#------------------------------------------------------------------------------
#$Date: 2016-03-23 21:14:58 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179445 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/42/4334222.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_4334222
loop_
_publ_author_name
'Deng Zhang'
'Yun Lu'
'Dunru Zhu'
'Yan Xu'
_publ_section_title
;
 (C4N2H12)3[Ln3(OH)(SO4)7] (Ln = Sm, Eu, and Tb): A Series of
 Honeycomb-like Open-Framework Lanthanide Sulfates with Extra-Large
 Channels Containing 24-Membered Rings
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3253
_journal_page_last               3258
_journal_paper_doi               10.1021/ic3027682
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         (C4N2H12)3[Eu3(OH)(SO4)7]
_chemical_formula_sum            'C12 H37 Eu3 N6 O29 S7'
_chemical_formula_weight         1409.78
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           159
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'P 3 -2c'
_symmetry_space_group_name_H-M   'P 3 1 c'
_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                120.00
_cell_formula_units_Z            2
_cell_length_a                   14.3280(9)
_cell_length_b                   14.3280(9)
_cell_length_c                   10.0966(7)
_cell_measurement_reflns_used    5062
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.535
_cell_measurement_theta_min      2.596
_cell_volume                     1795.1(2)
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker Apex2 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  0.0335
_diffrn_reflns_av_sigmaI/netI    0.0358
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            9922
_diffrn_reflns_theta_full        25.98
_diffrn_reflns_theta_max         25.98
_diffrn_reflns_theta_min         1.64
_exptl_absorpt_coefficient_mu    5.698
_exptl_absorpt_correction_T_max  0.5996
_exptl_absorpt_correction_T_min  0.5480
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    2.608
_exptl_crystal_description       Block
_exptl_crystal_F_000             1368
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.725
_refine_diff_density_min         -0.700
_refine_diff_density_rms         0.112
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.008(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         2179
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0201
_refine_ls_R_factor_gt           0.0197
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0217P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0454
_refine_ls_wR_factor_ref         0.0454
_reflns_number_gt                2147
_reflns_number_total             2179
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic3027682_si_001_2.cif
_cod_data_source_block           aa
_cod_database_code               4334222
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, z+1/2'
'x-y, -y, z+1/2'
'-x, -x+y, z+1/2'
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
Eu1 Eu 1.584067(11) 0.143469(12) 0.613081(14) 0.01145(4) Uani 1 1 d .
S1 S 1.33717(6) 0.14357(6) 0.57498(9) 0.0141(2) Uani 1 1 d .
S2 S 1.52440(6) 0.00489(6) 0.36328(9) 0.0150(2) Uani 1 1 d .
S3 S 1.6667 0.3333 0.82408(14) 0.0130(3) Uani 1 3 d S
O1 O 1.57412(19) 0.12260(18) 0.3671(3) 0.0207(7) Uani 1 1 d .
O2 O 1.41705(17) -0.04695(19) 0.3003(3) 0.0204(6) Uani 1 1 d .
O3 O 1.51624(18) -0.03111(17) 0.5015(2) 0.0179(6) Uani 1 1 d .
O4 O 1.58764(18) -0.02937(19) 0.2812(3) 0.0217(7) Uani 1 1 d .
O5 O 1.24741(17) 0.09469(19) 0.4792(2) 0.0211(7) Uani 1 1 d .
O6 O 1.4036(2) 0.25905(19) 0.5453(3) 0.0302(8) Uani 1 1 d .
O7 O 1.40363(18) 0.0923(2) 0.5565(3) 0.0254(7) Uani 1 1 d .
O8 O 1.29497(19) 0.1249(2) 0.7096(3) 0.0261(7) Uani 1 1 d .
O9 O 1.72241(17) 0.44457(16) 0.7664(2) 0.0172(6) Uani 1 1 d .
O10 O 1.6667 0.3333 0.9657(4) 0.0233(11) Uani 1 3 d S
OH O 1.6667 0.3333 0.5284(4) 0.0148(10) Uani 1 3 d S
N1 N 1.1373(2) 0.3540(3) 0.4763(3) 0.0310(9) Uani 1 1 d .
H1C H 1.1561 0.3796 0.3933 0.037 Uiso 1 1 calc R
H1D H 1.0661 0.3283 0.4853 0.037 Uiso 1 1 calc R
N2 N 1.1907(2) 0.3119(3) 0.7362(3) 0.0243(8) Uani 1 1 d .
H2C H 1.1690 0.2859 0.8185 0.029 Uiso 1 1 calc R
H2D H 1.2621 0.3371 0.7307 0.029 Uiso 1 1 calc R
C1 C 1.1968(3) 0.4433(3) 0.5725(4) 0.0303(11) Uani 1 1 d .
H1A H 1.1783 0.4990 0.5583 0.036 Uiso 1 1 calc R
H1B H 1.2738 0.4747 0.5588 0.036 Uiso 1 1 calc R
C2 C 1.1684(3) 0.4014(3) 0.7113(4) 0.0328(11) Uani 1 1 d .
H2A H 1.2098 0.4596 0.7730 0.039 Uiso 1 1 calc R
H2B H 1.0926 0.3759 0.7267 0.039 Uiso 1 1 calc R
C3 C 1.1609(3) 0.2645(3) 0.4972(4) 0.0326(11) Uani 1 1 d .
H3A H 1.2367 0.2904 0.4809 0.039 Uiso 1 1 calc R
H3B H 1.1192 0.2065 0.4353 0.039 Uiso 1 1 calc R
C4 C 1.1328(3) 0.2231(3) 0.6371(4) 0.0247(10) Uani 1 1 d .
H4A H 1.0557 0.1905 0.6500 0.030 Uiso 1 1 calc R
H4B H 1.1521 0.1678 0.6513 0.030 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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Eu Eu -0.1578 3.6682 '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
O6 Eu1 O7 145.46(9) 2_745 .
O6 Eu1 O3 76.26(9) 2_745 .
O7 Eu1 O3 76.14(9) . .
O6 Eu1 O2 128.79(9) 2_745 5
O7 Eu1 O2 70.42(9) . 5
O3 Eu1 O2 88.32(8) . 5
O6 Eu1 O9 77.70(9) 2_745 3_875
O7 Eu1 O9 135.17(8) . 3_875
O3 Eu1 O9 145.86(8) . 3_875
O2 Eu1 O9 91.07(9) 5 3_875
O6 Eu1 O1 72.98(9) 2_745 .
O7 Eu1 O1 74.68(9) . .
O3 Eu1 O1 56.79(8) . .
O2 Eu1 O1 135.57(8) 5 .
O9 Eu1 O1 133.34(7) 3_875 .
O6 Eu1 OH 87.85(8) 2_745 .
O7 Eu1 OH 95.90(7) . .
O3 Eu1 OH 132.72(10) . .
O2 Eu1 OH 133.46(8) 5 .
O9 Eu1 OH 67.27(9) 3_875 .
O1 Eu1 OH 76.05(10) . .
O6 Eu1 O4 73.45(10) 2_745 5
O7 Eu1 O4 118.82(9) . 5
O3 Eu1 O4 76.07(8) . 5
O2 Eu1 O4 55.41(8) 5 5
O9 Eu1 O4 75.61(8) 3_875 5
O1 Eu1 O4 126.94(8) . 5
OH Eu1 O4 141.26(8) . 5
O6 Eu1 O9 131.36(9) 2_745 2_745
O7 Eu1 O9 79.94(8) . 2_745
O3 Eu1 O9 151.49(7) . 2_745
O2 Eu1 O9 69.04(7) 5 2_745
O9 Eu1 O9 55.24(9) 3_875 2_745
O1 Eu1 O9 130.23(8) . 2_745
OH Eu1 O9 64.76(9) . 2_745
O4 Eu1 O9 102.77(7) 5 2_745
O6 Eu1 S2 73.67(7) 2_745 .
O7 Eu1 S2 72.15(7) . .
O3 Eu1 S2 28.42(6) . .
O2 Eu1 S2 112.26(6) 5 .
O9 Eu1 S2 150.54(6) 3_875 .
O1 Eu1 S2 28.42(5) . .
OH Eu1 S2 104.47(9) . .
O4 Eu1 S2 102.33(6) 5 .
O9 Eu1 S2 149.00(5) 2_745 .
O6 Eu1 S2 101.37(8) 2_745 5
O7 Eu1 S2 94.48(7) . 5
O3 Eu1 S2 81.17(6) . 5
O2 Eu1 S2 27.46(5) 5 5
O9 Eu1 S2 82.73(6) 3_875 5
O1 Eu1 S2 137.89(5) . 5
OH Eu1 S2 146.06(9) . 5
O4 Eu1 S2 27.95(6) 5 5
O9 Eu1 S2 85.51(5) 2_745 5
S2 Eu1 S2 109.471(7) . 5
O6 Eu1 S3 104.16(7) 2_745 .
O7 Eu1 S3 107.87(6) . .
O3 Eu1 S3 165.03(6) . .
O2 Eu1 S3 79.80(6) 5 .
O9 Eu1 S3 27.32(5) 3_875 .
O1 Eu1 S3 137.99(6) . .
OH Eu1 S3 61.94(9) . .
O4 Eu1 S3 89.62(6) 5 .
O9 Eu1 S3 27.94(4) 2_745 .
S2 Eu1 S3 166.41(3) . .
S2 Eu1 S3 84.12(3) 5 .
O8 S1 O6 111.87(17) . .
O8 S1 O5 109.94(14) . .
O6 S1 O5 108.70(16) . .
O8 S1 O7 109.80(17) . .
O6 S1 O7 108.58(16) . .
O5 S1 O7 107.86(15) . .
O1 S2 O3 106.59(15) . .
O1 S2 O2 112.01(16) . .
O3 S2 O2 110.59(14) . .
O1 S2 O4 111.72(15) . .
O3 S2 O4 111.64(16) . .
O2 S2 O4 104.39(15) . .
O1 S2 Eu1 54.11(11) . .
O3 S2 Eu1 52.60(9) . .
O2 S2 Eu1 124.40(12) . .
O4 S2 Eu1 131.17(10) . .
O1 S2 Eu1 127.11(12) . 5_554
O3 S2 Eu1 126.24(9) . 5_554
O2 S2 Eu1 50.29(11) . 5_554
O4 S2 Eu1 54.10(9) . 5_554
Eu1 S2 Eu1 174.58(3) . 5_554
O10 S3 O9 112.89(11) . 3_875
O10 S3 O9 112.89(11) . 2_745
O9 S3 O9 105.85(12) 3_875 2_745
O10 S3 O9 112.89(11) . .
O9 S3 O9 105.85(12) 3_875 .
O9 S3 O9 105.85(12) 2_745 .
O10 S3 Eu1 132.04(2) . .
O9 S3 Eu1 49.71(10) 3_875 .
O9 S3 Eu1 56.19(9) 2_745 .
O9 S3 Eu1 114.94(12) . .
O10 S3 Eu1 132.04(2) . 2_745
O9 S3 Eu1 56.19(10) 3_875 2_745
O9 S3 Eu1 114.94(12) 2_745 2_745
O9 S3 Eu1 49.71(10) . 2_745
Eu1 S3 Eu1 80.06(3) . 2_745
O10 S3 Eu1 132.041(19) . 3_875
O9 S3 Eu1 114.94(12) 3_875 3_875
O9 S3 Eu1 49.71(10) 2_745 3_875
O9 S3 Eu1 56.19(9) . 3_875
Eu1 S3 Eu1 80.06(3) . 3_875
Eu1 S3 Eu1 80.06(3) 2_745 3_875
S2 O1 Eu1 97.46(13) . .
S2 O2 Eu1 102.25(14) . 5_554
S2 O3 Eu1 98.99(11) . .
S2 O4 Eu1 97.94(11) . 5_554
S1 O6 Eu1 142.26(18) . 3_875
S1 O7 Eu1 133.52(14) . .
S3 O9 Eu1 102.97(12) . 2_745
S3 O9 Eu1 95.88(10) . 3_875
Eu1 O9 Eu1 105.27(9) 2_745 3_875
Eu1 OH Eu1 109.04(9) 2_745 .
Eu1 OH Eu1 109.04(9) 2_745 3_875
Eu1 OH Eu1 109.04(9) . 3_875
C1 N1 C3 111.5(3) . .
C1 N1 H1C 109.3 . .
C3 N1 H1C 109.3 . .
C1 N1 H1D 109.3 . .
C3 N1 H1D 109.3 . .
H1C N1 H1D 108.0 . .
C2 N2 C4 110.6(3) . .
C2 N2 H2C 109.5 . .
C4 N2 H2C 109.5 . .
C2 N2 H2D 109.5 . .
C4 N2 H2D 109.5 . .
H2C N2 H2D 108.1 . .
N1 C1 C2 110.0(3) . .
N1 C1 H1A 109.7 . .
C2 C1 H1A 109.7 . .
N1 C1 H1B 109.7 . .
C2 C1 H1B 109.7 . .
H1A C1 H1B 108.2 . .
N2 C2 C1 111.8(4) . .
N2 C2 H2A 109.3 . .
C1 C2 H2A 109.3 . .
N2 C2 H2B 109.3 . .
C1 C2 H2B 109.3 . .
H2A C2 H2B 107.9 . .
N1 C3 C4 109.8(3) . .
N1 C3 H3A 109.7 . .
C4 C3 H3A 109.7 . .
N1 C3 H3B 109.7 . .
C4 C3 H3B 109.7 . .
H3A C3 H3B 108.2 . .
N2 C4 C3 111.4(3) . .
N2 C4 H4A 109.3 . .
C3 C4 H4A 109.3 . .
N2 C4 H4B 109.3 . .
C3 C4 H4B 109.3 . .
H4A C4 H4B 108.0 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Eu1 O6 2.343(2) 2_745
Eu1 O7 2.378(2) .
Eu1 O3 2.457(2) .
Eu1 O2 2.463(3) 5
Eu1 O9 2.490(2) 3_875
Eu1 O1 2.497(3) .
Eu1 OH 2.5126(14) .
Eu1 O4 2.559(2) 5
Eu1 O9 2.657(2) 2_745
Eu1 S2 3.0556(9) .
Eu1 S2 3.1288(9) 5
Eu1 S3 3.1812(10) .
S1 O8 1.457(3) .
S1 O6 1.469(3) .
S1 O5 1.476(2) .
S1 O7 1.476(3) .
S2 O1 1.467(2) .
S2 O3 1.472(3) .
S2 O2 1.476(2) .
S2 O4 1.481(3) .
S2 Eu1 3.1288(9) 5_554
S3 O10 1.429(5) .
S3 O9 1.498(2) 3_875
S3 O9 1.498(2) 2_745
S3 O9 1.498(2) .
S3 Eu1 3.1812(10) 2_745
S3 Eu1 3.1812(10) 3_875
O2 Eu1 2.463(3) 5_554
O4 Eu1 2.559(2) 5_554
O6 Eu1 2.342(2) 3_875
O9 Eu1 2.490(2) 2_745
O9 Eu1 2.657(2) 3_875
OH Eu1 2.5126(14) 2_745
OH Eu1 2.5126(14) 3_875
N1 C1 1.488(5) .
N1 C3 1.497(6) .
N1 H1C 0.9000 .
N1 H1D 0.9000 .
N2 C2 1.490(6) .
N2 C4 1.501(5) .
N2 H2C 0.9000 .
N2 H2D 0.9000 .
C1 C2 1.499(6) .
C1 H1A 0.9700 .
C1 H1B 0.9700 .
C2 H2A 0.9700 .
C2 H2B 0.9700 .
C3 C4 1.507(5) .
C3 H3A 0.9700 .
C3 H3B 0.9700 .
C4 H4A 0.9700 .
C4 H4B 0.9700 .
