#------------------------------------------------------------------------------
#$Date: 2016-03-26 22:10:51 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180493 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/62/7216223.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_7216223
loop_
_publ_author_name
'Wang, Lei'
'Wang, Wenqiang'
'Guo, Dong'
'Zhang, Ao'
'Song, Yaoguang'
'Zhang, Yiheng'
'Huang, Keke'
_publ_section_title
;
 Design and syntheses of hybrid supramolecular architectures: based on
 [Fe(C2O4)3]3− metallotectons and diverse organic cations
;
_journal_issue                   24
_journal_name_full               CrystEngComm
_journal_page_first              5437
_journal_paper_doi               10.1039/c4ce00357h
_journal_volume                  16
_journal_year                    2014
_chemical_formula_sum            'C34 H32 Cl4 Fe2 N8 O12'
_chemical_formula_weight         998.18
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                113.219(8)
_cell_angle_beta                 109.138(7)
_cell_angle_gamma                99.294(6)
_cell_formula_units_Z            1
_cell_length_a                   10.6758(8)
_cell_length_b                   10.7457(8)
_cell_length_c                   10.8774(9)
_cell_measurement_temperature    293(2)
_cell_volume                     1020.84(18)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 'ACTA 50'
_diffrn_measured_fraction_theta_max 0.834
_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  0.0343
_diffrn_reflns_av_sigmaI/netI    0.0615
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8984
_diffrn_reflns_theta_full        'ACTA 50'
_diffrn_reflns_theta_max         29.51
_diffrn_reflns_theta_min         2.19
_exptl_absorpt_coefficient_mu    1.043
_exptl_crystal_colour            emerald
_exptl_crystal_density_diffrn    1.624
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             508
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.422
_refine_diff_density_min         -0.471
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     275
_refine_ls_number_reflns         4752
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0877
_refine_ls_R_factor_gt           0.0498
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0577P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1086
_refine_ls_wR_factor_ref         0.1294
_reflns_number_gt                3078
_reflns_number_total             4752
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ce00357h2.cif
_cod_data_source_block           compound3
_cod_original_cell_volume        1020.84(14)
_cod_original_sg_symbol_H-M      p-1
_cod_database_code               7216223
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Fe1 Fe 0.47474(4) 0.30412(5) 1.10471(5) 0.03912(16) Uani 1 1 d .
O2 O 0.5863(2) 0.5311(2) 1.1810(2) 0.0393(5) Uani 1 1 d .
O3 O 0.6439(2) 0.2832(2) 1.0532(2) 0.0437(5) Uani 1 1 d .
O6 O 0.6165(2) 0.3339(2) 1.2965(2) 0.0437(5) Uani 1 1 d .
O1 O 0.6067(2) 0.6774(2) 1.0829(2) 0.0444(6) Uani 1 1 d .
N2 N 0.9734(3) 0.3215(3) 0.7687(3) 0.0385(6) Uani 1 1 d .
O5 O 0.8398(2) 0.3538(3) 1.4131(3) 0.0641(7) Uani 1 1 d .
C5 C 1.0282(3) 0.1466(3) 0.5845(3) 0.0350(7) Uani 1 1 d .
C6 C 1.1194(3) 0.0797(3) 0.6307(4) 0.0484(9) Uani 1 1 d .
H6 H 1.2005 0.1330 0.7194 0.058 Uiso 1 1 calc R
C14 C 0.4872(3) 0.9749(4) 0.6115(4) 0.0495(9) Uani 1 1 d .
H14 H 0.4780 0.9589 0.6866 0.059 Uiso 1 1 calc R
N1 N 0.9007(3) 0.3159(3) 0.9289(3) 0.0502(7) Uani 1 1 d .
H1 H 0.8970 0.3094 1.0041 0.060 Uiso 1 1 calc R
O4 O 0.8722(2) 0.3116(3) 1.1613(3) 0.0560(6) Uani 1 1 d .
N4 N 0.7182(3) 0.7865(3) 0.6048(3) 0.0432(7) Uani 1 1 d .
C3 C 0.8440(4) 0.3366(4) 0.7282(4) 0.0519(9) Uani 1 1 d .
H3A H 0.7959 0.3468 0.6463 0.062 Uiso 1 1 calc R
C17 C 0.5547(3) 0.5592(3) 1.0761(3) 0.0332(7) Uani 1 1 d .
N3 N 0.9113(3) 0.7429(4) 0.6626(4) 0.0599(9) Uani 1 1 d .
C4 C 1.0560(3) 0.3045(3) 0.6810(4) 0.0425(8) Uani 1 1 d .
H4A H 1.1555 0.3519 0.7473 0.051 Uiso 1 1 calc R
H4B H 1.0305 0.3494 0.6190 0.051 Uiso 1 1 calc R
C16 C 0.7389(3) 0.3316(3) 1.3035(4) 0.0399(8) Uani 1 1 d .
C12 C 0.5335(3) 0.8857(3) 0.5177(4) 0.0415(8) Uani 1 1 d .
C13 C 0.5459(3) 0.9108(4) 0.4066(4) 0.0490(9) Uani 1 1 d .
H13 H 0.5767 0.8510 0.3430 0.059 Uiso 1 1 calc R
C15 C 0.7540(3) 0.3052(3) 1.1604(4) 0.0373(7) Uani 1 1 d .
C7 C 1.0917(3) -0.0650(3) 0.5467(4) 0.0479(9) Uani 1 1 d .
H7 H 1.1547 -0.1081 0.5790 0.057 Uiso 1 1 calc R
C1 C 1.0048(4) 0.3100(3) 0.8903(4) 0.0464(8) Uani 1 1 d .
H1A H 1.0878 0.2993 0.9411 0.056 Uiso 1 1 calc R
C2 C 0.7996(4) 0.3340(4) 0.8288(4) 0.0576(10) Uani 1 1 d .
H2 H 0.7148 0.3429 0.8302 0.069 Uiso 1 1 calc R
C8 C 0.7778(4) 0.6871(4) 0.5683(4) 0.0516(9) Uani 1 1 d .
H8 H 0.7329 0.5940 0.4895 0.062 Uiso 1 1 calc R
C10 C 0.8176(4) 0.9075(4) 0.7276(5) 0.0614(11) Uani 1 1 d .
H10 H 0.8042 0.9933 0.7777 0.074 Uiso 1 1 calc R
C9 C 0.9393(4) 0.8788(5) 0.7626(5) 0.0698(12) Uani 1 1 d .
H9 H 1.0259 0.9413 0.8411 0.084 Uiso 1 1 calc R
C11 C 0.5658(3) 0.7597(4) 0.5355(5) 0.0558(10) Uani 1 1 d .
H11A H 0.5240 0.7408 0.5960 0.067 Uiso 1 1 calc R
H11B H 0.5233 0.6748 0.4388 0.067 Uiso 1 1 calc R
Cl1 Cl 0.32648(9) 0.39107(10) 1.20331(12) 0.0570(3) Uani 1 1 d .
H3 H 0.981(4) 0.709(4) 0.666(4) 0.073(13) Uiso 1 1 d .
Cl2 Cl 0.34815(10) 0.06957(10) 0.98881(13) 0.0697(3) 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'
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
O6 Fe1 O1 159.07(9) . 2_667
O6 Fe1 O3 79.57(8) . .
O1 Fe1 O3 85.25(9) 2_667 .
O6 Fe1 O2 85.86(8) . .
O1 Fe1 O2 77.30(8) 2_667 .
O3 Fe1 O2 79.86(8) . .
O6 Fe1 Cl2 103.06(7) . .
O1 Fe1 Cl2 93.20(7) 2_667 .
O3 Fe1 Cl2 98.02(7) . .
O2 Fe1 Cl2 170.37(6) . .
O6 Fe1 Cl1 94.46(7) . .
O1 Fe1 Cl1 96.47(7) 2_667 .
O3 Fe1 Cl1 164.48(7) . .
O2 Fe1 Cl1 85.46(6) . .
Cl2 Fe1 Cl1 97.28(4) . .
C17 O2 Fe1 111.23(18) . .
C15 O3 Fe1 114.1(2) . .
C16 O6 Fe1 116.4(2) . .
C17 O1 Fe1 117.37(18) . 2_667
C1 N2 C3 108.2(3) . .
C1 N2 C4 126.0(3) . .
C3 N2 C4 125.4(3) . .
C7 C5 C6 118.5(3) 2_756 .
C7 C5 C4 121.1(3) 2_756 .
C6 C5 C4 120.4(3) . .
C7 C6 C5 120.7(3) . .
C12 C14 C13 120.1(3) . 2_676
C1 N1 C2 107.9(3) . .
C8 N4 C10 108.4(3) . .
C8 N4 C11 124.2(3) . .
C10 N4 C11 126.8(3) . .
C2 C3 N2 106.8(3) . .
O2 C17 O1 126.2(3) . .
O2 C17 C17 118.0(3) . 2_667
O1 C17 C17 115.8(3) . 2_667
C8 N3 C9 109.8(3) . .
N2 C4 C5 110.4(2) . .
O5 C16 O6 125.5(3) . .
O5 C16 C15 120.1(3) . .
O6 C16 C15 114.3(3) . .
C13 C12 C14 119.2(3) . .
C13 C12 C11 120.9(3) . .
C14 C12 C11 119.8(3) . .
C12 C13 C14 120.7(3) . 2_676
O4 C15 O3 126.2(3) . .
O4 C15 C16 118.3(3) . .
O3 C15 C16 115.4(3) . .
C6 C7 C5 120.8(3) . 2_756
N1 C1 N2 109.3(3) . .
C3 C2 N1 107.7(3) . .
N3 C8 N4 108.1(3) . .
C9 C10 N4 106.8(3) . .
N3 C9 C10 106.9(4) . .
N4 C11 C12 112.3(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 O6 1.997(2) .
Fe1 O1 2.043(2) 2_667
Fe1 O3 2.079(2) .
Fe1 O2 2.208(2) .
Fe1 Cl2 2.2462(10) .
Fe1 Cl1 2.3085(10) .
O2 C17 1.248(3) .
O3 C15 1.261(3) .
O6 C16 1.288(4) .
O1 C17 1.264(3) .
O1 Fe1 2.043(2) 2_667
N2 C1 1.315(4) .
N2 C3 1.363(4) .
N2 C4 1.479(4) .
O5 C16 1.221(4) .
C5 C7 1.378(4) 2_756
C5 C6 1.381(4) .
C5 C4 1.515(4) .
C6 C7 1.376(4) .
C14 C12 1.385(5) .
C14 C13 1.399(4) 2_676
N1 C1 1.313(4) .
N1 C2 1.361(4) .
O4 C15 1.249(4) .
N4 C8 1.324(4) .
N4 C10 1.362(4) .
N4 C11 1.474(4) .
C3 C2 1.335(5) .
C17 C17 1.521(6) 2_667
N3 C8 1.313(5) .
N3 C9 1.341(5) .
C16 C15 1.537(5) .
C12 C13 1.379(5) .
C12 C11 1.517(4) .
C13 C14 1.399(4) 2_676
C7 C5 1.378(4) 2_756
C10 C9 1.352(5) .
