#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:16:27 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179369 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/66/4326630.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_4326630
loop_
_publ_author_name
'Jung Hee Yoon'
'Woo Ram Lee'
'Dae Won Ryu'
'Jin Wuk Lee'
'Sung Won Yoon'
'Byoung Jin Suh'
'Hyoung Chan Kim'
'Chang Seop Hong'
_publ_section_title
;
 End-to-End Azide-Bridged Manganese(III) Chain Compounds: Field-Induced
 Magnetic Phase Transitions and Variation of TC to 38 K Depending on the
 Side Groups of the Schiff Bases
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10777
_journal_page_last               10785
_journal_paper_doi               10.1021/ic2013232
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C38 H36 Br4 Mn2 N10 O4'
_chemical_formula_weight         1126.29
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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
_cell_angle_alpha                97.999(4)
_cell_angle_beta                 112.472(3)
_cell_angle_gamma                96.399(3)
_cell_formula_units_Z            2
_cell_length_a                   11.8425(10)
_cell_length_b                   12.7124(10)
_cell_length_c                   15.4367(16)
_cell_measurement_reflns_used    2995
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.943
_cell_measurement_theta_min      2.273
_cell_volume                     2091.9(3)
_computing_cell_refinement       'Bruker SMART APEXll'
_computing_data_collection       'Bruker SMART APEXll'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    WingX
_computing_publication_material  WingX
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SHELXTL
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.946
_diffrn_measured_fraction_theta_max 0.946
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega scan'
_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  0.1799
_diffrn_reflns_av_sigmaI/netI    0.2425
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            33430
_diffrn_reflns_theta_full        28.43
_diffrn_reflns_theta_max         28.43
_diffrn_reflns_theta_min         1.46
_exptl_absorpt_coefficient_mu    4.477
_exptl_absorpt_correction_T_max  0.9158
_exptl_absorpt_correction_T_min  0.5063
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.788
_exptl_crystal_description       plate
_exptl_crystal_F_000             1112
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.212
_refine_diff_density_min         -1.239
_refine_diff_density_rms         0.177
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     523
_refine_ls_number_reflns         9962
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.994
_refine_ls_R_factor_all          0.2316
_refine_ls_R_factor_gt           0.0764
_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)+(0.0711P)²+9.0882P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1558
_refine_ls_wR_factor_ref         0.2148
_reflns_number_gt                3973
_reflns_number_total             9962
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2013232_si_002.cif
_cod_data_source_block           p-1
_cod_database_code               4326630
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
Mn1 Mn -0.19221(13) 0.27642(12) 0.86940(11) 0.0254(4) Uani 1 1 d .
N1 N 0.0075(8) 0.3472(7) 0.8948(6) 0.033(2) Uani 1 1 d .
N2 N 0.0843(7) 0.2922(6) 0.9145(6) 0.0240(19) Uani 1 1 d .
N3 N 0.1619(8) 0.2395(7) 0.9378(6) 0.035(2) Uani 1 1 d .
N4 N -0.1967(8) 0.3942(6) 0.9688(6) 0.029(2) Uani 1 1 d .
N5 N -0.2516(7) 0.3645(6) 0.7633(6) 0.0253(19) Uani 1 1 d .
O1 O -0.1235(6) 0.1962(5) 0.9660(5) 0.0318(17) Uani 1 1 d .
O2 O -0.1936(6) 0.1598(5) 0.7782(5) 0.0338(18) Uani 1 1 d .
C1 C -0.0455(10) 0.2349(9) 1.0557(9) 0.038(3) Uani 1 1 d .
C2 C 0.0371(11) 0.1743(10) 1.1085(9) 0.045(3) Uani 1 1 d .
H2 H 0.0423 0.1075 1.0783 0.055 Uiso 1 1 calc R
C3 C 0.1099(11) 0.2103(12) 1.2027(10) 0.052(4) Uani 1 1 d .
H3 H 0.1648 0.1683 1.2354 0.063 Uiso 1 1 calc R
C4 C 0.1043(10) 0.3075(11) 1.2509(8) 0.044(3) Uani 1 1 d .
C5 C 0.0270(10) 0.3727(10) 1.2039(8) 0.042(3) Uani 1 1 d .
H5 H 0.0246 0.4393 1.2362 0.051 Uiso 1 1 calc R
C6 C -0.0496(8) 0.3365(8) 1.1048(7) 0.025(2) Uani 1 1 d .
C7 C -0.1330(9) 0.4067(8) 1.0582(8) 0.028(2) Uani 1 1 d .
H7 H -0.1404 0.4658 1.0973 0.034 Uiso 1 1 calc R
C8 C -0.2856(10) 0.4715(8) 0.9401(8) 0.034(3) Uani 1 1 d .
H8A H -0.3698 0.4325 0.9181 0.041 Uiso 1 1 calc R
H8B H -0.2702 0.5263 0.9957 0.041 Uiso 1 1 calc R
C9 C -0.2741(10) 0.5257(8) 0.8624(7) 0.034(3) Uani 1 1 d .
H9A H -0.1871 0.5543 0.8804 0.040 Uiso 1 1 calc R
H9B H -0.3177 0.5862 0.8583 0.040 Uiso 1 1 calc R
C10 C -0.3250(9) 0.4521(8) 0.7634(7) 0.026(2) Uani 1 1 d .
H10 H -0.3142 0.4963 0.7190 0.031 Uiso 1 1 calc R
C11 C -0.4622(9) 0.4027(9) 0.7239(8) 0.039(3) Uani 1 1 d .
H11A H -0.5070 0.4568 0.7391 0.046 Uiso 1 1 calc R
H11B H -0.4721 0.3438 0.7557 0.046 Uiso 1 1 calc R
C12 C -0.5199(12) 0.3602(11) 0.6164(9) 0.063(4) Uani 1 1 d .
H12A H -0.6061 0.3305 0.5963 0.094 Uiso 1 1 calc R
H12B H -0.4777 0.3050 0.6009 0.094 Uiso 1 1 calc R
H12C H -0.5122 0.4182 0.5842 0.094 Uiso 1 1 calc R
C13 C -0.2212(9) 0.3468(8) 0.6909(7) 0.028(2) Uani 1 1 d .
H13 H -0.2374 0.3963 0.6506 0.033 Uiso 1 1 calc R
C14 C -0.1646(9) 0.2585(8) 0.6658(7) 0.024(2) Uani 1 1 d .
C15 C -0.1255(9) 0.2639(8) 0.5897(7) 0.029(2) Uani 1 1 d .
H15 H -0.1285 0.3254 0.5630 0.035 Uiso 1 1 calc R
C16 C -0.0836(9) 0.1784(8) 0.5563(7) 0.026(2) Uani 1 1 d .
C17 C -0.0817(9) 0.0855(8) 0.5936(8) 0.036(3) Uani 1 1 d .
H17 H -0.0549 0.0269 0.5690 0.043 Uiso 1 1 calc R
C18 C -0.1202(9) 0.0796(8) 0.6684(8) 0.032(3) Uani 1 1 d .
H18 H -0.1196 0.0166 0.6928 0.038 Uiso 1 1 calc R
C19 C -0.1597(9) 0.1684(8) 0.7073(8) 0.028(2) Uani 1 1 d .
Br1 Br 0.20647(11) 0.35403(12) 1.38418(9) 0.0566(4) Uani 1 1 d .
Br2 Br -0.01667(11) 0.18882(9) 0.46368(8) 0.0388(3) Uani 1 1 d .
Mn2 Mn 0.34906(13) 0.20417(12) 0.94842(11) 0.0241(4) Uani 1 1 d .
N6 N 0.5258(8) 0.1556(7) 0.9500(7) 0.042(3) Uani 1 1 d .
N7 N 0.5717(7) 0.1825(7) 0.8988(7) 0.032(2) Uani 1 1 d .
N8 N 0.6128(8) 0.2046(7) 0.8441(7) 0.037(2) Uani 1 1 d .
N9 N 0.3021(8) 0.0577(6) 0.9744(6) 0.031(2) Uani 1 1 d .
N10 N 0.2641(8) 0.1530(7) 0.8015(6) 0.034(2) Uani 1 1 d .
O3 O 0.4228(6) 0.2626(5) 1.0814(5) 0.0272(16) Uani 1 1 d .
O4 O 0.4009(6) 0.3423(5) 0.9310(5) 0.0304(17) Uani 1 1 d .
C20 C 0.4190(9) 0.2187(8) 1.1536(7) 0.026(2) Uani 1 1 d .
C21 C 0.4774(9) 0.2850(8) 1.2460(7) 0.031(3) Uani 1 1 d .
H21 H 0.5167 0.3553 1.2535 0.037 Uiso 1 1 calc R
C22 C 0.4766(9) 0.2467(8) 1.3243(7) 0.029(2) Uani 1 1 d .
H22 H 0.5149 0.2919 1.3842 0.034 Uiso 1 1 calc R
C23 C 0.4206(10) 0.1428(9) 1.3167(7) 0.033(3) Uani 1 1 d .
C24 C 0.3657(9) 0.0760(8) 1.2272(7) 0.030(2) Uani 1 1 d .
H24 H 0.3295 0.0051 1.2215 0.036 Uiso 1 1 calc R
C25 C 0.3632(9) 0.1127(8) 1.1450(7) 0.025(2) Uani 1 1 d .
C26 C 0.3084(9) 0.0399(8) 1.0556(8) 0.027(2) Uani 1 1 d .
H26 H 0.2729 -0.0290 1.0560 0.032 Uiso 1 1 calc R
C27 C 0.2633(14) -0.0386(9) 0.8947(9) 0.072(5) Uani 1 1 d .
H27A H 0.3369 -0.0551 0.8862 0.087 Uiso 1 1 calc R
H27B H 0.2299 -0.0998 0.9142 0.087 Uiso 1 1 calc R
C28 C 0.1745(16) -0.0284(12) 0.8051(10) 0.088(6) Uani 1 1 d .
H28A H 0.1094 0.0047 0.8152 0.106 Uiso 1 1 calc R
H28B H 0.1368 -0.0998 0.7659 0.106 Uiso 1 1 calc R
C29 C 0.2298(13) 0.0394(9) 0.7509(9) 0.051(3) Uani 1 1 d .
H29 H 0.1597 0.0384 0.6905 0.062 Uiso 1 1 calc R
C30 C 0.3321(13) 0.0054(10) 0.7212(9) 0.061(4) Uani 1 1 d .
H30A H 0.3104 -0.0714 0.6944 0.073 Uiso 1 1 calc R
H30B H 0.4092 0.0176 0.7778 0.073 Uiso 1 1 calc R
C31 C 0.3538(13) 0.0674(12) 0.6463(10) 0.072(4) Uani 1 1 d .
H31A H 0.4206 0.0442 0.6325 0.108 Uiso 1 1 calc R
H31B H 0.3745 0.1436 0.6719 0.108 Uiso 1 1 calc R
H31C H 0.2794 0.0523 0.5885 0.108 Uiso 1 1 calc R
C32 C 0.2297(10) 0.2217(9) 0.7485(8) 0.036(3) Uani 1 1 d .
H32 H 0.1814 0.1920 0.6844 0.043 Uiso 1 1 calc R
C33 C 0.2535(9) 0.3375(9) 0.7716(7) 0.031(3) Uani 1 1 d .
C34 C 0.1958(10) 0.3954(9) 0.7013(7) 0.035(3) Uani 1 1 d .
H34 H 0.1403 0.3584 0.6408 0.042 Uiso 1 1 calc R
C35 C 0.2206(9) 0.5076(10) 0.7210(7) 0.035(3) Uani 1 1 d .
C36 C 0.3119(9) 0.5621(8) 0.8093(7) 0.030(2) Uani 1 1 d .
H36 H 0.3326 0.6371 0.8217 0.037 Uiso 1 1 calc R
C37 C 0.3704(9) 0.5065(8) 0.8766(7) 0.028(2) Uani 1 1 d .
H37 H 0.4310 0.5444 0.9348 0.034 Uiso 1 1 calc R
C38 C 0.3429(9) 0.3935(8) 0.8619(7) 0.028(2) Uani 1 1 d .
Br3 Br 0.42080(13) 0.09227(10) 1.42602(8) 0.0472(4) Uani 1 1 d .
Br4 Br 0.13884(12) 0.58539(12) 0.62719(9) 0.0562(4) Uani 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'
Mn Mn 0.3368 0.7283 '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 O1 88.6(3) . .
O2 Mn1 N4 176.6(3) . .
O1 Mn1 N4 89.5(3) . .
O2 Mn1 N5 89.5(3) . .
O1 Mn1 N5 174.8(3) . .
N4 Mn1 N5 92.7(3) . .
O2 Mn1 N8 89.3(3) . 1_455
O1 Mn1 N8 91.8(3) . 1_455
N4 Mn1 N8 88.0(3) . 1_455
N5 Mn1 N8 93.0(3) . 1_455
O2 Mn1 N1 90.0(3) . .
O1 Mn1 N1 87.7(3) . .
N4 Mn1 N1 92.7(3) . .
N5 Mn1 N1 87.5(3) . .
N8 Mn1 N1 179.1(3) 1_455 .
N2 N1 Mn1 119.1(6) . .
N3 N2 N1 177.4(10) . .
N2 N3 Mn2 149.6(7) . .
C7 N4 C8 115.0(9) . .
C7 N4 Mn1 124.7(7) . .
C8 N4 Mn1 120.1(7) . .
C13 N5 C10 115.5(8) . .
C13 N5 Mn1 119.4(7) . .
C10 N5 Mn1 125.1(6) . .
C1 O1 Mn1 127.1(7) . .
C19 O2 Mn1 125.4(6) . .
O1 C1 C2 121.6(11) . .
O1 C1 C6 121.1(10) . .
C2 C1 C6 117.1(11) . .
C3 C2 C1 121.6(12) . .
C2 C3 C4 121.5(11) . .
C5 C4 C3 120.5(11) . .
C5 C4 Br1 119.4(10) . .
C3 C4 Br1 120.1(9) . .
C4 C5 C6 118.8(11) . .
C1 C6 C5 120.4(10) . .
C1 C6 C7 122.5(10) . .
C5 C6 C7 117.1(10) . .
N4 C7 C6 125.7(10) . .
C9 C8 N4 112.8(8) . .
C8 C9 C10 114.6(9) . .
N5 C10 C11 109.3(8) . .
N5 C10 C9 110.7(8) . .
C11 C10 C9 115.0(8) . .
C10 C11 C12 113.8(9) . .
N5 C13 C14 127.3(9) . .
C19 C14 C15 121.3(9) . .
C19 C14 C13 121.7(9) . .
C15 C14 C13 116.7(9) . .
C16 C15 C14 119.4(9) . .
C15 C16 C17 120.8(9) . .
C15 C16 Br2 120.2(8) . .
C17 C16 Br2 118.9(7) . .
C16 C17 C18 120.0(9) . .
C17 C18 C19 120.6(10) . .
O2 C19 C14 123.7(9) . .
O2 C19 C18 118.6(9) . .
C14 C19 C18 117.7(10) . .
O4 Mn2 O3 86.8(3) . .
O4 Mn2 N9 176.7(3) . .
O3 Mn2 N9 90.4(3) . .
O4 Mn2 N10 89.2(3) . .
O3 Mn2 N10 175.1(3) . .
N9 Mn2 N10 93.7(3) . .
O4 Mn2 N6 89.9(3) . .
O3 Mn2 N6 92.3(3) . .
N9 Mn2 N6 88.5(3) . .
N10 Mn2 N6 90.6(4) . .
O4 Mn2 N3 93.5(3) . .
O3 Mn2 N3 91.5(3) . .
N9 Mn2 N3 88.3(3) . .
N10 Mn2 N3 85.8(3) . .
N6 Mn2 N3 175.0(3) . .
N7 N6 Mn2 122.5(8) . .
N8 N7 N6 176.3(11) . .
N7 N8 Mn1 129.9(8) . 1_655
C26 N9 C27 116.9(9) . .
C26 N9 Mn2 124.8(7) . .
C27 N9 Mn2 118.1(7) . .
C32 N10 C29 115.3(9) . .
C32 N10 Mn2 119.6(7) . .
C29 N10 Mn2 125.0(7) . .
C20 O3 Mn2 129.5(6) . .
C38 O4 Mn2 128.6(6) . .
O3 C20 C25 125.0(9) . .
O3 C20 C21 116.7(9) . .
C25 C20 C21 118.3(9) . .
C22 C21 C20 120.5(10) . .
C21 C22 C23 121.7(10) . .
C22 C23 C24 118.5(9) . .
C22 C23 Br3 120.7(8) . .
C24 C23 Br3 120.8(8) . .
C23 C24 C25 121.5(10) . .
C20 C25 C24 119.4(9) . .
C20 C25 C26 121.5(9) . .
C24 C25 C26 119.0(9) . .
N9 C26 C25 127.7(9) . .
C28 C27 N9 116.2(12) . .
C27 C28 C29 113.3(13) . .
N10 C29 C30 111.2(10) . .
N10 C29 C28 108.5(10) . .
C30 C29 C28 121.3(12) . .
C29 C30 C31 113.7(11) . .
N10 C32 C33 130.5(10) . .
C34 C33 C38 119.6(10) . .
C34 C33 C32 119.5(10) . .
C38 C33 C32 120.6(10) . .
C35 C34 C33 120.6(10) . .
C34 C35 C36 119.2(10) . .
C34 C35 Br4 120.5(8) . .
C36 C35 Br4 120.2(9) . .
C37 C36 C35 120.2(10) . .
C36 C37 C38 122.4(10) . .
O4 C38 C37 120.3(9) . .
O4 C38 C33 122.0(9) . .
C37 C38 C33 117.7(9) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mn1 O2 1.891(7) .
Mn1 O1 1.900(7) .
Mn1 N4 2.010(9) .
Mn1 N5 2.058(8) .
Mn1 N8 2.249(9) 1_455
Mn1 N1 2.297(8) .
N1 N2 1.183(11) .
N2 N3 1.172(11) .
N3 Mn2 2.260(8) .
N4 C7 1.270(12) .
N4 C8 1.505(12) .
N5 C13 1.298(12) .
N5 C10 1.487(11) .
O1 C1 1.320(13) .
O2 C19 1.316(12) .
C1 C2 1.396(15) .
C1 C6 1.421(15) .
C2 C3 1.355(17) .
C3 C4 1.373(17) .
C4 C5 1.371(15) .
C4 Br1 1.909(12) .
C5 C6 1.422(14) .
C6 C7 1.457(13) .
C8 C9 1.504(14) .
C9 C10 1.532(13) .
C10 C11 1.521(14) .
C11 C12 1.522(15) .
C13 C14 1.450(13) .
C14 C19 1.383(13) .
C14 C15 1.426(14) .
C15 C16 1.361(13) .
C16 C17 1.383(14) .
C16 Br2 1.893(10) .
C17 C18 1.403(14) .
C18 C19 1.413(13) .
Mn2 O4 1.885(7) .
Mn2 O3 1.895(7) .
Mn2 N9 2.021(8) .
Mn2 N10 2.069(9) .
Mn2 N6 2.240(9) .
N6 N7 1.182(12) .
N7 N8 1.174(12) .
N8 Mn1 2.249(9) 1_655
N9 C26 1.281(12) .
N9 C27 1.499(14) .
N10 C32 1.273(13) .
N10 C29 1.474(14) .
O3 C20 1.327(11) .
O4 C38 1.329(11) .
C20 C25 1.398(13) .
C20 C21 1.416(14) .
C21 C22 1.367(13) .
C22 C23 1.378(13) .
C23 C24 1.384(14) .
C23 Br3 1.887(10) .
C24 C25 1.403(13) .
C25 C26 1.417(14) .
C27 C28 1.416(18) .
C28 C29 1.539(18) .
C29 C30 1.533(17) .
C30 C31 1.569(18) .
C32 C33 1.434(14) .
C33 C34 1.397(14) .
C33 C38 1.413(14) .
C34 C35 1.390(15) .
C35 C36 1.396(14) .
C35 Br4 1.885(10) .
C36 C37 1.351(13) .
C37 C38 1.403(13) .
