#------------------------------------------------------------------------------
#$Date: 2016-03-23 01:40:27 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179150 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/11/4311124.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_4311124
loop_
_publ_author_name
'Xavi Ribas'
'João C. Dias'
'Jorge Morgado'
'Klaus Wurst'
'Isabel C. Santos'
'Manuel Almeida'
'José Vidal-Gancedo'
'Jaume Veciana'
'Concepció Rovira'
_publ_section_title
;
 Alkaline Side-Coordination Strategy for the Design of Nickel(II) and
 Nickel(III) Bis(1,2-diselenolene) Complex Based Materials
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3631
_journal_page_last               3641
_journal_paper_doi               10.1021/ic049860x
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C8 H8 N4 Na2 Ni O2 Se4'
_chemical_formula_weight         612.71
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                   14.6372(4)
_cell_length_b                   6.8642(2)
_cell_length_c                   15.5030(4)
_cell_measurement_reflns_used    9405
_cell_measurement_temperature    233(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      1.0
_cell_volume                     1557.63(7)
_computing_data_collection       'Kappa CCD'
_computing_data_reduction        'DENZO and SCALEPACK'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      233(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Kappa CCD'
_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  0.0591
_diffrn_reflns_av_sigmaI/netI    0.0308
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            8369
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.63
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    10.653
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.613
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.116
_refine_diff_density_min         -0.953
_refine_diff_density_rms         0.130
_refine_ls_extinction_coef       0.0028(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    'mixed, refined at O1'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     106
_refine_ls_number_reflns         1371
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.115
_refine_ls_R_factor_all          0.0325
_refine_ls_R_factor_gt           0.0293
_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)+(0.0405P)²+1.9030P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0751
_refine_ls_wR_factor_ref         0.0770
_reflns_number_gt                1248
_reflns_number_total             1371
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic049860xsi20040203_051712.cif
_cod_data_source_block           x3p37
_cod_database_code               4311124
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, 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
Ni1 Ni 0.5000 0.0000 0.5000 0.0219(2) Uani 1 2 d S . .
Na1 Na 0.39820(11) -0.4152(3) 0.53451(10) 0.0486(4) Uani 1 1 d . . .
Se1 Se 0.34746(3) 0.07917(6) 0.497485(19) 0.03357(19) Uani 1 1 d . . .
Se2 Se 0.49952(2) -0.03657(6) 0.64759(2) 0.02699(18) Uani 1 1 d . . .
N1 N 0.2256(2) 0.0994(4) 0.63544(18) 0.0288(7) Uani 1 1 d . . .
N2 N 0.3594(2) 0.0532(4) 0.76263(18) 0.0285(7) Uani 1 1 d . . .
C1 C 0.3131(2) 0.0728(5) 0.6153(2) 0.0238(7) Uani 1 1 d . . .
C2 C 0.3798(2) 0.0401(5) 0.6794(2) 0.0238(7) Uani 1 1 d . . .
C3 C 0.2716(3) 0.0884(5) 0.7824(2) 0.0317(8) Uani 1 1 d . . .
H3 H 0.2550 0.1025 0.8407 0.038 Uiso 1 1 calc . . .
C4 C 0.2057(3) 0.1045(5) 0.7204(2) 0.0321(8) Uani 1 1 d . . .
H4 H 0.1445 0.1196 0.7374 0.039 Uiso 1 1 calc . . .
O1 O 0.4720(2) -0.4443(4) 0.40140(18) 0.0370(6) Uani 1 1 d . . .
H1A H 0.484(3) -0.315(9) 0.381(3) 0.060(14) Uiso 1 1 d . . .
H1B H 0.444(4) -0.499(9) 0.364(3) 0.059(15) Uiso 1 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'
Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 '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
Se1 Ni1 Se1 180.0 . 5_656 ?
Se1 Ni1 Se2 87.726(11) . 5_656 ?
Se1 Ni1 Se2 92.274(11) 5_656 5_656 ?
Se1 Ni1 Se2 92.274(11) . . ?
Se1 Ni1 Se2 87.726(11) 5_656 . ?
Se2 Ni1 Se2 180.0 5_656 . ?
Se1 Ni1 Na1 103.56(3) . 5_656 ?
Se1 Ni1 Na1 76.44(3) 5_656 5_656 ?
Se2 Ni1 Na1 74.94(3) 5_656 5_656 ?
Se2 Ni1 Na1 105.06(3) . 5_656 ?
Se1 Ni1 Na1 76.44(3) . . ?
Se1 Ni1 Na1 103.56(3) 5_656 . ?
Se2 Ni1 Na1 105.06(3) 5_656 . ?
Se2 Ni1 Na1 74.94(3) . . ?
Na1 Ni1 Na1 180.0 5_656 . ?
O1 Na1 O1 87.96(11) . 5_646 ?
O1 Na1 N1 158.36(14) . 8_655 ?
O1 Na1 N1 110.61(12) 5_646 8_655 ?
O1 Na1 Ni1 73.66(8) . . ?
O1 Na1 Ni1 93.37(9) 5_646 . ?
N1 Na1 Ni1 114.61(9) 8_655 . ?
O1 Na1 Na1 44.13(9) . 5_646 ?
O1 Na1 Na1 43.84(8) 5_646 5_646 ?
N1 Na1 Na1 152.80(12) 8_655 5_646 ?
Ni1 Na1 Na1 81.14(6) . 5_646 ?
O1 Na1 Se2 108.22(10) . . ?
O1 Na1 Se2 75.42(9) 5_646 . ?
N1 Na1 Se2 87.82(8) 8_655 . ?
Ni1 Na1 Se2 39.86(2) . . ?
Na1 Na1 Se2 92.37(7) 5_646 . ?
O1 Na1 Se1 92.07(9) . . ?
O1 Na1 Se1 129.41(10) 5_646 . ?
N1 Na1 Se1 84.66(8) 8_655 . ?
Ni1 Na1 Se1 39.39(2) . . ?
Na1 Na1 Se1 117.86(8) 5_646 . ?
Se2 Na1 Se1 56.66(3) . . ?
C1 Se1 Ni1 103.66(10) . . ?
C1 Se1 Na1 82.91(10) . . ?
Ni1 Se1 Na1 64.17(3) . . ?
C2 Se2 Ni1 103.36(10) . . ?
C2 Se2 Na1 86.79(10) . . ?
Ni1 Se2 Na1 65.20(3) . . ?
C1 N1 C4 116.1(3) . . ?
C1 N1 Na1 124.6(2) . 8_665 ?
C4 N1 Na1 118.4(2) . 8_665 ?
C2 N2 C3 116.7(3) . . ?
N1 C1 C2 121.5(3) . . ?
N1 C1 Se1 118.6(2) . . ?
C2 C1 Se1 119.9(2) . . ?
N2 C2 C1 121.3(3) . . ?
N2 C2 Se2 118.6(2) . . ?
C1 C2 Se2 120.0(2) . . ?
N2 C3 C4 121.9(3) . . ?
N1 C4 C3 122.2(3) . . ?
H1B O1 H1A 107(5) . . ?
H1B O1 Na1 117(4) . . ?
H1A O1 Na1 107(3) . . ?
H1B O1 Na1 121(4) . 5_646 ?
H1A O1 Na1 112(3) . 5_646 ?
Na1 O1 Na1 92.04(11) . 5_646 ?
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 Se1 2.2983(4) . ?
Ni1 Se1 2.2983(4) 5_656 ?
Ni1 Se2 2.3019(4) 5_656 ?
Ni1 Se2 2.3019(4) . ?
Ni1 Na1 3.2600(18) 5_656 ?
Ni1 Na1 3.2600(18) . ?
Na1 O1 2.338(3) . ?
Na1 O1 2.350(4) 5_646 ?
Na1 N1 2.396(3) 8_655 ?
Na1 Na1 3.374(3) 5_646 ?
Na1 Se2 3.4679(18) . ?
Na1 Se1 3.5207(18) . ?
Se1 C1 1.894(3) . ?
Se2 C2 1.895(3) . ?
N1 C1 1.331(4) . ?
N1 C4 1.349(4) . ?
N1 Na1 2.396(3) 8_665 ?
N2 C2 1.327(4) . ?
N2 C3 1.344(5) . ?
C1 C2 1.411(5) . ?
C3 C4 1.366(6) . ?
O1 H1B 0.80(6) . ?
O1 H1A 0.96(6) . ?
O1 Na1 2.350(4) 5_646 ?
