# Supplementary Material (ESI) for Chemical Communications
# This journal is (c) The Royal Society of Chemistry 2008

data_global
_journal_name_full               Chem.Commun.

_journal_coden_Cambridge         0182
_journal_volume                  ?
_journal_page_first              ?
_journal_year                    ?

_publ_contact_author_name        'Jorge Navarro'
_publ_contact_author_email       JARN@UGR.ES

_publ_section_title              
;
Electrochemically and Photochemically Active
Palladium(II) Heterotopic Metallacalix[3]arenes
;
loop_
_publ_author_name
'Jorge Navarro'
'William Clegg'
'Jose Dobado'
'Miguel A Galindo'
'Ross W Harrington'
;
A.Houlton
;
'M Angustias Romero'
'Francisco Santoyo-Gonzalez'

# Attachment '2b.cif'

data_2b
_database_code_depnum_ccdc_archive 'CCDC 677962'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C16 H12 Fe N2 O, H2 O, C H4 O'
_chemical_formula_sum            'C17 H18 Fe N2 O3'
_chemical_formula_weight         354.18

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'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'

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

_cell_length_a                   6.022(4)
_cell_length_b                   9.912(6)
_cell_length_c                   12.964(8)
_cell_angle_alpha                78.772(7)
_cell_angle_beta                 77.213(6)
_cell_angle_gamma                77.793(6)
_cell_volume                     728.6(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    2048
_cell_measurement_theta_min      2.3
_cell_measurement_theta_max      26.4

_exptl_crystal_description       needle
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.614
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             368
_exptl_absorpt_coefficient_mu    1.052
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.820
_exptl_absorpt_correction_T_max  0.980
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
Small crystal size and poor diffraction (resulting from disorder among
other factors) necessitated data collection with synchrotron radiation.
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.6751
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'Daresbury SRS station 9.8'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_measurement_device_type  'Bruker APEX2 CCD diffractometer'
_diffrn_measurement_method       'thin-slice \w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        5
_diffrn_reflns_number            4781
_diffrn_reflns_av_R_equivalents  0.0447
_diffrn_reflns_av_sigmaI/netI    0.0644
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.35
_diffrn_reflns_theta_max         22.49
_reflns_number_total             2205
_reflns_number_gt                1792
_reflns_threshold_expression     I>2\s(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'

_refine_special_details          
;
A water molecule could be located, as hydrogen bonding (acceptor for NH,
donor to O atoms of two other molecules) keeps it ordered; its H atoms
were constrained to an OH distance of 0.84 \%A and pointing in directions
giving linear hydrogen bonds, making an HOH angle of 94\%, which is
reasonable.

The asymmetric unit also probably contains one methanol molecule, but this
is highly disordered and could not be modelled with discrete atoms. Its
contribution to the diffraction was dealt with by the SQUEEZE procedure
of PLATON (A. L. Spek, J. Appl. Cryst. 2003, 36, 7-13), which indicated
the "void" volume and approximate electron count appropriate for this
molecule.

The disorder reduces the quality of the diffraction pattern and hence the
precision of the crystal structure overall.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.1336P)^2^+1.4426P] where P=(Fo^2^+2Fc^2^)/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     SHELXL
_refine_ls_extinction_coef       0.018(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns         2205
_refine_ls_number_parameters     194
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0869
_refine_ls_R_factor_gt           0.0751
_refine_ls_wR_factor_ref         0.2078
_refine_ls_wR_factor_gt          0.2007
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_restrained_S_all      1.071
_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
N1 N 0.5169(8) 0.4029(5) 0.7210(4) 0.0255(12) Uani 1 1 d . . .
C2 C 0.3449(10) 0.4060(7) 0.8075(5) 0.0283(14) Uani 1 1 d . . .
O2 O 0.3706(7) 0.4229(5) 0.8964(4) 0.0328(11) Uani 1 1 d . . .
N3 N 0.1278(8) 0.3908(5) 0.7962(4) 0.0251(12) Uani 1 1 d D . .
H3 H 0.023(9) 0.393(7) 0.855(3) 0.030 Uiso 1 1 d D . .
C4 C 0.0819(10) 0.3752(6) 0.7040(5) 0.0266(14) Uani 1 1 d . . .
H4 H -0.0711 0.3695 0.6995 0.032 Uiso 1 1 calc R . .
C5 C 0.2539(10) 0.3675(6) 0.6157(5) 0.0255(14) Uani 1 1 d . . .
C6 C 0.4730(10) 0.3838(6) 0.6299(5) 0.0243(13) Uani 1 1 d . . .
H6 H 0.5966 0.3808 0.5699 0.029 Uiso 1 1 calc R . .
C7 C 0.2137(10) 0.3448(7) 0.5158(5) 0.0273(14) Uani 1 1 d . . .
C8 C 0.1764(10) 0.3234(6) 0.4347(5) 0.0262(14) Uani 1 1 d . . .
C9 C 0.1280(10) 0.3002(6) 0.3373(5) 0.0237(13) Uani 1 1 d . . .
C10 C 0.2768(10) 0.3122(7) 0.2357(5) 0.0275(14) Uani 1 1 d . . .
H10 H 0.4263 0.3365 0.2209 0.033 Uiso 1 1 calc R . .
C11 C 0.1634(11) 0.2816(7) 0.1594(5) 0.0284(14) Uani 1 1 d . . .
H11 H 0.2237 0.2827 0.0851 0.034 Uiso 1 1 calc R . .
C12 C -0.0550(11) 0.2494(7) 0.2140(5) 0.0286(14) Uani 1 1 d . . .
H12 H -0.1662 0.2251 0.1824 0.034 Uiso 1 1 calc R . .
C13 C -0.0794(10) 0.2596(6) 0.3243(5) 0.0277(14) Uani 1 1 d . . .
H13 H -0.2086 0.2427 0.3792 0.033 Uiso 1 1 calc R . .
C14 C 0.3377(12) -0.0379(7) 0.3909(6) 0.0367(16) Uani 1 1 d . . .
H14 H 0.3504 -0.0257 0.4601 0.044 Uiso 1 1 calc R . .
C15 C 0.5062(12) -0.0202(7) 0.2971(6) 0.0436(19) Uani 1 1 d . . .
H15 H 0.6524 0.0049 0.2921 0.052 Uiso 1 1 calc R . .
C16 C 0.4182(14) -0.0467(8) 0.2114(6) 0.049(2) Uani 1 1 d . . .
H16 H 0.4933 -0.0421 0.1385 0.059 Uiso 1 1 calc R . .
C17 C 0.1951(13) -0.0814(7) 0.2562(7) 0.046(2) Uani 1 1 d . . .
H17 H 0.0947 -0.1043 0.2176 0.055 Uiso 1 1 calc R . .
C18 C 0.1488(12) -0.0764(7) 0.3651(6) 0.0402(17) Uani 1 1 d . . .
H18 H 0.0121 -0.0958 0.4138 0.048 Uiso 1 1 calc R . .
Fe Fe 0.20383(14) 0.11483(9) 0.27950(7) 0.0258(4) Uani 1 1 d . . .
O19 O -0.2234(7) 0.3696(5) 0.9694(3) 0.0321(11) Uani 1 1 d . . .
H19A H -0.3483 0.3856 0.9468 0.048 Uiso 1 1 d R . .
H19B H -0.2669 0.4312 1.0093 0.048 Uiso 1 1 d R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
N1 0.011(2) 0.039(3) 0.030(3) -0.001(2) -0.011(2) -0.008(2)
C2 0.017(3) 0.036(4) 0.031(4) 0.002(3) -0.010(3) -0.006(3)
O2 0.018(2) 0.053(3) 0.035(3) -0.008(2) -0.0137(19) -0.012(2)
N3 0.010(2) 0.039(3) 0.029(3) -0.004(2) -0.007(2) -0.008(2)
C4 0.015(3) 0.028(3) 0.041(4) -0.001(3) -0.017(3) -0.006(2)
C5 0.017(3) 0.029(3) 0.035(3) -0.004(3) -0.015(3) -0.005(2)
C6 0.011(3) 0.032(3) 0.030(3) -0.002(3) -0.008(2) -0.004(2)
C7 0.013(3) 0.039(4) 0.034(4) -0.002(3) -0.011(3) -0.009(3)
C8 0.013(3) 0.030(3) 0.038(4) -0.001(3) -0.013(3) -0.005(2)
C9 0.016(3) 0.031(3) 0.027(3) -0.002(2) -0.015(2) -0.002(2)
C10 0.017(3) 0.031(3) 0.037(4) 0.000(3) -0.012(3) -0.007(2)
C11 0.025(3) 0.034(4) 0.029(3) -0.001(3) -0.013(3) -0.006(3)
C12 0.024(3) 0.036(4) 0.031(3) -0.004(3) -0.016(3) -0.006(3)
C13 0.016(3) 0.030(3) 0.039(4) 0.002(3) -0.014(3) -0.005(2)
C14 0.038(4) 0.035(4) 0.039(4) -0.001(3) -0.022(3) 0.000(3)
C15 0.020(3) 0.039(4) 0.068(5) 0.001(4) -0.007(3) -0.006(3)
C16 0.051(5) 0.047(5) 0.039(4) -0.007(3) 0.000(4) 0.006(4)
C17 0.038(4) 0.030(4) 0.078(6) -0.003(4) -0.033(4) -0.008(3)
C18 0.027(4) 0.038(4) 0.053(5) 0.003(3) -0.010(3) -0.009(3)
Fe 0.0138(6) 0.0347(7) 0.0326(6) -0.0020(4) -0.0122(4) -0.0069(4)
O19 0.014(2) 0.054(3) 0.032(2) -0.006(2) -0.0109(18) -0.0082(19)

_geom_special_details            
;
;

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
N1 C2 1.348(8) . ?
N1 C6 1.321(8) . ?
C2 O2 1.244(8) . ?
C2 N3 1.389(8) . ?
N3 H3 0.88(2) . ?
N3 C4 1.329(8) . ?
C4 H4 0.950 . ?
C4 C5 1.366(9) . ?
C5 C6 1.418(8) . ?
C5 C7 1.436(9) . ?
C6 H6 0.950 . ?
C7 C8 1.189(9) . ?
C8 C9 1.427(8) . ?
C9 C10 1.419(9) . ?
C9 C13 1.444(8) . ?
C9 Fe 2.043(6) . ?
C10 H10 0.950 . ?
C10 C11 1.427(9) . ?
C10 Fe 2.041(6) . ?
C11 H11 0.950 . ?
C11 C12 1.418(9) . ?
C11 Fe 2.052(6) . ?
C12 H12 0.950 . ?
C12 C13 1.426(9) . ?
C12 Fe 2.048(6) . ?
C13 H13 0.950 . ?
C13 Fe 2.039(6) . ?
C14 H14 0.950 . ?
C14 C15 1.408(10) . ?
C14 C18 1.398(10) . ?
C14 Fe 2.043(6) . ?
C15 H15 0.950 . ?
C15 C16 1.420(11) . ?
C15 Fe 2.048(7) . ?
C16 H16 0.950 . ?
C16 C17 1.426(11) . ?
C16 Fe 2.044(8) . ?
C17 H17 0.950 . ?
C17 C18 1.386(11) . ?
C17 Fe 2.039(7) . ?
C18 H18 0.950 . ?
C18 Fe 2.054(7) . ?
O19 H19A 0.840 . ?
O19 H19B 0.8399 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 N1 C6 118.9(5) . . ?
N1 C2 O2 123.3(5) . . ?
N1 C2 N3 118.2(5) . . ?
O2 C2 N3 118.5(5) . . ?
C2 N3 H3 114(5) . . ?
C2 N3 C4 123.0(5) . . ?
H3 N3 C4 123(5) . . ?
N3 C4 H4 119.9 . . ?
N3 C4 C5 120.2(5) . . ?
H4 C4 C5 119.9 . . ?
C4 C5 C6 115.3(5) . . ?
C4 C5 C7 121.9(5) . . ?
C6 C5 C7 122.8(6) . . ?
N1 C6 C5 124.3(5) . . ?
N1 C6 H6 117.8 . . ?
C5 C6 H6 117.8 . . ?
C5 C7 C8 178.2(6) . . ?
C7 C8 C9 178.8(6) . . ?
C8 C9 C10 125.9(5) . . ?
C8 C9 C13 126.4(6) . . ?
C8 C9 Fe 126.4(4) . . ?
C10 C9 C13 107.7(5) . . ?
C10 C9 Fe 69.6(3) . . ?
C13 C9 Fe 69.1(4) . . ?
C9 C10 H10 125.8 . . ?
C9 C10 C11 108.3(5) . . ?
C9 C10 Fe 69.8(3) . . ?
H10 C10 C11 125.8 . . ?
H10 C10 Fe 126.0 . . ?
C11 C10 Fe 70.0(4) . . ?
C10 C11 H11 126.0 . . ?
C10 C11 C12 108.1(6) . . ?
C10 C11 Fe 69.2(4) . . ?
H11 C11 C12 126.0 . . ?
H11 C11 Fe 126.8 . . ?
C12 C11 Fe 69.6(4) . . ?
C11 C12 H12 125.8 . . ?
C11 C12 C13 108.4(5) . . ?
C11 C12 Fe 69.9(4) . . ?
H12 C12 C13 125.8 . . ?
H12 C12 Fe 126.7 . . ?
C13 C12 Fe 69.2(3) . . ?
C9 C13 C12 107.5(5) . . ?
C9 C13 H13 126.3 . . ?
C9 C13 Fe 69.5(3) . . ?
C12 C13 H13 126.3 . . ?
C12 C13 Fe 69.9(4) . . ?
H13 C13 Fe 125.9 . . ?
H14 C14 C15 125.7 . . ?
H14 C14 C18 125.7 . . ?
H14 C14 Fe 125.4 . . ?
C15 C14 C18 108.7(6) . . ?
C15 C14 Fe 70.0(4) . . ?
C18 C14 Fe 70.5(4) . . ?
C14 C15 H15 126.2 . . ?
C14 C15 C16 107.7(6) . . ?
C14 C15 Fe 69.7(4) . . ?
H15 C15 C16 126.2 . . ?
H15 C15 Fe 126.2 . . ?
C16 C15 Fe 69.6(4) . . ?
C15 C16 H16 126.7 . . ?
C15 C16 C17 106.6(7) . . ?
C15 C16 Fe 69.8(4) . . ?
H16 C16 C17 126.7 . . ?
H16 C16 Fe 125.7 . . ?
C17 C16 Fe 69.4(4) . . ?
C16 C17 H17 125.6 . . ?
C16 C17 C18 108.8(7) . . ?
C16 C17 Fe 69.8(4) . . ?
H17 C17 C18 125.6 . . ?
H17 C17 Fe 125.5 . . ?
C18 C17 Fe 70.8(4) . . ?
C14 C18 C17 108.2(6) . . ?
C14 C18 H18 125.9 . . ?
C14 C18 Fe 69.6(4) . . ?
C17 C18 H18 125.9 . . ?
C17 C18 Fe 69.6(4) . . ?
H18 C18 Fe 126.4 . . ?
C9 Fe C10 40.7(2) . . ?
C9 Fe C11 68.6(2) . . ?
C9 Fe C12 68.9(2) . . ?
C9 Fe C13 41.4(2) . . ?
C9 Fe C14 108.5(3) . . ?
C9 Fe C15 120.4(3) . . ?
C9 Fe C16 154.9(3) . . ?
C9 Fe C17 162.8(3) . . ?
C9 Fe C18 126.4(3) . . ?
C10 Fe C11 40.8(2) . . ?
C10 Fe C12 68.6(2) . . ?
C10 Fe C13 69.0(2) . . ?
C10 Fe C14 126.5(3) . . ?
C10 Fe C15 108.0(3) . . ?
C10 Fe C16 120.0(3) . . ?
C10 Fe C17 155.4(3) . . ?
C10 Fe C18 163.4(3) . . ?
C11 Fe C12 40.5(3) . . ?
C11 Fe C13 68.7(3) . . ?
C11 Fe C14 163.4(3) . . ?
C11 Fe C15 125.9(3) . . ?
C11 Fe C16 107.3(3) . . ?
C11 Fe C17 120.5(3) . . ?
C11 Fe C18 154.8(3) . . ?
C12 Fe C13 40.8(3) . . ?
C12 Fe C14 155.2(3) . . ?
C12 Fe C15 162.6(3) . . ?
C12 Fe C16 125.1(3) . . ?
C12 Fe C17 107.7(3) . . ?
C12 Fe C18 120.6(3) . . ?
C13 Fe C14 120.7(3) . . ?
C13 Fe C15 155.5(3) . . ?
C13 Fe C16 162.3(3) . . ?
C13 Fe C17 125.1(3) . . ?
C13 Fe C18 108.0(3) . . ?
C14 Fe C15 40.3(3) . . ?
C14 Fe C16 67.9(3) . . ?
C14 Fe C17 67.1(3) . . ?
C14 Fe C18 39.9(3) . . ?
C15 Fe C16 40.6(3) . . ?
C15 Fe C17 67.9(3) . . ?
C15 Fe C18 67.5(3) . . ?
C16 Fe C17 40.9(3) . . ?
C16 Fe C18 67.8(3) . . ?
C17 Fe C18 39.6(3) . . ?
H19A O19 H19B 94.2 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 N1 C2 O2 179.7(6) . . . . ?
C6 N1 C2 N3 -0.8(9) . . . . ?
N1 C2 N3 C4 -0.9(9) . . . . ?
O2 C2 N3 C4 178.5(6) . . . . ?
C2 N3 C4 C5 2.9(9) . . . . ?
N3 C4 C5 C6 -2.9(9) . . . . ?
N3 C4 C5 C7 177.3(5) . . . . ?
C2 N1 C6 C5 0.7(9) . . . . ?
C4 C5 C6 N1 1.2(9) . . . . ?
C7 C5 C6 N1 -179.0(6) . . . . ?
C8 C9 C10 C11 -179.5(6) . . . . ?
C8 C9 C10 Fe 120.8(6) . . . . ?
C13 C9 C10 C11 0.8(7) . . . . ?
C13 C9 C10 Fe -58.8(4) . . . . ?
Fe C9 C10 C11 59.6(4) . . . . ?
C9 C10 C11 C12 -0.5(7) . . . . ?
C9 C10 C11 Fe -59.5(4) . . . . ?
Fe C10 C11 C12 58.9(4) . . . . ?
C10 C11 C12 C13 0.0(7) . . . . ?
C10 C11 C12 Fe -58.6(4) . . . . ?
Fe C11 C12 C13 58.7(4) . . . . ?
C11 C12 C13 C9 0.5(7) . . . . ?
C11 C12 C13 Fe -59.1(4) . . . . ?
Fe C12 C13 C9 59.6(4) . . . . ?
C8 C9 C13 C12 179.5(6) . . . . ?
C8 C9 C13 Fe -120.6(6) . . . . ?
C10 C9 C13 C12 -0.8(7) . . . . ?
C10 C9 C13 Fe 59.1(4) . . . . ?
Fe C9 C13 C12 -59.9(4) . . . . ?
C18 C14 C15 C16 0.7(8) . . . . ?
C18 C14 C15 Fe 60.1(5) . . . . ?
Fe C14 C15 C16 -59.4(5) . . . . ?
C14 C15 C16 C17 -0.4(8) . . . . ?
C14 C15 C16 Fe 59.5(5) . . . . ?
Fe C15 C16 C17 -59.9(5) . . . . ?
C15 C16 C17 C18 0.0(8) . . . . ?
C15 C16 C17 Fe 60.2(5) . . . . ?
Fe C16 C17 C18 -60.2(5) . . . . ?
C16 C17 C18 C14 0.5(8) . . . . ?
C16 C17 C18 Fe 59.6(5) . . . . ?
Fe C17 C18 C14 -59.1(5) . . . . ?
C15 C14 C18 C17 -0.7(8) . . . . ?
C15 C14 C18 Fe -59.9(5) . . . . ?
Fe C14 C18 C17 59.1(5) . . . . ?
C9 C13 Fe C10 -37.5(3) . . . . ?
C9 C13 Fe C11 -81.4(4) . . . . ?
C9 C13 Fe C12 -118.5(5) . . . . ?
C9 C13 Fe C14 83.4(4) . . . . ?
C9 C13 Fe C15 50.1(8) . . . . ?
C9 C13 Fe C16 -161.5(9) . . . . ?
C9 C13 Fe C17 165.5(4) . . . . ?
C9 C13 Fe C18 125.2(4) . . . . ?
C12 C13 Fe C9 118.5(5) . . . . ?
C12 C13 Fe C10 81.1(4) . . . . ?
C12 C13 Fe C11 37.1(4) . . . . ?
C12 C13 Fe C14 -158.1(4) . . . . ?
C12 C13 Fe C15 168.6(6) . . . . ?
C12 C13 Fe C16 -43.0(11) . . . . ?
C12 C13 Fe C17 -75.9(5) . . . . ?
C12 C13 Fe C18 -116.3(4) . . . . ?
C9 C10 Fe C11 119.4(5) . . . . ?
C9 C10 Fe C12 82.1(4) . . . . ?
C9 C10 Fe C13 38.2(3) . . . . ?
C9 C10 Fe C14 -75.2(4) . . . . ?
C9 C10 Fe C15 -116.0(4) . . . . ?
C9 C10 Fe C16 -158.8(4) . . . . ?
C9 C10 Fe C17 168.0(6) . . . . ?
C9 C10 Fe C18 -44.5(10) . . . . ?
C11 C10 Fe C9 -119.4(5) . . . . ?
C11 C10 Fe C12 -37.3(4) . . . . ?
C11 C10 Fe C13 -81.2(4) . . . . ?
C11 C10 Fe C14 165.4(4) . . . . ?
C11 C10 Fe C15 124.6(4) . . . . ?
C11 C10 Fe C16 81.9(5) . . . . ?
C11 C10 Fe C17 48.6(8) . . . . ?
C11 C10 Fe C18 -163.9(8) . . . . ?
C16 C17 Fe C9 -160.7(7) . . . . ?
C16 C17 Fe C10 46.5(8) . . . . ?
C16 C17 Fe C11 81.2(5) . . . . ?
C16 C17 Fe C12 123.6(5) . . . . ?
C16 C17 Fe C13 165.4(4) . . . . ?
C16 C17 Fe C14 -82.3(5) . . . . ?
C16 C17 Fe C15 -38.5(5) . . . . ?
C16 C17 Fe C18 -119.5(6) . . . . ?
C18 C17 Fe C9 -41.2(10) . . . . ?
C18 C17 Fe C10 166.1(5) . . . . ?
C18 C17 Fe C11 -159.2(4) . . . . ?
C18 C17 Fe C12 -116.9(4) . . . . ?
C18 C17 Fe C13 -75.1(5) . . . . ?
C18 C17 Fe C14 37.3(4) . . . . ?
C18 C17 Fe C15 81.0(5) . . . . ?
C18 C17 Fe C16 119.5(6) . . . . ?
C8 C9 Fe C10 -120.2(6) . . . . ?
C8 C9 Fe C11 -157.9(6) . . . . ?
C8 C9 Fe C12 158.5(6) . . . . ?
C8 C9 Fe C13 120.5(7) . . . . ?
C8 C9 Fe C14 4.7(6) . . . . ?
C8 C9 Fe C15 -37.9(6) . . . . ?
C8 C9 Fe C16 -72.6(9) . . . . ?
C8 C9 Fe C17 76.8(10) . . . . ?
C8 C9 Fe C18 45.4(6) . . . . ?
C10 C9 Fe C11 -37.7(3) . . . . ?
C10 C9 Fe C12 -81.3(4) . . . . ?
C10 C9 Fe C13 -119.3(5) . . . . ?
C10 C9 Fe C14 124.9(4) . . . . ?
C10 C9 Fe C15 82.3(4) . . . . ?
C10 C9 Fe C16 47.6(7) . . . . ?
C10 C9 Fe C17 -163.0(8) . . . . ?
C10 C9 Fe C18 165.6(4) . . . . ?
C13 C9 Fe C10 119.3(5) . . . . ?
C13 C9 Fe C11 81.6(4) . . . . ?
C13 C9 Fe C12 38.0(4) . . . . ?
C13 C9 Fe C14 -115.8(4) . . . . ?
C13 C9 Fe C15 -158.3(4) . . . . ?
C13 C9 Fe C16 166.9(6) . . . . ?
C13 C9 Fe C17 -43.7(10) . . . . ?
C13 C9 Fe C18 -75.1(4) . . . . ?
C15 C16 Fe C9 49.1(8) . . . . ?
C15 C16 Fe C10 82.8(5) . . . . ?
C15 C16 Fe C11 125.5(4) . . . . ?
C15 C16 Fe C12 166.5(4) . . . . ?
C15 C16 Fe C13 -160.5(8) . . . . ?
C15 C16 Fe C14 -37.6(4) . . . . ?
C15 C16 Fe C17 -117.6(6) . . . . ?
C15 C16 Fe C18 -80.8(5) . . . . ?
C17 C16 Fe C9 166.7(5) . . . . ?
C17 C16 Fe C10 -159.6(4) . . . . ?
C17 C16 Fe C11 -116.9(5) . . . . ?
C17 C16 Fe C12 -75.9(5) . . . . ?
C17 C16 Fe C13 -42.9(11) . . . . ?
C17 C16 Fe C14 80.0(5) . . . . ?
C17 C16 Fe C15 117.6(6) . . . . ?
C17 C16 Fe C18 36.8(4) . . . . ?
C15 C14 Fe C9 -115.5(4) . . . . ?
C15 C14 Fe C10 -73.8(5) . . . . ?
C15 C14 Fe C11 -38.5(11) . . . . ?
C15 C14 Fe C12 165.0(6) . . . . ?
C15 C14 Fe C13 -159.3(4) . . . . ?
C15 C14 Fe C16 37.9(5) . . . . ?
C15 C14 Fe C17 82.3(5) . . . . ?
C15 C14 Fe C18 119.3(6) . . . . ?
C18 C14 Fe C9 125.2(4) . . . . ?
C18 C14 Fe C10 166.8(4) . . . . ?
C18 C14 Fe C11 -157.8(8) . . . . ?
C18 C14 Fe C12 45.7(8) . . . . ?
C18 C14 Fe C13 81.3(5) . . . . ?
C18 C14 Fe C15 -119.3(6) . . . . ?
C18 C14 Fe C16 -81.4(5) . . . . ?
C18 C14 Fe C17 -37.0(4) . . . . ?
C10 C11 Fe C9 37.6(4) . . . . ?
C10 C11 Fe C12 119.7(5) . . . . ?
C10 C11 Fe C13 82.2(4) . . . . ?
C10 C11 Fe C14 -45.4(11) . . . . ?
C10 C11 Fe C15 -75.2(5) . . . . ?
C10 C11 Fe C16 -116.1(4) . . . . ?
C10 C11 Fe C17 -158.7(4) . . . . ?
C10 C11 Fe C18 169.3(6) . . . . ?
C12 C11 Fe C9 -82.1(4) . . . . ?
C12 C11 Fe C10 -119.7(5) . . . . ?
C12 C11 Fe C13 -37.5(4) . . . . ?
C12 C11 Fe C14 -165.1(9) . . . . ?
C12 C11 Fe C15 165.1(4) . . . . ?
C12 C11 Fe C16 124.2(4) . . . . ?
C12 C11 Fe C17 81.6(4) . . . . ?
C12 C11 Fe C18 49.6(8) . . . . ?
C14 C15 Fe C9 82.9(5) . . . . ?
C14 C15 Fe C10 125.7(4) . . . . ?
C14 C15 Fe C11 167.3(4) . . . . ?
C14 C15 Fe C12 -158.7(8) . . . . ?
C14 C15 Fe C13 46.9(8) . . . . ?
C14 C15 Fe C16 -118.9(6) . . . . ?
C14 C15 Fe C17 -80.2(5) . . . . ?
C14 C15 Fe C18 -37.2(4) . . . . ?
C16 C15 Fe C9 -158.2(4) . . . . ?
C16 C15 Fe C10 -115.4(5) . . . . ?
C16 C15 Fe C11 -73.7(5) . . . . ?
C16 C15 Fe C12 -39.8(11) . . . . ?
C16 C15 Fe C13 165.8(6) . . . . ?
C16 C15 Fe C14 118.9(6) . . . . ?
C16 C15 Fe C17 38.7(5) . . . . ?
C16 C15 Fe C18 81.7(5) . . . . ?
C11 C12 Fe C9 81.4(4) . . . . ?
C11 C12 Fe C10 37.6(4) . . . . ?
C11 C12 Fe C13 119.9(5) . . . . ?
C11 C12 Fe C14 169.9(6) . . . . ?
C11 C12 Fe C15 -44.1(10) . . . . ?
C11 C12 Fe C16 -74.8(5) . . . . ?
C11 C12 Fe C17 -116.5(4) . . . . ?
C11 C12 Fe C18 -157.9(4) . . . . ?
C13 C12 Fe C9 -38.5(4) . . . . ?
C13 C12 Fe C10 -82.3(4) . . . . ?
C13 C12 Fe C11 -119.9(5) . . . . ?
C13 C12 Fe C14 50.0(8) . . . . ?
C13 C12 Fe C15 -164.0(8) . . . . ?
C13 C12 Fe C16 165.3(4) . . . . ?
C13 C12 Fe C17 123.5(4) . . . . ?
C13 C12 Fe C18 82.2(4) . . . . ?
C14 C18 Fe C9 -74.5(5) . . . . ?
C14 C18 Fe C10 -39.9(11) . . . . ?
C14 C18 Fe C11 165.4(6) . . . . ?
C14 C18 Fe C12 -159.6(4) . . . . ?
C14 C18 Fe C13 -116.7(4) . . . . ?
C14 C18 Fe C15 37.6(4) . . . . ?
C14 C18 Fe C16 81.6(5) . . . . ?
C14 C18 Fe C17 119.6(6) . . . . ?
C17 C18 Fe C9 166.0(4) . . . . ?
C17 C18 Fe C10 -159.5(8) . . . . ?
C17 C18 Fe C11 45.8(8) . . . . ?
C17 C18 Fe C12 80.8(5) . . . . ?
C17 C18 Fe C13 123.7(4) . . . . ?
C17 C18 Fe C14 -119.6(6) . . . . ?
C17 C18 Fe C15 -82.0(5) . . . . ?
C17 C18 Fe C16 -37.9(5) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N3 H3 O19 0.88(2) 1.87(3) 2.731(6) 168(7) .
O19 H19A O2 0.84 1.89 2.726(6) 179.6 1_455
O19 H19B O2 0.84 1.99 2.826(7) 179.8 2_567

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        22.49
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         1.357
_refine_diff_density_min         -0.886
_refine_diff_density_rms         0.143

#===END