#------------------------------------------------------------------------------
#$Date: 2016-09-10 02:21:03 +0300 (Sat, 10 Sep 2016) $
#$Revision: 186368 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/22/58/7225820.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_7225820
loop_
_publ_author_name
'Pan, Jia-li'
'Guo, Qian'
'Yang, Bing'
'Li, Yu-yi'
'Cao, Jin-ge'
'Meng, Xiang-gao'
'Xiao, Feng-ping'
_publ_section_title
;
 Tetra-Fe(iii) and deca-Mn(iii) metallacrowns built from
 bis-salicylhydrazide ligands: synthesis, structures and magnetic
 properties
;
_journal_issue                   33
_journal_name_full               CrystEngComm
_journal_page_first              6143
_journal_paper_doi               10.1039/C6CE01100D
_journal_volume                  18
_journal_year                    2016
_chemical_formula_moiety         'C38 H32 Cl4 Fe4 N8 O16, 8(C3 H7 N O)'
_chemical_formula_sum            'C62 H88 Cl4 Fe4 N16 O24'
_chemical_formula_weight         1806.68
_chemical_properties_physical    ', Air-sensitive'
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a'
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-06-23 deposited with the CCDC.
2016-07-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.284(3)
_cell_length_b                   26.284(3)
_cell_length_c                   12.9228(15)
_cell_measurement_reflns_used    5316
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      23.45
_cell_measurement_theta_min      2.34
_cell_volume                     8927.7(18)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0615
_diffrn_reflns_av_unetI/netI     0.0354
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            30373
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        24.844
_diffrn_reflns_theta_max         24.844
_diffrn_reflns_theta_min         1.549
_exptl_absorpt_coefficient_mu    0.830
_exptl_absorpt_correction_T_max  0.9216
_exptl_absorpt_correction_T_min  0.9216
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, (Sheldrick,2008)'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.344
_exptl_crystal_description       block
_exptl_crystal_F_000             3744
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.132
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.092
_refine_diff_density_max         1.087
_refine_diff_density_min         -0.566
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     251
_refine_ls_number_reflns         3857
_refine_ls_number_restraints     41
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0834
_refine_ls_R_factor_gt           0.0607
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1214P)²+30.6488P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1735
_refine_ls_wR_factor_ref         0.2001
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2880
_reflns_number_total             3857
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6ce01100d2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7225820--7225823.cif.'
_cod_original_cell_volume        8928(2)
_cod_database_code               7225820
_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   0.922
_shelx_estimated_absorpt_t_max   0.922
_solvent_exptl_crystal_recrystallization_method 'DMF and Pyridine'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'
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 0.87042(2) 0.24610(2) 0.10693(5) 0.0376(3) Uani 1 1 d . . .
C1 C 0.82341(16) 0.30252(16) 0.2795(4) 0.0422(10) Uani 1 1 d . . .
C2 C 0.85283(16) 0.34729(16) 0.2706(4) 0.0438(11) Uani 1 1 d . . .
C3 C 0.8403(2) 0.39038(19) 0.3288(4) 0.0597(14) Uani 1 1 d . . .
H3 H 0.8602 0.4204 0.3234 0.072 Uiso 1 1 calc R U .
C4 C 0.7992(3) 0.3890(2) 0.3934(6) 0.079(2) Uani 1 1 d . . .
C5 C 0.7693(2) 0.3450(2) 0.4036(5) 0.0745(18) Uani 1 1 d . . .
H5 H 0.7409 0.3447 0.4490 0.089 Uiso 1 1 calc R U .
C6 C 0.78129(19) 0.3033(2) 0.3482(4) 0.0563(13) Uani 1 1 d . . .
H6 H 0.7610 0.2735 0.3554 0.068 Uiso 1 1 calc R U .
C7 C 0.89713(16) 0.35140(15) 0.2004(3) 0.0392(10) Uani 1 1 d . . .
C8 C 0.95033(15) 0.29259(16) -0.0070(3) 0.0388(10) Uani 1 1 d . . .
C9 C 0.98973(17) 0.29832(17) -0.0886(3) 0.0426(10) Uani 1 1 d . . .
H9A H 1.0219 0.3091 -0.0555 0.051 Uiso 1 1 calc R U .
H9B H 0.9791 0.3258 -0.1363 0.051 Uiso 1 1 calc R U .
C10 C 1.0000 0.2500 -0.1522(5) 0.0443(15) Uani 1 2 d S T P
H10A H 0.9703 0.2437 -0.1975 0.053 Uiso 0.5 1 calc R U P
H10B H 1.0297 0.2563 -0.1975 0.053 Uiso 0.5 1 calc R U P
C11 C 0.7011(6) 0.4365(4) 0.0901(14) 0.269(11) Uani 1 1 d . . .
H11A H 0.7379 0.4422 0.0842 0.404 Uiso 1 1 calc R U .
H11B H 0.6856 0.4646 0.1285 0.404 Uiso 1 1 calc R U .
H11C H 0.6862 0.4347 0.0207 0.404 Uiso 1 1 calc R U .
C12 C 0.6564(5) 0.3933(4) 0.2261(10) 0.189(7) Uani 1 1 d . . .
H12A H 0.6226 0.4010 0.1982 0.283 Uiso 1 1 calc R U .
H12B H 0.6667 0.4204 0.2737 0.283 Uiso 1 1 calc R U .
H12C H 0.6552 0.3608 0.2634 0.283 Uiso 1 1 calc R U .
C13 C 0.7190(3) 0.3501(3) 0.1228(6) 0.088(2) Uani 1 1 d . . .
H13 H 0.7133 0.3211 0.1653 0.106 Uiso 1 1 calc R U .
C14 C 0.8346(10) 0.2567(10) 0.6115(17) 0.374(16) Uani 1 1 d D U .
H14A H 0.8049 0.2480 0.5691 0.561 Uiso 1 1 d R U .
H14B H 0.8648 0.2591 0.5673 0.561 Uiso 1 1 d R U .
H14C H 0.8287 0.2895 0.6456 0.561 Uiso 1 1 d R U .
C15 C 0.8641(11) 0.1647(10) 0.667(3) 0.67(4) Uani 1 1 d D U .
H15A H 0.8854 0.1631 0.6046 1.002 Uiso 1 1 d R U .
H15B H 0.8340 0.1432 0.6572 1.002 Uiso 1 1 d R U .
H15C H 0.8836 0.1525 0.7265 1.002 Uiso 1 1 d R U .
C16 C 0.8373(6) 0.2255(6) 0.7912(14) 0.258(10) Uani 1 1 d D U .
H16 H 0.8433 0.2008 0.8436 0.310 Uiso 1 1 calc R U .
Cl1 Cl 0.78359(10) 0.44282(8) 0.4670(2) 0.1429(12) Uani 1 1 d . . .
N1 N 0.90657(12) 0.31387(13) 0.1360(3) 0.0357(8) Uani 1 1 d . . .
N2 N 0.94988(13) 0.32351(13) 0.0737(3) 0.0382(8) Uani 1 1 d . . .
N3 N 0.6921(2) 0.3899(2) 0.1435(5) 0.095(2) Uani 1 1 d . . .
N4 N 0.8453(6) 0.2160(8) 0.6853(16) 0.330(10) Uani 1 1 d D U .
O1 O 0.83209(12) 0.25997(11) 0.2280(3) 0.0486(8) Uani 1 1 d . . .
O2 O 0.92594(11) 0.39122(10) 0.2051(3) 0.0439(8) Uani 1 1 d . . .
O3 O 0.91588(11) 0.25829(12) -0.0189(2) 0.0446(7) Uani 1 1 d . . .
O4 O 0.80980(12) 0.26794(13) 0.0168(3) 0.0573(9) Uani 1 1 d D . .
H4A H 0.7931 0.2923 0.0371 0.086 Uiso 1 1 d DR U .
H4B H 0.8181 0.2674 -0.0443 0.086 Uiso 1 1 d DR U .
O5 O 0.7497(2) 0.3456(2) 0.0573(5) 0.115(2) Uani 1 1 d . . .
O6 O 0.8205(4) 0.2719(6) 0.8107(9) 0.278(6) Uani 1 1 d 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'
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
O1 Fe1 O2 114.80(13) . 12_756
O1 Fe1 O3 159.59(13) . .
O2 Fe1 O3 85.21(12) 12_756 .
O1 Fe1 N1 85.88(13) . .
O2 Fe1 N1 158.15(13) 12_756 .
O3 Fe1 N1 74.87(13) . .
O1 Fe1 O4 90.11(15) . .
O2 Fe1 O4 85.03(13) 12_756 .
O3 Fe1 O4 87.63(14) . .
N1 Fe1 O4 102.71(14) . .
O1 Fe1 N2 97.53(15) . 12_756
O2 Fe1 N2 75.55(13) 12_756 12_756
O3 Fe1 N2 91.15(13) . 12_756
N1 Fe1 N2 95.65(13) . 12_756
O4 Fe1 N2 160.58(14) . 12_756
O1 C1 C2 124.7(4) . .
O1 C1 C6 117.5(4) . .
C2 C1 C6 117.8(4) . .
C3 C2 C1 120.1(4) . .
C3 C2 C7 117.1(4) . .
C1 C2 C7 122.8(4) . .
C4 C3 C2 119.6(5) . .
C4 C3 H3 120.2 . .
C2 C3 H3 120.2 . .
C3 C4 C5 121.5(5) . .
C3 C4 Cl1 119.7(4) . .
C5 C4 Cl1 118.8(4) . .
C6 C5 C4 119.3(5) . .
C6 C5 H5 120.4 . .
C4 C5 H5 120.4 . .
C5 C6 C1 121.7(5) . .
C5 C6 H6 119.1 . .
C1 C6 H6 119.1 . .
O2 C7 N1 121.7(4) . .
O2 C7 C2 119.4(4) . .
N1 C7 C2 118.8(4) . .
O3 C8 N2 121.2(4) . .
O3 C8 C9 118.5(4) . .
N2 C8 C9 120.2(4) . .
C8 C9 C10 114.7(4) . .
C8 C9 H9A 108.6 . .
C10 C9 H9A 108.6 . .
C8 C9 H9B 108.6 . .
C10 C9 H9B 108.6 . .
H9A C9 H9B 107.6 . .
C9 C10 C9 115.3(5) 6_654 .
C9 C10 H10A 108.5 6_654 .
C9 C10 H10A 108.5 . .
C9 C10 H10B 108.5 6_654 .
C9 C10 H10B 108.5 . .
H10A C10 H10B 107.5 . .
N3 C11 H11A 109.5 . .
N3 C11 H11B 109.5 . .
H11A C11 H11B 109.5 . .
N3 C11 H11C 109.5 . .
H11A C11 H11C 109.5 . .
H11B C11 H11C 109.5 . .
N3 C12 H12A 109.5 . .
N3 C12 H12B 109.5 . .
H12A C12 H12B 109.5 . .
N3 C12 H12C 109.5 . .
H12A C12 H12C 109.5 . .
H12B C12 H12C 109.5 . .
O5 C13 N3 127.2(7) . .
O5 C13 H13 116.4 . .
N3 C13 H13 116.4 . .
N4 C14 H14A 110.3 . .
N4 C14 H14B 105.6 . .
H14A C14 H14B 109.5 . .
N4 C14 H14C 112.4 . .
H14A C14 H14C 109.5 . .
H14B C14 H14C 109.5 . .
N4 C15 H15A 111.5 . .
N4 C15 H15B 106.3 . .
H15A C15 H15B 109.5 . .
N4 C15 H15C 110.5 . .
H15A C15 H15C 109.5 . .
H15B C15 H15C 109.5 . .
O6 C16 N4 113.5(15) . .
O6 C16 H16 123.3 . .
N4 C16 H16 123.3 . .
C7 N1 N2 112.2(3) . .
C7 N1 Fe1 132.8(3) . .
N2 N1 Fe1 115.0(2) . .
C8 N2 N1 110.2(3) . .
C8 N2 Fe1 139.4(3) . 15_665
N1 N2 Fe1 110.2(3) . 15_665
C13 N3 C12 124.5(7) . .
C13 N3 C11 120.3(7) . .
C12 N3 C11 114.8(7) . .
C16 N4 C15 112.0(14) . .
C16 N4 C14 118.5(15) . .
C15 N4 C14 130(2) . .
C1 O1 Fe1 132.0(3) . .
C7 O2 Fe1 113.0(3) . 15_665
C8 O3 Fe1 115.2(3) . .
Fe1 O4 H4A 116.9 . .
Fe1 O4 H4B 109.5 . .
H4A O4 H4B 117.7 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 O1 1.897(3) .
Fe1 O2 2.034(3) 12_756
Fe1 O3 2.043(3) .
Fe1 N1 2.053(3) .
Fe1 O4 2.055(3) .
Fe1 N2 2.110(4) 12_756
C1 O1 1.321(5) .
C1 C2 1.413(6) .
C1 C6 1.419(6) .
C2 C3 1.399(6) .
C2 C7 1.479(6) .
C3 C4 1.365(7) .
C3 H3 0.9500 .
C4 C5 1.404(8) .
C4 Cl1 1.754(6) .
C5 C6 1.348(7) .
C5 H5 0.9500 .
C6 H6 0.9500 .
C7 O2 1.293(5) .
C7 N1 1.315(5) .
C8 O3 1.287(5) .
C8 N2 1.323(6) .
C8 C9 1.485(6) .
C9 C10 1.537(6) .
C9 H9A 0.9900 .
C9 H9B 0.9900 .
C10 C9 1.537(5) 6_654
C10 H10A 0.9900 .
C10 H10B 0.9900 .
C11 N3 1.426(11) .
C11 H11A 0.9800 .
C11 H11B 0.9800 .
C11 H11C 0.9800 .
C12 N3 1.425(10) .
C12 H12A 0.9800 .
C12 H12B 0.9800 .
C12 H12C 0.9800 .
C13 O5 1.176(8) .
C13 N3 1.291(8) .
C13 H13 0.9500 .
C14 N4 1.461(10) .
C14 H14A 0.9799 .
C14 H14B 0.9801 .
C14 H14C 0.9801 .
C15 N4 1.457(10) .
C15 H15A 0.9801 .
C15 H15B 0.9798 .
C15 H15C 0.9800 .
C16 O6 1.322(9) .
C16 N4 1.407(10) .
C16 H16 0.9500 .
N1 N2 1.417(5) .
N2 Fe1 2.110(4) 15_665
O2 Fe1 2.034(3) 15_665
O4 H4A 0.8199 .
O4 H4B 0.8200 .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O4 H4B O6 0.82 1.88 2.680(13) 165.7 1_554
O4 H4A O5 0.82 1.83 2.634(6) 168.6 .
C9 H9A O3 0.99 2.46 3.030(5) 116.4 6_654
C9 H9A N1 0.99 2.61 3.472(6) 145.3 15_665
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
O1 C1 C2 C3 180.0(5) . .
C6 C1 C2 C3 0.3(7) . .
O1 C1 C2 C7 0.6(8) . .
C6 C1 C2 C7 -179.1(5) . .
C1 C2 C3 C4 -0.6(9) . .
C7 C2 C3 C4 178.9(6) . .
C2 C3 C4 C5 0.4(11) . .
C2 C3 C4 Cl1 179.7(5) . .
C3 C4 C5 C6 -0.1(12) . .
Cl1 C4 C5 C6 -179.3(6) . .
C4 C5 C6 C1 -0.2(10) . .
O1 C1 C6 C5 -179.6(6) . .
C2 C1 C6 C5 0.0(8) . .
C3 C2 C7 O2 8.7(7) . .
C1 C2 C7 O2 -171.8(4) . .
C3 C2 C7 N1 -172.3(5) . .
C1 C2 C7 N1 7.1(7) . .
O3 C8 C9 C10 -25.8(5) . .
N2 C8 C9 C10 156.7(4) . .
C8 C9 C10 C9 -50.7(3) . 6_654
O2 C7 N1 N2 -1.5(6) . .
C2 C7 N1 N2 179.6(4) . .
O2 C7 N1 Fe1 -180.0(3) . .
C2 C7 N1 Fe1 1.1(6) . .
O3 C8 N2 N1 -2.6(5) . .
C9 C8 N2 N1 174.8(3) . .
O3 C8 N2 Fe1 172.4(3) . 15_665
C9 C8 N2 Fe1 -10.2(7) . 15_665
C7 N1 N2 C8 -163.2(4) . .
Fe1 N1 N2 C8 15.6(4) . .
C7 N1 N2 Fe1 20.2(4) . 15_665
Fe1 N1 N2 Fe1 -160.97(16) . 15_665
O5 C13 N3 C12 -178.1(11) . .
O5 C13 N3 C11 -5.7(17) . .
O6 C16 N4 C15 179.7(11) . .
O6 C16 N4 C14 -0.2(17) . .
C2 C1 O1 Fe1 -18.3(7) . .
C6 C1 O1 Fe1 161.4(4) . .
O2 Fe1 O1 C1 -167.9(4) 12_756 .
O3 Fe1 O1 C1 0.2(7) . .
N1 Fe1 O1 C1 19.4(4) . .
O4 Fe1 O1 C1 -83.3(4) . .
N2 Fe1 O1 C1 114.6(4) 12_756 .
N1 C7 O2 Fe1 -19.2(5) . 15_665
C2 C7 O2 Fe1 159.7(3) . 15_665
N2 C8 O3 Fe1 -11.6(5) . .
C9 C8 O3 Fe1 170.9(3) . .
