#------------------------------------------------------------------------------
#$Date: 2016-03-24 02:18:16 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179571 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/36/4503612.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_4503612
loop_
_publ_author_name
'Yue, Yan-Feng'
'Gao, En-Qing'
'Fang, Chen-Jie'
'Zheng, Tao'
'Liang, Jue'
'Yan, Chun-Hua'
_publ_section_title
;
 Three Azido-Bridged Mn(II) Complexes Based on Open-Chain Diazine
 Schiff-base Ligands: Crystal Structures and Magnetic Properties
;
_journal_issue                   9
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              3295
_journal_paper_doi               10.1021/cg800138x
_journal_volume                  8
_journal_year                    2008
_chemical_formula_sum            'C13 H14 Br Mn N11 O'
_chemical_formula_weight         475.20
_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                106.9842(12)
_cell_angle_beta                 93.0774(12)
_cell_angle_gamma                109.8723(12)
_cell_formula_units_Z            2
_cell_length_a                   7.4368(2)
_cell_length_b                   10.5408(3)
_cell_length_c                   13.3439(3)
_cell_measurement_reflns_used    8037
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.022
_cell_measurement_theta_min      3.395
_cell_volume                     927.12(4)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'KappaCCD (Nonius B. V., 1998)'
_computing_data_reduction
'HKL Denzo (Otwinowski & Minor, 1997) & maXus (Mackay et al., 1998)'
_computing_molecular_graphics    'Bruker SHELXTL V5.1 (Sheldrick, 1998)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 0.76
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'NONIUS KappaCCD Diffractometer'
_diffrn_measurement_method       CCD
_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  0.0705
_diffrn_reflns_av_sigmaI/netI    0.0699
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            16225
_diffrn_reflns_theta_full        26.02
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         3.47
_exptl_absorpt_coefficient_mu    2.896
_exptl_absorpt_correction_T_max  0.759
_exptl_absorpt_correction_T_min  0.568
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(Blessing, 1995, 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.702
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             474
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.826
_refine_diff_density_min         -0.958
_refine_diff_density_rms         0.075
_refine_ls_extinction_coef       0.014(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.980
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         3634
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.983
_refine_ls_R_factor_all          0.0929
_refine_ls_R_factor_gt           0.0486
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0737P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1190
_refine_ls_wR_factor_ref         0.1320
_reflns_number_gt                2210
_reflns_number_total             3634
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg800138x-file001.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4503612
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 0.23212(8) 0.12303(5) 0.51912(5) 0.0389(2) Uani 1 1 d .
C1 C 0.0314(6) 0.1715(5) 0.3222(4) 0.0547(11) Uani 1 1 d .
H1A H -0.011(5) 0.063(4) 0.296(3) 0.032(9) Uiso 1 1 d .
C2 C -0.0155(7) 0.2460(5) 0.2629(4) 0.0634(12) Uani 1 1 d .
H2A H -0.0902 0.1974 0.1954 0.076 Uiso 1 1 calc R
C3 C 0.0465(7) 0.3892(6) 0.3025(4) 0.0632(13) Uani 1 1 d .
H3A H 0.031(6) 0.448(5) 0.274(4) 0.067(15) Uiso 1 1 d .
C4 C 0.1545(7) 0.4588(5) 0.4028(4) 0.0517(12) Uani 1 1 d .
H4A H 0.190(5) 0.540(4) 0.427(3) 0.028(10) Uiso 1 1 d .
C5 C 0.1987(5) 0.3807(4) 0.4605(3) 0.0399(9) Uani 1 1 d .
C6 C 0.3144(5) 0.4451(4) 0.5693(3) 0.0399(9) Uani 1 1 d .
C7 C 0.5091(6) 0.3592(5) 0.7636(3) 0.0486(10) Uani 1 1 d .
H7A H 0.466(6) 0.256(5) 0.734(3) 0.060(12) Uiso 1 1 d .
C8 C 0.6229(6) 0.4218(4) 0.8704(3) 0.0483(10) Uani 1 1 d .
C9 C 0.6577(7) 0.3322(6) 0.9210(4) 0.0608(12) Uani 1 1 d .
H9A H 0.607(8) 0.241(6) 0.872(4) 0.096(19) Uiso 1 1 d .
C10 C 0.7561(7) 0.3882(6) 1.0225(4) 0.0707(14) Uani 1 1 d .
H10A H 0.7793 0.3288 1.0569 0.085 Uiso 1 1 calc R
C11 C 0.8200(7) 0.5313(7) 1.0730(5) 0.0737(17) Uani 1 1 d .
H11A H 0.877(8) 0.559(6) 1.130(4) 0.08(2) Uiso 1 1 d .
C12 C 0.7846(6) 0.6126(5) 1.0161(4) 0.0675(14) Uani 1 1 d .
C13 C 0.6226(11) 0.9031(6) 0.8677(6) 0.122(2) Uani 1 1 d D
H1 H 0.625(7) 0.720(3) 0.853(8) 0.23(5) Uiso 1 1 d D
H5A H 0.369(6) 0.649(5) 0.580(3) 0.065(14) Uiso 1 1 d .
H5B H 0.420(6) 0.611(5) 0.676(4) 0.049(15) Uiso 1 1 d .
N1 N 0.1374(4) 0.2368(3) 0.4197(2) 0.0424(8) Uani 1 1 d .
N2 N 0.3485(4) 0.3579(3) 0.6141(3) 0.0409(8) Uani 1 1 d .
N3 N 0.4582(4) 0.4340(3) 0.7164(3) 0.0445(8) Uani 1 1 d .
N4 N 0.6872(5) 0.5638(4) 0.9191(3) 0.0561(9) Uani 1 1 d .
N5 N 0.3742(6) 0.5850(4) 0.6151(4) 0.0536(10) Uani 1 1 d .
N6 N 0.0364(5) -0.0866(3) 0.4050(3) 0.0451(8) Uani 1 1 d .
N7 N 0.0842(4) -0.1825(4) 0.3598(3) 0.0443(8) Uani 1 1 d .
N8 N 0.1269(6) -0.2757(4) 0.3152(3) 0.0767(13) Uani 1 1 d .
N9 N 0.3505(5) 0.0198(4) 0.6145(3) 0.0556(9) Uani 1 1 d .
N10 N 0.4315(4) -0.0594(3) 0.5888(2) 0.0417(8) Uani 1 1 d .
N11 N 0.5116(5) -0.1401(4) 0.5664(3) 0.0605(10) Uani 1 1 d .
O1 O 0.5375(8) 0.7539(4) 0.8327(4) 0.1136(15) Uani 1 1 d D
Br1 Br 0.88103(9) 0.81421(7) 1.08202(5) 0.1092(3) Uani 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'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 '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'
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
N9 Mn1 N6 92.12(13) . .
N9 Mn1 N2 106.00(13) . .
N6 Mn1 N2 159.85(12) . .
N9 Mn1 N6 91.40(13) . 2_556
N6 Mn1 N6 79.40(12) . 2_556
N2 Mn1 N6 91.18(11) . 2_556
N9 Mn1 N11 87.97(14) . 2_656
N6 Mn1 N11 95.75(13) . 2_656
N2 Mn1 N11 93.68(12) . 2_656
N6 Mn1 N11 175.09(12) 2_556 2_656
N9 Mn1 N1 175.16(12) . .
N6 Mn1 N1 90.27(12) . .
N2 Mn1 N1 72.35(11) . .
N6 Mn1 N1 93.17(12) 2_556 .
N11 Mn1 N1 87.60(12) 2_656 .
N1 C1 C2 122.1(4) . .
C3 C2 C1 119.9(5) . .
C2 C3 C4 119.2(5) . .
C3 C4 C5 119.5(5) . .
N1 C5 C4 121.0(4) . .
N1 C5 C6 115.1(3) . .
C4 C5 C6 123.9(4) . .
N2 C6 N5 124.4(4) . .
N2 C6 C5 117.3(3) . .
N5 C6 C5 118.3(4) . .
N3 C7 C8 122.1(4) . .
N4 C8 C9 121.4(4) . .
N4 C8 C7 119.6(4) . .
C9 C8 C7 119.0(4) . .
C10 C9 C8 119.8(5) . .
C11 C10 C9 119.4(5) . .
C10 C11 C12 117.0(5) . .
N4 C12 C11 126.0(5) . .
N4 C12 Br1 115.7(4) . .
C11 C12 Br1 118.3(4) . .
C1 N1 C5 118.3(4) . .
C1 N1 Mn1 124.2(3) . .
C5 N1 Mn1 117.4(3) . .
C6 N2 N3 110.7(3) . .
C6 N2 Mn1 117.7(3) . .
N3 N2 Mn1 131.5(2) . .
C7 N3 N2 115.2(3) . .
C12 N4 C8 116.4(4) . .
N7 N6 Mn1 125.7(3) . .
N7 N6 Mn1 122.0(2) . 2_556
Mn1 N6 Mn1 100.60(12) . 2_556
N8 N7 N6 178.8(4) . .
N10 N9 Mn1 129.5(3) . .
N9 N10 N11 177.6(4) . .
N10 N11 Mn1 128.2(3) . 2_656
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mn1 N9 2.217(4) .
Mn1 N6 2.220(3) .
Mn1 N2 2.253(3) .
Mn1 N6 2.255(3) 2_556
Mn1 N11 2.255(3) 2_656
Mn1 N1 2.257(3) .
C1 N1 1.337(5) .
C1 C2 1.373(6) .
C2 C3 1.343(7) .
C3 C4 1.372(7) .
C4 C5 1.380(6) .
C5 N1 1.352(5) .
C5 C6 1.483(6) .
C6 N2 1.316(5) .
C6 N5 1.321(5) .
C7 N3 1.276(5) .
C7 C8 1.457(6) .
C8 N4 1.343(5) .
C8 C9 1.391(6) .
C9 C10 1.361(7) .
C10 C11 1.356(8) .
C11 C12 1.376(8) .
C12 N4 1.313(6) .
C12 Br1 1.900(5) .
C13 O1 1.398(7) .
N2 N3 1.404(4) .
N6 N7 1.193(4) .
N6 Mn1 2.255(3) 2_556
N7 N8 1.145(5) .
N9 N10 1.172(5) .
N10 N11 1.176(5) .
N11 Mn1 2.255(3) 2_656
