#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:26:56 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179328 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/25/4322513.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_4322513
loop_
_publ_author_name
'Morsy A. M. Abu-Youssef'
'Albert Escuer'
'Dante Gatteschi'
'Mohamed A. S. Goher'
'Franz A. Mautner'
'Ramon Vicente'
_publ_section_title
;
 Synthesis, Structural Characterization, Magnetic Behavior, and Single
 Crystal EPR Spectra of Three New One-Dimensional Manganese Azido Systems
 with FM, Alternating FM-AF, and AF Coupling
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5716
_journal_page_last               5723
_journal_paper_doi               10.1021/ic990656x
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C14 H18 Mn N8'
_chemical_formula_weight         353.30
_chemical_name_common            '[Mn(3,5-dimethylpyridine)2(N3)2]n'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 101.69(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.552(6)
_cell_length_b                   7.730(3)
_cell_length_c                   16.554(6)
_cell_measurement_reflns_used    55
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      14.86
_cell_measurement_theta_min      7.54
_cell_volume                     1698.2(12)
_computing_molecular_graphics    'SHELXTL/PC v.5.03 (Siemens Ind. Aut.)'
_computing_publication_material  'SHELXTL/PC v.5.03 (Siemens Ind. Aut.)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measurement_device       'mod. STOE 4-circle diffractometer'
_diffrn_measurement_method       'Omega-scan, delta Omega: 1.20 deg.'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0320
_diffrn_reflns_av_sigmaI/netI    0.0727
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            4569
_diffrn_reflns_theta_max         27.99
_diffrn_reflns_theta_min         2.92
_diffrn_standards_decay_%        3
_diffrn_standards_interval_count 100
_diffrn_standards_interval_time  '1 h'
_diffrn_standards_number         '2 (-2 -1 2; 0 3 2)'
_exptl_absorpt_coefficient_mu    0.789
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.446
_exptl_absorpt_correction_type   DIFABS
_exptl_crystal_colour            'transparent light green'
_exptl_crystal_density_diffrn    1.382
_exptl_crystal_density_meas      1.39(2)
_exptl_crystal_density_method    'suspension method'
_exptl_crystal_description       prism
_exptl_crystal_F_000             732
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.299
_refine_diff_density_min         -0.440
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.077
_refine_ls_goodness_of_fit_obs   1.172
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     212
_refine_ls_number_reflns         3685
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_restrained_S_obs      1.172
_refine_ls_R_factor_all          0.0967
_refine_ls_R_factor_obs          0.0617
_refine_ls_shift/esd_max         0.067
_refine_ls_shift/esd_mean        0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0516P)²+0.2996P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1374
_refine_ls_wR_factor_obs         0.1225
_reflns_number_observed          2524
_reflns_number_total             3685
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic990656x_2.cif
_cod_data_source_block           mam12a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0516P)^2^+0.2996P] 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^)+(0.0516P)^2^+0.2996P] 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               4322513
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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 0.03662(4) 0.24918(8) 0.40757(3) 0.0300(2) Uani 1 d . .
N11 N 0.1070(2) 0.5099(4) 0.4274(2) 0.0405(8) Uani 1 d . .
N12 N 0.1032(2) 0.5931(4) 0.4861(2) 0.0325(7) Uani 1 d . .
N13 N 0.1017(2) 0.6787(5) 0.5441(2) 0.0469(9) Uani 1 d . .
N21 N -0.0275(2) -0.0115(4) 0.3742(2) 0.0425(8) Uani 1 d . .
N22 N -0.0645(2) -0.0954(4) 0.4186(2) 0.0303(7) Uani 1 d . .
N23 N -0.1034(2) -0.1821(5) 0.4607(2) 0.0472(9) Uani 1 d . .
N1 N -0.0408(2) 0.3421(4) 0.2818(2) 0.0337(7) Uani 1 d . .
C1 C -0.0827(3) 0.4993(5) 0.2756(2) 0.0373(9) Uani 1 d . .
H1 H -0.0685(3) 0.5718(5) 0.3213(2) 0.045 Uiso 1 calc R .
C2 C -0.1463(3) 0.5605(5) 0.2048(2) 0.0363(9) Uani 1 d . .
C3 C -0.1653(3) 0.4509(5) 0.1379(2) 0.0408(9) Uani 1 d . .
H3 H -0.2076(3) 0.4874(5) 0.0895(2) 0.049 Uiso 1 calc R .
C4 C -0.1231(3) 0.2875(5) 0.1412(2) 0.0387(9) Uani 1 d . .
C5 C -0.0613(3) 0.2389(6) 0.2156(2) 0.0370(8) Uani 1 d . .
H5 H -0.0329(3) 0.1290(6) 0.2195(2) 0.044 Uiso 1 calc R .
C6 C -0.1922(3) 0.7372(6) 0.2041(3) 0.0566(11) Uani 1 d . .
H6A H -0.1445(8) 0.8225(7) 0.1943(18) 0.074 Uiso 1 calc R .
H6B H -0.2101(19) 0.7591(15) 0.2564(7) 0.074 Uiso 1 calc R .
H6C H -0.2515(12) 0.7432(13) 0.1611(12) 0.074 Uiso 1 calc R .
C7 C -0.1444(4) 0.1639(7) 0.0700(3) 0.0591(12) Uani 1 d . .
H7A H -0.1005(15) 0.0656(18) 0.0817(8) 0.077 Uiso 1 calc R .
H7B H -0.1331(20) 0.2206(13) 0.0211(4) 0.077 Uiso 1 calc R .
H7C H -0.2132(7) 0.1263(29) 0.0617(11) 0.077 Uiso 1 calc R .
N2 N 0.1817(2) 0.1483(4) 0.3763(2) 0.0349(7) Uani 1 d . .
C8 C 0.2408(3) 0.2448(6) 0.3389(2) 0.0406(8) Uani 1 d . .
H8 H 0.2170(3) 0.3524(6) 0.3187(2) 0.049 Uiso 1 calc R .
C9 C 0.3352(3) 0.1941(6) 0.3286(3) 0.0482(11) Uani 1 d . .
C10 C 0.3687(3) 0.0342(6) 0.3595(3) 0.0508(11) Uani 1 d . .
H10 H 0.4322(3) -0.0036(6) 0.3542(3) 0.061 Uiso 1 calc R .
C11 C 0.3101(3) -0.0715(6) 0.3983(3) 0.0475(10) Uani 1 d . .
C12 C 0.2168(3) -0.0066(5) 0.4050(2) 0.0402(9) Uani 1 d . .
H12 H 0.1760(3) -0.0748(5) 0.4310(2) 0.048 Uiso 1 calc R .
C13 C 0.3989(4) 0.3109(8) 0.2864(4) 0.080(2) Uani 1 d . .
H13A H 0.3668(15) 0.4217(17) 0.2762(21) 0.104 Uiso 1 calc R .
H13B H 0.4060(23) 0.2600(24) 0.2350(11) 0.104 Uiso 1 calc R .
H13C H 0.4642(10) 0.3252(40) 0.3213(10) 0.104 Uiso 1 calc R .
C14 C 0.3440(4) -0.2452(7) 0.4337(4) 0.085(2) Uani 1 d . .
H14A H 0.2914(11) -0.2966(22) 0.4567(21) 0.110 Uiso 1 calc R .
H14B H 0.4033(17) -0.2318(8) 0.4761(15) 0.110 Uiso 1 calc R .
H14C H 0.3589(26) -0.3184(16) 0.3908(6) 0.110 Uiso 1 calc R .
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'
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
N21 Mn1 N11 173.41(12) . . yes
N21 Mn1 N23 95.33(13) . 3_556 yes
N11 Mn1 N23 89.40(13) . 3_556 yes
N21 Mn1 N1 88.50(12) . . yes
N11 Mn1 N1 87.29(12) . . yes
N23 Mn1 N1 172.99(12) 3_556 . yes
N21 Mn1 N13 90.06(13) . 3_566 yes
N11 Mn1 N13 94.94(13) . 3_566 yes
N23 Mn1 N13 85.04(13) 3_556 3_566 yes
N1 Mn1 N13 89.09(12) . 3_566 yes
N21 Mn1 N2 86.85(12) . . yes
N11 Mn1 N2 88.83(12) . . yes
N23 Mn1 N2 86.82(12) 3_556 . yes
N1 Mn1 N2 99.29(11) . . yes
N13 Mn1 N2 170.99(12) 3_566 . yes
N12 N11 Mn1 121.9(3) . . yes
N13 N12 N11 178.1(4) . . yes
N12 N13 Mn1 125.8(3) . 3_566 yes
N22 N21 Mn1 122.9(3) . . yes
N21 N22 N23 177.7(4) . . yes
N22 N23 Mn1 124.8(3) . 3_556 yes
C1 N1 C5 117.7(3) . . ?
C1 N1 Mn1 118.2(2) . . ?
C5 N1 Mn1 123.2(3) . . ?
N1 C1 C2 123.8(4) . . ?
N1 C1 H1 118.1(2) . . ?
C2 C1 H1 118.1(2) . . ?
C3 C2 C1 116.8(4) . . ?
C3 C2 C6 123.0(4) . . ?
C1 C2 C6 120.2(4) . . ?
C2 C3 C4 121.5(3) . . ?
C2 C3 H3 119.3(2) . . ?
C4 C3 H3 119.3(2) . . ?
C3 C4 C5 116.8(4) . . ?
C3 C4 C7 122.6(4) . . ?
C5 C4 C7 120.6(4) . . ?
N1 C5 C4 123.5(4) . . ?
N1 C5 H5 118.3(2) . . ?
C4 C5 H5 118.3(2) . . ?
C2 C6 H6A 109.5(2) . . ?
C2 C6 H6B 109.5(2) . . ?
H6A C6 H6B 109.5 . . ?
C2 C6 H6C 109.5(2) . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C4 C7 H7A 109.5(2) . . ?
C4 C7 H7B 109.5(2) . . ?
H7A C7 H7B 109.5 . . ?
C4 C7 H7C 109.5(2) . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C8 N2 C12 117.5(3) . . ?
C8 N2 Mn1 122.8(3) . . ?
C12 N2 Mn1 119.2(2) . . ?
N2 C8 C9 123.8(4) . . ?
N2 C8 H8 118.1(2) . . ?
C9 C8 H8 118.1(3) . . ?
C10 C9 C8 116.8(4) . . ?
C10 C9 C13 122.0(4) . . ?
C8 C9 C13 121.1(4) . . ?
C9 C10 C11 121.6(4) . . ?
C9 C10 H10 119.2(2) . . ?
C11 C10 H10 119.2(2) . . ?
C10 C11 C12 116.2(4) . . ?
C10 C11 C14 123.4(4) . . ?
C12 C11 C14 120.3(4) . . ?
N2 C12 C11 124.0(4) . . ?
N2 C12 H12 118.0(2) . . ?
C11 C12 H12 118.0(2) . . ?
C9 C13 H13A 109.5(3) . . ?
C9 C13 H13B 109.5(3) . . ?
H13A C13 H13B 109.5 . . ?
C9 C13 H13C 109.5(3) . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C11 C14 H14A 109.5(3) . . ?
C11 C14 H14B 109.5(3) . . ?
H14A C14 H14B 109.5 . . ?
C11 C14 H14C 109.5(3) . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
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 N21 2.220(3) . yes
Mn1 N11 2.225(3) . yes
Mn1 N23 2.245(3) 3_556 yes
Mn1 N1 2.251(3) . yes
Mn1 N13 2.252(3) 3_566 yes
Mn1 N2 2.271(3) . yes
N11 N12 1.175(4) . yes
N12 N13 1.170(4) . yes
N13 Mn1 2.252(3) 3_566 yes
N21 N22 1.167(4) . yes
N22 N23 1.168(4) . yes
N23 Mn1 2.245(3) 3_556 yes
N1 C1 1.336(5) . ?
N1 C5 1.338(5) . ?
C1 C2 1.390(5) . ?
C1 H1 0.93 . ?
C2 C3 1.377(5) . ?
C2 C6 1.500(5) . ?
C3 C4 1.383(5) . ?
C3 H3 0.93 . ?
C4 C5 1.393(5) . ?
C4 C7 1.499(6) . ?
C5 H5 0.93 . ?
C6 H6A 0.96 . ?
C6 H6B 0.96 . ?
C6 H6C 0.96 . ?
C7 H7A 0.96 . ?
C7 H7B 0.96 . ?
C7 H7C 0.96 . ?
N2 C8 1.334(5) . ?
N2 C12 1.339(5) . ?
C8 C9 1.382(5) . ?
C8 H8 0.93 . ?
C9 C10 1.379(6) . ?
C9 C13 1.514(6) . ?
C10 C11 1.384(6) . ?
C10 H10 0.93 . ?
C11 C12 1.386(5) . ?
C11 C14 1.499(6) . ?
C12 H12 0.93 . ?
C13 H13A 0.96 . ?
C13 H13B 0.96 . ?
C13 H13C 0.96 . ?
C14 H14A 0.96 . ?
C14 H14B 0.96 . ?
C14 H14C 0.96 . ?
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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N21 Mn1 N11 N12 178.6(9) . . . . ?
N23 Mn1 N11 N12 -45.5(3) 3_556 . . . ?
N1 Mn1 N11 N12 128.3(3) . . . . ?
N13 Mn1 N11 N12 39.4(3) 3_566 . . . ?
N2 Mn1 N11 N12 -132.4(3) . . . . ?
Mn1 N11 N12 N13 160.9(115) . . . . ?
N11 N12 N13 Mn1 147.1(115) . . . 3_566 ?
N11 Mn1 N21 N22 174.5(9) . . . . ?
N23 Mn1 N21 N22 38.9(3) 3_556 . . . ?
N1 Mn1 N21 N22 -135.3(3) . . . . ?
N13 Mn1 N21 N22 -46.2(3) 3_566 . . . ?
N2 Mn1 N21 N22 125.4(3) . . . . ?
Mn1 N21 N22 N23 153.7(89) . . . . ?
N21 N22 N23 Mn1 155.7(88) . . . 3_556 ?
N21 Mn1 N1 C1 140.5(3) . . . . ?
N11 Mn1 N1 C1 -44.6(3) . . . . ?
N23 Mn1 N1 C1 17.3(11) 3_556 . . . ?
N13 Mn1 N1 C1 50.4(3) 3_566 . . . ?
N2 Mn1 N1 C1 -133.0(3) . . . . ?
N21 Mn1 N1 C5 -28.2(3) . . . . ?
N11 Mn1 N1 C5 146.7(3) . . . . ?
N23 Mn1 N1 C5 -151.4(9) 3_556 . . . ?
N13 Mn1 N1 C5 -118.3(3) 3_566 . . . ?
N2 Mn1 N1 C5 58.3(3) . . . . ?
C5 N1 C1 C2 0.3(5) . . . . ?
Mn1 N1 C1 C2 -169.1(3) . . . . ?
N1 C1 C2 C3 -0.5(6) . . . . ?
N1 C1 C2 C6 178.4(3) . . . . ?
C1 C2 C3 C4 0.0(6) . . . . ?
C6 C2 C3 C4 -178.8(4) . . . . ?
C2 C3 C4 C5 0.7(6) . . . . ?
C2 C3 C4 C7 178.5(4) . . . . ?
C1 N1 C5 C4 0.5(5) . . . . ?
Mn1 N1 C5 C4 169.2(3) . . . . ?
C3 C4 C5 N1 -1.0(6) . . . . ?
C7 C4 C5 N1 -178.8(4) . . . . ?
N21 Mn1 N2 C8 142.2(3) . . . . ?
N11 Mn1 N2 C8 -32.8(3) . . . . ?
N23 Mn1 N2 C8 -122.2(3) 3_556 . . . ?
N1 Mn1 N2 C8 54.3(3) . . . . ?
N13 Mn1 N2 C8 -147.7(7) 3_566 . . . ?
N21 Mn1 N2 C12 -46.2(3) . . . . ?
N11 Mn1 N2 C12 138.8(3) . . . . ?
N23 Mn1 N2 C12 49.3(3) 3_556 . . . ?
N1 Mn1 N2 C12 -134.1(3) . . . . ?
N13 Mn1 N2 C12 23.9(9) 3_566 . . . ?
C12 N2 C8 C9 -0.2(6) . . . . ?
Mn1 N2 C8 C9 171.6(3) . . . . ?
N2 C8 C9 C10 -0.2(6) . . . . ?
N2 C8 C9 C13 -179.3(4) . . . . ?
C8 C9 C10 C11 0.7(7) . . . . ?
C13 C9 C10 C11 179.7(5) . . . . ?
C9 C10 C11 C12 -0.7(7) . . . . ?
C9 C10 C11 C14 -179.3(5) . . . . ?
C8 N2 C12 C11 0.2(6) . . . . ?
Mn1 N2 C12 C11 -171.9(3) . . . . ?
C10 C11 C12 N2 0.3(6) . . . . ?
C14 C11 C12 N2 178.9(4) . . . . ?
