#------------------------------------------------------------------------------
#$Date: 2019-11-26 06:57:13 +0200 (Tue, 26 Nov 2019) $
#$Revision: 242885 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/13/30/4133032.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_4133032
loop_
_publ_author_name
'Sahadevan, Suchithra Ashoka'
'Abhervé, Alexandre'
'Monni, Noemi'
'Sáenz de Pipaón, Cristina'
'Galán-Mascarós, José Ramón'
'Waerenborgh, João C'
'Vieira, Bruno J. C.'
'Auban-Senzier, Pascale'
'Pillet, Sébastien'
'Bendeif, El-Eulmi'
'Alemany, Pere'
'Canadell, Enric'
'Mercuri, Maria Laura'
'Avarvari, Narcis'
_publ_section_title
;
 Conducting Anilate-Based Mixed-Valence Fe(II)Fe(III) Coordination
 Polymer: Small-Polaron Hopping Model for Oxalate-Type Fe(II)Fe(III) 2D
 Networks.
;
_journal_issue                   39
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12611
_journal_page_last               12621
_journal_paper_doi               10.1021/jacs.8b08032
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         'C21 Cl3 Fe2 N3 O12, (C1 N6 H9)'
_chemical_formula_sum            'C22 H9 Cl3 Fe2 N9 O12'
_chemical_formula_weight         809.43
_space_group_crystal_system      trigonal
_space_group_IT_number           143
_space_group_name_Hall           'P 3'
_space_group_name_H-M_alt        'P 3'
_atom_sites_solution_hydrogens   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            1
_cell_length_a                   13.5493(16)
_cell_length_b                   13.5493(16)
_cell_length_c                   9.484(3)
_cell_measurement_reflns_used    8947
_cell_measurement_temperature    10(2)
_cell_measurement_theta_max      26.363
_cell_measurement_theta_min      2.147
_cell_volume                     1507.8(5)
_computing_cell_refinement       'CrysAlisPro 1.171.39.43b (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.43b (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.43b (Rigaku OD, 2018)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      10(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0604
_diffrn_reflns_av_unetI/netI     0.1094
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            8947
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.363
_diffrn_reflns_theta_min         2.147
_exptl_absorpt_coefficient_mu    0.653
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.704
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.43b (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    0.891
_exptl_crystal_description       block
_exptl_crystal_F_000             403
_exptl_crystal_size_max          0.219
_exptl_crystal_size_mid          0.191
_exptl_crystal_size_min          0.061
_refine_diff_density_max         0.476
_refine_diff_density_min         -0.501
_refine_diff_density_rms         0.059
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.57(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     125
_refine_ls_number_reflns         3976
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.1520
_refine_ls_R_factor_gt           0.0715
_refine_ls_shift/su_max          0.024
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0767P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1912
_refine_ls_wR_factor_ref         0.2391
_reflns_Friedel_coverage         1.000
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                1612
_reflns_number_total             3976
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja8b08032_si_003.cif
_cod_data_source_block           shelx
_cod_original_cell_volume        1507.8(6)
_cod_database_code               4133032
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
C1 C 0.1094(9) 0.5217(7) 0.6346(11) 0.073(3) Uani 1 1 d . . .
C2 C 0.1041(7) 0.5803(7) 0.5098(13) 0.075(4) Uani 1 1 d . . .
C3 C 0.0016(8) 0.5662(10) 0.4360(14) 0.098(4) Uani 1 1 d . . .
C4 C -0.1004(7) 0.4795(7) 0.5034(13) 0.072(3) Uani 1 1 d . . .
C5 C -0.1005(9) 0.4177(8) 0.6391(12) 0.080(3) Uani 1 1 d . . .
C6 C 0.0021(8) 0.4450(8) 0.6896(11) 0.071(3) Uani 1 1 d . . .
N1 N -0.0011(8) 0.3353(11) 0.8944(14) 0.148(6) Uani 1 1 d D . .
C7 C -0.0001(7) 0.3795(7) 0.8273(11) 0.054(3) Uani 1 1 d D . .
O1 O 0.2047(6) 0.5534(5) 0.6704(7) 0.072(2) Uani 1 1 d . . .
O2 O 0.2008(5) 0.6554(6) 0.4363(9) 0.086(2) Uani 1 1 d . . .
O3 O -0.1987(5) 0.4539(6) 0.4346(9) 0.094(3) Uani 1 1 d . . .
O4 O -0.2014(6) 0.3513(5) 0.6718(8) 0.085(2) Uani 1 1 d . . .
Cl1 Cl 0.0002(3) 0.6282(4) 0.2841(6) 0.168(2) Uani 1 1 d . . .
Fe1 Fe 0.3333 0.6667 0.5632(3) 0.0875(10) Uani 1 3 d S T P
Fe2 Fe -0.3333 0.3333 0.5624(3) 0.0873(11) Uani 1 3 d S T P
C8 C 0.3333 0.6667 0.0484 0.381 Uiso 1 3 d S . P
N2 N 0.2158 0.6179 0.0646 0.567 Uiso 1 1 d . . .
H2 H 0.1810 0.5475 0.0898 0.680 Uiso 1 1 d . U .
N3 N 0.1374 0.6702 0.0446 0.685 Uiso 1 1 d . . .
H3A H 0.1662 0.7403 0.0194 0.822 Uiso 1 1 d . U .
H3B H 0.0652 0.6291 0.0586 0.822 Uiso 1 1 d . U .
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'
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'
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'
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
O1 C1 C6 134.4(10) . .
O1 C1 C2 112.2(9) . .
C6 C1 C2 113.2(9) . .
O2 C2 C1 121.9(9) . .
O2 C2 C3 109.9(10) . .
C1 C2 C3 128.1(9) . .
C4 C3 C2 110.6(11) . .
C4 C3 Cl1 123.0(9) . .
C2 C3 Cl1 126.0(8) . .
O3 C4 C3 114.4(10) . .
O3 C4 C5 121.9(8) . .
C3 C4 C5 123.7(9) . .
O4 C5 C6 136.6(11) . .
O4 C5 C4 107.7(9) . .
C6 C5 C4 115.6(9) . .
C5 C6 C1 128.6(10) . .
C5 C6 C7 114.7(8) . .
C1 C6 C7 116.7(8) . .
N1 C7 C6 170.8(18) . .
C1 O1 Fe1 121.4(7) . .
C2 O2 Fe1 103.1(7) . .
C4 O3 Fe2 106.2(7) . .
C5 O4 Fe2 124.0(7) . .
O1 Fe1 O1 95.0(3) . 3_565
O1 Fe1 O1 95.0(3) . 2_665
O1 Fe1 O1 95.0(3) 3_565 2_665
O1 Fe1 O2 81.1(3) . .
O1 Fe1 O2 94.0(3) 3_565 .
O1 Fe1 O2 170.5(3) 2_665 .
O1 Fe1 O2 170.5(3) . 3_565
O1 Fe1 O2 81.1(3) 3_565 3_565
O1 Fe1 O2 94.0(3) 2_665 3_565
O2 Fe1 O2 90.5(3) . 3_565
O1 Fe1 O2 94.0(3) . 2_665
O1 Fe1 O2 170.5(3) 3_565 2_665
O1 Fe1 O2 81.1(3) 2_665 2_665
O2 Fe1 O2 90.5(3) . 2_665
O2 Fe1 O2 90.5(3) 3_565 2_665
O4 Fe2 O4 94.9(3) . 3_455
O4 Fe2 O4 94.9(3) . 2_565
O4 Fe2 O4 94.9(3) 3_455 2_565
O4 Fe2 O3 95.3(3) . 3_455
O4 Fe2 O3 80.1(3) 3_455 3_455
O4 Fe2 O3 168.9(3) 2_565 3_455
O4 Fe2 O3 168.9(3) . 2_565
O4 Fe2 O3 95.3(3) 3_455 2_565
O4 Fe2 O3 80.1(3) 2_565 2_565
O3 Fe2 O3 90.5(3) 3_455 2_565
O4 Fe2 O3 80.1(3) . .
O4 Fe2 O3 168.9(3) 3_455 .
O4 Fe2 O3 95.3(3) 2_565 .
O3 Fe2 O3 90.5(3) 3_455 .
O3 Fe2 O3 90.5(3) 2_565 .
N2 C8 N2 118.8 . 3_565
N2 C8 N2 118.8 . 2_665
N2 C8 N2 118.8 3_565 2_665
C8 N2 N3 130.5 . .
C8 N2 H2 114.8 . .
N3 N2 H2 114.8 . .
N2 N3 H3A 120.0 . .
N2 N3 H3B 120.0 . .
H3A N3 H3B 120.0 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 O1 1.188(11) .
C1 C6 1.398(13) .
C1 C2 1.447(15) .
C2 O2 1.379(12) .
C2 C3 1.480(14) .
C3 C4 1.441(13) .
C3 Cl1 1.672(13) .
C4 O3 1.362(11) .
C4 C5 1.536(15) .
C5 O4 1.243(11) .
C5 C6 1.336(13) .
C6 C7 1.571(12) .
N1 C7 0.869(10) .
O1 Fe1 1.937(7) .
O2 Fe1 2.103(7) .
O3 Fe2 2.117(7) .
O4 Fe2 1.974(7) .
Fe1 O1 1.937(7) 3_565
Fe1 O1 1.937(7) 2_665
Fe1 O2 2.103(7) 3_565
Fe1 O2 2.103(7) 2_665
Fe2 O4 1.974(7) 3_455
Fe2 O4 1.974(7) 2_565
Fe2 O3 2.117(7) 3_455
Fe2 O3 2.117(7) 2_565
C8 N2 1.3943 .
C8 N2 1.3943 3_565
C8 N2 1.3943 2_665
N2 N3 1.5554 .
N2 H2 0.8600 .
N3 H3A 0.8600 .
N3 H3B 0.8600 .
