#------------------------------------------------------------------------------
#$Date: 2015-10-07 10:19:19 +0300 (Wed, 07 Oct 2015) $
#$Revision: 160611 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/78/7117889.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_7117889
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 Fe6 Mn N2 O40'
_chemical_formula_weight         1304.48
_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   mixed
_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                111.14(3)
_cell_angle_beta                 97.28(3)
_cell_angle_gamma                92.22(3)
_cell_formula_units_Z            1
_cell_length_a                   6.8216(14)
_cell_length_b                   10.968(2)
_cell_length_c                   14.889(3)
_cell_measurement_temperature    293(2)
_cell_volume                     1026.3(4)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.902
_diffrn_measured_fraction_theta_max 0.902
_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  0.1054
_diffrn_reflns_av_unetI/netI     0.1385
_diffrn_reflns_laue_measured_fraction_full 0.902
_diffrn_reflns_laue_measured_fraction_max 0.902
_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            7750
_diffrn_reflns_point_group_measured_fraction_full 0.902
_diffrn_reflns_point_group_measured_fraction_max 0.902
_diffrn_reflns_theta_full        25.009
_diffrn_reflns_theta_max         25.009
_diffrn_reflns_theta_min         3.160
_exptl_absorpt_coefficient_mu    2.487
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.111
_exptl_crystal_description       block
_exptl_crystal_F_000             653
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.396
_refine_diff_density_min         -1.201
_refine_diff_density_rms         0.244
_refine_ls_extinction_coef       0.022(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.150
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     305
_refine_ls_number_reflns         3261
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.148
_refine_ls_R_factor_all          0.1652
_refine_ls_R_factor_gt           0.1391
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0001P)²+59.0782P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2700
_refine_ls_wR_factor_ref         0.2829
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2640
_reflns_number_total             3261
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c5cc05481h2.cif
_cod_data_source_block           2
_cod_database_code               7117889
_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'
'-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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
O16 O 1.1428(18) 0.3956(13) 0.0877(10) 0.025(3) Uani 1 1 d . U .
C1 C 1.092(3) 0.364(2) 0.1503(16) 0.030(5) Uani 1 1 d . . .
H1A H 1.1868 0.3342 0.1859 0.037 Uiso 1 1 calc R U .
Fe1 Fe 0.6636(4) 0.1978(3) 0.43036(17) 0.0153(7) Uani 1 1 d . . .
Fe2 Fe 0.8013(4) 0.2516(2) 0.23977(19) 0.0159(7) Uani 1 1 d . . .
Fe3 Fe 0.5872(4) -0.0412(2) 0.21135(18) 0.0159(7) Uani 1 1 d . . .
Mn1 Mn 0.0000 -0.5000 0.0000 0.0159(9) Uani 1 2 d S . P
O1 O 0.6777(17) 0.1338(10) 0.2914(8) 0.011(2) Uani 1 1 d . . .
O4 O 0.8402(18) -0.0834(12) 0.1486(9) 0.023(3) Uani 1 1 d . . .
O10 O 0.9457(19) 0.2903(15) 0.4720(10) 0.033(4) Uani 1 1 d . . .
O12 O 0.666(2) 0.4133(13) 0.3118(10) 0.030(3) Uani 1 1 d . . .
O20 O 0.649(2) 0.2679(13) 0.5744(8) 0.025(3) Uani 1 1 d . U .
O2 O 0.5614(19) 0.2181(14) 0.1339(9) 0.028(3) Uani 1 1 d . . .
O6 O 0.695(2) -0.1245(13) 0.3072(10) 0.031(3) Uani 1 1 d . . .
O8 O 0.380(2) 0.1208(17) 0.4085(11) 0.040(4) Uani 1 1 d . . .
O9 O 0.3250(18) -0.0353(13) 0.2608(9) 0.023(3) Uani 1 1 d . . .
O3 O 0.4442(19) 0.0127(13) 0.1042(9) 0.025(3) Uani 1 1 d . . .
O5 O 0.950(2) 0.1114(14) 0.1490(11) 0.035(4) Uani 1 1 d . . .
O14 O 0.4996(18) -0.2297(12) 0.1194(9) 0.022(3) Uani 1 1 d . . .
O15 O 0.2994(18) -0.3987(12) 0.0254(9) 0.021(3) Uani 1 1 d . . .
C3 C 0.949(3) -0.0093(17) 0.1267(12) 0.018(4) Uani 1 1 d . . .
H3A H 1.0423 -0.0493 0.0881 0.022 Uiso 1 1 calc R U .
O18 O 0.762(2) 0.3392(16) 0.7310(9) 0.037(4) Uani 1 1 d . . .
O1W O -0.0613(19) -0.3449(12) 0.1357(9) 0.024(3) Uani 1 1 d . . .
H1WA H -0.0355 -0.2549 0.1423 0.029 Uiso 1 1 d R U .
H1WB H 0.0810 -0.3417 0.1591 0.029 Uiso 1 1 d R U .
O7 O 0.765(2) 0.0369(15) 0.4512(11) 0.036(4) Uani 1 1 d . . .
O17 O 0.9124(18) 0.3682(13) 0.1734(10) 0.026(3) Uani 1 1 d . . .
C4 C 0.763(3) 0.283(2) 0.6442(17) 0.036(5) Uani 1 1 d . . .
H4A H 0.8790 0.2430 0.6301 0.043 Uiso 1 1 calc R U .
C5 C 0.557(3) 0.430(2) 0.3779(13) 0.025(4) Uani 1 1 d . . .
H5A H 0.4811 0.5014 0.3901 0.031 Uiso 1 1 calc R U .
C6 C 0.342(2) -0.2815(17) 0.0659(13) 0.017(4) Uani 1 1 d . U .
H6A H 0.2485 -0.2263 0.0559 0.021 Uiso 1 1 calc R U .
O11 O 1.0490(19) 0.3080(15) 0.3404(10) 0.030(3) Uani 1 1 d . . .
C7 C 0.755(3) -0.076(2) 0.3964(14) 0.024(4) Uani 1 1 d . U .
H7A H 0.7984 -0.1352 0.4247 0.029 Uiso 1 1 calc R U .
C8 C 0.275(3) 0.034(2) 0.3392(14) 0.029(5) Uani 1 1 d . . .
H8A H 0.1443 0.0181 0.3471 0.035 Uiso 1 1 calc R U .
O13 O 0.542(2) 0.3616(13) 0.4279(10) 0.031(3) Uani 1 1 d . . .
C9 C 1.068(3) 0.3215(19) 0.4253(15) 0.028(5) Uani 1 1 d . U .
H9A H 1.1905 0.3607 0.4615 0.034 Uiso 1 1 calc R U .
C10 C 0.442(3) 0.119(2) 0.0932(14) 0.028(5) Uani 1 1 d . . .
H10A H 0.3373 0.1257 0.0490 0.033 Uiso 1 1 calc R U .
N1 N 0.561(2) 0.5336(17) 0.1707(12) 0.028(4) Uani 1 1 d . . .
H21A H 0.5580 0.6253 0.1819 0.041 Uiso 1 1 d R U .
H21B H 0.6525 0.4964 0.1265 0.041 Uiso 1 1 d R U .
H21C H 0.4305 0.4896 0.1431 0.041 Uiso 1 1 d R U .
H21D H 0.6060 0.5220 0.2376 0.041 Uiso 1 1 d R 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'
Mn Mn 0.3368 0.7283 '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
C1 O16 Mn1 132.4(13) . 1_665
O16 C1 O17 125.5(19) . .
O16 C1 H1A 117.2 . .
O17 C1 H1A 117.2 . .
O1 Fe1 O13 92.6(5) . .
O1 Fe1 O20 178.8(5) . .
O13 Fe1 O20 86.3(6) . .
O1 Fe1 O8 92.7(5) . .
O13 Fe1 O8 85.0(6) . .
O20 Fe1 O8 87.6(6) . .
O1 Fe1 O7 95.4(6) . .
O13 Fe1 O7 171.2(6) . .
O20 Fe1 O7 85.8(6) . .
O8 Fe1 O7 91.0(7) . .
O1 Fe1 O10 95.0(5) . .
O13 Fe1 O10 92.9(6) . .
O20 Fe1 O10 84.6(5) . .
O8 Fe1 O10 172.1(6) . .
O7 Fe1 O10 90.1(6) . .
O1 Fe2 O11 96.5(5) . .
O1 Fe2 O12 96.8(5) . .
O11 Fe2 O12 92.8(6) . .
O1 Fe2 O2 91.3(5) . .
O11 Fe2 O2 171.7(6) . .
O12 Fe2 O2 83.7(6) . .
O1 Fe2 O5 95.1(5) . .
O11 Fe2 O5 89.4(6) . .
O12 Fe2 O5 167.6(6) . .
O2 Fe2 O5 92.4(6) . .
O1 Fe2 O17 174.5(5) . .
O11 Fe2 O17 88.8(5) . .
O12 Fe2 O17 84.2(5) . .
O2 Fe2 O17 83.4(5) . .
O5 Fe2 O17 83.6(6) . .
O1 Fe3 O9 94.5(5) . .
O1 Fe3 O6 96.7(5) . .
O9 Fe3 O6 88.9(6) . .
O1 Fe3 O14 176.8(5) . .
O9 Fe3 O14 88.4(5) . .
O6 Fe3 O14 84.7(5) . .
O1 Fe3 O3 92.8(5) . .
O9 Fe3 O3 86.3(5) . .
O6 Fe3 O3 169.7(5) . .
O14 Fe3 O3 86.0(5) . .
O1 Fe3 O4 95.9(5) . .
O9 Fe3 O4 169.5(5) . .
O6 Fe3 O4 88.1(6) . .
O14 Fe3 O4 81.3(5) . .
O3 Fe3 O4 94.9(5) . .
O16 Mn1 O16 180.0 2_655 1_445
O16 Mn1 O15 96.0(5) 2_655 .
O16 Mn1 O15 84.0(5) 1_445 .
O16 Mn1 O15 84.0(5) 2_655 2_545
O16 Mn1 O15 96.0(5) 1_445 2_545
O15 Mn1 O15 180.0 . 2_545
O16 Mn1 O1W 90.6(5) 2_655 .
O16 Mn1 O1W 89.4(5) 1_445 .
O15 Mn1 O1W 88.4(5) . .
O15 Mn1 O1W 91.6(5) 2_545 .
O16 Mn1 O1W 89.4(5) 2_655 2_545
O16 Mn1 O1W 90.6(5) 1_445 2_545
O15 Mn1 O1W 91.6(5) . 2_545
O15 Mn1 O1W 88.4(5) 2_545 2_545
O1W Mn1 O1W 180.0 . 2_545
Fe3 O1 Fe2 121.3(6) . .
Fe3 O1 Fe1 120.5(5) . .
Fe2 O1 Fe1 118.1(5) . .
C3 O4 Fe3 127.5(12) . .
C9 O10 Fe1 132.3(13) . .
C5 O12 Fe2 129.3(13) . .
C4 O20 Fe1 133.8(15) . .
C10 O2 Fe2 129.6(13) . .
C7 O6 Fe3 131.5(13) . .
C8 O8 Fe1 133.6(13) . .
C8 O9 Fe3 131.1(13) . .
C10 O3 Fe3 132.2(13) . .
C3 O5 Fe2 133.1(13) . .
C6 O14 Fe3 132.1(12) . .
C6 O15 Mn1 125.4(11) . .
O4 C3 O5 129.0(17) . .
O4 C3 H3A 115.5 . .
O5 C3 H3A 115.5 . .
Mn1 O1W H1WA 117.6 . .
Mn1 O1W H1WB 85.4 . .
H1WA O1W H1WB 86.5 . .
C7 O7 Fe1 131.0(13) . .
C1 O17 Fe2 123.4(12) . .
O20 C4 O18 134(2) . .
O20 C4 H4A 113.1 . .
O18 C4 H4A 113.1 . .
O13 C5 O12 126.7(19) . .
O13 C5 H5A 116.6 . .
O12 C5 H5A 116.6 . .
O15 C6 O14 125.0(16) . .
O15 C6 H6A 117.5 . .
O14 C6 H6A 117.5 . .
C9 O11 Fe2 128.9(13) . .
O7 C7 O6 129.0(18) . .
O7 C7 H7A 115.5 . .
O6 C7 H7A 115.5 . .
O9 C8 O8 127.1(18) . .
O9 C8 H8A 116.5 . .
O8 C8 H8A 116.5 . .
C5 O13 Fe1 133.5(13) . .
O11 C9 O10 129.5(18) . .
O11 C9 H9A 115.3 . .
O10 C9 H9A 115.3 . .
O3 C10 O2 128.0(18) . .
O3 C10 H10A 116.0 . .
O2 C10 H10A 116.0 . .
H21A N1 H21B 109.5 . .
H21A N1 H21C 109.5 . .
H21B N1 H21C 109.5 . .
H21A N1 H21D 109.5 . .
H21B N1 H21D 109.5 . .
H21C N1 H21D 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
O16 C1 1.19(2) .
O16 Mn1 2.193(12) 1_665
C1 O17 1.31(2) .
C1 H1A 0.9300 .
Fe1 O1 1.947(11) .
Fe1 O13 2.017(14) .
Fe1 O20 2.019(12) .
Fe1 O8 2.019(14) .
Fe1 O7 2.032(14) .
Fe1 O10 2.052(13) .
Fe2 O1 1.941(10) .
Fe2 O11 2.022(13) .
Fe2 O12 2.037(13) .
Fe2 O2 2.045(13) .
Fe2 O5 2.047(13) .
Fe2 O17 2.052(12) .
Fe3 O1 1.886(11) .
Fe3 O9 2.013(12) .
Fe3 O6 2.034(13) .
Fe3 O14 2.040(12) .
Fe3 O3 2.043(13) .
Fe3 O4 2.056(12) .
Mn1 O16 2.193(12) 2_655
Mn1 O16 2.193(12) 1_445
Mn1 O15 2.208(12) .
Mn1 O15 2.208(12) 2_545
Mn1 O1W 2.222(12) .
Mn1 O1W 2.222(12) 2_545
O4 C3 1.23(2) .
O10 C9 1.26(2) .
O12 C5 1.27(2) .
O20 C4 1.17(2) .
O2 C10 1.24(2) .
O6 C7 1.25(2) .
O8 C8 1.24(3) .
O9 C8 1.24(2) .
O3 C10 1.23(2) .
O5 C3 1.24(2) .
O14 C6 1.23(2) .
O15 C6 1.21(2) .
C3 H3A 0.9300 .
O18 C4 1.22(3) .
O1W H1WA 0.9631 .
O1W H1WB 0.9835 .
O7 C7 1.21(2) .
C4 H4A 0.9300 .
C5 O13 1.24(2) .
C5 H5A 0.9300 .
C6 H6A 0.9300 .
O11 C9 1.21(2) .
C7 H7A 0.9300 .
C8 H8A 0.9300 .
C9 H9A 0.9300 .
C10 H10A 0.9300 .
N1 H21A 0.9600 .
N1 H21B 0.9600 .
N1 H21C 0.9600 .
N1 H21D 1.0582 .
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
Mn1 O16 C1 O17 11(3) 1_665
O9 Fe3 O1 Fe2 -134.2(7) .
O6 Fe3 O1 Fe2 136.3(7) .
O3 Fe3 O1 Fe2 -47.7(7) .
O4 Fe3 O1 Fe2 47.5(7) .
O9 Fe3 O1 Fe1 49.5(7) .
O6 Fe3 O1 Fe1 -40.0(8) .
O3 Fe3 O1 Fe1 136.0(7) .
O4 Fe3 O1 Fe1 -128.8(7) .
Fe3 O4 C3 O5 11(3) .
Fe2 O5 C3 O4 6(3) .
O16 C1 O17 Fe2 155.1(17) .
Fe1 O20 C4 O18 169.3(19) .
Fe2 O12 C5 O13 16(3) .
Mn1 O15 C6 O14 144.4(15) .
Fe3 O14 C6 O15 -168.6(13) .
Fe1 O7 C7 O6 8(3) .
Fe3 O6 C7 O7 0(3) .
Fe3 O9 C8 O8 1(3) .
Fe1 O8 C8 O9 2(4) .
O12 C5 O13 Fe1 -2(3) .
Fe2 O11 C9 O10 9(3) .
Fe1 O10 C9 O11 2(4) .
Fe3 O3 C10 O2 18(3) .
Fe2 O2 C10 O3 -4(3) .
