#------------------------------------------------------------------------------
#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/01/2220117.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_2220117
loop_
_publ_author_name
'Hou, Jin'
_publ_section_title
;
 Di-μ~1,1~-azido-bis[azido(5,5'-dimethyl-2,2'-bipyridine)nickel(II)]
;
_journal_coeditor_code           CI2712
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1571
_journal_paper_doi               10.1107/S1600536808037902
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          '[Ni2 (N3)4 (C12 H12 N2)2]'
_chemical_formula_moiety         'C24 H24 N16 Ni2'
_chemical_formula_sum            'C24 H24 N16 Ni2'
_chemical_formula_weight         654.01
_chemical_name_systematic
;
Di-μ1,1-azido-bis[azido(5,5'-dimethyl-2,2'-bipyridine)nickel(II)]
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 91.650(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.938(2)
_cell_length_b                   15.067(3)
_cell_length_c                   11.755(2)
_cell_measurement_reflns_used    1576
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.1
_cell_measurement_theta_min      2.3
_cell_volume                     1405.3(5)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'SMART (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       'φ and ω scan'
_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  0.0632
_diffrn_reflns_av_sigmaI/netI    0.0643
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            11588
_diffrn_reflns_theta_full        26.99
_diffrn_reflns_theta_max         26.99
_diffrn_reflns_theta_min         2.20
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.387
_exptl_absorpt_correction_T_max  0.8971
_exptl_absorpt_correction_T_min  0.8403
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2001)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.546
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             672
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.673
_refine_diff_density_min         -0.767
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     192
_refine_ls_number_reflns         3060
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.123
_refine_ls_R_factor_all          0.0857
_refine_ls_R_factor_gt           0.0562
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_max_lt       0.001
_refine_ls_shift/su_mean         <0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0643P)²+1.1062P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1355
_refine_ls_wR_factor_ref         0.1493
_reflns_number_gt                2165
_reflns_number_total             3060
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ci2712.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2220117
_cod_database_fobs_code          2220117
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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
Ni Ni1 0.03235(7) 0.44079(4) 0.11356(5) 0.0386(2) Uani d . 1
N N1 0.2280(5) 0.3549(3) 0.1785(4) 0.0491(10) Uani d . 1
N N2 -0.0777(5) 0.3158(3) 0.0994(3) 0.0416(9) Uani d . 1
N N3 0.0029(5) 0.5108(3) 0.2626(4) 0.0459(11) Uani d D 1
N N4 0.0958(8) 0.5106(4) 0.3252(5) 0.0857(18) Uani d DU 1
N N5 0.1983(12) 0.5160(6) 0.4040(7) 0.144(3) Uani d DU 1
N N6 0.1668(5) 0.4913(3) -0.0170(4) 0.0583(12) Uani d . 1
N N7 0.2901(6) 0.4579(3) -0.0571(4) 0.0594(12) Uani d . 1
N N8 0.4096(8) 0.4282(4) -0.0950(6) 0.094(2) Uani d . 1
C C1 0.1794(6) 0.2706(3) 0.1926(4) 0.0445(11) Uani d . 1
C C2 0.2820(7) 0.2113(4) 0.2525(5) 0.0573(14) Uani d . 1
H H2 0.2475 0.1529 0.2628 0.069 Uiso calc R 1
C C3 0.4356(7) 0.2398(4) 0.2967(5) 0.0632(16) Uani d . 1
H H3 0.5057 0.2000 0.3357 0.076 Uiso calc R 1
C C4 0.4857(6) 0.3259(4) 0.2836(5) 0.0575(14) Uani d . 1
C C5 0.3771(6) 0.3811(4) 0.2219(5) 0.0570(14) Uani d . 1
H H5 0.4100 0.4396 0.2102 0.068 Uiso calc R 1
C C6 0.6485(7) 0.3623(5) 0.3348(5) 0.085(2) Uani d . 1
H H6A 0.6289 0.3847 0.4097 0.128 Uiso calc R 1
H H6B 0.6886 0.4095 0.2878 0.128 Uiso calc R 1
H H6C 0.7312 0.3159 0.3393 0.128 Uiso calc R 1
C C7 0.0139(6) 0.2474(3) 0.1428(4) 0.0442(12) Uani d . 1
C C8 -0.0506(7) 0.1625(4) 0.1383(5) 0.0626(15) Uani d . 1
H H8 0.0127 0.1155 0.1680 0.075 Uiso calc R 1
C C9 -0.2070(8) 0.1468(4) 0.0904(5) 0.0652(16) Uani d . 1
H H9 -0.2501 0.0894 0.0893 0.078 Uiso calc R 1
C C10 -0.3023(6) 0.2160(4) 0.0433(5) 0.0530(13) Uani d . 1
C C11 -0.2308(6) 0.2993(3) 0.0520(4) 0.0477(12) Uani d . 1
H H11 -0.2925 0.3472 0.0233 0.057 Uiso calc R 1
C C12 -0.4711(7) 0.2026(4) -0.0126(5) 0.0657(16) Uani d . 1
H H12A -0.5490 0.1824 0.0427 0.098 Uiso calc R 1
H H12B -0.4629 0.1591 -0.0719 0.098 Uiso calc R 1
H H12C -0.5103 0.2577 -0.0448 0.098 Uiso calc R 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'
Ni Ni 0.3393 1.1124 '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_3
_geom_angle
N6 Ni1 N3 . 121.5(2)
N6 Ni1 N2 . 120.32(18)
N3 Ni1 N2 . 118.23(17)
N6 Ni1 N1 . 95.97(17)
N3 Ni1 N1 . 96.02(17)
N2 Ni1 N1 . 77.30(15)
N6 Ni1 N6 3_565 79.63(18)
N3 Ni1 N6 3_565 95.99(18)
N2 Ni1 N6 3_565 94.98(16)
N1 Ni1 N6 3_565 167.78(18)
C5 N1 C1 . 119.3(5)
C5 N1 Ni1 . 125.6(4)
C1 N1 Ni1 . 114.1(3)
C11 N2 C7 . 119.0(4)
C11 N2 Ni1 . 124.9(3)
C7 N2 Ni1 . 116.1(3)
N4 N3 Ni1 . 120.7(5)
N3 N4 N5 . 174.4(8)
N7 N6 Ni1 . 125.8(4)
N7 N6 Ni1 3_565 125.2(4)
Ni1 N6 Ni1 3_565 100.37(18)
N8 N7 N6 . 178.1(6)
N1 C1 C2 . 120.5(5)
N1 C1 C7 . 115.8(4)
C2 C1 C7 . 123.8(5)
C3 C2 C1 . 119.3(5)
C3 C2 H2 . 120.3
C1 C2 H2 . 120.3
C4 C3 C2 . 120.7(5)
C4 C3 H3 . 119.7
C2 C3 H3 . 119.7
C3 C4 C5 . 116.7(5)
C3 C4 C6 . 123.2(5)
C5 C4 C6 . 120.1(6)
N1 C5 C4 . 123.5(5)
N1 C5 H5 . 118.2
C4 C5 H5 . 118.2
C4 C6 H6A . 109.5
C4 C6 H6B . 109.5
H6A C6 H6B . 109.5
C4 C6 H6C . 109.5
H6A C6 H6C . 109.5
H6B C6 H6C . 109.5
N2 C7 C8 . 119.8(5)
N2 C7 C1 . 115.8(4)
C8 C7 C1 . 124.3(5)
C9 C8 C7 . 120.5(5)
C9 C8 H8 . 119.8
C7 C8 H8 . 119.8
C8 C9 C10 . 120.6(5)
C8 C9 H9 . 119.7
C10 C9 H9 . 119.7
C11 C10 C9 . 115.7(5)
C11 C10 C12 . 121.3(5)
C9 C10 C12 . 123.0(5)
N2 C11 C10 . 124.3(5)
N2 C11 H11 . 117.8
C10 C11 H11 . 117.8
C10 C12 H12A . 109.5
C10 C12 H12B . 109.5
H12A C12 H12B . 109.5
C10 C12 H12C . 109.5
H12A C12 H12C . 109.5
H12B C12 H12C . 109.5
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 N1 . 2.145(4) y
Ni1 N2 . 2.081(4) y
Ni1 N3 . 2.064(5) y
Ni1 N6 . 2.041(4) y
Ni1 N6 3_565 2.175(4) y
N1 C5 . 1.336(6) ?
N1 C1 . 1.339(6) ?
N2 C11 . 1.345(6) ?
N2 C7 . 1.352(6) ?
N3 N4 . 1.027(6) ?
N4 N5 . 1.217(7) ?
N6 N7 . 1.209(6) ?
N6 Ni1 3_565 2.175(4) ?
N7 N8 . 1.149(7) ?
C1 C2 . 1.387(7) ?
C1 C7 . 1.465(7) ?
C2 C3 . 1.380(8) ?
C2 H2 . 0.93 ?
C3 C4 . 1.367(8) ?
C3 H3 . 0.93 ?
C4 C5 . 1.387(7) ?
C4 C6 . 1.512(8) ?
C5 H5 . 0.93 ?
C6 H6A . 0.96 ?
C6 H6B . 0.96 ?
C6 H6C . 0.96 ?
C7 C8 . 1.379(7) ?
C8 C9 . 1.369(8) ?
C8 H8 . 0.93 ?
C9 C10 . 1.394(8) ?
C9 H9 . 0.93 ?
C10 C11 . 1.380(7) ?
C10 C12 . 1.489(7) ?
C11 H11 . 0.93 ?
C12 H12A . 0.96 ?
C12 H12B . 0.96 ?
C12 H12C . 0.96 ?
