#------------------------------------------------------------------------------
#$Date: 2015-10-07 10:19:19 +0300 (Wed, 07 Oct 2015) $
#$Revision: 160611 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/78/7117890.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_7117890
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 Mg N2 O40'
_chemical_formula_weight         1273.85
_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                111.43(3)
_cell_angle_beta                 97.52(3)
_cell_angle_gamma                92.24(3)
_cell_formula_units_Z            1
_cell_length_a                   6.8025(14)
_cell_length_b                   10.887(2)
_cell_length_c                   14.826(3)
_cell_measurement_temperature    293(2)
_cell_volume                     1008.8(4)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_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  0.0245
_diffrn_reflns_av_unetI/netI     0.0281
_diffrn_reflns_laue_measured_fraction_full 0.988
_diffrn_reflns_laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            8751
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.007
_diffrn_reflns_theta_max         25.007
_diffrn_reflns_theta_min         3.034
_exptl_absorpt_coefficient_mu    2.247
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.097
_exptl_crystal_description       block
_exptl_crystal_F_000             640
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.531
_refine_diff_density_min         -0.567
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         3510
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0411
_refine_ls_R_factor_gt           0.0350
_refine_ls_shift/su_max          0.025
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0423P)²+1.4728P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0832
_refine_ls_wR_factor_ref         0.0858
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3146
_reflns_number_total             3510
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c5cc05481h2.cif
_cod_data_source_block           3
_cod_database_code               7117890
_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
Fe1 Fe 0.33418(7) 0.30223(5) 0.06940(3) 0.01892(14) Uani 1 1 d . . .
Fe2 Fe 0.19961(7) 0.24986(5) 0.26152(3) 0.01766(13) Uani 1 1 d . . .
Fe3 Fe 0.41351(7) 0.54375(5) 0.28954(3) 0.01706(13) Uani 1 1 d . . .
Mg1 Mg 0.0000 0.0000 0.5000 0.0009(2) Uani 1 2 d S U P
O1 O 0.3122(3) 0.3670(2) 0.20770(16) 0.0170(5) Uani 1 1 d . . .
O19 O 0.4980(4) 0.2680(2) 0.61703(18) 0.0258(6) Uani 1 1 d . . .
O9 O 0.1609(4) 0.5855(2) 0.35302(19) 0.0250(6) Uani 1 1 d . . .
O18 O 0.2841(3) 0.0969(2) 0.52580(17) 0.0221(5) Uani 1 1 d . . .
O7 O 0.5556(4) 0.4884(2) 0.39647(17) 0.0260(6) Uani 1 1 d . . .
O17 O -0.1306(4) 0.1009(3) 0.41673(19) 0.0269(6) Uani 1 1 d . . .
O11 O 0.6182(4) 0.3823(3) 0.09084(19) 0.0315(6) Uani 1 1 d . . .
O6 O 0.4398(4) 0.2814(3) 0.36647(19) 0.0292(6) Uani 1 1 d . . .
O16 O 0.0899(4) 0.1345(2) 0.32762(19) 0.0262(6) Uani 1 1 d . . .
O3 O 0.3329(4) 0.0882(2) 0.18852(19) 0.0311(6) Uani 1 1 d . . .
O4 O 0.0528(4) 0.2105(3) 0.02913(19) 0.0368(7) Uani 1 1 d . . .
O2 O 0.4532(4) 0.1358(3) 0.07175(18) 0.0294(6) Uani 1 1 d . . .
O13 O 0.3016(4) 0.6281(3) 0.19514(19) 0.0320(6) Uani 1 1 d . . .
O15 O 0.2401(4) 0.1609(3) -0.23120(19) 0.0392(7) Uani 1 1 d . . .
O1W O 0.0653(4) -0.1455(3) 0.3716(2) 0.0262(6) Uani 1 1 d . . .
O8 O 0.0524(4) 0.3906(3) 0.3536(2) 0.0322(6) Uani 1 1 d . . .
O12 O 0.2294(4) 0.4626(3) 0.04960(19) 0.0360(7) Uani 1 1 d . . .
C5 C 0.2417(6) 0.5802(4) 0.1043(3) 0.0262(8) Uani 1 1 d . . .
H5A H 0.2024 0.6398 0.0753 0.031 Uiso 1 1 calc R U .
O14 O 0.3592(4) 0.2278(3) -0.07416(18) 0.0295(6) Uani 1 1 d . . .
O5 O -0.0471(4) 0.1909(3) 0.1608(2) 0.0336(6) Uani 1 1 d . . .
N1 N 0.5589(6) 0.0335(4) 0.6673(3) 0.0352(9) Uani 1 1 d . . .
H24 H 0.6869 0.0097 0.6496 0.042 Uiso 1 1 d R U .
H23 H 0.5369 0.1251 0.6829 0.042 Uiso 1 1 d R U .
H22 H 0.4501 0.0078 0.6138 0.042 Uiso 1 1 d R U .
O10 O 0.6788(4) 0.5376(3) 0.24143(19) 0.0304(6) Uani 1 1 d . . .
C8 C 0.3369(5) 0.2174(3) 0.5636(3) 0.0245(8) Uani 1 1 d . . .
H8A H 0.2487 0.2743 0.5509 0.029 Uiso 1 1 calc R U .
C7 C -0.0807(5) 0.1354(4) 0.3506(3) 0.0243(8) Uani 1 1 d . . .
H7A H -0.1792 0.1642 0.3153 0.029 Uiso 1 1 calc R U .
C3 C 0.5610(5) 0.3804(4) 0.4074(3) 0.0229(8) Uani 1 1 d . . .
H3A H 0.6675 0.3734 0.4509 0.027 Uiso 1 1 calc R U .
C9 C 0.0477(5) 0.5119(4) 0.3743(3) 0.0227(8) Uani 1 1 d . . .
H9A H -0.0515 0.5516 0.4095 0.027 Uiso 1 1 calc R U .
C1 C 0.4376(5) 0.0690(4) 0.1224(3) 0.0244(8) Uani 1 1 d . . .
H1A H 0.5120 -0.0037 0.1099 0.029 Uiso 1 1 calc R U .
C4 C 0.7257(6) 0.4672(4) 0.1618(3) 0.0290(9) Uani 1 1 d . . .
H4A H 0.8579 0.4797 0.1546 0.035 Uiso 1 1 calc R U .
C2 C -0.0702(5) 0.1792(4) 0.0730(3) 0.0283(8) Uani 1 1 d . . .
H2A H -0.1947 0.1427 0.0364 0.034 Uiso 1 1 calc R U .
C6 C 0.2285(6) 0.2151(4) -0.1451(3) 0.0334(9) Uani 1 1 d . . .
H6A H 0.1096 0.2510 -0.1303 0.040 Uiso 1 1 calc R U .
H1WB H 0.090(7) -0.220(5) 0.379(3) 0.040(13) Uiso 1 1 d . . .
H1WA H -0.009(9) -0.144(6) 0.328(4) 0.07(2) Uiso 1 1 d . . .
H21 H 0.583(10) 0.007(7) 0.695(5) 0.07(2) Uiso 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'
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'
Mg Mg 0.0486 0.0363 '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 O12 94.13(11) . .
O1 Fe1 O14 177.70(10) . .
O12 Fe1 O14 88.12(11) . .
O1 Fe1 O2 93.33(10) . .
O12 Fe1 O2 172.22(11) . .
O14 Fe1 O2 84.43(11) . .
O1 Fe1 O11 94.65(10) . .
O12 Fe1 O11 90.86(12) . .
O14 Fe1 O11 85.73(11) . .
O2 Fe1 O11 86.34(12) . .
O1 Fe1 O4 92.78(11) . .
O12 Fe1 O4 89.40(13) . .
O14 Fe1 O4 86.82(11) . .
O2 Fe1 O4 92.44(12) . .
O11 Fe1 O4 172.53(11) . .
O1 Fe2 O5 94.87(10) . .
O1 Fe2 O3 97.18(10) . .
O5 Fe2 O3 92.03(12) . .
O1 Fe2 O6 93.75(10) . .
O5 Fe2 O6 170.66(11) . .
O3 Fe2 O6 83.32(12) . .
O1 Fe2 O16 176.08(10) . .
O5 Fe2 O16 88.47(11) . .
O3 Fe2 O16 84.73(10) . .
O6 Fe2 O16 83.05(11) . .
O1 Fe2 O8 94.81(10) . .
O5 Fe2 O8 90.08(12) . .
O3 Fe2 O8 167.60(10) . .
O6 Fe2 O8 92.78(12) . .
O16 Fe2 O8 83.12(10) . .
O1 Fe3 O10 96.35(10) . .
O1 Fe3 O19 175.16(10) . 2_666
O10 Fe3 O19 88.38(11) . 2_666
O1 Fe3 O13 95.98(10) . .
O10 Fe3 O13 90.55(12) . .
O19 Fe3 O13 85.00(11) 2_666 .
O1 Fe3 O7 93.40(10) . .
O10 Fe3 O7 85.89(11) . .
O19 Fe3 O7 85.86(11) 2_666 .
O13 Fe3 O7 170.28(11) . .
O1 Fe3 O9 94.03(10) . .
O10 Fe3 O9 169.59(10) . .
O19 Fe3 O9 81.26(10) 2_666 .
O13 Fe3 O9 87.51(11) . .
O7 Fe3 O9 94.37(11) . .
O17 Mg1 O17 180.0 2_556 .
O17 Mg1 O18 95.29(10) 2_556 2_556
O17 Mg1 O18 84.71(10) . 2_556
O17 Mg1 O18 84.71(10) 2_556 .
O17 Mg1 O18 95.29(10) . .
O18 Mg1 O18 180.0 2_556 .
O17 Mg1 O1W 90.54(12) 2_556 .
O17 Mg1 O1W 89.46(12) . .
O18 Mg1 O1W 89.67(11) 2_556 .
O18 Mg1 O1W 90.32(11) . .
O17 Mg1 O1W 89.46(12) 2_556 2_556
O17 Mg1 O1W 90.54(12) . 2_556
O18 Mg1 O1W 90.32(11) 2_556 2_556
O18 Mg1 O1W 89.68(11) . 2_556
O1W Mg1 O1W 180.0 . 2_556
Fe3 O1 Fe2 120.79(11) . .
Fe3 O1 Fe1 119.54(12) . .
Fe2 O1 Fe1 119.61(11) . .
C8 O19 Fe3 131.2(2) . 2_666
C9 O9 Fe3 129.1(2) . .
C8 O18 Mg1 128.8(2) . .
C3 O7 Fe3 133.1(2) . .
C7 O17 Mg1 134.7(2) . .
C4 O11 Fe1 133.3(2) . .
C3 O6 Fe2 129.5(2) . .
C7 O16 Fe2 125.3(2) . .
C1 O3 Fe2 130.5(2) . .
C2 O4 Fe1 134.5(3) . .
C1 O2 Fe1 133.0(2) . .
C5 O13 Fe3 131.7(2) . .
Mg1 O1W H1WB 113(3) . .
Mg1 O1W H1WA 108(4) . .
H1WB O1W H1WA 122(5) . .
C9 O8 Fe2 133.4(2) . .
C5 O12 Fe1 132.1(2) . .
O12 C5 O13 126.9(3) . .
O12 C5 H5A 116.5 . .
O13 C5 H5A 116.5 . .
C6 O14 Fe1 127.5(3) . .
C2 O5 Fe2 129.3(2) . .
H24 N1 H23 115.7 . .
H24 N1 H22 115.7 . .
H23 N1 H22 90.3 . .
H24 N1 H21 81.0 . .
H23 N1 H21 127.5 . .
H22 N1 H21 128.7 . .
C4 O10 Fe3 129.8(2) . .
O18 C8 O19 125.2(3) . .
O18 C8 H8A 117.4 . .
O19 C8 H8A 117.4 . .
O17 C7 O16 125.8(3) . .
O17 C7 H7A 117.1 . .
O16 C7 H7A 117.1 . .
O6 C3 O7 126.9(3) . .
O6 C3 H3A 116.5 . .
O7 C3 H3A 116.5 . .
O9 C9 O8 127.0(3) . .
O9 C9 H9A 116.5 . .
O8 C9 H9A 116.5 . .
O2 C1 O3 127.1(3) . .
O2 C1 H1A 116.5 . .
O3 C1 H1A 116.5 . .
O11 C4 O10 128.0(3) . .
O11 C4 H4A 116.0 . .
O10 C4 H4A 116.0 . .
O4 C2 O5 127.5(3) . .
O4 C2 H2A 116.2 . .
O5 C2 H2A 116.2 . .
O15 C6 O14 126.9(4) . .
O15 C6 H6A 116.6 . .
O14 C6 H6A 116.6 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 O1 1.938(2) .
Fe1 O12 2.015(3) .
Fe1 O14 2.015(3) .
Fe1 O2 2.024(3) .
Fe1 O11 2.025(3) .
Fe1 O4 2.033(3) .
Fe2 O1 1.917(2) .
Fe2 O5 2.004(3) .
Fe2 O3 2.020(3) .
Fe2 O6 2.027(3) .
Fe2 O16 2.028(2) .
Fe2 O8 2.041(3) .
Fe3 O1 1.903(2) .
Fe3 O10 2.020(3) .
Fe3 O19 2.023(3) 2_666
Fe3 O13 2.025(3) .
Fe3 O7 2.038(2) .
Fe3 O9 2.054(2) .
Mg1 O17 2.074(2) 2_556
Mg1 O17 2.074(2) .
Mg1 O18 2.084(2) 2_556
Mg1 O18 2.084(2) .
Mg1 O1W 2.098(3) .
Mg1 O1W 2.098(3) 2_556
O19 C8 1.240(4) .
O19 Fe3 2.023(3) 2_666
O9 C9 1.239(4) .
O18 C8 1.240(4) .
O7 C3 1.246(4) .
O17 C7 1.251(4) .
O11 C4 1.237(5) .
O6 C3 1.237(4) .
O16 C7 1.251(4) .
O3 C1 1.248(4) .
O4 C2 1.234(5) .
O2 C1 1.231(4) .
O13 C5 1.256(4) .
O15 C6 1.210(5) .
O1W H1WB 0.88(5) .
O1W H1WA 0.77(6) .
O8 C9 1.244(4) .
O12 C5 1.232(5) .
C5 H5A 0.9300 .
O14 C6 1.247(5) .
O5 C2 1.249(5) .
N1 H24 0.9600 .
N1 H23 0.9600 .
N1 H22 0.9599 .
N1 H21 0.60(6) .
O10 C4 1.241(5) .
C8 H8A 0.9300 .
C7 H7A 0.9300 .
C3 H3A 0.9300 .
C9 H9A 0.9300 .
C1 H1A 0.9300 .
C4 H4A 0.9300 .
C2 H2A 0.9300 .
C6 H6A 0.9300 .
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
Fe1 O12 C5 O13 -11.6(6) .
Fe3 O13 C5 O12 3.4(6) .
Mg1 O18 C8 O19 144.7(3) .
Fe3 O19 C8 O18 -163.2(3) 2_666
Mg1 O17 C7 O16 -13.0(6) .
Fe2 O16 C7 O17 -155.3(3) .
Fe2 O6 C3 O7 4.3(6) .
Fe3 O7 C3 O6 -19.8(6) .
Fe3 O9 C9 O8 -7.0(6) .
Fe2 O8 C9 O9 -12.0(6) .
Fe1 O2 C1 O3 1.7(6) .
Fe2 O3 C1 O2 -15.6(6) .
Fe1 O11 C4 O10 -6.6(7) .
Fe3 O10 C4 O11 0.5(6) .
Fe1 O4 C2 O5 -4.5(7) .
Fe2 O5 C2 O4 -5.5(6) .
Fe1 O14 C6 O15 -173.8(3) .
