#------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/51/45/1514503.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_1514503
loop_
_publ_author_name
'Cho, Jaeheung'
'Kang, Hye Yeon'
'Liu, Lei V.'
'Sarangi, Ritimukta'
'Solomon, Edward I.'
'Nam, Wonwoo'
_publ_section_title
;
 Mononuclear nickel(II)-superoxo and nickel(III)-peroxo complexes bearing
 a common macrocyclic TMC ligand.
;
_journal_issue                   4
_journal_name_full
'Chemical science (Royal Society of Chemistry : 2010)'
_journal_page_first              1502
_journal_page_last               1508
_journal_paper_doi               10.1039/C3SC22173C
_journal_volume                  4
_journal_year                    2013
_chemical_formula_sum            'C15 Cl2 N5 Ni O8'
_chemical_formula_weight         507.81
_chemical_name_systematic
;
?
;
_space_group_IT_number           129
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4a 2a'
_symmetry_space_group_name_H-M   'P 4/n m m :2'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.2584(6)
_cell_length_b                   9.2584(6)
_cell_length_c                   14.1473(17)
_cell_measurement_reflns_used    1470
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      20.00
_cell_measurement_theta_min      2.63
_cell_volume                     1212.68(18)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0619
_diffrn_reflns_av_sigmaI/netI    0.0542
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            7472
_diffrn_reflns_theta_full        28.24
_diffrn_reflns_theta_max         28.24
_diffrn_reflns_theta_min         1.44
_exptl_absorpt_coefficient_mu    1.065
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Blue
_exptl_crystal_density_diffrn    1.391
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             502
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.612
_refine_diff_density_min         -0.384
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_matrix_type           full
_refine_ls_number_parameters     75
_refine_ls_number_reflns         912
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0815
_refine_ls_R_factor_gt           0.0612
_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)+(0.1030P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1594
_refine_ls_wR_factor_ref         0.1651
_reflns_number_gt                565
_reflns_number_total             912
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3sc22173c.txt
_cod_data_source_block           cho092p4nmm
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      P4/nmm
_cod_database_code               1514503
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-y+1/2, x, z'
'y, -x+1/2, z'
'-x, y+1/2, -z'
'x+1/2, -y, -z'
'y+1/2, x+1/2, -z'
'-y, -x, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'y-1/2, -x, -z'
'-y, x-1/2, -z'
'x, -y-1/2, z'
'-x-1/2, y, z'
'-y-1/2, -x-1/2, z'
'y, x, 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
Ni1 Ni 0.2500 0.2500 0.75269(7) 0.0423(4) Uani 1 8 d S
Cl1 Cl 0.2500 0.2500 0.11623(17) 0.0618(7) Uani 1 8 d S
Cl2 Cl 0.7500 0.2500 0.5000 0.0878(10) Uani 1 8 d S
N2 N 0.2500 0.2500 0.6121(6) 0.068(2) Uani 1 8 d S
N1 N 0.4058(3) 0.0942(3) 0.7821(3) 0.0736(13) Uani 1 2 d S
C5 C 0.2500 0.2500 0.5352(8) 0.079(3) Uani 1 8 d S
C4 C 0.4754(5) 0.0246(5) 0.7002(6) 0.112(2) Uani 1 2 d S
O2 O 0.2500 0.2500 0.2120(9) 0.170(6) Uani 1 8 d S
O1 O 0.2500 0.1064(10) 0.0843(7) 0.187(4) Uani 0.75 2 d SP
C2 C 0.377(2) 0.0342(18) 0.8677(13) 0.075(5) Uani 0.25 1 d P
O3 O 0.7500 0.0923(17) 0.5084(12) 0.216(9) Uani 0.50 2 d SP
C1 C 0.3170(12) -0.0330(10) 0.8251(8) 0.165(5) Uani 0.75 1 d P
O4 O 0.6836(19) 0.2500 0.4195(10) 0.201(11) Uani 0.50 2 d SP
C6 C 0.2500 0.2500 0.4260(8) 0.126(6) Uani 1 8 d S
C3 C 0.2500 -0.052(4) 0.8741(19) 0.088(8) Uani 0.25 2 d SP
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'
Cl Cl 0.1484 0.1585 '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
N2 Ni1 N1 101.54(13) . .
N2 Ni1 N1 101.54(13) . 3
N1 Ni1 N1 87.71(5) . 3
N2 Ni1 N1 101.54(13) . 2
N1 Ni1 N1 156.9(3) . 2
N1 Ni1 N1 87.71(5) 3 2
N2 Ni1 N1 101.54(13) . 4
N1 Ni1 N1 87.71(5) . 4
N1 Ni1 N1 156.9(3) 3 4
N1 Ni1 N1 87.71(5) 2 4
O2 Cl1 O1 108.8(5) . 2
O2 Cl1 O1 108.8(5) . 4
O1 Cl1 O1 84.1(3) 2 4
O2 Cl1 O1 108.8(5) . 3
O1 Cl1 O1 84.1(3) 2 3
O1 Cl1 O1 142.5(10) 4 3
O2 Cl1 O1 108.8(5) . .
O1 Cl1 O1 142.5(10) 2 .
O1 Cl1 O1 84.1(3) 4 .
O1 Cl1 O1 84.1(3) 3 .
O4 Cl2 O4 56.7(18) . 2_655
O4 Cl2 O4 140.8(12) . 11_666
O4 Cl2 O4 140.8(12) 2_655 11_666
O4 Cl2 O4 140.8(12) . 12_656
O4 Cl2 O4 140.8(12) 2_655 12_656
O4 Cl2 O4 56.7(18) 11_666 12_656
O4 Cl2 O3 57.0(8) . 11_666
O4 Cl2 O3 113.7(14) 2_655 11_666
O4 Cl2 O3 94.1(6) 11_666 11_666
O4 Cl2 O3 94.1(6) 12_656 11_666
O4 Cl2 O3 113.7(14) . 12_656
O4 Cl2 O3 57.0(8) 2_655 12_656
O4 Cl2 O3 94.1(6) 11_666 12_656
O4 Cl2 O3 94.1(6) 12_656 12_656
O3 Cl2 O3 170.7(13) 11_666 12_656
O4 Cl2 O3 94.1(6) . .
O4 Cl2 O3 94.1(6) 2_655 .
O4 Cl2 O3 113.7(14) 11_666 .
O4 Cl2 O3 57.0(8) 12_656 .
O3 Cl2 O3 90.38(11) 11_666 .
O3 Cl2 O3 90.38(11) 12_656 .
O4 Cl2 O3 94.1(6) . 2_655
O4 Cl2 O3 94.1(6) 2_655 2_655
O4 Cl2 O3 57.0(8) 11_666 2_655
O4 Cl2 O3 113.7(14) 12_656 2_655
O3 Cl2 O3 90.38(11) 11_666 2_655
O3 Cl2 O3 90.38(11) 12_656 2_655
O3 Cl2 O3 170.7(13) . 2_655
C5 N2 Ni1 180.000(2) . .
C2 N1 C2 50.9(15) 15_665 .
C2 N1 C4 127.5(8) 15_665 .
C2 N1 C4 127.5(8) . .
C2 N1 C1 40.5(8) 15_665 15_665
C2 N1 C1 91.1(10) . 15_665
C4 N1 C1 101.9(5) . 15_665
C2 N1 C1 91.1(10) 15_665 .
C2 N1 C1 40.5(8) . .
C4 N1 C1 101.9(5) . .
C1 N1 C1 130.1(10) 15_665 .
C2 N1 Ni1 108.9(9) 15_665 .
C2 N1 Ni1 108.9(9) . .
C4 N1 Ni1 116.6(4) . .
C1 N1 Ni1 103.6(4) 15_665 .
C1 N1 Ni1 103.6(4) . .
N2 C5 C6 180.000(4) . .
C1 C2 C2 143.9(15) . 15_665
C1 C2 N1 80.3(15) . .
C2 C2 N1 64.6(8) 15_665 .
C1 C2 C3 41.7(17) . .
C2 C2 C3 168.6(13) 15_665 .
N1 C2 C3 116.7(17) . .
C1 C2 C1 31.7(11) . 14_655
C2 C2 C1 149.1(6) 15_665 14_655
N1 C2 C1 92.1(10) . 14_655
C3 C2 C1 26.0(11) . 14_655
O4 O3 Cl2 55.0(8) 12_656 .
C3 C1 C2 92(3) . .
C3 C1 C1 49.1(14) . 14_655
C2 C1 C1 122.5(16) . 14_655
C3 C1 N1 140(3) . .
C2 C1 N1 59.2(12) . .
C1 C1 N1 121.8(4) 14_655 .
C3 C1 C2 41.1(17) . 14_655
C2 C1 C2 97(2) . 14_655
C1 C1 C2 25.8(7) 14_655 14_655
N1 C1 C2 110.9(8) . 14_655
O4 O4 Cl2 61.6(9) 2_655 .
O4 O4 O3 129.7(10) 2_655 11_666
Cl2 O4 O3 68.0(10) . 11_666
C1 C3 C1 82(3) . 14_655
C1 C3 C2 113(3) . 14_655
C1 C3 C2 46.3(15) 14_655 14_655
C1 C3 C2 46.3(15) . .
C1 C3 C2 113(3) 14_655 .
C2 C3 C2 111(2) 14_655 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 N2 1.989(8) .
Ni1 N1 2.082(4) .
Ni1 N1 2.082(4) 3
Ni1 N1 2.082(4) 2
Ni1 N1 2.082(4) 4
Cl1 O2 1.355(12) .
Cl1 O1 1.404(8) 2
Cl1 O1 1.404(8) 4
Cl1 O1 1.404(8) 3
Cl1 O1 1.404(8) .
Cl2 O4 1.295(11) .
Cl2 O4 1.295(11) 2_655
Cl2 O4 1.295(11) 11_666
Cl2 O4 1.295(11) 12_656
Cl2 O3 1.465(15) 11_666
Cl2 O3 1.465(15) 12_656
Cl2 O3 1.465(15) .
Cl2 O3 1.465(15) 2_655
N2 C5 1.089(12) .
N1 C2 1.359(18) 15_665
N1 C2 1.359(18) .
N1 C4 1.475(8) .
N1 C1 1.560(9) 15_665
N1 C1 1.560(9) .
C5 C6 1.545(15) .
C2 C1 1.03(2) .
C2 C2 1.17(4) 15_665
C2 C3 1.42(3) .
C2 C1 1.991(18) 14_655
O3 O4 1.325(17) 12_656
C1 C3 0.95(2) .
C1 C1 1.24(2) 14_655
C1 C2 1.991(18) 14_655
O4 O4 1.23(4) 2_655
O4 O3 1.325(17) 11_666
C3 C1 0.95(2) 14_655
C3 C2 1.42(3) 14_655
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
N1 Ni1 N2 C5 33(100) . .
N1 Ni1 N2 C5 123(100) 3 .
N1 Ni1 N2 C5 -147(100) 2 .
N1 Ni1 N2 C5 -57(100) 4 .
N2 Ni1 N1 C2 153.0(8) . 15_665
N1 Ni1 N1 C2 51.7(9) 3 15_665
N1 Ni1 N1 C2 -27.0(8) 2 15_665
N1 Ni1 N1 C2 -105.7(8) 4 15_665
N2 Ni1 N1 C2 -153.0(8) . .
N1 Ni1 N1 C2 105.7(8) 3 .
N1 Ni1 N1 C2 27.0(8) 2 .
N1 Ni1 N1 C2 -51.7(9) 4 .
N2 Ni1 N1 C4 0.000(1) . .
N1 Ni1 N1 C4 -101.31(12) 3 .
N1 Ni1 N1 C4 180.000(2) 2 .
N1 Ni1 N1 C4 101.31(12) 4 .
N2 Ni1 N1 C1 111.1(5) . 15_665
N1 Ni1 N1 C1 9.8(6) 3 15_665
N1 Ni1 N1 C1 -68.9(5) 2 15_665
N1 Ni1 N1 C1 -147.6(5) 4 15_665
N2 Ni1 N1 C1 -111.1(5) . .
N1 Ni1 N1 C1 147.6(5) 3 .
N1 Ni1 N1 C1 68.9(5) 2 .
N1 Ni1 N1 C1 -9.8(6) 4 .
Ni1 N2 C5 C6 0(100) . .
C2 N1 C2 C1 -171.6(10) 15_665 .
C4 N1 C2 C1 -60.2(18) . .
C1 N1 C2 C1 -166.2(17) 15_665 .
Ni1 N1 C2 C1 89.0(14) . .
C4 N1 C2 C2 111.4(9) . 15_665
C1 N1 C2 C2 5.4(7) 15_665 15_665
C1 N1 C2 C2 171.6(10) . 15_665
Ni1 N1 C2 C2 -99.4(5) . 15_665
C2 N1 C2 C3 167.4(15) 15_665 .
C4 N1 C2 C3 -81.2(19) . .
C1 N1 C2 C3 172.9(18) 15_665 .
C1 N1 C2 C3 -21.0(17) . .
Ni1 N1 C2 C3 68.1(18) . .
C2 N1 C2 C1 158.9(4) 15_665 14_655
C4 N1 C2 C1 -89.7(10) . 14_655
C1 N1 C2 C1 164.3(9) 15_665 14_655
C1 N1 C2 C1 -29.5(10) . 14_655
Ni1 N1 C2 C1 59.5(8) . 14_655
O4 Cl2 O3 O4 -151.6(9) . 12_656
O4 Cl2 O3 O4 151.6(9) 2_655 12_656
O4 Cl2 O3 O4 0.000(5) 11_666 12_656
O3 Cl2 O3 O4 -94.6(7) 11_666 12_656
O3 Cl2 O3 O4 94.6(7) 12_656 12_656
O3 Cl2 O3 O4 0.000(14) 2_655 12_656
C2 C2 C1 C3 -164(2) 15_665 .
N1 C2 C1 C3 -151.3(18) . .
C1 C2 C1 C3 -41.0(19) 14_655 .
C2 C2 C1 C1 -123.3(18) 15_665 14_655
N1 C2 C1 C1 -110.3(9) . 14_655
C3 C2 C1 C1 41.0(19) . 14_655
C2 C2 C1 N1 -13.0(15) 15_665 .
C3 C2 C1 N1 151.3(18) . .
C1 C2 C1 N1 110.3(9) 14_655 .
C2 C2 C1 C2 -123.3(18) 15_665 14_655
N1 C2 C1 C2 -110.3(9) . 14_655
C3 C2 C1 C2 41.0(19) . 14_655
C1 C2 C1 C2 -0.002(5) 14_655 14_655
C2 N1 C1 C3 55(3) 15_665 .
C2 N1 C1 C3 49(3) . .
C4 N1 C1 C3 -176(3) . .
C1 N1 C1 C3 67(3) 15_665 .
Ni1 N1 C1 C3 -54(3) . .
C2 N1 C1 C2 6.5(8) 15_665 .
C4 N1 C1 C2 135.2(15) . .
C1 N1 C1 C2 18(2) 15_665 .
Ni1 N1 C1 C2 -103.2(16) . .
C2 N1 C1 C1 118.0(9) 15_665 14_655
C2 N1 C1 C1 111.5(16) . 14_655
C4 N1 C1 C1 -113.3(4) . 14_655
C1 N1 C1 C1 129.8(7) 15_665 14_655
Ni1 N1 C1 C1 8.3(5) . 14_655
C2 N1 C1 C2 91.8(14) 15_665 14_655
C2 N1 C1 C2 85(2) . 14_655
C4 N1 C1 C2 -139.4(9) . 14_655
C1 N1 C1 C2 103.6(9) 15_665 14_655
Ni1 N1 C1 C2 -17.9(10) . 14_655
O4 Cl2 O4 O4 131.4(2) 11_666 2_655
O4 Cl2 O4 O4 -131.3(2) 12_656 2_655
O3 Cl2 O4 O4 180.000(3) 11_666 2_655
O3 Cl2 O4 O4 0.000(2) 12_656 2_655
O3 Cl2 O4 O4 -92.2(3) . 2_655
O3 Cl2 O4 O4 92.2(3) 2_655 2_655
O4 Cl2 O4 O3 180.000(2) 2_655 11_666
O4 Cl2 O4 O3 -48.7(2) 11_666 11_666
O4 Cl2 O4 O3 48.7(2) 12_656 11_666
O3 Cl2 O4 O3 180.000(2) 12_656 11_666
O3 Cl2 O4 O3 87.8(3) . 11_666
O3 Cl2 O4 O3 -87.8(3) 2_655 11_666
C2 C1 C3 C1 133(2) . 14_655
N1 C1 C3 C1 93(3) . 14_655
C2 C1 C3 C1 35.0(12) 14_655 14_655
C2 C1 C3 C2 98(3) . 14_655
C1 C1 C3 C2 -35.0(12) 14_655 14_655
N1 C1 C3 C2 58(4) . 14_655
C1 C1 C3 C2 -133(2) 14_655 .
N1 C1 C3 C2 -40.3(19) . .
C2 C1 C3 C2 -98(3) 14_655 .
C2 C2 C3 C1 126(6) 15_665 .
N1 C2 C3 C1 32(2) . .
C1 C2 C3 C1 52(3) 14_655 .
C1 C2 C3 C1 -52(3) . 14_655
C2 C2 C3 C1 74(8) 15_665 14_655
N1 C2 C3 C1 -20(4) . 14_655
C1 C2 C3 C2 -102(3) . 14_655
C2 C2 C3 C2 24(8) 15_665 14_655
N1 C2 C3 C2 -70(3) . 14_655
C1 C2 C3 C2 -50(2) 14_655 14_655
