#------------------------------------------------------------------------------
#$Date: 2016-03-23 02:51:16 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179211 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/41/4314162.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_4314162
loop_
_publ_author_name
'Wendy Hibbs'
'Petra J. van Koningsbruggen'
'Atta M. Arif'
'William W. Shum'
'Joel S. Miller'
_publ_section_title
;
 One- and Two-Step Spin-Crossover Behavior of [FeII(isoxazole)6]2+ and the
 Structure and Magnetic Properties of Triangular
 [FeIII3O(OAc)6(isoxazole)3][ClO4]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5645
_journal_page_last               5653
_journal_paper_doi               10.1021/ic034226p
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C21 H27 Cl Fe3 N3 O20'
_chemical_formula_weight         844.46
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'I 2y'
_symmetry_space_group_name_H-M   'I 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 109.820(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.1547(7)
_cell_length_b                   16.5497(11)
_cell_length_c                   10.3205(9)
_cell_measurement_temperature    200.00(10)
_cell_volume                     1631.7(2)
_computing_cell_refinement       Denzo
_computing_data_collection       'Nonius Collect'
_computing_data_reduction        Denzo
_computing_molecular_graphics    'Wingx, Oretp3'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR97
_diffrn_ambient_temperature      200.00(10)
_diffrn_measured_fraction_theta_full 0.870
_diffrn_measured_fraction_theta_max 0.870
_diffrn_measurement_device_type  'Nonius Kappaccd'
_diffrn_measurement_method       'Phi plus Omega scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0437
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            2775
_diffrn_reflns_theta_full        33.08
_diffrn_reflns_theta_max         33.08
_diffrn_reflns_theta_min         4.20
_exptl_absorpt_coefficient_mu    1.485
_exptl_absorpt_correction_type   Scalepack
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.719
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             858
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.541
_refine_diff_density_min         -0.517
_refine_diff_density_rms         0.083
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.52(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     225
_refine_ls_number_reflns         2775
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0512
_refine_ls_R_factor_gt           0.0405
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0632P)²+0.7738P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1006
_refine_ls_wR_factor_ref         0.1066
_reflns_number_gt                2402
_reflns_number_total             2775
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic034226p_s3.cif
_cod_data_source_block           '[FeIII3O(OAc)6(oxazole)3][ClO4]'
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/adriana/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1555 2011-01-17 13:19:09Z saulius 

The following automatic conversions were performed:

'_cell_measurement_temperature' value '200(0.1)' was changed to
'200.00(10)' - precision was
estimated.

'_diffrn_ambient_temperature' value '200(0.1)' was
changed to '200.00(10)' - precision was estimated.

Automatic conversion script
Id: cif_fix_values 1569 2011-02-09 13:29:24Z adriana 
;
_cod_original_sg_symbol_H-M      'I 2'
_cod_database_code               4314162
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, y+1/2, -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 0.32803(5) 0.06065(3) 0.44273(6) 0.02530(13) Uani 1 1 d . . .
Fe2 Fe 0.5000 -0.11120(4) 0.5000 0.02544(16) Uani 1 2 d S . .
Cl Cl 0.5000 0.00337(17) 0.0000 0.0694(6) Uani 1 2 d S . .
N1 N 0.5000 -0.2433(3) 0.5000 0.0306(9) Uani 1 2 d S . .
N2 N 0.1302(3) 0.1271(2) 0.3766(4) 0.0300(7) Uani 1 1 d . . .
O1 O 0.3812(3) 0.1406(2) 0.3228(4) 0.0378(7) Uani 1 1 d . . .
O2 O 0.6156(3) 0.1392(2) 0.3977(4) 0.0366(7) Uani 1 1 d . . .
O3 O 0.6462(3) -0.12203(19) 0.4081(4) 0.0371(7) Uani 1 1 d . . .
O4 O 0.7643(3) -0.0056(2) 0.4509(4) 0.0368(7) Uani 1 1 d . . .
O5 O 0.6457(3) -0.12438(19) 0.6862(3) 0.0365(6) Uani 1 1 d . . .
O6 O 0.7615(3) -0.0067(2) 0.7283(4) 0.0357(7) Uani 1 1 d . . .
O7C O 0.3824(7) -0.2886(3) 0.4485(5) 0.0635(14) Uani 0.88 1 d P . .
O8 O 0.1203(6) 0.2082(3) 0.3612(6) 0.0736(16) Uani 1 1 d . . .
O9 O 0.5000 0.0036(2) 0.5000 0.0249(7) Uani 1 2 d S . .
C1 C 0.4983(4) 0.1595(2) 0.3151(5) 0.0323(8) Uani 1 1 d . . .
C2 C 0.4932(6) 0.2114(4) 0.1937(8) 0.0621(19) Uani 1 1 d . . .
H2A H 0.3955 0.2226 0.1386 0.093 Uiso 1 1 calc R . .
H2B H 0.5386 0.1829 0.1369 0.093 Uiso 1 1 calc R . .
H2C H 0.5422 0.2624 0.2265 0.093 Uiso 1 1 calc R . .
C3 C 0.7351(4) -0.0735(3) 0.3938(5) 0.0340(8) Uani 1 1 d . . .
C4 C 0.8140(6) -0.0983(4) 0.3009(8) 0.0602(17) Uani 1 1 d . . .
H4A H 0.7823 -0.1519 0.2625 0.090 Uiso 1 1 calc R . .
H4B H 0.9143 -0.1002 0.3536 0.090 Uiso 1 1 calc R . .
H4C H 0.7967 -0.0591 0.2257 0.090 Uiso 1 1 calc R . .
C5 C 0.7333(4) -0.0760(3) 0.7635(5) 0.0337(8) Uani 1 1 d . . .
C6 C 0.8073(7) -0.1033(4) 0.9079(7) 0.0599(16) Uani 1 1 d . . .
H6A H 0.8719 -0.0610 0.9583 0.090 Uiso 1 1 calc R . .
H6B H 0.8599 -0.1528 0.9069 0.090 Uiso 1 1 calc R . .
H6C H 0.7385 -0.1140 0.9533 0.090 Uiso 1 1 calc R . .
C7 C 0.4340(14) -0.3688(4) 0.4682(7) 0.115(5) Uani 1 1 d . . .
H7 H 0.3784 -0.4159 0.4383 0.138 Uiso 1 1 calc R . .
C8 C -0.0231(12) 0.2243(7) 0.3170(10) 0.112(5) Uani 1 1 d . . .
H8 H -0.0641 0.2762 0.2937 0.134 Uiso 1 1 calc R . .
C9 C -0.0922(7) 0.1576(10) 0.3124(9) 0.119(5) Uani 1 1 d . . .
H9 H -0.1908 0.1539 0.2900 0.142 Uiso 1 1 calc R . .
C10 C 0.0036(4) 0.0900(4) 0.3465(6) 0.0498(14) Uani 1 1 d . . .
H10 H -0.0166 0.0340 0.3477 0.060 Uiso 1 1 calc R . .
O10 O 0.5000 -0.0817(8) 0.0000 0.189(9) Uani 1 2 d S . .
O11 O 0.6278(11) 0.0467(7) 0.0381(19) 0.138(5) Uani 0.75 1 d P . .
O12 O 0.480(3) 0.0070(13) 0.121(2) 0.207(10) Uani 0.75 1 d P . .
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'
N N 0.0061 0.0033 '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'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
O9 Fe1 O4 96.31(12) . 2_656 ?
O9 Fe1 O1 96.21(11) . . ?
O4 Fe1 O1 167.48(13) 2_656 . ?
O9 Fe1 O2 95.15(11) . 2_656 ?
O4 Fe1 O2 87.78(15) 2_656 2_656 ?
O1 Fe1 O2 91.01(16) . 2_656 ?
O9 Fe1 O6 95.25(12) . 2_656 ?
O4 Fe1 O6 91.21(16) 2_656 2_656 ?
O1 Fe1 O6 87.73(15) . 2_656 ?
O2 Fe1 O6 169.60(13) 2_656 2_656 ?
O9 Fe1 N2 179.67(15) . . ?
O4 Fe1 N2 83.96(12) 2_656 . ?
O1 Fe1 N2 83.51(13) . . ?
O2 Fe1 N2 84.67(15) 2_656 . ?
O6 Fe1 N2 84.93(13) 2_656 . ?
O9 Fe2 O5 96.26(10) . . ?
O9 Fe2 O5 96.26(10) . 2_656 ?
O5 Fe2 O5 167.48(19) . 2_656 ?
O9 Fe2 O3 95.09(10) . . ?
O5 Fe2 O3 91.11(15) . . ?
O5 Fe2 O3 87.78(15) 2_656 . ?
O9 Fe2 O3 95.09(10) . 2_656 ?
O5 Fe2 O3 87.78(15) . 2_656 ?
O5 Fe2 O3 91.11(15) 2_656 2_656 ?
O3 Fe2 O3 169.83(19) . 2_656 ?
O9 Fe2 N1 180.0 . . ?
O5 Fe2 N1 83.74(10) . . ?
O5 Fe2 N1 83.74(10) 2_656 . ?
O3 Fe2 N1 84.91(10) . . ?
O3 Fe2 N1 84.91(10) 2_656 . ?
O12 Cl O12 174.9(18) . 2_655 ?
O12 Cl O10 92.6(9) . . ?
O12 Cl O10 92.6(9) 2_655 . ?
O12 Cl O11 97.7(11) . . ?
O12 Cl O11 79.6(14) 2_655 . ?
O10 Cl O11 120.4(5) . . ?
O12 Cl O11 79.6(14) . 2_655 ?
O12 Cl O11 97.7(11) 2_655 2_655 ?
O10 Cl O11 120.4(5) . 2_655 ?
O11 Cl O11 119.2(9) . 2_655 ?
O7C N1 O7C 112.9(6) . 2_656 ?
O7C N1 Fe2 123.6(3) . . ?
O7C N1 Fe2 123.6(3) 2_656 . ?
O8 N2 C10 113.3(4) . . ?
O8 N2 Fe1 124.0(3) . . ?
C10 N2 Fe1 122.7(3) . . ?
C1 O1 Fe1 131.4(3) . . ?
C1 O2 Fe1 131.8(3) . 2_656 ?
C3 O3 Fe2 132.1(3) . . ?
C3 O4 Fe1 132.0(3) . 2_656 ?
C5 O5 Fe2 132.3(3) . . ?
C5 O6 Fe1 132.2(3) . 2_656 ?
N1 O7C C7 103.2(7) . . ?
N2 O8 C8 104.8(7) . . ?
Fe1 O9 Fe1 120.3(2) 2_656 . ?
Fe1 O9 Fe2 119.86(10) 2_656 . ?
Fe1 O9 Fe2 119.86(10) . . ?
O2 C1 O1 126.3(4) . . ?
O2 C1 C2 118.4(4) . . ?
O1 C1 C2 115.3(4) . . ?
O3 C3 O4 125.7(4) . . ?
O3 C3 C4 117.4(4) . . ?
O4 C3 C4 116.9(4) . . ?
O5 C5 O6 125.0(4) . . ?
O5 C5 C6 116.6(4) . . ?
O6 C5 C6 118.3(4) . . ?
C7 C7 O7C 110.2(5) 2_656 . ?
C9 C8 O8 109.9(6) . . ?
C8 C9 C10 109.8(5) . . ?
N2 C10 C9 102.2(7) . . ?
Cl O11 O12 48.0(6) . 2_655 ?
Cl O12 O11 52.4(10) . 2_655 ?
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 O9 1.8944(19) . ?
Fe1 O4 1.997(3) 2_656 ?
Fe1 O1 2.006(3) . ?
Fe1 O2 2.023(3) 2_656 ?
Fe1 O6 2.024(3) 2_656 ?
Fe1 N2 2.187(3) . ?
Fe2 O9 1.901(4) . ?
Fe2 O5 2.000(3) . ?
Fe2 O5 2.000(3) 2_656 ?
Fe2 O3 2.023(3) . ?
Fe2 O3 2.023(3) 2_656 ?
Fe2 N1 2.185(5) . ?
Cl O12 1.329(15) . ?
Cl O12 1.329(15) 2_655 ?
Cl O10 1.408(13) . ?
Cl O11 1.417(10) . ?
Cl O11 1.417(10) 2_655 ?
N1 O7C 1.356(5) . ?
N1 O7C 1.356(5) 2_656 ?
N2 O8 1.351(5) . ?
N2 C10 1.362(5) . ?
O1 C1 1.258(5) . ?
O2 C1 1.252(5) . ?
O2 Fe1 2.023(3) 2_656 ?
O3 C3 1.254(5) . ?
O4 C3 1.256(5) . ?
O4 Fe1 1.997(3) 2_656 ?
O5 C5 1.260(5) . ?
O6 C5 1.264(5) . ?
O6 Fe1 2.024(3) 2_656 ?
O7C C7 1.417(11) . ?
O8 C8 1.397(11) . ?
O9 Fe1 1.8944(19) 2_656 ?
C1 C2 1.506(7) . ?
C3 C4 1.501(7) . ?
C5 C6 1.493(8) . ?
C7 C7 1.28(3) 2_656 ?
C8 C9 1.299(18) . ?
C9 C10 1.446(13) . ?
O11 O12 1.76(3) 2_655 ?
O12 O11 1.76(3) 2_655 ?
