#------------------------------------------------------------------------------
#$Date: 2016-02-20 05:06:23 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176774 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/31/2203139.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_2203139
loop_
_publ_author_name
'Albada, Gerard A.van'
'Mohamadou, Aminou'
'Mutikainen, Ilpo'
'Turpeinen, Urho'
'Reedijk, Jan'
_publ_section_title
;
 Diazidobis(2,2'-biimidazoline)nickel(II)
;
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m237
_journal_page_last               m238
_journal_paper_doi               10.1107/S1600536804001795
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac          '[Ni (N3)2 (C6 H10 N4)2]'
_chemical_formula_moiety         'C12 H20 N14 Ni'
_chemical_formula_sum            'C12 H20 N14 Ni'
_chemical_formula_weight         419.13
_chemical_name_systematic        ?
_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                97.637(14)
_cell_angle_beta                 103.327(8)
_cell_angle_gamma                111.756(15)
_cell_formula_units_Z            1
_cell_length_a                   7.2960(6)
_cell_length_b                   7.9420(18)
_cell_length_c                   8.2080(9)
_cell_measurement_reflns_used    6148
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      3.16
_cell_volume                     417.11(13)
_computing_cell_refinement       COLLECT
_computing_data_collection       'COLLECT (Nonius, 2002)'
_computing_data_reduction        COLLECT
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1997)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Nonius KappaCCD'
_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  0.0291
_diffrn_reflns_av_sigmaI/netI    0.0302
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            6148
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         3.16
_diffrn_standards_decay_%        <2
_diffrn_standards_number         200
_exptl_absorpt_coefficient_mu    1.198
_exptl_absorpt_correction_T_max  0.716
_exptl_absorpt_correction_T_min  0.701
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.669
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             218
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.506
_refine_diff_density_min         -0.575
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     120
_refine_ls_number_reflns         1916
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0281
_refine_ls_R_factor_gt           0.0250
_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)+(0.0311P)²+0.2437P] where P = (Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0659
_refine_ls_wR_factor_ref         0.0672
_reflns_number_gt                1785
_reflns_number_total             1916
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ac6079.cif
_cod_data_source_block           I
_cod_original_cell_volume        417.11(11)
_cod_database_code               2203139
_cod_database_fobs_code          2203139
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_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
_atom_site_type_symbol
Ni1 0.0000 0.0000 0.0000 0.01336(10) Uani d S 1 Ni
N11 -0.4064(2) 0.2593(2) -0.06998(19) 0.0203(3) Uani d . 1 N
H11A -0.5279 0.2405 -0.1385 0.024 Uiso calc R 1 H
C12 -0.3060(2) 0.1474(2) -0.08305(19) 0.0136(3) Uiso d . 1 C
N13 -0.1227(2) 0.20128(18) 0.02327(17) 0.0150(3) Uani d . 1 N
C14 -0.0848(2) 0.3727(2) 0.1480(2) 0.0168(3) Uani d . 1 C
H14A 0.0452 0.4770 0.1524 0.020 Uiso calc R 1 H
H14B -0.0745 0.3508 0.2651 0.020 Uiso calc R 1 H
C15 -0.2753(3) 0.4180(2) 0.0797(2) 0.0178(3) Uani d . 1 C
H15A -0.3471 0.4232 0.1677 0.021 Uiso calc R 1 H
H15B -0.2335 0.5380 0.0448 0.021 Uiso calc R 1 H
N21 -0.5633(2) -0.1022(2) -0.34460(19) 0.0241(3) Uani d . 1 N
H21A -0.6529 -0.0521 -0.3659 0.029 Uiso calc R 1 H
C22 -0.3873(2) -0.0324(2) -0.21275(19) 0.0138(3) Uani d . 1 C
N23 -0.2745(2) -0.12646(18) -0.20090(17) 0.0154(3) Uani d . 1 N
C24 -0.3745(3) -0.2878(2) -0.3520(2) 0.0197(3) Uani d . 1 C
H24A -0.4036 -0.4065 -0.3153 0.024 Uiso calc R 1 H
H24B -0.2851 -0.2787 -0.4277 0.024 Uiso calc R 1 H
C25 -0.5805(3) -0.2772(2) -0.4475(2) 0.0203(3) Uani d . 1 C
H25A -0.5887 -0.2709 -0.5685 0.024 Uiso calc R 1 H
H25B -0.7032 -0.3857 -0.4460 0.024 Uiso calc R 1 H
N1 0.1537(2) 0.1094(2) -0.18638(18) 0.0194(3) Uani d . 1 N
N2 0.0651(2) 0.15830(19) -0.30087(18) 0.0184(3) Uani d . 1 N
N3 -0.0198(3) 0.2073(3) -0.4108(2) 0.0315(4) Uani d . 1 N
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Ni Ni 0.3393 1.1124 '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'
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'
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
N23 Ni1 N23 . 2 180.0 yes
N23 Ni1 N13 . 2 101.22(5) yes
N23 Ni1 N13 2 2 78.78(5) yes
N23 Ni1 N13 . . 78.78(5) ?
N23 Ni1 N13 2 . 101.22(5) ?
N13 Ni1 N13 2 . 180.0 ?
N23 Ni1 N1 . . 87.81(5) yes
N23 Ni1 N1 2 . 92.19(5) yes
N13 Ni1 N1 2 . 85.70(5) yes
N13 Ni1 N1 . . 94.30(5) yes
N23 Ni1 N1 . 2 92.19(5) ?
N23 Ni1 N1 2 2 87.81(5) ?
N13 Ni1 N1 2 2 94.30(5) ?
N13 Ni1 N1 . 2 85.70(5) ?
N1 Ni1 N1 . 2 180.0 ?
C12 N11 C15 . . 107.51(13) ?
C12 N11 H11A . . 126.2 ?
C15 N11 H11A . . 126.2 ?
N13 C12 N11 . . 118.15(14) ?
N13 C12 C22 . . 116.54(14) ?
N11 C12 C22 . . 125.30(14) ?
C12 N13 C14 . . 106.33(13) ?
C12 N13 Ni1 . . 113.15(10) ?
C14 N13 Ni1 . . 138.97(10) ?
N13 C14 C15 . . 105.34(12) ?
N13 C14 H14A . . 110.7 ?
C15 C14 H14A . . 110.7 ?
N13 C14 H14B . . 110.7 ?
C15 C14 H14B . . 110.7 ?
H14A C14 H14B . . 108.8 ?
N11 C15 C14 . . 102.31(12) ?
N11 C15 H15A . . 111.3 ?
C14 C15 H15A . . 111.3 ?
N11 C15 H15B . . 111.3 ?
C14 C15 H15B . . 111.3 ?
H15A C15 H15B . . 109.2 ?
C22 N21 C25 . . 108.12(14) ?
C22 N21 H21A . . 125.9 ?
C25 N21 H21A . . 125.9 ?
N23 C22 N21 . . 117.40(14) ?
N23 C22 C12 . . 117.02(13) ?
N21 C22 C12 . . 125.53(15) ?
C22 N23 C24 . . 107.33(13) ?
C22 N23 Ni1 . . 114.18(10) ?
C24 N23 Ni1 . . 138.06(11) ?
N23 C24 C25 . . 104.72(13) ?
N23 C24 H24A . . 110.8 ?
C25 C24 H24A . . 110.8 ?
N23 C24 H24B . . 110.8 ?
C25 C24 H24B . . 110.8 ?
H24A C24 H24B . . 108.9 ?
N21 C25 C24 . . 102.23(12) ?
N21 C25 H25A . . 111.3 ?
C24 C25 H25A . . 111.3 ?
N21 C25 H25B . . 111.3 ?
C24 C25 H25B . . 111.3 ?
H25A C25 H25B . . 109.2 ?
N2 N1 Ni1 . . 119.52(11) ?
N3 N2 N1 . . 179.37(17) yes
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
Ni1 N23 . 2.0701(13) yes
Ni1 N23 2 2.0701(13) ?
Ni1 N13 2 2.1099(14) yes
Ni1 N13 . 2.1099(14) ?
Ni1 N1 . 2.1851(14) yes
Ni1 N1 2 2.1851(14) ?
N11 C12 . 1.353(2) ?
N11 C15 . 1.472(2) ?
N11 H11A . 0.8800 ?
C12 N13 . 1.293(2) ?
C12 C22 . 1.484(2) ?
N13 C14 . 1.4828(19) ?
C14 C15 . 1.562(2) ?
C14 H14A . 0.9900 ?
C14 H14B . 0.9900 ?
C15 H15A . 0.9900 ?
C15 H15B . 0.9900 ?
N21 C22 . 1.341(2) ?
N21 C25 . 1.473(2) ?
N21 H21A . 0.8800 ?
C22 N23 . 1.297(2) ?
N23 C24 . 1.4767(19) ?
C24 C25 . 1.565(2) ?
C24 H24A . 0.9900 ?
C24 H24B . 0.9900 ?
C25 H25A . 0.9900 ?
C25 H25B . 0.9900 ?
N1 N2 . 1.206(2) ?
N2 N3 . 1.168(2) ?
