#------------------------------------------------------------------------------
#$Date: 2016-03-26 16:38:37 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180347 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/16/7201605.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_7201605
loop_
_publ_author_name
'Yue, Yan-Feng'
'Gao, En-Qing'
'Fang, Chen-Jie'
'Zheng, Tao'
'Liang, Jue'
'Yan, Chun-Hua'
_publ_section_title
;
 The crystal structures of four azido-bridged Zn(ii) complexes based on
 open-chain diazine Schiff-base ligands
;
_journal_issue                   5
_journal_name_full               CrystEngComm
_journal_page_first              614
_journal_paper_doi               10.1039/b711831g
_journal_volume                  10
_journal_year                    2008
_chemical_formula_sum            'C13 H13 N14 Zn2'
_chemical_formula_weight         496.11
_chemical_name_systematic
;
?
;
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 117.949(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.6683(2)
_cell_length_b                   10.2683(2)
_cell_length_c                   18.9476(7)
_cell_measurement_reflns_used    39057
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      3.395
_cell_volume                     1833.53(10)
_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 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0705
_diffrn_reflns_av_sigmaI/netI    0.0524
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            31994
_diffrn_reflns_theta_full        27.46
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_min         3.54
_exptl_absorpt_coefficient_mu    2.651
_exptl_absorpt_correction_T_max  0.790
_exptl_absorpt_correction_T_min  0.510
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(Blessing, 1995, 1997)'
_exptl_crystal_colour            'Light yellow'
_exptl_crystal_density_diffrn    1.797
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             996
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.884
_refine_diff_density_min         -0.994
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         4168
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0770
_refine_ls_R_factor_gt           0.0457
_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)+(0.0696P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1194
_refine_ls_wR_factor_ref         0.1266
_reflns_number_gt                2744
_reflns_number_total             4168
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b711831g.txt
_cod_data_source_block           1
_cod_original_cell_volume        1833.53(8)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7201605
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.00486(4) 0.83871(4) 0.39909(3) 0.04061(17) Uani 1 1 d . . .
Zn2 Zn -0.35421(5) 1.01360(5) 0.48428(3) 0.04301(17) Uani 1 1 d . . .
C1 C 0.2206(4) 0.6305(4) 0.5095(3) 0.0549(12) Uani 1 1 d . . .
H1A H 0.2634 0.6417 0.4770 0.066 Uiso 1 1 calc R . .
C2 C 0.2742(5) 0.5382(5) 0.5689(3) 0.0633(13) Uani 1 1 d . . .
H2A H 0.3528 0.4890 0.5766 0.076 Uiso 1 1 calc R . .
C3 C 0.2120(5) 0.5194(5) 0.6159(3) 0.0648(14) Uani 1 1 d . . .
H3A H 0.2476 0.4571 0.6562 0.078 Uiso 1 1 calc R . .
C4 C 0.0938(5) 0.5942(4) 0.6037(3) 0.0524(11) Uani 1 1 d . . .
H4A H 0.0488 0.5818 0.6350 0.063 Uiso 1 1 calc R . .
C5 C 0.0456(4) 0.6874(4) 0.5437(2) 0.0382(9) Uani 1 1 d . . .
C6 C -0.0761(4) 0.7731(4) 0.5274(2) 0.0387(9) Uani 1 1 d . . .
C7 C -0.2273(4) 1.0044(4) 0.3779(2) 0.0372(9) Uani 1 1 d . . .
C8 C -0.3467(4) 1.0982(4) 0.3403(2) 0.0371(8) Uani 1 1 d . . .
C9 C -0.3796(5) 1.1618(4) 0.2688(3) 0.0555(11) Uani 1 1 d . . .
H9A H -0.3248 1.1501 0.2430 0.067 Uiso 1 1 calc R . .
C10 C -0.4980(5) 1.2437(5) 0.2374(3) 0.0673(14) Uani 1 1 d . . .
H10A H -0.5217 1.2892 0.1904 0.081 Uiso 1 1 calc R . .
C11 C -0.5784(5) 1.2571(5) 0.2749(3) 0.0613(13) Uani 1 1 d . . .
H11A H -0.6590 1.3094 0.2531 0.074 Uiso 1 1 calc R . .
C12 C -0.5393(4) 1.1926(4) 0.3454(3) 0.0532(11) Uani 1 1 d . . .
H12A H -0.5942 1.2032 0.3713 0.064 Uiso 1 1 calc R . .
C13 C -0.1456(5) 0.7611(5) 0.5796(3) 0.0582(12) Uani 1 1 d . . .
H13A H -0.2227 0.8219 0.5624 0.087 Uiso 1 1 calc R . .
H13B H -0.0776 0.7794 0.6339 0.087 Uiso 1 1 calc R . .
H13C H -0.1813 0.6742 0.5760 0.087 Uiso 1 1 calc R . .
N1 N 0.1084(3) 0.7052(3) 0.4967(2) 0.0422(8) Uani 1 1 d . . .
N2 N -0.1099(3) 0.8487(3) 0.46743(19) 0.0403(8) Uani 1 1 d . . .
N3 N -0.2210(3) 0.9374(3) 0.44087(19) 0.0381(7) Uani 1 1 d . . .
N4 N -0.4247(3) 1.1144(3) 0.37886(19) 0.0393(7) Uani 1 1 d . . .
N5 N -0.1347(4) 0.9875(3) 0.3503(2) 0.0457(8) Uani 1 1 d . . .
N6 N -0.0554(4) 0.7130(4) 0.3079(2) 0.0624(11) Uani 1 1 d . . .
N7 N 0.0248(5) 0.6414(4) 0.3003(2) 0.0640(11) Uani 1 1 d . . .
N8 N 0.1004(7) 0.5707(6) 0.2919(4) 0.110(2) Uani 1 1 d . . .
N9 N 0.1966(3) 0.9148(3) 0.4126(2) 0.0420(8) Uani 1 1 d . . .
N10 N 0.2166(4) 0.9139(4) 0.3547(2) 0.0488(9) Uani 1 1 d . . .
N11 N 0.2356(5) 0.9150(6) 0.3013(3) 0.0865(15) Uani 1 1 d . . .
N12 N -0.4853(3) 0.8763(4) 0.4853(2) 0.0473(9) Uani 1 1 d . . .
N13 N -0.5028(4) 0.7665(4) 0.4584(2) 0.0552(10) Uani 1 1 d . . .
N14 N -0.5256(5) 0.6632(5) 0.4347(4) 0.0932(17) 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'
Zn Zn 0.2839 1.4301 '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
N6 Zn1 N5 102.81(16) . . ?
N6 Zn1 N9 104.24(15) . . ?
N5 Zn1 N9 103.98(13) . . ?
N6 Zn1 N1 99.14(16) . . ?
N5 Zn1 N1 147.69(14) . . ?
N9 Zn1 N1 93.12(13) . . ?
N6 Zn1 N2 120.25(15) . . ?
N5 Zn1 N2 74.72(13) . . ?
N9 Zn1 N2 134.86(12) . . ?
N1 Zn1 N2 73.81(12) . . ?
N12 Zn2 N9 121.07(15) . 3_576 ?
N12 Zn2 N4 115.31(14) . . ?
N9 Zn2 N4 121.01(13) 3_576 . ?
N12 Zn2 N3 110.35(13) . . ?
N9 Zn2 N3 96.02(13) 3_576 . ?
N4 Zn2 N3 79.22(12) . . ?
N12 Zn2 N12 74.99(16) . 3_476 ?
N9 Zn2 N12 87.68(13) 3_576 3_476 ?
N4 Zn2 N12 91.11(13) . 3_476 ?
N3 Zn2 N12 170.22(13) . 3_476 ?
N1 C1 C2 122.3(4) . . ?
C3 C2 C1 119.6(4) . . ?
C2 C3 C4 119.7(5) . . ?
C5 C4 C3 118.1(5) . . ?
N1 C5 C4 121.7(4) . . ?
N1 C5 C6 116.1(3) . . ?
C4 C5 C6 122.2(4) . . ?
N2 C6 C5 113.6(4) . . ?
N2 C6 C13 128.1(4) . . ?
C5 C6 C13 118.3(4) . . ?
N5 C7 N3 122.8(4) . . ?
N5 C7 C8 121.7(4) . . ?
N3 C7 C8 115.5(3) . . ?
N4 C8 C9 122.1(4) . . ?
N4 C8 C7 115.3(3) . . ?
C9 C8 C7 122.6(4) . . ?
C8 C9 C10 117.5(4) . . ?
C11 C10 C9 120.5(4) . . ?
C10 C11 C12 119.0(4) . . ?
N4 C12 C11 122.8(4) . . ?
C1 N1 C5 118.5(4) . . ?
C1 N1 Zn1 125.1(3) . . ?
C5 N1 Zn1 116.1(2) . . ?
C6 N2 N3 123.8(3) . . ?
C6 N2 Zn1 120.0(3) . . ?
N3 N2 Zn1 116.2(2) . . ?
C7 N3 N2 109.6(3) . . ?
C7 N3 Zn2 113.2(2) . . ?
N2 N3 Zn2 136.2(3) . . ?
C12 N4 C8 118.2(3) . . ?
C12 N4 Zn2 126.6(3) . . ?
C8 N4 Zn2 115.3(2) . . ?
C7 N5 Zn1 116.2(3) . . ?
N7 N6 Zn1 123.0(3) . . ?
N8 N7 N6 178.7(6) . . ?
N10 N9 Zn2 117.2(3) . 3_576 ?
N10 N9 Zn1 117.6(3) . . ?
Zn2 N9 Zn1 125.15(17) 3_576 . ?
N11 N10 N9 179.0(5) . . ?
N13 N12 Zn2 128.5(3) . . ?
N13 N12 Zn2 124.4(3) . 3_476 ?
Zn2 N12 Zn2 105.01(16) . 3_476 ?
N14 N13 N12 175.8(5) . . ?
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
Zn1 N6 2.007(4) . ?
Zn1 N5 2.028(3) . ?
Zn1 N9 2.090(3) . ?
Zn1 N1 2.145(3) . ?
Zn1 N2 2.161(3) . ?
Zn2 N12 1.992(4) . ?
Zn2 N9 2.026(3) 3_576 ?
Zn2 N4 2.054(3) . ?
Zn2 N3 2.098(3) . ?
Zn2 N12 2.338(3) 3_476 ?
C1 N1 1.345(5) . ?
C1 C2 1.374(7) . ?
C2 C3 1.352(8) . ?
C3 C4 1.400(6) . ?
C4 C5 1.388(6) . ?
C5 N1 1.354(5) . ?
C5 C6 1.477(5) . ?
C6 N2 1.281(5) . ?
C6 C13 1.494(6) . ?
C7 N5 1.329(5) . ?
C7 N3 1.351(5) . ?
C7 C8 1.486(5) . ?
C8 N4 1.349(5) . ?
C8 C9 1.393(6) . ?
C9 C10 1.397(6) . ?
C10 C11 1.352(7) . ?
C11 C12 1.370(7) . ?
C12 N4 1.347(5) . ?
N2 N3 1.389(4) . ?
N6 N7 1.187(6) . ?
N7 N8 1.150(6) . ?
N9 N10 1.212(5) . ?
N9 Zn2 2.026(3) 3_576 ?
N10 N11 1.122(6) . ?
N12 N13 1.215(5) . ?
N12 Zn2 2.338(3) 3_476 ?
N13 N14 1.134(6) . ?
