#------------------------------------------------------------------------------
#$Date: 2016-03-23 02:40:15 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179198 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/36/4313699.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_4313699
loop_
_publ_author_name
'En-Qing Gao'
'Shi-Qiang Bai'
'Yan-Feng Yue'
'Zhe-Ming Wang'
'Chun-Hua Yan'
_publ_contact_author_address
;
State Key Lab of Rare Earth Materials Chemistry and Applications & 
PKU-HKU Joint Lab on Rare Earth Materials and Bioinorganic Chemistry, 
College of Chemistry and Molecular Engineering, 
Peking University, 
Beijing 100871, 
China
;
_publ_contact_author_email       chyan@chem.pku.edu.cn
_publ_contact_author_fax         86-(10)-62754179
_publ_contact_author_name        'Prof. Chun-Hua Yan'
_publ_contact_author_phone       86-(10)-62754179
_publ_section_title
;
 New One-Dimensional Azido-Bridged Manganese(II) Coordination Polymers
 Exhibiting Alternating Ferromagnetic-Antiferromagnetic Interactions:
 Structural and Magnetic Studies
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3642
_journal_page_last               3649
_journal_paper_doi               10.1021/ic0262987
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C13 H12 Mn N8'
_chemical_formula_weight         335.25
_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                103.4941(15)
_cell_angle_beta                 113.9738(16)
_cell_angle_gamma                97.7399(14)
_cell_formula_units_Z            4
_cell_length_a                   10.5952(3)
_cell_length_b                   12.3357(3)
_cell_length_c                   12.9904(4)
_cell_measurement_reflns_used    15265
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      3.395
_cell_volume                     1457.35(8)
_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 0.964
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  'NONIUS KappaCCD'
_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  0.0950
_diffrn_reflns_av_sigmaI/netI    0.1078
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            26350
_diffrn_reflns_theta_full        27.44
_diffrn_reflns_theta_max         27.44
_diffrn_reflns_theta_min         3.40
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    0.915
_exptl_absorpt_correction_T_max  0.965
_exptl_absorpt_correction_T_min  0.910
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(Blessing, 1995, 1997)'
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.528
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             684
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.336
_refine_diff_density_min         -0.355
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         6410
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.1356
_refine_ls_R_factor_gt           0.0468
_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)+(0.0340P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0850
_refine_ls_wR_factor_ref         0.1038
_reflns_number_gt                3231
_reflns_number_total             6410
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0262987si20021223_061038_2.cif
_cod_data_source_block           2
_cod_original_cell_volume        1457.35(7)
_cod_database_code               4313699
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn1 Mn 0.03525(5) 0.14806(4) 0.05097(4) 0.03433(16) Uani 1 1 d . . .
Mn2 Mn -0.02477(5) 0.35405(4) 0.44335(4) 0.03493(16) Uani 1 1 d . . .
N1 N 0.2393(3) 0.1743(2) 0.0323(2) 0.0384(7) Uani 1 1 d . . .
N2 N 0.0300(3) 0.2837(2) -0.0506(2) 0.0370(7) Uani 1 1 d . . .
N3 N -0.2298(3) 0.3032(2) 0.4569(2) 0.0364(7) Uani 1 1 d . . .
N4 N 0.0034(3) 0.2172(2) 0.5459(2) 0.0356(7) Uani 1 1 d . . .
N5 N -0.1543(3) 0.1529(3) 0.0806(2) 0.0494(8) Uani 1 1 d . . .
N6 N -0.1495(3) 0.1870(2) 0.1747(3) 0.0366(7) Uani 1 1 d . . .
N7 N -0.1507(3) 0.2187(3) 0.2656(3) 0.0601(9) Uani 1 1 d . . .
N8 N 0.1679(3) 0.2727(3) 0.2325(3) 0.0549(8) Uani 1 1 d . . .
N9 N 0.1606(3) 0.3204(2) 0.3182(3) 0.0379(7) Uani 1 1 d . . .
N10 N 0.1601(3) 0.3714(3) 0.4057(3) 0.0514(8) Uani 1 1 d . . .
N11 N 0.0820(3) -0.0020(2) 0.1155(2) 0.0392(7) Uani 1 1 d . . .
N12 N 0.1363(3) -0.0017(2) 0.2164(3) 0.0429(7) Uani 1 1 d . . .
N13 N 0.1887(4) -0.0012(3) 0.3128(3) 0.0777(11) Uani 1 1 d . . .
N14 N -0.0916(3) 0.5024(2) 0.3860(2) 0.0426(7) Uani 1 1 d . . .
N15 N -0.1669(3) 0.5036(2) 0.2891(3) 0.0416(7) Uani 1 1 d . . .
N16 N -0.2412(4) 0.5044(3) 0.1955(3) 0.0712(10) Uani 1 1 d . . .
C1 C 0.3476(4) 0.1278(3) 0.0781(3) 0.0523(10) Uani 1 1 d . . .
H1A H 0.3346 0.0707 0.1113 0.063 Uiso 1 1 calc R . .
C2 C 0.4775(4) 0.1598(4) 0.0789(3) 0.0649(12) Uani 1 1 d . . .
H2A H 0.5502 0.1255 0.1127 0.078 Uiso 1 1 calc R . .
C3 C 0.4984(4) 0.2423(4) 0.0296(4) 0.0638(11) Uani 1 1 d . . .
H3A H 0.5857 0.2658 0.0298 0.077 Uiso 1 1 calc R . .
C4 C 0.3868(4) 0.2906(3) -0.0211(3) 0.0589(11) Uani 1 1 d . . .
H4A H 0.3973 0.3458 -0.0571 0.071 Uiso 1 1 calc R . .
C5 C 0.2609(3) 0.2555(3) -0.0171(3) 0.0393(8) Uani 1 1 d . . .
C6 C 0.1418(4) 0.3080(3) -0.0632(3) 0.0464(9) Uani 1 1 d . . .
H6A H 0.1487 0.3607 -0.1027 0.056 Uiso 1 1 calc R . .
C7 C -0.0824(3) 0.3378(3) -0.1007(3) 0.0380(8) Uani 1 1 d . . .
C8 C -0.1062(4) 0.3688(3) -0.2018(3) 0.0495(9) Uani 1 1 d . . .
H8A H -0.0486 0.3549 -0.2390 0.059 Uiso 1 1 calc R . .
C9 C -0.2157(4) 0.4201(3) -0.2472(3) 0.0545(10) Uani 1 1 d . . .
H9A H -0.2308 0.4405 -0.3150 0.065 Uiso 1 1 calc R . .
C10 C -0.3022(4) 0.4417(3) -0.1944(3) 0.0464(9) Uani 1 1 d . . .
C11 C -0.2763(4) 0.4121(3) -0.0927(3) 0.0552(10) Uani 1 1 d . . .
H11A H -0.3329 0.4270 -0.0547 0.066 Uiso 1 1 calc R . .
C12 C -0.1666(4) 0.3606(3) -0.0467(3) 0.0492(10) Uani 1 1 d . . .
H12A H -0.1504 0.3413 0.0218 0.059 Uiso 1 1 calc R . .
C13 C -0.4233(4) 0.4971(3) -0.2471(3) 0.0656(12) Uani 1 1 d . . .
H13A H -0.4233 0.5128 -0.3161 0.098 Uiso 1 1 calc R . .
H13B H -0.4098 0.5679 -0.1892 0.098 Uiso 1 1 calc R . .
H13C H -0.5130 0.4454 -0.2693 0.098 Uiso 1 1 calc R . .
C14 C -0.3451(4) 0.3420(3) 0.4148(3) 0.0527(10) Uani 1 1 d . . .
H14A H -0.3388 0.4053 0.3881 0.063 Uiso 1 1 calc R . .
C15 C -0.4739(4) 0.2929(3) 0.4086(3) 0.0598(11) Uani 1 1 d . . .
H15A H -0.5525 0.3224 0.3777 0.072 Uiso 1 1 calc R . .
C16 C -0.4850(4) 0.2014(4) 0.4480(3) 0.0589(11) Uani 1 1 d . . .
H16A H -0.5709 0.1670 0.4446 0.071 Uiso 1 1 calc R . .
C17 C -0.3659(4) 0.1603(3) 0.4933(3) 0.0546(10) Uani 1 1 d . . .
H17A H -0.3703 0.0982 0.5219 0.066 Uiso 1 1 calc R . .
C18 C -0.2414(3) 0.2116(3) 0.4959(3) 0.0382(8) Uani 1 1 d . . .
C19 C -0.1124(4) 0.1721(3) 0.5447(3) 0.0452(9) Uani 1 1 d . . .
H19A H -0.1150 0.1118 0.5760 0.054 Uiso 1 1 calc R . .
C20 C 0.1289(3) 0.1787(3) 0.6012(3) 0.0383(8) Uani 1 1 d . . .
C21 C 0.1332(4) 0.0906(3) 0.6511(3) 0.0578(11) Uani 1 1 d . . .
H21A H 0.0502 0.0511 0.6485 0.069 Uiso 1 1 calc R . .
C22 C 0.2607(4) 0.0611(3) 0.7050(3) 0.0671(12) Uani 1 1 d . . .
H22A H 0.2613 0.0023 0.7387 0.080 Uiso 1 1 calc R . .
C23 C 0.3845(4) 0.1153(3) 0.7100(3) 0.0523(10) Uani 1 1 d . . .
C24 C 0.3806(4) 0.2025(3) 0.6612(3) 0.0613(11) Uani 1 1 d . . .
H24A H 0.4641 0.2415 0.6642 0.074 Uiso 1 1 calc R . .
C25 C 0.2543(4) 0.2341(3) 0.6071(3) 0.0585(11) Uani 1 1 d . . .
H25A H 0.2549 0.2936 0.5745 0.070 Uiso 1 1 calc R . .
C26 C 0.5238(4) 0.0834(4) 0.7698(3) 0.0777(13) Uani 1 1 d . . .
H26A H 0.5059 0.0167 0.7928 0.117 Uiso 1 1 calc R . .
H26B H 0.5898 0.1467 0.8390 0.117 Uiso 1 1 calc R . .
H26C H 0.5639 0.0667 0.7154 0.117 Uiso 1 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
N5 Mn1 N11 93.55(10) . 2 ?
N5 Mn1 N8 88.65(11) . . ?
N11 Mn1 N8 170.12(10) 2 . ?
N5 Mn1 N11 96.16(10) . . ?
N11 Mn1 N11 78.35(10) 2 . ?
N8 Mn1 N11 91.84(10) . . ?
N5 Mn1 N1 170.79(10) . . ?
N11 Mn1 N1 93.77(10) 2 . ?
N8 Mn1 N1 85.08(10) . . ?
N11 Mn1 N1 90.80(9) . . ?
N5 Mn1 N2 101.63(10) . . ?
N11 Mn1 N2 92.79(9) 2 . ?
N8 Mn1 N2 96.20(10) . . ?
N11 Mn1 N2 160.61(9) . . ?
N1 Mn1 N2 72.43(9) . . ?
N10 Mn2 N14 92.59(11) . 2_566 ?
N10 Mn2 N14 94.63(10) . . ?
N14 Mn2 N14 78.89(10) 2_566 . ?
N10 Mn2 N7 88.42(11) . . ?
N14 Mn2 N7 175.67(11) 2_566 . ?
N14 Mn2 N7 96.83(11) . . ?
N10 Mn2 N3 169.36(11) . . ?
N14 Mn2 N3 97.49(10) 2_566 . ?
N14 Mn2 N3 90.65(9) . . ?
N7 Mn2 N3 81.78(10) . . ?
N10 Mn2 N4 103.93(10) . . ?
N14 Mn2 N4 90.81(9) 2_566 . ?
N14 Mn2 N4 159.20(9) . . ?
N7 Mn2 N4 93.04(10) . . ?
N3 Mn2 N4 72.65(9) . . ?
C1 N1 C5 116.8(3) . . ?
C1 N1 Mn1 126.1(2) . . ?
C5 N1 Mn1 116.54(19) . . ?
C6 N2 C7 118.0(3) . . ?
C6 N2 Mn1 113.2(2) . . ?
C7 N2 Mn1 128.7(2) . . ?
C14 N3 C18 117.4(3) . . ?
C14 N3 Mn2 126.7(2) . . ?
C18 N3 Mn2 115.1(2) . . ?
C19 N4 C20 119.5(3) . . ?
C19 N4 Mn2 112.1(2) . . ?
C20 N4 Mn2 128.3(2) . . ?
N6 N5 Mn1 124.0(2) . . ?
N7 N6 N5 177.2(3) . . ?
N6 N7 Mn2 140.4(3) . . ?
N9 N8 Mn1 141.8(2) . . ?
N10 N9 N8 176.7(3) . . ?
N9 N10 Mn2 125.5(2) . . ?
N12 N11 Mn1 129.9(2) . 2 ?
N12 N11 Mn1 127.4(2) . . ?
Mn1 N11 Mn1 101.65(10) 2 . ?
N13 N12 N11 179.8(4) . . ?
N15 N14 Mn2 130.0(2) . 2_566 ?
N15 N14 Mn2 128.9(2) . . ?
Mn2 N14 Mn2 101.11(10) 2_566 . ?
N16 N15 N14 179.1(3) . . ?
N1 C1 C2 123.5(3) . . ?
C3 C2 C1 119.2(3) . . ?
C2 C3 C4 118.7(3) . . ?
C5 C4 C3 118.8(3) . . ?
N1 C5 C4 123.0(3) . . ?
N1 C5 C6 115.6(3) . . ?
C4 C5 C6 121.3(3) . . ?
N2 C6 C5 121.9(3) . . ?
C12 C7 C8 118.9(3) . . ?
C12 C7 N2 119.2(3) . . ?
C8 C7 N2 121.9(3) . . ?
C9 C8 C7 120.0(3) . . ?
C10 C9 C8 121.4(3) . . ?
C9 C10 C11 118.2(3) . . ?
C9 C10 C13 120.4(3) . . ?
C11 C10 C13 121.4(3) . . ?
C10 C11 C12 120.6(3) . . ?
C7 C12 C11 120.8(3) . . ?
N3 C14 C15 123.0(3) . . ?
C16 C15 C14 119.5(3) . . ?
C15 C16 C17 118.4(3) . . ?
C18 C17 C16 119.6(3) . . ?
N3 C18 C17 122.1(3) . . ?
N3 C18 C19 116.5(3) . . ?
C17 C18 C19 121.4(3) . . ?
N4 C19 C18 122.3(3) . . ?
C25 C20 C21 117.5(3) . . ?
C25 C20 N4 117.9(3) . . ?
C21 C20 N4 124.6(3) . . ?
C20 C21 C22 120.4(3) . . ?
C23 C22 C21 122.2(3) . . ?
C22 C23 C24 117.5(3) . . ?
C22 C23 C26 122.0(3) . . ?
C24 C23 C26 120.5(4) . . ?
C23 C24 C25 121.4(3) . . ?
C20 C25 C24 121.0(3) . . ?
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 N5 2.199(3) . ?
Mn1 N11 2.205(3) 2 ?
Mn1 N8 2.221(3) . ?
Mn1 N11 2.237(2) . ?
Mn1 N1 2.261(2) . ?
Mn1 N2 2.354(2) . ?
Mn2 N10 2.199(3) . ?
Mn2 N14 2.221(3) 2_566 ?
Mn2 N14 2.227(2) . ?
Mn2 N7 2.236(3) . ?
Mn2 N3 2.267(2) . ?
Mn2 N4 2.361(2) . ?
N1 C1 1.336(4) . ?
N1 C5 1.350(3) . ?
N2 C6 1.266(4) . ?
N2 C7 1.440(4) . ?
N3 C14 1.326(4) . ?
N3 C18 1.352(4) . ?
N4 C19 1.269(4) . ?
N4 C20 1.437(4) . ?
N5 N6 1.174(3) . ?
N6 N7 1.159(3) . ?
N8 N9 1.170(3) . ?
N9 N10 1.166(3) . ?
N11 N12 1.197(3) . ?
N11 Mn1 2.205(3) 2 ?
N12 N13 1.144(3) . ?
N14 N15 1.191(3) . ?
N14 Mn2 2.221(3) 2_566 ?
N15 N16 1.152(3) . ?
C1 C2 1.375(4) . ?
C2 C3 1.361(5) . ?
C3 C4 1.387(5) . ?
C4 C5 1.372(4) . ?
C5 C6 1.469(4) . ?
C7 C12 1.361(4) . ?
C7 C8 1.387(4) . ?
C8 C9 1.382(4) . ?
C9 C10 1.368(4) . ?
C10 C11 1.383(4) . ?
C10 C13 1.524(4) . ?
C11 C12 1.387(4) . ?
C14 C15 1.379(4) . ?
C15 C16 1.354(5) . ?
C16 C17 1.379(4) . ?
C17 C18 1.368(4) . ?
C18 C19 1.459(4) . ?
C20 C25 1.373(4) . ?
C20 C21 1.385(4) . ?
C21 C22 1.390(4) . ?
C22 C23 1.358(5) . ?
C23 C24 1.367(5) . ?
C23 C26 1.518(4) . ?
C24 C25 1.393(4) . ?
