#------------------------------------------------------------------------------
#$Date: 2016-03-23 21:59:38 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179461 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/58/4335885.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_4335885
loop_
_publ_author_name
'Matteo Atzori'
'Samia Benmansour'
'Guillermo Mínguez Espallargas'
'Miguel Clemente-León'
'Alexandre Abhervé'
'Patricia Gómez-Claramunt'
'Eugenio Coronado'
'Flavia Artizzu'
'Elisa Sessini'
'Paola Deplano'
'Angela Serpe'
'Maria Laura Mercuri'
'Carlos J. Gómez García'
_publ_section_title
;
 A Family of Layered Chiral Porous Magnets Exhibiting Tunable Ordering
 Temperatures
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10031
_journal_page_last               10040
_journal_paper_doi               10.1021/ic4013284
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety
'C18 Br6 Fe Mn O12, 3(C12 H8 N2), (H2 O), (H3 O)'
_chemical_formula_sum            'C54 H29 Br6 Fe Mn N6 O14'
_chemical_formula_weight         1576.08
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           162
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-P 3 2'
_symmetry_space_group_name_H-M   'P -3 1 m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            1
_cell_length_a                   13.9147(2)
_cell_length_b                   13.9147(2)
_cell_length_c                   9.1747(4)
_cell_measurement_reflns_used    3631
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.4360
_cell_measurement_theta_min      2.9219
_cell_volume                     1538.40(7)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 16.0267
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type
'SuperNova, Single source at offset), Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Mo) x-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0553
_diffrn_reflns_av_sigmaI/netI    0.0213
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            23232
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.93
_exptl_absorpt_coefficient_mu    4.402
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85453
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.701
_exptl_crystal_description       needle
_exptl_crystal_F_000             768
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.310
_refine_diff_density_min         -1.129
_refine_diff_density_rms         0.226
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.153
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     66
_refine_ls_number_reflns         1270
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.153
_refine_ls_R_factor_all          0.0673
_refine_ls_R_factor_gt           0.0557
_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)+(0.1364P)²+3.6404P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2048
_refine_ls_wR_factor_ref         0.2157
_reflns_number_gt                1048
_reflns_number_total             1270
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic4013284_si_003.cif
_cod_data_source_block           sbml60b4
_cod_database_code               4335885
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-y, -x, -z'
'-x+y, y, -z'
'x, x-y, -z'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'y, x, z'
'x-y, -y, z'
'-x, -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
_atom_site_disorder_group
Mn1 Mn 0.6667 0.3333 1.0000 0.0219(5) Uani 0.50 6 d SP 1
Fe1 Fe 0.6667 0.3333 1.0000 0.0219(5) Uani 0.50 6 d SP 2
C1 C 0.4249(5) 0.0000 1.1091(7) 0.0195(13) Uani 1 2 d S .
Br1 Br 0.32500(5) 0.0000 1.24856(8) 0.0269(4) Uani 1 2 d S .
C2 C 0.5126(4) 0.1010(4) 1.0616(5) 0.0189(10) Uani 1 1 d . .
O2 O 0.5372(3) 0.1950(3) 1.1095(4) 0.0254(9) Uani 1 1 d . .
N11 N 0.4412(3) -0.1176(5) 1.5000 0.0262(13) Uani 1 2 d S .
C12 C 0.4091(4) -0.0596(4) 1.5867(5) 0.0238(11) Uani 1 1 d . .
C13 C 0.3157(5) -0.1175(5) 1.6787(6) 0.0299(12) Uani 1 1 d . .
H13 H 0.2752 -0.1964 1.6796 0.036 Uiso 1 1 calc R .
C14 C 0.2846(5) -0.0585(6) 1.7662(7) 0.0337(13) Uani 1 1 d . .
H14 H 0.2222 -0.0970 1.8285 0.040 Uiso 1 1 calc R .
O11W O 0.3333(5) -0.3334(6) 1.5000(7) 0.085(6) Uiso 1 6 d SRD .
H11W H 0.3689 -0.2622 1.5000 0.127 Uiso 0.83 2 d SPRD .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Mn1 0.0118(6) 0.0118(6) 0.0420(12) 0.000 0.000 0.0059(3)
Fe1 0.0118(6) 0.0118(6) 0.0420(12) 0.000 0.000 0.0059(3)
C1 0.016(2) 0.022(3) 0.023(3) 0.000 0.002(2) 0.0108(17)
Br1 0.0232(4) 0.0302(5) 0.0296(6) 0.000 0.0056(2) 0.0151(3)
C2 0.015(2) 0.021(2) 0.023(2) -0.0026(18) -0.0033(18) 0.0112(19)
O2 0.026(2) 0.0208(19) 0.034(2) 0.0007(15) 0.0029(16) 0.0155(17)
N11 0.025(2) 0.023(3) 0.029(3) 0.000 -0.007(2) 0.0113(15)
C12 0.025(3) 0.023(3) 0.023(2) -0.0008(19) -0.004(2) 0.011(2)
C13 0.027(3) 0.025(3) 0.032(3) 0.001(2) -0.006(2) 0.008(2)
C14 0.028(3) 0.042(4) 0.031(3) 0.003(3) 0.002(2) 0.018(3)
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'
Br Br -0.2901 2.4595 '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
O2 Mn1 O2 85.2(2) 5_657 2_655
O2 Mn1 O2 76.26(19) 5_657 .
O2 Mn1 O2 99.39(14) 2_655 .
O2 Mn1 O2 99.39(14) 5_657 4_667
O2 Mn1 O2 76.26(19) 2_655 4_667
O2 Mn1 O2 174.20(17) . 4_667
O2 Mn1 O2 99.39(14) 5_657 6_557
O2 Mn1 O2 174.20(18) 2_655 6_557
O2 Mn1 O2 85.2(2) . 6_557
O2 Mn1 O2 99.39(14) 4_667 6_557
O2 Mn1 O2 174.20(18) 5_657 3_665
O2 Mn1 O2 99.39(14) 2_655 3_665
O2 Mn1 O2 99.39(14) . 3_665
O2 Mn1 O2 85.2(2) 4_667 3_665
O2 Mn1 O2 76.26(19) 6_557 3_665
C2 C1 C2 121.8(6) . 11
C2 C1 Br1 119.1(3) . .
C2 C1 Br1 119.1(3) 11 .
O2 C2 C1 126.0(4) . .
O2 C2 C2 115.2(3) . 5_657
C1 C2 C2 118.8(3) . 5_657
C2 O2 Mn1 116.5(3) . .
C12 N11 C12 118.0(6) 5_658 .
N11 C12 C13 119.5(5) . .
N11 C12 C12 121.0(3) . 11
C13 C12 C12 119.5(3) . 11
C14 C13 C12 119.0(6) . .
C14 C13 H13 120.5 . .
C12 C13 H13 120.5 . .
C13 C14 C14 121.4(4) . 11
C13 C14 H14 119.3 . .
C14 C14 H14 119.3 11 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mn1 O2 2.119(4) 5_657
Mn1 O2 2.119(4) 2_655
Mn1 O2 2.119(4) .
Mn1 O2 2.119(4) 4_667
Mn1 O2 2.119(4) 6_557
Mn1 O2 2.119(4) 3_665
C1 C2 1.393(6) .
C1 C2 1.393(6) 11
C1 Br1 1.889(7) .
C2 O2 1.254(6) .
C2 C2 1.546(9) 5_657
N11 C12 1.358(6) 5_658
N11 C12 1.358(6) .
C12 C13 1.416(7) .
C12 C12 1.437(10) 11
C13 C14 1.365(8) .
C13 H13 0.9500 .
C14 C14 1.410(14) 11
C14 H14 0.9500 .
O11W H11W 0.8574 .
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
C2 C1 C2 O2 -172.4(4) 11 .
Br1 C1 C2 O2 4.7(8) . .
C2 C1 C2 C2 7.9(10) 11 5_657
Br1 C1 C2 C2 -175.0(5) . 5_657
C1 C2 O2 Mn1 -174.4(4) . .
C2 C2 O2 Mn1 5.3(6) 5_657 .
O2 Mn1 O2 C2 -2.1(3) 5_657 .
O2 Mn1 O2 C2 -84.8(4) 2_655 .
O2 Mn1 O2 C2 -43.9(3) 4_667 .
O2 Mn1 O2 C2 98.8(4) 6_557 .
O2 Mn1 O2 C2 174.0(3) 3_665 .
C12 N11 C12 C13 -179.8(5) 5_658 .
C12 N11 C12 C12 0.000(1) 5_658 11
N11 C12 C13 C14 179.5(5) . .
C12 C12 C13 C14 -0.3(6) 11 .
C12 C13 C14 C14 0.3(6) . 11
