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#$Date: 2016-03-23 01:59:37 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179165 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/26/4312679.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_4312679
loop_
_publ_author_name
'En-Qing Gao'
'Shi-Qiang Bai'
'Chuan-Feng Wang'
'Yan-Feng Yue'
'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
;
 Structural and Magnetic Properties of Three One-Dimensional Azido-Bridged
 Copper(II) and Manganese(II) Coordination Polymers
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8456
_journal_page_last               8464
_journal_paper_doi               10.1021/ic034618w
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C9 H9 Mn N9'
_chemical_formula_weight         298.19
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.0000
_cell_angle_beta                 109.5816(14)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            8
_cell_length_a                   14.16450(40)
_cell_length_b                   14.59350(40)
_cell_length_c                   12.78810(40)
_cell_measurement_reflns_used    16851
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      3.395
_cell_volume                     2490.54(13)
_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 0.985
_diffrn_measured_fraction_theta_max 0.985
_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  0.0655
_diffrn_reflns_av_sigmaI/netI    0.0422
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            22593
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         3.50
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    1.062
_exptl_absorpt_correction_T_max  0.856
_exptl_absorpt_correction_T_min  0.773
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(Blessing, 1995, 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.591
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1208
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.655
_refine_diff_density_min         -0.375
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         2829
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0719
_refine_ls_R_factor_gt           0.0418
_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)+(0.0606P)²+2.3611P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1059
_refine_ls_wR_factor_ref         0.1180
_reflns_number_gt                1981
_reflns_number_total             2829
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic034618wsi20030604_105834_1.cif
_cod_data_source_block           3
_cod_database_code               4312679
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x, -y, z+1/2'
'x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z+1/2'
'-x, -y, -z'
'-x, y, -z-1/2'
'-x+1/2, -y+1/2, -z'
'-x+1/2, y+1/2, -z-1/2'
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 0.06249(3) 0.13327(3) 0.15461(3) 0.03501(16) Uani 1 1 d . . .
N1 N 0.07140(16) 0.29086(15) 0.15994(18) 0.0377(5) Uani 1 1 d . . .
N2 N 0.27768(18) 0.22647(18) 0.1964(2) 0.0479(6) Uani 1 1 d . . .
N3 N 0.22185(18) 0.15184(16) 0.1555(2) 0.0433(6) Uani 1 1 d . . .
N4 N 0.0807(2) -0.01732(18) 0.1477(2) 0.0554(7) Uani 1 1 d . . .
N5 N 0.03963(16) -0.07592(16) 0.08772(18) 0.0358(5) Uani 1 1 d . . .
N6 N 0.0016(2) -0.13771(18) 0.0310(2) 0.0499(6) Uani 1 1 d . . .
N7 N -0.09219(17) 0.13113(16) 0.16318(19) 0.0397(5) Uani 1 1 d . . .
N8 N -0.16866(18) 0.11909(17) 0.0902(2) 0.0441(6) Uani 1 1 d . . .
N9 N -0.2437(2) 0.1094(3) 0.0190(3) 0.0845(11) Uani 1 1 d . . .
C1 C -0.0101(2) 0.3408(2) 0.1088(2) 0.0457(7) Uani 1 1 d . . .
H1A H -0.0696 0.3102 0.0721 0.055 Uiso 1 1 calc R . .
C2 C -0.0107(3) 0.4319(3) 0.1077(3) 0.0671(10) Uani 1 1 d . . .
H2A H -0.0702 0.4630 0.0724 0.081 Uiso 1 1 calc R . .
C3 C 0.0703(3) 0.4775(3) 0.1550(3) 0.0762(11) Uani 1 1 d . . .
H3A H 0.0696 0.5412 0.1524 0.091 Uiso 1 1 calc R . .
C4 C 0.1544(3) 0.4334(2) 0.2070(3) 0.0560(8) Uani 1 1 d . . .
H4A H 0.2132 0.4659 0.2412 0.067 Uiso 1 1 calc R . .
C5 C 0.1547(2) 0.33937(18) 0.2105(2) 0.0356(6) Uani 1 1 d . . .
C6 C 0.2481(2) 0.2876(2) 0.2711(3) 0.0485(7) Uani 1 1 d . . .
H6A H 0.3019 0.3307 0.3049 0.058 Uiso 1 1 calc R . .
H6B H 0.2372 0.2518 0.3299 0.058 Uiso 1 1 calc R . .
C7 C 0.3555(3) 0.2383(3) 0.1575(4) 0.0746(12) Uani 1 1 d . . .
H7 H 0.4024 0.2855 0.1747 0.090 Uiso 1 1 calc R . .
C8 C 0.3491(4) 0.1587(4) 0.0809(4) 0.105(2) Uani 1 1 d . . .
H8 H 0.3906 0.1442 0.0403 0.126 Uiso 1 1 calc R . .
C9 C 0.2609(3) 0.1100(2) 0.0865(3) 0.0566(9) Uani 1 1 d . . .
H9A H 0.2352 0.0568 0.0472 0.068 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
N4 Mn1 N7 92.52(9) . 6_556 ?
N4 Mn1 N7 96.73(10) . . ?
N7 Mn1 N7 78.02(9) 6_556 . ?
N4 Mn1 N6 89.88(10) . 5 ?
N7 Mn1 N6 167.77(9) 6_556 5 ?
N7 Mn1 N6 89.80(9) . 5 ?
N4 Mn1 N3 89.42(10) . . ?
N7 Mn1 N3 99.09(9) 6_556 . ?
N7 Mn1 N3 173.28(9) . . ?
N6 Mn1 N3 92.92(10) 5 . ?
N4 Mn1 N1 169.97(10) . . ?
N7 Mn1 N1 89.64(8) 6_556 . ?
N7 Mn1 N1 93.30(8) . . ?
N6 Mn1 N1 90.07(9) 5 . ?
N3 Mn1 N1 80.56(8) . . ?
C1 N1 C5 115.1(2) . . ?
C1 N1 Mn1 120.04(19) . . ?
C5 N1 Mn1 124.87(18) . . ?
N3 N2 C7 113.8(3) . . ?
N3 N2 C6 119.1(2) . . ?
C7 N2 C6 127.0(3) . . ?
C9 N3 N2 107.9(3) . . ?
C9 N3 Mn1 125.0(2) . . ?
N2 N3 Mn1 123.57(18) . . ?
N5 N4 Mn1 135.6(2) . . ?
N4 N5 N6 176.7(3) . . ?
N5 N6 Mn1 125.0(2) . 5 ?
N8 N7 Mn1 129.1(2) . 6_556 ?
N8 N7 Mn1 128.2(2) . . ?
Mn1 N7 Mn1 101.96(9) 6_556 . ?
N9 N8 N7 178.5(3) . . ?
C2 C1 N1 123.5(3) . . ?
C3 C2 C1 120.7(4) . . ?
C2 C3 C4 119.7(4) . . ?
C3 C4 C5 119.8(3) . . ?
N1 C5 C4 121.3(3) . . ?
N1 C5 C6 117.8(2) . . ?
C4 C5 C6 121.0(3) . . ?
N2 C6 C5 111.5(2) . . ?
N2 C7 C8 105.1(3) . . ?
C9 C8 C7 102.1(3) . . ?
N3 C9 C8 111.1(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 N4 2.218(3) . ?
Mn1 N7 2.225(2) 6_556 ?
Mn1 N7 2.230(2) . ?
Mn1 N6 2.240(3) 5 ?
Mn1 N3 2.270(2) . ?
Mn1 N1 2.303(2) . ?
N1 C1 1.337(4) . ?
N1 C5 1.342(3) . ?
N2 N3 1.344(3) . ?
N2 C7 1.363(4) . ?
N2 C6 1.467(4) . ?
N3 C9 1.336(4) . ?
N4 N5 1.166(3) . ?
N5 N6 1.169(3) . ?
N6 Mn1 2.240(3) 5 ?
N7 N8 1.182(3) . ?
N7 Mn1 2.225(2) 6_556 ?
N8 N9 1.153(4) . ?
C1 C2 1.328(5) . ?
C2 C3 1.289(5) . ?
C3 C4 1.321(5) . ?
C4 C5 1.372(4) . ?
C5 C6 1.494(4) . ?
C7 C8 1.503(7) . ?
C8 C9 1.460(6) . ?
