#------------------------------------------------------------------------------
#$Date: 2016-03-25 14:23:13 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179893 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/89/7018973.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_7018973
loop_
_publ_author_name
'Liang, Li'
'Peng, Guo'
'Li, Guizhu'
'Lan, Yanhua'
'Powell, Annie K.'
'Deng, Hong'
_publ_section_title
;
 In situ hydrothermal synthesis of dysprosium(iii) single-molecule magnet
 with lanthanide salt as catalyst
;
_journal_issue                   19
_journal_name_full               'Dalton Transactions'
_journal_page_first              5816
_journal_paper_doi               10.1039/c2dt30175j
_journal_volume                  41
_journal_year                    2012
_chemical_formula_moiety         'C32 H34 N16 O16 Tb2, 4(H2 O)'
_chemical_formula_sum            'C32 H42 N16 O20 Tb2'
_chemical_formula_weight         1288.68
_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                117.2750(10)
_cell_angle_beta                 98.1120(10)
_cell_angle_gamma                99.4350(10)
_cell_formula_units_Z            1
_cell_length_a                   9.1459(18)
_cell_length_b                   11.9522(10)
_cell_length_c                   12.1423(10)
_cell_measurement_reflns_used    3974
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.19
_cell_measurement_theta_min      1.95
_cell_volume                     1127.8(3)
_computing_cell_refinement       'Apex2 (Bruker, 2005)'
_computing_data_collection       'Apex2 (Bruker, 2005)'
_computing_data_reduction        'Apex2 (Bruker, 2005)'
_computing_molecular_graphics    'SHELXTL 6.12'
_computing_publication_material  'SHELXTL 6.12'
_computing_structure_refinement  'SHELXTL 6.12'
_computing_structure_solution    'SHELXTL 6.12 (Bruker, 2000-2003)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Bruker AXS SMART APEX CCD diffractometer'
_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  0.0146
_diffrn_reflns_av_sigmaI/netI    0.0279
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            5802
_diffrn_reflns_theta_full        25.19
_diffrn_reflns_theta_max         25.19
_diffrn_reflns_theta_min         1.95
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.206
_exptl_absorpt_correction_T_max  0.5019
_exptl_absorpt_correction_T_min  0.4471
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Apex2 (Bruker, 2005)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.897
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             636.0
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.508
_refine_diff_density_min         -0.651
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     330
_refine_ls_number_reflns         3974
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0229
_refine_ls_R_factor_gt           0.0210
_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)+(0.0227P)²+0.9385P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0489
_refine_ls_wR_factor_ref         0.0498
_reflns_number_gt                3744
_reflns_number_total             3974
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt30175j.txt
_cod_data_source_block           4
_cod_database_code               7018973
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
C1 C 0.7891(4) 0.6297(3) -0.1689(3) 0.0292(7) Uani 1 1 d .
C2 C 0.8942(4) 0.5432(3) -0.2121(3) 0.0271(7) Uani 1 1 d .
C3 C 0.9999(4) 0.5327(3) -0.1260(3) 0.0316(7) Uani 1 1 d .
C4 C 1.0962(4) 0.4527(3) -0.1688(3) 0.0385(8) Uani 1 1 d .
C5 C 1.0898(4) 0.3857(3) -0.2976(3) 0.0361(8) Uani 1 1 d .
C6 C 0.9855(4) 0.3949(3) -0.3855(3) 0.0282(7) Uani 1 1 d .
C7 C 0.9757(3) 0.3241(3) -0.5229(3) 0.0282(7) Uani 1 1 d .
C8 C 0.8865(4) 0.4734(3) -0.3413(3) 0.0274(7) Uani 1 1 d .
C9 C 0.5901(3) 1.0012(3) 0.1877(3) 0.0266(7) Uani 1 1 d .
C10 C 0.6519(3) 1.0143(3) 0.3156(3) 0.0251(6) Uani 1 1 d .
C11 C 0.7458(4) 0.9377(3) 0.3260(3) 0.0360(8) Uani 1 1 d .
C12 C 0.8018(5) 0.9494(4) 0.4440(4) 0.0445(9) Uani 1 1 d .
C13 C 0.7672(4) 1.0389(3) 0.5526(3) 0.0380(8) Uani 1 1 d .
C14 C 0.6740(4) 1.1174(3) 0.5430(3) 0.0264(6) Uani 1 1 d .
C15 C 0.6157(4) 1.1031(3) 0.4240(3) 0.0253(6) Uani 1 1 d .
C16 C 0.6407(4) 1.2126(3) 0.6593(3) 0.0276(7) Uani 1 1 d .
N1 N 1.0820(3) 0.2672(3) -0.5746(3) 0.0374(7) Uani 1 1 d .
N2 N 1.0271(3) 0.2139(3) -0.7017(3) 0.0395(7) Uani 1 1 d .
N3 N 0.8961(3) 0.2386(3) -0.7243(3) 0.0367(7) Uani 1 1 d .
N4 N 0.8608(3) 0.3091(3) -0.6126(3) 0.0332(6) Uani 1 1 d .
N5 N 0.6913(4) 1.2323(3) 0.7760(2) 0.0371(7) Uani 1 1 d .
N6 N 0.6319(4) 1.3263(3) 0.8536(3) 0.0425(7) Uani 1 1 d .
N7 N 0.5476(4) 1.3639(3) 0.7889(3) 0.0383(7) Uani 1 1 d .
N8 N 0.5522(3) 1.2934(3) 0.6668(2) 0.0313(6) Uani 1 1 d .
H8 H 0.5058 1.2990 0.6035 0.038 Uiso 1 1 calc R
O7 O 0.6786(3) 0.6178(2) -0.2528(2) 0.0340(5) Uani 1 1 d .
O8 O 0.8099(3) 0.7126(2) -0.0530(2) 0.0396(6) Uani 1 1 d .
O9 O 0.6283(3) 0.9209(2) 0.0933(2) 0.0382(6) Uani 1 1 d .
O10 O 0.50400(11) 1.07089(9) 0.18234(9) 0.0360(5) Uani 1 1 d .
O1W O 0.88573(11) 0.14359(9) 0.90388(9) 0.0642(8) Uani 1 1 d R
H1A H 0.9416 0.1243 0.8522 0.096 Uiso 1 1 d R
H1B H 0.9385 0.2151 0.9689 0.096 Uiso 1 1 d R
O2W O 0.39406(11) 0.36203(9) 0.51361(9) 0.0394(6) Uani 1 1 d R
H2A H 0.4287 0.3495 0.4495 0.059 Uiso 1 1 d R
H2B H 0.2984 0.3298 0.4862 0.059 Uiso 1 1 d R
O3W O 0.78894(11) 0.89928(9) -0.14307(9) 0.0509(7) Uani 1 1 d R
H3B H 0.8254 0.9783 -0.1060 0.076 Uiso 1 1 d R
H3A H 0.8463 0.8617 -0.1850 0.076 Uiso 1 1 d R
O4W O 0.47906(11) 0.61204(9) -0.08294(9) 0.0473(7) Uani 1 1 d R
H4B H 0.4423 0.6274 -0.0220 0.071 Uiso 1 1 d R
H4A H 0.5036 0.5441 -0.1106 0.071 Uiso 1 1 d R
O5W O 0.40970(11) 0.64279(9) -0.33436(9) 0.0346(5) Uani 1 1 d R
H5A H 0.3247 0.6538 -0.3530 0.052 Uiso 1 1 d R
H5B H 0.4031 0.5644 -0.3676 0.052 Uiso 1 1 d R
O6W O 0.32472(11) 0.79538(9) -0.07788(9) 0.0433(6) Uani 1 1 d R
H6A H 0.3019 0.8276 -0.0096 0.065 Uiso 1 1 d R
H6B H 0.2512 0.7743 -0.1371 0.065 Uiso 1 1 d R
Tb1 Tb 0.573695(16) 0.785879(13) -0.120737(12) 0.02412(6) Uani 1 1 d .
H5 H 0.774(3) 0.886(3) 0.258(3) 0.019(8) Uiso 1 1 d .
H9 H 0.551(4) 1.148(3) 0.412(3) 0.031(9) Uiso 1 1 d .
H1 H 1.005(4) 0.580(3) -0.045(3) 0.023(8) Uiso 1 1 d .
H2 H 1.165(4) 0.446(3) -0.106(4) 0.043(10) Uiso 1 1 d .
H4 H 0.821(4) 0.484(3) -0.394(3) 0.029(9) Uiso 1 1 d .
H7 H 0.812(5) 1.053(4) 0.638(4) 0.061(12) Uiso 1 1 d .
H6 H 0.863(5) 0.904(4) 0.453(4) 0.056(12) Uiso 1 1 d .
H3 H 1.148(4) 0.337(4) -0.324(4) 0.047(11) Uiso 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'
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'
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
O8 C1 O7 120.8(3) . .
O8 C1 C2 121.2(3) . .
O7 C1 C2 118.1(3) . .
C3 C2 C8 119.4(3) . .
C3 C2 C1 121.7(3) . .
C8 C2 C1 118.9(3) . .
C2 C3 C4 120.3(3) . .
C2 C3 H1 118(2) . .
C4 C3 H1 122(2) . .
C5 C4 C3 119.8(3) . .
C5 C4 H2 123(2) . .
C3 C4 H2 117(2) . .
C4 C5 C6 120.9(3) . .
C4 C5 H3 120(3) . .
C6 C5 H3 119(3) . .
C5 C6 C8 118.7(3) . .
C5 C6 C7 121.9(3) . .
C8 C6 C7 119.4(3) . .
N4 C7 N1 111.0(3) . .
N4 C7 C6 124.2(3) . .
N1 C7 C6 124.7(3) . .
C2 C8 C6 120.8(3) . .
C2 C8 H4 118(2) . .
C6 C8 H4 121(2) . .
O10 C9 O9 124.4(3) . .
O10 C9 C10 118.0(2) . .
O9 C9 C10 117.6(3) . .
C11 C10 C15 119.5(3) . .
C11 C10 C9 120.1(3) . .
C15 C10 C9 120.3(3) . .
C12 C11 C10 120.0(3) . .
C12 C11 H5 121(2) . .
C10 C11 H5 119(2) . .
C11 C12 C13 120.5(3) . .
C11 C12 H6 121(3) . .
C13 C12 H6 118(3) . .
C12 C13 C14 119.8(3) . .
C12 C13 H7 121(2) . .
C14 C13 H7 119(2) . .
C15 C14 C13 119.3(3) . .
C15 C14 C16 121.9(3) . .
C13 C14 C16 118.9(3) . .
C14 C15 C10 120.8(3) . .
C14 C15 H9 123(2) . .
C10 C15 H9 116(2) . .
N5 C16 N8 107.8(3) . .
N5 C16 C14 125.7(3) . .
N8 C16 C14 126.5(3) . .
C7 N1 N2 104.8(3) . .
N3 N2 N1 109.5(3) . .
N2 N3 N4 109.4(3) . .
C7 N4 N3 105.2(2) . .
C16 N5 N6 106.2(3) . .
N7 N6 N5 110.8(3) . .
N6 N7 N8 106.3(3) . .
C16 N8 N7 108.9(3) . .
C16 N8 H8 125.6 . .
N7 N8 H8 125.6 . .
C1 O7 Tb1 99.43(18) . .
C1 O8 Tb1 87.94(18) . .
C9 O9 Tb1 148.6(2) . .
C9 O10 Tb1 153.09(15) . 2_675
H1A O1W H1B 104.9 . .
H2A O2W H2B 106.7 . .
Tb1 O3W H3B 127.6 . .
Tb1 O3W H3A 122.0 . .
H3B O3W H3A 110.0 . .
Tb1 O4W H4B 119.0 . .
Tb1 O4W H4A 124.7 . .
H4B O4W H4A 113.4 . .
Tb1 O5W H5A 119.5 . .
Tb1 O5W H5B 118.6 . .
H5A O5W H5B 109.1 . .
Tb1 O6W H6A 129.3 . .
Tb1 O6W H6B 119.0 . .
H6A O6W H6B 111.0 . .
O9 Tb1 O3W 93.08(7) . .
O9 Tb1 O10 97.20(6) . 2_675
O3W Tb1 O10 72.93(4) . 2_675
O9 Tb1 O7 133.14(8) . .
O3W Tb1 O7 76.76(6) . .
O10 Tb1 O7 121.83(6) 2_675 .
O9 Tb1 O4W 87.59(7) . .
O3W Tb1 O4W 144.1 . .
O10 Tb1 O4W 142.560(18) 2_675 .
O7 Tb1 O4W 76.84(6) . .
O9 Tb1 O6W 76.58(6) . .
O3W Tb1 O6W 144.0 . .
O10 Tb1 O6W 74.33(4) 2_675 .
O7 Tb1 O6W 134.74(6) . .
O4W Tb1 O6W 70.7 . .
O9 Tb1 O5W 155.96(7) . .
O3W Tb1 O5W 106.7 . .
O10 Tb1 O5W 76.39(4) 2_675 .
O7 Tb1 O5W 66.53(6) . .
O4W Tb1 O5W 84.3 . .
O6W Tb1 O5W 79.4 . .
O9 Tb1 O8 81.43(7) . .
O3W Tb1 O8 72.04(6) . .
O10 Tb1 O8 144.80(6) 2_675 .
O7 Tb1 O8 51.80(7) . .
O4W Tb1 O8 72.63(6) . .
O6W Tb1 O8 137.67(6) . .
O5W Tb1 O8 117.22(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 O8 1.258(4) .
C1 O7 1.268(4) .
C1 C2 1.497(4) .
C2 C3 1.384(4) .
C2 C8 1.383(4) .
C3 C4 1.382(5) .
C3 H1 0.87(3) .
C4 C5 1.378(5) .
C4 H2 0.96(4) .
C5 C6 1.385(5) .
C5 H3 0.83(4) .
C6 C8 1.393(4) .
C6 C7 1.465(4) .
C7 N4 1.327(4) .
C7 N1 1.342(4) .
C8 H4 0.88(3) .
C9 O10 1.252(3) .
C9 O9 1.253(4) .
C9 C10 1.501(4) .
C10 C11 1.388(4) .
C10 C15 1.388(4) .
C11 C12 1.386(5) .
C11 H5 0.88(3) .
C12 C13 1.386(5) .
C12 H6 0.87(4) .
C13 C14 1.399(5) .
C13 H7 0.98(4) .
C14 C15 1.388(4) .
C14 C16 1.464(4) .
C15 H9 0.90(3) .
C16 N5 1.324(4) .
C16 N8 1.339(4) .
N1 N2 1.347(4) .
N2 N3 1.301(4) .
N3 N4 1.349(4) .
N5 N6 1.349(4) .
N6 N7 1.297(4) .
N7 N8 1.340(4) .
N8 H8 0.8600 .
O7 Tb1 2.375(2) .
O8 Tb1 2.625(2) .
O9 Tb1 2.266(2) .
O10 Tb1 2.3275(9) 2_675
O1W H1A 0.8397 .
O1W H1B 0.8521 .
O2W H2A 0.8408 .
O2W H2B 0.8448 .
O3W Tb1 2.3235 .
O3W H3B 0.8186 .
O3W H3A 0.8244 .
O4W Tb1 2.3818 .
O4W H4B 0.8122 .
O4W H4A 0.8087 .
O5W Tb1 2.4286 .
O5W H5A 0.8268 .
O5W H5B 0.8199 .
O6W Tb1 2.4153 .
O6W H6A 0.8135 .
O6W H6B 0.8208 .
Tb1 O10 2.3275(9) 2_675
