data_2005src1061
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          'C28 H20 Br2 Fe4 In2 O8'
_chemical_formula_sum
 'C28 H20 Br2 Fe4 In2 O8'
_chemical_formula_weight          1097.30
 
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'
 'Fe'  'Fe'   0.3463   0.8444
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Br'  'Br'  -0.2901   2.4595
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'In'  'In'  -0.7276   1.3100
 '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
_symmetry_space_group_name_hall   '-P 1'
 
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x, -y, -z'
 
_cell_length_a                    6.71040(10)
_cell_length_b                    9.9705(3)
_cell_length_c                    12.0246(4)
_cell_angle_alpha                 106.0930(10)
_cell_angle_beta                  90.916(2)
_cell_angle_gamma                 90.823(2)
_cell_volume                      772.74(4)
_cell_formula_units_Z             1
_cell_measurement_temperature     120(2)
_cell_measurement_reflns_used     3467
_cell_measurement_theta_min       2.91
_cell_measurement_theta_max       27.48
 
_exptl_crystal_description        plate
_exptl_crystal_colour             orange
_exptl_crystal_size_max           0.10
_exptl_crystal_size_mid           0.10
_exptl_crystal_size_min           0.02
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     2.358
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              524
_exptl_absorpt_coefficient_mu     5.929
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.5886
_exptl_absorpt_correction_T_max   0.8906
_exptl_absorpt_process_details    'SADABS V2.10 (Sheldrick, G.M., 2003)'
 
_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature       120(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_radiation_source          'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_monochromator   '10cm confocal mirrors'
_diffrn_measurement_device_type   'Bruker-Nonius KappaCCD Area Detector'
_diffrn_measurement_method        'φ and ω scans'
_diffrn_detector_area_resol_mean  9.091
_diffrn_standards_number          none
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         negligible
_diffrn_reflns_number             18313
_diffrn_reflns_av_R_equivalents   0.0350
_diffrn_reflns_av_sigmaI/netI     0.0280
_diffrn_reflns_limit_h_min        -8
_diffrn_reflns_limit_h_max        8
_diffrn_reflns_limit_k_min        -12
_diffrn_reflns_limit_k_max        12
_diffrn_reflns_limit_l_min        -15
_diffrn_reflns_limit_l_max        15
_diffrn_reflns_theta_min          3.48
_diffrn_reflns_theta_max          27.49
_reflns_number_total              3538
_reflns_number_gt                 3276
_reflns_threshold_expression      >2sigma(I)
 
_computing_data_collection        ?
_computing_cell_refinement        'DENZO, COLLECT'
_computing_data_reduction         'DENZO, COLLECT'
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)'
_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)+(0.0184P)²+0.7958P] 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          3538
_refine_ls_number_parameters      199
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0261
_refine_ls_R_factor_gt            0.0230
_refine_ls_wR_factor_ref          0.0513
_refine_ls_wR_factor_gt           0.0499
_refine_ls_goodness_of_fit_ref    1.110
_refine_ls_restrained_S_all       1.110
_refine_ls_shift/su_max           0.001
_refine_ls_shift/su_mean          0.000
 
loop_
 _atom_site_label
 _atom_site_type_symbol
 _atom_site_fract_x
 _atom_site_fract_y
 _atom_site_fract_z
 _atom_site_U_iso_or_equiv
 _atom_site_adp_type
 _atom_site_occupancy
 _atom_site_symmetry_multiplicity
 _atom_site_calc_flag
 _atom_site_refinement_flags
 _atom_site_disorder_assembly
 _atom_site_disorder_group
C1 C 0.2185(4) 0.3958(3) 0.1015(2) 0.0164(5) Uani 1 1 d . . .
C2 C -0.1361(4) 0.4920(3) 0.1425(2) 0.0181(5) Uani 1 1 d . . .
C3 C 0.1799(4) 0.6962(3) 0.3494(2) 0.0211(6) Uani 1 1 d . . .
H3 H 0.1602 0.6900 0.4259 0.025 Uiso 1 1 calc R . .
C4 C 0.0414(4) 0.7467(3) 0.2813(3) 0.0237(6) Uani 1 1 d . . .
H4 H -0.0884 0.7791 0.3036 0.028 Uiso 1 1 calc R . .
C5 C 0.1318(5) 0.7403(3) 0.1731(2) 0.0238(6) Uani 1 1 d . . .
H5 H 0.0729 0.7689 0.1113 0.029 Uiso 1 1 calc R . .
C6 C 0.3215(4) 0.6847(3) 0.1741(2) 0.0208(6) Uani 1 1 d . . .
H6 H 0.4138 0.6684 0.1129 0.025 Uiso 1 1 calc R . .
C7 C 0.3525(4) 0.6565(3) 0.2835(2) 0.0200(6) Uani 1 1 d . . .
H7 H 0.4687 0.6179 0.3075 0.024 Uiso 1 1 calc R . .
C8 C 0.0547(4) 0.0848(3) 0.1697(2) 0.0164(5) Uani 1 1 d . . .
C9 C 0.0352(4) 0.1067(3) 0.3840(2) 0.0172(5) Uani 1 1 d . . .
C10 C -0.3532(4) -0.0046(3) 0.1892(3) 0.0297(7) Uani 1 1 d . . .
H10 H -0.3306 -0.0932 0.1364 0.036 Uiso 1 1 calc R . .
C11 C -0.3685(4) 0.1240(3) 0.1605(3) 0.0260(6) Uani 1 1 d . . .
H11 H -0.3570 0.1362 0.0853 0.031 Uiso 1 1 calc R . .
C12 C -0.4036(4) 0.2300(3) 0.2628(2) 0.0210(6) Uani 1 1 d . . .
H12 H -0.4219 0.3260 0.2686 0.025 Uiso 1 1 calc R . .
C13 C -0.4070(4) 0.1682(3) 0.3556(2) 0.0221(6) Uani 1 1 d . . .
H13 H -0.4257 0.2154 0.4348 0.027 Uiso 1 1 calc R . .
C14 C -0.3771(4) 0.0222(3) 0.3084(3) 0.0277(7) Uani 1 1 d . . .
H14 H -0.3741 -0.0452 0.3508 0.033 Uiso 1 1 calc R . .
O1 O 0.2932(3) 0.3048(2) 0.03493(17) 0.0235(4) Uani 1 1 d . . .
O2 O -0.2970(3) 0.4628(2) 0.10787(17) 0.0278(5) Uani 1 1 d . . .
O3 O 0.1688(3) 0.0449(2) 0.09814(17) 0.0244(4) Uani 1 1 d . . .
O4 O 0.1439(3) 0.0827(2) 0.45057(17) 0.0243(4) Uani 1 1 d . . .
Fe1 Fe 0.10653(5) 0.53936(4) 0.19654(3) 0.01255(9) Uani 1 1 d . . .
Fe2 Fe -0.12703(5) 0.13471(4) 0.27617(3) 0.01367(9) Uani 1 1 d . . .
Br1 Br -0.25082(4) 0.55780(2) 0.47779(2) 0.01475(7) Uani 1 1 d . . .
In1 In 0.01478(2) 0.383293(17) 0.324884(14) 0.01208(6) 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
C1 O1 1.157(3) . ?
C1 Fe1 1.752(3) . ?
C2 O2 1.155(3) . ?
C2 Fe1 1.752(3) . ?
C3 C7 1.412(4) . ?
C3 C4 1.416(4) . ?
C3 Fe1 2.102(3) . ?
C4 C5 1.430(4) . ?
C4 Fe1 2.092(3) . ?
C5 C6 1.397(4) . ?
C5 Fe1 2.104(3) . ?
C6 C7 1.431(4) . ?
C6 Fe1 2.103(3) . ?
C7 Fe1 2.096(3) . ?
C8 O3 1.152(3) . ?
C8 Fe2 1.757(3) . ?
C9 O4 1.150(3) . ?
C9 Fe2 1.763(3) . ?
C10 C14 1.396(5) . ?
C10 C11 1.421(5) . ?
C10 Fe2 2.100(3) . ?
C11 C12 1.408(4) . ?
C11 Fe2 2.100(3) . ?
C12 C13 1.416(4) . ?
C12 Fe2 2.121(3) . ?
C13 C14 1.426(4) . ?
C13 Fe2 2.110(3) . ?
C14 Fe2 2.105(3) . ?
Fe1 In1 2.5527(4) . ?
Fe2 In1 2.5497(4) . ?
Br1 In1 2.7503(3) 2_566 ?
Br1 In1 2.8293(3) . ?
In1 Br1 2.7503(3) 2_566 ?
 
loop_
 _geom_angle_atom_site_label_1
 _geom_angle_atom_site_label_2
 _geom_angle_atom_site_label_3
 _geom_angle
 _geom_angle_site_symmetry_1
 _geom_angle_site_symmetry_3
 _geom_angle_publ_flag
O1 C1 Fe1 176.7(2) . . ?
O2 C2 Fe1 179.0(3) . . ?
C7 C3 C4 108.0(2) . . ?
C7 C3 Fe1 70.11(15) . . ?
C4 C3 Fe1 69.88(15) . . ?
C3 C4 C5 107.8(3) . . ?
C3 C4 Fe1 70.67(15) . . ?
C5 C4 Fe1 70.51(15) . . ?
C6 C5 C4 108.2(2) . . ?
C6 C5 Fe1 70.57(15) . . ?
C4 C5 Fe1 69.63(15) . . ?
C5 C6 C7 108.0(2) . . ?
C5 C6 Fe1 70.63(15) . . ?
C7 C6 Fe1 69.81(14) . . ?
C3 C7 C6 108.0(2) . . ?
C3 C7 Fe1 70.60(15) . . ?
C6 C7 Fe1 70.33(14) . . ?
O3 C8 Fe2 176.2(2) . . ?
O4 C9 Fe2 176.7(2) . . ?
C14 C10 C11 108.0(3) . . ?
C14 C10 Fe2 70.83(16) . . ?
C11 C10 Fe2 70.25(15) . . ?
C12 C11 C10 108.2(3) . . ?
C12 C11 Fe2 71.32(16) . . ?
C10 C11 Fe2 70.20(16) . . ?
C11 C12 C13 107.9(3) . . ?
C11 C12 Fe2 69.73(16) . . ?
C13 C12 Fe2 70.00(15) . . ?
C12 C13 C14 107.6(3) . . ?
C12 C13 Fe2 70.87(16) . . ?
C14 C13 Fe2 70.07(16) . . ?
C10 C14 C13 108.3(3) . . ?
C10 C14 Fe2 70.39(16) . . ?
C13 C14 Fe2 70.39(15) . . ?
C2 Fe1 C1 94.91(12) . . ?
C2 Fe1 C4 95.54(12) . . ?
C1 Fe1 C4 159.99(12) . . ?
C2 Fe1 C7 161.73(12) . . ?
C1 Fe1 C7 102.63(12) . . ?
C4 Fe1 C7 66.20(11) . . ?
C2 Fe1 C3 125.12(12) . . ?
C1 Fe1 C3 138.60(12) . . ?
C4 Fe1 C3 39.46(11) . . ?
C7 Fe1 C3 39.30(11) . . ?
C2 Fe1 C6 134.45(11) . . ?
C1 Fe1 C6 94.45(11) . . ?
C4 Fe1 C6 66.19(11) . . ?
C7 Fe1 C6 39.86(10) . . ?
C3 Fe1 C6 66.31(11) . . ?
C2 Fe1 C5 100.50(12) . . ?
C1 Fe1 C5 121.15(12) . . ?
C4 Fe1 C5 39.85(12) . . ?
C7 Fe1 C5 66.04(11) . . ?
C3 Fe1 C5 66.28(11) . . ?
C6 Fe1 C5 38.80(11) . . ?
C2 Fe1 In1 81.66(8) . . ?
C1 Fe1 In1 88.79(8) . . ?
C4 Fe1 In1 109.58(8) . . ?
C7 Fe1 In1 103.54(8) . . ?
C3 Fe1 In1 87.28(7) . . ?
C6 Fe1 In1 143.02(8) . . ?
C5 Fe1 In1 149.35(8) . . ?
C8 Fe2 C9 91.92(12) . . ?
C8 Fe2 C10 97.08(12) . . ?
C9 Fe2 C10 125.25(12) . . ?
C8 Fe2 C11 96.03(12) . . ?
C9 Fe2 C11 163.64(12) . . ?
C10 Fe2 C11 39.55(12) . . ?
C8 Fe2 C14 129.71(12) . . ?
C9 Fe2 C14 98.34(12) . . ?
C10 Fe2 C14 38.78(13) . . ?
C11 Fe2 C14 65.65(12) . . ?
C8 Fe2 C13 161.02(11) . . ?
C9 Fe2 C13 104.58(12) . . ?
C10 Fe2 C13 65.82(11) . . ?
C11 Fe2 C13 65.68(11) . . ?
C14 Fe2 C13 39.55(11) . . ?
C8 Fe2 C12 127.72(12) . . ?
C9 Fe2 C12 139.16(11) . . ?
C10 Fe2 C12 65.77(11) . . ?
C11 Fe2 C12 38.96(11) . . ?
C14 Fe2 C12 65.73(11) . . ?
C13 Fe2 C12 39.12(11) . . ?
C8 Fe2 In1 88.61(8) . . ?
C9 Fe2 In1 87.55(8) . . ?
C10 Fe2 In1 146.25(9) . . ?
C11 Fe2 In1 106.87(9) . . ?
C14 Fe2 In1 140.61(8) . . ?
C13 Fe2 In1 101.22(8) . . ?
C12 Fe2 In1 84.45(7) . . ?
In1 Br1 In1 98.234(9) 2_566 . ?
Fe2 In1 Fe1 131.592(13) . . ?
Fe2 In1 Br1 110.991(11) . 2_566 ?
Fe1 In1 Br1 111.470(11) . 2_566 ?
Fe2 In1 Br1 107.558(11) . . ?
Fe1 In1 Br1 100.481(11) . . ?
Br1 In1 Br1 81.766(9) 2_566 . ?
 
_diffrn_measured_fraction_theta_max    0.996
_diffrn_reflns_theta_full              27.49
_diffrn_measured_fraction_theta_full   0.996
_refine_diff_density_max    0.629
_refine_diff_density_min   -0.741
_refine_diff_density_rms    0.115
