#------------------------------------------------------------------------------
#$Date: 2016-03-26 00:02:01 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180056 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/02/7050224.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_7050224
loop_
_publ_author_name
'Sébastien Floquet'
'M. Carmen Muñoz'
'Eric Rivière'
'René Clément'
'Jean-Paul Audière'
'Marie-Laure Boillot'
_publ_section_title
;
 Structural effects on the magnetic properties of ferric complexes in
 molecular materials or a lamellar CdPS3 host matrix
;
_journal_issue                   4
_journal_name_full               'New J. Chem.'
_journal_page_first              535
_journal_page_last               541
_journal_paper_doi               10.1039/b311371j
_journal_volume                  28
_journal_year                    2004
_chemical_formula_sum            'C20 H20 Cl5 Fe N4 O6'
_chemical_formula_weight         645.50
_chemical_name_systematic
;
?
;
_space_group_IT_number           56
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ab 2ac'
_symmetry_space_group_name_H-M   'P c c n'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.4143(19)
_cell_length_b                   13.959(3)
_cell_length_c                   16.933(5)
_cell_measurement_temperature    293(2)
_cell_volume                     2461.6(10)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Enraf Nonius CAD4'
_diffrn_measurement_method       (-2(
_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  0.0182
_diffrn_reflns_av_sigmaI/netI    0.0363
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            2857
_diffrn_reflns_theta_full        24.97
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         2.41
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.202
_exptl_absorpt_correction_T_max  0.999
_exptl_absorpt_correction_T_min  0.902
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.742
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1308
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.624
_refine_diff_density_min         -0.420
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         2148
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0737
_refine_ls_R_factor_gt           0.0458
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0563P)²+4.3116P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1130
_refine_ls_wR_factor_ref         0.1248
_reflns_number_gt                1535
_reflns_number_total             2148
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b311371j.txt
_cod_data_source_block           ja127
_cod_original_sg_symbol_H-M      Pccn
_cod_database_code               7050224
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-x, y+1/2, -z+1/2'
'x+1/2, -y, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'x, -y-1/2, z-1/2'
'-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
Cl1 Cl 0.07068(13) 0.64827(8) 0.32160(8) 0.0589(4) Uani 1 1 d . . .
Fe Fe -0.2500 0.7500 0.49624(4) 0.0332(2) Uani 1 2 d S . .
Cl2 Cl 0.18013(13) 1.00466(9) 0.22896(7) 0.0584(4) Uani 1 1 d . . .
Cl3 Cl 0.2500 0.7500 0.55795(10) 0.0590(5) Uani 1 2 d S . .
C6 C -0.0656(4) 0.9021(3) 0.3907(2) 0.0378(9) Uani 1 1 d . . .
C5 C 0.0043(5) 0.9649(3) 0.3425(2) 0.0446(11) Uani 1 1 d . . .
H5 H -0.007(4) 1.028(3) 0.349(2) 0.034(11) Uiso 1 1 d . . .
C3 C 0.1107(4) 0.8314(3) 0.2821(2) 0.0411(10) Uani 1 1 d . . .
H3 H 0.165(4) 0.807(3) 0.238(2) 0.040(11) Uiso 1 1 d . . .
C7 C -0.1576(5) 0.9425(3) 0.4458(3) 0.0458(11) Uani 1 1 d . . .
H7 H -0.157(5) 1.006(4) 0.452(3) 0.064(15) Uiso 1 1 d . . .
N1 N -0.2281(3) 0.8944(3) 0.4930(2) 0.0480(10) Uani 1 1 d . . .
O1 O -0.1111(3) 0.7382(2) 0.42627(17) 0.0496(8) Uani 1 1 d . . .
C1 C -0.0484(4) 0.8017(3) 0.3846(2) 0.0392(10) Uani 1 1 d . . .
N2 N -0.3704(4) 0.7890(3) 0.5908(3) 0.0513(11) Uani 1 1 d . . .
H2 H -0.429(5) 0.763(4) 0.583(3) 0.064(19) Uiso 1 1 d . . .
C4 C 0.0907(4) 0.9291(3) 0.2893(2) 0.0411(10) Uani 1 1 d . . .
C2 C 0.0452(4) 0.7699(3) 0.3297(2) 0.0404(10) Uani 1 1 d . . .
C10 C -0.3227(5) 0.7503(5) 0.6653(3) 0.0714(15) Uani 1 1 d . . .
H10A H -0.3545 0.6856 0.6724 0.23(2) Uiso 1 1 calc R . .
H10B H -0.3537 0.7891 0.7088 0.23(2) Uiso 1 1 calc R . .
O2 O 0.1542(5) 0.7935(4) 0.6053(3) 0.128(2) Uani 1 1 d . . .
C8 C -0.3182(7) 0.9460(4) 0.5439(5) 0.122(3) Uani 1 1 d . . .
H8A H -0.2695 0.9874 0.5788 0.23(2) Uiso 1 1 calc R . .
H8B H -0.3716 0.9866 0.5110 0.23(2) Uiso 1 1 calc R . .
C9 C -0.3936(9) 0.8910(5) 0.5873(5) 0.133(4) Uani 1 1 d . . .
H9A H -0.4808 0.9001 0.5686 0.23(2) Uiso 1 1 calc R . .
H9B H -0.3905 0.9151 0.6410 0.23(2) Uiso 1 1 calc R . .
O3 O 0.1991(10) 0.6826(6) 0.5136(6) 0.275(6) Uani 1 1 d . . .
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'
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
O1 Fe O1 101.7(2) 2_465 . ?
O1 Fe N1 89.07(13) 2_465 2_465 ?
O1 Fe N1 88.97(14) . 2_465 ?
O1 Fe N1 88.97(14) 2_465 . ?
O1 Fe N1 89.07(13) . . ?
N1 Fe N1 176.9(2) 2_465 . ?
O1 Fe N2 164.11(17) 2_465 2_465 ?
O1 Fe N2 89.89(16) . 2_465 ?
N1 Fe N2 80.24(16) 2_465 2_465 ?
N1 Fe N2 102.16(17) . 2_465 ?
O1 Fe N2 89.89(16) 2_465 . ?
O1 Fe N2 164.11(17) . . ?
N1 Fe N2 102.16(17) 2_465 . ?
N1 Fe N2 80.24(16) . . ?
N2 Fe N2 81.0(2) 2_465 . ?
O3 Cl3 O3 110.4(11) . 2_565 ?
O3 Cl3 O2 110.2(5) . . ?
O3 Cl3 O2 107.5(4) 2_565 . ?
O3 Cl3 O2 107.5(4) . 2_565 ?
O3 Cl3 O2 110.2(5) 2_565 2_565 ?
O2 Cl3 O2 111.1(5) . 2_565 ?
C5 C6 C1 120.7(4) . . ?
C5 C6 C7 118.3(4) . . ?
C1 C6 C7 121.0(4) . . ?
C4 C5 C6 119.8(4) . . ?
C4 C5 H5 122(3) . . ?
C6 C5 H5 118(3) . . ?
C2 C3 C4 119.6(4) . . ?
C2 C3 H3 121(2) . . ?
C4 C3 H3 119(2) . . ?
N1 C7 C6 125.2(4) . . ?
N1 C7 H7 117(3) . . ?
C6 C7 H7 118(3) . . ?
C7 N1 C8 118.6(4) . . ?
C7 N1 Fe 127.2(3) . . ?
C8 N1 Fe 113.7(3) . . ?
C1 O1 Fe 131.8(3) . . ?
O1 C1 C2 119.0(4) . . ?
O1 C1 C6 124.6(4) . . ?
C2 C1 C6 116.4(4) . . ?
C9 N2 C10 117.2(6) . . ?
C9 N2 Fe 108.9(4) . . ?
C10 N2 Fe 111.0(3) . . ?
C9 N2 H2 110(5) . . ?
C10 N2 H2 105(5) . . ?
Fe N2 H2 104(5) . . ?
C5 C4 C3 121.1(4) . . ?
C5 C4 Cl2 121.2(4) . . ?
C3 C4 Cl2 117.7(3) . . ?
C3 C2 C1 122.4(4) . . ?
C3 C2 Cl1 119.8(3) . . ?
C1 C2 Cl1 117.8(3) . . ?
N2 C10 C10 110.0(4) . 2_465 ?
N2 C10 H10A 109.7 . . ?
C10 C10 H10A 109.7 2_465 . ?
N2 C10 H10B 109.7 . . ?
C10 C10 H10B 109.7 2_465 . ?
H10A C10 H10B 108.2 . . ?
C9 C8 N1 115.0(5) . . ?
C9 C8 H8A 108.5 . . ?
N1 C8 H8A 108.5 . . ?
C9 C8 H8B 108.5 . . ?
N1 C8 H8B 108.5 . . ?
H8A C8 H8B 107.5 . . ?
C8 C9 N2 119.7(5) . . ?
C8 C9 H9A 107.4 . . ?
N2 C9 H9A 107.4 . . ?
C8 C9 H9B 107.4 . . ?
N2 C9 H9B 107.4 . . ?
H9A C9 H9B 106.9 . . ?
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
Cl1 C2 1.724(4) . ?
Fe O1 1.877(3) 2_465 ?
Fe O1 1.877(3) . ?
Fe N1 2.029(4) 2_465 ?
Fe N1 2.029(4) . ?
Fe N2 2.105(4) 2_465 ?
Fe N2 2.105(4) . ?
Cl2 C4 1.739(4) . ?
Cl3 O3 1.316(6) . ?
Cl3 O3 1.316(6) 2_565 ?
Cl3 O2 1.417(5) . ?
Cl3 O2 1.417(5) 2_565 ?
C6 C5 1.402(6) . ?
C6 C1 1.417(6) . ?
C6 C7 1.452(6) . ?
C5 C4 1.368(6) . ?
C5 H5 0.89(4) . ?
C3 C2 1.360(6) . ?
C3 C4 1.386(6) . ?
C3 H3 1.01(4) . ?
C7 N1 1.276(6) . ?
C7 H7 0.89(5) . ?
N1 C8 1.463(6) . ?
O1 C1 1.308(5) . ?
C1 C2 1.417(6) . ?
N2 C9 1.445(8) . ?
N2 C10 1.460(6) . ?
N2 H2 0.72(5) . ?
C10 C10 1.514(10) 2_465 ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C8 C9 1.323(8) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
