#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:14:46 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179052 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/14/4301427.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_4301427
loop_
_publ_author_name
'Xiu-Teng Wang'
'Xiao-Hua Wang'
'Zhe-Ming Wang'
'Song Gao'
_publ_section_title
;
Diversity of Azido Magnetic Chains Constructed with Flexible Ligand
2,2'-Dipyridylamine
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1301
_journal_page_last               1308
_journal_paper_doi               10.1021/ic801505a
_journal_volume                  48
_journal_year                    2009
_chemical_formula_sum            'C20 H22 N18 Ni2 O2'
_chemical_formula_weight         663.98
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 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                 98.092(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.1404(3)
_cell_length_b                   14.9543(7)
_cell_length_c                   10.7338(5)
_cell_measurement_reflns_used    9435
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.028
_cell_measurement_theta_min      3.395
_cell_volume                     1293.66(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, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 9
_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  0.1672
_diffrn_reflns_av_sigmaI/netI    0.1263
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            18750
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.65
_exptl_absorpt_coefficient_mu    1.515
_exptl_absorpt_correction_T_max  0.905
_exptl_absorpt_correction_T_min  0.828
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.705
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       column
_exptl_crystal_F_000             680
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.564
_refine_diff_density_min         -0.414
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.891
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         2356
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.891
_refine_ls_R_factor_all          0.1127
_refine_ls_R_factor_gt           0.0445
_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)+(0.0306P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0687
_refine_ls_wR_factor_ref         0.0807
_reflns_number_gt                1332
_reflns_number_total             2356
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic801505a_si_001_4.cif
_cod_data_source_block           NiN3
_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 
;
_cod_original_sg_symbol_H-M      'P 21/m'
_cod_database_code               4301427
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, 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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.59081(6) 0.84801(3) 0.83464(5) 0.02861(18) Uani 1 1 d . . .
N10 N 0.3953(6) 0.7500 0.8462(5) 0.0304(13) Uani 1 2 d S . .
N7 N 0.7200(6) 0.7500 0.9582(5) 0.0307(13) Uani 1 2 d S . .
N4 N 0.6440(6) 0.7500 0.7022(5) 0.0331(13) Uani 1 2 d S . .
N1 N 0.4579(4) 0.9253(2) 0.6997(3) 0.0305(9) Uani 1 1 d . . .
N3 N 0.7944(4) 0.9264(2) 0.8217(3) 0.0311(9) Uani 1 1 d . . .
N11 N 0.3220(6) 0.7500 0.9352(6) 0.0374(14) Uani 1 2 d S . .
C5 C 0.4882(5) 1.0124(3) 0.6840(4) 0.0327(11) Uani 1 1 d . . .
C6 C 0.7827(5) 1.0131(3) 0.7916(4) 0.0319(11) Uani 1 1 d . . .
N5 N 0.7645(7) 0.7500 0.6494(5) 0.0449(15) Uani 1 2 d S . .
N6 N 0.8794(9) 0.7500 0.5985(6) 0.085(3) Uani 1 2 d S . .
N12 N 0.2464(7) 0.7500 1.0189(6) 0.0618(19) Uani 1 2 d S . .
C3 C 0.2467(6) 1.0311(3) 0.5326(5) 0.0446(13) Uani 1 1 d . . .
H3A H 0.1750 1.0664 0.4781 0.054 Uiso 1 1 calc R . .
C1 C 0.3247(5) 0.8917(3) 0.6272(4) 0.0397(12) Uani 1 1 d . . .
H1A H 0.3030 0.8311 0.6349 0.048 Uiso 1 1 calc R . .
N9 N 0.7308(9) 0.7500 1.1791(7) 0.078(2) Uani 1 2 d S . .
N8 N 0.7229(6) 0.7500 1.0688(7) 0.0421(15) Uani 1 2 d S . .
C7 C 0.9495(5) 0.8936(3) 0.8581(4) 0.0390(12) Uani 1 1 d . . .
H7B H 0.9602 0.8332 0.8780 0.047 Uiso 1 1 calc R . .
C4 C 0.3823(6) 1.0679(3) 0.6043(5) 0.0444(13) Uani 1 1 d . . .
H4B H 0.4036 1.1289 0.6000 0.053 Uiso 1 1 calc R . .
N2 N 0.6299(5) 1.0503(2) 0.7486(4) 0.0402(10) Uani 1 1 d . . .
H2A H 0.6216 1.1063 0.7648 0.048 Uiso 1 1 calc R . .
C2 C 0.2182(6) 0.9400(3) 0.5427(5) 0.0480(14) Uani 1 1 d . . .
H2B H 0.1292 0.9125 0.4934 0.058 Uiso 1 1 calc R . .
N14 N 0.5000 1.0000 1.0000 0.0286(13) Uani 1 2 d S . .
N13 N 0.5249(4) 0.9239(2) 0.9810(3) 0.0387(10) Uani 1 1 d . . .
C9 C 1.0763(6) 1.0326(3) 0.8385(5) 0.0445(12) Uani 1 1 d . . .
H9A H 1.1704 1.0685 0.8443 0.053 Uiso 1 1 calc R . .
C10 C 0.9245(6) 1.0680(3) 0.8015(4) 0.0442(13) Uani 1 1 d . . .
H10B H 0.9137 1.1286 0.7827 0.053 Uiso 1 1 calc R . .
C8 C 1.0904(6) 0.9441(3) 0.8672(4) 0.0441(14) Uani 1 1 d . . .
H8A H 1.1939 0.9185 0.8925 0.053 Uiso 1 1 calc R . .
O1 O 0.3510(7) 0.7500 1.2858(6) 0.107(2) Uani 1 2 d S . .
O2 O 1.0154(7) 0.7500 0.3736(5) 0.0907(19) Uani 1 2 d S . .
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'
O O 0.0106 0.0060 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ni1 N3 88.91(14) . . ?
N1 Ni1 N13 93.43(14) . . ?
N3 Ni1 N13 92.08(13) . . ?
N1 Ni1 N4 93.06(15) . . ?
N3 Ni1 N4 96.10(15) . . ?
N13 Ni1 N4 169.65(13) . . ?
N1 Ni1 N7 171.38(15) . . ?
N3 Ni1 N7 95.84(15) . . ?
N13 Ni1 N7 93.57(16) . . ?
N4 Ni1 N7 79.32(16) . . ?
N1 Ni1 N10 95.90(15) . . ?
N3 Ni1 N10 172.62(13) . . ?
N13 Ni1 N10 93.21(15) . . ?
N4 Ni1 N10 78.10(16) . . ?
N7 Ni1 N10 78.70(15) . . ?
N1 Ni1 Ni1 124.49(10) . 4_575 ?
N3 Ni1 Ni1 124.87(9) . 4_575 ?
N13 Ni1 Ni1 123.27(10) . 4_575 ?
N4 Ni1 Ni1 46.47(9) . 4_575 ?
N7 Ni1 Ni1 47.01(10) . 4_575 ?
N10 Ni1 Ni1 47.75(8) . 4_575 ?
N11 N10 Ni1 119.7(3) . . ?
N11 N10 Ni1 119.7(3) . 4_575 ?
Ni1 N10 Ni1 84.50(17) . 4_575 ?
N8 N7 Ni1 123.9(3) . 4_575 ?
N8 N7 Ni1 123.9(3) . . ?
Ni1 N7 Ni1 86.0(2) 4_575 . ?
N5 N4 Ni1 124.9(3) . 4_575 ?
N5 N4 Ni1 124.9(3) . . ?
Ni1 N4 Ni1 87.06(18) 4_575 . ?
C1 N1 C5 116.1(4) . . ?
C1 N1 Ni1 120.3(3) . . ?
C5 N1 Ni1 123.4(3) . . ?
C6 N3 C7 116.8(4) . . ?
C6 N3 Ni1 122.7(3) . . ?
C7 N3 Ni1 120.1(3) . . ?
N12 N11 N10 177.9(7) . . ?
N1 C5 N2 119.5(4) . . ?
N1 C5 C4 123.0(4) . . ?
N2 C5 C4 117.5(4) . . ?
N3 C6 N2 120.1(4) . . ?
N3 C6 C10 121.2(4) . . ?
N2 C6 C10 118.7(4) . . ?
N6 N5 N4 179.8(7) . . ?
C4 C3 C2 118.7(5) . . ?
N1 C1 C2 124.9(4) . . ?
N9 N8 N7 178.0(7) . . ?
N3 C7 C8 123.9(4) . . ?
C3 C4 C5 118.9(4) . . ?
C6 N2 C5 130.6(4) . . ?
C1 C2 C3 118.2(5) . . ?
N13 N14 N13 180.0(4) . 3_677 ?
N14 N13 Ni1 136.9(2) . . ?
C10 C9 C8 119.5(4) . . ?
C9 C10 C6 120.0(4) . . ?
C9 C8 C7 118.6(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
Ni1 N1 2.041(3) . ?
Ni1 N3 2.050(3) . ?
Ni1 N13 2.069(3) . ?
Ni1 N4 2.128(3) . ?
Ni1 N7 2.150(4) . ?
Ni1 N10 2.180(4) . ?
Ni1 Ni1 2.9312(10) 4_575 ?
N10 N11 1.195(7) . ?
N10 Ni1 2.180(3) 4_575 ?
N7 N8 1.184(7) . ?
N7 Ni1 2.150(4) 4_575 ?
N4 N5 1.200(6) . ?
N4 Ni1 2.128(3) 4_575 ?
N1 C1 1.340(5) . ?
N1 C5 1.340(5) . ?
N3 C6 1.337(5) . ?
N3 C7 1.360(5) . ?
N11 N12 1.159(7) . ?
C5 N2 1.382(5) . ?
C5 C4 1.400(6) . ?
C6 N2 1.381(5) . ?
C6 C10 1.408(6) . ?
N5 N6 1.148(7) . ?
C3 C4 1.369(6) . ?
C3 C2 1.389(6) . ?
C1 C2 1.369(6) . ?
N9 N8 1.176(8) . ?
C7 C8 1.365(5) . ?
N14 N13 1.179(3) . ?
N14 N13 1.179(3) 3_677 ?
C9 C10 1.352(6) . ?
C9 C8 1.361(6) . ?
