#------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/51/26/1512623.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_1512623
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 Cu N4 O3'
_chemical_formula_weight         319.76
_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                 94.6930(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.9405(3)
_cell_length_b                   6.3841(2)
_cell_length_c                   23.4650(7)
_cell_measurement_reflns_used    7557
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.17
_cell_measurement_theta_min      2.57
_cell_volume                     1185.52(7)
_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 0.962
_diffrn_measured_fraction_theta_max 0.962
_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  0.0260
_diffrn_reflns_av_sigmaI/netI    0.0204
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            15500
_diffrn_reflns_theta_full        28.29
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         1.74
_exptl_absorpt_coefficient_mu    1.855
_exptl_absorpt_correction_T_max  0.8362
_exptl_absorpt_correction_T_min  0.6060
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.792
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             644
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.383
_refine_diff_density_min         -0.297
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         2844
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0300
_refine_ls_R_factor_gt           0.0259
_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)+(0.0420P)²+0.4095P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0709
_refine_ls_wR_factor_ref         0.0734
_reflns_number_gt                2548
_reflns_number_total             2844
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2012-392-311-316-2.cif
_cod_data_source_block           2
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               1512623
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
Cu1 Cu 0.02425(3) 0.55225(3) 0.245925(8) 0.02354(9) Uani 1 1 d .
C1 C 0.0624(2) 0.3049(2) 0.35375(7) 0.0216(3) Uani 1 1 d .
C2 C 0.1222(2) 0.3242(3) 0.41596(7) 0.0224(3) Uani 1 1 d .
C3 C 0.1430(3) 0.1522(3) 0.45200(8) 0.0318(4) Uani 1 1 d .
H3A H 0.1158 0.0189 0.4381 0.038 Uiso 1 1 calc R
C4 C 0.2040(3) 0.1777(3) 0.50858(8) 0.0332(4) Uani 1 1 d .
H4A H 0.2180 0.0609 0.5322 0.040 Uiso 1 1 calc R
C5 C 0.2449(2) 0.3751(3) 0.53070(7) 0.0248(3) Uani 1 1 d .
C6 C 0.2236(3) 0.5466(3) 0.49429(8) 0.0301(4) Uani 1 1 d .
H6A H 0.2503 0.6800 0.5082 0.036 Uiso 1 1 calc R
C7 C 0.1638(3) 0.5218(3) 0.43793(8) 0.0281(4) Uani 1 1 d .
H7A H 0.1509 0.6385 0.4143 0.034 Uiso 1 1 calc R
C8 C 0.3095(2) 0.4082(3) 0.59122(7) 0.0252(3) Uani 1 1 d .
C9 C 0.2493(2) 0.2892(3) 0.63469(7) 0.0263(4) Uani 1 1 d .
H9A H 0.1697 0.1850 0.6257 0.032 Uiso 1 1 calc R
C10 C 0.4253(2) 0.4692(3) 0.70385(8) 0.0295(4) Uani 1 1 d .
H10A H 0.4657 0.4870 0.7419 0.035 Uiso 1 1 calc R
C11 C 0.4872(2) 0.5905(3) 0.66249(8) 0.0331(4) Uani 1 1 d .
H11A H 0.5685 0.6919 0.6724 0.040 Uiso 1 1 calc R
C12 C 0.4292(2) 0.5628(3) 0.60572(8) 0.0313(4) Uani 1 1 d .
H12A H 0.4698 0.6467 0.5775 0.038 Uiso 1 1 calc R
O1 O 0.07316(18) 0.46944(19) 0.32512(5) 0.0300(3) Uani 1 1 d .
O2 O 0.01064(17) 0.12951(19) 0.33535(5) 0.0282(3) Uani 1 1 d .
O3 O 0.24170(17) 0.2158(2) 0.73121(5) 0.0354(3) Uani 1 1 d .
N1 N 0.30525(18) 0.3228(2) 0.68982(6) 0.0260(3) Uani 1 1 d .
N2 N 0.14239(18) 0.8191(2) 0.26645(6) 0.0230(3) Uani 1 1 d .
N3 N 0.24418(19) 0.8423(2) 0.30771(7) 0.0277(3) Uani 1 1 d .
N4 N 0.3433(2) 0.8717(3) 0.34490(8) 0.0420(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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 '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 Cu1 O2 176.27(6) . 2
O1 Cu1 N2 87.01(6) . .
O2 Cu1 N2 92.65(6) 2 .
O1 Cu1 N2 90.83(6) . 2_545
O2 Cu1 N2 90.39(6) 2 2_545
N2 Cu1 N2 165.77(4) . 2_545
O1 C1 O2 126.66(16) . .
O1 C1 C2 114.96(14) . .
O2 C1 C2 118.36(14) . .
C3 C2 C7 118.59(16) . .
C3 C2 C1 122.66(15) . .
C7 C2 C1 118.71(15) . .
C4 C3 C2 120.39(16) . .
C4 C3 H3A 119.8 . .
C2 C3 H3A 119.8 . .
C3 C4 C5 121.11(16) . .
C3 C4 H4A 119.4 . .
C5 C4 H4A 119.4 . .
C6 C5 C4 118.11(16) . .
C6 C5 C8 119.38(16) . .
C4 C5 C8 122.51(16) . .
C7 C6 C5 120.96(16) . .
C7 C6 H6A 119.5 . .
C5 C6 H6A 119.5 . .
C6 C7 C2 120.83(16) . .
C6 C7 H7A 119.6 . .
C2 C7 H7A 119.6 . .
C9 C8 C12 118.52(16) . .
C9 C8 C5 120.81(16) . .
C12 C8 C5 120.66(16) . .
N1 C9 C8 120.74(16) . .
N1 C9 H9A 119.6 . .
C8 C9 H9A 119.6 . .
N1 C10 C11 120.37(17) . .
N1 C10 H10A 119.8 . .
C11 C10 H10A 119.8 . .
C10 C11 C12 120.04(18) . .
C10 C11 H11A 120.0 . .
C12 C11 H11A 120.0 . .
C11 C12 C8 119.51(17) . .
C11 C12 H12A 120.2 . .
C8 C12 H12A 120.2 . .
C1 O1 Cu1 136.42(11) . .
C1 O2 Cu1 124.92(11) . 2_545
O3 N1 C9 120.44(15) . .
O3 N1 C10 118.77(15) . .
C9 N1 C10 120.78(15) . .
N3 N2 Cu1 124.51(11) . .
N3 N2 Cu1 114.43(11) . 2
Cu1 N2 Cu1 108.06(7) . 2
N4 N3 N2 176.58(19) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O1 1.9405(12) .
Cu1 O2 1.9673(12) 2
Cu1 N2 1.9850(14) .
Cu1 N2 1.9969(14) 2_545
C1 O1 1.2535(19) .
C1 O2 1.257(2) .
C1 C2 1.503(2) .
C2 C3 1.388(2) .
C2 C7 1.392(2) .
C3 C4 1.385(3) .
C3 H3A 0.9300 .
C4 C5 1.391(3) .
C4 H4A 0.9300 .
C5 C6 1.390(3) .
C5 C8 1.485(2) .
C6 C7 1.377(3) .
C6 H6A 0.9300 .
C7 H7A 0.9300 .
C8 C9 1.388(2) .
C8 C12 1.393(3) .
C9 N1 1.350(2) .
C9 H9A 0.9300 .
C10 N1 1.356(2) .
C10 C11 1.364(3) .
C10 H10A 0.9300 .
C11 C12 1.385(3) .
C11 H11A 0.9300 .
C12 H12A 0.9300 .
O2 Cu1 1.9673(12) 2_545
O3 N1 1.3209(19) .
N2 N3 1.218(2) .
N2 Cu1 1.9969(14) 2
N3 N4 1.142(2) .
