#------------------------------------------------------------------------------
#$Date: 2015-10-07 10:19:19 +0300 (Wed, 07 Oct 2015) $
#$Revision: 160611 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/78/7117888.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_7117888
loop_
_publ_author_name
'Wu, Qi-Long'
'Han, Song-De'
'Wang, Qing-Lun'
'Zhao, Jiong-Peng'
'Ma, Feng'
'Jiang, Xue'
'Liu, Fu-Chen'
'Bu, Xian-He'
_publ_section_title
;
 Divalent metal ions modulated strong frustrated M(ii)-Fe(iii)3O (M = Fe,
 Mn, Mg) chains with metamagnetism only in a mixed valence iron complex.
;
_journal_issue                   83
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              15336
_journal_page_last               15339
_journal_paper_doi               10.1039/c5cc05481h
_journal_volume                  51
_journal_year                    2015
_chemical_formula_sum            'C18 H30 Fe7 N2 O40'
_chemical_formula_weight         1305.39
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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
_audit_update_record
;
2015-05-20 deposited with the CCDC.
2015-08-20 downloaded from the CCDC.
;
_cell_angle_alpha                111.35(3)
_cell_angle_beta                 97.42(3)
_cell_angle_gamma                92.39(3)
_cell_formula_units_Z            1
_cell_length_a                   6.8366(14)
_cell_length_b                   10.967(2)
_cell_length_c                   14.884(3)
_cell_measurement_temperature    293(2)
_cell_volume                     1025.9(4)
_computing_cell_refinement       RAPID-AUTO
_computing_data_collection       'RAPID-AUTO (Rigaku, 2004)'
_computing_data_reduction        'CrystalStructure (Rigaku/MSC'2004)'
_computing_molecular_graphics    'SHELXTL (Bruker, 1998)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXL-97
_computing_structure_solution    SHELXS-97
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID IP'
_diffrn_measurement_method       'ω scans'
_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  0.0788
_diffrn_reflns_av_unetI/netI     0.0968
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            8745
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         3.02
_exptl_absorpt_coefficient_mu    2.534
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.113
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             654
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.487
_refine_diff_density_min         -0.763
_refine_diff_density_rms         0.190
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.171
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     304
_refine_ls_number_reflns         3599
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.171
_refine_ls_R_factor_all          0.1188
_refine_ls_R_factor_gt           0.0884
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0908P)²+3.0194P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1908
_refine_ls_wR_factor_ref         0.2038
_reflns_number_gt                2774
_reflns_number_total             3599
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5cc05481h2.cif
_cod_data_source_block           1
_cod_original_cell_volume        1026.0(4)
_cod_database_code               7117888
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
O2 O 0.9969(10) 0.7701(6) 0.1167(5) 0.0280(16) Uani 1 1 d .
C9 C 0.8369(14) 0.7171(9) 0.0634(7) 0.023(2) Uani 1 1 d .
H9A H 0.7459 0.7724 0.0517 0.028 Uiso 1 1 calc R
Fe1 Fe 0.5000 0.5000 0.0000 0.0177(5) Uani 1 2 d S
Fe2 Fe 0.08487(19) -0.04253(13) 0.21015(9) 0.0191(4) Uani 1 1 d .
Fe3 Fe 0.16393(19) 0.19804(13) 0.43013(9) 0.0202(4) Uani 1 1 d .
Fe4 Fe 0.30007(19) 0.25087(13) 0.23808(9) 0.0193(4) Uani 1 1 d .
O17 O 0.1386(10) 0.2718(6) 0.5730(4) 0.0258(15) Uani 1 1 d .
O19 O 0.1863(8) 0.1326(6) 0.2925(4) 0.0182(14) Uani 1 1 d .
O6 O 0.3371(9) -0.0848(6) 0.1463(5) 0.0265(16) Uani 1 1 d .
O7 O -0.0563(10) 0.0129(7) 0.1028(4) 0.0261(16) Uani 1 1 d .
O1 O 0.7887(9) 0.5978(6) 0.0248(4) 0.0214(14) Uani 1 1 d .
O12 O -0.1207(10) 0.1190(7) 0.4090(5) 0.0341(18) Uani 1 1 d .
O9 O 0.1958(11) -0.1275(6) 0.3042(5) 0.0312(17) Uani 1 1 d .
O13 O 0.4445(10) 0.2875(7) 0.4699(5) 0.0378(19) Uani 1 1 d .
O15 O 0.1672(10) 0.4119(6) 0.3121(5) 0.0304(17) Uani 1 1 d .
O16 O 0.0458(10) 0.3638(6) 0.4277(5) 0.0300(17) Uani 1 1 d .
O8 O 0.0607(10) 0.2194(7) 0.1331(5) 0.0298(17) Uani 1 1 d .
O4 O 0.4117(9) 0.3681(6) 0.1729(5) 0.0275(16) Uani 1 1 d .
O5 O 0.4493(10) 0.1094(7) 0.1467(5) 0.0310(17) Uani 1 1 d .
O3 O 0.6356(9) 0.3977(7) 0.0844(5) 0.0271(16) Uani 1 1 d .
C4 C 0.2551(15) -0.0801(11) 0.3940(8) 0.030(2) Uani 1 1 d .
H5A H 0.2951 -0.1394 0.4225 0.036 Uiso 1 1 calc R
O18 O 0.2566(11) 0.3377(7) 0.7300(5) 0.0384(19) Uani 1 1 d .
O10 O 0.2670(11) 0.0388(7) 0.4505(5) 0.0368(18) Uani 1 1 d .
O14 O 0.5456(10) 0.3076(7) 0.3397(5) 0.0339(18) Uani 1 1 d .
O11 O -0.1795(10) -0.0368(7) 0.2585(5) 0.0329(18) Uani 1 1 d .
C8 C 0.2667(15) 0.2823(11) 0.6446(7) 0.033(3) Uani 1 1 d .
H1A H 0.3825 0.2427 0.6301 0.040 Uiso 1 1 calc R
C1 C 0.5848(14) 0.3650(10) 0.1506(7) 0.026(2) Uani 1 1 d .
H8A H 0.6811 0.3362 0.1863 0.031 Uiso 1 1 calc R
C7 C 0.0598(15) 0.4308(9) 0.3768(7) 0.027(2) Uani 1 1 d .
H3A H -0.0166 0.5015 0.3879 0.032 Uiso 1 1 calc R
C6 C 0.5690(14) 0.3204(9) 0.4259(7) 0.027(2) Uani 1 1 d .
H2A H 0.6920 0.3585 0.4624 0.032 Uiso 1 1 calc R
C2 C 0.4508(14) -0.0107(10) 0.1254(7) 0.025(2) Uani 1 1 d .
H7A H 0.5483 -0.0504 0.0895 0.030 Uiso 1 1 calc R
C3 C -0.0619(14) 0.1216(10) 0.0929(7) 0.027(2) Uani 1 1 d .
H6A H -0.1695 0.1298 0.0511 0.032 Uiso 1 1 calc R
C5 C -0.2260(15) 0.0330(11) 0.3374(7) 0.030(2) Uani 1 1 d .
H4A H -0.3575 0.0195 0.3444 0.036 Uiso 1 1 calc R
N1 N 0.9393(12) 0.4665(9) 0.8320(6) 0.039(2) Uani 1 1 d .
H12 H 0.8438 0.4487 0.8579 0.046 Uiso 1 1 d R
H11 H 1.0007 0.4184 0.7879 0.046 Uiso 1 1 d R
H13 H 0.8999 0.5053 0.7939 0.046 Uiso 1 1 d R
H14 H 1.0129 0.4867 0.8857 0.046 Uiso 1 1 d R
O2W O 0.4331(10) 0.6482(6) 0.1317(4) 0.0257(15) Uani 1 1 d .
H2WB H 0.4222 0.7302 0.1488 0.031 Uiso 1 1 d R
H1W2 H 0.5034 0.6684 0.1874 0.031 Uiso 1 1 d R
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'
Fe Fe 0.3463 0.8444 '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'
N N 0.0061 0.0033 '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
C9 O2 Fe2 132.3(6) . 1_665
O1 C9 O2 125.7(9) . .
O1 C9 H9A 117.2 . .
O2 C9 H9A 117.2 . .
O3 Fe1 O3 180.0(3) 2_665 .
O3 Fe1 O1 95.5(2) 2_665 .
O3 Fe1 O1 84.5(2) . .
O3 Fe1 O1 84.5(2) 2_665 2_665
O3 Fe1 O1 95.5(2) . 2_665
O1 Fe1 O1 180.0(3) . 2_665
O3 Fe1 O2W 90.3(2) 2_665 .
O3 Fe1 O2W 89.7(2) . .
O1 Fe1 O2W 90.1(2) . .
O1 Fe1 O2W 89.9(2) 2_665 .
O3 Fe1 O2W 89.7(2) 2_665 2_665
O3 Fe1 O2W 90.3(2) . 2_665
O1 Fe1 O2W 89.9(2) . 2_665
O1 Fe1 O2W 90.1(2) 2_665 2_665
O2W Fe1 O2W 180.0(3) . 2_665
O19 Fe2 O11 96.2(3) . .
O19 Fe2 O2 175.2(3) . 1_445
O11 Fe2 O2 88.5(3) . 1_445
O19 Fe2 O9 95.8(3) . .
O11 Fe2 O9 90.4(3) . .
O2 Fe2 O9 84.8(3) 1_445 .
O19 Fe2 O7 93.8(3) . .
O11 Fe2 O7 86.2(3) . .
O2 Fe2 O7 85.8(3) 1_445 .
O9 Fe2 O7 170.1(3) . .
O19 Fe2 O6 94.4(3) . .
O11 Fe2 O6 169.3(3) . .
O2 Fe2 O6 80.9(3) 1_445 .
O9 Fe2 O6 87.4(3) . .
O7 Fe2 O6 94.2(3) . .
O19 Fe3 O17 178.1(3) . .
O19 Fe3 O10 94.0(3) . .
O17 Fe3 O10 87.9(3) . .
O19 Fe3 O13 92.8(3) . .
O17 Fe3 O13 87.0(3) . .
O10 Fe3 O13 89.0(3) . .
O19 Fe3 O16 93.7(3) . .
O17 Fe3 O16 84.4(3) . .
O10 Fe3 O16 172.0(3) . .
O13 Fe3 O16 92.9(3) . .
O19 Fe3 O12 94.7(3) . .
O17 Fe3 O12 85.6(3) . .
O10 Fe3 O12 91.0(3) . .
O13 Fe3 O12 172.5(3) . .
O16 Fe3 O12 86.1(3) . .
O19 Fe4 O14 94.0(3) . .
O19 Fe4 O15 96.9(3) . .
O14 Fe4 O15 92.0(3) . .
O19 Fe4 O8 93.9(3) . .
O14 Fe4 O8 171.5(3) . .
O15 Fe4 O8 83.7(3) . .
O19 Fe4 O4 176.7(3) . .
O14 Fe4 O4 88.9(3) . .
O15 Fe4 O4 84.7(3) . .
O8 Fe4 O4 83.4(3) . .
O19 Fe4 O5 94.4(3) . .
O14 Fe4 O5 89.6(3) . .
O15 Fe4 O5 168.5(3) . .
O8 Fe4 O5 93.2(3) . .
O4 Fe4 O5 83.9(3) . .
C8 O17 Fe3 128.0(6) . .
Fe2 O19 Fe3 120.3(3) . .
Fe2 O19 Fe4 120.4(3) . .
Fe3 O19 Fe4 119.2(3) . .
C2 O6 Fe2 128.7(6) . .
C3 O7 Fe2 132.6(6) . .
C9 O1 Fe1 127.1(6) . .
C5 O12 Fe3 132.4(6) . .
C4 O9 Fe2 131.3(6) . .
C6 O13 Fe3 134.6(7) . .
C7 O15 Fe4 131.2(6) . .
C7 O16 Fe3 133.5(6) . .
C3 O8 Fe4 129.7(6) . .
C1 O4 Fe4 123.8(6) . .
C2 O5 Fe4 133.4(6) . .
C1 O3 Fe1 133.4(6) . .
O9 C4 O10 127.7(9) . .
O9 C4 H5A 116.2 . .
O10 C4 H5A 116.2 . .
C4 O10 Fe3 131.5(6) . .
C6 O14 Fe4 130.5(7) . .
C5 O11 Fe2 129.8(7) . .
O18 C8 O17 127.3(10) . .
O18 C8 H1A 116.3 . .
O17 C8 H1A 116.3 . .
O3 C1 O4 124.9(9) . .
O3 C1 H8A 117.5 . .
O4 C1 H8A 117.5 . .
O16 C7 O15 126.0(9) . .
O16 C7 H3A 117.0 . .
O15 C7 H3A 117.0 . .
O14 C6 O13 126.9(9) . .
O14 C6 H2A 116.6 . .
O13 C6 H2A 116.6 . .
O5 C2 O6 127.7(9) . .
O5 C2 H7A 116.2 . .
O6 C2 H7A 116.2 . .
O8 C3 O7 127.0(9) . .
O8 C3 H6A 116.5 . .
O7 C3 H6A 116.5 . .
O11 C5 O12 128.9(10) . .
O11 C5 H4A 115.6 . .
O12 C5 H4A 115.6 . .
H12 N1 H11 132.0 . .
H12 N1 H13 110.4 . .
H11 N1 H13 88.2 . .
H12 N1 H14 88.8 . .
H11 N1 H14 107.7 . .
H13 N1 H14 136.5 . .
Fe1 O2W H2WB 133.4 . .
Fe1 O2W H1W2 123.6 . .
H2WB O2W H1W2 85.4 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
O2 C9 1.246(11) .
O2 Fe2 2.029(6) 1_665
C9 O1 1.233(11) .
C9 H9A 0.9300 .
Fe1 O3 2.123(6) 2_665
Fe1 O3 2.123(6) .
Fe1 O1 2.128(6) .
Fe1 O1 2.128(6) 2_665
Fe1 O2W 2.160(6) .
Fe1 O2W 2.160(6) 2_665
Fe2 O19 1.905(6) .
Fe2 O11 2.025(7) .
Fe2 O2 2.029(6) 1_445
Fe2 O9 2.034(7) .
Fe2 O7 2.053(6) .
Fe2 O6 2.064(7) .
Fe3 O19 1.938(6) .
Fe3 O17 2.016(6) .
Fe3 O10 2.018(7) .
Fe3 O13 2.030(7) .
Fe3 O16 2.030(6) .
Fe3 O12 2.034(7) .
Fe4 O19 1.946(6) .
Fe4 O14 2.016(7) .
Fe4 O15 2.033(6) .
Fe4 O8 2.034(6) .
Fe4 O4 2.048(7) .
Fe4 O5 2.062(6) .
O17 C8 1.256(11) .
O6 C2 1.248(11) .
O7 C3 1.254(11) .
O12 C5 1.248(12) .
O9 C4 1.248(12) .
O13 C6 1.255(12) .
O15 C7 1.249(11) .
O16 C7 1.242(11) .
O8 C3 1.241(12) .
O4 C1 1.268(11) .
O5 C2 1.238(11) .
O3 C1 1.248(11) .
C4 O10 1.260(12) .
C4 H5A 0.9300 .
O18 C8 1.205(11) .
O14 C6 1.227(11) .
O11 C5 1.236(11) .
C8 H1A 0.9300 .
C1 H8A 0.9300 .
C7 H3A 0.9300 .
C6 H2A 0.9300 .
C2 H7A 0.9300 .
C3 H6A 0.9300 .
C5 H4A 0.9300 .
N1 H12 0.8501 .
N1 H11 0.8500 .
N1 H13 0.8499 .
N1 H14 0.8360 .
O2W H2WB 0.8500 .
O2W H1W2 0.8500 .
