#------------------------------------------------------------------------------
#$Date: 2016-02-18 14:25:00 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176728 $
#$URL: svn://www.crystallography.net/cod/cif/8/10/21/8102195.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_8102195
loop_
_publ_author_name
'Peng, San-Jun'
'Ping, Wei-Jun'
'Song, Liu-Bin'
_publ_section_title
;
Crystal structure of dibromo(N-ethyl-N'-pyridinylmethyleneethane-1,
2-diamino)zinc(II), ZnBr₂(C₁₀H₁₅N₃)
;
_journal_issue                   4
_journal_name_full
'Zeitschrift für Kristallographie - New Crystal Structures'
_journal_page_first              425
_journal_page_last               426
_journal_volume                  222
_journal_year                    2007
_chemical_formula_moiety         'C10 H15 Br2 N3 Zn'
_chemical_formula_structural     '[ZnBr2(C10H15N3)]'
_chemical_formula_sum            'C10 H15 Br2 N3 Zn'
_chemical_formula_weight         402.44
_chemical_name_systematic
; 
dibromo(N-ethyl-N'-pyridinylmethyleneethane-1,2-diamino)zinc(II),
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                111.791(3)
_cell_angle_beta                 96.397(2)
_cell_angle_gamma                106.341(3)
_cell_formula_units_Z            2
_cell_length_a                   8.446(3)
_cell_length_b                   8.561(3)
_cell_length_c                   11.258(3)
_cell_measurement_reflns_used    1701
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.2
_cell_measurement_theta_min      2.3
_cell_volume                     703.7(4)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'Siemens P4'
_diffrn_measurement_method       omega
_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  0.0170
_diffrn_reflns_av_sigmaI/netI    0.0358
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            3956
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         26.50
_diffrn_reflns_theta_min         2.01
_exptl_absorpt_coefficient_mu    7.402
_exptl_absorpt_correction_T_max  0.3659
_exptl_absorpt_correction_T_min  0.2928
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.899
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             392
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.526
_refine_diff_density_min         -0.514
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     146
_refine_ls_number_reflns         2841
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0451
_refine_ls_R_factor_gt           0.0328
_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)+(0.0353P)²+0.3397P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0738
_refine_ls_wR_factor_ref         0.0780
_reflns_number_gt                2296
_reflns_number_total             2841
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            1267-2121.cff
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               8102195
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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_Wyckoff_symbol
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.50611(6) 0.61408(6) 0.80172(4) 0.03650(13) Uani 1 2 i d . . .
Br1 Br 0.52237(6) 0.79946(6) 0.68145(4) 0.04656(13) Uani 1 2 i d . . .
Br2 Br 0.29146(6) 0.60800(6) 0.92429(4) 0.05000(14) Uani 1 2 i d . . .
N1 N 0.7138(4) 0.8074(4) 0.9831(3) 0.0381(7) Uani 1 2 i d . . .
N2 N 0.7015(4) 0.5072(5) 0.7924(3) 0.0429(8) Uani 1 2 i d . . .
N3 N 0.3830(4) 0.3421(4) 0.6331(3) 0.0435(8) Uani 1 2 i d . . .
H3A H 0.4088 0.3549 0.5601 0.052 Uiso 1 2 i calc R . .
C1 C 0.8362(6) 0.5905(6) 0.8815(4) 0.0458(10) Uani 1 2 i d . . .
H1 H 0.9241 0.5448 0.8796 0.055 Uiso 1 2 i calc R . .
C2 C 0.8534(5) 0.7610(6) 0.9890(4) 0.0397(9) Uani 1 2 i d . . .
C3 C 0.9969(5) 0.8623(6) 1.0916(4) 0.0482(10) Uani 1 2 i d . . .
H3 H 1.0920 0.8279 1.0931 0.058 Uiso 1 2 i calc R . .
C4 C 0.9962(6) 1.0167(6) 1.1924(4) 0.0528(11) Uani 1 2 i d . . .
H4 H 1.0910 1.0877 1.2628 0.063 Uiso 1 2 i calc R . .
C5 C 0.8540(6) 1.0627(6) 1.1867(4) 0.0517(11) Uani 1 2 i d . . .
H5 H 0.8509 1.1655 1.2533 0.062 Uiso 1 2 i calc R . .
C6 C 0.7152(5) 0.9551(6) 1.0812(4) 0.0461(10) Uani 1 2 i d . . .
H6 H 0.6188 0.9870 1.0785 0.055 Uiso 1 2 i calc R . .
C7 C 0.6638(6) 0.3292(6) 0.6882(4) 0.0556(12) Uani 1 2 i d . . .
H7A H 0.7269 0.2654 0.7166 0.067 Uiso 1 2 i calc R . .
H7B H 0.6950 0.3383 0.6100 0.067 Uiso 1 2 i calc R . .
C8 C 0.4754(6) 0.2318(6) 0.6590(4) 0.0546(12) Uani 1 2 i d . . .
H8A H 0.4421 0.1175 0.5827 0.066 Uiso 1 2 i calc R . .
H8B H 0.4477 0.2085 0.7335 0.066 Uiso 1 2 i calc R . .
C9 C 0.1956(6) 0.2532(7) 0.5998(5) 0.0647(13) Uani 1 2 i d . . .
H9A H 0.1609 0.2441 0.6769 0.078 Uiso 1 2 i calc R . .
H9B H 0.1637 0.1325 0.5312 0.078 Uiso 1 2 i calc R . .
C10 C 0.1047(7) 0.3553(8) 0.5533(6) 0.0817(17) Uani 1 2 i d . . .
H10A H 0.1290 0.4715 0.6235 0.123 Uiso 1 2 i calc R . .
H10B H -0.0156 0.2905 0.5276 0.123 Uiso 1 2 i calc R . .
H10C H 0.1425 0.3690 0.4793 0.123 Uiso 1 2 i 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'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 '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
N2 Zn1 N3 77.35(13) . . ?
N2 Zn1 N1 74.58(13) . . ?
N3 Zn1 N1 150.54(12) . . ?
N2 Zn1 Br2 131.66(9) . . ?
N3 Zn1 Br2 99.46(9) . . ?
N1 Zn1 Br2 92.58(8) . . ?
N2 Zn1 Br1 112.35(9) . . ?
N3 Zn1 Br1 99.45(9) . . ?
N1 Zn1 Br1 99.32(8) . . ?
Br2 Zn1 Br1 115.69(2) . . ?
C6 N1 C2 118.2(3) . . ?
C6 N1 Zn1 129.1(3) . . ?
C2 N1 Zn1 112.7(3) . . ?
C1 N2 C7 123.8(4) . . ?
C1 N2 Zn1 119.2(3) . . ?
C7 N2 Zn1 116.7(3) . . ?
C8 N3 C9 112.8(4) . . ?
C8 N3 Zn1 105.0(2) . . ?
C9 N3 Zn1 119.4(3) . . ?
C8 N3 H3A 106.3 . . ?
C9 N3 H3A 106.3 . . ?
Zn1 N3 H3A 106.3 . . ?
N2 C1 C2 119.1(4) . . ?
N2 C1 H1 120.5 . . ?
C2 C1 H1 120.5 . . ?
N1 C2 C3 122.3(4) . . ?
N1 C2 C1 114.3(3) . . ?
C3 C2 C1 123.3(4) . . ?
C2 C3 C4 118.6(4) . . ?
C2 C3 H3 120.7 . . ?
C4 C3 H3 120.7 . . ?
C5 C4 C3 119.0(4) . . ?
C5 C4 H4 120.5 . . ?
C3 C4 H4 120.5 . . ?
C4 C5 C6 119.3(4) . . ?
C4 C5 H5 120.3 . . ?
C6 C5 H5 120.3 . . ?
N1 C6 C5 122.6(4) . . ?
N1 C6 H6 118.7 . . ?
C5 C6 H6 118.7 . . ?
N2 C7 C8 106.9(4) . . ?
N2 C7 H7A 110.3 . . ?
C8 C7 H7A 110.3 . . ?
N2 C7 H7B 110.3 . . ?
C8 C7 H7B 110.3 . . ?
H7A C7 H7B 108.6 . . ?
N3 C8 C7 109.4(4) . . ?
N3 C8 H8A 109.8 . . ?
C7 C8 H8A 109.8 . . ?
N3 C8 H8B 109.8 . . ?
C7 C8 H8B 109.8 . . ?
H8A C8 H8B 108.2 . . ?
N3 C9 C10 111.6(4) . . ?
N3 C9 H9A 109.3 . . ?
C10 C9 H9A 109.3 . . ?
N3 C9 H9B 109.3 . . ?
C10 C9 H9B 109.3 . . ?
H9A C9 H9B 108.0 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
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 N2 2.095(3) . ?
Zn1 N3 2.241(3) . ?
Zn1 N1 2.246(3) . ?
Zn1 Br2 2.3982(8) . ?
Zn1 Br1 2.4260(8) . ?
N1 C6 1.330(5) . ?
N1 C2 1.349(5) . ?
N2 C1 1.252(5) . ?
N2 C7 1.455(5) . ?
N3 C8 1.468(5) . ?
N3 C9 1.484(6) . ?
N3 H3A 0.9100 . ?
C1 C2 1.464(6) . ?
C1 H1 0.9300 . ?
C2 C3 1.381(6) . ?
C3 C4 1.388(6) . ?
C3 H3 0.9300 . ?
C4 C5 1.367(6) . ?
C4 H4 0.9300 . ?
C5 C6 1.380(6) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C7 C8 1.506(7) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C10 1.501(7) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N3 H3A Br1 0.91 2.76 3.555(3) 147.1 2_666
