#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/24/2212463.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# 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_2212463
loop_
_publ_author_name
'Jing Qian'
'Wu Gu'
'Shi-Ping Yan'
'Dai-Zheng Liao'
'Peng Cheng'
_publ_section_title
Di-μ-azido-κ⁴N:N-bis{(azido-κN)[N,N-bis(2-pyridylmethyl-κN)ethylamine]manganese(II)}
_journal_coeditor_code           BI2156
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m687
_journal_page_last               m688
_journal_paper_doi               10.1107/S1600536807005405
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '[Mn2 (N3)4 (C14 H17 N3)2]'
_chemical_formula_moiety         'C28 H34 Mn2 N18'
_chemical_formula_sum            'C28 H34 Mn2 N18'
_chemical_formula_weight         732.61
_chemical_name_common            '[Mn2(bpea)2(μ2-N3)2(N3)2]'
_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
_cell_angle_alpha                74.254(2)
_cell_angle_beta                 76.212(2)
_cell_angle_gamma                75.797(3)
_cell_formula_units_Z            1
_cell_length_a                   8.8943(18)
_cell_length_b                   9.1784(19)
_cell_length_c                   10.963(2)
_cell_measurement_reflns_used    3298
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.80
_cell_measurement_theta_min      2.70
_cell_volume                     820.8(3)
_computing_cell_refinement       'SAINT (Bruker, 1997)'
_computing_data_collection       'SMART (Bruker, 1997)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL (Bruker, 1997)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker SMART CCD'
_diffrn_measurement_method       'φ and ω'
_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  0.0104
_diffrn_reflns_av_sigmaI/netI    0.0168
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            4422
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         1.96
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.821
_exptl_absorpt_correction_T_max  0.891
_exptl_absorpt_correction_T_min  0.742
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.482
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             378
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.363
_refine_diff_density_min         -0.235
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         2851
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0288
_refine_ls_R_factor_gt           0.0262
_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)+(0.0298P)²+0.423P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0682
_refine_ls_wR_factor_ref         0.0694
_reflns_number_gt                2627
_reflns_number_total             2851
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            bi2156.cif
_cod_data_source_block           I
_cod_database_code               2212463
_cod_database_fobs_code          2212463
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
Mn Mn1 0.48019(3) 0.06585(3) 0.33525(2) 0.03146(10) Uani d . 1
N N1 0.62510(19) -0.05477(19) 0.17180(15) 0.0399(4) Uani d . 1
N N2 0.33657(18) -0.11375(17) 0.32158(14) 0.0339(3) Uani d . 1
N N3 0.24754(17) 0.19962(17) 0.27929(14) 0.0335(3) Uani d . 1
N N4 0.59403(18) 0.26502(19) 0.25100(17) 0.0408(4) Uani d . 1
N N5 0.6488(2) 0.3005(2) 0.1416(2) 0.0602(5) Uani d . 1
N N6 0.7094(4) 0.3445(3) 0.0305(3) 0.0953(9) Uani d . 1
N N7 0.64453(19) -0.08553(19) 0.46262(15) 0.0421(4) Uani d . 1
N N8 0.75848(18) -0.17766(18) 0.43475(15) 0.0372(4) Uani d . 1
N N9 0.8692(2) -0.2657(2) 0.4075(2) 0.0667(6) Uani d . 1
C C1 0.7811(2) -0.0665(3) 0.13284(19) 0.0485(5) Uani d . 1
H H1 0.8298 0.0020 0.1510 0.058 Uiso calc R 1
C C2 0.8729(3) -0.1755(3) 0.0671(2) 0.0585(6) Uani d . 1
H H2 0.9812 -0.1807 0.0414 0.070 Uiso calc R 1
C C3 0.8009(3) -0.2758(3) 0.0405(2) 0.0635(7) Uani d . 1
H H3 0.8606 -0.3517 -0.0023 0.076 Uiso calc R 1
C C4 0.6395(3) -0.2644(3) 0.0773(2) 0.0556(6) Uani d . 1
H H4 0.5888 -0.3310 0.0587 0.067 Uiso calc R 1
C C5 0.5548(2) -0.1511(2) 0.14271(17) 0.0405(4) Uani d . 1
C C6 0.3794(2) -0.1270(2) 0.18594(19) 0.0429(5) Uani d . 1
H H6A 0.3301 -0.0337 0.1319 0.051 Uiso calc R 1
H H6B 0.3409 -0.2131 0.1772 0.051 Uiso calc R 1
C C7 0.3822(2) -0.2636(2) 0.4120(2) 0.0431(5) Uani d . 1
H H7A 0.3584 -0.2461 0.4985 0.052 Uiso calc R 1
H H7B 0.4956 -0.2974 0.3906 0.052 Uiso calc R 1
C C8 0.3039(3) -0.3935(3) 0.4132(3) 0.0678(7) Uani d . 1
H H8A 0.1914 -0.3611 0.4320 0.102 Uiso calc R 1
H H8B 0.3363 -0.4823 0.4782 0.102 Uiso calc R 1
H H8C 0.3345 -0.4193 0.3304 0.102 Uiso calc R 1
C C9 0.1681(2) -0.0495(2) 0.3533(2) 0.0417(4) Uani d . 1
H H9A 0.1343 -0.0749 0.4461 0.050 Uiso calc R 1
H H9B 0.1096 -0.0971 0.3159 0.050 Uiso calc R 1
C C10 0.1294(2) 0.1228(2) 0.30508(17) 0.0339(4) Uani d . 1
C C11 -0.0239(2) 0.1986(2) 0.29585(19) 0.0432(5) Uani d . 1
H H11 -0.1032 0.1430 0.3097 0.052 Uiso calc R 1
C C12 -0.0577(2) 0.3576(3) 0.2658(2) 0.0499(5) Uani d . 1
H H12 -0.1606 0.4105 0.2618 0.060 Uiso calc R 1
C C13 0.0626(3) 0.4366(2) 0.2420(2) 0.0497(5) Uani d . 1
H H13 0.0424 0.5439 0.2231 0.060 Uiso calc R 1
C C14 0.2132(2) 0.3542(2) 0.2468(2) 0.0422(5) Uani d . 1
H H14 0.2951 0.4080 0.2265 0.051 Uiso calc R 1
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_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N1 Mn1 N2 . 72.88(6) y
N1 Mn1 N3 . 108.85(6) y
N1 Mn1 N4 . 91.00(6) y
N1 Mn1 N7 . 88.39(6) y
N1 Mn1 N7 2_656 157.36(6) y
N2 Mn1 N3 . 72.11(5) y
N2 Mn1 N4 . 151.84(6) y
N2 Mn1 N7 . 100.79(6) y
N2 Mn1 N7 2_656 94.86(6) y
N3 Mn1 N4 . 92.46(6) y
N3 Mn1 N7 . 157.59(6) y
N3 Mn1 N7 2_656 84.29(6) y
N4 Mn1 N7 . 101.69(7) y
N4 Mn1 N7 2_656 107.18(6) y
N7 Mn1 N7 2_656 75.02(6) y
C1 N1 C5 . 118.35(17) ?
C1 N1 Mn1 . 123.68(14) ?
C5 N1 Mn1 . 115.35(13) ?
C9 N2 C6 . 110.21(15) ?
C9 N2 C7 . 111.61(15) ?
C6 N2 C7 . 112.05(15) ?
C9 N2 Mn1 . 108.09(11) ?
C6 N2 Mn1 . 105.39(11) ?
C7 N2 Mn1 . 109.23(11) ?
C10 N3 C14 . 118.12(16) ?
C10 N3 Mn1 . 117.57(12) ?
C14 N3 Mn1 . 122.89(12) ?
N5 N4 Mn1 . 123.86(15) ?
N4 N5 N6 . 175.6(2) ?
N8 N7 Mn1 . 127.53(13) ?
N8 N7 Mn1 2_656 126.22(13) ?
Mn1 N7 Mn1 2_656 104.98(6) ?
N9 N8 N7 . 179.5(2) ?
N1 C1 C2 . 123.0(2) ?
N1 C1 H1 . 118.5 ?
C2 C1 H1 . 118.5 ?
C3 C2 C1 . 118.3(2) ?
C3 C2 H2 . 120.8 ?
C1 C2 H2 . 120.8 ?
C2 C3 C4 . 120.0(2) ?
C2 C3 H3 . 120.0 ?
C4 C3 H3 . 120.0 ?
C3 C4 C5 . 118.3(2) ?
C3 C4 H4 . 120.8 ?
C5 C4 H4 . 120.8 ?
N1 C5 C4 . 122.0(2) ?
N1 C5 C6 . 115.01(16) ?
C4 C5 C6 . 123.0(2) ?
N2 C6 C5 . 110.34(15) ?
N2 C6 H6A . 109.6 ?
C5 C6 H6A . 109.6 ?
N2 C6 H6B . 109.6 ?
C5 C6 H6B . 109.6 ?
H6A C6 H6B . 108.1 ?
N2 C7 C8 . 116.23(17) ?
N2 C7 H7A . 108.2 ?
C8 C7 H7A . 108.2 ?
N2 C7 H7B . 108.2 ?
C8 C7 H7B . 108.2 ?
H7A C7 H7B . 107.4 ?
C7 C8 H8A . 109.5 ?
C7 C8 H8B . 109.5 ?
H8A C8 H8B . 109.5 ?
C7 C8 H8C . 109.5 ?
H8A C8 H8C . 109.5 ?
H8B C8 H8C . 109.5 ?
N2 C9 C10 . 112.97(15) ?
N2 C9 H9A . 109.0 ?
C10 C9 H9A . 109.0 ?
N2 C9 H9B . 109.0 ?
C10 C9 H9B . 109.0 ?
H9A C9 H9B . 107.8 ?
N3 C10 C11 . 121.75(17) ?
N3 C10 C9 . 117.10(16) ?
C11 C10 C9 . 121.02(17) ?
C12 C11 C10 . 119.25(19) ?
C12 C11 H11 . 120.4 ?
C10 C11 H11 . 120.4 ?
C13 C12 C11 . 119.06(19) ?
C13 C12 H12 . 120.5 ?
C11 C12 H12 . 120.5 ?
C14 C13 C12 . 118.69(19) ?
C14 C13 H13 . 120.7 ?
C12 C13 H13 . 120.7 ?
N3 C14 C13 . 123.02(19) ?
N3 C14 H14 . 118.5 ?
C13 C14 H14 . 118.5 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Mn1 N1 . 2.3180(16) y
Mn1 N2 . 2.3728(15) y
Mn1 N3 . 2.2617(15) y
Mn1 N4 . 2.1832(17) y
Mn1 N7 . 2.2226(16) y
Mn1 N7 2_656 2.2628(16) y
N1 C1 . 1.337(3) ?
N1 C5 . 1.339(3) ?
N2 C9 . 1.464(2) ?
N2 C6 . 1.475(2) ?
N2 C7 . 1.489(2) ?
N3 C10 . 1.340(2) ?
N3 C14 . 1.341(2) ?
N4 N5 . 1.170(3) ?
N5 N6 . 1.210(3) ?
N7 N8 . 1.186(2) ?
N7 Mn1 2_656 2.2628(16) ?
N8 N9 . 1.145(2) ?
C1 C2 . 1.377(3) ?
C1 H1 . 0.930 ?
C2 C3 . 1.366(4) ?
C2 H2 . 0.930 ?
C3 C4 . 1.381(4) ?
C3 H3 . 0.930 ?
C4 C5 . 1.388(3) ?
C4 H4 . 0.930 ?
C5 C6 . 1.497(3) ?
C6 H6A . 0.970 ?
C6 H6B . 0.970 ?
C7 C8 . 1.517(3) ?
C7 H7A . 0.970 ?
C7 H7B . 0.970 ?
C8 H8A . 0.960 ?
C8 H8B . 0.960 ?
C8 H8C . 0.960 ?
C9 C10 . 1.505(3) ?
C9 H9A . 0.970 ?
C9 H9B . 0.970 ?
C10 C11 . 1.384(3) ?
C11 C12 . 1.378(3) ?
C11 H11 . 0.930 ?
C12 C13 . 1.372(3) ?
C12 H12 . 0.930 ?
C13 C14 . 1.372(3) ?
C13 H13 . 0.930 ?
C14 H14 . 0.930 ?
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_site_symmetry_1
_geom_torsion_site_symmetry_4
_geom_torsion
N4 Mn1 N1 C1 . . 47.77(16)
N7 Mn1 N1 C1 . . -53.90(16)
N3 Mn1 N1 C1 . . 140.71(15)
N7 Mn1 N1 C1 2_656 . -96.2(2)
N2 Mn1 N1 C1 . . -155.70(17)
N4 Mn1 N1 C5 . . -150.93(13)
N7 Mn1 N1 C5 . . 107.41(14)
N3 Mn1 N1 C5 . . -57.99(14)
N7 Mn1 N1 C5 2_656 . 65.1(2)
N2 Mn1 N1 C5 . . 5.60(13)
N4 Mn1 N2 C9 . . -88.86(16)
N7 Mn1 N2 C9 . . 128.67(12)
N3 Mn1 N2 C9 . . -29.36(11)
N7 Mn1 N2 C9 2_656 . 53.03(12)
N1 Mn1 N2 C9 . . -146.41(12)
N4 Mn1 N2 C6 . . 28.97(18)
N7 Mn1 N2 C6 . . -113.49(11)
N3 Mn1 N2 C6 . . 88.47(12)
N7 Mn1 N2 C6 2_656 . 170.86(11)
N1 Mn1 N2 C6 . . -28.57(11)
N4 Mn1 N2 C7 . . 149.52(14)
N7 Mn1 N2 C7 . . 7.06(13)
N3 Mn1 N2 C7 . . -150.98(13)
N7 Mn1 N2 C7 2_656 . -68.59(12)
N1 Mn1 N2 C7 . . 91.98(12)
N4 Mn1 N3 C10 . . 176.61(13)
N7 Mn1 N3 C10 . . -53.9(2)
N7 Mn1 N3 C10 2_656 . -76.36(13)
N1 Mn1 N3 C10 . . 84.71(13)
N2 Mn1 N3 C10 . . 20.63(12)
N4 Mn1 N3 C14 . . -17.25(15)
N7 Mn1 N3 C14 . . 112.24(19)
N7 Mn1 N3 C14 2_656 . 89.77(15)
N1 Mn1 N3 C14 . . -109.15(15)
N2 Mn1 N3 C14 . . -173.23(16)
N7 Mn1 N4 N5 . . 113.73(18)
N3 Mn1 N4 N5 . . -83.75(18)
N7 Mn1 N4 N5 2_656 . -168.53(17)
N1 Mn1 N4 N5 . . 25.17(18)
N2 Mn1 N4 N5 . . -28.6(2)
N4 Mn1 N7 N8 . . -87.43(18)
N3 Mn1 N7 N8 . . 144.52(16)
N7 Mn1 N7 N8 2_656 . 167.7(2)
N1 Mn1 N7 N8 . . 3.26(18)
N2 Mn1 N7 N8 . . 75.50(18)
N4 Mn1 N7 Mn1 . 2_656 104.88(8)
N3 Mn1 N7 Mn1 . 2_656 -23.17(19)
N7 Mn1 N7 Mn1 2_656 2_656 0.0
N1 Mn1 N7 Mn1 . 2_656 -164.43(7)
N2 Mn1 N7 Mn1 . 2_656 -92.19(7)
C5 N1 C1 C2 . . -1.7(3)
Mn1 N1 C1 C2 . . 159.13(16)
N1 C1 C2 C3 . . 0.1(3)
C1 C2 C3 C4 . . 1.2(3)
C2 C3 C4 C5 . . -0.9(3)
C1 N1 C5 C4 . . 1.9(3)
Mn1 N1 C5 C4 . . -160.42(15)
C1 N1 C5 C6 . . -178.05(17)
Mn1 N1 C5 C6 . . 19.6(2)
C3 C4 C5 N1 . . -0.7(3)
C3 C4 C5 C6 . . 179.31(19)
C9 N2 C6 C5 . . 164.70(15)
C7 N2 C6 C5 . . -70.4(2)
Mn1 N2 C6 C5 . . 48.31(17)
N1 C5 C6 N2 . . -47.7(2)
C4 C5 C6 N2 . . 132.29(19)
C9 N2 C7 C8 . . 61.9(2)
C6 N2 C7 C8 . . -62.2(2)
Mn1 N2 C7 C8 . . -178.59(17)
C6 N2 C9 C10 . . -78.8(2)
C7 N2 C9 C10 . . 156.05(16)
Mn1 N2 C9 C10 . . 35.92(18)
C14 N3 C10 C11 . . 1.6(3)
Mn1 N3 C10 C11 . . 168.38(14)
C14 N3 C10 C9 . . -174.46(17)
Mn1 N3 C10 C9 . . -7.6(2)
N2 C9 C10 N3 . . -20.8(2)
N2 C9 C10 C11 . . 163.19(17)
N3 C10 C11 C12 . . -3.4(3)
C9 C10 C11 C12 . . 172.47(18)
C10 C11 C12 C13 . . 1.9(3)
C11 C12 C13 C14 . . 1.1(3)
C10 N3 C14 C13 . . 1.7(3)
Mn1 N3 C14 C13 . . -164.33(15)
C12 C13 C14 N3 . . -3.1(3)
