#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:13:32 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179051 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/13/4301326.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_4301326
loop_
_publ_author_name
'Grigory B. Andreev'
'Nina A. Budantseva'
'Ivan G. Tananaev'
'Boris F. Myasoedov'
_publ_contact_author_address
;
A. N. Frumkin Institute of Physical Chemistry and 
Electrochemistry, 31 Leninskiy pr., Moscow, 119991, Russia
;
_publ_contact_author_email       grigory_andreev@mail.ru
_publ_contact_author_name        'Grigory Andreev'
_publ_section_title
;
Interaction of Transuranium Elements with Biologically Important Molecules:
Structural and Spectroscopic Study of Np(V) Complexes with Imidazole
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1232
_journal_page_last               1235
_journal_paper_doi               10.1021/ic801882p
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'C12 H16 N9 Np O4'
_chemical_formula_sum            'C12 H16 N9 Np O4'
_chemical_formula_weight         587.34
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                101.547(3)
_cell_angle_beta                 104.552(3)
_cell_angle_gamma                95.024(3)
_cell_formula_units_Z            2
_cell_length_a                   8.0715(4)
_cell_length_b                   8.0920(5)
_cell_length_c                   14.5070(8)
_cell_measurement_temperature    100(2)
_cell_volume                     889.01(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker Kappa APEX II 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  0.0317
_diffrn_reflns_av_sigmaI/netI    0.0271
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            22712
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         1.49
_exptl_absorpt_coefficient_mu    5.884
_exptl_absorpt_correction_T_max  0.55
_exptl_absorpt_correction_T_min  0.42
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'APEX 2 (Bruker, 2006)'
_exptl_crystal_density_diffrn    2.194
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             552
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.522
_refine_diff_density_min         -2.005
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         5150
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0508
_refine_ls_R_factor_gt           0.0500
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1000P)²+6.5000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1348
_refine_ls_wR_factor_ref         0.1357
_reflns_number_gt                4931
_reflns_number_total             5150
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic801882p_si_001_3.cif
_cod_data_source_block           3
_cod_database_code               4301326
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Np1 Np -0.47962(3) 0.00808(3) 0.256679(14) 0.00993(10) Uani 1 1 d . . .
O1 O -0.5804(7) -0.1019(6) 0.3333(4) 0.0149(9) Uani 1 1 d . . .
O2 O -0.3820(7) 0.1206(7) 0.1796(4) 0.0165(9) Uani 1 1 d . . .
O3 O -0.2362(7) -0.1692(7) 0.2646(4) 0.0192(10) Uani 1 1 d . . .
O4 O -0.0971(10) -0.3721(9) 0.2347(4) 0.0351(16) Uani 1 1 d . . .
N7 N -0.2298(8) 0.1327(7) 0.4086(4) 0.0133(10) Uani 1 1 d . . .
N1 N -0.6004(9) -0.2420(8) 0.1095(4) 0.0181(11) Uani 1 1 d . . .
N5 N -0.5456(9) 0.2958(8) 0.3372(4) 0.0181(11) Uani 1 1 d . . .
N3 N -0.7816(9) 0.0519(9) 0.1681(4) 0.0193(11) Uani 1 1 d . . .
N6 N -0.5897(10) 0.5620(8) 0.3594(5) 0.0233(13) Uani 1 1 d . . .
H6A H -0.5817 0.6672 0.3560 0.028 Uiso 1 1 calc R . .
N8 N -0.0640(10) 0.1849(10) 0.5601(5) 0.0243(13) Uani 1 1 d . . .
H8A H -0.0289 0.1830 0.6209 0.029 Uiso 1 1 calc R . .
N4 N -1.0536(9) 0.0926(10) 0.1451(5) 0.0256(14) Uani 1 1 d . . .
H4A H -1.1590 0.0835 0.1481 0.031 Uiso 1 1 calc R . .
N2 N -0.6654(10) -0.3933(10) -0.0421(5) 0.0272(15) Uani 1 1 d . . .
H2A H -0.6675 -0.4233 -0.1027 0.033 Uiso 1 1 calc R . .
N9 N -0.2408(10) -0.3240(9) 0.2218(5) 0.0263(14) Uani 1 1 d . . .
C9 C -0.5057(10) 0.4437(9) 0.3187(5) 0.0190(13) Uani 1 1 d . . .
H9A H -0.4295 0.4643 0.2823 0.023 Uiso 1 1 calc R . .
C1 C -0.5716(10) -0.2523(10) 0.0227(5) 0.0205(13) Uani 1 1 d . . .
H1A H -0.4970 -0.1732 0.0084 0.025 Uiso 1 1 calc R . .
C10 C -0.2139(10) 0.1018(9) 0.4970(5) 0.0188(13) Uani 1 1 d . . .
H10A H -0.2953 0.0323 0.5130 0.023 Uiso 1 1 calc R . .
C12 C -0.0815(10) 0.2394(9) 0.4180(5) 0.0183(12) Uani 1 1 d . . .
H12A H -0.0559 0.2829 0.3677 0.022 Uiso 1 1 calc R . .
C11 C 0.0230(11) 0.2727(10) 0.5114(5) 0.0233(14) Uani 1 1 d . . .
H11A H 0.1304 0.3407 0.5365 0.028 Uiso 1 1 calc R . .
C7 C -0.6597(12) 0.3202(10) 0.3930(6) 0.0272(17) Uani 1 1 d . . .
H7A H -0.7094 0.2371 0.4177 0.033 Uiso 1 1 calc R . .
C2 C -0.7573(11) -0.4813(10) 0.0059(6) 0.0253(15) Uani 1 1 d . . .
H2B H -0.8327 -0.5832 -0.0203 0.030 Uiso 1 1 calc R . .
C3 C -0.7144(11) -0.3874(10) 0.0993(5) 0.0242(15) Uani 1 1 d . . .
H3A H -0.7554 -0.4164 0.1492 0.029 Uiso 1 1 calc R . .
C8 C -0.6890(14) 0.4868(11) 0.4064(8) 0.034(2) Uani 1 1 d . . .
H8B H -0.7617 0.5373 0.4406 0.040 Uiso 1 1 calc R . .
C6 C -0.8152(14) 0.1604(18) 0.1076(10) 0.051(3) Uani 1 1 d . . .
H6B H -0.7363 0.2065 0.0792 0.061 Uiso 1 1 calc R . .
C5 C -0.9792(17) 0.191(2) 0.0948(12) 0.069(5) Uani 1 1 d . . .
H5A H -1.0323 0.2643 0.0590 0.083 Uiso 1 1 calc R . .
C4 C -0.9269(10) 0.0140(11) 0.1884(5) 0.0212(14) Uani 1 1 d . . .
H4B H -0.9409 -0.0593 0.2286 0.025 Uiso 1 1 calc R . .
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'
Np Np -11.4937 4.1493 '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
O1 Np1 O2 178.9(2) . . ?
O1 Np1 O3 94.0(2) . . ?
O2 Np1 O3 87.0(2) . . ?
O1 Np1 N7 87.6(2) . . ?
O2 Np1 N7 92.9(2) . . ?
O3 Np1 N7 68.87(17) . . ?
O1 Np1 N3 87.8(2) . . ?
O2 Np1 N3 91.3(2) . . ?
O3 Np1 N3 148.58(19) . . ?
N7 Np1 N3 142.53(19) . . ?
O1 Np1 N1 91.1(2) . . ?
O2 Np1 N1 89.0(2) . . ?
O3 Np1 N1 76.67(19) . . ?
N7 Np1 N1 145.33(19) . . ?
N3 Np1 N1 71.9(2) . . ?
O1 Np1 N5 91.7(2) . . ?
O2 Np1 N5 87.5(2) . . ?
O3 Np1 N5 140.9(2) . . ?
N7 Np1 N5 72.75(19) . . ?
N3 Np1 N5 70.2(2) . . ?
N1 Np1 N5 141.9(2) . . ?
N9 O3 Np1 128.9(5) . . ?
C10 N7 C12 105.1(6) . . ?
C10 N7 Np1 126.1(5) . . ?
C12 N7 Np1 128.8(4) . . ?
C1 N1 C3 105.6(6) . . ?
C1 N1 Np1 125.0(5) . . ?
C3 N1 Np1 129.3(4) . . ?
C9 N5 C7 106.1(6) . . ?
C9 N5 Np1 126.9(5) . . ?
C7 N5 Np1 125.8(5) . . ?
C4 N3 C6 105.4(7) . . ?
C4 N3 Np1 128.0(5) . . ?
C6 N3 Np1 124.5(6) . . ?
C9 N6 C8 108.2(6) . . ?
C10 N8 C11 108.5(6) . . ?
C4 N4 C5 105.3(7) . . ?
C1 N2 C2 108.1(6) . . ?
O4 N9 O3 113.8(7) . . ?
N5 C9 N6 110.9(6) . . ?
N1 C1 N2 110.8(7) . . ?
N7 C10 N8 110.7(7) . . ?
C11 C12 N7 110.5(6) . . ?
N8 C11 C12 105.2(7) . . ?
C8 C7 N5 109.3(7) . . ?
C3 C2 N2 105.4(7) . . ?
C2 C3 N1 110.2(6) . . ?
N6 C8 C7 105.5(7) . . ?
C5 C6 N3 109.7(8) . . ?
C6 C5 N4 106.8(9) . . ?
N3 C4 N4 112.6(6) . . ?
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
Np1 O1 1.847(5) . ?
Np1 O2 1.851(5) . ?
Np1 O3 2.526(5) . ?
Np1 N7 2.542(6) . ?
Np1 N3 2.545(7) . ?
Np1 N1 2.546(6) . ?
Np1 N5 2.551(6) . ?
O3 N9 1.274(8) . ?
O4 N9 1.237(10) . ?
N7 C10 1.332(8) . ?
N7 C12 1.374(9) . ?
N1 C1 1.324(8) . ?
N1 C3 1.388(10) . ?
N5 C9 1.309(9) . ?
N5 C7 1.373(9) . ?
N3 C4 1.305(9) . ?
N3 C6 1.358(10) . ?
N6 C9 1.346(9) . ?
N6 C8 1.354(10) . ?
N8 C10 1.345(10) . ?
N8 C11 1.363(10) . ?
N4 C4 1.340(10) . ?
N4 C5 1.376(12) . ?
N2 C1 1.349(10) . ?
N2 C2 1.381(11) . ?
C12 C11 1.364(10) . ?
C7 C8 1.372(11) . ?
C2 C3 1.355(10) . ?
C6 C5 1.342(15) . ?
