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#$Date: 2016-03-23 02:44:31 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179202 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/37/4313701.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_4313701
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            'C12 H9 Cl Mn N8'
_chemical_formula_weight         355.66
_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                74.5845(15)
_cell_angle_beta                 76.4177(13)
_cell_angle_gamma                83.2995(15)
_cell_formula_units_Z            2
_cell_length_a                   8.0054(2)
_cell_length_b                   9.7308(3)
_cell_length_c                   9.9532(3)
_cell_measurement_reflns_used    9523
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      3.395
_cell_volume                     725.33(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 0.966
_diffrn_measured_fraction_theta_max 0.966
_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  0.0559
_diffrn_reflns_av_sigmaI/netI    0.0549
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            14372
_diffrn_reflns_theta_full        27.46
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_min         3.43
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    1.103
_exptl_absorpt_correction_T_max  0.919
_exptl_absorpt_correction_T_min  0.861
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(Blessing, 1995, 1997)'
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.628
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             358
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.279
_refine_diff_density_min         -0.383
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         3222
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0685
_refine_ls_R_factor_gt           0.0377
_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)+(0.0414P)²+0.1514P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0816
_refine_ls_wR_factor_ref         0.0921
_reflns_number_gt                2279
_reflns_number_total             3222
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0262987si20021223_061038_4.cif
_cod_data_source_block           4
_cod_database_code               4313701
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 0.15435(4) 0.57592(4) 0.54450(4) 0.03497(13) Uani 1 1 d . . .
N1 N -0.0200(2) 0.6288(2) 0.7402(2) 0.0375(4) Uani 1 1 d . . .
N2 N 0.1901(2) 0.8194(2) 0.5328(2) 0.0418(5) Uani 1 1 d . . .
N3 N 0.0385(2) 0.3675(2) 0.5918(2) 0.0400(5) Uani 1 1 d . . .
N4 N 0.0550(3) 0.2602(2) 0.6810(2) 0.0442(5) Uani 1 1 d . . .
N5 N 0.0701(5) 0.1575(3) 0.7667(3) 0.0852(9) Uani 1 1 d . . .
N6 N 0.3495(3) 0.5099(3) 0.6776(2) 0.0636(7) Uani 1 1 d . . .
N7 N 0.4985(3) 0.4900(2) 0.65411(18) 0.0349(4) Uani 1 1 d . . .
N8 N 0.6467(3) 0.4694(2) 0.6362(2) 0.0506(6) Uani 1 1 d . . .
C1 C -0.1271(3) 0.5420(3) 0.8417(3) 0.0429(6) Uani 1 1 d . . .
H1A H -0.1457 0.4553 0.8266 0.052 Uiso 1 1 calc R . .
C2 C -0.2116(3) 0.5746(3) 0.9680(3) 0.0510(7) Uani 1 1 d . . .
H2A H -0.2855 0.5111 1.0360 0.061 Uiso 1 1 calc R . .
C3 C -0.1849(4) 0.7023(3) 0.9917(3) 0.0536(7) Uani 1 1 d . . .
H3A H -0.2393 0.7262 1.0766 0.064 Uiso 1 1 calc R . .
C4 C -0.0766(4) 0.7940(3) 0.8881(3) 0.0528(7) Uani 1 1 d . . .
H4A H -0.0573 0.8813 0.9016 0.063 Uiso 1 1 calc R . .
C5 C 0.0035(3) 0.7554(2) 0.7634(3) 0.0412(6) Uani 1 1 d . . .
C6 C 0.1162(3) 0.8509(3) 0.6499(3) 0.0496(7) Uani 1 1 d . . .
H6A H 0.1352 0.9384 0.6632 0.060 Uiso 1 1 calc R . .
C7 C 0.2948(3) 0.9199(3) 0.4234(3) 0.0446(6) Uani 1 1 d . . .
C8 C 0.3091(4) 1.0586(3) 0.4274(3) 0.0618(8) Uani 1 1 d . . .
H8A H 0.2472 1.0913 0.5055 0.074 Uiso 1 1 calc R . .
C9 C 0.4125(5) 1.1489(3) 0.3187(4) 0.0731(10) Uani 1 1 d . . .
H9A H 0.4192 1.2426 0.3225 0.088 Uiso 1 1 calc R . .
C10 C 0.5048(4) 1.1015(3) 0.2059(4) 0.0639(8) Uani 1 1 d . . .
C11 C 0.4904(5) 0.9666(4) 0.1969(5) 0.1109(16) Uani 1 1 d . . .
H11A H 0.5522 0.9347 0.1183 0.133 Uiso 1 1 calc R . .
C12 C 0.3827(5) 0.8777(3) 0.3061(4) 0.0974(14) Uani 1 1 d . . .
H12A H 0.3703 0.7863 0.2988 0.117 Uiso 1 1 calc R . .
Cl1 Cl 0.63684(12) 1.21442(11) 0.06556(12) 0.1020(4) 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'
Cl Cl 0.1484 0.1585 '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
N8 Mn1 N6 87.92(8) 2_666 . ?
N8 Mn1 N3 90.46(8) 2_666 2_566 ?
N6 Mn1 N3 177.32(9) . 2_566 ?
N8 Mn1 N3 93.23(8) 2_666 . ?
N6 Mn1 N3 98.60(9) . . ?
N3 Mn1 N3 79.36(8) 2_566 . ?
N8 Mn1 N1 172.43(7) 2_666 . ?
N6 Mn1 N1 85.46(8) . . ?
N3 Mn1 N1 96.29(7) 2_566 . ?
N3 Mn1 N1 91.40(7) . . ?
N8 Mn1 N2 103.56(8) 2_666 . ?
N6 Mn1 N2 89.11(9) . . ?
N3 Mn1 N2 93.34(7) 2_566 . ?
N3 Mn1 N2 161.79(7) . . ?
N1 Mn1 N2 72.69(7) . . ?
N8 Mn1 Mn1 92.40(5) 2_666 2_566 ?
N6 Mn1 Mn1 138.24(7) . 2_566 ?
N3 Mn1 Mn1 39.70(5) 2_566 2_566 ?
N3 Mn1 Mn1 39.66(5) . 2_566 ?
N1 Mn1 Mn1 94.99(5) . 2_566 ?
N2 Mn1 Mn1 130.93(5) . 2_566 ?
N8 Mn1 Mn1 44.50(5) 2_666 2_666 ?
N6 Mn1 Mn1 43.73(6) . 2_666 ?
N3 Mn1 Mn1 134.83(5) 2_566 2_666 ?
N3 Mn1 Mn1 102.37(5) . 2_666 ?
N1 Mn1 Mn1 128.47(5) . 2_666 ?
N2 Mn1 Mn1 94.62(5) . 2_666 ?
Mn1 Mn1 Mn1 126.662(16) 2_566 2_666 ?
C1 N1 C5 117.5(2) . . ?
C1 N1 Mn1 126.58(15) . . ?
C5 N1 Mn1 115.41(15) . . ?
C6 N2 C7 119.9(2) . . ?
C6 N2 Mn1 110.90(16) . . ?
C7 N2 Mn1 128.75(16) . . ?
N4 N3 Mn1 128.37(15) . 2_566 ?
N4 N3 Mn1 130.13(15) . . ?
Mn1 N3 Mn1 100.64(8) 2_566 . ?
N5 N4 N3 179.7(4) . . ?
N7 N6 Mn1 134.73(18) . . ?
N8 N7 N6 177.4(2) . . ?
N7 N8 Mn1 133.11(17) . 2_666 ?
N1 C1 C2 123.2(2) . . ?
C3 C2 C1 118.9(2) . . ?
C4 C3 C2 118.9(2) . . ?
C3 C4 C5 119.4(2) . . ?
N1 C5 C4 122.1(2) . . ?
N1 C5 C6 116.9(2) . . ?
C4 C5 C6 121.0(2) . . ?
N2 C6 C5 122.6(2) . . ?
C12 C7 C8 117.6(3) . . ?
C12 C7 N2 117.9(2) . . ?
C8 C7 N2 124.5(2) . . ?
C9 C8 C7 121.3(3) . . ?
C10 C9 C8 119.7(3) . . ?
C9 C10 C11 120.5(3) . . ?
C9 C10 Cl1 120.7(2) . . ?
C11 C10 Cl1 118.8(3) . . ?
C10 C11 C12 119.1(3) . . ?
C7 C12 C11 121.8(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 N8 2.208(2) 2_666 ?
Mn1 N6 2.212(2) . ?
Mn1 N3 2.2168(19) 2_566 ?
Mn1 N3 2.2183(19) . ?
Mn1 N1 2.2575(19) . ?
Mn1 N2 2.3884(18) . ?
Mn1 Mn1 3.4133(6) 2_566 ?
Mn1 Mn1 5.4845(7) 2_666 ?
N1 C1 1.333(3) . ?
N1 C5 1.353(3) . ?
N2 C6 1.275(3) . ?
N2 C7 1.429(3) . ?
N3 N4 1.194(3) . ?
N3 Mn1 2.2168(19) 2_566 ?
N4 N5 1.144(3) . ?
N6 N7 1.163(3) . ?
N7 N8 1.159(3) . ?
N8 Mn1 2.208(2) 2_666 ?
C1 C2 1.378(3) . ?
C2 C3 1.374(4) . ?
C3 C4 1.372(4) . ?
C4 C5 1.383(3) . ?
C5 C6 1.454(3) . ?
C7 C12 1.352(4) . ?
C7 C8 1.379(3) . ?
C8 C9 1.368(4) . ?
C9 C10 1.352(5) . ?
C10 C11 1.358(5) . ?
C10 Cl1 1.743(3) . ?
C11 C12 1.382(4) . ?
