#------------------------------------------------------------------------------
#$Date: 2016-03-26 18:14:25 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180418 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/87/7208784.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_7208784
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[Ho2(SO4)8]'
_chemical_formula_sum            'C10 H50 Ho2 N10 O32 S8'
_chemical_formula_weight         1408.94
_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                99.028(3)
_cell_angle_beta                 92.819(3)
_cell_angle_gamma                115.737(3)
_cell_formula_units_Z            1
_cell_length_a                   8.734(2)
_cell_length_b                   9.824(3)
_cell_length_c                   13.466(4)
_cell_measurement_reflns_used    3027
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.85
_cell_measurement_theta_min      2.35
_cell_volume                     1018.9(5)
_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 0.974
_diffrn_measured_fraction_theta_max 0.974
_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  0.0289
_diffrn_reflns_av_sigmaI/netI    0.0454
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            7485
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         1.54
_exptl_absorpt_coefficient_mu    4.381
_exptl_absorpt_correction_T_max  0.6685
_exptl_absorpt_correction_T_min  0.5997
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.296
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             698
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.556
_refine_diff_density_min         -0.633
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         3695
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0307
_refine_ls_R_factor_gt           0.0267
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0300P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0596
_refine_ls_wR_factor_ref         0.0611
_reflns_number_gt                3346
_reflns_number_total             3695
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2ce25937k.txt
_cod_data_source_block           zd-26
_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        1019.0(5)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7208784
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
Ho1 Ho 0.85384(2) 0.81834(2) -0.208667(15) 0.01423(8) Uani 1 1 d .
S1 S 0.96577(14) 1.05156(13) -0.34239(9) 0.0203(3) Uani 1 1 d .
S2 S 1.23580(13) 1.01296(12) -0.02571(8) 0.0163(2) Uani 1 1 d .
S3 S 0.86143(14) 0.52154(13) -0.19559(9) 0.0218(3) Uani 1 1 d .
S4 S 0.50818(13) 0.65965(13) -0.34371(8) 0.0211(3) Uani 1 1 d .
O1 O 0.5601(4) 0.7701(4) -0.2429(2) 0.0243(7) Uani 1 1 d .
O2 O 0.8829(4) 1.0540(3) -0.2468(2) 0.0229(7) Uani 1 1 d .
O3 O 1.2113(4) 1.1279(4) 0.0485(2) 0.0272(8) Uani 1 1 d .
O4 O 0.9914(4) 0.9097(3) -0.3491(2) 0.0253(7) Uani 1 1 d .
O5 O 1.4112(4) 1.0849(4) -0.0486(2) 0.0295(8) Uani 1 1 d .
O6 O 0.9728(4) 0.6419(4) -0.2490(3) 0.0308(8) Uani 1 1 d .
O7 O 0.7484(4) 0.5841(4) -0.1487(2) 0.0268(8) Uani 1 1 d .
O8 O 1.1198(4) 0.9762(4) -0.1201(2) 0.0318(8) Uani 1 1 d .
O9 O 0.6652(4) 0.6410(4) -0.3612(2) 0.0314(8) Uani 1 1 d .
O10 O 1.1298(4) 1.1883(4) -0.3287(3) 0.0329(8) Uani 1 1 d .
O11 O 0.7614(4) 0.3766(4) -0.2654(3) 0.0367(9) Uani 1 1 d .
O12 O 1.1993(5) 0.8766(4) 0.0160(3) 0.0401(9) Uani 1 1 d .
O13 O 0.4596(4) 0.7251(4) -0.4214(3) 0.0378(9) Uani 1 1 d .
O14 O 0.3658(4) 0.5146(4) -0.3347(3) 0.0408(10) Uani 1 1 d .
O15 O 0.9624(5) 0.5009(4) -0.1154(3) 0.0437(10) Uani 1 1 d .
O16 O 0.8561(5) 1.0446(5) -0.4280(3) 0.0475(11) Uani 1 1 d .
N1 N 0.5749(5) 0.0842(4) -0.2190(3) 0.0248(9) Uani 1 1 d .
H1C H 0.5551 0.0580 -0.1589 0.037 Uiso 1 1 calc R
H1D H 0.6321 0.1863 -0.2106 0.037 Uiso 1 1 calc R
H1E H 0.6369 0.0414 -0.2484 0.037 Uiso 1 1 calc R
N2 N 0.4424(5) 0.2229(5) -0.3912(3) 0.0378(11) Uani 1 1 d .
H2C H 0.4571 0.2416 -0.4535 0.057 Uiso 1 1 calc R
H2D H 0.5294 0.2960 -0.3472 0.057 Uiso 1 1 calc R
H2E H 0.3446 0.2227 -0.3754 0.057 Uiso 1 1 calc R
N3 N 0.0876(5) 0.3566(5) -0.4925(3) 0.0327(10) Uani 1 1 d .
H3C H 0.0354 0.2570 -0.4897 0.049 Uiso 1 1 calc R
H3D H 0.1638 0.4084 -0.4373 0.049 Uiso 1 1 calc R
H3E H 0.1411 0.3684 -0.5474 0.049 Uiso 1 1 calc R
N4 N 0.3262(5) -0.3234(5) -0.0976(3) 0.0310(10) Uani 1 1 d .
H4C H 0.3873 -0.2301 -0.0592 0.046 Uiso 1 1 calc R
H4D H 0.2151 -0.3523 -0.0946 0.046 Uiso 1 1 calc R
H4E H 0.3468 -0.3208 -0.1616 0.046 Uiso 1 1 calc R
N5 N 0.1139(5) -0.6894(4) -0.0865(3) 0.0260(9) Uani 1 1 d .
H5C H 0.0630 -0.7828 -0.1260 0.039 Uiso 1 1 calc R
H5D H 0.0461 -0.6434 -0.0893 0.039 Uiso 1 1 calc R
H5E H 0.1336 -0.6980 -0.0228 0.039 Uiso 1 1 calc R
C1 C 0.4098(6) 0.0292(6) -0.2840(4) 0.0324(12) Uani 1 1 d .
H1A H 0.3413 0.0738 -0.2510 0.039 Uiso 1 1 calc R
H1B H 0.3474 -0.0820 -0.2925 0.039 Uiso 1 1 calc R
C2 C 0.4361(7) 0.0722(6) -0.3873(4) 0.0369(14) Uani 1 1 d .
H2A H 0.5423 0.0729 -0.4058 0.044 Uiso 1 1 calc R
H2B H 0.3434 -0.0062 -0.4371 0.044 Uiso 1 1 calc R
C3 C -0.0410(6) 0.4165(5) -0.4975(4) 0.0318(12) Uani 1 1 d .
H3A H -0.1003 0.4021 -0.4381 0.038 Uiso 1 1 calc R
H3B H -0.1251 0.3585 -0.5570 0.038 Uiso 1 1 calc R
C4 C 0.3749(6) -0.4347(5) -0.0604(4) 0.0291(12) Uani 1 1 d .
H4A H 0.3539 -0.4355 0.0097 0.035 Uiso 1 1 calc R
H4B H 0.4968 -0.4007 -0.0620 0.035 Uiso 1 1 calc R
C5 C 0.2781(6) -0.5965(5) -0.1218(4) 0.0310(12) Uani 1 1 d .
H5A H 0.2555 -0.5911 -0.1919 0.037 Uiso 1 1 calc R
H5B H 0.3501 -0.6486 -0.1195 0.037 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'
Ho Ho -0.2175 4.6783 '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
O8 Ho1 O3 78.14(11) . 2_775
O8 Ho1 O2 81.52(12) . .
O3 Ho1 O2 93.14(11) 2_775 .
O8 Ho1 O7 107.24(12) . .
O3 Ho1 O7 73.71(11) 2_775 .
O2 Ho1 O7 161.80(11) . .
O8 Ho1 O4 83.12(11) . .
O3 Ho1 O4 148.81(11) 2_775 .
O2 Ho1 O4 59.32(10) . .
O7 Ho1 O4 136.32(10) . .
O8 Ho1 O6 83.86(12) . .
O3 Ho1 O6 121.17(11) 2_775 .
O2 Ho1 O6 138.73(11) . .
O7 Ho1 O6 59.23(11) . .
O4 Ho1 O6 80.76(11) . .
O8 Ho1 O1 147.38(12) . .
O3 Ho1 O1 78.04(11) 2_775 .
O2 Ho1 O1 77.88(10) . .
O7 Ho1 O1 86.96(11) . .
O4 Ho1 O1 107.06(11) . .
O6 Ho1 O1 127.84(11) . .
O8 Ho1 O9 151.89(11) . .
O3 Ho1 O9 129.51(11) 2_775 .
O2 Ho1 O9 99.55(11) . .
O7 Ho1 O9 80.33(11) . .
O4 Ho1 O9 73.75(11) . .
O6 Ho1 O9 76.94(11) . .
O1 Ho1 O9 57.77(11) . .
O8 Ho1 S3 96.58(10) . .
O3 Ho1 S3 98.10(8) 2_775 .
O2 Ho1 S3 167.98(8) . .
O7 Ho1 S3 29.67(8) . .
O4 Ho1 S3 108.71(8) . .
O6 Ho1 S3 29.56(8) . .
O1 Ho1 S3 108.57(8) . .
O9 Ho1 S3 76.52(8) . .
O8 Ho1 S1 82.75(9) . .
O3 Ho1 S1 122.21(9) 2_775 .
O2 Ho1 S1 29.85(8) . .
O7 Ho1 S1 163.29(8) . .
O4 Ho1 S1 29.55(8) . .
O6 Ho1 S1 110.04(8) . .
O1 Ho1 S1 91.45(8) . .
O9 Ho1 S1 84.75(9) . .
S3 Ho1 S1 138.23(3) . .
O8 Ho1 S4 169.36(9) . .
O3 Ho1 S4 104.62(8) 2_775 .
O2 Ho1 S4 88.04(8) . .
O7 Ho1 S4 83.36(8) . .
O4 Ho1 S4 89.82(8) . .
O6 Ho1 S4 102.91(9) . .
O1 Ho1 S4 29.08(8) . .
O9 Ho1 S4 28.71(8) . .
S3 Ho1 S4 93.21(3) . .
S1 Ho1 S4 87.18(3) . .
O16 S1 O10 110.7(2) . .
O16 S1 O4 112.8(2) . .
O10 S1 O4 110.70(19) . .
O16 S1 O2 110.7(2) . .
O10 S1 O2 109.05(19) . .
O4 S1 O2 102.47(18) . .
O16 S1 Ho1 122.83(16) . .
O10 S1 Ho1 126.36(16) . .
O4 S1 Ho1 51.61(12) . .
O2 S1 Ho1 51.03(12) . .
O12 S2 O5 112.2(2) . .
O12 S2 O8 111.2(2) . .
O5 S2 O8 107.88(19) . .
O12 S2 O3 109.6(2) . .
O5 S2 O3 107.76(19) . .
O8 S2 O3 108.1(2) . .
O11 S3 O15 110.3(2) . .
O11 S3 O6 111.3(2) . .
O15 S3 O6 110.9(2) . .
O11 S3 O7 111.0(2) . .
O15 S3 O7 108.7(2) . .
O6 S3 O7 104.52(18) . .
O11 S3 Ho1 125.19(16) . .
O15 S3 Ho1 124.48(15) . .
O6 S3 Ho1 52.62(13) . .
O7 S3 Ho1 51.90(12) . .
O13 S4 O14 110.5(2) . .
O13 S4 O9 112.2(2) . .
O14 S4 O9 111.5(2) . .
O13 S4 O1 110.1(2) . .
O14 S4 O1 109.0(2) . .
O9 S4 O1 103.24(18) . .
O13 S4 Ho1 124.00(15) . .
O14 S4 Ho1 125.35(15) . .
O9 S4 Ho1 52.52(13) . .
O1 S4 Ho1 50.75(12) . .
S4 O1 Ho1 100.17(15) . .
S1 O2 Ho1 99.12(15) . .
S2 O3 Ho1 145.0(2) . 2_775
S1 O4 Ho1 98.84(15) . .
S3 O6 Ho1 97.81(16) . .
S3 O7 Ho1 98.43(15) . .
S2 O8 Ho1 145.9(2) . .
S4 O9 Ho1 98.77(16) . .
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 . .
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 . .
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 . .
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 . .
N1 C1 C2 111.7(4) . .
N1 C1 H1A 109.3 . .
C2 C1 H1A 109.3 . .
N1 C1 H1B 109.3 . .
C2 C1 H1B 109.3 . .
H1A C1 H1B 107.9 . .
N2 C2 C1 113.5(4) . .
N2 C2 H2A 108.9 . .
C1 C2 H2A 108.9 . .
N2 C2 H2B 108.9 . .
C1 C2 H2B 108.9 . .
H2A C2 H2B 107.7 . .
N3 C3 C3 111.4(5) . 2_564
N3 C3 H3A 109.4 . .
C3 C3 H3A 109.4 2_564 .
N3 C3 H3B 109.4 . .
C3 C3 H3B 109.4 2_564 .
H3A C3 H3B 108.0 . .
N4 C4 C5 113.2(4) . .
N4 C4 H4A 108.9 . .
C5 C4 H4A 108.9 . .
N4 C4 H4B 108.9 . .
C5 C4 H4B 108.9 . .
H4A C4 H4B 107.8 . .
N5 C5 C4 114.0(4) . .
N5 C5 H5A 108.7 . .
C4 C5 H5A 108.7 . .
N5 C5 H5B 108.8 . .
C4 C5 H5B 108.8 . .
H5A C5 H5B 107.6 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ho1 O8 2.289(3) .
Ho1 O3 2.297(3) 2_775
Ho1 O2 2.358(3) .
Ho1 O7 2.369(3) .
Ho1 O4 2.376(3) .
Ho1 O6 2.388(3) .
Ho1 O1 2.404(3) .
Ho1 O9 2.453(3) .
Ho1 S3 2.9775(14) .
Ho1 S1 2.9950(13) .
Ho1 S4 3.0553(12) .
S1 O16 1.435(4) .
S1 O10 1.455(3) .
S1 O4 1.495(3) .
S1 O2 1.510(3) .
S2 O12 1.448(3) .
S2 O5 1.455(3) .
S2 O8 1.478(3) .
S2 O3 1.482(3) .
S3 O11 1.447(3) .
S3 O15 1.455(3) .
S3 O6 1.483(3) .
S3 O7 1.490(3) .
S4 O13 1.446(3) .
S4 O14 1.457(3) .
S4 O9 1.485(3) .
S4 O1 1.509(3) .
O3 Ho1 2.297(3) 2_775
N1 C1 1.480(6) .
N1 H1C 0.8900 .
N1 H1D 0.8900 .
N1 H1E 0.8900 .
N2 C2 1.467(7) .
N2 H2C 0.8900 .
N2 H2D 0.8900 .
N2 H2E 0.8900 .
N3 C3 1.480(6) .
N3 H3C 0.8900 .
N3 H3D 0.8900 .
N3 H3E 0.8900 .
N4 C4 1.478(6) .
N4 H4C 0.8900 .
N4 H4D 0.8900 .
N4 H4E 0.8900 .
N5 C5 1.477(6) .
N5 H5C 0.8900 .
N5 H5D 0.8900 .
N5 H5E 0.8900 .
C1 C2 1.515(6) .
C1 H1A 0.9700 .
C1 H1B 0.9700 .
C2 H2A 0.9700 .
C2 H2B 0.9700 .
C3 C3 1.493(9) 2_564
C3 H3A 0.9700 .
C3 H3B 0.9700 .
C4 C5 1.509(6) .
C4 H4A 0.9700 .
C4 H4B 0.9700 .
C5 H5A 0.9700 .
C5 H5B 0.9700 .
