#------------------------------------------------------------------------------
#$Date: 2016-03-26 18:14:25 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180418 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/87/7208783.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_7208783
loop_
_publ_author_name
'Zhang, Deng'
'Lu, Yun'
'Chen, Lei'
'Cai, Hu'
'Zhu, Dunru'
'Xu, Yan'
_publ_section_title
;
 A series of new rare earth sulfates based on lanthanide contraction and
 dual organic-amine templating effects
;
_journal_issue                   20
_journal_name_full               CrystEngComm
_journal_page_first              6627
_journal_paper_doi               10.1039/c2ce25937k
_journal_volume                  14
_journal_year                    2012
_chemical_formula_moiety         '[H3N(CH2)2NH3]5[Dy2(SO4)8]'
_chemical_formula_sum            'C10 H50 Dy2 N10 O32 S8'
_chemical_formula_weight         1404.08
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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                99.102(2)
_cell_angle_beta                 92.703(3)
_cell_angle_gamma                115.764(2)
_cell_formula_units_Z            1
_cell_length_a                   8.7260(18)
_cell_length_b                   9.828(2)
_cell_length_c                   13.475(3)
_cell_measurement_reflns_used    1848
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      23.34
_cell_measurement_theta_min      2.54
_cell_volume                     1018.9(4)
_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 0.986
_diffrn_measured_fraction_theta_max 0.986
_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  0.0631
_diffrn_reflns_av_sigmaI/netI    0.0757
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            7183
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         1.54
_exptl_absorpt_coefficient_mu    4.165
_exptl_absorpt_correction_T_max  0.6348
_exptl_absorpt_correction_T_min  0.5554
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.288
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             696
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.967
_refine_diff_density_min         -1.708
_refine_diff_density_rms         0.202
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         3546
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0541
_refine_ls_R_factor_gt           0.0428
_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)+(0.0536P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0984
_refine_ls_wR_factor_ref         0.1029
_reflns_number_gt                3004
_reflns_number_total             3546
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2ce25937k.txt
_cod_data_source_block           zd-49
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        1018.8(4)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7208783
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
Dy1 Dy -0.85344(4) 0.18164(4) 0.20858(3) 0.01823(13) Uani 1 1 d .
S1 S -0.9661(2) -0.0527(2) 0.34248(14) 0.0245(4) Uani 1 1 d .
S2 S -0.5064(2) 0.3414(2) 0.34433(14) 0.0243(4) Uani 1 1 d .
S3 S -0.7634(2) 0.0143(2) -0.02592(14) 0.0202(4) Uani 1 1 d .
S4 S -0.8615(3) 0.4792(2) 0.19557(15) 0.0253(4) Uani 1 1 d .
O1 O -0.5589(6) 0.2305(6) 0.2433(4) 0.0275(12) Uani 1 1 d .
O2 O -0.8821(6) -0.0548(6) 0.2470(4) 0.0246(12) Uani 1 1 d .
O3 O -0.7873(7) 0.1286(6) 0.0473(4) 0.0313(13) Uani 1 1 d .
O4 O -0.5882(7) 0.0846(7) -0.0498(4) 0.0328(13) Uani 1 1 d .
O5 O -0.9911(7) 0.0886(6) 0.3495(4) 0.0289(13) Uani 1 1 d .
O6 O -0.7477(7) 0.4179(6) 0.1493(4) 0.0304(13) Uani 1 1 d .
O7 O -0.9748(7) 0.3576(6) 0.2485(4) 0.0349(14) Uani 1 1 d .
O8 O -0.6640(7) 0.3575(6) 0.3610(4) 0.0339(14) Uani 1 1 d .
O9 O -0.8801(7) -0.0222(7) -0.1195(4) 0.0368(14) Uani 1 1 d .
O10 O -1.1290(7) -0.1881(6) 0.3286(5) 0.0350(14) Uani 1 1 d .
O11 O -0.7620(8) 0.6244(6) 0.2663(5) 0.0428(16) Uani 1 1 d .
O12 O -0.8016(8) -0.1225(7) 0.0153(5) 0.0449(16) Uani 1 1 d .
O13 O -0.4596(8) 0.2742(7) 0.4215(4) 0.0422(16) Uani 1 1 d .
O14 O -0.9627(8) 0.4993(7) 0.1152(5) 0.0459(17) Uani 1 1 d .
O15 O -0.3660(8) 0.4859(7) 0.3361(5) 0.0459(17) Uani 1 1 d .
N5 N -0.5729(8) 0.9173(7) 0.2200(5) 0.0306(16) Uani 1 1 d .
H5C H -0.5519 0.9422 0.1597 0.046 Uiso 1 1 calc R
H5D H -0.6342 0.9616 0.2485 0.046 Uiso 1 1 calc R
H5E H -0.6316 0.8154 0.2123 0.046 Uiso 1 1 calc R
N2 N -0.1117(8) 0.6896(7) 0.0871(5) 0.0283(15) Uani 1 1 d .
H2C H -0.0619 0.7833 0.1263 0.042 Uiso 1 1 calc R
H2D H -0.1305 0.6973 0.0232 0.042 Uiso 1 1 calc R
H2E H -0.0433 0.6443 0.0910 0.042 Uiso 1 1 calc R
N1 N -0.3262(9) 0.3232(8) 0.0975(5) 0.0341(17) Uani 1 1 d .
H1C H -0.3865 0.2301 0.0587 0.051 Uiso 1 1 calc R
H1D H -0.3476 0.3197 0.1613 0.051 Uiso 1 1 calc R
H1E H -0.2148 0.3529 0.0948 0.051 Uiso 1 1 calc R
N3 N 0.9104(9) 0.6429(8) 0.4932(6) 0.0368(18) Uani 1 1 d .
H3C H 0.9627 0.7424 0.4902 0.055 Uiso 1 1 calc R
H3D H 0.8582 0.6315 0.5486 0.055 Uiso 1 1 calc R
H3E H 0.8331 0.5910 0.4386 0.055 Uiso 1 1 calc R
O16 O -0.8569(8) -0.0459(8) 0.4277(5) 0.0488(17) Uani 1 1 d .
N4 N -0.4411(10) 0.7776(9) 0.3924(5) 0.0410(19) Uani 1 1 d .
H4C H -0.4548 0.7605 0.4551 0.061 Uiso 1 1 calc R
H4D H -0.3441 0.7761 0.3760 0.061 Uiso 1 1 calc R
H4E H -0.5293 0.7046 0.3492 0.061 Uiso 1 1 calc R
C2 C -0.2785(11) 0.5955(9) 0.1221(7) 0.034(2) Uani 1 1 d .
H2A H -0.3500 0.6481 0.1202 0.041 Uiso 1 1 calc R
H2B H -0.2566 0.5892 0.1921 0.041 Uiso 1 1 calc R
C1 C -0.3758(11) 0.4349(9) 0.0606(6) 0.033(2) Uani 1 1 d .
H1A H -0.4977 0.4011 0.0627 0.040 Uiso 1 1 calc R
H1B H -0.3552 0.4361 -0.0094 0.040 Uiso 1 1 calc R
C3 C 1.0396(11) 0.5821(9) 0.4967(7) 0.034(2) Uani 1 1 d .
H3A H 1.0964 0.5949 0.4363 0.041 Uiso 1 1 calc R
H3B H 1.1259 0.6412 0.5550 0.041 Uiso 1 1 calc R
C5 C -0.4098(10) 0.9711(11) 0.2853(7) 0.040(2) Uani 1 1 d .
H5A H -0.3478 1.0824 0.2943 0.048 Uiso 1 1 calc R
H5B H -0.3406 0.9278 0.2516 0.048 Uiso 1 1 calc R
C4 C -0.4327(12) 0.9280(11) 0.3875(7) 0.044(2) Uani 1 1 d .
H4A H -0.3380 1.0061 0.4363 0.053 Uiso 1 1 calc R
H4B H -0.5375 0.9291 0.4077 0.053 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'
Dy Dy -0.1892 4.4098 '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
O9 Dy1 O3 78.00(19) 2_355 .
O9 Dy1 O2 81.4(2) 2_355 .
O3 Dy1 O2 93.42(18) . .
O9 Dy1 O6 107.5(2) 2_355 .
O3 Dy1 O6 73.86(19) . .
O2 Dy1 O6 162.04(17) . .
O9 Dy1 O5 83.27(19) 2_355 .
O3 Dy1 O5 148.76(19) . .
O2 Dy1 O5 58.93(17) . .
O6 Dy1 O5 136.29(18) . .
O9 Dy1 O7 83.8(2) 2_355 .
O3 Dy1 O7 120.81(19) . .
O2 Dy1 O7 138.67(17) . .
O6 Dy1 O7 59.01(17) . .
O5 Dy1 O7 81.17(17) . .
O9 Dy1 O1 147.2(2) 2_355 .
O3 Dy1 O1 78.26(18) . .
O2 Dy1 O1 77.78(17) . .
O6 Dy1 O1 87.08(18) . .
O5 Dy1 O1 106.65(18) . .
O7 Dy1 O1 128.07(19) . .
O9 Dy1 O8 152.32(19) 2_355 .
O3 Dy1 O8 129.31(18) . .
O2 Dy1 O8 99.02(19) . .
O6 Dy1 O8 80.40(19) . .
O5 Dy1 O8 73.72(18) . .
O7 Dy1 O8 77.74(19) . .
O1 Dy1 O8 57.24(18) . .
O9 Dy1 S4 96.78(16) 2_355 .
O3 Dy1 S4 97.87(14) . .
O2 Dy1 S4 167.96(12) . .
O6 Dy1 S4 29.38(13) . .
O5 Dy1 S4 109.07(13) . .
O7 Dy1 S4 29.64(13) . .
O1 Dy1 S4 108.57(13) . .
O8 Dy1 S4 77.00(14) . .
O9 Dy1 S1 82.64(15) 2_355 .
O3 Dy1 S1 122.39(14) . .
O2 Dy1 S1 29.79(12) . .
O6 Dy1 S1 162.99(14) . .
O5 Dy1 S1 29.20(13) . .
O7 Dy1 S1 110.06(13) . .
O1 Dy1 S1 91.38(13) . .
O8 Dy1 S1 84.52(14) . .
S4 Dy1 S1 138.25(6) . .
O9 Dy1 S2 169.18(15) 2_355 .
O3 Dy1 S2 104.70(14) . .
O2 Dy1 S2 87.92(13) . .
O6 Dy1 S2 83.29(14) . .
O5 Dy1 S2 89.62(14) . .
O7 Dy1 S2 103.21(15) . .
O1 Dy1 S2 28.98(13) . .
O8 Dy1 S2 28.27(13) . .
S4 Dy1 S2 93.23(5) . .
S1 Dy1 S2 87.17(5) . .
O16 S1 O10 110.9(4) . .
O16 S1 O5 112.7(4) . .
O10 S1 O5 110.7(3) . .
O16 S1 O2 110.4(3) . .
O10 S1 O2 109.1(3) . .
O5 S1 O2 102.6(3) . .
O16 S1 Dy1 122.9(3) . .
O10 S1 Dy1 126.1(3) . .
O5 S1 Dy1 51.6(2) . .
O2 S1 Dy1 51.14(19) . .
O15 S2 O13 111.3(4) . .
O15 S2 O8 111.7(4) . .
O13 S2 O8 111.9(3) . .
O15 S2 O1 109.6(3) . .
O13 S2 O1 109.6(3) . .
O8 S2 O1 102.4(3) . .
O15 S2 Dy1 125.3(3) . .
O13 S2 Dy1 123.3(3) . .
O8 S2 Dy1 51.9(2) . .
O1 S2 Dy1 50.5(2) . .
O12 S3 O4 112.3(4) . .
O12 S3 O3 109.8(3) . .
O4 S3 O3 108.2(3) . .
O12 S3 O9 110.8(4) . .
O4 S3 O9 107.9(3) . .
O3 S3 O9 107.7(3) . .
O11 S4 O14 110.6(4) . .
O11 S4 O6 110.8(4) . .
O14 S4 O6 108.8(4) . .
O11 S4 O7 111.3(4) . .
O14 S4 O7 110.4(4) . .
O6 S4 O7 104.7(3) . .
O11 S4 Dy1 125.0(3) . .
O14 S4 Dy1 124.3(3) . .
O6 S4 Dy1 52.0(2) . .
O7 S4 Dy1 52.7(2) . .
S2 O1 Dy1 100.5(3) . .
S1 O2 Dy1 99.1(2) . .
S3 O3 Dy1 144.5(3) . .
S1 O5 Dy1 99.2(3) . .
S4 O6 Dy1 98.6(2) . .
S4 O7 Dy1 97.7(3) . .
S2 O8 Dy1 99.8(3) . .
S3 O9 Dy1 146.1(3) . 2_355
C5 N5 H5C 109.5 . .
C5 N5 H5D 109.5 . .
H5C N5 H5D 109.5 . .
C5 N5 H5E 109.5 . .
H5C N5 H5E 109.5 . .
H5D N5 H5E 109.5 . .
C2 N2 H2C 109.5 . .
C2 N2 H2D 109.5 . .
H2C N2 H2D 109.5 . .
C2 N2 H2E 109.5 . .
H2C N2 H2E 109.5 . .
H2D N2 H2E 109.5 . .
C1 N1 H1C 109.5 . .
C1 N1 H1D 109.5 . .
H1C N1 H1D 109.5 . .
C1 N1 H1E 109.5 . .
H1C N1 H1E 109.5 . .
H1D N1 H1E 109.5 . .
C3 N3 H3C 109.5 . .
C3 N3 H3D 109.5 . .
H3C N3 H3D 109.5 . .
C3 N3 H3E 109.5 . .
H3C N3 H3E 109.5 . .
H3D N3 H3E 109.5 . .
C4 N4 H4C 109.5 . .
C4 N4 H4D 109.5 . .
H4C N4 H4D 109.5 . .
C4 N4 H4E 109.5 . .
H4C N4 H4E 109.5 . .
H4D N4 H4E 109.5 . .
N2 C2 C1 114.3(7) . .
N2 C2 H2A 108.7 . .
C1 C2 H2A 108.7 . .
N2 C2 H2B 108.7 . .
C1 C2 H2B 108.7 . .
H2A C2 H2B 107.6 . .
N1 C1 C2 112.7(7) . .
N1 C1 H1A 109.1 . .
C2 C1 H1A 109.1 . .
N1 C1 H1B 109.1 . .
C2 C1 H1B 109.1 . .
H1A C1 H1B 107.8 . .
C3 C3 N3 111.9(9) 2_766 .
C3 C3 H3A 109.2 2_766 .
N3 C3 H3A 109.2 . .
C3 C3 H3B 109.2 2_766 .
N3 C3 H3B 109.2 . .
H3A C3 H3B 107.9 . .
N5 C5 C4 113.2(7) . .
N5 C5 H5A 108.9 . .
C4 C5 H5A 108.9 . .
N5 C5 H5B 108.9 . .
C4 C5 H5B 108.9 . .
H5A C5 H5B 107.7 . .
N4 C4 C5 114.8(8) . .
N4 C4 H4A 108.6 . .
C5 C4 H4A 108.6 . .
N4 C4 H4B 108.6 . .
C5 C4 H4B 108.6 . .
H4A C4 H4B 107.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Dy1 O9 2.297(5) 2_355
Dy1 O3 2.313(5) .
Dy1 O2 2.371(5) .
Dy1 O6 2.382(5) .
Dy1 O5 2.386(5) .
Dy1 O7 2.398(5) .
Dy1 O1 2.408(5) .
Dy1 O8 2.452(5) .
Dy1 S4 2.9876(19) .
Dy1 S1 3.0065(18) .
Dy1 S2 3.069(2) .
S1 O16 1.431(6) .
S1 O10 1.441(5) .
S1 O5 1.486(5) .
S1 O2 1.512(5) .
S2 O15 1.443(6) .
S2 O13 1.447(6) .
S2 O8 1.475(6) .
S2 O1 1.512(6) .
S3 O12 1.446(6) .
S3 O4 1.455(5) .
S3 O3 1.467(5) .
S3 O9 1.475(6) .
S4 O11 1.454(6) .
S4 O14 1.457(6) .
S4 O6 1.482(5) .
S4 O7 1.491(5) .
O9 Dy1 2.297(5) 2_355
N5 C5 1.469(10) .
N5 H5C 0.8900 .
N5 H5D 0.8900 .
N5 H5E 0.8900 .
N2 C2 1.493(9) .
N2 H2C 0.8900 .
N2 H2D 0.8900 .
N2 H2E 0.8900 .
N1 C1 1.485(10) .
N1 H1C 0.8900 .
N1 H1D 0.8900 .
N1 H1E 0.8900 .
N3 C3 1.490(10) .
N3 H3C 0.8900 .
N3 H3D 0.8900 .
N3 H3E 0.8900 .
N4 C4 1.460(11) .
N4 H4C 0.8900 .
N4 H4D 0.8900 .
N4 H4E 0.8900 .
C2 C1 1.501(12) .
C2 H2A 0.9700 .
C2 H2B 0.9700 .
C1 H1A 0.9700 .
C1 H1B 0.9700 .
C3 C3 1.473(15) 2_766
C3 H3A 0.9700 .
C3 H3B 0.9700 .
C5 C4 1.502(11) .
C5 H5A 0.9700 .
C5 H5B 0.9700 .
C4 H4A 0.9700 .
C4 H4B 0.9700 .
