#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/25/4332530.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_4332530
loop_
_publ_author_name
'Ge, Chun-Hua'
'Cui, Ai-Li'
'Ni, Zhong-Hai'
'Jiang, Yun-Bo'
'Zhang, Li-Fang'
'Ribas, Joan'
'Kou, Hui-Zhong'
_publ_section_title
;
 μ1,1-Azide-Bridged Ferromagnetic MnIIIDimer with Slow Relaxation of
 Magnetization
;
_journal_issue                   13
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4883
_journal_page_last               4885
_journal_paper_doi               10.1021/ic060479h
_journal_volume                  45
_journal_year                    2006
_chemical_formula_moiety         'C14 H13 Mn N6 O3'
_chemical_formula_sum            'C28 H26 Mn2 N12 O6'
_chemical_formula_weight         736.46
_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                95.50(3)
_cell_angle_beta                 105.46(3)
_cell_angle_gamma                93.93(3)
_cell_formula_units_Z            1
_cell_length_a                   7.8721(16)
_cell_length_b                   10.017(2)
_cell_length_c                   10.443(2)
_cell_measurement_temperature    293(2)
_cell_volume                     786.2(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Rigaku IP'
_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    0.0354
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            2748
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.06
_exptl_absorpt_coefficient_mu    0.866
_exptl_crystal_colour            'red brown'
_exptl_crystal_density_diffrn    1.555
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             376
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.730
_refine_diff_density_min         -0.515
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     222
_refine_ls_number_reflns         2748
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0543
_refine_ls_R_factor_gt           0.0463
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0715P)²+0.4040P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1246
_refine_ls_wR_factor_ref         0.1294
_reflns_number_gt                2340
_reflns_number_total             2748
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic060479hsup1.cif
_cod_data_source_block           1
_cod_original_sg_symbol_Hall     -P1
_cod_original_sg_symbol_H-M      p-1
_cod_database_code               4332530
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 -0.06656(6) -0.02855(4) 0.13532(4) 0.0430(2) Uani 1 1 d .
O1 O 0.0421(3) -0.1851(2) 0.1707(2) 0.0513(5) Uani 1 1 d .
O2 O -0.1686(3) 0.1391(2) 0.1288(2) 0.0476(5) Uani 1 1 d .
N1 N 0.1612(3) 0.0790(2) 0.0590(3) 0.0450(6) Uani 1 1 d .
C13 C 0.1634(4) -0.2119(3) 0.2784(3) 0.0471(7) Uani 1 1 d .
N4 N 0.0497(3) 0.0586(2) 0.3198(3) 0.0441(6) Uani 1 1 d .
C2 C -0.1649(4) 0.3567(3) 0.2396(3) 0.0466(7) Uani 1 1 d .
N5 N 0.0047(4) 0.1890(3) 0.3484(3) 0.0477(6) Uani 1 1 d .
C1 C -0.1065(4) 0.2202(3) 0.2408(3) 0.0447(7) Uani 1 1 d .
C6 C -0.2278(6) 0.4064(3) 0.1185(4) 0.0655(10) Uani 1 1 d .
H4 H -0.2382 0.3531 0.0383 0.079 Uiso 1 1 calc R
C10 C 0.4311(6) -0.2776(4) 0.4931(5) 0.0766(12) Uani 1 1 d .
H7 H 0.5227 -0.2981 0.5631 0.092 Uiso 1 1 calc R
N6 N -0.2655(4) 0.6175(3) 0.2286(4) 0.0666(8) Uani 1 1 d .
C12 C 0.2302(5) -0.3376(3) 0.2745(4) 0.0551(8) Uani 1 1 d .
H9 H 0.1841 -0.4007 0.1996 0.066 Uiso 1 1 calc R
N2 N 0.2328(4) 0.1932(3) 0.1095(3) 0.0656(8) Uani 1 1 d .
C8 C 0.2273(4) -0.1204(3) 0.3952(3) 0.0498(7) Uani 1 1 d .
C3 C -0.1576(5) 0.4399(3) 0.3547(4) 0.0570(8) Uani 1 1 d .
H1 H -0.1189 0.4098 0.4382 0.068 Uiso 1 1 calc R
C4 C -0.2083(5) 0.5679(4) 0.3442(4) 0.0657(10) Uani 1 1 d .
H2 H -0.2021 0.6229 0.4225 0.079 Uiso 1 1 calc R
C7 C 0.1641(4) 0.0095(3) 0.4111(3) 0.0485(7) Uani 1 1 d .
H5 H 0.2091 0.0620 0.4933 0.058 Uiso 1 1 calc R
C5 C -0.2748(6) 0.5367(4) 0.1190(4) 0.0734(11) Uani 1 1 d .
H3 H -0.3155 0.5695 0.0371 0.088 Uiso 1 1 calc R
C9 C 0.3624(5) -0.1574(4) 0.5007(4) 0.0624(9) Uani 1 1 d .
H6 H 0.4059 -0.0973 0.5782 0.075 Uiso 1 1 calc R
C11 C 0.3622(5) -0.3699(4) 0.3787(4) 0.0667(10) Uani 1 1 d .
H8 H 0.4060 -0.4535 0.3732 0.080 Uiso 1 1 calc R
N3 N 0.2925(10) 0.2946(5) 0.1613(5) 0.157(3) Uani 1 1 d .
O3 O -0.2925(3) -0.1202(3) 0.1951(3) 0.0574(7) Uani 1 1 d .
C14 C -0.4703(5) -0.0933(4) 0.1561(4) 0.0697(11) Uani 1 1 d .
H12 H -0.4764 0.0020 0.1553 0.105 Uiso 1 1 calc R
H11 H -0.5299 -0.1248 0.2182 0.105 Uiso 1 1 calc R
H13 H -0.5263 -0.1387 0.0681 0.105 Uiso 1 1 calc R
H10 H -0.287(5) -0.186(4) 0.206(4) 0.059(13) Uiso 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'
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
O1 Mn1 O2 170.96(9) . .
O1 Mn1 N1 96.24(10) . 2
O2 Mn1 N1 92.73(10) . 2
O1 Mn1 N4 91.51(10) . .
O2 Mn1 N4 79.86(10) . .
N1 Mn1 N4 167.59(10) 2 .
O1 Mn1 O3 87.62(10) . .
O2 Mn1 O3 90.07(10) . .
N1 Mn1 O3 97.57(11) 2 .
N4 Mn1 O3 92.41(11) . .
O1 Mn1 N1 96.15(10) . .
O2 Mn1 N1 86.56(9) . .
N1 Mn1 N1 79.70(11) 2 .
N4 Mn1 N1 89.86(10) . .
O3 Mn1 N1 175.55(9) . .
C13 O1 Mn1 130.3(2) . .
C1 O2 Mn1 112.44(19) . .
N2 N1 Mn1 123.0(2) . 2
N2 N1 Mn1 121.4(2) . .
Mn1 N1 Mn1 100.30(11) 2 .
O1 C13 C12 118.0(3) . .
O1 C13 C8 123.3(3) . .
C12 C13 C8 118.7(3) . .
C7 N4 N5 118.3(3) . .
C7 N4 Mn1 126.7(2) . .
N5 N4 Mn1 114.93(19) . .
C3 C2 C6 117.6(3) . .
C3 C2 C1 123.1(3) . .
C6 C2 C1 119.3(3) . .
C1 N5 N4 107.9(2) . .
N5 C1 O2 124.7(3) . .
N5 C1 C2 119.4(3) . .
O2 C1 C2 115.9(3) . .
C5 C6 C2 118.7(3) . .
C5 C6 H4 120.7 . .
C2 C6 H4 120.7 . .
C9 C10 C11 119.0(4) . .
C9 C10 H7 120.5 . .
C11 C10 H7 120.5 . .
C5 N6 C4 116.8(3) . .
C11 C12 C13 121.4(3) . .
C11 C12 H9 119.3 . .
C13 C12 H9 119.3 . .
N3 N2 N1 175.6(4) . .
C13 C8 C9 118.3(3) . .
C13 C8 C7 123.1(3) . .
C9 C8 C7 118.6(3) . .
C4 C3 C2 119.0(3) . .
C4 C3 H1 120.5 . .
C2 C3 H1 120.5 . .
N6 C4 C3 123.8(3) . .
N6 C4 H2 118.1 . .
C3 C4 H2 118.1 . .
N4 C7 C8 124.7(3) . .
N4 C7 H5 117.6 . .
C8 C7 H5 117.6 . .
N6 C5 C6 124.1(4) . .
N6 C5 H3 118.0 . .
C6 C5 H3 118.0 . .
C10 C9 C8 122.3(4) . .
C10 C9 H6 118.8 . .
C8 C9 H6 118.8 . .
C12 C11 C10 120.2(3) . .
C12 C11 H8 119.9 . .
C10 C11 H8 119.9 . .
C14 O3 Mn1 128.4(2) . .
C14 O3 H10 110(3) . .
Mn1 O3 H10 114(3) . .
O3 C14 H12 109.5 . .
O3 C14 H11 109.5 . .
H12 C14 H11 109.5 . .
O3 C14 H13 109.5 . .
H12 C14 H13 109.5 . .
H11 C14 H13 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mn1 O1 1.859(2) .
Mn1 O2 1.909(2) .
Mn1 N1 1.968(3) 2
Mn1 N4 1.985(3) .
Mn1 O3 2.208(3) .
Mn1 N1 2.381(3) .
O1 C13 1.330(4) .
O2 C1 1.314(4) .
N1 N2 1.242(4) .
N1 Mn1 1.968(3) 2
C13 C12 1.399(4) .
C13 C8 1.406(5) .
N4 C7 1.286(4) .
N4 N5 1.402(3) .
C2 C3 1.381(4) .
C2 C6 1.383(5) .
C2 C1 1.473(4) .
N5 C1 1.306(4) .
C6 C5 1.380(5) .
C6 H4 0.9300 .
C10 C9 1.357(5) .
C10 C11 1.397(6) .
C10 H7 0.9300 .
N6 C5 1.319(5) .
N6 C4 1.328(5) .
C12 C11 1.371(5) .
C12 H9 0.9300 .
N2 N3 1.113(5) .
C8 C9 1.410(5) .
C8 C7 1.435(4) .
C3 C4 1.374(5) .
C3 H1 0.9300 .
C4 H2 0.9300 .
C7 H5 0.9300 .
C5 H3 0.9300 .
C9 H6 0.9300 .
C11 H8 0.9300 .
O3 C14 1.402(4) .
O3 H10 0.68(4) .
C14 H12 0.9600 .
C14 H11 0.9600 .
C14 H13 0.9600 .
