#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:14:46 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179052 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/14/4301428.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_4301428
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            'C22 H25 N15 Ni2 O4'
_chemical_formula_weight         680.99
_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                95.0084(9)
_cell_angle_beta                 97.6127(9)
_cell_angle_gamma                103.9581(9)
_cell_formula_units_Z            2
_cell_length_a                   8.4022(2)
_cell_length_b                   11.6981(3)
_cell_length_c                   15.2421(4)
_cell_measurement_reflns_used    23651
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.373
_cell_measurement_theta_min      3.395
_cell_volume                     1429.97(6)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0617
_diffrn_reflns_av_sigmaI/netI    0.0513
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            29873
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         3.41
_exptl_absorpt_coefficient_mu    1.375
_exptl_absorpt_correction_T_max  0.765
_exptl_absorpt_correction_T_min  0.652
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995)
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.582
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             700
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.519
_refine_diff_density_min         -0.441
_refine_diff_density_rms         0.061
_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     388
_refine_ls_number_reflns         5838
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0622
_refine_ls_R_factor_gt           0.0345
_refine_ls_shift/su_max          0.081
_refine_ls_shift/su_mean         0.018
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0511P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0846
_refine_ls_wR_factor_ref         0.0914
_reflns_number_gt                4125
_reflns_number_total             5838
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic801505a_si_001_5.cif
_cod_data_source_block           NiAcN3
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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_database_code               4301428
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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.40983(4) 0.16619(3) 0.72040(2) 0.03403(11) Uani 1 1 d . . .
Ni2 Ni 0.14272(4) 0.24827(3) 0.82401(2) 0.03227(11) Uani 1 1 d . . .
N8 N 0.4506(2) 0.19509(18) 0.92235(15) 0.0352(5) Uani 1 1 d . . .
N4 N -0.0025(2) 0.09503(19) 0.86189(14) 0.0356(5) Uani 1 1 d . . .
N10 N 0.1541(2) 0.16420(19) 0.69785(14) 0.0352(5) Uani 1 1 d . . .
O1 O 0.2798(2) 0.40294(16) 0.78947(12) 0.0435(5) Uani 1 1 d . . .
N11 N 0.0944(3) 0.19481(19) 0.63097(15) 0.0405(5) Uani 1 1 d . . .
O2 O 0.4751(2) 0.34471(16) 0.72300(12) 0.0440(5) Uani 1 1 d . . .
N6 N 0.1454(2) 0.33156(19) 0.94996(14) 0.0371(5) Uani 1 1 d . . .
N1 N 0.3458(2) -0.01611(18) 0.71278(13) 0.0355(5) Uani 1 1 d . . .
N7 N 0.3612(3) 0.1900(2) 0.85434(14) 0.0379(5) Uani 1 1 d . . .
C16 C 0.0181(3) 0.3049(2) 0.99497(17) 0.0379(6) Uani 1 1 d . . .
N13 N 0.6562(3) 0.1669(2) 0.75787(18) 0.0566(7) Uani 1 1 d . . .
N3 N 0.4136(3) 0.1420(2) 0.58527(15) 0.0437(6) Uani 1 1 d . . .
N5 N -0.1095(3) 0.2041(2) 0.96632(15) 0.0428(6) Uani 1 1 d . . .
H5A H -0.2049 0.2085 0.9787 0.051 Uiso 1 1 calc R . .
C14 C -0.2168(3) -0.0057(3) 0.93741(19) 0.0467(7) Uani 1 1 d . . .
H14A H -0.2883 -0.0015 0.9785 0.056 Uiso 1 1 calc R . .
N9 N 0.5372(3) 0.1980(3) 0.98856(16) 0.0611(8) Uani 1 1 d . . .
C21 C 0.4055(3) 0.4213(2) 0.75094(18) 0.0407(6) Uani 1 1 d . . .
N12 N 0.0370(4) 0.2226(3) 0.56588(17) 0.0686(8) Uani 1 1 d . . .
C15 C -0.1068(3) 0.0971(2) 0.92070(17) 0.0365(6) Uani 1 1 d . . .
N2 N 0.2098(3) -0.0396(2) 0.56478(14) 0.0476(6) Uani 1 1 d . . .
H2A H 0.1158 -0.0737 0.5322 0.057 Uiso 1 1 calc R . .
C5 C 0.2402(3) -0.0851(2) 0.64445(17) 0.0407(6) Uani 1 1 d . . .
C2 C 0.3142(4) -0.1833(3) 0.79489(19) 0.0490(7) Uani 1 1 d . . .
H2B H 0.3445 -0.2156 0.8462 0.059 Uiso 1 1 calc R . .
C1 C 0.3837(3) -0.0683(2) 0.78645(18) 0.0409(6) Uani 1 1 d . . .
H1A H 0.4613 -0.0226 0.8335 0.049 Uiso 1 1 calc R . .
C11 C -0.0057(3) -0.0120(2) 0.82023(19) 0.0435(7) Uani 1 1 d . . .
H11A H 0.0681 -0.0153 0.7802 0.052 Uiso 1 1 calc R . .
C4 C 0.1602(4) -0.2028(3) 0.64969(19) 0.0490(7) Uani 1 1 d . . .
H4A H 0.0826 -0.2474 0.6023 0.059 Uiso 1 1 calc R . .
C12 C -0.1108(4) -0.1165(3) 0.8331(2) 0.0511(8) Uani 1 1 d . . .
H12A H -0.1091 -0.1881 0.8020 0.061 Uiso 1 1 calc R . .
C13 C -0.2185(3) -0.1129(3) 0.8928(2) 0.0516(8) Uani 1 1 d . . .
H13B H -0.2916 -0.1822 0.9029 0.062 Uiso 1 1 calc R . .
C19 C 0.2691(4) 0.5006(3) 1.0595(2) 0.0541(8) Uani 1 1 d . . .
H19A H 0.3579 0.5660 1.0808 0.065 Uiso 1 1 calc R . .
C17 C 0.0080(4) 0.3756(3) 1.07142(19) 0.0488(7) Uani 1 1 d . . .
H17A H -0.0839 0.3561 1.1003 0.059 Uiso 1 1 calc R . .
C10 C 0.5096(4) 0.2281(3) 0.5473(2) 0.0572(8) Uani 1 1 d . . .
H10A H 0.5863 0.2898 0.5845 0.069 Uiso 1 1 calc R . .
C20 C 0.2698(3) 0.4293(2) 0.98429(19) 0.0465(7) Uani 1 1 d . . .
H20A H 0.3606 0.4485 0.9546 0.056 Uiso 1 1 calc R . .
C3 C 0.1974(4) -0.2519(3) 0.7258(2) 0.0535(8) Uani 1 1 d . . .
H3A H 0.1449 -0.3301 0.7309 0.064 Uiso 1 1 calc R . .
C8 C 0.3874(5) 0.1372(4) 0.4013(2) 0.0747(11) Uani 1 1 d . . .
H8A H 0.3778 0.1358 0.3397 0.090 Uiso 1 1 calc R . .
C9 C 0.4996(5) 0.2292(3) 0.4565(2) 0.0719(10) Uani 1 1 d . . .
H9A H 0.5669 0.2906 0.4331 0.086 Uiso 1 1 calc R . .
C18 C 0.1350(4) 0.4742(3) 1.1037(2) 0.0555(8) Uani 1 1 d . . .
H18A H 0.1304 0.5225 1.1546 0.067 Uiso 1 1 calc R . .
C6 C 0.3077(4) 0.0520(3) 0.52992(19) 0.0450(7) Uani 1 1 d . . .
C22 C 0.4789(4) 0.5471(3) 0.7360(3) 0.0683(10) Uani 1 1 d . . .
H22A H 0.5730 0.5503 0.7059 0.102 Uiso 1 1 calc R . .
H22B H 0.5137 0.5963 0.7924 0.102 Uiso 1 1 calc R . .
H22C H 0.3971 0.5753 0.7001 0.102 Uiso 1 1 calc R . .
N14 N 0.7879(3) 0.23066(19) 0.76370(14) 0.0365(5) Uani 1 1 d . . .
C7 C 0.2917(4) 0.0491(3) 0.43701(19) 0.0601(9) Uani 1 1 d . . .
H7A H 0.2154 -0.0132 0.4002 0.072 Uiso 1 1 calc R . .
N15 N 0.9230(3) 0.2933(2) 0.77025(15) 0.0431(6) Uani 1 1 d . . .
O3 O 0.9682(7) 0.4813(3) 0.6383(3) 0.205(2) Uani 1 1 d . . .
O4 O 0.7709(11) 0.5161(6) 0.4955(5) 0.379(6) Uani 1 1 d . . .
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
O2 Ni1 N1 177.74(8) . . ?
O2 Ni1 N3 91.49(8) . . ?
N1 Ni1 N3 86.31(9) . . ?
O2 Ni1 N13 90.34(9) . . ?
N1 Ni1 N13 89.36(9) . . ?
N3 Ni1 N13 95.30(10) . . ?
O2 Ni1 N10 90.75(8) . . ?
N1 Ni1 N10 89.80(8) . . ?
N3 Ni1 N10 91.28(9) . . ?
N13 Ni1 N10 173.30(10) . . ?
O2 Ni1 N7 88.82(8) . . ?
N1 Ni1 N7 93.43(8) . . ?
N3 Ni1 N7 170.03(8) . . ?
N13 Ni1 N7 94.66(9) . . ?
N10 Ni1 N7 78.76(8) . . ?
O1 Ni2 N6 90.70(8) . . ?
O1 Ni2 N4 177.58(8) . . ?
N6 Ni2 N4 87.46(8) . . ?
O1 Ni2 N10 88.24(8) . . ?
N6 Ni2 N10 176.84(8) . . ?
N4 Ni2 N10 93.67(8) . . ?
O1 Ni2 N7 90.27(8) . . ?
N6 Ni2 N7 97.29(8) . . ?
N4 Ni2 N7 91.53(8) . . ?
N10 Ni2 N7 79.74(8) . . ?
O1 Ni2 N15 89.10(8) . 1_455 ?
N6 Ni2 N15 92.84(8) . 1_455 ?
N4 Ni2 N15 89.41(8) . 1_455 ?
N10 Ni2 N15 90.13(9) . 1_455 ?
N7 Ni2 N15 169.86(9) . 1_455 ?
N9 N8 N7 178.9(3) . . ?
C15 N4 C11 116.8(2) . . ?
C15 N4 Ni2 123.12(17) . . ?
C11 N4 Ni2 119.76(17) . . ?
N11 N10 Ni2 120.79(18) . . ?
N11 N10 Ni1 120.66(18) . . ?
Ni2 N10 Ni1 97.79(8) . . ?
C21 O1 Ni2 130.05(18) . . ?
N12 N11 N10 178.9(3) . . ?
C21 O2 Ni1 130.03(17) . . ?
C16 N6 C20 116.8(2) . . ?
C16 N6 Ni2 123.00(18) . . ?
C20 N6 Ni2 119.52(18) . . ?
C5 N1 C1 117.1(2) . . ?
C5 N1 Ni1 122.26(17) . . ?
C1 N1 Ni1 119.32(17) . . ?
N8 N7 Ni2 131.92(18) . . ?
N8 N7 Ni1 129.04(17) . . ?
Ni2 N7 Ni1 96.95(8) . . ?
N6 C16 N5 120.1(2) . . ?
N6 C16 C17 122.3(3) . . ?
N5 C16 C17 117.6(2) . . ?
N14 N13 Ni1 139.3(2) . . ?
C6 N3 C10 117.0(2) . . ?
C6 N3 Ni1 122.94(18) . . ?
C10 N3 Ni1 119.4(2) . . ?
C16 N5 C15 129.7(2) . . ?
C13 C14 C15 119.4(3) . . ?
O2 C21 O1 126.5(2) . . ?
O2 C21 C22 116.6(2) . . ?
O1 C21 C22 116.8(3) . . ?
N4 C15 N5 119.9(2) . . ?
N4 C15 C14 122.2(3) . . ?
N5 C15 C14 117.9(2) . . ?
C6 N2 C5 129.7(2) . . ?
N1 C5 N2 119.5(2) . . ?
N1 C5 C4 122.3(2) . . ?
N2 C5 C4 118.2(2) . . ?
C1 C2 C3 118.9(3) . . ?
C2 C1 N1 123.4(3) . . ?
N4 C11 C12 124.1(3) . . ?
C3 C4 C5 119.0(3) . . ?
C13 C12 C11 118.4(3) . . ?
C12 C13 C14 119.0(3) . . ?
C20 C19 C18 118.8(3) . . ?
C18 C17 C16 119.4(3) . . ?
N3 C10 C9 123.5(3) . . ?
C19 C20 N6 123.8(3) . . ?
C4 C3 C2 119.0(3) . . ?
C7 C8 C9 119.7(3) . . ?
C10 C9 C8 118.3(3) . . ?
C17 C18 C19 118.9(3) . . ?
N3 C6 N2 119.6(2) . . ?
N3 C6 C7 121.9(3) . . ?
N2 C6 C7 118.6(3) . . ?
N13 N14 N15 178.5(3) . . ?
C8 C7 C6 119.7(3) . . ?
N14 N15 Ni2 124.41(18) . 1_655 ?
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 O2 2.0226(18) . ?
Ni1 N1 2.058(2) . ?
Ni1 N3 2.060(2) . ?
Ni1 N13 2.071(2) . ?
Ni1 N10 2.125(2) . ?
Ni1 N7 2.142(2) . ?
Ni2 O1 2.0490(18) . ?
Ni2 N6 2.070(2) . ?
Ni2 N4 2.085(2) . ?
Ni2 N10 2.107(2) . ?
Ni2 N7 2.117(2) . ?
Ni2 N15 2.121(2) 1_455 ?
N8 N9 1.156(3) . ?
N8 N7 1.185(3) . ?
N4 C15 1.336(3) . ?
N4 C11 1.346(3) . ?
N10 N11 1.197(3) . ?
O1 C21 1.259(3) . ?
N11 N12 1.153(3) . ?
O2 C21 1.256(3) . ?
N6 C16 1.335(3) . ?
N6 C20 1.359(3) . ?
N1 C5 1.337(3) . ?
N1 C1 1.361(3) . ?
C16 N5 1.380(3) . ?
C16 C17 1.393(4) . ?
N13 N14 1.163(3) . ?
N3 C6 1.344(4) . ?
N3 C10 1.355(4) . ?
N5 C15 1.385(3) . ?
C14 C13 1.369(4) . ?
C14 C15 1.394(4) . ?
C21 C22 1.502(4) . ?
N2 C6 1.377(4) . ?
N2 C5 1.385(3) . ?
C5 C4 1.392(4) . ?
C2 C1 1.357(4) . ?
C2 C3 1.383(4) . ?
C11 C12 1.371(4) . ?
C4 C3 1.372(4) . ?
C12 C13 1.371(4) . ?
C19 C20 1.359(4) . ?
C19 C18 1.374(4) . ?
C17 C18 1.371(4) . ?
C10 C9 1.376(4) . ?
C8 C7 1.349(5) . ?
C8 C9 1.378(5) . ?
C6 C7 1.401(4) . ?
N14 N15 1.180(3) . ?
N15 Ni2 2.121(2) 1_655 ?
