#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/20/2212024.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2212024
loop_
_publ_author_name
'Xiao-Li Yu'
'Yong Fang'
'Cui-Ying Huang'
'Yuan-Peng Gu'
'Wan-Sheng You'
_publ_section_title
Bis(dicyanamido-κN)(di-2-pyridylamine-κ²N,N')zinc(II)
_journal_coeditor_code           BI2122
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m358
_journal_page_last               m359
_journal_paper_doi               10.1107/S1600536806055747
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '[Zn (C2 N3)2 (C10 H9 N3)2]'
_chemical_formula_moiety         'C24 H18 N12 Zn'
_chemical_formula_sum            'C24 H18 N12 Zn'
_chemical_formula_weight         539.89
_chemical_name_systematic
;
Bis(dicyanamidato-\kN)(di-2-pyridylamine-κ²N,N')zinc(II)
;
_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                90.00
_cell_angle_beta                 94.549(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.6474(11)
_cell_length_b                   13.5964(18)
_cell_length_c                   21.632(3)
_cell_measurement_reflns_used    3872
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.21
_cell_measurement_theta_min      1.00
_cell_volume                     2535.3(6)
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1997b)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997a)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997a)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX2 CCD'
_diffrn_measurement_method       ω
_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  0.0449
_diffrn_reflns_av_sigmaI/netI    0.0609
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            7391
_diffrn_reflns_theta_full        27.32
_diffrn_reflns_theta_max         27.32
_diffrn_reflns_theta_min         2.80
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.007
_exptl_absorpt_correction_T_max  0.906
_exptl_absorpt_correction_T_min  0.752
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.414
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1104
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.313
_refine_diff_density_min         -0.259
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     168
_refine_ls_number_reflns         2836
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0797
_refine_ls_R_factor_gt           0.0441
_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)+(0.0478P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0941
_refine_ls_wR_factor_ref         0.1080
_reflns_number_gt                1840
_reflns_number_total             2836
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            bi2122.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2212024
_cod_database_fobs_code          2212024
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_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
Zn Zn1 0.0000 0.36207(4) 0.2500 0.04165(18) Uani d S 1
N N1 -0.1186(3) 0.46817(18) 0.19043(10) 0.0444(6) Uani d . 1
N N2 -0.0311(3) 0.39874(19) 0.09911(10) 0.0506(7) Uani d . 1
H H2B -0.0667 0.3766 0.0635 0.061 Uiso calc R 1
N N3 0.1637(3) 0.36217(18) 0.17850(10) 0.0459(6) Uani d . 1
N N4 0.1350(3) 0.2507(2) 0.30072(11) 0.0524(7) Uani d . 1
N N5 0.2619(5) 0.1225(2) 0.36359(15) 0.0952(12) Uani d . 1
N N6 0.3854(4) 0.1240(3) 0.46720(14) 0.0980(12) Uani d . 1
C C1 -0.1317(3) 0.4580(2) 0.12882(13) 0.0451(7) Uani d . 1
C C2 -0.2484(4) 0.5057(3) 0.09182(14) 0.0625(9) Uani d . 1
H H2A -0.2589 0.4948 0.0493 0.075 Uiso calc R 1
C C3 -0.3458(5) 0.5678(3) 0.11817(18) 0.0815(12) Uani d . 1
H H3A -0.4235 0.6002 0.0939 0.098 Uiso calc R 1
C C4 -0.3286(4) 0.5826(3) 0.18223(17) 0.0735(11) Uani d . 1
H H4A -0.3928 0.6258 0.2015 0.088 Uiso calc R 1
C C5 -0.2155(4) 0.5319(2) 0.21532(14) 0.0591(9) Uani d . 1
H H5A -0.2040 0.5417 0.2580 0.071 Uiso calc R 1
C C6 0.1178(3) 0.3700(2) 0.11811(13) 0.0468(7) Uani d . 1
C C7 0.2145(4) 0.3473(3) 0.07186(15) 0.0661(10) Uani d . 1
H H7A 0.1775 0.3499 0.0303 0.079 Uiso calc R 1
C C8 0.3649(5) 0.3212(3) 0.08821(18) 0.0867(13) Uani d . 1
H H8A 0.4316 0.3056 0.0580 0.104 Uiso calc R 1
C C9 0.4165(4) 0.3185(4) 0.15046(18) 0.0866(13) Uani d . 1
H H9A 0.5193 0.3036 0.1628 0.104 Uiso calc R 1
C C10 0.3140(4) 0.3378(3) 0.19263(15) 0.0664(10) Uani d . 1
H H10A 0.3490 0.3342 0.2343 0.080 Uiso calc R 1
C C11 0.1953(4) 0.1947(2) 0.33352(14) 0.0492(8) Uani d . 1
C C12 0.3235(4) 0.1290(3) 0.41984(15) 0.0613(9) Uani d . 1
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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N1 Zn1 N1 2 . 95.27(12) y
N1 Zn1 N4 2 2 173.16(9) ?
N1 Zn1 N4 . 2 87.30(9) y
N1 Zn1 N4 2 . 87.30(9) ?
N1 Zn1 N4 . . 173.16(9) y
N4 Zn1 N4 2 . 90.88(13) y
N1 Zn1 N3 2 . 96.89(9) y
N1 Zn1 N3 . . 83.07(9) y
N4 Zn1 N3 2 . 89.72(9) y
N4 Zn1 N3 . . 90.33(9) y
N1 Zn1 N3 2 2 83.07(9) ?
N1 Zn1 N3 . 2 96.89(9) ?
N4 Zn1 N3 2 2 90.33(9) ?
N4 Zn1 N3 . 2 89.72(9) ?
N3 Zn1 N3 . 2 179.93(13) y
C1 N1 C5 . . 117.3(2) ?
C1 N1 Zn1 . . 121.98(19) ?
C5 N1 Zn1 . . 118.43(19) ?
C6 N2 C1 . . 129.4(2) ?
C6 N2 H2B . . 115.3 ?
C1 N2 H2B . . 115.3 ?
C6 N3 C10 . . 116.4(3) ?
C6 N3 Zn1 . . 122.27(19) ?
C10 N3 Zn1 . . 120.4(2) ?
C11 N4 Zn1 . . 171.4(3) ?
C11 N5 C12 . . 123.9(3) ?
N1 C1 N2 . . 121.2(2) ?
N1 C1 C2 . . 121.6(3) ?
N2 C1 C2 . . 117.2(3) ?
C3 C2 C1 . . 119.7(3) ?
C3 C2 H2A . . 120.2 ?
C1 C2 H2A . . 120.2 ?
C2 C3 C4 . . 119.2(3) ?
C2 C3 H3A . . 120.4 ?
C4 C3 H3A . . 120.4 ?
C5 C4 C3 . . 117.8(3) ?
C5 C4 H4A . . 121.1 ?
C3 C4 H4A . . 121.1 ?
N1 C5 C4 . . 124.2(3) ?
N1 C5 H5A . . 117.9 ?
C4 C5 H5A . . 117.9 ?
N3 C6 N2 . . 120.8(3) ?
N3 C6 C7 . . 122.4(3) ?
N2 C6 C7 . . 116.8(3) ?
C8 C7 C6 . . 119.1(3) ?
C8 C7 H7A . . 120.5 ?
C6 C7 H7A . . 120.5 ?
C7 C8 C9 . . 119.0(3) ?
C7 C8 H8A . . 120.5 ?
C9 C8 H8A . . 120.5 ?
C10 C9 C8 . . 118.3(3) ?
C10 C9 H9A . . 120.8 ?
C8 C9 H9A . . 120.8 ?
C9 C10 N3 . . 124.5(3) ?
C9 C10 H10A . . 117.7 ?
N3 C10 H10A . . 117.7 ?
N4 C11 N5 . . 171.4(3) ?
N6 C12 N5 . . 171.5(4) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Zn1 N1 2 2.141(2) ?
Zn1 N1 . 2.141(2) y
Zn1 N4 2 2.157(3) ?
Zn1 N4 . 2.157(3) y
Zn1 N3 . 2.178(2) y
Zn1 N3 2 2.178(2) ?
N1 C1 . 1.336(3) ?
N1 C5 . 1.347(4) ?
N2 C6 . 1.377(4) ?
N2 C1 . 1.381(4) ?
N2 H2B . 0.860 ?
N3 C6 . 1.339(3) ?
N3 C10 . 1.353(4) ?
N4 C11 . 1.139(4) ?
N5 C11 . 1.288(4) ?
N5 C12 . 1.292(4) ?
N6 C12 . 1.120(4) ?
C1 C2 . 1.397(4) ?
C2 C3 . 1.350(5) ?
C2 H2A . 0.930 ?
C3 C4 . 1.397(5) ?
C3 H3A . 0.930 ?
C4 C5 . 1.354(4) ?
C4 H4A . 0.930 ?
C5 H5A . 0.930 ?
C6 C7 . 1.389(4) ?
C7 C8 . 1.367(5) ?
C7 H7A . 0.930 ?
C8 C9 . 1.385(5) ?
C8 H8A . 0.930 ?
C9 C10 . 1.348(5) ?
C9 H9A . 0.930 ?
C10 H10A . 0.930 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
N2 H2B N6 8_455 0.86 2.09 2.904(4) 157.0
