#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:33:12 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179334 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/31/4323152.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_4323152
loop_
_publ_author_name
'K. Rajender Reddy'
'M. V. Rajasekharan'
'J.-P. Tuchagues'
_publ_section_title
;
 Synthesis, Structure, and Magnetic Properties of Mn(salpn)N3, a Helical
 Polymer, and Fe(salpn)N3, a Ferromagnetically Coupled Dimer (salpnH2 =
 N,N'-bis(Salicylidene)-1,3-diaminopropane)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5978
_journal_page_last               5982
_journal_paper_doi               10.1021/ic971592y
_journal_volume                  37
_journal_year                    1998
_chemical_formula_analytical     Mn(salpn)N3
_chemical_formula_structural     '[Mn(salpn)N3]n'
_chemical_formula_sum            'C17 H16 Mn N5 O2'
_chemical_formula_weight         377.29
_chemical_name_systematic
; 

 Azido-N,N'-bis(salicylidene-1,3-diaminopropanato)manganese(III)  

;
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.947(2)
_cell_length_b                   11.818(2)
_cell_length_c                   11.227(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      14
_cell_measurement_theta_min      5
_cell_volume                     1585.1(8)
_computing_cell_refinement       'CAD-4 system'
_computing_data_collection       'CAD-4 system'
_computing_data_reduction        'CAD-4 system'
_computing_molecular_graphics    ORTEP
_computing_publication_material  SHELXL-93
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Enraf Nonius CAD-4'
_diffrn_measurement_method       omega-2theta
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0222
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1472
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         2.42
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  '60 min'
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.855
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.96
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.581
_exptl_crystal_description       needle
_exptl_crystal_F_000             776
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.125
_refine_diff_density_max         0.225
_refine_diff_density_min         -0.284
_refine_diff_density_rms         0.049
_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   1.093
_refine_ls_goodness_of_fit_obs   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     227
_refine_ls_number_reflns         1472
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.093
_refine_ls_restrained_S_obs      1.055
_refine_ls_R_factor_all          0.0344
_refine_ls_R_factor_obs          0.0260
_refine_ls_shift/esd_max         -0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0386P)²+0.3856P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0686
_refine_ls_wR_factor_obs         0.0617
_reflns_number_observed          1307
_reflns_number_total             1472
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic971592y_1.cif
_cod_data_source_block           mnsbaz
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0386P)^2^+0.3856P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0386P)^2^+0.3856P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1585.2(8)
_cod_database_code               4323152
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 0.02487(4) 0.09830(4) -0.00027(6) 0.02646(15) Uani 1 d . .
O1 O 0.1451(2) -0.0028(2) -0.0147(4) 0.0401(7) Uani 1 d . .
O2 O 0.1191(2) 0.2047(2) -0.0741(3) 0.0362(6) Uani 1 d . .
N1 N -0.0751(2) -0.0254(3) 0.0723(3) 0.0283(7) Uani 1 d . .
N2 N -0.0914(2) 0.2207(2) 0.0179(3) 0.0286(7) Uani 1 d . .
N3 N -0.0595(3) 0.0431(3) -0.1782(3) 0.0408(8) Uani 1 d . .
N4 N -0.0654(3) -0.0380(3) -0.2368(3) 0.0334(8) Uani 1 d . .
N5 N 0.0724(3) 0.1196(3) 0.2014(3) 0.0449(9) Uani 1 d . .
C1 C 0.1407(3) -0.1140(3) -0.0279(3) 0.0345(9) Uani 1 d . .
C2 C 0.2336(4) -0.1701(4) -0.0760(4) 0.0448(10) Uani 1 d . .
H2 H 0.2965(4) -0.1288(4) -0.0981(4) 0.053(4) Uiso 1 calc R .
C3 C 0.2328(4) -0.2854(4) -0.0910(4) 0.0577(14) Uani 1 d . .
H3 H 0.2946(4) -0.3213(4) -0.1244(4) 0.053(4) Uiso 1 calc R .
C4 C 0.1409(5) -0.3485(4) -0.0571(5) 0.0614(14) Uani 1 d . .
H4 H 0.1408(5) -0.4265(4) -0.0680(5) 0.053(4) Uiso 1 calc R .
C5 C 0.0509(4) -0.2968(3) -0.0079(7) 0.0531(12) Uani 1 d . .
H5 H -0.0100(4) -0.3399(3) 0.0165(7) 0.053(4) Uiso 1 calc R .
C6 C 0.0487(3) -0.1779(3) 0.0067(5) 0.0374(8) Uani 1 d . .
C7 C -0.0485(3) -0.1315(4) 0.0642(4) 0.0360(9) Uani 1 d . .
H7 H -0.0974(3) -0.1829(4) 0.0992(4) 0.053(4) Uiso 1 calc R .
C8 C -0.1743(3) -0.0006(4) 0.1459(4) 0.0354(9) Uani 1 d . .
H8A H -0.1504(3) 0.0129(4) 0.2273(4) 0.053(4) Uiso 1 calc R .
H8B H -0.2229(3) -0.0663(4) 0.1462(4) 0.053(4) Uiso 1 calc R .
C9 C -0.2398(3) 0.1004(4) 0.1031(4) 0.0396(9) Uani 1 d . .
H9A H -0.3082(3) 0.1059(4) 0.1493(4) 0.053(4) Uiso 1 calc R .
H9B H -0.2607(3) 0.0881(4) 0.0206(4) 0.053(4) Uiso 1 calc R .
C10 C -0.1776(3) 0.2114(3) 0.1120(4) 0.0367(9) Uani 1 d . .
H10A H -0.2302(3) 0.2735(3) 0.1045(4) 0.053(4) Uiso 1 calc R .
H10B H -0.1422(3) 0.2170(3) 0.1895(4) 0.053(4) Uiso 1 calc R .
C11 C -0.0975(3) 0.3080(3) -0.0509(3) 0.0316(8) Uani 1 d . .
H11 H -0.1610(3) 0.3530(3) -0.0442(3) 0.053(4) Uiso 1 calc R .
C12 C -0.0151(3) 0.3418(3) -0.1369(4) 0.0321(8) Uani 1 d . .
C13 C -0.0387(4) 0.4353(4) -0.2098(4) 0.0420(10) Uani 1 d . .
H13 H -0.1098(4) 0.4672(4) -0.2074(4) 0.053(4) Uiso 1 calc R .
C14 C 0.0402(4) 0.4806(4) -0.2843(4) 0.0489(11) Uani 1 d . .
H14 H 0.0231(4) 0.5424(4) -0.3322(4) 0.053(4) Uiso 1 calc R .
C15 C 0.1465(4) 0.4325(4) -0.2870(4) 0.0445(10) Uani 1 d . .
H15 H 0.2012(4) 0.4634(4) -0.3361(4) 0.053(4) Uiso 1 calc R .
C16 C 0.1717(3) 0.3396(3) -0.2179(4) 0.0372(9) Uani 1 d . .
H16 H 0.2430(3) 0.3082(3) -0.2218(4) 0.053(4) Uiso 1 calc R .
C17 C 0.0914(3) 0.2914(3) -0.1412(3) 0.0308(8) 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'
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 85.94(12) . . y
O1 Mn1 N2 173.55(11) . . y
O2 Mn1 N2 88.70(11) . . y
O1 Mn1 N1 91.51(12) . . y
O2 Mn1 N1 176.34(13) . . y
N2 Mn1 N1 94.01(12) . . y
O1 Mn1 N3 94.53(15) . . y
O2 Mn1 N3 93.91(14) . . y
N2 Mn1 N3 89.41(13) . . y
N1 Mn1 N3 83.66(12) . . y
O1 Mn1 N5 88.1(2) . . y
O2 Mn1 N5 102.06(14) . . y
N2 Mn1 N5 89.56(14) . . y
N1 Mn1 N5 80.46(13) . . y
N3 Mn1 N5 163.97(13) . . y
C1 O1 Mn1 127.7(2) . . ?
C17 O2 Mn1 128.5(2) . . ?
C7 N1 C8 115.4(3) . . ?
C7 N1 Mn1 121.2(3) . . ?
C8 N1 Mn1 123.2(2) . . ?
C11 N2 C10 116.6(3) . . ?
C11 N2 Mn1 123.5(2) . . ?
C10 N2 Mn1 119.9(2) . . ?
N4 N3 Mn1 137.8(3) . . y
N3 N4 N5 178.7(4) . 2_554 y
N4 N5 Mn1 117.3(3) 2 . y
O1 C1 C6 122.7(3) . . ?
O1 C1 C2 118.7(4) . . ?
C6 C1 C2 118.5(4) . . ?
C3 C2 C1 120.7(5) . . ?
C2 C3 C4 120.6(5) . . ?
C5 C4 C3 120.0(4) . . ?
C4 C5 C6 120.7(5) . . ?
C1 C6 C5 119.5(4) . . ?
C1 C6 C7 123.9(3) . . ?
C5 C6 C7 116.5(4) . . ?
N1 C7 C6 126.7(4) . . ?
N1 C8 C9 113.3(3) . . ?
C8 C9 C10 114.3(3) . . ?
N2 C10 C9 111.0(3) . . ?
N2 C11 C12 125.9(3) . . ?
C13 C12 C17 119.7(4) . . ?
C13 C12 C11 118.2(4) . . ?
C17 C12 C11 121.7(4) . . ?
C14 C13 C12 121.7(4) . . ?
C13 C14 C15 118.8(4) . . ?
C16 C15 C14 120.9(4) . . ?
C15 C16 C17 121.1(4) . . ?
O2 C17 C12 122.6(3) . . ?
O2 C17 C16 119.6(3) . . ?
C12 C17 C16 117.8(4) . . ?
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 1.875(2) . y
Mn1 O2 1.881(3) . y
Mn1 N2 2.016(3) . y
Mn1 N1 2.056(3) . y
Mn1 N3 2.331(4) . y
Mn1 N5 2.348(4) . y
O1 C1 1.324(4) . ?
O2 C17 1.313(4) . ?
N1 C7 1.297(5) . ?
N1 C8 1.474(5) . ?
N2 C11 1.291(5) . ?
N2 C10 1.479(5) . ?
N3 N4 1.165(5) . y
N4 N5 1.190(5) 2_554 y
N5 N4 1.190(5) 2 y
C1 C6 1.388(5) . ?
C1 C2 1.402(6) . ?
C2 C3 1.373(6) . ?
C3 C4 1.380(8) . ?
C4 C5 1.354(7) . ?
C5 C6 1.415(5) . ?
C6 C7 1.438(5) . ?
C8 C9 1.506(6) . ?
C9 C10 1.512(6) . ?
C11 C12 1.435(6) . ?
C12 C13 1.404(6) . ?
C12 C17 1.406(5) . ?
C13 C14 1.369(6) . ?
C14 C15 1.392(6) . ?
C15 C16 1.378(6) . ?
C16 C17 1.409(5) . ?
