#------------------------------------------------------------------------------
#$Date: 2016-03-25 13:23:34 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179841 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/37/7013729.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_7013729
loop_
_publ_author_name
'Kirin, Srecko I.'
'Happel, Christoph M.'
'Hrubanova, Silvia'
'Weyhermuller, Thomas'
'Klein, Christoph'
'Metzler-Nolte, Nils'
_publ_section_title
;
 Synthesis, structure and comparison of the DNA cleavage ability of
 metal complexes M(II)L with the
 N-(2-ethoxyethanol)-bis(2-picolyl)amine ligand L (M = Co, Ni, Cu and
 Zn).
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1201
_journal_page_last               1207
_journal_paper_doi               10.1039/b313634e
_journal_year                    2004
_chemical_formula_moiety         '[C16 H21 N4 Ni O5]+, (N O3)-'
_chemical_formula_sum            'C16 H21 N5 Ni O8'
_chemical_formula_weight         470.09
_chemical_name_systematic
;
?
;
_space_group_IT_number           144
_symmetry_cell_setting           trigonal
_symmetry_Int_Tables_number      144
_symmetry_space_group_name_Hall  'P 31'
_symmetry_space_group_name_H-M   'P 31'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   9.0763(3)
_cell_length_b                   9.0763(3)
_cell_length_c                   20.7667(6)
_cell_measurement_temperature    100(2)
_cell_volume                     1481.55(8)
_computing_cell_refinement       'Nonius Collect Software'
_computing_data_collection       'Nonius Collect Software'
_computing_data_reduction        'Nonius Collect Software'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Nonius Kappa-CCD'
_diffrn_measurement_method       '539 images at 1.0 deg. in ω, 10 sec./frame'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0280
_diffrn_reflns_av_sigmaI/netI    0.0317
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            19817
_diffrn_reflns_theta_full        30.96
_diffrn_reflns_theta_max         30.96
_diffrn_reflns_theta_min         3.92
_exptl_absorpt_coefficient_mu    1.038
_exptl_absorpt_correction_T_max  0.7206
_exptl_absorpt_correction_T_min  0.6887
_exptl_absorpt_correction_type   gaussian
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.581
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'transparent block'
_exptl_crystal_F_000             732
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.302
_refine_diff_density_min         -0.255
_refine_diff_density_rms         0.042
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.017(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     274
_refine_ls_number_reflns         4648
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0219
_refine_ls_R_factor_gt           0.0211
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0181P)²+0.3666P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0505
_refine_ls_wR_factor_ref         0.0510
_reflns_number_gt                4561
_reflns_number_total             4648
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b313634e.txt
_cod_data_source_block           1Ni(ST4465)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal' according
to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Gaussian' changed to
'gaussian' 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^)+(0.0181P)^2^+0.3666P] 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^)+(0.0181P)^2^+0.3666P] 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      P3(1)
_cod_database_code               7013729
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z+1/3'
'-x+y, -x, z+2/3'
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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.08578(2) 0.54990(2) 0.392110(8) 0.01231(4) Uani 1 d . . .
N1 N 0.16871(17) 0.39207(16) 0.42914(6) 0.0169(2) Uani 1 d . . .
C2 C 0.0748(2) 0.2301(2) 0.44831(8) 0.0225(3) Uani 1 d . . .
H2 H -0.0457 0.1779 0.4471 0.027 Uiso 1 calc R . .
C3 C 0.1475(3) 0.1358(2) 0.46993(8) 0.0291(4) Uani 1 d . . .
H3 H 0.0782 0.0211 0.4834 0.035 Uiso 1 calc R . .
C4 C 0.3224(3) 0.2124(2) 0.47137(9) 0.0311(4) Uani 1 d . . .
H4 H 0.3752 0.1509 0.4861 0.037 Uiso 1 calc R . .
C5 C 0.4215(2) 0.3805(2) 0.45108(8) 0.0269(3) Uani 1 d . . .
H5 H 0.5421 0.4346 0.4512 0.032 Uiso 1 calc R . .
C6 C 0.3401(2) 0.4673(2) 0.43065(7) 0.0190(3) Uani 1 d . . .
C7 C 0.43609(19) 0.6524(2) 0.41049(8) 0.0206(3) Uani 1 d . . .
H7A H 0.4544 0.7260 0.4483 0.025 Uiso 1 calc R . .
H7B H 0.5487 0.6810 0.3929 0.025 Uiso 1 calc R . .
N8 N 0.33683(16) 0.68212(16) 0.36112(6) 0.0156(2) Uani 1 d . . .
C9 C 0.38582(19) 0.86304(18) 0.35449(7) 0.0189(3) Uani 1 d . . .
H9A H 0.4764 0.9174 0.3216 0.023 Uiso 1 calc R . .
H9B H 0.4320 0.9221 0.3960 0.023 Uiso 1 calc R . .
C10 C 0.23579(19) 0.88194(18) 0.33512(7) 0.0178(3) Uani 1 d . . .
C11 C 0.2577(2) 1.0291(2) 0.30503(9) 0.0276(3) Uani 1 d . . .
H11 H 0.3679 1.1178 0.2933 0.033 Uiso 1 calc R . .
C12 C 0.1154(3) 1.0430(2) 0.29259(9) 0.0327(4) Uani 1 d . . .
H12 H 0.1271 1.1422 0.2724 0.039 Uiso 1 calc R . .
C13 C -0.0435(3) 0.9124(2) 0.30966(9) 0.0296(4) Uani 1 d . . .
H13 H -0.1424 0.9204 0.3017 0.035 Uiso 1 calc R . .
C14 C -0.0557(2) 0.7690(2) 0.33871(7) 0.0220(3) Uani 1 d . . .
H14 H -0.1649 0.6781 0.3501 0.026 Uiso 1 calc R . .
N15 N 0.08179(16) 0.75440(16) 0.35125(6) 0.0169(2) Uani 1 d . . .
C16 C 0.3463(2) 0.6053(2) 0.29865(7) 0.0215(3) Uani 1 d . . .
H16A H 0.3673 0.5101 0.3074 0.026 Uiso 1 calc R . .
H16B H 0.4431 0.6918 0.2731 0.026 Uiso 1 calc R . .
C17 C 0.1845(2) 0.5402(2) 0.26002(7) 0.0232(3) Uani 1 d . . .
H17A H 0.1688 0.6356 0.2458 0.028 Uiso 1 calc R . .
H17B H 0.1875 0.4773 0.2215 0.028 Uiso 1 calc R . .
O18 O 0.04994(14) 0.42931(14) 0.30269(5) 0.0201(2) Uani 1 d . . .
C19 C -0.1209(2) 0.3697(2) 0.28048(8) 0.0267(3) Uani 1 d . . .
H19A H -0.1481 0.2917 0.2434 0.032 Uiso 1 calc R . .
H19B H -0.1359 0.4663 0.2673 0.032 Uiso 1 calc R . .
C20 C -0.2322(2) 0.2781(2) 0.33701(9) 0.0282(4) Uani 1 d . . .
H20A H -0.3524 0.2413 0.3271 0.034 Uiso 1 calc R . .
H20B H -0.2238 0.1762 0.3476 0.034 Uiso 1 calc R . .
O21 O -0.17362(14) 0.39551(15) 0.39067(6) 0.0218(2) Uani 1 d . . .
H21 H -0.223(3) 0.345(3) 0.4287(11) 0.026 Uiso 1 d . . .
N30 N 0.01802(17) 0.68135(16) 0.51107(6) 0.0179(2) Uani 1 d . . .
O31 O 0.12380(14) 0.64609(15) 0.48358(5) 0.0198(2) Uani 1 d . . .
O32 O -0.09797(15) 0.68068(16) 0.47999(6) 0.0241(2) Uani 1 d . . .
O33 O 0.03649(17) 0.71479(17) 0.56941(6) 0.0290(3) Uani 1 d . . .
N40 N -0.34687(18) 0.14506(19) 0.52339(7) 0.0268(3) Uani 1 d . . .
O41 O -0.27686(19) 0.30026(17) 0.50872(7) 0.0344(3) Uani 1 d . . .
O42 O -0.3546(2) 0.04099(19) 0.48300(9) 0.0471(4) Uani 1 d . . .
O43 O -0.40516(19) 0.1025(2) 0.57862(7) 0.0444(4) 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
O31 Ni1 O21 101.31(5) . . ?
O31 Ni1 N15 94.20(5) . . ?
O21 Ni1 N15 94.50(5) . . ?
O31 Ni1 N1 84.74(5) . . ?
O21 Ni1 N1 102.88(5) . . ?
N15 Ni1 N1 162.48(5) . . ?
O31 Ni1 N8 97.98(5) . . ?
O21 Ni1 N8 160.60(5) . . ?
N15 Ni1 N8 81.95(5) . . ?
N1 Ni1 N8 80.88(5) . . ?
O31 Ni1 O18 173.62(5) . . ?
O21 Ni1 O18 78.76(5) . . ?
N15 Ni1 O18 92.15(5) . . ?
N1 Ni1 O18 89.02(5) . . ?
N8 Ni1 O18 82.31(5) . . ?
C2 N1 C6 119.22(14) . . ?
C2 N1 Ni1 128.14(11) . . ?
C6 N1 Ni1 112.59(10) . . ?
N1 C2 C3 122.27(17) . . ?
C4 C3 C2 118.51(17) . . ?
C3 C4 C5 119.72(16) . . ?
C6 C5 C4 118.58(17) . . ?
N1 C6 C5 121.70(15) . . ?
N1 C6 C7 115.63(13) . . ?
C5 C6 C7 122.66(15) . . ?
N8 C7 C6 109.25(12) . . ?
C7 N8 C9 113.32(12) . . ?
C7 N8 C16 109.55(12) . . ?
C9 N8 C16 112.46(12) . . ?
C7 N8 Ni1 105.82(9) . . ?
C9 N8 Ni1 107.74(9) . . ?
C16 N8 Ni1 107.55(9) . . ?
N8 C9 C10 111.33(12) . . ?
N15 C10 C11 121.83(15) . . ?
N15 C10 C9 116.54(13) . . ?
C11 C10 C9 121.54(14) . . ?
C12 C11 C10 118.58(16) . . ?
C13 C12 C11 119.75(16) . . ?
C12 C13 C14 118.48(16) . . ?
N15 C14 C13 122.28(16) . . ?
C10 N15 C14 119.08(13) . . ?
C10 N15 Ni1 113.70(10) . . ?
C14 N15 Ni1 127.21(11) . . ?
N8 C16 C17 111.83(13) . . ?
O18 C17 C16 105.43(12) . . ?
C17 O18 C19 116.41(12) . . ?
C17 O18 Ni1 108.98(8) . . ?
C19 O18 Ni1 109.68(9) . . ?
O18 C19 C20 104.93(13) . . ?
O21 C20 C19 107.28(13) . . ?
C20 O21 Ni1 112.81(10) . . ?
O32 N30 O33 121.58(13) . . ?
O32 N30 O31 120.52(12) . . ?
O33 N30 O31 117.89(13) . . ?
N30 O31 Ni1 122.01(9) . . ?
O42 N40 O43 122.40(16) . . ?
O42 N40 O41 119.57(16) . . ?
O43 N40 O41 118.03(16) . . ?
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 O31 2.0465(11) . ?
Ni1 O21 2.0514(12) . ?
Ni1 N15 2.0576(12) . ?
Ni1 N1 2.0708(13) . ?
Ni1 N8 2.0765(12) . ?
Ni1 O18 2.0966(10) . ?
N1 C2 1.339(2) . ?
N1 C6 1.351(2) . ?
C2 C3 1.391(2) . ?
C3 C4 1.379(3) . ?
C4 C5 1.394(3) . ?
C5 C6 1.388(2) . ?
C6 C7 1.514(2) . ?
C7 N8 1.4762(19) . ?
N8 C9 1.4775(19) . ?
N8 C16 1.4955(19) . ?
C9 C10 1.510(2) . ?
C10 N15 1.3371(19) . ?
C10 C11 1.396(2) . ?
C11 C12 1.383(3) . ?
C12 C13 1.379(3) . ?
C13 C14 1.387(2) . ?
C14 N15 1.345(2) . ?
C16 C17 1.510(2) . ?
C17 O18 1.4355(19) . ?
O18 C19 1.439(2) . ?
C19 C20 1.500(3) . ?
C20 O21 1.447(2) . ?
N30 O32 1.2324(17) . ?
N30 O33 1.2398(16) . ?
N30 O31 1.2875(16) . ?
N40 O42 1.239(2) . ?
N40 O43 1.241(2) . ?
N40 O41 1.2594(18) . ?
