#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/56/2215616.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_2215616
loop_
_publ_author_name
Hu,Sheng
'Zhang, Shu-Hua'
'Zeng, Ming-Hua'
_publ_section_title
Poly[bis(μ₂-azido-κ²N¹:N³)(μ₂-3,5-di-2-pyridyl-1,2,4-triazole-κ⁴N¹,N⁵:N²,N³)manganese(II)]
_journal_coeditor_code           NG2325
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m2543
_journal_page_last               m2543
_journal_paper_doi               10.1107/S1600536807044066
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '[Mn2 (N3)2 (C12 H8 N5)2]'
_chemical_formula_moiety         '(C12 H8 N5)2 (N3)2 Mn2'
_chemical_formula_sum            'C24 H16 Mn2 N16'
_chemical_formula_weight         638.38
_chemical_name_systematic
;
Poly[bis(μ₂-azido-κ²N¹:N³)(μ₂-3,5-di-2-pyridyl-
1,2,4-triazole-κ⁴N¹,N⁵:N²,N³)manganese(II)]
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 109.245(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            1
_cell_length_a                   8.6965(9)
_cell_length_b                   6.5597(7)
_cell_length_c                   11.8601(13)
_cell_measurement_reflns_used    2337
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.99
_cell_measurement_theta_min      1.82
_cell_volume                     638.77(12)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL (Bruker, 1997)'
_computing_publication_material  'SHELXTL (Bruker, 1997)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX area-detector'
_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  0.0193
_diffrn_reflns_av_sigmaI/netI    0.0475
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            3598
_diffrn_reflns_theta_full        26.99
_diffrn_reflns_theta_max         26.99
_diffrn_reflns_theta_min         1.82
_exptl_absorpt_coefficient_mu    1.039
_exptl_absorpt_correction_T_max  0.796
_exptl_absorpt_correction_T_min  0.732
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.660
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             322
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.403
_refine_diff_density_min         -0.232
_refine_ls_abs_structure_details 'Flack (1983), with 825 Friedel pairs'
_refine_ls_abs_structure_Flack   0.02(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         2337
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0375
_refine_ls_R_factor_gt           0.0349
_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)+(0.0334P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0751
_refine_ls_wR_factor_ref         0.0762
_reflns_number_gt                2207
_reflns_number_total             2337
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ng2325.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2215616
_cod_database_fobs_code          2215616
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -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 0.20518(4) 0.28461(8) 0.01852(3) 0.02671(12) Uani d . 1
C C1 0.2386(4) -0.0499(5) -0.1771(3) 0.0378(8) Uani d . 1
H H1A 0.2845 -0.1357 -0.1123 0.045 Uiso calc R 1
C C2 0.2498(4) -0.1043(6) -0.2863(3) 0.0432(9) Uani d . 1
H H2A 0.3023 -0.2240 -0.2948 0.052 Uiso calc R 1
C C3 0.1817(4) 0.0222(6) -0.3828(3) 0.0433(9) Uani d . 1
H H3A 0.1896 -0.0090 -0.4572 0.052 Uiso calc R 1
C C4 0.1025(4) 0.1938(6) -0.3673(3) 0.0398(8) Uani d . 1
H H4A 0.0545 0.2800 -0.4316 0.048 Uiso calc R 1
C C5 0.0938(3) 0.2397(5) -0.2553(3) 0.0301(8) Uani d . 1
C C6 0.0090(3) 0.4189(5) -0.2304(2) 0.0279(6) Uani d . 1
C C7 -0.1260(4) 0.6830(5) -0.2408(3) 0.0271(6) Uani d . 1
C C8 -0.2227(4) 0.8677(5) -0.2788(3) 0.0298(7) Uani d . 1
C C9 -0.2739(4) 0.9397(6) -0.3957(3) 0.0412(8) Uani d . 1
H H9A -0.2508 0.8674 -0.4556 0.049 Uiso calc R 1
C C10 -0.3587(5) 1.1186(6) -0.4209(3) 0.0492(10) Uani d . 1
H H10A -0.3943 1.1689 -0.4985 0.059 Uiso calc R 1
C C11 -0.3914(4) 1.2242(6) -0.3312(3) 0.0475(9) Uani d . 1
H H11A -0.4469 1.3477 -0.3463 0.057 Uiso calc R 1
C C12 -0.3394(4) 1.1413(6) -0.2185(3) 0.0418(8) Uani d . 1
H H12A -0.3627 1.2112 -0.1579 0.050 Uiso calc R 1
N N1 0.0114(3) 0.4542(4) -0.1192(2) 0.0277(6) Uani d . 1
N N2 -0.0767(3) 0.6266(4) -0.1258(2) 0.0272(6) Uani d . 1
N N3 -0.0742(3) 0.5565(4) -0.3107(2) 0.0311(6) Uani d . 1
N N4 0.1652(3) 0.1196(4) -0.1599(2) 0.0305(6) Uani d . 1
N N5 -0.2582(3) 0.9683(4) -0.1913(2) 0.0315(6) Uani d . 1
N N6 0.3757(3) 0.4973(5) -0.0301(3) 0.0504(8) Uani d . 1
N N7 0.4788(3) 0.5367(4) -0.0680(2) 0.0302(6) Uani d . 1
N N8 0.5818(3) 0.5817(5) -0.1066(3) 0.0400(7) Uani d . 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_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N2 Mn1 N1 2_545 . 104.67(9) n
N2 Mn1 N8 2_545 2_645 87.13(10) n
N1 Mn1 N8 . 2_645 162.01(9) n
N2 Mn1 N6 2_545 . 160.37(11) n
N1 Mn1 N6 . . 84.57(10) n
N8 Mn1 N6 2_645 . 88.54(11) n
N2 Mn1 N5 2_545 2_545 73.88(9) n
N1 Mn1 N5 . 2_545 105.95(9) n
N8 Mn1 N5 2_645 2_545 90.21(10) n
N6 Mn1 N5 . 2_545 87.01(11) n
N2 Mn1 N4 2_545 . 110.94(9) n
N1 Mn1 N4 . . 73.20(9) n
N8 Mn1 N4 2_645 . 90.03(10) n
N6 Mn1 N4 . . 88.19(11) n
N5 Mn1 N4 2_545 . 175.18(10) n
N4 C1 C2 . . 123.2(3) ?
N4 C1 H1A . . 118.4 ?
C2 C1 H1A . . 118.4 ?
C1 C2 C3 . . 118.7(3) ?
C1 C2 H2A . . 120.7 ?
C3 C2 H2A . . 120.7 ?
C4 C3 C2 . . 118.9(3) ?
C4 C3 H3A . . 120.6 ?
C2 C3 H3A . . 120.6 ?
C3 C4 C5 . . 119.8(3) ?
C3 C4 H4A . . 120.1 ?
C5 C4 H4A . . 120.1 ?
N4 C5 C4 . . 121.4(3) ?
N4 C5 C6 . . 114.9(3) ?
C4 C5 C6 . . 123.7(3) ?
N1 C6 N3 . . 114.5(3) ?
N1 C6 C5 . . 119.6(3) ?
N3 C6 C5 . . 125.9(2) ?
N2 C7 N3 . . 113.3(3) ?
N2 C7 C8 . . 120.1(3) ?
N3 C7 C8 . . 126.5(3) ?
N5 C8 C9 . . 121.5(3) ?
N5 C8 C7 . . 115.1(3) ?
C9 C8 C7 . . 123.5(3) ?
C10 C9 C8 . . 118.8(3) ?
C10 C9 H9A . . 120.6 ?
C8 C9 H9A . . 120.6 ?
C9 C10 C11 . . 119.9(3) ?
C9 C10 H10A . . 120.1 ?
C11 C10 H10A . . 120.1 ?
C12 C11 C10 . . 117.9(3) ?
C12 C11 H11A . . 121.1 ?
C10 C11 H11A . . 121.1 ?
N5 C12 C11 . . 123.8(3) ?
N5 C12 H12A . . 118.1 ?
C11 C12 H12A . . 118.1 ?
C6 N1 N2 . . 105.3(2) ?
C6 N1 Mn1 . . 113.65(19) ?
N2 N1 Mn1 . . 137.63(19) ?
C7 N2 N1 . . 105.9(2) ?
C7 N2 Mn1 . 2 113.8(2) ?
N1 N2 Mn1 . 2 137.99(19) ?
C6 N3 C7 . . 100.9(2) ?
C1 N4 C5 . . 118.0(3) ?
C1 N4 Mn1 . . 126.9(2) ?
C5 N4 Mn1 . . 112.7(2) ?
C12 N5 C8 . . 118.2(3) ?
C12 N5 Mn1 . 2 127.3(2) ?
C8 N5 Mn1 . 2 113.7(2) ?
N7 N6 Mn1 . . 154.2(3) ?
N6 N7 N8 . . 178.3(4) ?
N7 N8 Mn1 . 2_655 126.1(2) ?
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 N2 2_545 2.208(2) n
Mn1 N1 . 2.221(2) n
Mn1 N8 2_645 2.240(3) n
Mn1 N6 . 2.245(3) ?
Mn1 N5 2_545 2.289(3) n
Mn1 N4 . 2.299(3) n
C1 N4 . 1.331(4) ?
C1 C2 . 1.377(5) ?
C1 H1A . 0.9300 ?
C2 C3 . 1.380(5) ?
C2 H2A . 0.9300 ?
C3 C4 . 1.363(5) ?
C3 H3A . 0.9300 ?
C4 C5 . 1.389(4) ?
C4 H4A . 0.9300 ?
C5 N4 . 1.351(4) ?
C5 C6 . 1.468(4) ?
C6 N1 . 1.333(4) ?
C6 N3 . 1.339(4) ?
C7 N2 . 1.340(4) ?
C7 N3 . 1.351(4) ?
C7 C8 . 1.459(4) ?
C8 N5 . 1.348(4) ?
C8 C9 . 1.392(4) ?
C9 C10 . 1.365(5) ?
C9 H9A . 0.9300 ?
C10 C11 . 1.375(5) ?
C10 H10A . 0.9300 ?
C11 C12 . 1.374(5) ?
C11 H11A . 0.9300 ?
C12 N5 . 1.319(4) ?
C12 H12A . 0.9300 ?
N1 N2 . 1.354(3) ?
N2 Mn1 2 2.208(2) ?
N5 Mn1 2 2.289(3) ?
N6 N7 . 1.157(4) ?
N7 N8 . 1.170(4) ?
N8 Mn1 2_655 2.240(3) ?
