#------------------------------------------------------------------------------
#$Date: 2017-11-08 07:01:44 +0200 (Wed, 08 Nov 2017) $
#$Revision: 202944 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/47/7044706.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_7044706
loop_
_publ_author_name
'Xue, Yuanshan'
'Tan, Xu'
'Zhou, Mengjie'
'Mei, Hua'
'Xu, Yan'
_publ_section_title
;
 Synthesis, structures and magnetic properties of two chiral mixed-valence
 iron(II, III) coordination networks
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C7DT03411C
_journal_year                    2017
_chemical_formula_sum            'C42 H43 Fe4 N3 O22.5'
_chemical_formula_weight         1173.19
_space_group_crystal_system      trigonal
_space_group_IT_number           155
_space_group_name_Hall           'R 3 2"'
_space_group_name_H-M_alt        'R 3 2 :H'
_symmetry_space_group_name_Hall  'R 3 2"'
_symmetry_space_group_name_H-M   'R 3 2 :H'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-10-10 deposited with the CCDC.
2017-11-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   16.210(8)
_cell_length_b                   16.210(8)
_cell_length_c                   18.208(18)
_cell_measurement_reflns_used    4015
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.94
_cell_measurement_theta_min      2.51
_cell_volume                     4143(5)
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Apex2 CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1126
_diffrn_reflns_av_unetI/netI     0.0630
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            7813
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.980
_diffrn_reflns_theta_min         1.832
_exptl_absorpt_coefficient_mu    1.105
_exptl_absorpt_correction_T_max  0.879
_exptl_absorpt_correction_T_min  0.834
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.411
_exptl_crystal_description       block
_exptl_crystal_F_000             1800
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.573
_refine_diff_density_min         -0.502
_refine_diff_density_rms         0.119
_refine_ls_abs_structure_details
;
 Flack x determined using 698 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.03(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     137
_refine_ls_number_reflns         1797
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0650
_refine_ls_R_factor_gt           0.0636
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1046P)²+33.9496P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1782
_refine_ls_wR_factor_ref         0.1795
_reflns_Friedel_coverage         0.786
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.985
_reflns_number_gt                1736
_reflns_number_total             1797
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7dt03411c2.cif
_cod_data_source_block           D1
_cod_original_cell_volume        4143(6)
_cod_original_formula_sum        'C42 H43 Fe4 N3 O22.50'
_cod_database_code               7044706
_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.
;
_shelx_estimated_absorpt_t_min   0.834
_shelx_estimated_absorpt_t_max   0.879
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+1/3'
'x-y+2/3, -y+1/3, -z+1/3'
'-x+2/3, -x+y+1/3, -z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+2/3'
'x-y+1/3, -y+2/3, -z+2/3'
'-x+1/3, -x+y+2/3, -z+2/3'
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
Fe1 Fe 0.54868(9) -0.6667 0.8333 0.0188(4) Uani 1 2 d S T P
Fe2 Fe 0.0000 -1.0000 1.0000 0.0363(9) Uani 1 6 d S T P
O1 O 0.5688(4) -0.8507(5) 0.9186(4) 0.0330(14) Uani 1 1 d . . .
O2 O 0.4821(5) -0.7786(5) 0.9048(3) 0.0333(14) Uani 1 1 d . . .
O3 O 0.1367(5) -0.9542(6) 0.9511(5) 0.053(2) Uani 1 1 d . . .
O4 O 0.6667 -0.6667 0.8333 0.018(3) Uani 1 6 d S T P
O5 O 0.4192(5) -0.6667 0.8333 0.038(2) Uani 1 2 d S T P
C1 C 0.4939(6) -0.8457(6) 0.9272(4) 0.0229(16) Uani 1 1 d . . .
C2 C 0.4108(6) -0.9270(6) 0.9653(4) 0.0261(16) Uani 1 1 d . . .
C3 C 0.4174(7) -1.0000 1.0000 0.023(2) Uani 1 2 d S T P
H3A H 0.4747 -1.0000 1.0000 0.027 Uiso 1 2 calc R U P
C4 C 0.3240(6) -0.9272(6) 0.9649(5) 0.032(2) Uani 1 1 d . . .
H4A H 0.3199 -0.8786 0.9411 0.038 Uiso 1 1 calc R U .
C5 C 0.2437(7) -1.0000 1.0000 0.034(3) Uani 1 2 d S T P
C6 C 0.1520(9) -1.0000 1.0000 0.040(3) Uani 1 2 d S T P
C7 C 0.4067(16) -0.6009(17) 0.8508(11) 0.042(5) Uani 0.5 1 d . . P
H7A H 0.4516 -0.5414 0.8328 0.051 Uiso 0.5 1 calc R U P
C8 C 0.333(3) -0.512(3) 0.903(2) 0.089(11) Uani 0.5 1 d . . P
H8A H 0.3346 -0.5038 0.9560 0.107 Uiso 0.5 1 calc R U P
H8B H 0.3926 -0.4607 0.8848 0.107 Uiso 0.5 1 calc R U P
C9 C 0.274(4) -0.496(4) 0.882(3) 0.14(2) Uani 0.5 1 d . . P
H9A H 0.2885 -0.4332 0.8977 0.208 Uiso 0.5 1 calc R U P
H9B H 0.2714 -0.4983 0.8291 0.208 Uiso 0.5 1 calc R U P
H9C H 0.2127 -0.5420 0.9013 0.208 Uiso 0.5 1 calc R U P
C10 C 0.275(2) -0.695(2) 0.9323(16) 0.065(7) Uani 0.5 1 d . . P
H10A H 0.2107 -0.7044 0.9359 0.078 Uiso 0.5 1 calc R U P
H10B H 0.2714 -0.7482 0.9058 0.078 Uiso 0.5 1 calc R U P
C11 C 0.310(2) -0.690(2) 1.0000 0.136(16) Uani 1 2 d S T P
H11A H 0.2707 -0.7449 1.0272 0.203 Uiso 0.5 1 d R U P
H11B H 0.3730 -0.6782 0.9955 0.203 Uiso 0.5 1 d R U P
H11C H 0.3125 -0.6343 1.0253 0.203 Uiso 0.5 1 d R U P
N1 N 0.3387(17) -0.6024(17) 0.8914(13) 0.057(5) Uani 0.5 1 d . . P
O1W O 0.3333 -0.3333 0.874(11) 0.21(3) Uani 0.25 3 d S TU 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'
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'
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
O4 Fe1 O2 94.82(19) . 17_436
O4 Fe1 O2 94.83(19) . .
O2 Fe1 O2 170.3(4) 17_436 .
O4 Fe1 O1 97.60(19) . 3_755
O2 Fe1 O1 87.5(3) 17_436 3_755
O2 Fe1 O1 91.2(3) . 3_755
O4 Fe1 O1 97.60(19) . 16_636
O2 Fe1 O1 91.2(3) 17_436 16_636
O2 Fe1 O1 87.5(3) . 16_636
O1 Fe1 O1 164.8(4) 3_755 16_636
O4 Fe1 O5 180.0 . .
O2 Fe1 O5 85.18(19) 17_436 .
O2 Fe1 O5 85.17(19) . .
O1 Fe1 O5 82.40(18) 3_755 .
O1 Fe1 O5 82.40(18) 16_636 .
O3 Fe2 O3 104.0(3) . 3_645
O3 Fe2 O3 92.9(5) . 4_647
O3 Fe2 O3 160.3(4) 3_645 4_647
O3 Fe2 O3 160.3(4) . 6_557
O3 Fe2 O3 61.5(4) 3_645 6_557
O3 Fe2 O3 104.0(3) 4_647 6_557
O3 Fe2 O3 61.5(4) . 5_437
O3 Fe2 O3 92.9(5) 3_645 5_437
O3 Fe2 O3 104.0(3) 4_647 5_437
O3 Fe2 O3 104.0(3) 6_557 5_437
O3 Fe2 O3 104.0(3) . 2_435
O3 Fe2 O3 104.0(3) 3_645 2_435
O3 Fe2 O3 61.5(4) 4_647 2_435
O3 Fe2 O3 92.9(5) 6_557 2_435
O3 Fe2 O3 160.3(4) 5_437 2_435
O3 Fe2 C6 133.5(3) . 3_645
O3 Fe2 C6 30.7(2) 3_645 3_645
O3 Fe2 C6 133.5(3) 4_647 3_645
O3 Fe2 C6 30.7(2) 6_557 3_645
O3 Fe2 C6 99.8(2) 5_437 3_645
O3 Fe2 C6 99.8(2) 2_435 3_645
O3 Fe2 C6 99.8(2) . 2_435
O3 Fe2 C6 133.5(3) 3_645 2_435
O3 Fe2 C6 30.7(2) 4_647 2_435
O3 Fe2 C6 99.8(2) 6_557 2_435
O3 Fe2 C6 133.5(3) 5_437 2_435
O3 Fe2 C6 30.7(2) 2_435 2_435
C6 Fe2 C6 120.000(1) 3_645 2_435
O3 Fe2 C6 30.7(2) . .
O3 Fe2 C6 99.8(2) 3_645 .
O3 Fe2 C6 99.8(2) 4_647 .
O3 Fe2 C6 133.5(3) 6_557 .
O3 Fe2 C6 30.7(2) 5_437 .
O3 Fe2 C6 133.5(3) 2_435 .
C6 Fe2 C6 120.000(2) 3_645 .
C6 Fe2 C6 120.000(3) 2_435 .
C1 O1 Fe1 124.4(5) . 2_535
C1 O2 Fe1 136.7(6) . .
C6 O3 Fe2 88.6(7) . .
Fe1 O4 Fe1 120.000(2) 2_535 3_755
Fe1 O4 Fe1 119.999(1) 2_535 .
Fe1 O4 Fe1 120.001(2) 3_755 .
C7 O5 C7 106(2) 17_436 .
C7 O5 Fe1 126.9(11) 17_436 .
C7 O5 Fe1 127.0(11) . .
O2 C1 O1 125.3(8) . .
O2 C1 C2 116.6(7) . .
O1 C1 C2 118.1(7) . .
C3 C2 C4 120.1(8) . .
C3 C2 C1 122.5(8) . .
C4 C2 C1 117.3(7) . .
C2 C3 C2 119.8(11) 5_437 .
C2 C3 H3A 120.1 5_437 .
C2 C3 H3A 120.1 . .
C5 C4 C2 120.6(8) . .
C5 C4 H4A 119.7 . .
C2 C4 H4A 119.7 . .
C4 C5 C4 118.8(11) 5_437 .
C4 C5 C6 120.6(5) 5_437 .
C4 C5 C6 120.6(5) . .
O3 C6 O3 121.3(13) 5_437 .
O3 C6 C5 119.4(7) 5_437 .
O3 C6 C5 119.4(7) . .
O3 C6 Fe2 60.6(7) 5_437 .
O3 C6 Fe2 60.6(7) . .
C5 C6 Fe2 180.0 . .
O5 C7 N1 129(2) . .
O5 C7 C7 36.9(11) . 17_436
N1 C7 C7 99.6(16) . 17_436
O5 C7 H7A 115.4 . .
N1 C7 H7A 115.5 . .
C7 C7 H7A 137.4 17_436 .
C9 C8 N1 128(5) . .
C9 C8 H8A 105.3 . .
N1 C8 H8A 105.3 . .
C9 C8 H8B 105.3 . .
N1 C8 H8B 105.3 . .
H8A C8 H8B 106.0 . .
C8 C9 H9A 109.5 . .
C8 C9 H9B 109.4 . .
H9A C9 H9B 109.5 . .
C8 C9 H9C 109.5 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
C11 C10 N1 109(3) . .
C11 C10 H10A 109.8 . .
N1 C10 H10A 109.8 . .
C11 C10 H10B 109.8 . .
N1 C10 H10B 109.8 . .
H10A C10 H10B 108.3 . .
C10 C11 C10 152(4) . 4_647
C10 C11 H11A 111.4 . .
C10 C11 H11A 40.8 4_647 .
C10 C11 H11B 108.5 . .
C10 C11 H11B 89.6 4_647 .
H11A C11 H11B 113.1 . .
C10 C11 H11C 107.4 . .
C10 C11 H11C 85.9 4_647 .
H11A C11 H11C 108.5 . .
H11B C11 H11C 107.6 . .
C7 N1 C10 117(2) . .
C7 N1 C8 121(2) . .
C10 N1 C8 122(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 O4 1.9126(17) .
Fe1 O2 2.048(6) 17_436
Fe1 O2 2.048(6) .
Fe1 O1 2.092(6) 3_755
Fe1 O1 2.092(6) 16_636
Fe1 O5 2.100(9) .
Fe2 O3 2.147(8) .
Fe2 O3 2.147(8) 3_645
Fe2 O3 2.147(8) 4_647
Fe2 O3 2.147(8) 6_557
Fe2 O3 2.147(8) 5_437
Fe2 O3 2.147(8) 2_435
Fe2 C6 2.463(14) 3_645
Fe2 C6 2.463(14) 2_435
Fe2 C6 2.463(14) .
O1 C1 1.265(11) .
O1 Fe1 2.092(6) 2_535
O2 C1 1.264(11) .
O3 C6 1.259(10) .
O4 Fe1 1.9126(17) 2_535
O4 Fe1 1.9126(18) 3_755
O5 C7 1.22(2) 17_436
O5 C7 1.22(2) .
C1 C2 1.502(11) .
C2 C3 1.393(10) .
C2 C4 1.404(13) .
C3 C2 1.393(10) 5_437
C3 H3A 0.9300 .
C4 C5 1.400(10) .
C4 H4A 0.9300 .
C5 C4 1.400(10) 5_437
C5 C6 1.487(18) .
C6 O3 1.259(10) 5_437
C7 N1 1.32(3) .
C7 C7 1.95(5) 17_436
C7 H7A 0.9300 .
C8 C9 1.19(5) .
C8 N1 1.53(4) .
C8 H8A 0.9700 .
C8 H8B 0.9700 .
C9 H9A 0.9600 .
C9 H9B 0.9600 .
C9 H9C 0.9600 .
C10 C11 1.34(3) .
C10 N1 1.52(4) .
C10 H10A 0.9700 .
C10 H10B 0.9700 .
C11 C10 1.34(3) 4_647
C11 H11A 0.9337 .
C11 H11B 0.9449 .
C11 H11C 0.9971 .
