#------------------------------------------------------------------------------
#$Date: 2016-03-25 13:23:34 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179841 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/37/7013730.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_7013730
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 Co N4 O5]+, (NO3)-'
_chemical_formula_sum            'C16 H21 Co N5 O8'
_chemical_formula_weight         470.31
_chemical_name_systematic
;
?
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      33
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.6361(6)
_cell_length_b                   9.8378(3)
_cell_length_c                   13.0708(5)
_cell_measurement_temperature    100(2)
_cell_volume                     2010.61(13)
_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       'ω, 1.0 deg/frame, 30 sec. each'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0624
_diffrn_reflns_av_sigmaI/netI    0.0385
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            36199
_diffrn_reflns_theta_full        31.00
_diffrn_reflns_theta_max         31.00
_diffrn_reflns_theta_min         3.96
_exptl_absorpt_coefficient_mu    0.908
_exptl_absorpt_correction_type   'not corrected'
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.554
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'transparent block'
_exptl_crystal_F_000             972
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.618
_refine_diff_density_min         -0.581
_refine_diff_density_rms         0.063
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.018(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     274
_refine_ls_number_reflns         6370
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0331
_refine_ls_R_factor_gt           0.0309
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0436P)²+0.3140P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0768
_refine_ls_wR_factor_ref         0.0781
_reflns_number_gt                6076
_reflns_number_total             6370
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b313634e.txt
_cod_data_source_block           1Co(ST4538)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
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^)+(0.0436P)^2^+0.3140P] 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^)+(0.0436P)^2^+0.3140P] 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      Pna2(1)
_cod_database_code               7013730
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'x+1/2, -y+1/2, z'
'-x+1/2, 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_adp_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.742604(10) 0.135046(18) 0.92203(2) 0.01368(5) Uani 1 d . . .
N1 N 0.66644(8) 0.29339(14) 0.86952(10) 0.0154(2) Uani 1 d . . .
C2 C 0.58988(9) 0.27503(17) 0.82449(12) 0.0183(3) Uani 1 d . . .
H2 H 0.5682 0.1853 0.8172 0.022 Uiso 1 calc R . .
C3 C 0.54179(10) 0.38302(18) 0.78848(13) 0.0207(3) Uani 1 d . . .
H3 H 0.4881 0.3677 0.7565 0.025 Uiso 1 calc R . .
C4 C 0.57332(10) 0.51382(17) 0.79979(12) 0.0201(3) Uani 1 d . . .
H4 H 0.5417 0.5894 0.7751 0.024 Uiso 1 calc R . .
C5 C 0.65145(10) 0.53304(16) 0.84754(12) 0.0177(3) Uani 1 d . . .
H5 H 0.6734 0.6221 0.8576 0.021 Uiso 1 calc R . .
C6 C 0.69757(9) 0.41981(15) 0.88064(11) 0.0151(3) Uani 1 d . . .
C7 C 0.78627(8) 0.43233(13) 0.92505(14) 0.0160(2) Uani 1 d . . .
H7A H 0.8287 0.4385 0.8690 0.019 Uiso 1 calc R . .
H7B H 0.7902 0.5164 0.9665 0.019 Uiso 1 calc R . .
N8 N 0.80553(8) 0.31303(13) 0.98995(9) 0.0140(2) Uani 1 d . . .
C9 C 0.89841(9) 0.28462(16) 0.99775(12) 0.0176(3) Uani 1 d . . .
H9A H 0.9215 0.3299 1.0595 0.021 Uiso 1 calc R . .
H9B H 0.9279 0.3234 0.9374 0.021 Uiso 1 calc R . .
C10 C 0.91722(10) 0.13427(15) 1.00369(12) 0.0171(3) Uani 1 d . . .
C11 C 0.99344(10) 0.08653(19) 1.04478(12) 0.0213(3) Uani 1 d . . .
H11 H 1.0332 0.1476 1.0749 0.026 Uiso 1 calc R . .
C12 C 1.01061(11) -0.0524(2) 1.04114(13) 0.0246(3) Uani 1 d . . .
H12 H 1.0625 -0.0872 1.0684 0.030 Uiso 1 calc R . .
C13 C 0.95144(12) -0.13899(18) 0.99750(15) 0.0248(3) Uani 1 d . . .
H13 H 0.9620 -0.2340 0.9940 0.030 Uiso 1 calc R . .
C14 C 0.87661(11) -0.08490(18) 0.95903(14) 0.0228(3) Uani 1 d . . .
H14 H 0.8357 -0.1444 0.9293 0.027 Uiso 1 calc R . .
N15 N 0.85941(8) 0.04938(14) 0.96216(10) 0.0172(2) Uani 1 d . . .
C16 C 0.76614(10) 0.33436(17) 1.09293(12) 0.0169(3) Uani 1 d . . .
H16A H 0.7123 0.3863 1.0852 0.020 Uiso 1 calc R . .
H16B H 0.8055 0.3885 1.1360 0.020 Uiso 1 calc R . .
C17 C 0.74765(10) 0.20157(18) 1.14487(13) 0.0187(3) Uani 1 d . . .
H17A H 0.8013 0.1509 1.1579 0.022 Uiso 1 calc R . .
H17B H 0.7180 0.2167 1.2108 0.022 Uiso 1 calc R . .
O18 O 0.69391(8) 0.12828(11) 1.07537(9) 0.0179(2) Uani 1 d . . .
C19 C 0.67424(11) -0.00868(17) 1.10561(12) 0.0205(3) Uani 1 d . . .
H19A H 0.6413 -0.0095 1.1703 0.025 Uiso 1 calc R . .
H19B H 0.7273 -0.0622 1.1152 0.025 Uiso 1 calc R . .
C20 C 0.62178(10) -0.06566(17) 1.01947(13) 0.0212(3) Uani 1 d . . .
H20A H 0.6121 -0.1642 1.0298 0.025 Uiso 1 calc R . .
H20B H 0.5656 -0.0196 1.0162 0.025 Uiso 1 calc R . .
O21 O 0.66896(6) -0.04277(11) 0.92637(10) 0.0198(2) Uani 1 d D . .
H21 H 0.6440(14) -0.079(2) 0.8710(11) 0.026 Uiso 1 d D . .
N30 N 0.79659(9) 0.15606(13) 0.70922(11) 0.0177(2) Uani 1 d . . .
O31 O 0.75250(7) 0.07689(13) 0.76574(9) 0.0214(2) Uani 1 d . . .
O32 O 0.84649(8) 0.23875(13) 0.74993(10) 0.0248(2) Uani 1 d . . .
O33 O 0.78922(11) 0.14875(13) 0.61540(10) 0.0295(3) Uani 1 d . . .
N40 N 0.50120(9) -0.12987(14) 0.78407(11) 0.0197(3) Uani 1 d . . .
O41 O 0.58058(8) -0.15646(13) 0.77740(10) 0.0253(3) Uani 1 d . . .
O42 O 0.47777(9) -0.03484(16) 0.83912(13) 0.0376(4) Uani 1 d . . .
O43 O 0.44977(9) -0.20061(16) 0.73570(13) 0.0366(3) 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'
Co Co 0.3494 0.9721 '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 Co1 N15 153.00(5) . . ?
N1 Co1 O21 108.66(5) . . ?
N15 Co1 O21 97.91(5) . . ?
N1 Co1 O31 85.76(5) . . ?
N15 Co1 O31 93.98(5) . . ?
O21 Co1 O31 80.88(5) . . ?
N1 Co1 O18 97.38(5) . . ?
N15 Co1 O18 93.64(5) . . ?
O21 Co1 O18 75.74(5) . . ?
O31 Co1 O18 156.18(5) . . ?
N1 Co1 N8 78.02(5) . . ?
N15 Co1 N8 80.07(5) . . ?
O21 Co1 N8 154.30(5) . . ?
O31 Co1 N8 124.76(5) . . ?
O18 Co1 N8 78.81(4) . . ?
C6 N1 C2 119.58(14) . . ?
C6 N1 Co1 116.79(10) . . ?
C2 N1 Co1 123.62(11) . . ?
N1 C2 C3 121.93(15) . . ?
C2 C3 C4 118.88(15) . . ?
C5 C4 C3 119.26(14) . . ?
C4 C5 C6 119.11(15) . . ?
N1 C6 C5 121.20(14) . . ?
N1 C6 C7 116.76(13) . . ?
C5 C6 C7 121.95(13) . . ?
N8 C7 C6 110.07(11) . . ?
C7 N8 C9 112.86(11) . . ?
C7 N8 C16 108.73(12) . . ?
C9 N8 C16 111.60(11) . . ?
C7 N8 Co1 108.03(9) . . ?
C9 N8 Co1 108.45(9) . . ?
C16 N8 Co1 106.94(9) . . ?
N8 C9 C10 112.27(12) . . ?
N15 C10 C11 121.51(15) . . ?
N15 C10 C9 117.17(13) . . ?
C11 C10 C9 121.21(15) . . ?
C10 C11 C12 118.93(16) . . ?
C13 C12 C11 119.34(15) . . ?
C14 C13 C12 118.72(16) . . ?
N15 C14 C13 122.39(16) . . ?
C10 N15 C14 119.10(14) . . ?
C10 N15 Co1 116.14(10) . . ?
C14 N15 Co1 124.38(11) . . ?
N8 C16 C17 111.38(13) . . ?
O18 C17 C16 105.33(12) . . ?
C17 O18 C19 115.03(12) . . ?
C17 O18 Co1 111.64(9) . . ?
C19 O18 Co1 111.22(9) . . ?
O18 C19 C20 105.11(13) . . ?
O21 C20 C19 107.18(12) . . ?
C20 O21 Co1 115.77(10) . . ?
O33 N30 O32 121.39(14) . . ?
O33 N30 O31 119.31(14) . . ?
O32 N30 O31 119.31(14) . . ?
N30 O31 Co1 115.54(10) . . ?
O42 N40 O43 122.05(15) . . ?
O42 N40 O41 119.02(14) . . ?
O43 N40 O41 118.93(14) . . ?
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
Co1 N1 2.0774(13) . ?
Co1 N15 2.0787(13) . ?
Co1 O21 2.0951(10) . ?
Co1 O31 2.1270(12) . ?
Co1 O18 2.1451(12) . ?
Co1 N8 2.1959(13) . ?
N1 C6 1.343(2) . ?
N1 C2 1.3462(19) . ?
C2 C3 1.384(2) . ?
C3 C4 1.386(2) . ?
C4 C5 1.385(2) . ?
C5 C6 1.396(2) . ?
C6 C7 1.508(2) . ?
C7 N8 1.4791(19) . ?
N8 C9 1.4826(18) . ?
N8 C16 1.495(2) . ?
C9 C10 1.510(2) . ?
C10 N15 1.345(2) . ?
C10 C11 1.389(2) . ?
C11 C12 1.394(3) . ?
C12 C13 1.381(3) . ?
C13 C14 1.380(2) . ?
C14 N15 1.349(2) . ?
C16 C17 1.500(2) . ?
C17 O18 1.432(2) . ?
O18 C19 1.4374(19) . ?
C19 C20 1.502(2) . ?
C20 O21 1.441(2) . ?
N30 O33 1.2338(19) . ?
N30 O32 1.2464(18) . ?
N30 O31 1.2758(18) . ?
N40 O42 1.2353(19) . ?
N40 O43 1.2372(19) . ?
N40 O41 1.2716(18) . ?
