#------------------------------------------------------------------------------
#$Date: 2016-03-26 00:11:53 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180064 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/10/7051047.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_7051047
loop_
_publ_author_name
'Rahaman Laskar, Inamur'
'Das, Debasis'
'Mostafa, Golam'
'Lu, Tian-Huey'
'Keng, Tai-Chiun'
'Wang, Ju-Chun'
'Ghosh, Ashutosh'
'Ray Chaudhuri, Nirmalendu'
_publ_section_title
;
 First report on thermally induced nitro→ nitrito(O,O)
 linkage isomerization in diamine complexes of nickel(II) in the solid
 state: X-ray single crystal structural analyses of nitro and nitrito
 isomers
;
_journal_issue                   5
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              764
_journal_paper_doi               10.1039/b008254f
_journal_volume                  25
_journal_year                    2001
_chemical_formula_sum            'C16 H40 N6 Ni O4'
_chemical_formula_weight         439.25
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 96.470(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.3131(7)
_cell_length_b                   19.2548(12)
_cell_length_c                   12.0523(8)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      18
_cell_measurement_theta_min      12
_cell_volume                     2378.1(3)
_computing_molecular_graphics    'ORTEX (P.McArdle, 1995)'
_computing_publication_material  'SHELXL-97/2 (Sheldrick,1997)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_method       'scintillation counter'
_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  0.0243
_diffrn_reflns_av_sigmaI/netI    0.0258
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            6836
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.00
_exptl_absorpt_coefficient_mu    0.845
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.227
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Parallelepiped
_exptl_crystal_F_000             952
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.962
_refine_diff_density_min         -0.433
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.050
_refine_ls_goodness_of_fit_obs   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         3995
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_restrained_S_obs      1.049
_refine_ls_R_factor_all          0.0423
_refine_ls_R_factor_obs          0.0404
_refine_ls_shift/esd_max         -0.009
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0534P)²+2.1492P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1095
_refine_ls_wR_factor_obs         0.1069
_reflns_number_observed          3823
_reflns_number_total             3995
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b008254f.txt
_cod_data_source_block           1b
_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:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0534P)^2^+2.1492P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0534P)^2^+2.1492P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7051047
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Ni Ni 0.25427(3) 0.097063(14) 0.05852(2) 0.03195(13) Uani 1 d . .
N5 N 0.2411(2) -0.02895(11) -0.0100(2) 0.0480(5) Uani 1 d . .
O1 O 0.1536(2) 0.00025(9) 0.0382(2) 0.0452(4) Uani 1 d . .
O2 O 0.3361(2) 0.01113(9) -0.0200(2) 0.0454(4) Uani 1 d . .
N1 N 0.3540(2) 0.06849(12) 0.2166(2) 0.0429(5) Uani 1 d . .
H1 H 0.3169(2) 0.09391(12) 0.2683(2) 0.052 Uiso 1 calc R .
N2 N 0.4064(2) 0.16968(11) 0.0560(2) 0.0404(5) Uani 1 d . .
H2 H 0.3705(2) 0.21251(11) 0.0434(2) 0.049 Uiso 1 calc R .
N3 N 0.1541(2) 0.13507(10) -0.0932(2) 0.0399(5) Uani 1 d . .
H3 H 0.1994(2) 0.17312(10) -0.1117(2) 0.048 Uiso 1 calc R .
N4 N 0.1181(2) 0.15803(10) 0.1332(2) 0.0390(5) Uani 1 d . .
H4 H 0.1624(2) 0.18587(10) 0.1854(2) 0.047 Uiso 1 calc R .
C1 C 0.4863(3) 0.0963(2) 0.2150(3) 0.0551(8) Uani 1 d . .
H1A H 0.5349(3) 0.0673(2) 0.1685(3) 0.066 Uiso 1 calc R .
H1B H 0.5316(3) 0.0964(2) 0.2900(3) 0.066 Uiso 1 calc R .
C2 C 0.4779(3) 0.1689(2) 0.1696(2) 0.0540(7) Uani 1 d . .
H2A H 0.4332(3) 0.1984(2) 0.2185(2) 0.065 Uiso 1 calc R .
H2B H 0.5651(3) 0.1873(2) 0.1672(2) 0.065 Uiso 1 calc R .
C3 C 0.0290(3) 0.16122(14) -0.0629(2) 0.0470(6) Uani 1 d . .
H3A H -0.0288(3) 0.12259(14) -0.0524(2) 0.056 Uiso 1 calc R .
H3B H -0.0124(3) 0.19033(14) -0.1223(2) 0.056 Uiso 1 calc R .
C4 C 0.0528(3) 0.20252(13) 0.0433(3) 0.0475(7) Uani 1 d . .
H4A H 0.1072(3) 0.24235(13) 0.0318(3) 0.057 Uiso 1 calc R .
H4B H -0.0296(3) 0.21931(13) 0.0646(3) 0.057 Uiso 1 calc R .
C5 C 0.3526(4) -0.0049(2) 0.2554(3) 0.0664(9) Uani 1 d . .
H5A H 0.2646(4) -0.0227(2) 0.2385(3) 0.080 Uiso 1 calc R .
H5B H 0.4086(4) -0.0318(2) 0.2123(3) 0.080 Uiso 1 calc R .
C6 C 0.3941(8) -0.0170(3) 0.3740(4) 0.133(2) Uani 1 d . .
H6A H 0.3523(8) 0.0168(3) 0.4179(4) 0.159 Uiso 1 calc R .
H6B H 0.4877(8) -0.0101(3) 0.3883(4) 0.159 Uiso 1 calc R .
C7 C 0.3602(11) -0.0910(3) 0.4118(5) 0.179(4) Uani 1 d . .
H7A H 0.3892(11) -0.0964(3) 0.4899(5) 0.268 Uiso 1 calc R .
H7B H 0.4028(11) -0.1246(3) 0.3697(5) 0.268 Uiso 1 calc R .
H7C H 0.2675(11) -0.0977(3) 0.3994(5) 0.268 Uiso 1 calc R .
C8 C 0.4912(3) 0.15508(14) -0.0327(2) 0.0436(6) Uani 1 d . .
H8A H 0.4367(3) 0.14933(14) -0.1031(2) 0.052 Uiso 1 calc R .
H8B H 0.5366(3) 0.11156(14) -0.0158(2) 0.052 Uiso 1 calc R .
C9 C 0.5923(3) 0.2120(2) -0.0463(3) 0.0675(9) Uani 1 d . .
H9A H 0.5482(3) 0.2563(2) -0.0583(3) 0.081 Uiso 1 calc R .
H9B H 0.6520(3) 0.2154(2) 0.0217(3) 0.081 Uiso 1 calc R .
C10 C 0.6684(4) 0.1969(2) -0.1429(4) 0.0766(11) Uani 1 d . .
H10A H 0.7307(4) 0.2333(2) -0.1494(4) 0.115 Uiso 1 calc R .
H10B H 0.6097(4) 0.1943(2) -0.2105(4) 0.115 Uiso 1 calc R .
H10C H 0.7133(4) 0.1534(2) -0.1306(4) 0.115 Uiso 1 calc R .
C11 C 0.1389(4) 0.09073(15) -0.1938(2) 0.0544(8) Uani 1 d . .
H11A H 0.0779(4) 0.05376(15) -0.1825(2) 0.065 Uiso 1 calc R .
H11B H 0.2224(4) 0.06939(15) -0.2025(2) 0.065 Uiso 1 calc R .
C12 C 0.0911(5) 0.1286(2) -0.3010(3) 0.0891(14) Uani 1 d . .
H12A H 0.0066(5) 0.1491(2) -0.2935(3) 0.107 Uiso 1 calc R .
H12B H 0.1512(5) 0.1660(2) -0.3122(3) 0.107 Uiso 1 calc R .
C13 C 0.0790(7) 0.0820(2) -0.4025(3) 0.117(2) Uani 1 d . .
H13A H 0.0486(7) 0.1087(2) -0.4676(3) 0.153 Uiso 1 calc R .
H13B H 0.0181(7) 0.0454(2) -0.3929(3) 0.153 Uiso 1 calc R .
H13C H 0.1627(7) 0.0624(2) -0.4116(3) 0.153 Uiso 1 calc R .
C14 C 0.0251(3) 0.11486(13) 0.1887(2) 0.0413(6) Uani 1 d . .
H14A H 0.0746(3) 0.08259(13) 0.2388(2) 0.050 Uiso 1 calc R .
H14B H -0.0267(3) 0.08771(13) 0.1322(2) 0.050 Uiso 1 calc R .
C15 C -0.0668(3) 0.1554(2) 0.2548(3) 0.0620(8) Uani 1 d . .
H15A H -0.0158(3) 0.1828(2) 0.3116(3) 0.074 Uiso 1 calc R .
H15B H -0.1180(3) 0.1872(2) 0.2051(3) 0.074 Uiso 1 calc R .
C16 C -0.1572(3) 0.1086(2) 0.3098(3) 0.0647(9) Uani 1 d . .
H16A H -0.2134(3) 0.1361(2) 0.3505(3) 0.097 Uiso 1 calc R .
H16B H -0.1070(3) 0.0776(2) 0.3602(3) 0.097 Uiso 1 calc R .
H16C H -0.2091(3) 0.0821(2) 0.2538(3) 0.097 Uiso 1 calc R .
O3 O 0.2559(3) 0.2247(2) 0.3462(3) 0.0736(7) Uani 1 d . .
N6 N 0.2792(3) 0.1793(2) 0.3975(3) 0.0746(10) Uani 1 d . .
O4 O 0.3134(3) 0.1832(2) 0.4978(3) 0.0999(10) Uani 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
N2 Ni N4 99.78(8) . . ?
N2 Ni N3 92.84(8) . . ?
N4 Ni N3 83.87(8) . . ?
N2 Ni O2 100.15(8) . . ?
N4 Ni O2 160.01(8) . . ?
N3 Ni O2 93.66(8) . . ?
N2 Ni N1 84.21(9) . . ?
N4 Ni N1 92.28(9) . . ?
N3 Ni N1 174.70(8) . . ?
O2 Ni N1 91.20(8) . . ?
N2 Ni O1 158.82(8) . . ?
N4 Ni O1 101.34(8) . . ?
N3 Ni O1 91.10(8) . . ?
O2 Ni O1 58.80(7) . . ?
N1 Ni O1 93.24(8) . . ?
O1 N5 O2 112.0(2) . . ?
N5 O1 Ni 94.50(14) . . ?
N5 O2 Ni 94.69(14) . . ?
C1 N1 C5 113.1(2) . . ?
C1 N1 Ni 104.4(2) . . ?
C5 N1 Ni 120.3(2) . . ?
C2 N2 C8 113.1(2) . . ?
C2 N2 Ni 105.9(2) . . ?
C8 N2 Ni 112.7(2) . . ?
C3 N3 C11 112.8(2) . . ?
C3 N3 Ni 105.0(2) . . ?
C11 N3 Ni 120.2(2) . . ?
C4 N4 C14 112.9(2) . . ?
C4 N4 Ni 106.3(2) . . ?
C14 N4 Ni 112.07(15) . . ?
N1 C1 C2 109.2(2) . . ?
N2 C2 C1 110.4(2) . . ?
N3 C3 C4 109.2(2) . . ?
N4 C4 C3 109.5(2) . . ?
C6 C5 N1 116.5(3) . . ?
C5 C6 C7 112.5(5) . . ?
N2 C8 C9 113.9(2) . . ?
C10 C9 C8 111.4(3) . . ?
N3 C11 C12 114.6(3) . . ?
C13 C12 C11 113.2(3) . . ?
N4 C14 C15 114.9(2) . . ?
C16 C15 C14 112.1(3) . . ?
O3 N6 O4 122.3(4) . . ?
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
Ni N2 2.105(2) . ?
Ni N4 2.108(2) . ?
Ni N3 2.126(2) . ?
Ni O2 2.127(2) . ?
Ni N1 2.133(2) . ?
Ni O1 2.134(2) . ?
N5 O1 1.260(3) . ?
N5 O2 1.264(3) . ?
N1 C1 1.468(4) . ?
N1 C5 1.489(4) . ?
N2 C2 1.481(4) . ?
N2 C8 1.482(3) . ?
N3 C3 1.470(3) . ?
N3 C11 1.477(4) . ?
N4 C4 1.482(4) . ?
N4 C14 1.484(3) . ?
C1 C2 1.501(4) . ?
C3 C4 1.503(4) . ?
C5 C6 1.464(6) . ?
C6 C7 1.547(7) . ?
C8 C9 1.535(4) . ?
C9 C10 1.504(5) . ?
C11 C12 1.517(4) . ?
C12 C13 1.510(5) . ?
C14 C15 1.521(4) . ?
C15 C16 1.504(4) . ?
O3 N6 1.082(4) . ?
N6 O4 1.222(4) . ?
