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#$Date: 2016-03-24 02:01:11 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179551 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/20/4502049.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_4502049
loop_
_publ_author_name
'Callejo, Lorena M.'
'de la Pinta, Noelia'
'Madariaga, Gotzon'
'Fidalgo, Luz'
'Lezama, Luis'
'Cortés, Roberto'
_publ_section_title
;
 Structural, Spectroscopic, and Magnetic Characterization of the
 Coordination Polymers [MII(NCS)2(bpe)2]·3H2O·2C2H6SO [M =
 Co, Ni; bpe = 1,2-Bis(4-pyridyl)ethylene]. Two Interpenetrated Porous
 Networks
;
_journal_issue                   11
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              4874
_journal_paper_doi               10.1021/cg100919a
_journal_volume                  10
_journal_year                    2010
_chemical_formula_moiety         'C26 H20 N6 Ni S2, 4(C O0.50 S0.50), 3(O)'
_chemical_formula_sum            'C30 H20 N6 Ni O5 S4'
_chemical_formula_weight         731.47
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           130
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4a 2ac'
_symmetry_space_group_name_H-M   'P 4/n c c :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.000
_cell_angle_beta                 90.000
_cell_angle_gamma                90.000
_cell_formula_units_Z            4
_cell_length_a                   15.6228(19)
_cell_length_b                   15.6228(19)
_cell_length_c                   15.732(2)
_cell_measurement_reflns_used    3436
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.68
_cell_measurement_theta_min      2.90
_cell_volume                     3839.7(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.953
_diffrn_measured_fraction_theta_max 0.953
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0537
_diffrn_reflns_av_sigmaI/netI    0.0756
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            15330
_diffrn_reflns_theta_full        24.68
_diffrn_reflns_theta_max         24.68
_diffrn_reflns_theta_min         2.90
_exptl_absorpt_coefficient_mu    0.764
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.265
_exptl_crystal_density_meas      1.300
_exptl_crystal_density_method    flotation
_exptl_crystal_description       prism
_exptl_crystal_F_000             1496
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.295
_refine_diff_density_min         -0.176
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     133
_refine_ls_number_reflns         1558
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.1162
_refine_ls_R_factor_gt           0.0418
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0450P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0960
_refine_ls_wR_factor_ref         0.1075
_reflns_number_gt                786
_reflns_number_total             1558
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg100919a_si_002.cif
_cod_data_source_block           286ni
_cod_original_sg_symbol_H-M      'P 4/n c c'
_cod_database_code               4502049
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'x+1/2, -y, -z+1/2'
'-x, y+1/2, -z+1/2'
'-y, -x, -z+1/2'
'y+1/2, x+1/2, -z+1/2'
'y, -x+1/2, z'
'-y+1/2, x, z'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'-x-1/2, y, z-1/2'
'x, -y-1/2, z-1/2'
'y, x, z-1/2'
'-y-1/2, -x-1/2, z-1/2'
'-y, x-1/2, -z'
'y-1/2, -x, -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
Ni1 Ni 0.7500 0.2500 0.2500 0.0369(3) Uani 1 4 d S
N1 N 0.8193(2) 0.1819(2) 0.34437(16) 0.0417(7) Uani 1 1 d .
C1 C 0.7809(3) 0.1341(3) 0.4030(2) 0.0544(12) Uani 1 1 d .
H1 H 0.7216 0.1370 0.4076 0.082 Uiso 1 1 calc R
C2 C 0.8247(3) 0.0804(3) 0.4575(2) 0.0590(12) Uani 1 1 d .
H2 H 0.7950 0.0492 0.4983 0.088 Uiso 1 1 calc R
C3 C 0.9134(3) 0.0730(3) 0.4513(2) 0.0523(11) Uani 1 1 d .
C4 C 0.9540(3) 0.1254(3) 0.3920(2) 0.0545(12) Uani 1 1 d .
H4 H 1.0133 0.1254 0.3871 0.082 Uiso 1 1 calc R
C5 C 0.9048(3) 0.1768(2) 0.3411(2) 0.0495(11) Uani 1 1 d .
H5 H 0.9329 0.2107 0.3013 0.074 Uiso 1 1 calc R
C6 C 0.9608(2) 0.0115(3) 0.5049(3) 0.0609(13) Uani 1 1 d .
H6 H 0.9311 -0.0128 0.5500 0.091 Uiso 1 1 calc R
N2 N 0.6571(2) 0.1571(2) 0.2500 0.0490(11) Uani 1 2 d S
C7 C 0.6059(3) 0.1059(3) 0.2500 0.0695(18) Uani 1 2 d S
S1 S 0.5520(4) 0.0146(5) 0.2554(13) 0.142(4) Uani 0.50 1 d P
S2 S 0.887(2) -0.147(3) 0.365(5) 1.27(7) Uani 0.50 1 d PD
C21 C 0.799(4) -0.098(2) 0.312(3) 0.71(7) Uani 0.50 1 d PD
C22 C 0.886(5) -0.245(5) 0.308(7) 1.6(3) Uani 0.50 1 d PD
O2 O 0.852(6) -0.170(3) 0.453(4) 1.46(19) Uani 0.50 1 d PD
O1W O 0.8836(11) -0.2012(10) 0.125(2) 0.531(16) Uani 0.75 1 d P
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'
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'
S S 0.1246 0.1234 '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'
H H 0.0000 0.0000 '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
N2 Ni1 N2 180.0 2_655 .
N2 Ni1 N1 89.64(11) 2_655 .
N2 Ni1 N1 90.36(11) . .
N2 Ni1 N1 90.36(11) 2_655 5_665
N2 Ni1 N1 89.64(11) . 5_665
N1 Ni1 N1 88.76(14) . 5_665
N2 Ni1 N1 89.64(11) 2_655 6_545
N2 Ni1 N1 90.36(11) . 6_545
N1 Ni1 N1 179.3(2) . 6_545
N1 Ni1 N1 91.25(14) 5_665 6_545
N2 Ni1 N1 90.37(11) 2_655 2_655
N2 Ni1 N1 89.64(11) . 2_655
N1 Ni1 N1 91.25(14) . 2_655
N1 Ni1 N1 179.3(2) 5_665 2_655
N1 Ni1 N1 88.76(14) 6_545 2_655
C1 N1 C5 116.3(3) . .
C1 N1 Ni1 122.5(3) . .
C5 N1 Ni1 120.8(3) . .
N1 C1 C2 123.3(4) . .
N1 C1 H1 118.4 . .
C2 C1 H1 118.4 . .
C1 C2 C3 120.0(4) . .
C1 C2 H2 120.0 . .
C3 C2 H2 120.0 . .
C4 C3 C2 116.8(4) . .
C4 C3 C6 122.4(4) . .
C2 C3 C6 120.8(4) . .
C5 C4 C3 118.7(4) . .
C5 C4 H4 120.7 . .
C3 C4 H4 120.7 . .
N1 C5 C4 124.9(4) . .
N1 C5 H5 117.5 . .
C4 C5 H5 117.5 . .
C6 C6 C3 126.3(5) 9_756 .
C6 C6 H6 116.9 9_756 .
C3 C6 H6 116.9 . .
C7 N2 Ni1 180.0(4) . .
N2 C7 S1 165.3(3) . .
O2 S2 C22 105.02(7) . .
O2 S2 C21 105.04(7) . .
C22 S2 C21 97.60(6) . .
C22 C21 S2 131(10) 8_545 .
C21 C22 S2 142(9) 7_655 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 N2 2.053(5) .
Ni1 N1 2.123(3) .
N1 C1 1.330(5) .
N1 C5 1.340(4) .
C1 C2 1.380(5) .
C1 H1 0.9300 .
C2 C3 1.394(5) .
C2 H2 0.9300 .
C3 C4 1.393(5) .
C3 C6 1.477(5) .
C4 C5 1.370(5) .
C4 H4 0.9300 .
C5 H5 0.9300 .
C6 C6 1.285(7) 9_756
C6 H6 0.9300 .
N2 C7 1.132(6) .
C7 S1 1.658(7) .
S2 O2 1.5261(5) .
S2 C22 1.7729(6) .
S2 C21 1.7730(6) .
C21 C22 0.88(5) 8_545
C22 C21 0.88(5) 7_655
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
N2 Ni1 N1 C1 148.5(3) 2_655 .
N2 Ni1 N1 C1 -31.5(3) . .
N1 Ni1 N1 C1 -121.2(4) 5_665 .
N1 Ni1 N1 C1 58.1(3) 2_655 .
N2 Ni1 N1 C5 -39.8(3) 2_655 .
N2 Ni1 N1 C5 140.2(3) . .
N1 Ni1 N1 C5 50.5(2) 5_665 .
N1 Ni1 N1 C5 -130.2(4) 2_655 .
C5 N1 C1 C2 -1.1(6) . .
Ni1 N1 C1 C2 170.9(3) . .
N1 C1 C2 C3 -1.4(7) . .
C1 C2 C3 C4 3.6(6) . .
C1 C2 C3 C6 -175.8(4) . .
C2 C3 C4 C5 -3.4(6) . .
C6 C3 C4 C5 176.0(4) . .
C1 N1 C5 C4 1.4(6) . .
Ni1 N1 C5 C4 -170.8(3) . .
C3 C4 C5 N1 1.0(6) . .
C4 C3 C6 C6 -12.1(8) . 9_756
C2 C3 C6 C6 167.3(6) . 9_756
N2 C7 S1 S1 180.002(3) . 6_545
O2 S2 C21 C22 -47(10) . 8_545
C22 S2 C21 C22 61(10) . 8_545
O2 S2 C22 C21 -48(17) . 7_655
C21 S2 C22 C21 -155(17) . 7_655
