data_s93
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 Dr. J. H. R. Tucker
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          'C44 H40 Fe2 N6 O4, 2(H2 O)'
_chemical_formula_sum
 'C42 H44 Fe2 N6 O6'
_chemical_formula_weight          840.53
 
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            monoclinic
_symmetry_space_group_name_H-M    P2(1)/n
_symmetry_space_group_name_hall   '-P 2yn'
 
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                    12.8537(12)
_cell_length_b                    8.4774(10)
_cell_length_c                    17.831(2)
_cell_angle_alpha                 90.00
_cell_angle_beta                  94.064(3)
_cell_angle_gamma                 90.00
_cell_volume                      1938.1(4)
_cell_formula_units_Z             2
_cell_measurement_temperature     120(2)
_cell_measurement_reflns_used     4924
_cell_measurement_theta_min       2.910
_cell_measurement_theta_max       27.485
 
_exptl_crystal_description        Blade
_exptl_crystal_colour             Orange
_exptl_crystal_size_max           0.06
_exptl_crystal_size_mid           0.03
_exptl_crystal_size_min           0.01
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.440
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              876
_exptl_absorpt_coefficient_mu     0.805
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.9533
_exptl_absorpt_correction_T_max   0.9920
_exptl_absorpt_process_details    'SORTAV Blessing (1997)'
_exptl_special_details
;
 PLEASE NOTE cell_measurement_ fields are not relevant to area detector data,
 the entire data set is used to refine the cell, which is indexed from all
 observed reflections in a 10 degree phi range.
;
_diffrn_ambient_temperature       120(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'Nonius FR591 rotating anode'
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   'Nonius KappaCCD Area Detector'
_diffrn_measurement_method        'φ and ω scans to fill Ewald Sphere'
_diffrn_detector_area_resol_mean  9.091
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             14887
_diffrn_reflns_av_R_equivalents   0.2219
_diffrn_reflns_av_sigmaI/netI     0.2566
_diffrn_reflns_limit_h_min        -15
_diffrn_reflns_limit_h_max        15
_diffrn_reflns_limit_k_min        -10
_diffrn_reflns_limit_k_max        10
_diffrn_reflns_limit_l_min        -21
_diffrn_reflns_limit_l_max        21
_diffrn_reflns_theta_min          3.06
_diffrn_reflns_theta_max          25.03
_reflns_number_total              3277
_reflns_number_gt                 1348
_reflns_threshold_expression      >2sigma(I)
 
_computing_data_collection
' DENZO (Otwinowski and Minor, 1997)'
_computing_cell_refinement        
' DENZO (Otwinowski & Minor, 1997) and COLLECT (Hooft, 1998)'
_computing_data_reduction         
' DENZO (Otwinowski & Minor, 1997) and COLLECT (Hooft, 1998)'
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1997a)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997b)' 
_computing_molecular_graphics     'PLATON (Spek, 1990)'
_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.
;
 
_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)+(0.0633P)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     mixed
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        ?
_refine_ls_number_reflns          3277
_refine_ls_number_parameters      271
_refine_ls_number_restraints      3
_refine_ls_R_factor_all           0.2305
_refine_ls_R_factor_gt            0.0813
_refine_ls_wR_factor_ref          0.1794
_refine_ls_wR_factor_gt           0.1348
_refine_ls_goodness_of_fit_ref    0.937
_refine_ls_restrained_S_all       0.936
_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
Fe1 Fe 0.89951(8) 0.63529(12) 0.12374(7) 0.0423(4) Uani 1 1 d . . .
O2 O 0.8621(4) 1.0404(5) 0.0274(3) 0.0523(17) Uani 1 1 d . . .
O1 O 0.8419(4) 0.3377(5) 0.2703(3) 0.0501(16) Uani 1 1 d . . .
N2 N 0.9759(4) 0.2359(7) 0.2083(4) 0.0401(18) Uani 1 1 d . . .
H2 H 1.0022 0.2314 0.1641 0.048 Uiso 1 1 calc R . .
N1 N 1.1105(5) 0.0730(7) 0.2386(4) 0.045(2) Uani 1 1 d . . .
C11 C 0.8864(6) 0.3276(8) 0.2111(5) 0.039(2) Uani 1 1 d . . .
N3 N 0.7515(5) 1.0269(6) 0.1195(4) 0.0426(19) Uani 1 1 d . . .
H3 H 0.7386 0.9830 0.1626 0.051 Uiso 1 1 calc R . .
C12 C 1.0301(5) 0.1501(9) 0.2653(5) 0.039(2) Uani 1 1 d . . .
C20 C 0.5860(6) 1.0654(8) 0.0420(5) 0.045(2) Uani 1 1 d . . .
C19 C 0.6787(6) 1.1390(9) 0.0863(5) 0.046(2) Uani 1 1 d . . .
H19A H 0.7156 1.2088 0.0525 0.055 Uiso 1 1 calc R . .
H19B H 0.6527 1.2054 0.1267 0.055 Uiso 1 1 calc R . .
C9 C 1.0505(6) 0.7063(9) 0.1507(5) 0.048(3) Uani 1 1 d . . .
H9 H 1.1123 0.6480 0.1441 0.057 Uiso 1 1 calc R . .
C18 C 0.8380(6) 0.9869(9) 0.0875(5) 0.041(2) Uani 1 1 d . . .
C3 C 0.8438(6) 0.5256(8) 0.0260(5) 0.044(2) Uani 1 1 d . . .
H3A H 0.8579 0.5510 -0.0242 0.052 Uiso 1 1 calc R . .
C5 C 0.7654(6) 0.5174(8) 0.1378(5) 0.045(2) Uani 1 1 d . . .
H5 H 0.7187 0.5365 0.1758 0.054 Uiso 1 1 calc R . .
C2 C 0.9019(6) 0.4196(8) 0.0744(5) 0.039(2) Uani 1 1 d . . .
H2A H 0.9627 0.3634 0.0628 0.047 Uiso 1 1 calc R . .
C6 C 0.9112(6) 0.8732(8) 0.1302(5) 0.036(2) Uani 1 1 d . . .
C1 C 0.8528(6) 0.4131(8) 0.1431(5) 0.040(2) Uani 1 1 d . . .
C4 C 0.7610(6) 0.5868(8) 0.0659(5) 0.042(2) Uani 1 1 d . . .
H4 H 0.7109 0.6621 0.0472 0.050 Uiso 1 1 calc R . .
C10 C 1.0006(6) 0.8104(8) 0.0984(5) 0.044(2) Uani 1 1 d . . .
H10 H 1.0228 0.8346 0.0500 0.052 Uiso 1 1 calc R . .
C16 C 1.1713(7) -0.0143(10) 0.2876(7) 0.055(3) Uani 1 1 d . . .
C17 C 1.2608(6) -0.0937(9) 0.2524(6) 0.070(3) Uani 1 1 d . . .
H17A H 1.2359 -0.1901 0.2267 0.105 Uiso 1 1 calc R . .
H17B H 1.3152 -0.1205 0.2917 0.105 Uiso 1 1 calc R . .
H17C H 1.2896 -0.0220 0.2161 0.105 Uiso 1 1 calc R . .
C21 C 0.4843(7) 1.1034(9) 0.0568(6) 0.060(3) Uani 1 1 d . . .
H21 H 0.4733 1.1742 0.0968 0.072 Uiso 1 1 calc R . .
C15 C 1.1526(8) -0.0249(10) 0.3618(7) 0.069(3) Uani 1 1 d . . .
H15 H 1.1956 -0.0892 0.3948 0.083 Uiso 1 1 calc R . .
C22 C 0.6017(7) 0.9578(10) -0.0157(6) 0.058(3) Uani 1 1 d . . .
H22 H 0.6702 0.9273 -0.0264 0.069 Uiso 1 1 calc R . .
C8 C 0.9915(6) 0.7038(8) 0.2158(5) 0.044(2) Uani 1 1 d . . .
H8 H 1.0065 0.6419 0.2596 0.053 Uiso 1 1 calc R . .
C13 C 1.0085(6) 0.1500(10) 0.3392(6) 0.061(3) Uani 1 1 d . . .
H13 H 0.9525 0.2108 0.3558 0.073 Uiso 1 1 calc R . .
C14 C 1.0695(8) 0.0600(12) 0.3891(6) 0.077(3) Uani 1 1 d . . .
H14 H 1.0558 0.0553 0.4407 0.092 Uiso 1 1 calc R . .
C7 C 0.9086(6) 0.8076(8) 0.2036(5) 0.041(2) Uani 1 1 d . . .
H7 H 0.8583 0.8311 0.2385 0.049 Uiso 1 1 calc R . .
O1W O 0.8727(4) 0.8211(6) -0.0899(4) 0.0524(17) Uani 1 1 d D . .
H1W H 0.874(5) 0.874(7) -0.133(2) 0.04(2) Uiso 1 1 d D . .
H2W H 0.884(10) 0.893(8) -0.054(3) 0.20(7) Uiso 1 1 d 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
Fe1 C1 2.015(7) . ?
Fe1 C5 2.024(7) . ?
Fe1 C6 2.025(7) . ?
Fe1 C2 2.030(7) . ?
Fe1 C4 2.036(8) . ?
Fe1 C8 2.038(8) . ?
Fe1 C7 2.037(7) . ?
Fe1 C10 2.044(7) . ?
Fe1 C9 2.056(8) . ?
Fe1 C3 2.059(8) . ?
O2 C18 1.223(9) . ?
O1 C11 1.238(8) . ?
N2 C11 1.393(8) . ?
N2 C12 1.395(9) . ?
N1 C12 1.338(9) . ?
N1 C16 1.352(11) . ?
C11 C1 1.451(11) . ?
N3 C18 1.329(8) . ?
N3 C19 1.432(9) . ?
C12 C13 1.365(11) . ?
C20 C21 1.391(9) . ?
C20 C22 1.400(11) . ?
C20 C19 1.516(11) . ?
C9 C10 1.406(11) . ?
C9 C8 1.430(10) . ?
C18 C6 1.514(11) . ?
C3 C4 1.420(9) . ?
C3 C2 1.421(10) . ?
C5 C4 1.408(11) . ?
C5 C1 1.428(10) . ?
C2 C1 1.419(10) . ?
C6 C10 1.420(9) . ?
C6 C7 1.425(10) . ?
C16 C15 1.365(13) . ?
C16 C17 1.507(10) . ?
C21 C22 1.382(11) 3_675 ?
C15 C14 1.403(12) . ?
C22 C21 1.382(11) 3_675 ?
C8 C7 1.387(9) . ?
C13 C14 1.375(12) . ?
 
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
C1 Fe1 C5 41.4(3) . . ?
C1 Fe1 C6 160.6(3) . . ?
C5 Fe1 C6 123.1(3) . . ?
C1 Fe1 C2 41.1(3) . . ?
C5 Fe1 C2 69.4(3) . . ?
C6 Fe1 C2 156.6(3) . . ?
C1 Fe1 C4 68.7(3) . . ?
C5 Fe1 C4 40.6(3) . . ?
C6 Fe1 C4 106.8(3) . . ?
C2 Fe1 C4 68.8(3) . . ?
C1 Fe1 C8 106.9(3) . . ?
C5 Fe1 C8 119.5(3) . . ?
C6 Fe1 C8 68.5(3) . . ?
C2 Fe1 C8 125.4(3) . . ?
C4 Fe1 C8 154.5(3) . . ?
C1 Fe1 C7 123.6(3) . . ?
C5 Fe1 C7 106.0(3) . . ?
C6 Fe1 C7 41.1(3) . . ?
C2 Fe1 C7 161.2(3) . . ?
C4 Fe1 C7 120.3(3) . . ?
C8 Fe1 C7 39.8(3) . . ?
C1 Fe1 C10 156.8(3) . . ?
C5 Fe1 C10 161.1(3) . . ?
C6 Fe1 C10 40.8(3) . . ?
C2 Fe1 C10 121.9(3) . . ?
C4 Fe1 C10 125.5(3) . . ?
C8 Fe1 C10 68.3(3) . . ?
C7 Fe1 C10 68.2(3) . . ?
C1 Fe1 C9 121.4(3) . . ?
C5 Fe1 C9 156.1(4) . . ?
C6 Fe1 C9 68.3(3) . . ?
C2 Fe1 C9 108.8(3) . . ?
C4 Fe1 C9 162.7(3) . . ?
C8 Fe1 C9 40.9(3) . . ?
C7 Fe1 C9 67.7(3) . . ?
C10 Fe1 C9 40.1(3) . . ?
C1 Fe1 C3 68.5(3) . . ?
C5 Fe1 C3 68.5(3) . . ?
C6 Fe1 C3 121.2(3) . . ?
C2 Fe1 C3 40.7(3) . . ?
C4 Fe1 C3 40.6(3) . . ?
C8 Fe1 C3 163.2(3) . . ?
C7 Fe1 C3 156.2(3) . . ?
C10 Fe1 C3 109.2(3) . . ?
C9 Fe1 C3 126.6(3) . . ?
C11 N2 C12 129.6(7) . . ?
C12 N1 C16 117.6(8) . . ?
O1 C11 N2 120.0(8) . . ?
O1 C11 C1 123.3(7) . . ?
N2 C11 C1 116.6(7) . . ?
C18 N3 C19 122.3(7) . . ?
N1 C12 C13 123.9(8) . . ?
N1 C12 N2 110.7(7) . . ?
C13 C12 N2 125.3(8) . . ?
C21 C20 C22 118.4(7) . . ?
C21 C20 C19 121.3(8) . . ?
C22 C20 C19 120.2(7) . . ?
N3 C19 C20 114.1(6) . . ?
C10 C9 C8 107.7(6) . . ?
C10 C9 Fe1 69.5(4) . . ?
C8 C9 Fe1 68.9(4) . . ?
O2 C18 N3 123.6(8) . . ?
O2 C18 C6 119.3(7) . . ?
N3 C18 C6 117.1(7) . . ?
C4 C3 C2 107.9(7) . . ?
C4 C3 Fe1 68.8(4) . . ?
C2 C3 Fe1 68.6(5) . . ?
C4 C5 C1 107.5(7) . . ?
C4 C5 Fe1 70.2(4) . . ?
C1 C5 Fe1 69.0(4) . . ?
C1 C2 C3 107.6(7) . . ?
C1 C2 Fe1 68.9(4) . . ?
C3 C2 Fe1 70.7(4) . . ?
C10 C6 C7 107.0(7) . . ?
C10 C6 C18 122.0(7) . . ?
C7 C6 C18 131.0(7) . . ?
C10 C6 Fe1 70.3(4) . . ?
C7 C6 Fe1 69.9(4) . . ?
C18 C6 Fe1 124.3(5) . . ?
C2 C1 C5 108.3(8) . . ?
C2 C1 C11 128.0(7) . . ?
C5 C1 C11 123.5(7) . . ?
C2 C1 Fe1 70.0(4) . . ?
C5 C1 Fe1 69.6(4) . . ?
C11 C1 Fe1 122.4(6) . . ?
C5 C4 C3 108.7(7) . . ?
C5 C4 Fe1 69.2(5) . . ?
C3 C4 Fe1 70.6(4) . . ?
C9 C10 C6 108.3(7) . . ?
C9 C10 Fe1 70.4(4) . . ?
C6 C10 Fe1 68.9(4) . . ?
N1 C16 C15 122.0(8) . . ?
N1 C16 C17 113.5(9) . . ?
C15 C16 C17 124.5(10) . . ?
C22 C21 C20 122.6(8) 3_675 . ?
C16 C15 C14 119.5(9) . . ?
C21 C22 C20 118.9(8) 3_675 . ?
C7 C8 C9 108.0(8) . . ?
C7 C8 Fe1 70.1(5) . . ?
C9 C8 Fe1 70.2(5) . . ?
C12 C13 C14 118.6(8) . . ?
C13 C14 C15 118.3(9) . . ?
C8 C7 C6 108.9(7) . . ?
C8 C7 Fe1 70.1(4) . . ?
C6 C7 Fe1 69.0(4) . . ?
 
_diffrn_measured_fraction_theta_max    0.956
_diffrn_reflns_theta_full              25.03
_diffrn_measured_fraction_theta_full   0.956
_refine_diff_density_max    0.407
_refine_diff_density_min   -0.353
_refine_diff_density_rms    0.087
