#------------------------------------------------------------------------------
#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/81/2228157.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_2228157
loop_
_publ_author_name
'Quinn-Elmore, Benjamin G.'
'Buchner, James D.'
'Beach, Keith B.'
'Knaust, Jacqueline M.'
_publ_section_title
;
 Poly[[tetrakis(μ₂-pyrazine
 N,N'-dioxide-κ²O:O')neodymium(III)]
 tris(perchlorate)]
;
_journal_coeditor_code           ZL2298
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1104
_journal_page_last               m1105
_journal_paper_doi               10.1107/S1600536810031818
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '[Nd (C4 H4 N2 O2)4] (Cl O4)3'
_chemical_formula_moiety         'C16 H16 N8 Nd O8 3+, 3(Cl O4 -)'
_chemical_formula_sum            'C16 H16 Cl3 N8 Nd O20'
_chemical_formula_weight         890.96
_chemical_name_systematic
;
Poly[[tetrakis(μ₂-pyrazine
N,N'-dioxide-κ²O:O')neodymium(III)]
tris(perchlorate)]
;
_space_group_IT_number           142
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4bd 2c'
_symmetry_space_group_name_H-M   'I 41/a c d :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   15.3804(4)
_cell_length_b                   15.3804(4)
_cell_length_c                   22.9843(12)
_cell_measurement_reflns_used    15053
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.5215
_cell_measurement_theta_min      2.578
_cell_volume                     5437.1(3)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2007)'
_computing_data_collection       'SMART (Bruker, 2007)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2007)'
_computing_molecular_graphics    'X-SEED (Barbour, 2001)'
_computing_publication_material  'X-SEED (Barbour, 2001)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       'ω 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  0.0239
_diffrn_reflns_av_sigmaI/netI    0.0100
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            30711
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         30.52
_diffrn_reflns_theta_min         2.58
_exptl_absorpt_coefficient_mu    2.315
_exptl_absorpt_correction_T_max  0.659
_exptl_absorpt_correction_T_min  0.593
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2001)'
_exptl_crystal_colour            Rose
_exptl_crystal_density_diffrn    2.177
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3512
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.18
_refine_diff_density_max         2.267
_refine_diff_density_min         -1.946
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     110
_refine_ls_number_reflns         2086
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0410
_refine_ls_R_factor_gt           0.0376
_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)+(0.0535P)²+38.3560P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1027
_refine_ls_wR_factor_ref         0.1062
_reflns_number_gt                1842
_reflns_number_total             2086
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            zl2298.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'I 41/a c d'
_cod_database_code               2228157
_cod_database_fobs_code          2228157
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y+1/4, x+3/4, z+1/4'
'-x, -y+1/2, z'
'y+1/4, -x+1/4, z+3/4'
'x, -y, -z+1/2'
'-x+1/2, y, -z'
'y+3/4, x+1/4, -z+1/4'
'-y+1/4, -x+1/4, -z+1/4'
'x+1/2, y+1/2, z+1/2'
'-y+3/4, x+5/4, z+3/4'
'-x+1/2, -y+1, z+1/2'
'y+3/4, -x+3/4, z+5/4'
'x+1/2, -y+1/2, -z+1'
'-x+1, y+1/2, -z+1/2'
'y+5/4, x+3/4, -z+3/4'
'-y+3/4, -x+3/4, -z+3/4'
'-x, -y, -z'
'y-1/4, -x-3/4, -z-1/4'
'x, y-1/2, -z'
'-y-1/4, x-1/4, -z-3/4'
'-x, y, z-1/2'
'x-1/2, -y, z'
'-y-3/4, -x-1/4, z-1/4'
'y-1/4, x-1/4, z-1/4'
'-x+1/2, -y+1/2, -z+1/2'
'y+1/4, -x-1/4, -z+1/4'
'x+1/2, y, -z+1/2'
'-y+1/4, x+1/4, -z-1/4'
'-x+1/2, y+1/2, z'
'x, -y+1/2, z+1/2'
'-y-1/4, -x+1/4, z+1/4'
'y+1/4, x+1/4, z+1/4'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Nd Nd1 0.5000 0.2500 0.3750 0.00589(11) Uani d S 1 . .
Cl Cl1 0.5000 0.2500 0.1250 0.0119(3) Uani d S 1 . .
Cl Cl2 0.72544(6) -0.02456(6) 0.1250 0.0319(3) Uani d S 1 . .
O O1 0.59191(12) 0.21965(14) 0.29303(8) 0.0171(4) Uani d . 1 . .
O O2 0.53338(14) 0.39686(12) 0.34324(8) 0.0168(4) Uani d . 1 . .
O O3 0.57573(16) 0.24613(16) 0.16135(10) 0.0277(5) Uani d . 1 . .
O O4 0.6477(5) -0.0172(6) 0.1497(5) 0.191(4) Uani d . 1 . .
O O5 0.7895(5) -0.0023(6) 0.1623(5) 0.180(5) Uani d . 1 . .
N N1 0.66963(15) 0.23449(15) 0.27293(10) 0.0141(4) Uani d . 1 . .
N N2 0.52833(15) 0.44642(14) 0.29745(9) 0.0129(4) Uani d . 1 . .
C C1 0.70832(17) 0.17377(17) 0.23897(11) 0.0154(5) Uani d . 1 . .
H H1 0.6797 0.1202 0.2315 0.018 Uiso calc R 1 . .
C C2 0.78886(16) 0.18959(17) 0.21540(11) 0.0152(5) Uani d . 1 . .
H H2 0.8155 0.1475 0.1910 0.018 Uiso calc R 1 . .
C C3 0.52715(18) 0.41238(16) 0.24314(11) 0.0148(5) Uani d . 1 . .
H H3 0.5264 0.3511 0.2380 0.018 Uiso calc R 1 . .
C C4 0.52702(18) 0.46617(16) 0.19547(11) 0.0147(5) Uani d . 1 . .
H H4 0.5260 0.4420 0.1574 0.018 Uiso calc R 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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nd Nd -0.1943 3.0179 '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 Nd1 O1 15_445 16 76.62(10) ?
O1 Nd1 O1 15_445 . 147.62(10) ?
O1 Nd1 O1 16 . 112.75(10) ?
O1 Nd1 O1 15_445 3_655 112.75(10) ?
O1 Nd1 O1 16 3_655 147.62(10) ?
O1 Nd1 O1 . 3_655 76.63(10) ?
O1 Nd1 O2 15_445 15_445 79.66(7) ?
O1 Nd1 O2 16 15_445 73.01(7) ?
O1 Nd1 O2 . 15_445 74.30(6) ?
O1 Nd1 O2 3_655 15_445 137.92(6) ?
O1 Nd1 O2 15_445 16 73.01(7) ?
O1 Nd1 O2 16 16 79.66(7) ?
O1 Nd1 O2 . 16 137.92(6) ?
O1 Nd1 O2 3_655 16 74.30(6) ?
O2 Nd1 O2 15_445 16 145.02(9) ?
O1 Nd1 O2 15_445 . 74.30(6) ?
O1 Nd1 O2 16 . 137.92(6) ?
O1 Nd1 O2 . . 79.66(7) ?
O1 Nd1 O2 3_655 . 73.01(7) ?
O2 Nd1 O2 15_445 . 72.37(10) ?
O2 Nd1 O2 16 . 118.92(10) ?
O1 Nd1 O2 15_445 3_655 137.92(6) ?
O1 Nd1 O2 16 3_655 74.30(6) ?
O1 Nd1 O2 . 3_655 73.01(7) ?
O1 Nd1 O2 3_655 3_655 79.66(7) ?
O2 Nd1 O2 15_445 3_655 118.92(10) ?
O2 Nd1 O2 16 3_655 72.37(10) ?
O2 Nd1 O2 . 3_655 145.02(9) ?
O3 Cl1 O3 . 20_656 109.83(10) ?
O3 Cl1 O3 . 3_655 108.76(19) ?
O3 Cl1 O3 20_656 3_655 109.83(10) ?
O3 Cl1 O3 . 26_565 109.83(10) ?
O3 Cl1 O3 20_656 26_565 108.76(19) ?
O3 Cl1 O3 3_655 26_565 109.83(10) ?
O4 Cl2 O4 7_545 . 109.6(8) ?
O4 Cl2 O5 7_545 . 115.9(6) ?
O4 Cl2 O5 . . 111.4(7) ?
O4 Cl2 O5 7_545 7_545 111.4(7) ?
O4 Cl2 O5 . 7_545 115.9(6) ?
O5 Cl2 O5 . 7_545 91.8(11) ?
N1 O1 Nd1 . . 141.71(16) ?
N2 O2 Nd1 . . 140.80(15) ?
O1 N1 C1 . . 119.1(2) ?
O1 N1 C2 . 25_655 120.8(2) ?
C1 N1 C2 . 25_655 120.0(2) ?
O2 N2 C3 . . 121.3(2) ?
O2 N2 C4 . 5_565 119.0(2) ?
C3 N2 C4 . 5_565 119.7(2) ?
N1 C1 C2 . . 120.1(2) ?
N1 C1 H1 . . 120.0 ?
C2 C1 H1 . . 120.0 ?
N1 C2 C1 25_655 . 119.9(2) ?
N1 C2 H2 25_655 . 120.1 ?
C1 C2 H2 . . 120.1 ?
N2 C3 C4 . . 120.2(2) ?
N2 C3 H3 . . 119.9 ?
C4 C3 H3 . . 119.9 ?
N2 C4 C3 5_565 . 120.1(2) ?
N2 C4 H4 5_565 . 119.9 ?
C3 C4 H4 . . 119.9 ?
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
Nd1 O1 15_445 2.4012(18) ?
Nd1 O1 16 2.4012(18) ?
Nd1 O1 . 2.4012(18) ?
Nd1 O1 3_655 2.4012(18) ?
Nd1 O2 15_445 2.4286(18) ?
Nd1 O2 16 2.4286(18) ?
Nd1 O2 . 2.4286(18) ?
Nd1 O2 3_655 2.4287(18) ?
Cl1 O3 . 1.435(2) ?
Cl1 O3 20_656 1.435(2) ?
Cl1 O3 3_655 1.435(2) ?
Cl1 O3 26_565 1.435(2) ?
Cl2 O4 7_545 1.328(5) ?
Cl2 O4 . 1.328(5) ?
Cl2 O5 . 1.350(7) ?
Cl2 O5 7_545 1.350(7) ?
O1 N1 . 1.302(3) ?
O2 N2 . 1.302(3) ?
N1 C1 . 1.355(3) ?
N1 C2 25_655 1.358(3) ?
N2 C3 . 1.354(3) ?
N2 C4 5_565 1.354(3) ?
C1 C2 . 1.374(3) ?
C1 H1 . 0.9500 ?
C2 N1 25_655 1.358(3) ?
C2 H2 . 0.9500 ?
C3 C4 . 1.373(3) ?
C3 H3 . 0.9500 ?
C4 N2 5_565 1.354(3) ?
C4 H4 . 0.9500 ?
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
C2 H2 O2 25_655 0.95 2.55 3.326(3) 139.3
C2 H2 O5 . 0.95 2.43 3.194(7) 137.4
C3 H3 O1 . 0.95 2.59 3.331(3) 135.2
C3 H3 O3 . 0.95 2.51 3.260(3) 136.3
C4 H4 O3 20_656 0.95 2.41 3.289(3) 153.6
