#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:30:45 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179381 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/78/4327849.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_4327849
loop_
_publ_author_name
'Limin Yang'
'Xiaohui Hua'
'Junhui Xue'
'Qinghua Pan'
'Lei Yu'
'Weihong Li'
'Yizhuang Xu'
'Guozhong Zhao'
'Liming Liu'
'Kexin Liu'
'Jia'er Chen'
'Jinguang Wu'
_publ_contact_author             'LiMin Yang'
_publ_contact_author_address
;  School of Physics
   Peking University
   Beijing,100871
   P.R.China
;
_publ_contact_author_email       yanglm@pku.edu.cn
_publ_contact_author_fax         +86-10-62758849
_publ_contact_author_phone       +86-10-62751889
_publ_section_title
;
 Interactions between Metal Ions and Carbohydrates. Spectroscopic
 Characterization and the Topology Coordination Behavior of Erythritol
 with Trivalent Lanthanide Ions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              499
_journal_page_last               510
_journal_paper_doi               10.1021/ic2019605
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C12 H34 Cl6 O14 Tb2'
_chemical_formula_weight         932.93
_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                69.99(3)
_cell_angle_beta                 76.44(3)
_cell_angle_gamma                66.88(3)
_cell_formula_units_Z            1
_cell_length_a                   7.1120(14)
_cell_length_b                   8.7190(17)
_cell_length_c                   12.492(3)
_cell_measurement_reflns_used    2732
_cell_measurement_temperature    173.15
_cell_measurement_theta_max      27.4854
_cell_measurement_theta_min      1.7467
_cell_volume                     664.9(3)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0226
_diffrn_reflns_av_sigmaI/netI    0.0266
_diffrn_reflns_limit_h_max       9
_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            5879
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         1.75
_exptl_absorpt_coefficient_mu    5.938
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6745
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.330
_exptl_crystal_description       block
_exptl_crystal_F_000             450
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.071
_refine_diff_density_max         2.950
_refine_diff_density_min         -0.893
_refine_diff_density_rms         0.243
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.245
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     187
_refine_ls_number_reflns         3033
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.243
_refine_ls_R_factor_all          0.0263
_refine_ls_R_factor_gt           0.0257
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0402P)²+1.6049P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0783
_refine_ls_wR_factor_ref         0.0787
_reflns_number_gt                2989
_reflns_number_total             3033
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2019605_si_001_5.cif
_cod_data_source_block           mx1040
_cod_original_cell_volume        664.9(2)
_cod_database_code               4327849
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
Tb1 Tb 0.62492(3) 0.41094(2) 0.222072(15) 0.01092(8) Uani 1 1 d .
Cl1 Cl 0.72683(17) 0.66691(14) 0.05780(9) 0.0170(2) Uani 1 1 d .
Cl2 Cl 0.24773(17) 0.59537(14) 0.15282(10) 0.0192(2) Uani 1 1 d .
O4 O 0.5156(5) 0.2276(4) 0.1565(3) 0.0172(6) Uani 1 1 d D
H10 H 0.403(6) 0.291(7) 0.114(4) 0.021 Uiso 1 1 d D
O1 O 0.9145(5) 0.2502(4) 0.1127(3) 0.0167(6) Uani 1 1 d D
H7 H 0.997(8) 0.303(7) 0.055(4) 0.020 Uiso 1 1 d D
O2 O 0.7811(5) 0.1158(4) 0.3210(3) 0.0154(6) Uani 1 1 d D
H8 H 0.764(9) 0.053(7) 0.398(2) 0.018 Uiso 1 1 d D
O6 O 0.4196(5) 0.3306(4) 0.3981(3) 0.0209(7) Uani 1 1 d D
H12 H 0.379(9) 0.232(5) 0.413(5) 0.025 Uiso 1 1 d D
O5 O 0.5128(5) 0.6033(4) 0.3431(3) 0.0210(7) Uani 1 1 d D
H11 H 0.552(9) 0.699(5) 0.326(3) 0.025 Uiso 1 1 d D
O7 O 0.9255(5) 0.4029(5) 0.2873(3) 0.0224(7) Uani 1 1 d D
H13 H 1.016(8) 0.460(8) 0.241(4) 0.027 Uiso 1 1 d D
H14 H 1.033(7) 0.306(5) 0.319(5) 0.027 Uiso 1 1 d D
O3 O 0.6392(5) -0.1332(4) 0.3084(3) 0.0196(7) Uani 1 1 d D
H9 H 0.524(6) -0.059(6) 0.342(5) 0.024 Uiso 1 1 d D
C1 C 1.0436(7) 0.0770(6) 0.1650(4) 0.0178(9) Uani 1 1 d .
H1A H 1.1520 0.0804 0.1980 0.021 Uiso 1 1 calc R
H1B H 1.1063 0.0124 0.1085 0.021 Uiso 1 1 calc R
C2 C 0.9055(7) -0.0078(5) 0.2579(4) 0.0148(8) Uani 1 1 d D
H2 H 0.999(6) -0.113(3) 0.302(4) 0.018 Uiso 1 1 d D
C3 C 0.7663(7) -0.0623(6) 0.2132(4) 0.0165(9) Uani 1 1 d D
H3 H 0.854(5) -0.152(6) 0.174(4) 0.020 Uiso 1 1 d D
C4 C 0.6426(8) 0.0750(6) 0.1195(4) 0.0190(9) Uani 1 1 d .
H4A H 0.7351 0.1061 0.0520 0.023 Uiso 1 1 calc R
H4B H 0.5561 0.0291 0.0990 0.023 Uiso 1 1 calc R
C5 C 0.4174(7) 0.5546(6) 0.4596(4) 0.0176(9) Uani 1 1 d D
H5 H 0.332(7) 0.654(4) 0.489(4) 0.021 Uiso 1 1 d D
C6 C 0.2852(7) 0.4614(6) 0.4534(4) 0.0203(9) Uani 1 1 d .
H6A H 0.2295 0.4088 0.5296 0.024 Uiso 1 1 calc R
H6B H 0.1722 0.5405 0.4090 0.024 Uiso 1 1 calc R
Cl3 Cl 0.22835(19) 0.06709(16) 0.42868(10) 0.0232(2) Uani 1 1 d .
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'
Cl Cl 0.1484 0.1585 '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'
Tb Tb -0.1723 4.1537 '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
O2 Tb1 O6 69.46(12) . .
O2 Tb1 O1 65.48(11) . .
O6 Tb1 O1 133.95(11) . .
O2 Tb1 O5 113.20(12) . .
O6 Tb1 O5 63.90(12) . .
O1 Tb1 O5 145.26(12) . .
O2 Tb1 O7 75.35(12) . .
O6 Tb1 O7 102.48(13) . .
O1 Tb1 O7 75.10(12) . .
O5 Tb1 O7 71.37(13) . .
O2 Tb1 O4 70.53(11) . .
O6 Tb1 O4 85.51(12) . .
O1 Tb1 O4 71.34(11) . .
O5 Tb1 O4 142.95(11) . .
O7 Tb1 O4 139.49(12) . .
O2 Tb1 Cl1 139.37(8) . .
O6 Tb1 Cl1 147.14(9) . .
O1 Tb1 Cl1 78.44(8) . .
O5 Tb1 Cl1 85.93(9) . .
O7 Tb1 Cl1 77.96(9) . .
O4 Tb1 Cl1 115.83(8) . .
O2 Tb1 Cl2 132.74(9) . .
O6 Tb1 Cl2 80.74(10) . .
O1 Tb1 Cl2 124.89(9) . .
O5 Tb1 Cl2 82.92(9) . .
O7 Tb1 Cl2 148.80(9) . .
O4 Tb1 Cl2 71.36(8) . .
Cl1 Tb1 Cl2 82.99(5) . .
C4 O4 Tb1 128.1(3) . .
C4 O4 H10 110(4) . .
Tb1 O4 H10 113(4) . .
C1 O1 Tb1 121.4(3) . .
C1 O1 H7 107(4) . .
Tb1 O1 H7 122(4) . .
C2 O2 Tb1 120.1(2) . .
C2 O2 H8 107(4) . .
Tb1 O2 H8 132(4) . .
C6 O6 Tb1 119.5(3) . .
C6 O6 H12 116(4) . .
Tb1 O6 H12 119(4) . .
C5 O5 Tb1 121.2(3) . .
C5 O5 H11 114.2(19) . .
Tb1 O5 H11 123(2) . .
Tb1 O7 H13 123(4) . .
Tb1 O7 H14 128(4) . .
H13 O7 H14 92(5) . .
C3 O3 H9 120(4) . .
O1 C1 C2 106.6(3) . .
O1 C1 H1A 110.4 . .
C2 C1 H1A 110.4 . .
O1 C1 H1B 110.4 . .
C2 C1 H1B 110.4 . .
H1A C1 H1B 108.6 . .
O2 C2 C1 106.9(3) . .
O2 C2 C3 109.5(4) . .
C1 C2 C3 114.4(4) . .
O2 C2 H2 114(3) . .
C1 C2 H2 105(3) . .
C3 C2 H2 106.8(17) . .
O3 C3 C4 112.1(4) . .
O3 C3 C2 108.7(4) . .
C4 C3 C2 115.8(4) . .
O3 C3 H3 110(3) . .
C4 C3 H3 102(3) . .
C2 C3 H3 109(2) . .
O4 C4 C3 110.7(4) . .
O4 C4 H4A 109.5 . .
C3 C4 H4A 109.5 . .
O4 C4 H4B 109.5 . .
C3 C4 H4B 109.5 . .
H4A C4 H4B 108.1 . .
O5 C5 C6 104.5(4) . .
O5 C5 C5 109.9(5) . 2_666
C6 C5 C5 114.2(5) . 2_666
O5 C5 H5 114(2) . .
C6 C5 H5 110(3) . .
C5 C5 H5 105(3) 2_666 .
O6 C6 C5 105.0(4) . .
O6 C6 H6A 110.7 . .
C5 C6 H6A 110.7 . .
O6 C6 H6B 110.7 . .
C5 C6 H6B 110.7 . .
H6A C6 H6B 108.8 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Tb1 O2 2.368(3) .
Tb1 O6 2.387(3) .
Tb1 O1 2.408(3) .
Tb1 O5 2.419(3) .
Tb1 O7 2.429(3) .
Tb1 O4 2.449(3) .
Tb1 Cl1 2.6750(14) .
Tb1 Cl2 2.6979(15) .
O4 C4 1.443(5) .
O4 H10 0.94(2) .
O1 C1 1.438(5) .
O1 H7 0.93(2) .
O2 C2 1.439(5) .
O2 H8 0.93(2) .
O6 C6 1.437(6) .
O6 H12 0.95(2) .
O5 C5 1.449(5) .
O5 H11 0.925(19) .
O7 H13 0.94(2) .
O7 H14 0.93(2) .
O3 C3 1.430(5) .
O3 H9 0.93(2) .
C1 C2 1.519(6) .
C1 H1A 0.9700 .
C1 H1B 0.9700 .
C2 C3 1.526(6) .
C2 H2 0.970(19) .
C3 C4 1.508(7) .
C3 H3 0.994(19) .
C4 H4A 0.9700 .
C4 H4B 0.9700 .
C5 C6 1.492(7) .
C5 C5 1.525(9) 2_666
C5 H5 0.980(19) .
C6 H6A 0.9700 .
C6 H6B 0.9700 .
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
O2 Tb1 O4 C4 -49.5(3) . .
O6 Tb1 O4 C4 -119.3(4) . .
O1 Tb1 O4 C4 20.3(3) . .
O5 Tb1 O4 C4 -152.5(3) . .
O7 Tb1 O4 C4 -15.3(4) . .
Cl1 Tb1 O4 C4 86.8(3) . .
Cl2 Tb1 O4 C4 159.0(4) . .
O2 Tb1 O1 C1 -8.8(3) . .
O6 Tb1 O1 C1 -21.5(4) . .
O5 Tb1 O1 C1 87.1(4) . .
O7 Tb1 O1 C1 71.6(3) . .
O4 Tb1 O1 C1 -85.3(3) . .
Cl1 Tb1 O1 C1 152.1(3) . .
Cl2 Tb1 O1 C1 -135.0(3) . .
O6 Tb1 O2 C2 149.4(3) . .
O1 Tb1 O2 C2 -20.9(3) . .
O5 Tb1 O2 C2 -162.8(3) . .
O7 Tb1 O2 C2 -101.0(3) . .
O4 Tb1 O2 C2 56.9(3) . .
Cl1 Tb1 O2 C2 -50.4(3) . .
Cl2 Tb1 O2 C2 94.8(3) . .
O2 Tb1 O6 C6 153.9(3) . .
O1 Tb1 O6 C6 166.2(3) . .
O5 Tb1 O6 C6 23.2(3) . .
O7 Tb1 O6 C6 84.9(3) . .
O4 Tb1 O6 C6 -135.3(3) . .
Cl1 Tb1 O6 C6 -2.1(4) . .
Cl2 Tb1 O6 C6 -63.4(3) . .
O2 Tb1 O5 C5 -40.2(3) . .
O6 Tb1 O5 C5 10.4(3) . .
O1 Tb1 O5 C5 -120.1(3) . .
O7 Tb1 O5 C5 -104.4(3) . .
O4 Tb1 O5 C5 47.8(4) . .
Cl1 Tb1 O5 C5 176.9(3) . .
Cl2 Tb1 O5 C5 93.5(3) . .
Tb1 O1 C1 C2 33.1(5) . .
Tb1 O2 C2 C1 44.6(4) . .
Tb1 O2 C2 C3 -79.9(4) . .
O1 C1 C2 O2 -46.1(5) . .
O1 C1 C2 C3 75.2(4) . .
O2 C2 C3 O3 -57.7(4) . .
C1 C2 C3 O3 -177.6(3) . .
O2 C2 C3 C4 69.5(5) . .
C1 C2 C3 C4 -50.4(5) . .
Tb1 O4 C4 C3 58.8(5) . .
O3 C3 C4 O4 68.3(5) . .
C2 C3 C4 O4 -57.2(5) . .
Tb1 O5 C5 C6 -38.2(4) . .
Tb1 O5 C5 C5 84.8(5) . 2_666
Tb1 O6 C6 C5 -50.7(4) . .
O5 C5 C6 O6 52.2(4) . .
C5 C5 C6 O6 -67.9(6) 2_666 .
