C55 H55B 107.8 . . ?
O42 C42 C32 124.7(7) . . ?
O42 C42 C52 116.8(6) . . ?
C32 C42 C52 118.5(6) . . ?
O52 C52 C62 124.4(6) . . ?
O52 C52 C42 117.4(6) . . ?
C62 C52 C42 118.2(6) . . ?
C24 C14 N14 115.1(6) . . ?
C24 C14 H14A 108.5 . . ?
N14 C14 H14A 108.5 . . ?
C24 C14 H14B 108.5 . . ?
N14 C14 H14B 108.5 . . ?
H14A C14 H14B 107.5 . . ?
C12 C62 C52 121.2(6) . . ?
C12 C62 Cl62 120.0(5) . . ?
C52 C62 Cl62 118.8(5) . . ?
O53 C53 C63 125.5(6) . . ?
O53 C53 C43 114.8(6) . . ?
C63 C53 C43 119.6(6) . . ?
C36 C46 H46A 109.5 . . ?
C36 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C36 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
N14 C34 C44 113.2(6) . . ?
N14 C34 H34A 108.9 . . ?
C44 C34 H34A 108.9 . . ?
N14 C34 H34B 108.9 . . ?
C44 C34 H34B 108.9 . . ?
H34A C34 H34B 107.8 . . ?
N16 C16 C26 113.9(6) . . ?
N16 C16 H16A 108.8 . . ?
C26 C16 H16A 108.8 . . ?
N16 C16 H16B 108.8 . . ?
C26 C16 H16B 108.8 . . ?
H16A C16 H16B 107.7 . . ?
C34 C44 H44A 109.5 . . ?
C34 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C34 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C45 C35 N15 113.2(5) . . ?
C45 C35 H35A 108.9 . . ?
N15 C35 H35A 108.9 . . ?
C45 C35 H35B 108.9 . . ?
N15 C35 H35B 108.9 . . ?
H35A C35 H35B 107.8 . . ?
C14 C24 H24A 109.5 . . ?
C14 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C14 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C46 C36 N16 114.2(7) . . ?
C46 C36 H36A 108.7 . . ?
N16 C36 H36A 108.7 . . ?
C46 C36 H36B 108.7 . . ?
N16 C36 H36B 108.7 . . ?
H36A C36 H36B 107.6 . . ?
C16 C26 H26A 109.5 . . ?
C16 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C16 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C35 C45 H45A 109.5 . . ?
C35 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C35 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C55 C65 H65A 109.5 . . ?
C55 C65 H65B 109.5 . . ?
H65A C65 H65B 109.5 . . ?
C55 C65 H65C 109.5 . . ?
H65A C65 H65C 109.5 . . ?
H65B C65 H65C 109.5 . . ?
C66 C56 N16 113.1(7) . . ?
C66 C56 H56A 109.0 . . ?
N16 C56 H56A 109.0 . . ?
C66 C56 H56B 109.0 . . ?
N16 C56 H56B 109.0 . . ?
H56A C56 H56B 107.8 . . ?
C56 C66 H66A 109.5 . . ?
C56 C66 H66B 109.5 . . ?
H66A C66 H66B 109.5 . . ?
C56 C66 H66C 109.5 . . ?
H66A C66 H66C 109.5 . . ?
H66B C66 H66C 109.5 . . ?
C54 C64 H64A 109.5 . . ?
C54 C64 H64B 109.5 . . ?
H64A C64 H64B 109.5 . . ?
C54 C64 H64C 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
N15 C15 C25 115.0(7) . . ?
N15 C15 H15A 108.5 . . ?
C25 C15 H15A 108.5 . . ?
N15 C15 H15B 108.5 . . ?
C25 C15 H15B 108.5 . . ?
H15A C15 H15B 107.5 . . ?
C15 C25 H25A 109.5 . . ?
C15 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C15 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
N14 C54 C64 112.8(6) . . ?
N14 C54 H54A 109.0 . . ?
C64 C54 H54A 109.0 . . ?
N14 C54 H54B 109.0 . . ?
C64 C54 H54B 109.0 . . ?
H54A C54 H54B 107.8 . . ?

_diffrn_measured_fraction_theta_max 0.969
_diffrn_reflns_theta_full        27.58
_diffrn_measured_fraction_theta_full 0.969
_refine_diff_density_max         0.886
_refine_diff_density_min         -0.385
_refine_diff_density_rms         0.092
_database_code_depnum_ccdc_archive 'CCDC 941115'
data_publication_text
_journal_name_full               Dalton
_journal_coden_Cambridge         ?

_publ_contact_author_name        'Prof. Maria Laura Mercuri'
_publ_contact_author_address     
;
Dipartimento di Scienze Chimiche e Geologiche, 
Universita' degli Studi di Cagliari, Cagliari, Italy
;
_publ_contact_author_phone       '0039 070 6754486'
_publ_contact_author_fax         '0039 070 6754456'

_publ_contact_author_email       mercuri@unipr.it

_publ_section_title              
;
Halogen-Bonding in a New Family of tris(haloanilato)metallate(III)
Magnetic Molecular Building Blocks

;

#END
#BEGIN

data_cria511

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C18 Cr I6 O12 3-, 3(N C16 H36 1+)'
_chemical_formula_sum            'C66 H108 Cr I6 N3 O12'
_chemical_formula_weight         1948.95

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Pbca

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

_cell_length_a                   24.339(1)
_cell_length_b                   20.262(1)
_cell_length_c                   32.155(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     15857.5(14)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    48438
_cell_measurement_theta_min      1.45
_cell_measurement_theta_max      24.00

_exptl_crystal_description       plate
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.633
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             7704
_exptl_absorpt_coefficient_mu    2.534
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.787
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   SADABS

_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  'Bruker Smart APEXII CCD'
_diffrn_measurement_method       'theta & omega scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        none
_diffrn_reflns_number            152710
_diffrn_reflns_av_R_equivalents  0.1185
_diffrn_reflns_av_sigmaI/netI    0.0575
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_theta_min         1.45
_diffrn_reflns_theta_max         24.00
_reflns_number_total             12407
_reflns_number_gt                7959
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       Smart
_computing_cell_refinement       Saint
_computing_data_reduction        Saint
_computing_structure_solution    Sir2004
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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.
 The crystal was affected by non-merohedral twinning. The major component could
 be isolated from the minor components (two or more) by inspecting the
 reciprocal lattice. Since the minor components minimally contributed to the
 overall diffraction, they were neglected during the data reduction.
 Two peripheral residues of two distinct NBu4+ cations were disordered in two
 positions that were refined with 0.60/0.40 and 0.67/0.33 site occupancy factors
 respectively.
 
;

_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)+(0.0659P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         12407
_refine_ls_number_parameters     825
_refine_ls_number_restraints     20
_refine_ls_R_factor_all          0.1069
_refine_ls_R_factor_gt           0.0570
_refine_ls_wR_factor_ref         0.1416
_refine_ls_wR_factor_gt          0.1206
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_restrained_S_all      1.072
_refine_ls_shift/su_max          0.003
_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
I31 I 0.29231(2) 0.69118(3) -0.270804(19) 0.0767(2) Uani 1 1 d . . .
I61 I 0.35311(3) 0.59125(3) -0.474884(18) 0.0737(2) Uani 1 1 d . . .
I62 I 0.31583(2) 0.34446(3) -0.27444(2) 0.0792(2) Uani 1 1 d . . .
I32 I 0.53743(3) 0.51527(3) -0.18533(2) 0.0817(2) Uani 1 1 d . . .
I63 I 0.56927(3) 0.35879(4) -0.40288(2) 0.0968(3) Uani 1 1 d . . .
I33 I 0.59067(3) 0.70235(4) -0.38107(3) 0.1121(3) Uani 1 1 d . . .
Cr Cr 0.44316(4) 0.53254(5) -0.33151(4) 0.0435(3) Uani 1 1 d . . .
O23 O 0.49968(19) 0.5948(2) -0.35034(15) 0.0523(12) Uani 1 1 d . . .
O12 O 0.39704(18) 0.4607(2) -0.30888(16) 0.0489(12) Uani 1 1 d . . .
O11 O 0.40226(18) 0.5487(2) -0.38332(14) 0.0462(12) Uani 1 1 d . . .
O21 O 0.39031(18) 0.5980(2) -0.31018(14) 0.0455(12) Uani 1 1 d . . .
O13 O 0.4936(2) 0.4698(2) -0.35835(15) 0.0505(12) Uani 1 1 d . . .
O22 O 0.47798(18) 0.5230(2) -0.27649(15) 0.0495(12) Uani 1 1 d . . .
O51 O 0.2709(3) 0.6967(3) -0.4362(2) 0.101(2) Uani 1 1 d . . .
N15 N 0.3284(2) 0.3673(3) -0.4349(2) 0.0603(18) Uani 1 1 d . . .
C32 C 0.4692(3) 0.4709(4) -0.2115(2) 0.0522(19) Uani 1 1 d . . .
O52 O 0.3694(3) 0.3466(3) -0.18429(19) 0.0862(18) Uani 1 1 d . . .
C22 C 0.4544(3) 0.4825(3) -0.2517(2) 0.0432(17) Uani 1 1 d . . .
O42 O 0.4470(3) 0.4185(3) -0.1484(2) 0.093(2) Uani 1 1 d . . .
C42 C 0.4387(3) 0.4268(4) -0.1856(3) 0.061(2) Uani 1 1 d . . .
C21 C 0.3565(3) 0.6208(3) -0.3377(2) 0.0468(18) Uani 1 1 d . . .
C23 C 0.5391(3) 0.5690(4) -0.3713(2) 0.0492(19) Uani 1 1 d . . .
O41 O 0.2484(3) 0.7350(3) -0.3591(2) 0.099(2) Uani 1 1 d . . .
C13 C 0.5354(3) 0.4957(4) -0.3760(2) 0.0491(19) Uani 1 1 d . . .
O43 O 0.6637(3) 0.5965(4) -0.4283(2) 0.119(3) Uani 1 1 d . . .
C14 C 0.5359(3) 0.7405(4) -0.2482(3) 0.069(2) Uani 1 1 d . . .
H14A H 0.5490 0.7485 -0.2201 0.083 Uiso 1 1 calc R . .
H14B H 0.5519 0.7742 -0.2659 0.083 Uiso 1 1 calc R . .
N14 N 0.4739(3) 0.7490(3) -0.2485(2) 0.0583(17) Uani 1 1 d . . .
C11 C 0.3663(3) 0.5958(4) -0.3811(2) 0.0473(18) Uani 1 1 d . . .
C61 C 0.3380(3) 0.6211(4) -0.4138(2) 0.055(2) Uani 1 1 d . . .
C31 C 0.3140(3) 0.6641(4) -0.3302(2) 0.0516(19) Uani 1 1 d . . .
N16 N 0.3187(3) 0.4073(4) -0.0660(2) 0.0664(19) Uani 1 1 d . . .
C41 C 0.2846(3) 0.6935(4) -0.3632(3) 0.065(2) Uani 1 1 d . . .
O53 O 0.6567(3) 0.4643(4) -0.4359(2) 0.110(3) Uani 1 1 d . . .
C62 C 0.3788(3) 0.3989(3) -0.2478(2) 0.0512(19) Uani 1 1 d . . .
C54 C 0.4626(3) 0.8182(4) -0.2311(3) 0.063(2) Uani 1 1 d . . .
H54A H 0.4803 0.8220 -0.2042 0.076 Uiso 1 1 calc R . .
H54B H 0.4792 0.8505 -0.2494 0.076 Uiso 1 1 calc R . .
C12 C 0.4064(3) 0.4453(3) -0.2708(2) 0.0440(17) Uani 1 1 d . . .
C15 C 0.3106(3) 0.4260(4) -0.4094(3) 0.063(2) Uani 1 1 d . . .
H15A H 0.3416 0.4393 -0.3923 0.076 Uiso 1 1 calc R . .
H15B H 0.3031 0.4620 -0.4284 0.076 Uiso 1 1 calc R . .
C33 C 0.5831(3) 0.6020(4) -0.3879(3) 0.067(2) Uani 1 1 d . . .
C135 C 0.3698(3) 0.3892(4) -0.4667(3) 0.073(2) Uani 1 1 d D . .
H13A H 0.3754 0.3531 -0.4861 0.088 Uiso 1 1 calc R . .
H13B H 0.3540 0.4256 -0.4823 0.088 Uiso 1 1 calc R . .
C74 C 0.3960(4) 0.9076(4) -0.2147(3) 0.071(2) Uani 1 1 d . . .
H74A H 0.4203 0.9181 -0.1918 0.086 Uiso 1 1 calc R . .
H74B H 0.4066 0.9346 -0.2383 0.086 Uiso 1 1 calc R . .
C65 C 0.2484(4) 0.3806(5) -0.4861(3) 0.095(3) Uani 1 1 d D . .
H65A H 0.2744 0.4087 -0.5005 0.114 Uiso 1 1 calc R A .
H65B H 0.2256 0.4091 -0.4691 0.114 Uiso 1 1 calc R . .
C51 C 0.2970(4) 0.6696(4) -0.4087(3) 0.069(2) Uani 1 1 d . . .
C104 C 0.4680(5) 0.7943(5) -0.3238(3) 0.094(3) Uani 1 1 d . . .
H10A H 0.5075 0.7929 -0.3278 0.112 Uiso 1 1 calc R . .
H10B H 0.4584 0.8375 -0.3132 0.112 Uiso 1 1 calc R . .
C16 C 0.3739(4) 0.3795(6) -0.0660(3) 0.096(3) Uani 1 1 d D B .
H16A H 0.3723 0.3387 -0.0502 0.115 Uiso 1 1 calc R . .
H16B H 0.3824 0.3675 -0.0945 0.115 Uiso 1 1 calc R . .
C94 C 0.4517(4) 0.7430(4) -0.2931(3) 0.075(3) Uani 1 1 d . . .
H94A H 0.4629 0.7004 -0.3039 0.090 Uiso 1 1 calc R . .
H94B H 0.4118 0.7426 -0.2915 0.090 Uiso 1 1 calc R . .
C64 C 0.4030(3) 0.8347(4) -0.2262(3) 0.072(2) Uani 1 1 d . . .
H64A H 0.3871 0.8073 -0.2046 0.087 Uiso 1 1 calc R . .
H64B H 0.3838 0.8256 -0.2520 0.087 Uiso 1 1 calc R . .
C53 C 0.6195(4) 0.4927(5) -0.4163(3) 0.075(3) Uani 1 1 d . . .
C95 C 0.3517(4) 0.3164(5) -0.4054(3) 0.091(3) Uani 1 1 d D . .
H95A H 0.3814 0.3370 -0.3900 0.109 Uiso 1 1 calc R . .
H95B H 0.3233 0.3053 -0.3854 0.109 Uiso 1 1 calc R . .
C52 C 0.3916(4) 0.3879(4) -0.2055(3) 0.062(2) Uani 1 1 d . . .
C144 C 0.4609(4) 0.6928(4) -0.1789(3) 0.076(3) Uani 1 1 d . . .
H14C H 0.4593 0.7364 -0.1666 0.091 Uiso 1 1 calc R . .
H14D H 0.4981 0.6764 -0.1761 0.091 Uiso 1 1 calc R . .
C156 C 0.2786(5) 0.5482(6) -0.1446(5) 0.125(5) Uani 1 1 d . . .
H15C H 0.2446 0.5727 -0.1479 0.149 Uiso 1 1 calc R . .
H15D H 0.3055 0.5787 -0.1333 0.149 Uiso 1 1 calc R . .
C63 C 0.5740(3) 0.4607(4) -0.3969(2) 0.064(2) Uani 1 1 d . . .
C34 C 0.6184(4) 0.6717(5) -0.2605(3) 0.090(3) Uani 1 1 d . . .
H34A H 0.6302 0.6802 -0.2322 0.108 Uiso 1 1 calc R . .
H34B H 0.6331 0.7065 -0.2780 0.108 Uiso 1 1 calc R . .
C56 C 0.2741(5) 0.3579(6) -0.0754(3) 0.116(4) Uani 1 1 d D . .
H56A H 0.2747 0.3246 -0.0537 0.139 Uiso 1 1 calc R . .
H56B H 0.2391 0.3805 -0.0734 0.139 Uiso 1 1 calc R . .
C145 C 0.4233(4) 0.4099(5) -0.4515(3) 0.092(3) Uani 1 1 d D . .
H14E H 0.4381 0.3763 -0.4332 0.110 Uiso 1 1 calc R . .
H14F H 0.4195 0.4504 -0.4357 0.110 Uiso 1 1 calc R . .
C24 C 0.5572(3) 0.6735(4) -0.2624(3) 0.068(2) Uani 1 1 d . . .
H24A H 0.5423 0.6392 -0.2446 0.081 Uiso 1 1 calc R . .
H24B H 0.5452 0.6650 -0.2906 0.081 Uiso 1 1 calc R . .
C43 C 0.6243(4) 0.5683(6) -0.4115(3) 0.081(3) Uani 1 1 d . . .
C166 C 0.2973(5) 0.5296(6) -0.1860(5) 0.136(5) Uani 1 1 d . . .
H16C H 0.3345 0.5142 -0.1845 0.204 Uiso 1 1 calc R . .
H16D H 0.2954 0.5672 -0.2041 0.204 Uiso 1 1 calc R . .
H16E H 0.2742 0.4951 -0.1967 0.204 Uiso 1 1 calc R . .
C25 C 0.2616(3) 0.4188(5) -0.3812(3) 0.080(3) Uani 1 1 d . . .
H25A H 0.2660 0.3797 -0.3641 0.096 Uiso 1 1 calc R . .
H25B H 0.2287 0.4133 -0.3979 0.096 Uiso 1 1 calc R . .
C26 C 0.4199(5) 0.4165(8) -0.0504(4) 0.159(6) Uani 1 1 d D . .
H26A H 0.4107 0.4379 -0.0244 0.191 Uiso 1 1 calc R B .
H26B H 0.4313 0.4498 -0.0703 0.191 Uiso 1 1 calc R . .
C155 C 0.4641(5) 0.4215(8) -0.4889(4) 0.142(6) Uani 1 1 d D . .
H15E H 0.4469 0.4522 -0.5080 0.170 Uiso 1 1 calc R . .
H15F H 0.4967 0.4429 -0.4780 0.170 Uiso 1 1 calc R . .
C35 C 0.2553(4) 0.4790(5) -0.3535(3) 0.090(3) Uani 1 1 d . . .
H35A H 0.2531 0.5180 -0.3708 0.109 Uiso 1 1 calc R . .
H35B H 0.2879 0.4831 -0.3362 0.109 Uiso 1 1 calc R . .
C84 C 0.3373(4) 0.9242(5) -0.2026(4) 0.100(3) Uani 1 1 d . . .
H84A H 0.3130 0.9128 -0.2249 0.150 Uiso 1 1 calc R . .
H84B H 0.3345 0.9706 -0.1969 0.150 Uiso 1 1 calc R . .
H84C H 0.3273 0.8996 -0.1781 0.150 Uiso 1 1 calc R . .
C154 C 0.4208(4) 0.6462(5) -0.1560(3) 0.100(3) Uani 1 1 d . . .
H15G H 0.3838 0.6639 -0.1580 0.120 Uiso 1 1 calc R . .
H15H H 0.4211 0.6034 -0.1694 0.120 Uiso 1 1 calc R . .
C134 C 0.4456(3) 0.6966(4) -0.2240(3) 0.066(2) Uani 1 1 d . . .
H13C H 0.4535 0.6543 -0.2368 0.079 Uiso 1 1 calc R . .
H13D H 0.4063 0.7038 -0.2260 0.079 Uiso 1 1 calc R . .
C44 C 0.6418(4) 0.6053(5) -0.2749(3) 0.099(3) Uani 1 1 d . . .
H44A H 0.6810 0.6055 -0.2718 0.148 Uiso 1 1 calc R . .
H44B H 0.6326 0.5982 -0.3036 0.148 Uiso 1 1 calc R . .
H44C H 0.6264 0.5705 -0.2583 0.148 Uiso 1 1 calc R . .
C126 C 0.3627(6) 0.4835(8) 0.0610(5) 0.167(6) Uani 1 1 d . . .
H12A H 0.3956 0.4574 0.0600 0.250 Uiso 1 1 calc R . .
H12B H 0.3594 0.5037 0.0879 0.250 Uiso 1 1 calc R . .
H12C H 0.3643 0.5172 0.0400 0.250 Uiso 1 1 calc R . .
C96 C 0.3046(4) 0.4387(7) -0.0247(3) 0.109(4) Uani 1 1 d D . .
H96A H 0.3267 0.4783 -0.0216 0.131 Uiso 1 1 calc R . .
H96B H 0.2664 0.4523 -0.0256 0.131 Uiso 1 1 calc R . .
C114 C 0.4396(6) 0.7833(7) -0.3653(4) 0.127(4) Uani 1 1 d D . .
H11A H 0.4631 0.7988 -0.3876 0.152 Uiso 1 1 calc R . .
H11B H 0.4331 0.7366 -0.3693 0.152 Uiso 1 1 calc R . .
C66 C 0.2760(5) 0.3243(6) -0.1153(4) 0.130(4) Uani 1 1 d D . .
H66A H 0.3122 0.3052 -0.1190 0.156 Uiso 1 1 calc R . .
H66B H 0.2704 0.3564 -0.1373 0.156 Uiso 1 1 calc R . .
C116 C 0.3146(7) 0.4409(8) 0.0533(4) 0.151(6) Uani 1 1 d . . .
H11C H 0.2822 0.4688 0.0537 0.181 Uiso 1 1 calc R . .
H11D H 0.3115 0.4108 0.0767 0.181 Uiso 1 1 calc R . .
C106 C 0.3126(5) 0.3979(7) 0.0118(4) 0.140(5) Uani 1 1 d D . .
H10C H 0.3467 0.3735 0.0090 0.168 Uiso 1 1 calc R . .
H10D H 0.2828 0.3662 0.0138 0.168 Uiso 1 1 calc R . .
C55 C 0.2798(4) 0.3374(5) -0.4579(3) 0.085(3) Uani 1 1 d . . .
H55A H 0.2933 0.3003 -0.4740 0.102 Uiso 1 1 calc R . .
H55B H 0.2546 0.3200 -0.4374 0.102 Uiso 1 1 calc R . .
C146 C 0.2685(5) 0.4947(7) -0.1119(5) 0.143(5) Uani 1 1 d D . .
H14G H 0.2536 0.5150 -0.0870 0.172 Uiso 1 1 calc R . .
H14H H 0.2415 0.4638 -0.1224 0.172 Uiso 1 1 calc R . .
C86 C 0.2347(6) 0.2417(7) -0.1622(5) 0.142(5) Uani 1 1 d . . .
H86A H 0.2318 0.2769 -0.1820 0.214 Uiso 1 1 calc R . .
H86B H 0.2050 0.2112 -0.1662 0.214 Uiso 1 1 calc R . .
H86C H 0.2691 0.2191 -0.1661 0.214 Uiso 1 1 calc R . .
C124 C 0.3869(8) 0.8191(9) -0.3664(7) 0.257(12) Uani 1 1 d D . .
H12D H 0.3663 0.8095 -0.3416 0.386 Uiso 1 1 calc R . .
H12E H 0.3662 0.8055 -0.3903 0.386 Uiso 1 1 calc R . .
H12F H 0.3937 0.8657 -0.3679 0.386 Uiso 1 1 calc R . .
C76 C 0.2323(5) 0.2691(6) -0.1194(4) 0.118(4) Uani 1 1 d . . .
H76A H 0.2396 0.2345 -0.0992 0.141 Uiso 1 1 calc R . .
H76B H 0.1961 0.2869 -0.1139 0.141 Uiso 1 1 calc R . .
C115 C 0.4123(6) 0.2161(9) -0.3947(7) 0.222(11) Uani 1 1 d D . .
H11E H 0.4316 0.1825 -0.4105 0.266 Uiso 1 1 calc R . .
H11F H 0.4392 0.2460 -0.3828 0.266 Uiso 1 1 calc R . .
C45 C 0.2048(5) 0.4764(7) -0.3254(4) 0.142(5) Uani 1 1 d . . .
H45A H 0.1740 0.4957 -0.3396 0.212 Uiso 1 1 calc R . .
H45B H 0.2119 0.5005 -0.3003 0.212 Uiso 1 1 calc R . .
H45C H 0.1966 0.4313 -0.3186 0.212 Uiso 1 1 calc R . .
C105 C 0.3729(5) 0.2542(6) -0.4232(5) 0.148(5) Uani 1 1 d D . .
H10E H 0.3918 0.2641 -0.4490 0.178 Uiso 1 1 calc R . .
H10F H 0.3419 0.2259 -0.4299 0.178 Uiso 1 1 calc R . .
C136 C 0.3170(5) 0.4599(5) -0.1013(4) 0.115(4) Uani 1 1 d D . .
H13E H 0.3446 0.4928 -0.0945 0.138 Uiso 1 1 calc R . .
H13F H 0.3295 0.4381 -0.1265 0.138 Uiso 1 1 calc R . .
C164 C 0.4358(6) 0.6377(7) -0.1100(4) 0.160(6) Uani 1 1 d . . .
H16F H 0.4732 0.6232 -0.1078 0.241 Uiso 1 1 calc R . .
H16G H 0.4120 0.6055 -0.0976 0.241 Uiso 1 1 calc R . .
H16H H 0.4316 0.6791 -0.0959 0.241 Uiso 1 1 calc R . .
C165 C 0.4821(6) 0.3626(9) -0.5132(5) 0.171(7) Uani 1 1 d D . .
H16I H 0.5014 0.3327 -0.4953 0.256 Uiso 1 1 calc R . .
H16J H 0.5060 0.3763 -0.5354 0.256 Uiso 1 1 calc R . .
H16K H 0.4505 0.3408 -0.5247 0.256 Uiso 1 1 calc R . .
C125 C 0.3803(6) 0.1854(9) -0.3618(5) 0.192(7) Uani 1 1 d D . .
H12G H 0.3759 0.2161 -0.3393 0.287 Uiso 1 1 calc R . .
H12H H 0.3991 0.1468 -0.3520 0.287 Uiso 1 1 calc R . .
H12I H 0.3449 0.1733 -0.3724 0.287 Uiso 1 1 calc R . .
C85A C 0.1680(14) 0.3096(19) -0.4986(11) 0.23(2) Uani 0.61 1 d PD A -1
H85A H 0.1846 0.2806 -0.4785 0.349 Uiso 0.61 1 calc PR A -1
H85B H 0.1488 0.2839 -0.5190 0.349 Uiso 0.61 1 calc PR A -1
H85C H 0.1426 0.3385 -0.4848 0.349 Uiso 0.61 1 calc PR A -1
C75A C 0.2111(10) 0.3491(16) -0.5191(7) 0.157(12) Uani 0.61 1 d PD A -1
H75A H 0.1943 0.3833 -0.5360 0.188 Uiso 0.61 1 calc PR A -1
H75B H 0.2328 0.3211 -0.5373 0.188 Uiso 0.61 1 calc PR A -1
C75B C 0.1994(13) 0.3338(18) -0.4958(9) 0.135(18) Uani 0.39 1 d PD A -2
H75C H 0.2132 0.2905 -0.5036 0.162 Uiso 0.39 1 calc PR A -2
H75D H 0.1766 0.3288 -0.4713 0.162 Uiso 0.39 1 calc PR A -2
C85B C 0.1664(15) 0.362(2) -0.5304(11) 0.17(2) Uani 0.39 1 d PD A -2
H85D H 0.1362 0.3328 -0.5364 0.260 Uiso 0.39 1 calc PR A -2
H85E H 0.1891 0.3662 -0.5546 0.260 Uiso 0.39 1 calc PR A -2
H85F H 0.1526 0.4043 -0.5224 0.260 Uiso 0.39 1 calc PR A -2
C36B C 0.4660(9) 0.3648(13) -0.0439(14) 0.228(10) Uani 0.67 1 d PD B -3
H36A H 0.4536 0.3304 -0.0251 0.274 Uiso 0.67 1 calc PR B -3
H36B H 0.4759 0.3447 -0.0702 0.274 Uiso 0.67 1 calc PR B -3
C46B C 0.5152(8) 0.4008(16) -0.0255(9) 0.228(10) Uani 0.67 1 d PD B -3
H46A H 0.5358 0.4213 -0.0474 0.343 Uiso 0.67 1 calc PR B -3
H46B H 0.5381 0.3698 -0.0111 0.343 Uiso 0.67 1 calc PR B -3
H46C H 0.5026 0.4339 -0.0064 0.343 Uiso 0.67 1 calc PR B -3
C36A C 0.4772(11) 0.385(3) -0.050(2) 0.228(10) Uani 0.33 1 d PD B -4
H36C H 0.5053 0.4188 -0.0458 0.274 Uiso 0.33 1 calc PR B -4
H36D H 0.4845 0.3619 -0.0754 0.274 Uiso 0.33 1 calc PR B -4
C46A C 0.475(2) 0.338(4) -0.0127(18) 0.228(10) Uani 0.33 1 d PD B -4
H46D H 0.4596 0.2967 -0.0214 0.343 Uiso 0.33 1 calc PR B -4
H46E H 0.4530 0.3568 0.0090 0.343 Uiso 0.33 1 calc PR B -4
H46F H 0.5118 0.3308 -0.0025 0.343 Uiso 0.33 1 calc PR B -4


_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
I31 C31 2.058(7) . ?
I61 C61 2.088(7) . ?
I62 C62 2.074(7) . ?
I32 C32 2.068(8) . ?
I63 C63 2.078(9) . ?
I33 C33 2.053(9) . ?
Cr O23 1.962(5) . ?
Cr O13 1.966(5) . ?
Cr O11 1.968(5) . ?
Cr O22 1.971(5) . ?
Cr O21 1.971(4) . ?
Cr O12 1.978(5) . ?
O23 C23 1.284(8) . ?
O12 C12 1.284(8) . ?
O11 C11 1.298(8) . ?
O21 C21 1.292(8) . ?
O13 C13 1.279(8) . ?
O22 C22 1.280(8) . ?
O51 C51 1.222(9) . ?
N15 C135 1.503(10) . ?
N15 C15 1.507(10) . ?
N15 C95 1.512(11) . ?
N15 C55 1.522(10) . ?
C32 C22 1.363(10) . ?
C32 C42 1.428(11) . ?
O52 C52 1.207(9) . ?
C22 C12 1.519(10) . ?
O42 C42 1.225(9) . ?
C42 C52 1.532(12) . ?
C21 C31 1.378(9) . ?
C21 C11 1.505(10) . ?
C23 C33 1.371(10) . ?
C23 C13 1.495(10) . ?
O41 C41 1.226(8) . ?
C13 C63 1.354(10) . ?
O43 C43 1.239(10) . ?
C14 N14 1.519(9) . ?
C14 C24 1.524(11) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
N14 C134 1.490(10) . ?
N14 C54 1.536(9) . ?
N14 C94 1.536(10) . ?
C11 C61 1.356(10) . ?
C61 C51 1.409(11) . ?
C31 C41 1.411(10) . ?
N16 C16 1.456(11) . ?
N16 C56 1.507(13) . ?
N16 C96 1.513(12) . ?
N16 C136 1.557(13) . ?
C41 C51 1.571(12) . ?
O53 C53 1.245(9) . ?
C62 C12 1.371(10) . ?
C62 C52 1.415(11) . ?
C54 C64 1.496(11) . ?
C54 H54A 0.9700 . ?
C54 H54B 0.9700 . ?
C15 C25 1.503(11) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C33 C43 1.431(12) . ?
C135 C145 1.453(10) . ?
C135 H13A 0.9700 . ?
C135 H13B 0.9700 . ?
C74 C84 1.519(12) . ?
C74 C64 1.532(11) . ?
C74 H74A 0.9700 . ?
C74 H74B 0.9700 . ?
C65 C55 1.475(12) . ?
C65 C75A 1.534(16) . ?
C65 C75B 1.554(17) . ?
C65 H65A 0.9700 . ?
C65 H65B 0.9700 . ?
C104 C94 1.489(12) . ?
C104 C114 1.516(14) . ?
C104 H10A 0.9700 . ?
C104 H10B 0.9700 . ?
C16 C26 1.438(12) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C94 H94A 0.9700 . ?
C94 H94B 0.9700 . ?
C64 H64A 0.9700 . ?
C64 H64B 0.9700 . ?
C53 C63 1.428(12) . ?
C53 C43 1.542(13) . ?
C95 C105 1.478(12) . ?
C95 H95A 0.9700 . ?
C95 H95B 0.9700 . ?
C144 C134 1.499(11) . ?
C144 C154 1.545(12) . ?
C144 H14C 0.9700 . ?
C144 H14D 0.9700 . ?
C156 C166 1.455(16) . ?
C156 C146 1.532(16) . ?
C156 H15C 0.9700 . ?
C156 H15D 0.9700 . ?
C34 C24 1.491(11) . ?
C34 C44 1.533(12) . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
C56 C66 1.454(12) . ?
C56 H56A 0.9700 . ?
C56 H56B 0.9700 . ?
C145 C155 1.577(12) . ?
C145 H14E 0.9700 . ?
C145 H14F 0.9700 . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C166 H16C 0.9600 . ?
C166 H16D 0.9600 . ?
C166 H16E 0.9600 . ?
C25 C35 1.520(12) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C26 C36A 1.53(2) . ?
C26 C36B 1.547(18) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C155 C165 1.494(14) . ?
C155 H15E 0.9700 . ?
C155 H15F 0.9700 . ?
C35 C45 1.528(14) . ?
C35 H35A 0.9700 . ?
C35 H35B 0.9700 . ?
C84 H84A 0.9600 . ?
C84 H84B 0.9600 . ?
C84 H84C 0.9600 . ?
C154 C164 1.531(15) . ?
C154 H15G 0.9700 . ?
C154 H15H 0.9700 . ?
C134 H13C 0.9700 . ?
C134 H13D 0.9700 . ?
C44 H44A 0.9600 . ?
C44 H44B 0.9600 . ?
C44 H44C 0.9600 . ?
C126 C116 1.475(17) . ?
C126 H12A 0.9600 . ?
C126 H12B 0.9600 . ?
C126 H12C 0.9600 . ?
C96 C106 1.450(12) . ?
C96 H96A 0.9700 . ?
C96 H96B 0.9700 . ?
C114 C124 1.475(15) . ?
C114 H11A 0.9700 . ?
C114 H11B 0.9700 . ?
C66 C76 1.549(15) . ?
C66 H66A 0.9700 . ?
C66 H66B 0.9700 . ?
C116 C106 1.594(17) . ?
C116 H11C 0.9700 . ?
C116 H11D 0.9700 . ?
C106 H10C 0.9700 . ?
C106 H10D 0.9700 . ?
C55 H55A 0.9700 . ?
C55 H55B 0.9700 . ?
C146 C136 1.417(12) . ?
C146 H14G 0.9700 . ?
C146 H14H 0.9700 . ?
C86 C76 1.487(15) . ?
C86 H86A 0.9600 . ?
C86 H86B 0.9600 . ?
C86 H86C 0.9600 . ?
C124 H12D 0.9600 . ?
C124 H12E 0.9600 . ?
C124 H12F 0.9600 . ?
C76 H76A 0.9700 . ?
C76 H76B 0.9700 . ?
C115 C125 1.452(12) . ?
C115 C105 1.536(17) . ?
C115 H11E 0.9700 . ?
C115 H11F 0.9700 . ?
C45 H45A 0.9600 . ?
C45 H45B 0.9600 . ?
C45 H45C 0.9600 . ?
C105 H10E 0.9700 . ?
C105 H10F 0.9700 . ?
C136 H13E 0.9700 . ?
C136 H13F 0.9700 . ?
C164 H16F 0.9600 . ?
C164 H16G 0.9600 . ?
C164 H16H 0.9600 . ?
C165 H16I 0.9600 . ?
C165 H16J 0.9600 . ?
C165 H16K 0.9600 . ?
C125 H12G 0.9600 . ?
C125 H12H 0.9600 . ?
C125 H12I 0.9600 . ?
C85A C75A 1.477(18) . ?
C85A H85A 0.9600 . ?
C85A H85B 0.9600 . ?
C85A H85C 0.9600 . ?
C75A H75A 0.9700 . ?
C75A H75B 0.9700 . ?
C75B C85B 1.483(19) . ?
C75B H75C 0.9700 . ?
C75B H75D 0.9700 . ?
C85B H85D 0.9600 . ?
C85B H85E 0.9600 . ?
C85B H85F 0.9600 . ?
C36B C46B 1.521(18) . ?
C36B H36A 0.9700 . ?
C36B H36B 0.9700 . ?
C46B H46A 0.9600 . ?
C46B H46B 0.9600 . ?
C46B H46C 0.9600 . ?
C36A C46A 1.53(2) . ?
C36A H36C 0.9700 . ?
C36A H36D 0.9700 . ?
C46A H46D 0.9600 . ?
C46A H46E 0.9600 . ?
C46A H46F 0.9600 . ?

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
O23 Cr O13 81.0(2) . . ?
O23 Cr O11 89.24(19) . . ?
O13 Cr O11 92.9(2) . . ?
O23 Cr O22 92.2(2) . . ?
O13 Cr O22 93.6(2) . . ?
O11 Cr O22 173.5(2) . . ?
O23 Cr O21 97.6(2) . . ?
O13 Cr O21 174.3(2) . . ?
O11 Cr O21 81.52(19) . . ?
O22 Cr O21 91.98(19) . . ?
O23 Cr O12 170.0(2) . . ?
O13 Cr O12 92.3(2) . . ?
O11 Cr O12 98.4(2) . . ?
O22 Cr O12 80.9(2) . . ?
O21 Cr O12 89.85(19) . . ?
C23 O23 Cr 115.1(4) . . ?
C12 O12 Cr 115.4(4) . . ?
C11 O11 Cr 114.7(4) . . ?
C21 O21 Cr 114.7(4) . . ?
C13 O13 Cr 115.2(5) . . ?
C22 O22 Cr 115.4(4) . . ?
C135 N15 C15 109.4(6) . . ?
C135 N15 C95 112.1(6) . . ?
C15 N15 C95 107.7(7) . . ?
C135 N15 C55 107.8(7) . . ?
C15 N15 C55 110.8(6) . . ?
C95 N15 C55 109.0(7) . . ?
C22 C32 C42 121.6(7) . . ?
C22 C32 I32 121.5(6) . . ?
C42 C32 I32 116.8(6) . . ?
O22 C22 C32 125.7(7) . . ?
O22 C22 C12 114.3(6) . . ?
C32 C22 C12 120.0(7) . . ?
O42 C42 C32 124.8(8) . . ?
O42 C42 C52 117.3(8) . . ?
C32 C42 C52 117.9(7) . . ?
O21 C21 C31 125.9(7) . . ?
O21 C21 C11 114.5(6) . . ?
C31 C21 C11 119.5(7) . . ?
O23 C23 C33 126.1(7) . . ?
O23 C23 C13 114.3(6) . . ?
C33 C23 C13 119.5(7) . . ?
O13 C13 C63 123.8(8) . . ?
O13 C13 C23 114.3(6) . . ?
C63 C13 C23 121.9(7) . . ?
N14 C14 C24 115.9(6) . . ?
N14 C14 H14A 108.3 . . ?
C24 C14 H14A 108.3 . . ?
N14 C14 H14B 108.3 . . ?
C24 C14 H14B 108.3 . . ?
H14A C14 H14B 107.4 . . ?
C134 N14 C14 112.0(6) . . ?
C134 N14 C54 111.9(6) . . ?
C14 N14 C54 106.2(6) . . ?
C134 N14 C94 105.9(6) . . ?
C14 N14 C94 110.4(6) . . ?
C54 N14 C94 110.4(6) . . ?
O11 C11 C61 125.3(7) . . ?
O11 C11 C21 113.8(6) . . ?
C61 C11 C21 120.8(7) . . ?
C11 C61 C51 122.1(8) . . ?
C11 C61 I61 122.0(6) . . ?
C51 C61 I61 115.9(6) . . ?
C21 C31 C41 121.4(7) . . ?
C21 C31 I31 121.6(6) . . ?
C41 C31 I31 117.1(5) . . ?
C16 N16 C56 114.1(8) . . ?
C16 N16 C96 111.8(7) . . ?
C56 N16 C96 106.9(8) . . ?
C16 N16 C136 106.9(8) . . ?
C56 N16 C136 106.9(8) . . ?
C96 N16 C136 110.2(8) . . ?
O41 C41 C31 125.0(8) . . ?
O41 C41 C51 116.8(7) . . ?
C31 C41 C51 118.1(7) . . ?
C12 C62 C52 121.3(7) . . ?
C12 C62 I62 120.3(6) . . ?
C52 C62 I62 118.4(6) . . ?
C64 C54 N14 114.6(6) . . ?
C64 C54 H54A 108.6 . . ?
N14 C54 H54A 108.6 . . ?
C64 C54 H54B 108.6 . . ?
N14 C54 H54B 108.6 . . ?
H54A C54 H54B 107.6 . . ?
O12 C12 C62 126.4(7) . . ?
O12 C12 C22 113.7(6) . . ?
C62 C12 C22 119.9(7) . . ?
C25 C15 N15 118.6(7) . . ?
C25 C15 H15A 107.7 . . ?
N15 C15 H15A 107.7 . . ?
C25 C15 H15B 107.7 . . ?
N15 C15 H15B 107.7 . . ?
H15A C15 H15B 107.1 . . ?
C23 C33 C43 121.3(8) . . ?
C23 C33 I33 120.8(6) . . ?
C43 C33 I33 117.9(7) . . ?
C145 C135 N15 117.2(7) . . ?
C145 C135 H13A 108.0 . . ?
N15 C135 H13A 108.0 . . ?
C145 C135 H13B 108.0 . . ?
N15 C135 H13B 108.0 . . ?
H13A C135 H13B 107.2 . . ?
C84 C74 C64 112.4(7) . . ?
C84 C74 H74A 109.1 . . ?
C64 C74 H74A 109.1 . . ?
C84 C74 H74B 109.1 . . ?
C64 C74 H74B 109.1 . . ?
H74A C74 H74B 107.9 . . ?
C55 C65 C75A 119.1(14) . . ?
C55 C65 C75B 99.2(13) . . ?
C75A C65 C75B 32.3(12) . . ?
C55 C65 H65A 107.5 . . ?
C75A C65 H65A 107.5 . . ?
C75B C65 H65A 139.9 . . ?
C55 C65 H65B 107.5 . . ?
C75A C65 H65B 107.6 . . ?
C75B C65 H65B 92.3 . . ?
H65A C65 H65B 107.0 . . ?
O51 C51 C61 126.7(9) . . ?
O51 C51 C41 115.9(7) . . ?
C61 C51 C41 117.4(7) . . ?
C94 C104 C114 111.1(9) . . ?
C94 C104 H10A 109.4 . . ?
C114 C104 H10A 109.4 . . ?
C94 C104 H10B 109.4 . . ?
C114 C104 H10B 109.4 . . ?
H10A C104 H10B 108.0 . . ?
C26 C16 N16 121.2(10) . . ?
C26 C16 H16A 107.0 . . ?
N16 C16 H16A 107.0 . . ?
C26 C16 H16B 107.0 . . ?
N16 C16 H16B 107.0 . . ?
H16A C16 H16B 106.8 . . ?
C104 C94 N14 118.1(7) . . ?
C104 C94 H94A 107.8 . . ?
N14 C94 H94A 107.8 . . ?
C104 C94 H94B 107.8 . . ?
N14 C94 H94B 107.8 . . ?
H94A C94 H94B 107.1 . . ?
C54 C64 C74 110.4(7) . . ?
C54 C64 H64A 109.6 . . ?
C74 C64 H64A 109.6 . . ?
C54 C64 H64B 109.6 . . ?
C74 C64 H64B 109.6 . . ?
H64A C64 H64B 108.1 . . ?
O53 C53 C63 125.2(10) . . ?
O53 C53 C43 117.1(9) . . ?
C63 C53 C43 117.7(8) . . ?
C105 C95 N15 118.0(10) . . ?
C105 C95 H95A 107.8 . . ?
N15 C95 H95A 107.8 . . ?
C105 C95 H95B 107.8 . . ?
N15 C95 H95B 107.8 . . ?
H95A C95 H95B 107.2 . . ?
O52 C52 C62 123.6(9) . . ?
O52 C52 C42 117.2(8) . . ?
C62 C52 C42 119.0(7) . . ?
C134 C144 C154 109.7(8) . . ?
C134 C144 H14C 109.7 . . ?
C154 C144 H14C 109.7 . . ?
C134 C144 H14D 109.7 . . ?
C154 C144 H14D 109.7 . . ?
H14C C144 H14D 108.2 . . ?
C166 C156 C146 119.6(13) . . ?
C166 C156 H15C 107.4 . . ?
C146 C156 H15C 107.4 . . ?
C166 C156 H15D 107.4 . . ?
C146 C156 H15D 107.4 . . ?
H15C C156 H15D 106.9 . . ?
C13 C63 C53 121.1(8) . . ?
C13 C63 I63 121.9(6) . . ?
C53 C63 I63 116.9(6) . . ?
C24 C34 C44 112.3(8) . . ?
C24 C34 H34A 109.1 . . ?
C44 C34 H34A 109.1 . . ?
C24 C34 H34B 109.1 . . ?
C44 C34 H34B 109.1 . . ?
H34A C34 H34B 107.9 . . ?
C66 C56 N16 117.6(10) . . ?
C66 C56 H56A 107.9 . . ?
N16 C56 H56A 107.9 . . ?
C66 C56 H56B 107.9 . . ?
N16 C56 H56B 107.9 . . ?
H56A C56 H56B 107.2 . . ?
C135 C145 C155 110.6(9) . . ?
C135 C145 H14E 109.5 . . ?
C155 C145 H14E 109.5 . . ?
C135 C145 H14F 109.5 . . ?
C155 C145 H14F 109.5 . . ?
H14E C145 H14F 108.1 . . ?
C34 C24 C14 110.5(7) . . ?
C34 C24 H24A 109.6 . . ?
C14 C24 H24A 109.6 . . ?
C34 C24 H24B 109.6 . . ?
C14 C24 H24B 109.6 . . ?
H24A C24 H24B 108.1 . . ?
O43 C43 C33 123.5(10) . . ?
O43 C43 C53 118.2(9) . . ?
C33 C43 C53 118.3(8) . . ?
C156 C166 H16C 109.5 . . ?
C156 C166 H16D 109.5 . . ?
H16C C166 H16D 109.5 . . ?
C156 C166 H16E 109.5 . . ?
H16C C166 H16E 109.5 . . ?
H16D C166 H16E 109.5 . . ?
C15 C25 C35 110.8(8) . . ?
C15 C25 H25A 109.5 . . ?
C35 C25 H25A 109.5 . . ?
C15 C25 H25B 109.5 . . ?
C35 C25 H25B 109.5 . . ?
H25A C25 H25B 108.1 . . ?
C16 C26 C36A 120(3) . . ?
C16 C26 C36B 105.0(14) . . ?
C36A C26 C36B 20(3) . . ?
C16 C26 H26A 110.7 . . ?
C36A C26 H26A 112.5 . . ?
C36B C26 H26A 110.7 . . ?
C16 C26 H26B 110.7 . . ?
C36A C26 H26B 92.1 . . ?
C36B C26 H26B 110.7 . . ?
H26A C26 H26B 108.8 . . ?
C165 C155 C145 117.7(12) . . ?
C165 C155 H15E 107.9 . . ?
C145 C155 H15E 107.9 . . ?
C165 C155 H15F 107.9 . . ?
C145 C155 H15F 107.9 . . ?
H15E C155 H15F 107.2 . . ?
C25 C35 C45 113.6(9) . . ?
C25 C35 H35A 108.8 . . ?
C45 C35 H35A 108.8 . . ?
C25 C35 H35B 108.8 . . ?
C45 C35 H35B 108.8 . . ?
H35A C35 H35B 107.7 . . ?
C74 C84 H84A 109.5 . . ?
C74 C84 H84B 109.5 . . ?
H84A C84 H84B 109.5 . . ?
C74 C84 H84C 109.5 . . ?
H84A C84 H84C 109.5 . . ?
H84B C84 H84C 109.5 . . ?
C164 C154 C144 112.2(9) . . ?
C164 C154 H15G 109.2 . . ?
C144 C154 H15G 109.2 . . ?
C164 C154 H15H 109.2 . . ?
C144 C154 H15H 109.2 . . ?
H15G C154 H15H 107.9 . . ?
N14 C134 C144 115.8(7) . . ?
N14 C134 H13C 108.3 . . ?
C144 C134 H13C 108.3 . . ?
N14 C134 H13D 108.3 . . ?
C144 C134 H13D 108.3 . . ?
H13C C134 H13D 107.4 . . ?
C34 C44 H44A 109.5 . . ?
C34 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C34 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C116 C126 H12A 109.5 . . ?
C116 C126 H12B 109.5 . . ?
H12A C126 H12B 109.5 . . ?
C116 C126 H12C 109.5 . . ?
H12A C126 H12C 109.5 . . ?
H12B C126 H12C 109.5 . . ?
C106 C96 N16 116.2(11) . . ?
C106 C96 H96A 108.2 . . ?
N16 C96 H96A 108.2 . . ?
C106 C96 H96B 108.2 . . ?
N16 C96 H96B 108.2 . . ?
H96A C96 H96B 107.4 . . ?
C124 C114 C104 110.3(13) . . ?
C124 C114 H11A 109.6 . . ?
C104 C114 H11A 109.6 . . ?
C124 C114 H11B 109.6 . . ?
C104 C114 H11B 109.6 . . ?
H11A C114 H11B 108.1 . . ?
C56 C66 C76 113.0(12) . . ?
C56 C66 H66A 109.0 . . ?
C76 C66 H66A 109.0 . . ?
C56 C66 H66B 109.0 . . ?
C76 C66 H66B 109.0 . . ?
H66A C66 H66B 107.8 . . ?
C126 C116 C106 119.0(13) . . ?
C126 C116 H11C 107.6 . . ?
C106 C116 H11C 107.6 . . ?
C126 C116 H11D 107.6 . . ?
C106 C116 H11D 107.6 . . ?
H11C C116 H11D 107.0 . . ?
C96 C106 C116 111.8(12) . . ?
C96 C106 H10C 109.3 . . ?
C116 C106 H10C 109.3 . . ?
C96 C106 H10D 109.3 . . ?
C116 C106 H10D 109.3 . . ?
H10C C106 H10D 107.9 . . ?
C65 C55 N15 117.9(8) . . ?
C65 C55 H55A 107.8 . . ?
N15 C55 H55A 107.8 . . ?
C65 C55 H55B 107.8 . . ?
N15 C55 H55B 107.8 . . ?
H55A C55 H55B 107.2 . . ?
C136 C146 C156 112.5(11) . . ?
C136 C146 H14G 109.1 . . ?
C156 C146 H14G 109.1 . . ?
C136 C146 H14H 109.1 . . ?
C156 C146 H14H 109.1 . . ?
H14G C146 H14H 107.8 . . ?
C76 C86 H86A 109.5 . . ?
C76 C86 H86B 109.5 . . ?
H86A C86 H86B 109.5 . . ?
C76 C86 H86C 109.5 . . ?
H86A C86 H86C 109.5 . . ?
H86B C86 H86C 109.5 . . ?
C114 C124 H12D 109.5 . . ?
C114 C124 H12E 109.5 . . ?
H12D C124 H12E 109.5 . . ?
C114 C124 H12F 109.5 . . ?
H12D C124 H12F 109.5 . . ?
H12E C124 H12F 109.5 . . ?
C86 C76 C66 108.8(11) . . ?
C86 C76 H76A 109.9 . . ?
C66 C76 H76A 109.9 . . ?
C86 C76 H76B 109.9 . . ?
C66 C76 H76B 109.9 . . ?
H76A C76 H76B 108.3 . . ?
C125 C115 C105 108.4(13) . . ?
C125 C115 H11E 110.0 . . ?
C105 C115 H11E 110.0 . . ?
C125 C115 H11F 110.0 . . ?
C105 C115 H11F 110.0 . . ?
H11E C115 H11F 108.4 . . ?
C35 C45 H45A 109.5 . . ?
C35 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C35 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C95 C105 C115 114.4(14) . . ?
C95 C105 H10E 108.6 . . ?
C115 C105 H10E 108.6 . . ?
C95 C105 H10F 108.6 . . ?
C115 C105 H10F 108.6 . . ?
H10E C105 H10F 107.6 . . ?
C146 C136 N16 122.5(11) . . ?
C146 C136 H13E 106.7 . . ?
N16 C136 H13E 106.7 . . ?
C146 C136 H13F 106.7 . . ?
N16 C136 H13F 106.7 . . ?
H13E C136 H13F 106.6 . . ?
C154 C164 H16F 109.5 . . ?
C154 C164 H16G 109.5 . . ?
H16F C164 H16G 109.5 . . ?
C154 C164 H16H 109.5 . . ?
H16F C164 H16H 109.5 . . ?
H16G C164 H16H 109.5 . . ?
C155 C165 H16I 109.5 . . ?
C155 C165 H16J 109.5 . . ?
H16I C165 H16J 109.5 . . ?
C155 C165 H16K 109.5 . . ?
H16I C165 H16K 109.5 . . ?
H16J C165 H16K 109.5 . . ?
C115 C125 H12G 109.5 . . ?
C115 C125 H12H 109.5 . . ?
H12G C125 H12H 109.5 . . ?
C115 C125 H12I 109.5 . . ?
H12G C125 H12I 109.5 . . ?
H12H C125 H12I 109.5 . . ?
C85A C75A C65 110(2) . . ?
C85A C75A H75A 109.7 . . ?
C65 C75A H75A 109.7 . . ?
C85A C75A H75B 109.7 . . ?
C65 C75A H75B 109.7 . . ?
H75A C75A H75B 108.2 . . ?
C85B C75B C65 109(2) . . ?
C85B C75B H75C 109.8 . . ?
C65 C75B H75C 109.8 . . ?
C85B C75B H75D 109.8 . . ?
C65 C75B H75D 109.8 . . ?
H75C C75B H75D 108.2 . . ?
C75B C85B H85D 109.5 . . ?
C75B C85B H85E 109.5 . . ?
H85D C85B H85E 109.5 . . ?
C75B C85B H85F 109.5 . . ?
H85D C85B H85F 109.5 . . ?
H85E C85B H85F 109.5 . . ?
C46B C36B C26 107.4(18) . . ?
C46B C36B H36A 110.2 . . ?
C26 C36B H36A 110.2 . . ?
C46B C36B H36B 110.2 . . ?
C26 C36B H36B 110.2 . . ?
H36A C36B H36B 108.5 . . ?
C26 C36A C46A 104(4) . . ?
C26 C36A H36C 111.0 . . ?
C46A C36A H36C 111.0 . . ?
C26 C36A H36D 111.0 . . ?
C46A C36A H36D 111.0 . . ?
H36C C36A H36D 109.0 . . ?
C36A C46A H46D 109.5 . . ?
C36A C46A H46E 109.5 . . ?
H46D C46A H46E 109.5 . . ?
C36A C46A H46F 109.5 . . ?
H46D C46A H46F 109.5 . . ?
H46E C46A H46F 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        24.00
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.837
_refine_diff_density_min         -0.505
_refine_diff_density_rms         0.085
_database_code_depnum_ccdc_archive 'CCDC 941116'
data_publication_text
_journal_name_full               Dalton
_journal_coden_Cambridge         ?

_publ_contact_author_name        'Prof. Maria Laura Mercuri'
_publ_contact_author_address     
;
Dipartimento di Scienze Chimiche e Geologiche, 
Universita' degli Studi di Cagliari, Cagliari, Italy
;
_publ_contact_author_phone       '0039 070 6754486'
_publ_contact_author_fax         '0039 070 6754456'

_publ_contact_author_email       mercuri@unipr.it

_publ_section_title              
;
Halogen-Bonding in a New Family of tris(haloanilato)metallate(III)
Magnetic Molecular Building Blocks

;

#END
#BEGIN

data_fecai113

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C90 H60 Fe I6 O12 P3, 4(O H2)'
_chemical_formula_sum            'C90 H68 Fe I6 O16 P3'
_chemical_formula_weight         2311.57

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'
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'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   C2/c

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

_cell_length_a                   35.023(5)
_cell_length_b                   12.482(2)
_cell_length_c                   46.347(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 114.467(2)
_cell_angle_gamma                90.00
_cell_volume                     18441(5)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    12328
_cell_measurement_theta_min      1.75
_cell_measurement_theta_max      23.42

_exptl_crystal_description       plate
_exptl_crystal_colour            'dark red'
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.07
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.665
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             8968
_exptl_absorpt_coefficient_mu    2.286
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.721
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   SADABS

_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  'Bruker Smart APEXII CCD'
_diffrn_measurement_method       'theta & omega scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        none
_diffrn_reflns_number            36575
_diffrn_reflns_av_R_equivalents  0.1016
_diffrn_reflns_av_sigmaI/netI    0.1210
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_theta_min         1.75
_diffrn_reflns_theta_max         23.42
_reflns_number_total             13255
_reflns_number_gt                6928
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       Smart
_computing_cell_refinement       Saint
_computing_data_reduction        Saint
_computing_structure_solution    Sir2004
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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.
 The crystal contained water molecules of crystallization. These molecues were
 refined isotropically and their H atoms were not included into the model during
 the refinement. Four water molecules were refined with a site occupancy factor
 of 0.5.
 
;

_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)+(0.0111P)²+460.7010P] 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         13255
_refine_ls_number_parameters     1033
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.1688
_refine_ls_R_factor_gt           0.0894
_refine_ls_wR_factor_ref         0.1792
_refine_ls_wR_factor_gt          0.1518
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_restrained_S_all      1.042
_refine_ls_shift/su_max          0.003
_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
I31 I 0.92954(4) 0.95382(10) 0.48412(3) 0.0717(4) Uani 1 1 d . . .
I61 I 0.86878(4) 1.25788(10) 0.58657(3) 0.0736(4) Uani 1 1 d . . .
I62 I 0.96066(4) 0.45974(10) 0.60708(3) 0.0802(4) Uani 1 1 d . . .
I33 I 0.77035(4) 0.73486(10) 0.54568(3) 0.0811(4) Uani 1 1 d . . .
I32 I 1.08568(4) 0.91658(12) 0.67301(4) 0.0953(5) Uani 1 1 d . . .
I63 I 0.90846(5) 0.87040(14) 0.70253(3) 0.1102(5) Uani 1 1 d . . .
Fe Fe 0.92780(7) 0.86769(18) 0.59577(5) 0.0547(6) Uani 1 1 d . . .
P16 P 0.90949(12) 0.5457(4) 0.43588(10) 0.0569(11) Uani 1 1 d . . .
P15 P 0.76231(13) 1.1076(3) 0.41669(10) 0.0554(11) Uani 1 1 d . . .
P14 P 1.07906(16) 1.3229(4) 0.72691(11) 0.0732(14) Uani 1 1 d . . .
O13 O 0.9173(3) 0.8606(8) 0.6358(2) 0.056(3) Uani 1 1 d . . .
O21 O 0.9275(3) 0.9041(8) 0.5535(2) 0.056(3) Uani 1 1 d . . .
O51 O 0.8534(4) 1.2857(9) 0.5140(3) 0.082(4) Uani 1 1 d . . .
O23 O 0.8671(3) 0.8242(9) 0.5773(2) 0.066(3) Uani 1 1 d . . .
O22 O 0.9894(3) 0.8820(9) 0.6222(2) 0.065(3) Uani 1 1 d . . .
O52 O 1.0599(4) 0.4872(9) 0.6508(3) 0.085(4) Uani 1 1 d . . .
C21 C 0.9158(4) 0.9992(12) 0.5427(3) 0.045(4) Uani 1 1 d . . .
O11 O 0.9138(3) 1.0244(8) 0.5929(2) 0.055(3) Uani 1 1 d . . .
C215 C 0.6465(8) 0.9651(17) 0.3788(8) 0.113(9) Uani 1 1 d . . .
H215 H 0.6271 0.9378 0.3857 0.136 Uiso 1 1 calc R . .
C65 C 0.7487(5) 1.1190(14) 0.4703(4) 0.072(5) Uani 1 1 d . . .
H65 H 0.7281 1.1680 0.4586 0.086 Uiso 1 1 calc R . .
O41 O 0.8841(3) 1.1810(9) 0.4772(3) 0.075(4) Uani 1 1 d . . .
C46 C 0.8699(6) 0.624(2) 0.5158(5) 0.086(6) Uani 1 1 d . . .
H46 H 0.8606 0.6391 0.5315 0.104 Uiso 1 1 calc R . .
C104 C 0.9790(6) 1.0820(18) 0.6696(5) 0.082(6) Uani 1 1 d . . .
H104 H 0.9605 1.0283 0.6582 0.098 Uiso 1 1 calc R . .
C195 C 0.7137(5) 1.0514(13) 0.3897(4) 0.065(5) Uani 1 1 d . . .
C44 C 1.1192(7) 1.2000(19) 0.8267(5) 0.094(7) Uani 1 1 d . . .
H44 H 1.1251 1.1679 0.8462 0.112 Uiso 1 1 calc R . .
C31 C 0.9100(4) 1.0423(13) 0.5138(3) 0.049(4) Uani 1 1 d . . .
O53 O 0.8100(4) 0.8044(12) 0.6696(3) 0.109(5) Uani 1 1 d . . .
O43 O 0.7593(4) 0.7465(10) 0.6113(3) 0.094(4) Uani 1 1 d . . .
C76 C 0.8632(4) 0.5188(13) 0.4002(4) 0.053(4) Uani 1 1 d . . .
C55 C 0.7556(6) 1.0959(14) 0.5006(5) 0.078(5) Uani 1 1 d . . .
H55 H 0.7403 1.1322 0.5098 0.094 Uiso 1 1 calc R . .
C106 C 0.7906(6) 0.478(2) 0.3476(5) 0.106(8) Uani 1 1 d . . .
H106 H 0.7656 0.4610 0.3304 0.127 Uiso 1 1 calc R . .
C63 C 0.8670(5) 0.8366(13) 0.6564(4) 0.064(5) Uani 1 1 d . . .
C105 C 0.7525(6) 1.4760(15) 0.4162(5) 0.082(6) Uani 1 1 d . . .
H105 H 0.7501 1.5502 0.4163 0.098 Uiso 1 1 calc R . .
C52 C 1.0444(5) 0.5771(14) 0.6447(4) 0.065(5) Uani 1 1 d . . .
C96 C 0.7927(7) 0.564(2) 0.3674(5) 0.099(7) Uani 1 1 d . . .
H96 H 0.7699 0.6093 0.3624 0.119 Uiso 1 1 calc R . .
C226 C 0.9798(7) 0.8330(17) 0.4214(7) 0.104(8) Uani 1 1 d . . .
H226 H 0.9950 0.8905 0.4188 0.125 Uiso 1 1 calc R . .
C11 C 0.9047(4) 1.0705(11) 0.5656(4) 0.044(4) Uani 1 1 d . . .
C125 C 0.7253(6) 1.3033(12) 0.3927(4) 0.068(5) Uani 1 1 d . . .
H125 H 0.7041 1.2649 0.3770 0.082 Uiso 1 1 calc R . .
C206 C 0.9669(5) 0.7094(14) 0.4561(5) 0.070(5) Uani 1 1 d . . .
H206 H 0.9723 0.6850 0.4764 0.084 Uiso 1 1 calc R . .
C94 C 0.9878(6) 1.1633(19) 0.6545(5) 0.081(6) Uani 1 1 d . . .
H94 H 0.9734 1.1703 0.6326 0.098 Uiso 1 1 calc R . .
C86 C 0.8276(5) 0.5799(14) 0.3938(4) 0.069(5) Uani 1 1 d . . .
H86 H 0.8280 0.6331 0.4079 0.082 Uiso 1 1 calc R . .
C136 C 0.9441(4) 0.4300(12) 0.4446(4) 0.053(4) Uani 1 1 d . . .
C24 C 1.0770(6) 1.3155(18) 0.7856(5) 0.100(7) Uani 1 1 d . . .
H24 H 1.0541 1.3613 0.7769 0.120 Uiso 1 1 calc R . .
C95 C 0.7867(5) 1.4203(14) 0.4389(4) 0.066(5) Uani 1 1 d . . .
H95 H 0.8078 1.4585 0.4548 0.079 Uiso 1 1 calc R . .
C23 C 0.8503(5) 0.8139(12) 0.5982(4) 0.054(4) Uani 1 1 d . . .
C25 C 0.8022(5) 0.9967(12) 0.4738(4) 0.057(4) Uani 1 1 d . . .
H25 H 0.8185 0.9635 0.4649 0.069 Uiso 1 1 calc R . .
C186 C 0.9841(5) 0.4429(14) 0.4473(3) 0.063(4) Uani 1 1 d . . .
H186 H 0.9944 0.5109 0.4464 0.076 Uiso 1 1 calc R . .
C33 C 0.8106(5) 0.7833(12) 0.5915(4) 0.061(4) Uani 1 1 d . . .
C15 C 0.7730(4) 1.0683(12) 0.4569(4) 0.052(4) Uani 1 1 d . . .
C35 C 0.8082(5) 0.9721(13) 0.5045(4) 0.064(5) Uani 1 1 d . . .
H35 H 0.8286 0.9221 0.5159 0.077 Uiso 1 1 calc R . .
O12 O 0.9441(3) 0.7140(8) 0.5973(2) 0.058(3) Uani 1 1 d . . .
C246 C 0.9266(5) 0.7002(14) 0.3992(4) 0.073(5) Uani 1 1 d . . .
H246 H 0.9055 0.6681 0.3817 0.088 Uiso 1 1 calc R . .
C74 C 1.0389(5) 1.2302(13) 0.7056(4) 0.067(5) Uani 1 1 d . . .
C61 C 0.8853(5) 1.1666(13) 0.5568(4) 0.054(4) Uani 1 1 d . . .
C32 C 1.0501(5) 0.7824(14) 0.6510(4) 0.059(4) Uani 1 1 d . . .
C165 C 0.8633(6) 0.9840(16) 0.3859(4) 0.085(6) Uani 1 1 d . . .
H165 H 0.8842 0.9586 0.3802 0.102 Uiso 1 1 calc R . .
C16 C 0.8954(4) 0.5751(13) 0.4684(4) 0.055(4) Uani 1 1 d . . .
C115 C 0.7228(6) 1.4117(16) 0.3937(5) 0.085(6) Uani 1 1 d . . .
H115 H 0.6995 1.4449 0.3782 0.102 Uiso 1 1 calc R . .
C22 C 1.0096(5) 0.7922(12) 0.6303(4) 0.051(4) Uani 1 1 d . . .
C175 C 0.8375(7) 0.9160(15) 0.3916(4) 0.089(6) Uani 1 1 d . . .
H175 H 0.8404 0.8431 0.3890 0.107 Uiso 1 1 calc R . .
C176 C 1.0092(6) 0.3531(18) 0.4515(4) 0.083(6) Uani 1 1 d . . .
H176 H 1.0366 0.3614 0.4536 0.100 Uiso 1 1 calc R . .
C75 C 0.7586(5) 1.2506(12) 0.4147(4) 0.052(4) Uani 1 1 d . . .
C204 C 1.0164(8) 1.475(2) 0.7049(6) 0.104(7) Uani 1 1 d . . .
H204 H 0.9976 1.4215 0.6940 0.125 Uiso 1 1 calc R . .
C134 C 1.1176(6) 1.3128(17) 0.7121(4) 0.080(6) Uani 1 1 d . . .
C245 C 0.7060(6) 1.0451(18) 0.3576(5) 0.100(7) Uani 1 1 d . . .
H245 H 0.7255 1.0709 0.3505 0.120 Uiso 1 1 calc R . .
C84 C 1.0190(5) 1.2382(16) 0.6717(4) 0.069(5) Uani 1 1 d . . .
H84 H 1.0266 1.2921 0.6613 0.082 Uiso 1 1 calc R . .
C51 C 0.8738(5) 1.2074(11) 0.5251(4) 0.049(4) Uani 1 1 d . . .
C145 C 0.8296(5) 1.1323(14) 0.3996(4) 0.070(5) Uani 1 1 d . . .
H145 H 0.8281 1.2054 0.4029 0.084 Uiso 1 1 calc R . .
C26 C 0.8980(5) 0.4956(13) 0.4903(4) 0.068(5) Uani 1 1 d . . .
H26 H 0.9076 0.4270 0.4891 0.081 Uiso 1 1 calc R . .
C166 C 0.9941(6) 0.2516(17) 0.4526(4) 0.083(6) Uani 1 1 d . . .
H166 H 1.0106 0.1913 0.4545 0.100 Uiso 1 1 calc R . .
C85 C 0.7895(6) 1.3104(14) 0.4381(4) 0.069(5) Uani 1 1 d . . .
H85 H 0.8125 1.2757 0.4534 0.082 Uiso 1 1 calc R . .
C135 C 0.8025(4) 1.0599(13) 0.4057(3) 0.051(4) Uani 1 1 d . . .
C12 C 0.9836(5) 0.6929(12) 0.6169(4) 0.050(4) Uani 1 1 d . . .
C146 C 0.9267(5) 0.3291(14) 0.4455(4) 0.067(5) Uani 1 1 d . . .
H146 H 0.8991 0.3207 0.4429 0.081 Uiso 1 1 calc R . .
C114 C 0.9979(6) 1.0784(15) 0.7027(6) 0.093(6) Uani 1 1 d . . .
H114 H 0.9890 1.0260 0.7128 0.111 Uiso 1 1 calc R . .
C185 C 0.8066(5) 0.9491(15) 0.4014(4) 0.078(5) Uani 1 1 d . . .
H185 H 0.7892 0.8996 0.4050 0.093 Uiso 1 1 calc R . .
C155 C 0.8581(6) 1.0940(17) 0.3888(5) 0.099(7) Uani 1 1 d . . .
H155 H 0.8742 1.1422 0.3834 0.119 Uiso 1 1 calc R . .
C156 C 0.9543(6) 0.2421(15) 0.4507(4) 0.087(6) Uani 1 1 d . . .
H156 H 0.9449 0.1743 0.4530 0.105 Uiso 1 1 calc R . .
O42 O 1.1073(4) 0.6622(11) 0.6770(3) 0.099(4) Uani 1 1 d . . .
C225 C 0.6397(7) 0.965(2) 0.3473(8) 0.118(10) Uani 1 1 d . . .
H225 H 0.6141 0.9396 0.3325 0.142 Uiso 1 1 calc R . .
C45 C 0.7849(6) 1.0193(14) 0.5184(4) 0.071(5) Uani 1 1 d . . .
H45 H 0.7885 1.0013 0.5388 0.086 Uiso 1 1 calc R . .
C43 C 0.7946(5) 0.7793(13) 0.6154(4) 0.066(5) Uani 1 1 d . . .
C126 C 0.8624(6) 0.4358(15) 0.3801(5) 0.085(6) Uani 1 1 d . . .
H126 H 0.8859 0.3932 0.3844 0.102 Uiso 1 1 calc R . .
C205 C 0.6844(6) 1.0091(13) 0.3994(5) 0.075(5) Uani 1 1 d . . .
H205 H 0.6905 1.0103 0.4209 0.090 Uiso 1 1 calc R . .
C196 C 0.9362(5) 0.6608(11) 0.4293(4) 0.052(4) Uani 1 1 d . . .
C13 C 0.8800(5) 0.8411(12) 0.6319(4) 0.054(4) Uani 1 1 d . . .
C62 C 0.9993(5) 0.5917(12) 0.6246(4) 0.057(4) Uani 1 1 d . . .
C236 C 0.9482(6) 0.7868(15) 0.3949(5) 0.080(6) Uani 1 1 d . . .
H236 H 0.9418 0.8137 0.3747 0.096 Uiso 1 1 calc R . .
C41 C 0.8906(4) 1.1420(12) 0.5030(4) 0.054(4) Uani 1 1 d . . .
C216 C 0.9889(6) 0.7948(17) 0.4516(6) 0.092(7) Uani 1 1 d . . .
H216 H 1.0101 0.8268 0.4690 0.111 Uiso 1 1 calc R . .
C56 C 0.8678(6) 0.700(2) 0.4953(5) 0.103(7) Uani 1 1 d . . .
H56 H 0.8586 0.7689 0.4972 0.124 Uiso 1 1 calc R . .
C194 C 1.0573(8) 1.4532(18) 0.7229(5) 0.088(6) Uani 1 1 d . . .
C66 C 0.8798(5) 0.6757(14) 0.4703(5) 0.081(6) Uani 1 1 d . . .
H66 H 0.8772 0.7273 0.4551 0.098 Uiso 1 1 calc R . .
C53 C 0.8258(6) 0.8086(14) 0.6496(4) 0.073(5) Uani 1 1 d . . .
C36 C 0.8852(6) 0.5246(19) 0.5146(4) 0.085(6) Uani 1 1 d . . .
H36 H 0.8873 0.4745 0.5301 0.102 Uiso 1 1 calc R . .
C116 C 0.8263(7) 0.418(2) 0.3539(5) 0.141(11) Uani 1 1 d . . .
H116 H 0.8256 0.3645 0.3398 0.170 Uiso 1 1 calc R . .
C42 C 1.0706(6) 0.6791(16) 0.6591(4) 0.073(5) Uani 1 1 d . . .
C124 C 1.0275(6) 1.1448(16) 0.7205(4) 0.088(6) Uani 1 1 d . . .
H124 H 1.0407 1.1357 0.7423 0.106 Uiso 1 1 calc R . .
C235 C 0.6683(9) 0.999(2) 0.3365(5) 0.135(11) Uani 1 1 d . . .
H235 H 0.6628 0.9919 0.3152 0.162 Uiso 1 1 calc R . .
C244 C 1.0848(8) 1.536(3) 0.7386(6) 0.126(9) Uani 1 1 d . . .
H244 H 1.1127 1.5210 0.7516 0.151 Uiso 1 1 calc R . .
C214 C 1.0032(8) 1.583(3) 0.7034(6) 0.131(9) Uani 1 1 d . . .
H214 H 0.9750 1.5980 0.6913 0.157 Uiso 1 1 calc R . .
C164 C 1.1816(10) 1.281(3) 0.6926(7) 0.160(10) Uani 1 1 d U . .
H164 H 1.2044 1.2733 0.6873 0.192 Uiso 1 1 calc R . .
C184 C 1.1249(6) 1.216(2) 0.7019(5) 0.132(9) Uani 1 1 d U . .
H184 H 1.1069 1.1595 0.7006 0.159 Uiso 1 1 calc R . .
C34 C 1.0897(7) 1.278(2) 0.8161(6) 0.110(8) Uani 1 1 d . . .
H34 H 1.0781 1.3053 0.8293 0.132 Uiso 1 1 calc R . .
C54 C 1.1401(7) 1.168(2) 0.8095(5) 0.115(8) Uani 1 1 d . . .
H54 H 1.1617 1.1187 0.8178 0.138 Uiso 1 1 calc R . .
C64 C 1.1296(6) 1.2092(19) 0.7796(5) 0.097(7) Uani 1 1 d . . .
H64 H 1.1433 1.1857 0.7674 0.116 Uiso 1 1 calc R . .
C14 C 1.0992(5) 1.2836(15) 0.7683(4) 0.071(5) Uani 1 1 d . . .
C144 C 1.1397(8) 1.396(3) 0.7095(8) 0.191(12) Uani 1 1 d U . .
H144 H 1.1340 1.4654 0.7141 0.229 Uiso 1 1 calc R . .
C234 C 1.0700(14) 1.638(3) 0.7344(8) 0.179(16) Uani 1 1 d . . .
H234 H 1.0896 1.6923 0.7433 0.215 Uiso 1 1 calc R . .
C174 C 1.1586(8) 1.197(3) 0.6932(6) 0.145(9) Uani 1 1 d U . .
H174 H 1.1644 1.1283 0.6882 0.174 Uiso 1 1 calc R . .
C224 C 1.0297(15) 1.668(3) 0.7188(11) 0.19(2) Uani 1 1 d . . .
H224 H 1.0205 1.7386 0.7183 0.225 Uiso 1 1 calc R . .
O3W O 0.7467(18) 0.308(5) 0.7063(14) 0.30(3) Uiso 0.50 1 d P . .
O2W O 1.1835(9) 0.722(2) 0.7276(7) 0.288(13) Uiso 1 1 d . . .
O1W O 0.8115(12) 0.908(3) 0.7311(9) 0.39(2) Uiso 1 1 d . . .
O4W O 0.786(2) 0.561(6) 0.7219(16) 0.35(3) Uiso 0.50 1 d P . .
C154 C 1.1708(10) 1.378(3) 0.7000(9) 0.210(12) Uani 1 1 d U . .
H154 H 1.1860 1.4366 0.6984 0.252 Uiso 1 1 calc R . .
O5W O 0.7541(10) 0.659(3) 0.6750(8) 0.150(12) Uiso 0.50 1 d P . .
O6W O 0.7272(19) 0.412(5) 0.2647(14) 0.32(3) Uiso 0.50 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
I31 C31 2.088(14) . ?
I61 C61 2.050(14) . ?
I62 C62 2.072(15) . ?
I33 C33 2.094(16) . ?
I32 C32 2.085(16) . ?
I63 C63 2.070(16) . ?
Fe O12 1.994(10) . ?
Fe O22 1.999(10) . ?
Fe O21 2.006(9) . ?
Fe O11 2.007(10) . ?
Fe O23 2.010(10) . ?
Fe O13 2.038(10) . ?
P16 C76 1.804(15) . ?
P16 C196 1.808(14) . ?
P16 C16 1.809(15) . ?
P16 C136 1.821(14) . ?
P15 C135 1.785(15) . ?
P15 C195 1.787(17) . ?
P15 C75 1.788(15) . ?
P15 C15 1.810(16) . ?
P14 C134 1.754(18) . ?
P14 C194 1.77(2) . ?
P14 C74 1.774(17) . ?
P14 C14 1.816(18) . ?
O13 C13 1.264(16) . ?
O21 C21 1.290(16) . ?
O51 C51 1.195(16) . ?
O23 C23 1.328(17) . ?
O22 C22 1.296(16) . ?
O52 C52 1.227(17) . ?
C21 C31 1.376(19) . ?
C21 C11 1.556(18) . ?
O11 C11 1.301(15) . ?
C215 C225 1.38(3) . ?
C215 C205 1.39(3) . ?
C215 H215 0.9300 . ?
C65 C55 1.35(2) . ?
C65 C15 1.40(2) . ?
C65 H65 0.9300 . ?
O41 C41 1.223(17) . ?
C46 C56 1.33(3) . ?
C46 C36 1.36(3) . ?
C46 H46 0.9300 . ?
C104 C94 1.34(2) . ?
C104 C114 1.40(2) . ?
C104 H104 0.9300 . ?
C195 C205 1.38(2) . ?
C195 C245 1.40(2) . ?
C44 C54 1.35(3) . ?
C44 C34 1.35(3) . ?
C44 H44 0.9300 . ?
C31 C41 1.41(2) . ?
O53 C53 1.261(18) . ?
O43 C43 1.238(17) . ?
C76 C86 1.38(2) . ?
C76 C126 1.39(2) . ?
C55 C45 1.40(2) . ?
C55 H55 0.9300 . ?
C106 C116 1.38(3) . ?
C106 C96 1.39(3) . ?
C106 H106 0.9300 . ?
C63 C53 1.39(2) . ?
C63 C13 1.39(2) . ?
C105 C115 1.38(2) . ?
C105 C95 1.41(2) . ?
C105 H105 0.9300 . ?
C52 C62 1.48(2) . ?
C52 C42 1.55(2) . ?
C96 C86 1.34(2) . ?
C96 H96 0.9300 . ?
C226 C216 1.38(3) . ?
C226 C236 1.40(3) . ?
C226 H226 0.9300 . ?
C11 C61 1.356(19) . ?
C125 C115 1.36(2) . ?
C125 C75 1.36(2) . ?
C125 H125 0.9300 . ?
C206 C216 1.38(2) . ?
C206 C196 1.40(2) . ?
C206 H206 0.9300 . ?
C94 C84 1.41(2) . ?
C94 H94 0.9300 . ?
C86 H86 0.9300 . ?
C136 C186 1.362(18) . ?
C136 C146 1.41(2) . ?
C24 C34 1.38(3) . ?
C24 C14 1.39(2) . ?
C24 H24 0.9300 . ?
C95 C85 1.38(2) . ?
C95 H95 0.9300 . ?
C23 C33 1.35(2) . ?
C23 C13 1.51(2) . ?
C25 C15 1.339(19) . ?
C25 C35 1.383(19) . ?
C25 H25 0.9300 . ?
C186 C176 1.39(2) . ?
C186 H186 0.9300 . ?
C33 C43 1.43(2) . ?
C35 C45 1.36(2) . ?
C35 H35 0.9300 . ?
O12 C12 1.331(16) . ?
C246 C236 1.38(2) . ?
C246 C196 1.38(2) . ?
C246 H246 0.9300 . ?
C74 C124 1.41(2) . ?
C74 C84 1.43(2) . ?
C61 C51 1.44(2) . ?
C32 C22 1.35(2) . ?
C32 C42 1.45(2) . ?
C165 C175 1.34(2) . ?
C165 C155 1.40(2) . ?
C165 H165 0.9300 . ?
C16 C66 1.39(2) . ?
C16 C26 1.40(2) . ?
C115 H115 0.9300 . ?
C22 C12 1.510(19) . ?
C175 C185 1.40(2) . ?
C175 H175 0.9300 . ?
C176 C166 1.38(2) . ?
C176 H176 0.9300 . ?
C75 C85 1.39(2) . ?
C204 C194 1.36(3) . ?
C204 C214 1.41(3) . ?
C204 H204 0.9300 . ?
C134 C144 1.33(3) . ?
C134 C184 1.36(3) . ?
C245 C235 1.40(3) . ?
C245 H245 0.9300 . ?
C84 H84 0.9300 . ?
C51 C41 1.60(2) . ?
C145 C155 1.37(2) . ?
C145 C135 1.42(2) . ?
C145 H145 0.9300 . ?
C26 C36 1.42(2) . ?
C26 H26 0.9300 . ?
C166 C156 1.37(2) . ?
C166 H166 0.9300 . ?
C85 H85 0.9300 . ?
C135 C185 1.41(2) . ?
C12 C62 1.364(19) . ?
C146 C156 1.41(2) . ?
C146 H146 0.9300 . ?
C114 C124 1.32(2) . ?
C114 H114 0.9300 . ?
C185 H185 0.9300 . ?
C155 H155 0.9300 . ?
C156 H156 0.9300 . ?
O42 C42 1.225(19) . ?
C225 C235 1.36(3) . ?
C225 H225 0.9300 . ?
C45 H45 0.9300 . ?
C43 C53 1.55(2) . ?
C126 C116 1.36(2) . ?
C126 H126 0.9300 . ?
C205 H205 0.9300 . ?
C236 H236 0.9300 . ?
C216 H216 0.9300 . ?
C56 C66 1.42(2) . ?
C56 H56 0.9300 . ?
C194 C244 1.39(3) . ?
C66 H66 0.9300 . ?
C36 H36 0.9300 . ?
C116 H116 0.9300 . ?
C124 H124 0.9300 . ?
C235 H235 0.9300 . ?
C244 C234 1.36(4) . ?
C244 H244 0.9300 . ?
C214 C224 1.40(4) . ?
C214 H214 0.9300 . ?
C164 C174 1.33(3) . ?
C164 C154 1.35(4) . ?
C164 H164 0.9300 . ?
C184 C174 1.42(3) . ?
C184 H184 0.9300 . ?
C34 H34 0.9300 . ?
C54 C64 1.37(2) . ?
C54 H54 0.9300 . ?
C64 C14 1.35(2) . ?
C64 H64 0.9300 . ?
C144 C154 1.35(3) . ?
C144 H144 0.9300 . ?
C234 C224 1.34(5) . ?
C234 H234 0.9300 . ?
C174 H174 0.9300 . ?
C224 H224 0.9300 . ?
C154 H154 0.9300 . ?

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
O12 Fe O22 81.0(4) . . ?
O12 Fe O21 97.9(4) . . ?
O22 Fe O21 98.3(4) . . ?
O12 Fe O11 176.3(4) . . ?
O22 Fe O11 97.2(4) . . ?
O21 Fe O11 79.2(4) . . ?
O12 Fe O23 89.6(4) . . ?
O22 Fe O23 165.4(4) . . ?
O21 Fe O23 94.0(4) . . ?
O11 Fe O23 92.8(4) . . ?
O12 Fe O13 94.8(4) . . ?
O22 Fe O13 90.2(4) . . ?
O21 Fe O13 165.7(4) . . ?
O11 Fe O13 88.4(4) . . ?
O23 Fe O13 79.5(4) . . ?
C76 P16 C196 108.9(8) . . ?
C76 P16 C16 110.5(7) . . ?
C196 P16 C16 108.6(7) . . ?
C76 P16 C136 108.5(7) . . ?
C196 P16 C136 108.9(7) . . ?
C16 P16 C136 111.3(7) . . ?
C135 P15 C195 107.7(7) . . ?
C135 P15 C75 111.6(7) . . ?
C195 P15 C75 109.2(8) . . ?
C135 P15 C15 110.6(7) . . ?
C195 P15 C15 110.2(8) . . ?
C75 P15 C15 107.6(7) . . ?
C134 P14 C194 113.1(10) . . ?
C134 P14 C74 107.2(9) . . ?
C194 P14 C74 109.4(10) . . ?
C134 P14 C14 111.7(9) . . ?
C194 P14 C14 108.7(9) . . ?
C74 P14 C14 106.5(9) . . ?
C13 O13 Fe 116.2(10) . . ?
C21 O21 Fe 117.5(9) . . ?
C23 O23 Fe 115.2(9) . . ?
C22 O22 Fe 114.9(10) . . ?
O21 C21 C31 129.4(13) . . ?
O21 C21 C11 112.9(13) . . ?
C31 C21 C11 117.7(13) . . ?
C11 O11 Fe 116.8(9) . . ?
C225 C215 C205 115(2) . . ?
C225 C215 H215 122.4 . . ?
C205 C215 H215 122.4 . . ?
C55 C65 C15 119.0(16) . . ?
C55 C65 H65 120.5 . . ?
C15 C65 H65 120.5 . . ?
C56 C46 C36 122(2) . . ?
C56 C46 H46 118.9 . . ?
C36 C46 H46 118.9 . . ?
C94 C104 C114 119(2) . . ?
C94 C104 H104 120.3 . . ?
C114 C104 H104 120.3 . . ?
C205 C195 C245 118.9(17) . . ?
C205 C195 P15 122.8(15) . . ?
C245 C195 P15 118.2(15) . . ?
C54 C44 C34 121(2) . . ?
C54 C44 H44 119.5 . . ?
C34 C44 H44 119.5 . . ?
C21 C31 C41 123.1(14) . . ?
C21 C31 I31 118.5(11) . . ?
C41 C31 I31 118.4(11) . . ?
C86 C76 C126 120.1(16) . . ?
C86 C76 P16 118.8(13) . . ?
C126 C76 P16 121.1(13) . . ?
C65 C55 C45 122.0(16) . . ?
C65 C55 H55 119.0 . . ?
C45 C55 H55 119.0 . . ?
C116 C106 C96 119(2) . . ?
C116 C106 H106 120.7 . . ?
C96 C106 H106 120.7 . . ?
C53 C63 C13 119.2(16) . . ?
C53 C63 I63 120.3(13) . . ?
C13 C63 I63 120.5(13) . . ?
C115 C105 C95 114.8(17) . . ?
C115 C105 H105 122.6 . . ?
C95 C105 H105 122.6 . . ?
O52 C52 C62 121.0(17) . . ?
O52 C52 C42 121.6(16) . . ?
C62 C52 C42 117.3(14) . . ?
C86 C96 C106 120(2) . . ?
C86 C96 H96 120.1 . . ?
C106 C96 H96 120.1 . . ?
C216 C226 C236 121.1(19) . . ?
C216 C226 H226 119.5 . . ?
C236 C226 H226 119.5 . . ?
O11 C11 C61 125.3(13) . . ?
O11 C11 C21 112.4(12) . . ?
C61 C11 C21 122.2(14) . . ?
C115 C125 C75 120.3(17) . . ?
C115 C125 H125 119.8 . . ?
C75 C125 H125 119.8 . . ?
C216 C206 C196 118.2(18) . . ?
C216 C206 H206 120.9 . . ?
C196 C206 H206 120.9 . . ?
C104 C94 C84 119.8(19) . . ?
C104 C94 H94 120.1 . . ?
C84 C94 H94 120.1 . . ?
C96 C86 C76 120.9(18) . . ?
C96 C86 H86 119.6 . . ?
C76 C86 H86 119.6 . . ?
C186 C136 C146 123.1(14) . . ?
C186 C136 P16 119.4(13) . . ?
C146 C136 P16 117.3(11) . . ?
C34 C24 C14 118(2) . . ?
C34 C24 H24 120.9 . . ?
C14 C24 H24 120.9 . . ?
C85 C95 C105 121.3(18) . . ?
C85 C95 H95 119.3 . . ?
C105 C95 H95 119.3 . . ?
O23 C23 C33 125.8(15) . . ?
O23 C23 C13 114.0(14) . . ?
C33 C23 C13 120.2(15) . . ?
C15 C25 C35 120.3(15) . . ?
C15 C25 H25 119.9 . . ?
C35 C25 H25 119.9 . . ?
C136 C186 C176 119.0(17) . . ?
C136 C186 H186 120.5 . . ?
C176 C186 H186 120.5 . . ?
C23 C33 C43 121.9(16) . . ?
C23 C33 I33 120.8(12) . . ?
C43 C33 I33 117.2(12) . . ?
C25 C15 C65 120.1(15) . . ?
C25 C15 P15 124.5(12) . . ?
C65 C15 P15 115.5(13) . . ?
C45 C35 C25 121.5(16) . . ?
C45 C35 H35 119.2 . . ?
C25 C35 H35 119.2 . . ?
C12 O12 Fe 114.6(9) . . ?
C236 C246 C196 120.4(18) . . ?
C236 C246 H246 119.8 . . ?
C196 C246 H246 119.8 . . ?
C124 C74 C84 118.7(16) . . ?
C124 C74 P14 122.5(15) . . ?
C84 C74 P14 118.6(14) . . ?
C11 C61 C51 121.0(14) . . ?
C11 C61 I61 122.2(12) . . ?
C51 C61 I61 116.8(11) . . ?
C22 C32 C42 121.9(16) . . ?
C22 C32 I32 121.0(13) . . ?
C42 C32 I32 117.1(12) . . ?
C175 C165 C155 118.3(17) . . ?
C175 C165 H165 120.8 . . ?
C155 C165 H165 120.8 . . ?
C66 C16 C26 120.6(15) . . ?
C66 C16 P16 119.1(13) . . ?
C26 C16 P16 120.3(12) . . ?
C125 C115 C105 124.3(19) . . ?
C125 C115 H115 117.9 . . ?
C105 C115 H115 117.9 . . ?
O22 C22 C32 124.8(15) . . ?
O22 C22 C12 115.3(14) . . ?
C32 C22 C12 119.6(15) . . ?
C165 C175 C185 123.5(18) . . ?
C165 C175 H175 118.2 . . ?
C185 C175 H175 118.2 . . ?
C166 C176 C186 121.0(17) . . ?
C166 C176 H176 119.5 . . ?
C186 C176 H176 119.5 . . ?
C125 C75 C85 118.3(15) . . ?
C125 C75 P15 122.9(13) . . ?
C85 C75 P15 118.7(12) . . ?
C194 C204 C214 118(2) . . ?
C194 C204 H204 121.1 . . ?
C214 C204 H204 121.1 . . ?
C144 C134 C184 118(2) . . ?
C144 C134 P14 123.3(19) . . ?
C184 C134 P14 119.1(17) . . ?
C195 C245 C235 118(2) . . ?
C195 C245 H245 120.8 . . ?
C235 C245 H245 120.8 . . ?
C94 C84 C74 119.2(17) . . ?
C94 C84 H84 120.4 . . ?
C74 C84 H84 120.4 . . ?
O51 C51 C61 126.5(15) . . ?
O51 C51 C41 116.9(15) . . ?
C61 C51 C41 116.6(13) . . ?
C155 C145 C135 119.7(16) . . ?
C155 C145 H145 120.1 . . ?
C135 C145 H145 120.1 . . ?
C16 C26 C36 116.6(16) . . ?
C16 C26 H26 121.7 . . ?
C36 C26 H26 121.7 . . ?
C156 C166 C176 118.2(17) . . ?
C156 C166 H166 120.9 . . ?
C176 C166 H166 120.9 . . ?
C95 C85 C75 121.0(17) . . ?
C95 C85 H85 119.5 . . ?
C75 C85 H85 119.5 . . ?
C185 C135 C145 118.7(14) . . ?
C185 C135 P15 120.3(12) . . ?
C145 C135 P15 121.0(12) . . ?
O12 C12 C62 123.7(14) . . ?
O12 C12 C22 113.4(13) . . ?
C62 C12 C22 122.9(14) . . ?
C156 C146 C136 114.8(14) . . ?
C156 C146 H146 122.6 . . ?
C136 C146 H146 122.6 . . ?
C124 C114 C104 124(2) . . ?
C124 C114 H114 118.0 . . ?
C104 C114 H114 118.0 . . ?
C175 C185 C135 118.1(17) . . ?
C175 C185 H185 120.9 . . ?
C135 C185 H185 120.9 . . ?
C145 C155 C165 121.5(17) . . ?
C145 C155 H155 119.3 . . ?
C165 C155 H155 119.3 . . ?
C166 C156 C146 123.7(18) . . ?
C166 C156 H156 118.1 . . ?
C146 C156 H156 118.1 . . ?
C235 C225 C215 124(3) . . ?
C235 C225 H225 118.0 . . ?
C215 C225 H225 118.0 . . ?
C35 C45 C55 117.1(16) . . ?
C35 C45 H45 121.5 . . ?
C55 C45 H45 121.5 . . ?
O43 C43 C33 125.3(17) . . ?
O43 C43 C53 118.0(16) . . ?
C33 C43 C53 116.5(15) . . ?
C116 C126 C76 118(2) . . ?
C116 C126 H126 120.9 . . ?
C76 C126 H126 120.9 . . ?
C195 C205 C215 124(2) . . ?
C195 C205 H205 118.2 . . ?
C215 C205 H205 118.2 . . ?
C246 C196 C206 121.1(15) . . ?
C246 C196 P16 121.8(13) . . ?
C206 C196 P16 117.1(13) . . ?
O13 C13 C63 124.0(15) . . ?
O13 C13 C23 114.8(14) . . ?
C63 C13 C23 121.1(15) . . ?
C12 C62 C52 119.3(15) . . ?
C12 C62 I62 120.4(11) . . ?
C52 C62 I62 120.3(12) . . ?
C246 C236 C226 118.6(19) . . ?
C246 C236 H236 120.7 . . ?
C226 C236 H236 120.7 . . ?
O41 C41 C31 124.5(15) . . ?
O41 C41 C51 117.0(14) . . ?
C31 C41 C51 118.4(14) . . ?
C206 C216 C226 121(2) . . ?
C206 C216 H216 119.7 . . ?
C226 C216 H216 119.7 . . ?
C46 C56 C66 119(2) . . ?
C46 C56 H56 120.6 . . ?
C66 C56 H56 120.6 . . ?
C204 C194 C244 120(2) . . ?
C204 C194 P14 123(2) . . ?
C244 C194 P14 117(2) . . ?
C16 C66 C56 120.3(18) . . ?
C16 C66 H66 119.8 . . ?
C56 C66 H66 119.8 . . ?
O53 C53 C63 125.2(18) . . ?
O53 C53 C43 113.7(17) . . ?
C63 C53 C43 121.1(15) . . ?
C46 C36 C26 121(2) . . ?
C46 C36 H36 119.3 . . ?
C26 C36 H36 119.3 . . ?
C126 C116 C106 122(2) . . ?
C126 C116 H116 119.0 . . ?
C106 C116 H116 119.0 . . ?
O42 C42 C32 126.7(18) . . ?
O42 C42 C52 114.8(17) . . ?
C32 C42 C52 118.5(15) . . ?
C114 C124 C74 118.5(18) . . ?
C114 C124 H124 120.8 . . ?
C74 C124 H124 120.8 . . ?
C225 C235 C245 120(2) . . ?
C225 C235 H235 120.1 . . ?
C245 C235 H235 120.1 . . ?
C234 C244 C194 119(3) . . ?
C234 C244 H244 120.7 . . ?
C194 C244 H244 120.7 . . ?
C224 C214 C204 124(3) . . ?
C224 C214 H214 117.8 . . ?
C204 C214 H214 117.8 . . ?
C174 C164 C154 118(3) . . ?
C174 C164 H164 121.2 . . ?
C154 C164 H164 121.2 . . ?
C134 C184 C174 123(2) . . ?
C134 C184 H184 118.4 . . ?
C174 C184 H184 118.4 . . ?
C44 C34 C24 120(2) . . ?
C44 C34 H34 120.2 . . ?
C24 C34 H34 120.2 . . ?
C44 C54 C64 120(2) . . ?
C44 C54 H54 119.9 . . ?
C64 C54 H54 119.9 . . ?
C14 C64 C54 119(2) . . ?
C14 C64 H64 120.4 . . ?
C54 C64 H64 120.4 . . ?
C64 C14 C24 121.0(19) . . ?
C64 C14 P14 119.8(15) . . ?
C24 C14 P14 117.9(15) . . ?
C134 C144 C154 118(3) . . ?
C134 C144 H144 120.9 . . ?
C154 C144 H144 120.9 . . ?
C224 C234 C244 126(4) . . ?
C224 C234 H234 116.8 . . ?
C244 C234 H234 116.8 . . ?
C164 C174 C184 117(3) . . ?
C164 C174 H174 121.4 . . ?
C184 C174 H174 121.4 . . ?
C234 C224 C214 113(4) . . ?
C234 C224 H224 123.7 . . ?
C214 C224 H224 123.7 . . ?
C144 C154 C164 126(3) . . ?
C144 C154 H154 117.1 . . ?
C164 C154 H154 117.1 . . ?

_diffrn_measured_fraction_theta_max 0.982
_diffrn_reflns_theta_full        23.42
_diffrn_measured_fraction_theta_full 0.982
_refine_diff_density_max         0.734
_refine_diff_density_min         -0.691
_refine_diff_density_rms         0.118

#END

_database_code_depnum_ccdc_archive 'CCDC 941119'
