#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/06/2210649.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2210649
loop_
_publ_author_name
'Hong-Wei Lin'
'Zhen-Feng Chen'
_publ_section_title
;
 Bis{2-[2-(ethylamino)ethyliminomethyl]-4-nitrophenolato}cobalt(III)
 nitrate
;
_journal_coeditor_code           HG2103
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m2512
_journal_page_last               m2514
_journal_paper_doi               10.1107/S1600536806035446
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '[Co (C11 H14 N3 O3)2], N O3'
_chemical_formula_moiety         'C22 H28 Co N6 O6 +, N O3 -'
_chemical_formula_sum            'C22 H28 Co N7 O9'
_chemical_formula_weight         593.44
_chemical_name_systematic
;
Bis{2-[2-(ethylamino)ethyliminomethyl]-4-nitrophenolato}cobalt(III) nitrate
;
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_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                   12.0410(10)
_cell_length_b                   11.4360(10)
_cell_length_c                   18.908(2)
_cell_measurement_reflns_used    3542
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      23.7
_cell_measurement_theta_min      2.4
_cell_volume                     2603.6(4)
_computing_cell_refinement       'SAINT (Bruker, 2000)'
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Bruker, 2000)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area-detector'
_diffrn_measurement_method       ω
_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  0.0472
_diffrn_reflns_av_sigmaI/netI    0.0323
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            21071
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.15
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.724
_exptl_absorpt_correction_T_max  0.8512
_exptl_absorpt_correction_T_min  0.8015
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.514
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1232
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.380
_refine_diff_density_min         -0.235
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     182
_refine_ls_number_reflns         3001
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0681
_refine_ls_R_factor_gt           0.0458
_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)+(0.0652P)²+0.9222P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1167
_refine_ls_wR_factor_ref         0.1304
_reflns_number_gt                2148
_reflns_number_total             3001
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            hg2103.cif
_cod_data_source_block           I
_cod_original_cell_volume        2603.7(4)
_cod_database_code               2210649
_cod_database_fobs_code          2210649
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'-x, y, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'x, -y, z-1/2'
'-x-1/2, y-1/2, z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
Co Co1 0.0000 0.03402(4) 0.2500 0.03881(17) Uani d S 1
O O1 -0.04502(14) 0.15390(16) 0.31330(9) 0.0483(4) Uani d . 1
O O2 0.1788(3) 0.5372(3) 0.49678(17) 0.1081(10) Uani d . 1
O O3 0.3038(2) 0.4062(3) 0.50192(16) 0.1093(10) Uani d . 1
O O4 0.4249(3) 0.1867(3) 0.2741(2) 0.1395(15) Uani d . 1
O O5 0.5000 0.0270(4) 0.2500 0.139(2) Uani d S 1
N N1 0.14924(16) 0.03026(18) 0.28435(11) 0.0420(5) Uani d . 1
N N2 0.05317(18) -0.0857(2) 0.18109(11) 0.0465(5) Uani d D 1
N N3 0.2153(3) 0.4417(3) 0.48053(15) 0.0734(8) Uani d . 1
N N4 0.5000 0.1301(4) 0.2500 0.0778(12) Uani d S 1
C C1 0.1363(2) 0.1976(2) 0.36031(12) 0.0436(6) Uani d . 1
C C2 0.0216(2) 0.2209(2) 0.34820(13) 0.0450(6) Uani d . 1
C C3 -0.0214(2) 0.3244(3) 0.37833(16) 0.0607(8) Uani d . 1
H H3 -0.0954 0.3433 0.3702 0.073 Uiso calc R 1
C C4 0.0408(3) 0.3975(3) 0.41863(16) 0.0622(8) Uani d . 1
H H4 0.0103 0.4662 0.4364 0.075 Uiso calc R 1
C C5 0.1505(2) 0.3685(3) 0.43308(14) 0.0551(7) Uani d . 1
C C6 0.1975(2) 0.2706(2) 0.40488(14) 0.0515(7) Uani d . 1
H H6 0.2709 0.2522 0.4154 0.062 Uiso calc R 1
C C7 0.1931(2) 0.1020(2) 0.32743(13) 0.0447(6) Uani d . 1
H H7 0.2677 0.0916 0.3384 0.054 Uiso calc R 1
C C8 0.2161(2) -0.0634(3) 0.25286(15) 0.0546(7) Uani d . 1
H H8A 0.2062 -0.1358 0.2788 0.065 Uiso calc R 1
H H8B 0.2942 -0.0428 0.2534 0.065 Uiso calc R 1
C C9 0.1756(2) -0.0765(3) 0.17860(15) 0.0592(8) Uani d . 1
H H9A 0.1975 -0.0093 0.1506 0.071 Uiso calc R 1
H H9B 0.2072 -0.1461 0.1573 0.071 Uiso calc R 1
C C10 0.0039(2) -0.0847(3) 0.10897(15) 0.0602(8) Uani d . 1
H H10A 0.0210 -0.0105 0.0865 0.072 Uiso calc R 1
H H10B -0.0762 -0.0906 0.1129 0.072 Uiso calc R 1
C C11 0.0458(3) -0.1828(4) 0.06262(18) 0.0843(11) Uani d . 1
H H11A 0.1233 -0.1715 0.0531 0.127 Uiso calc R 1
H H11B 0.0052 -0.1832 0.0189 0.127 Uiso calc R 1
H H11C 0.0353 -0.2561 0.0864 0.127 Uiso calc R 1
H H2 0.034(3) -0.1550(16) 0.2004(17) 0.080 Uiso d D 1
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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 Co1 O1 . 3 87.56(11) y
O1 Co1 N1 . 3 87.82(8) y
O1 Co1 N1 3 3 94.04(8) ?
O1 Co1 N1 . . 94.04(8) y
O1 Co1 N1 3 . 87.82(8) ?
N1 Co1 N1 3 . 177.43(13) y
O1 Co1 N2 . 3 89.57(9) y
O1 Co1 N2 3 3 176.84(8) ?
N1 Co1 N2 3 3 84.54(9) ?
N1 Co1 N2 . 3 93.69(9) y
O1 Co1 N2 . . 176.84(8) y
O1 Co1 N2 3 . 89.57(9) ?
N1 Co1 N2 3 . 93.69(9) ?
N1 Co1 N2 . . 84.54(9) y
N2 Co1 N2 3 . 93.33(13) y
C2 O1 Co1 . . 124.97(16) ?
C7 N1 C8 . . 120.3(2) ?
C7 N1 Co1 . . 126.42(18) ?
C8 N1 Co1 . . 113.23(16) ?
C9 N2 C10 . . 111.6(2) ?
C9 N2 Co1 . . 106.95(17) ?
C10 N2 Co1 . . 117.71(18) ?
C9 N2 H2 . . 109(2) ?
C10 N2 H2 . . 106(2) ?
Co1 N2 H2 . . 105(2) ?
O3 N3 O2 . . 122.4(3) ?
O3 N3 C5 . . 119.0(3) ?
O2 N3 C5 . . 118.6(3) ?
O5 N4 O4 . . 122.6(2) ?
O5 N4 O4 . 3_655 122.6(2) ?
O4 N4 O4 . 3_655 114.8(4) ?
C6 C1 C2 . . 119.8(2) ?
C6 C1 C7 . . 117.8(2) ?
C2 C1 C7 . . 122.4(2) ?
O1 C2 C3 . . 118.4(2) ?
O1 C2 C1 . . 125.0(2) ?
C3 C2 C1 . . 116.5(2) ?
C4 C3 C2 . . 122.7(3) ?
C4 C3 H3 . . 118.6 ?
C2 C3 H3 . . 118.6 ?
C3 C4 C5 . . 119.2(3) ?
C3 C4 H4 . . 120.4 ?
C5 C4 H4 . . 120.4 ?
C6 C5 C4 . . 120.9(3) ?
C6 C5 N3 . . 119.5(3) ?
C4 C5 N3 . . 119.6(3) ?
C5 C6 C1 . . 120.5(3) ?
C5 C6 H6 . . 119.7 ?
C1 C6 H6 . . 119.7 ?
N1 C7 C1 . . 125.0(2) ?
N1 C7 H7 . . 117.5 ?
C1 C7 H7 . . 117.5 ?
N1 C8 C9 . . 106.0(2) ?
N1 C8 H8A . . 110.5 ?
C9 C8 H8A . . 110.5 ?
N1 C8 H8B . . 110.5 ?
C9 C8 H8B . . 110.5 ?
H8A C8 H8B . . 108.7 ?
N2 C9 C8 . . 107.6(2) ?
N2 C9 H9A . . 110.2 ?
C8 C9 H9A . . 110.2 ?
N2 C9 H9B . . 110.2 ?
C8 C9 H9B . . 110.2 ?
H9A C9 H9B . . 108.5 ?
N2 C10 C11 . . 113.1(3) ?
N2 C10 H10A . . 109.0 ?
C11 C10 H10A . . 109.0 ?
N2 C10 H10B . . 109.0 ?
C11 C10 H10B . . 109.0 ?
H10A C10 H10B . . 107.8 ?
C10 C11 H11A . . 109.5 ?
C10 C11 H11B . . 109.5 ?
H11A C11 H11B . . 109.5 ?
C10 C11 H11C . . 109.5 ?
H11A C11 H11C . . 109.5 ?
H11B C11 H11C . . 109.5 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Co1 O1 . 1.899(2) y
Co1 O1 3 1.899(2) ?
Co1 N1 3 1.911(2) ?
Co1 N1 . 1.911(2) y
Co1 N2 3 1.996(2) ?
Co1 N2 . 1.996(2) y
O1 C2 . 1.291(3) ?
O2 N3 . 1.217(4) ?
O3 N3 . 1.209(4) ?
O4 N4 . 1.202(4) ?
O5 N4 . 1.179(5) ?
N1 C7 . 1.271(3) ?
N1 C8 . 1.466(3) ?
N2 C9 . 1.479(3) ?
N2 C10 . 1.487(4) ?
N2 H2 . 0.902(10) ?
N3 C5 . 1.454(4) ?
N4 O4 3_655 1.202(4) ?
C1 C6 . 1.396(4) ?
C1 C2 . 1.424(3) ?
C1 C7 . 1.432(4) ?
C2 C3 . 1.413(4) ?
C3 C4 . 1.356(4) ?
C3 H3 . 0.9300 ?
C4 C5 . 1.390(4) ?
C4 H4 . 0.9300 ?
C5 C6 . 1.363(4) ?
C6 H6 . 0.9300 ?
C7 H7 . 0.9300 ?
C8 C9 . 1.494(4) ?
C8 H8A . 0.9700 ?
C8 H8B . 0.9700 ?
C9 H9A . 0.9700 ?
C9 H9B . 0.9700 ?
C10 C11 . 1.510(4) ?
C10 H10A . 0.9700 ?
C10 H10B . 0.9700 ?
C11 H11A . 0.9600 ?
C11 H11B . 0.9600 ?
C11 H11C . 0.9600 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
N2 H2 O4 6_556 0.902(10) 2.288(17) 3.142(4) 158(3)
N2 H2 O4 8_655 0.902(10) 2.337(19) 3.152(4) 150(3)
