#------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/51/26/1512622.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_1512622
loop_
_publ_author_name
'Xiu-Mei Zhang'
'Wei Gao'
'Jie-Ping Liu'
'En-Qing Gao'
_publ_section_title
;
 Mixed-bridging manganese(II) and copper(II) complexes with azide and
 pyridylbenzoate N-oxide: Structures and magnetic properties
;
_journal_name_full
;
Inorganica Chimica Acta
;
_journal_page_first              311
_journal_page_last               316
_journal_paper_doi               10.1016/j.ica.2012.03.050
_journal_volume                  392
_journal_year                    2012
_chemical_formula_sum            'C12 H8 Mn N4 O3'
_chemical_formula_weight         311.16
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 100.8140(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.1675(2)
_cell_length_b                   23.4539(6)
_cell_length_c                   6.5517(2)
_cell_measurement_reflns_used    9685
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.24
_cell_measurement_theta_min      2.54
_cell_volume                     1232.75(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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    0.0144
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            16575
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.74
_exptl_absorpt_coefficient_mu    1.083
_exptl_absorpt_correction_T_max  0.9183
_exptl_absorpt_correction_T_min  0.8125
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.677
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             628
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.416
_refine_diff_density_min         -0.288
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         2984
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0319
_refine_ls_R_factor_gt           0.0290
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0366P)²+0.6109P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0747
_refine_ls_wR_factor_ref         0.0767
_reflns_number_gt                2758
_reflns_number_total             2984
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2012-392-311-316-1.cif
_cod_data_source_block           submission
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               1512622
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
Mn1 Mn 0.41932(3) 0.744531(9) 1.00284(3) 0.02477(9) Uani 1 1 d .
C1 C 0.40195(19) 0.86076(6) 1.2393(2) 0.0266(3) Uani 1 1 d .
C2 C 0.35073(19) 0.92161(6) 1.1931(2) 0.0264(3) Uani 1 1 d .
C3 C 0.3164(2) 0.94048(7) 0.9893(3) 0.0331(4) Uani 1 1 d .
H3A H 0.3251 0.9154 0.8820 0.040 Uiso 1 1 calc R
C4 C 0.2691(2) 0.99637(7) 0.9439(3) 0.0350(4) Uani 1 1 d .
H4A H 0.2440 1.0083 0.8062 0.042 Uiso 1 1 calc R
C5 C 0.2587(2) 1.03486(7) 1.1024(3) 0.0286(3) Uani 1 1 d .
C6 C 0.2910(3) 1.01577(7) 1.3063(3) 0.0385(4) Uani 1 1 d .
H6A H 0.2828 1.0409 1.4136 0.046 Uiso 1 1 calc R
C7 C 0.3353(2) 0.95955(7) 1.3515(3) 0.0358(4) Uani 1 1 d .
H7A H 0.3548 0.9471 1.4886 0.043 Uiso 1 1 calc R
C8 C 0.2168(2) 1.09548(7) 1.0514(3) 0.0286(3) Uani 1 1 d .
C9 C 0.0851(2) 1.11065(8) 0.8948(3) 0.0351(4) Uani 1 1 d .
H9A H 0.0201 1.0826 0.8183 0.042 Uiso 1 1 calc R
C10 C 0.0509(2) 1.16772(8) 0.8529(3) 0.0376(4) Uani 1 1 d .
H10A H -0.0401 1.1782 0.7521 0.045 Uiso 1 1 calc R
C11 C 0.1517(2) 1.20874(7) 0.9604(3) 0.0325(3) Uani 1 1 d .
H11A H 0.1292 1.2471 0.9331 0.039 Uiso 1 1 calc R
C12 C 0.3154(2) 1.13821(7) 1.1564(2) 0.0279(3) Uani 1 1 d .
H12A H 0.4040 1.1289 1.2624 0.034 Uiso 1 1 calc R
N1 N 0.28346(17) 1.19313(5) 1.1057(2) 0.0263(3) Uani 1 1 d .
N2 N 0.24379(18) 0.73096(6) 1.2149(2) 0.0318(3) Uani 1 1 d .
N3 N 0.14795(18) 0.69167(7) 1.1944(2) 0.0346(3) Uani 1 1 d .
N4 N 0.0525(3) 0.65528(10) 1.1714(3) 0.0627(5) Uani 1 1 d .
O1 O 0.43058(17) 0.83138(5) 1.09067(19) 0.0355(3) Uani 1 1 d .
O2 O 0.41182(17) 0.84305(5) 1.42299(19) 0.0359(3) Uani 1 1 d .
O3 O 0.38921(15) 1.23466(5) 1.19304(18) 0.0289(2) 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'
O O 0.0106 0.0060 '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
O1 Mn1 O2 178.43(5) . 4_575
O1 Mn1 N2 88.15(5) . .
O2 Mn1 N2 91.36(5) 4_575 .
O1 Mn1 N2 88.28(5) . 4_575
O2 Mn1 N2 93.27(5) 4_575 4_575
N2 Mn1 N2 100.41(6) . 4_575
O1 Mn1 O3 86.96(4) . 3_677
O2 Mn1 O3 93.46(5) 4_575 3_677
N2 Mn1 O3 174.32(5) . 3_677
N2 Mn1 O3 82.33(5) 4_575 3_677
O1 Mn1 O3 82.73(5) . 2_647
O2 Mn1 O3 95.72(4) 4_575 2_647
N2 Mn1 O3 81.73(5) . 2_647
N2 Mn1 O3 170.71(5) 4_575 2_647
O3 Mn1 O3 94.78(5) 3_677 2_647
O1 C1 O2 125.02(15) . .
O1 C1 C2 116.89(14) . .
O2 C1 C2 118.09(14) . .
C3 C2 C7 119.00(14) . .
C3 C2 C1 119.78(14) . .
C7 C2 C1 121.22(14) . .
C4 C3 C2 120.55(15) . .
C4 C3 H3A 119.7 . .
C2 C3 H3A 119.7 . .
C3 C4 C5 120.56(15) . .
C3 C4 H4A 119.7 . .
C5 C4 H4A 119.7 . .
C6 C5 C4 118.85(15) . .
C6 C5 C8 121.34(15) . .
C4 C5 C8 119.80(15) . .
C7 C6 C5 120.57(16) . .
C7 C6 H6A 119.7 . .
C5 C6 H6A 119.7 . .
C6 C7 C2 120.42(15) . .
C6 C7 H7A 119.8 . .
C2 C7 H7A 119.8 . .
C12 C8 C9 118.68(15) . .
C12 C8 C5 119.52(14) . .
C9 C8 C5 121.74(15) . .
C10 C9 C8 119.63(16) . .
C10 C9 H9A 120.2 . .
C8 C9 H9A 120.2 . .
C11 C10 C9 119.80(16) . .
C11 C10 H10A 120.1 . .
C9 C10 H10A 120.1 . .
N1 C11 C10 119.69(15) . .
N1 C11 H11A 120.2 . .
C10 C11 H11A 120.2 . .
N1 C12 C8 120.19(14) . .
N1 C12 H12A 119.9 . .
C8 C12 H12A 119.9 . .
C12 N1 C11 121.87(14) . .
C12 N1 O3 120.38(13) . .
C11 N1 O3 117.67(13) . .
N3 N2 Mn1 121.96(12) . .
N3 N2 Mn1 126.67(11) . 4_576
Mn1 N2 Mn1 96.07(6) . 4_576
N4 N3 N2 177.8(2) . .
C1 O1 Mn1 137.57(11) . .
C1 O2 Mn1 123.29(10) . 4_576
N1 O3 Mn1 111.74(9) . 3_677
N1 O3 Mn1 135.51(9) . 2_657
Mn1 O3 Mn1 92.28(4) 3_677 2_657
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mn1 O1 2.1140(11) .
Mn1 O2 2.1178(12) 4_575
Mn1 N2 2.1986(14) .
Mn1 N2 2.2204(14) 4_575
Mn1 O3 2.2548(12) 3_677
Mn1 O3 2.3022(12) 2_647
C1 O1 1.2503(19) .
C1 O2 1.2614(19) .
C1 C2 1.502(2) .
C2 C3 1.384(2) .
C2 C7 1.391(2) .
C3 C4 1.383(2) .
C3 H3A 0.9300 .
C4 C5 1.391(2) .
C4 H4A 0.9300 .
C5 C6 1.386(2) .
C5 C8 1.486(2) .
C6 C7 1.385(2) .
C6 H6A 0.9300 .
C7 H7A 0.9300 .
C8 C12 1.385(2) .
C8 C9 1.387(2) .
C9 C10 1.384(3) .
C9 H9A 0.9300 .
C10 C11 1.372(3) .
C10 H10A 0.9300 .
C11 N1 1.347(2) .
C11 H11A 0.9300 .
C12 N1 1.343(2) .
C12 H12A 0.9300 .
N1 O3 1.3553(17) .
N2 N3 1.200(2) .
N2 Mn1 2.2204(14) 4_576
N3 N4 1.147(2) .
O2 Mn1 2.1178(12) 4_576
O3 Mn1 2.2548(12) 3_677
O3 Mn1 2.3022(12) 2_657
