#------------------------------------------------------------------------------
#$Date: 2016-03-25 23:03:05 +0100 (vie 25 de mar de 2016) $
#$Revision: 180057 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/03/7050339.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7050339
loop_
_publ_author_name
'Jaisa Fernandes Soares'
'David J. Evans'
'Geraldo R. Friedermann'
'Peter B. Hitchcock'
'G. Jeffery Leigh'
'Giovana G. Nunes'
'Dayane M. Reis'
'Eduardo L. Sa'
_publ_section_title
;
Iron(III) and Titanium(IV) Oxoalkoxide Chemistry:
Synthetic, Structural, Magnetochemical and Spectroscopic Studies of
[Ti3(m3-OPri)2(m-OPri)3(OPri)6][FeCl4] and [Fe5(m5-O)(m-OPri)8Cl5]
;
_journal_name_full               'New J.Chem.(Nouv.J.Chim.)'
_journal_year                    2004
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C24 H56 Cl5 Fe5 O9'
_chemical_formula_sum            'C24 H56 Cl5 Fe5 O9'
_chemical_formula_weight         945.19
_chemical_name_common            '[Fe5Cl5(O){OiPr}8]'
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 91.861(1)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.0547(3)
_cell_length_b                   9.9251(2)
_cell_length_c                   16.7734(5)
_cell_measurement_reflns_used    12217
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.028
_cell_measurement_theta_min      3.705
_cell_measurement_wavelength     0.71073
_cell_volume                     2005.78(9)
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      -0.645144E-1
_diffrn_orient_matrix_UB_12      0.128418E-1
_diffrn_orient_matrix_UB_13      0.352249E-1
_diffrn_orient_matrix_UB_21      -0.493596E-1
_diffrn_orient_matrix_UB_22      0.171993E-1
_diffrn_orient_matrix_UB_23      -0.479889E-1
_diffrn_orient_matrix_UB_31      -0.170398E-1
_diffrn_orient_matrix_UB_32      -0.984417E-1
_diffrn_orient_matrix_UB_33      -0.37893E-2
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.105
_diffrn_reflns_av_unetI/netI     0.0664
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            20515
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         3.96
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    2.138
_exptl_absorpt_correction_T_max  0.9417
_exptl_absorpt_correction_T_min  0.7479
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.565
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             974
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.782
_refine_diff_density_min         -0.588
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     196
_refine_ls_number_reflns         3527
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0902
_refine_ls_R_factor_gt           0.0557
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0585P)²+4.1745P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1221
_refine_ls_wR_factor_ref         0.1388
_reflns_number_gt                2532
_reflns_number_total             3527
_reflns_threshold_expression     >2sigma(I)
_cod_original_sg_symbol_H-M      'P 2/n'
_cod_database_code               7050339
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z-1/2'
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 0.25 0.97600(10) 0.25 0.0243(3) Uani 1 2 d S . .
Fe2 Fe 0.41716(6) 0.74841(7) 0.20657(5) 0.0252(2) Uani 1 1 d . . .
Fe3 Fe 0.18369(6) 0.74774(7) 0.12933(5) 0.0258(2) Uani 1 1 d . . .
Cl1 Cl 0.25 1.20197(19) 0.25 0.0391(5) Uani 1 2 d S . .
Cl2 Cl 0.57886(12) 0.72466(15) 0.14724(10) 0.0404(4) Uani 1 1 d . . .
Cl3 Cl 0.09887(13) 0.72205(16) 0.01011(10) 0.0409(4) Uani 1 1 d . . .
O1 O 0.25 0.7740(5) 0.25 0.0220(11) Uani 1 2 d S . .
O2 O 0.2163(3) 0.9368(3) 0.1328(2) 0.0276(9) Uani 1 1 d . . .
O3 O 0.4141(3) 0.9386(3) 0.2294(2) 0.0270(9) Uani 1 1 d . . .
O4 O 0.3259(3) 0.6604(4) 0.1232(2) 0.0289(9) Uani 1 1 d . . .
O5 O 0.4312(3) 0.6600(4) 0.3085(2) 0.0279(9) Uani 1 1 d . . .
C1 C 0.2440(5) 1.0345(6) 0.0708(4) 0.0437(16) Uani 1 1 d . . .
H1 H 0.2853 1.1084 0.0993 0.052 Uiso 1 1 calc R . .
C2 C 0.1420(6) 1.0974(7) 0.0375(4) 0.0486(17) Uani 1 1 d . . .
H2A H 0.098 1.1323 0.0811 0.073 Uiso 1 1 calc R . .
H2B H 0.0985 1.0302 0.0072 0.073 Uiso 1 1 calc R . .
H2C H 0.1616 1.1717 0.0021 0.073 Uiso 1 1 calc R . .
C3 C 0.3226(7) 0.9783(8) 0.0139(5) 0.064(2) Uani 1 1 d . . .
H3A H 0.3872 0.9412 0.0433 0.096 Uiso 1 1 calc R . .
H3B H 0.3468 1.0498 -0.0219 0.096 Uiso 1 1 calc R . .
H3C H 0.286 0.9067 -0.0174 0.096 Uiso 1 1 calc R . .
C4 C 0.5004(5) 1.0338(6) 0.2518(4) 0.0363(15) Uani 1 1 d . . .
H4 H 0.4647 1.1097 0.2806 0.044 Uiso 1 1 calc R . .
C5 C 0.5515(6) 1.0912(7) 0.1792(5) 0.056(2) Uani 1 1 d . . .
H5A H 0.4935 1.1319 0.1447 0.084 Uiso 1 1 calc R . .
H5B H 0.5885 1.0193 0.1501 0.084 Uiso 1 1 calc R . .
H5C H 0.6059 1.1602 0.1952 0.084 Uiso 1 1 calc R . .
C6 C 0.5850(5) 0.9704(7) 0.3087(5) 0.0511(18) Uani 1 1 d . . .
H6A H 0.5475 0.9351 0.3553 0.077 Uiso 1 1 calc R . .
H6B H 0.6397 1.0384 0.326 0.077 Uiso 1 1 calc R . .
H6C H 0.6228 0.8966 0.2818 0.077 Uiso 1 1 calc R . .
C7 C 0.3623(5) 0.5552(6) 0.0679(4) 0.0357(15) Uani 1 1 d . . .
H7 H 0.4352 0.5194 0.0887 0.043 Uiso 1 1 calc R . .
C8 C 0.3795(6) 0.6126(7) -0.0128(4) 0.0442(16) Uani 1 1 d . . .
H8A H 0.4348 0.6849 -0.0089 0.066 Uiso 1 1 calc R . .
H8B H 0.3091 0.649 -0.0344 0.066 Uiso 1 1 calc R . .
H8C H 0.4058 0.5417 -0.0482 0.066 Uiso 1 1 calc R . .
C9 C 0.2790(6) 0.4406(6) 0.0679(4) 0.0466(17) Uani 1 1 d . . .
H9A H 0.2722 0.4067 0.1224 0.07 Uiso 1 1 calc R . .
H9B H 0.3044 0.3678 0.0335 0.07 Uiso 1 1 calc R . .
H9C H 0.2066 0.4733 0.0478 0.07 Uiso 1 1 calc R . .
C10 C 0.5042(5) 0.5502(5) 0.3367(4) 0.0328(14) Uani 1 1 d . . .
H10 H 0.475 0.5154 0.3879 0.039 Uiso 1 1 calc R . .
C11 C 0.6204(5) 0.6009(6) 0.3533(4) 0.0426(16) Uani 1 1 d . . .
H11A H 0.6188 0.6734 0.3929 0.064 Uiso 1 1 calc R . .
H11B H 0.651 0.6353 0.3039 0.064 Uiso 1 1 calc R . .
H11C H 0.6669 0.527 0.374 0.064 Uiso 1 1 calc R . .
C12 C 0.4998(6) 0.4373(6) 0.2771(5) 0.0514(19) Uani 1 1 d . . .
H12A H 0.4229 0.4068 0.2692 0.077 Uiso 1 1 calc R . .
H12B H 0.5458 0.3623 0.2969 0.077 Uiso 1 1 calc R . .
H12C H 0.5279 0.4691 0.2262 0.077 Uiso 1 1 calc R . .
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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 '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'
