#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:33:12 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179334 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/31/4323153.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_4323153
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     Fe(salpn)N3
_chemical_formula_structural     '[Fe(salpn)N3]2'
_chemical_formula_sum            'C17 H16 Fe N5 O2'
_chemical_formula_weight         378.20
_chemical_name_systematic
; 

 azido-N,N'-bis(salicylidene)-1,3-diaminopropanatomanganese(III)

;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 105.19(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.199(7)
_cell_length_b                   14.081(6)
_cell_length_c                   12.017(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      14
_cell_measurement_theta_min      5
_cell_volume                     1665.5(14)
_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 CAD4'
_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  0.0452
_diffrn_reflns_av_sigmaI/netI    0.0452
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            2466
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.07
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  '60 min'
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.927
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.98
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.508
_exptl_crystal_description       needle
_exptl_crystal_F_000             780
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.739
_refine_diff_density_min         -0.434
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.132
_refine_ls_goodness_of_fit_obs   1.097
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     228
_refine_ls_number_reflns         2293
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.134
_refine_ls_restrained_S_obs      1.097
_refine_ls_R_factor_all          0.0824
_refine_ls_R_factor_obs          0.0525
_refine_ls_shift/esd_max         0.003
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0642P)²+2.3678P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1431
_refine_ls_wR_factor_obs         0.1156
_reflns_number_observed          1661
_reflns_number_total             2294
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic971592y_2.cif
_cod_data_source_block           kr137
_cod_depositor_comments
;
The following automatic conversions were performed:

'_geom_bond_publ_flag' value 'Y' changed to 'y' according to the
built-in table from CIF Core dictionary named 'cif_core.dic' version
2.4.1 from 2010-06-29 (9 times).

'_geom_angle_publ_flag' value 'Y'
changed to 'y' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (19
times).

Automatic conversion script
Id: cif_fix_values 1673 2011-04-08 12:14:43Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0642P)^2^+2.3678P] 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^)+(0.0642P)^2^+2.3678P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4323153
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
Fe1 Fe 0.16924(7) 0.02089(5) 0.02038(6) 0.0344(3) Uani 1 d . .
O1 O 0.1629(4) 0.1513(3) 0.0583(3) 0.0435(10) Uani 1 d . .
O2 O 0.3180(4) -0.0057(3) 0.1516(3) 0.0479(10) Uani 1 d . .
N1 N 0.2574(4) 0.0651(3) -0.1134(4) 0.0383(11) Uani 1 d . .
N2 N 0.2017(5) -0.1184(3) -0.0394(4) 0.0430(12) Uani 1 d . .
N3 N 0.0257(4) -0.0268(3) 0.1034(4) 0.0389(11) Uani 1 d . .
N4 N 0.0537(5) -0.0795(4) 0.1872(5) 0.0523(13) Uani 1 d . .
N5 N 0.0762(6) -0.1265(5) 0.2681(6) 0.077(2) Uani 1 d . .
C1 C 0.1694(5) 0.2310(4) 0.0045(4) 0.0368(13) Uani 1 d . .
C2 C 0.1275(6) 0.3163(4) 0.0431(5) 0.050(2) Uani 1 d . .
H2 H 0.0904(6) 0.3158(4) 0.1060(5) 0.064(6) Uiso 1 calc R .
C3 C 0.1398(7) 0.4005(4) -0.0094(6) 0.056(2) Uani 1 d . .
H3 H 0.1125(7) 0.4564(4) 0.0191(6) 0.064(6) Uiso 1 calc R .
C4 C 0.1922(7) 0.4040(4) -0.1044(6) 0.056(2) Uani 1 d . .
H4 H 0.2006(7) 0.4618(4) -0.1393(6) 0.064(6) Uiso 1 calc R .
C5 C 0.2311(6) 0.3224(4) -0.1458(5) 0.049(2) Uani 1 d . .
H5 H 0.2650(6) 0.3248(4) -0.2104(5) 0.064(6) Uiso 1 calc R .
C6 C 0.2216(5) 0.2352(4) -0.0945(4) 0.0373(13) Uani 1 d . .
C7 C 0.2657(5) 0.1515(4) -0.1435(4) 0.0392(14) Uani 1 d . .
H7 H 0.3048(5) 0.1615(4) -0.2043(4) 0.064(6) Uiso 1 calc R .
C8 C 0.2990(6) -0.0084(4) -0.1851(5) 0.051(2) Uani 1 d . .
H8A H 0.3711(6) -0.0467(4) -0.1374(5) 0.045(6) Uiso 1 calc R .
H8B H 0.3340(6) 0.0220(4) -0.2439(5) 0.045(6) Uiso 1 calc R .
C9 C 0.1813(6) -0.0710(4) -0.2415(5) 0.052(2) Uani 1 d . .
H9A H 0.2041(6) -0.1056(4) -0.3037(5) 0.045(6) Uiso 1 calc R .
H9B H 0.1036(6) -0.0311(4) -0.2755(5) 0.045(6) Uiso 1 calc R .
C10 C 0.1397(6) -0.1429(4) -0.1608(5) 0.050(2) Uani 1 d . .
H10A H 0.0416(6) -0.1433(4) -0.1752(5) 0.045(6) Uiso 1 calc R .
H10B H 0.1685(6) -0.2060(4) -0.1765(5) 0.045(6) Uiso 1 calc R .
C11 C 0.2754(6) -0.1822(4) 0.0224(6) 0.052(2) Uani 1 d . .
H11 H 0.2801(6) -0.2405(4) -0.0127(6) 0.064(6) Uiso 1 calc R .
C12 C 0.3525(6) -0.1730(5) 0.1419(5) 0.049(2) Uani 1 d . .
C13 C 0.4159(6) -0.2546(5) 0.1987(6) 0.064(2) Uani 1 d . .
H13 H 0.4075(6) -0.3118(5) 0.1588(6) 0.064(6) Uiso 1 calc R .
C14 C 0.4904(7) -0.2515(7) 0.3125(7) 0.076(2) Uani 1 d . .
H14 H 0.5330(7) -0.3058(7) 0.3490(7) 0.064(6) Uiso 1 calc R .
C15 C 0.5003(7) -0.1682(7) 0.3698(6) 0.071(2) Uani 1 d . .
H15 H 0.5474(7) -0.1665(7) 0.4474(6) 0.064(6) Uiso 1 calc R .
C16 C 0.4428(6) -0.0855(5) 0.3172(5) 0.058(2) Uani 1 d . .
H16 H 0.4538(6) -0.0290(5) 0.3588(5) 0.064(6) Uiso 1 calc R .
C17 C 0.3675(5) -0.0865(5) 0.2008(5) 0.046(2) 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'
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
_geom_angle_publ_flag
O1 Fe1 O2 93.5(2) . . y
O1 Fe1 N3 97.1(2) . . y
O2 Fe1 N3 92.7(2) . . y
O1 Fe1 N1 87.0(2) . . y
O2 Fe1 N1 106.1(2) . . y
N3 Fe1 N1 160.5(2) . . y
O1 Fe1 N2 169.7(2) . . y
O2 Fe1 N2 86.5(2) . . y
N3 Fe1 N2 93.2(2) . . y
N1 Fe1 N2 83.2(2) . . y
O1 Fe1 N3 92.6(2) . 3 y
O2 Fe1 N3 165.0(2) . 3 y
N3 Fe1 N3 72.9(2) . 3 y
N1 Fe1 N3 87.9(2) . 3 y
N2 Fe1 N3 90.0(2) . 3 y
C1 O1 Fe1 134.7(3) . . ?
C17 O2 Fe1 131.6(4) . . ?
C7 N1 C8 116.8(5) . . ?
C7 N1 Fe1 124.3(4) . . ?
C8 N1 Fe1 118.6(4) . . ?
C11 N2 C10 116.5(5) . . ?
C11 N2 Fe1 124.6(4) . . ?
C10 N2 Fe1 118.9(4) . . ?
N4 N3 Fe1 123.2(4) . . y
N4 N3 Fe1 124.6(4) . 3 y
Fe1 N3 Fe1 107.1(2) . 3 y
N5 N4 N3 176.8(6) . . y
O1 C1 C2 121.1(5) . . ?
O1 C1 C6 121.9(5) . . ?
C2 C1 C6 117.0(5) . . ?
C3 C2 C1 121.5(6) . . ?
C2 C3 C4 121.0(6) . . ?
C5 C4 C3 119.2(6) . . ?
C4 C5 C6 121.8(6) . . ?
C5 C6 C1 119.4(5) . . ?
C5 C6 C7 118.5(5) . . ?
C1 C6 C7 122.1(5) . . ?
N1 C7 C6 127.7(5) . . ?
N1 C8 C9 110.9(5) . . ?
C8 C9 C10 115.0(5) . . ?
N2 C10 C9 110.7(4) . . ?
N2 C11 C12 126.6(6) . . ?
C17 C12 C13 119.5(6) . . ?
C17 C12 C11 122.6(5) . . ?
C13 C12 C11 118.0(6) . . ?
C14 C13 C12 121.3(7) . . ?
C15 C14 C13 118.7(7) . . ?
C14 C15 C16 122.2(7) . . ?
C15 C16 C17 120.2(7) . . ?
O2 C17 C12 123.1(5) . . ?
O2 C17 C16 118.8(6) . . ?
C12 C17 C16 118.1(6) . . ?
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
Fe1 O1 1.897(4) . y
Fe1 O2 1.917(4) . y
Fe1 N3 2.087(4) . y
Fe1 N1 2.131(4) . y
Fe1 N2 2.144(5) . y
Fe1 N3 2.150(4) 3 y
O1 C1 1.305(6) . ?
O2 C17 1.319(7) . ?
N1 C7 1.278(7) . ?
N1 C8 1.477(7) . ?
N2 C11 1.277(7) . ?
N2 C10 1.471(7) . ?
N3 N4 1.223(7) . y
N3 Fe1 2.150(4) 3 y
N4 N5 1.148(7) . y
C1 C2 1.395(8) . ?
C1 C6 1.427(7) . ?
C2 C3 1.364(8) . ?
C3 C4 1.382(9) . ?
C4 C5 1.352(8) . ?
C5 C6 1.388(8) . ?
C6 C7 1.442(8) . ?
C8 C9 1.501(8) . ?
C9 C10 1.536(8) . ?
C11 C12 1.451(9) . ?
C12 C17 1.397(8) . ?
C12 C13 1.405(8) . ?
C13 C14 1.381(10) . ?
C14 C15 1.351(11) . ?
C15 C16 1.381(10) . ?
C16 C17 1.409(8) . ?
