#------------------------------------------------------------------------------
#$Date: 2016-03-23 02:02:00 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179167 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/28/4312872.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_4312872
loop_
_publ_author_name
'S. Sailaja'
'K. Rajender Reddy'
'M. V. Rajasekharan'
'C. Hureau'
'E. Rivière'
'J. Cano'
'J.-J. Girerd'
_publ_section_title
;
 Synthesis, Structure, and Magnetic Properties of [MnIII(salpn)NCS]n, a
 Helical Polymer, and the Dimer [MnIII(salpn)NCS]2. Weak Ferromagnetism in
 [MnIII(salpn)NCS]n Related to the Strong Magnetic Anisotropy in
 Jahn-Teller Mn(III) (salpnH2=N,N'-Bis(salicylidene)-1,3-diaminopropane)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              180
_journal_page_last               186
_journal_paper_doi               10.1021/ic0256617
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C18 H16 Mn N3 O2 S'
_chemical_formula_weight         393.34
_chemical_name_systematic
; 
[{N,N'-bis(salicylidene)-1,3-diaminopropane}manganese(III)] thiocyanate
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-93
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.5277(14)
_cell_length_b                   11.576(2)
_cell_length_c                   11.513(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      13.5
_cell_measurement_theta_min      4.6
_cell_volume                     1669.6(4)
_computing_cell_refinement       'CAD-4 Data collection software'
_computing_data_collection       'CAD-4 Data collection software'
_computing_data_reduction        'XTAL-3.5 (Hall et al., 1996)'
_computing_molecular_graphics    'ORTEP-III (Burnett & Johnson, 1996)'
_computing_publication_material  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       CAD-4
_diffrn_measurement_method       w-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  0.0216
_diffrn_reflns_av_sigmaI/netI    0.0235
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3021
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         2.40
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  60
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.933
_exptl_absorpt_correction_T_max  99.93
_exptl_absorpt_correction_T_min  88.08
_exptl_absorpt_correction_type   semiempirical
_exptl_absorpt_process_details   'North et al., 1968'
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.565
_exptl_crystal_description       needle
_exptl_crystal_F_000             808
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.304
_refine_diff_density_min         -0.248
_refine_diff_density_rms         0.046
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.049
_refine_ls_goodness_of_fit_obs   1.053
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     227
_refine_ls_number_reflns         1543
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.064
_refine_ls_restrained_S_obs      1.052
_refine_ls_R_factor_all          0.0237
_refine_ls_R_factor_obs          0.0219
_refine_ls_shift/esd_max         0.006
_refine_ls_shift/esd_mean        0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0411P)²+0.1457P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0585
_refine_ls_wR_factor_obs         0.0563
_reflns_number_observed          1480
_reflns_number_total             1551
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic0256617_s1_2.cif
_cod_data_source_block           '[Mn(salpn)NCS]n'
_cod_database_code               4312872
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z+1/2'
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Mn1 Mn 0.01529(3) 0.10886(3) 0.00226(5) 0.02468(12) Uani 1 d . .
S1 S -0.07340(6) -0.17885(6) -0.27618(7) 0.0386(2) Uani 1 d . .
O1 O 0.13083(13) 0.0053(2) -0.0020(3) 0.0378(4) Uani 1 d . .
O2 O 0.10757(14) 0.2119(2) -0.0774(2) 0.0352(5) Uani 1 d . .
N1 N -0.0759(2) -0.0103(2) 0.0874(2) 0.0252(5) Uani 1 d . .
N2 N -0.09670(15) 0.2363(2) 0.0078(2) 0.0266(4) Uani 1 d . .
N3 N -0.0584(2) 0.0334(2) -0.1610(2) 0.0390(6) Uani 1 d . .
C1 C 0.1268(2) -0.1086(2) -0.0059(3) 0.0314(5) Uani 1 d . .
C2 C 0.2145(3) -0.1698(3) -0.0498(3) 0.0428(7) Uani 1 d . .
H2 H 0.2746(3) -0.1299(3) -0.0750(3) 0.044(2) Uiso 1 calc R .
C3 C 0.2123(3) -0.2888(3) -0.0557(3) 0.0500(8) Uani 1 d . .
H3 H 0.2704(3) -0.3281(3) -0.0868(3) 0.044(2) Uiso 1 calc R .
C4 C 0.1248(3) -0.3508(3) -0.0159(4) 0.0517(9) Uani 1 d . .
H4 H 0.1243(3) -0.4311(3) -0.0200(4) 0.044(2) Uiso 1 calc R .
C5 C 0.0399(3) -0.2930(3) 0.0291(3) 0.0457(9) Uani 1 d . .
H5 H -0.0187(3) -0.3342(3) 0.0563(3) 0.044(2) Uiso 1 calc R .
C6 C 0.0394(2) -0.1721(2) 0.0349(3) 0.0323(6) Uani 1 d . .
C7 C -0.0526(2) -0.1177(2) 0.0874(3) 0.0310(6) Uani 1 d . .
H7 H -0.1002(2) -0.1664(2) 0.1254(3) 0.044(2) Uiso 1 calc R .
C8 C -0.1712(2) 0.0222(3) 0.1556(3) 0.0337(6) Uani 1 d . .
H8A H -0.1486(2) 0.0514(3) 0.2307(3) 0.044(2) Uiso 1 calc R .
H8B H -0.2144(2) -0.0461(3) 0.1689(3) 0.044(2) Uiso 1 calc R .
C9 C -0.2382(2) 0.1128(2) 0.0955(3) 0.0349(7) Uani 1 d . .
H9A H -0.3062(2) 0.1191(2) 0.1351(3) 0.044(2) Uiso 1 calc R .
H9B H -0.2522(2) 0.0879(2) 0.0164(3) 0.044(2) Uiso 1 calc R .
C10 C -0.1854(2) 0.2309(2) 0.0925(3) 0.0335(6) Uani 1 d . .
H10A H -0.2384(2) 0.2887(2) 0.0725(3) 0.044(2) Uiso 1 calc R .
H10B H -0.1582(2) 0.2491(2) 0.1693(3) 0.044(2) Uiso 1 calc R .
C11 C -0.0972(2) 0.3249(2) -0.0594(3) 0.0317(6) Uani 1 d . .
H11 H -0.1576(2) 0.3715(2) -0.0568(3) 0.044(2) Uiso 1 calc R .
C12 C -0.0141(2) 0.3597(3) -0.1384(3) 0.0333(6) Uani 1 d . .
C13 C -0.0302(3) 0.4603(3) -0.2061(4) 0.0446(8) Uani 1 d . .
H13 H -0.0963(3) 0.4967(3) -0.2046(4) 0.044(2) Uiso 1 calc R .
C14 C 0.0497(3) 0.5050(3) -0.2739(3) 0.0495(9) Uani 1 d . .
H14 H 0.0380(3) 0.5708(3) -0.3185(3) 0.044(2) Uiso 1 calc R .
C15 C 0.1487(3) 0.4503(3) -0.2747(3) 0.0461(8) Uani 1 d . .
H15 H 0.2036(3) 0.4806(3) -0.3198(3) 0.044(2) Uiso 1 calc R .
C16 C 0.1670(2) 0.3520(3) -0.2102(3) 0.0393(7) Uani 1 d . .
H16 H 0.2338(2) 0.3170(3) -0.2128(3) 0.044(2) Uiso 1 calc R .
C17 C 0.0864(2) 0.3039(2) -0.1405(3) 0.0308(6) Uani 1 d . .
C18 C -0.0654(2) -0.0538(3) -0.2095(3) 0.0318(6) Uani 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'
S S 0.1246 0.1234 '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'
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
_geom_angle_publ_flag
O1 Mn1 O2 85.37(9) . . y
O1 Mn1 N2 173.20(8) . . y
O2 Mn1 N2 88.83(9) . . y
O1 Mn1 N1 90.70(9) . . y
O2 Mn1 N1 176.06(8) . . y
N2 Mn1 N1 95.10(9) . . y
O1 Mn1 N3 92.63(11) . . y
O2 Mn1 N3 95.13(10) . . y
N2 Mn1 N3 91.43(10) . . y
N1 Mn1 N3 84.84(10) . . y
O1 Mn1 S1 90.47(9) . 2 y
O2 Mn1 S1 95.80(8) . 2 y
N2 Mn1 S1 86.57(8) . 2 y
N1 Mn1 S1 84.41(7) . 2 y
N3 Mn1 S1 168.84(7) . 2 y
C18 S1 Mn1 99.00(11) . 2_554 ?
C1 O1 Mn1 127.5(2) . . ?
C17 O2 Mn1 130.7(2) . . ?
C7 N1 C8 115.6(2) . . ?
C7 N1 Mn1 122.0(2) . . ?
C8 N1 Mn1 122.4(2) . . ?
C11 N2 C10 115.3(2) . . ?
C11 N2 Mn1 124.2(2) . . ?
C10 N2 Mn1 120.5(2) . . ?
C18 N3 Mn1 140.0(2) . . ?
O1 C1 C6 122.9(2) . . ?
O1 C1 C2 119.1(3) . . ?
C6 C1 C2 118.0(2) . . ?
C3 C2 C1 120.5(3) . . ?
C2 C3 C4 121.1(3) . . ?
C5 C4 C3 119.3(3) . . ?
C4 C5 C6 120.9(3) . . ?
C1 C6 C5 120.3(3) . . ?
C1 C6 C7 122.4(3) . . ?
C5 C6 C7 117.3(3) . . ?
N1 C7 C6 127.3(3) . . ?
N1 C8 C9 112.4(2) . . ?
C8 C9 C10 113.2(2) . . ?
N2 C10 C9 112.3(2) . . ?
N2 C11 C12 126.9(3) . . ?
C17 C12 C13 119.5(3) . . ?
C17 C12 C11 121.8(3) . . ?
C13 C12 C11 118.4(3) . . ?
C14 C13 C12 121.4(3) . . ?
C13 C14 C15 118.8(3) . . ?
C16 C15 C14 121.3(3) . . ?
C15 C16 C17 121.1(3) . . ?
O2 C17 C16 119.4(3) . . ?
O2 C17 C12 122.6(3) . . ?
C16 C17 C12 117.9(3) . . ?
N3 C18 S1 178.7(3) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mn1 O1 1.880(2) . y
Mn1 O2 1.897(2) . y
Mn1 N2 2.037(2) . y
Mn1 N1 2.042(2) . y
Mn1 N3 2.270(3) . y
Mn1 S1 2.7737(11) 2 y
S1 C18 1.642(3) . ?
S1 Mn1 2.7737(11) 2_554 ?
O1 C1 1.320(3) . ?
O2 C17 1.316(3) . ?
N1 C7 1.277(3) . ?
N1 C8 1.477(3) . ?
N2 C11 1.285(4) . ?
N2 C10 1.480(4) . ?
N3 C18 1.156(4) . ?
C1 C6 1.400(4) . ?
C1 C2 1.402(4) . ?
C2 C3 1.380(4) . ?
C3 C4 1.388(5) . ?
C4 C5 1.360(5) . ?
C5 C6 1.401(4) . ?
C6 C7 1.446(4) . ?
C8 C9 1.512(4) . ?
C9 C10 1.519(4) . ?
C11 C12 1.439(4) . ?
C12 C17 1.416(4) . ?
C12 C13 1.416(5) . ?
C13 C14 1.371(5) . ?
C14 C15 1.393(5) . ?
C15 C16 1.378(5) . ?
C16 C17 1.405(4) . ?
