#------------------------------------------------------------------------------
#$Date: 2016-03-25 14:23:13 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179893 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/89/7018976.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_7018976
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 Eu2 N16 O16, 4(H2 O)'
_chemical_formula_sum            'C32 H42 Eu2 N16 O20'
_chemical_formula_weight         1274.76
_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                117.270(2)
_cell_angle_beta                 98.188(3)
_cell_angle_gamma                99.407(3)
_cell_formula_units_Z            1
_cell_length_a                   9.150(4)
_cell_length_b                   11.993(2)
_cell_length_c                   12.181(2)
_cell_measurement_reflns_used    4007
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.20
_cell_measurement_theta_min      1.94
_cell_volume                     1135.6(6)
_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 0.983
_diffrn_measured_fraction_theta_max 0.983
_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  0.0234
_diffrn_reflns_av_sigmaI/netI    0.0406
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            5801
_diffrn_reflns_theta_full        25.20
_diffrn_reflns_theta_max         25.20
_diffrn_reflns_theta_min         1.94
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.832
_exptl_absorpt_correction_T_max  0.5387
_exptl_absorpt_correction_T_min  0.4846
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Apex2 (Bruker, 2005)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.864
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             632.0
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.181
_refine_diff_density_min         -1.034
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         4007
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0304
_refine_ls_R_factor_gt           0.0281
_refine_ls_shift/su_max          0.045
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0393P)²+0.7653P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0706
_refine_ls_wR_factor_ref         0.0720
_reflns_number_gt                3750
_reflns_number_total             4007
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt30175j.txt
_cod_data_source_block           3
_cod_database_code               7018976
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
C1 C 0.4102(4) 0.4997(4) 0.8098(3) 0.0270(8) Uani 1 1 d
C2 C 0.3476(4) 0.4853(4) 0.6817(4) 0.0256(8) Uani 1 1 d
C3 C 0.3828(4) 0.3964(4) 0.5740(4) 0.0263(8) Uani 1 1 d
C4 C 0.3251(4) 0.3817(4) 0.4556(4) 0.0274(8) Uani 1 1 d
C5 C 0.3588(4) 0.2868(4) 0.3399(4) 0.0276(8) Uani 1 1 d
C6 C 0.2336(6) 0.4605(5) 0.4458(4) 0.0382(10) Uani 1 1 d
C7 C 0.1991(6) 0.5499(5) 0.5531(4) 0.0441(12) Uani 1 1 d
C8 C 0.2547(5) 0.5625(4) 0.6712(4) 0.0354(10) Uani 1 1 d
C9 C 0.7908(4) 0.1298(4) 0.8307(4) 0.0281(8) Uani 1 1 d
C10 C 0.8955(4) 0.0426(4) 0.7872(4) 0.0270(8) Uani 1 1 d
C11 C 1.0012(5) 0.0315(4) 0.8740(4) 0.0332(9) Uani 1 1 d
C12 C 1.0958(5) -0.0481(4) 0.8314(4) 0.0377(10) Uani 1 1 d
C13 C 1.0912(5) -0.1151(4) 0.7029(4) 0.0373(10) Uani 1 1 d
C14 C 0.9859(4) -0.1046(4) 0.6149(4) 0.0283(8) Uani 1 1 d
C15 C 0.9772(4) -0.1759(4) 0.4778(4) 0.0290(8) Uani 1 1 d
C16 C 0.8877(4) -0.0271(4) 0.6585(4) 0.0283(8) Uani 1 1 d
Eu1 Eu 0.57485(2) 0.287281(17) 0.880537(15) 0.02436(8) Uani 1 1 d
H1 H 1.003(5) 0.080(4) 0.956(4) 0.029(11) Uiso 1 1 d
H2 H 1.163(6) -0.065(5) 0.885(5) 0.053(15) Uiso 1 1 d
H3 H 1.154(6) -0.163(5) 0.672(5) 0.048(14) Uiso 1 1 d
H4 H 0.824(5) -0.015(4) 0.598(4) 0.036(12) Uiso 1 1 d
H5 H 0.217(5) 0.613(4) 0.744(4) 0.030(11) Uiso 1 1 d
H6 H 0.136(6) 0.590(6) 0.547(5) 0.061(17) Uiso 1 1 d
H7 H 0.441(5) 0.342(4) 0.580(4) 0.021(10) Uiso 1 1 d
H8 H 0.192(6) 0.450(5) 0.362(5) 0.055(15) Uiso 1 1 d
N1 N 0.3091(4) 0.2668(4) 0.2235(3) 0.0377(8) Uani 1 1 d
N2 N 0.3678(5) 0.1731(4) 0.1468(3) 0.0427(9) Uani 1 1 d
N3 N 0.4517(4) 0.1367(4) 0.2117(3) 0.0386(9) Uani 1 1 d
N4 N 0.4463(4) 0.2061(3) 0.3327(3) 0.0316(8) Uani 1 1 d
N5 N 0.8613(4) -0.1910(3) 0.3881(3) 0.0325(8) Uani 1 1 d
N6 N 0.8960(4) -0.2613(4) 0.2785(3) 0.0374(8) Uani 1 1 d
N7 N 1.0266(4) -0.2872(4) 0.2998(3) 0.0386(9) Uani 1 1 d
N8 N 1.0824(4) -0.2332(4) 0.4267(3) 0.0375(8) Uani 1 1 d
O7 O 0.4950(3) 0.4286(3) 0.8150(3) 0.0371(7) Uani 1 1 d
O8 O 0.3727(3) 0.5802(3) 0.9035(2) 0.0384(7) Uani 1 1 d
O9 O 0.6800(3) 0.1175(3) 0.7469(3) 0.0347(7) Uani 1 1 d
O10 O 0.8113(3) 0.2116(3) 0.9455(3) 0.0395(7) Uani 1 1 d
O1W O 0.6054(4) 0.1381(4) 0.4859(3) 0.0416(8) Uani 1 1 d
H1A H 0.563(7) 0.132(6) 0.524(6) 0.062 Uiso 1 1 d
H1B H 0.687(7) 0.180(6) 0.516(6) 0.062 Uiso 1 1 d
O2W O 0.8850(5) 0.6454(4) 0.9066(4) 0.0619(11) Uani 1 1 d
H2A H 0.860(9) 0.686(8) 0.882(8) 0.093 Uiso 1 1 d
H2B H 0.970(9) 0.650(8) 0.894(8) 0.093 Uiso 1 1 d
O3W O 0.4093(4) 0.1420(3) 0.6647(3) 0.0351(7) Uani 1 1 d
H3A H 0.324(6) 0.151(5) 0.644(5) 0.053 Uiso 1 1 d
H3B H 0.404(6) 0.063(6) 0.635(5) 0.053 Uiso 1 1 d
O4W O 0.7935(5) 0.4024(3) 0.8589(4) 0.0530(10) Uani 1 1 d
H4B H 0.805(9) 0.459(7) 0.866(7) 0.079 Uiso 1 1 d
H4A H 0.861(7) 0.362(6) 0.812(6) 0.079 Uiso 1 1 d
O5W O 0.3216(4) 0.2969(4) 0.9215(3) 0.0452(9) Uani 1 1 d
H5A H 0.251(7) 0.293(6) 0.864(6) 0.068 Uiso 1 1 d
H5B H 0.303(7) 0.322(6) 0.977(6) 0.068 Uiso 1 1 d
O6W O 0.4791(5) 0.1112(3) 0.9182(4) 0.0477(9) Uani 1 1 d
H6B H 0.491(7) 0.041(6) 0.884(6) 0.072 Uiso 1 1 d
H6A H 0.437(7) 0.125(6) 0.971(6) 0.072 Uiso 1 1 d
H9 H 0.495(5) 0.192(5) 0.382(5) 0.037(14) 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'
Eu Eu -0.1578 3.6682 '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'
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 124.6(4) . .
O8 C1 C2 117.7(3) . .
O7 C1 C2 117.7(3) . .
C3 C2 C8 119.6(4) . .
C3 C2 C1 120.4(3) . .
C8 C2 C1 119.9(3) . .
C4 C3 C2 121.0(4) . .
C4 C3 H7 119(2) . .
C2 C3 H7 120(3) . .
C3 C4 C6 119.1(4) . .
C3 C4 C5 122.0(4) . .
C6 C4 C5 118.8(4) . .
N1 C5 N4 107.5(3) . .
N1 C5 C4 126.0(4) . .
N4 C5 C4 126.5(4) . .
C7 C6 C4 120.0(4) . .
C7 C6 H8 120(3) . .
C4 C6 H8 120(3) . .
C6 C7 C8 120.7(4) . .
C6 C7 H6 121(4) . .
C8 C7 H6 118(4) . .
C7 C8 C2 119.6(4) . .
C7 C8 H5 122(2) . .
C2 C8 H5 118(2) . .
O10 C9 O9 120.8(3) . .
O10 C9 C10 121.4(4) . .
O9 C9 C10 117.8(3) . .
C16 C10 C11 119.4(4) . .
C16 C10 C9 119.1(4) . .
C11 C10 C9 121.5(3) . .
C12 C11 C10 120.1(4) . .
C12 C11 H1 124(3) . .
C10 C11 H1 116(3) . .
C11 C12 C13 120.6(4) . .
C11 C12 H2 123(3) . .
C13 C12 H2 116(3) . .
C12 C13 C14 119.9(4) . .
C12 C13 H3 123(3) . .
C14 C13 H3 117(3) . .
C16 C14 C13 119.1(4) . .
C16 C14 C15 119.9(4) . .
C13 C14 C15 121.0(4) . .
N5 C15 N8 111.3(4) . .
N5 C15 C14 123.6(3) . .
N8 C15 C14 125.2(4) . .
C14 C16 C10 120.9(4) . .
C14 C16 H4 118(3) . .
C10 C16 H4 121(3) . .
O8 Eu1 O7 98.92(10) 2_667 .
O8 Eu1 O4W 93.95(14) 2_667 .
O7 Eu1 O4W 73.13(12) . .
O8 Eu1 O9 133.11(10) 2_667 .
O7 Eu1 O9 120.97(10) . .
O4W Eu1 O9 76.99(11) . .
O8 Eu1 O6W 86.55(12) 2_667 .
O7 Eu1 O6W 142.35(12) . .
O4W Eu1 O6W 144.04(13) . .
O9 Eu1 O6W 76.68(11) . .
O8 Eu1 O5W 76.49(12) 2_667 .
O7 Eu1 O5W 73.97(12) . .
O4W Eu1 O5W 143.73(13) . .
O9 Eu1 O5W 134.45(12) . .
O6W Eu1 O5W 71.20(13) . .
O8 Eu1 O3W 155.49(11) 2_667 .
O7 Eu1 O3W 75.73(11) . .
O4W Eu1 O3W 106.90(14) . .
O9 Eu1 O3W 66.07(10) . .
O6W Eu1 O3W 84.01(13) . .
O5W Eu1 O3W 79.06(11) . .
O8 Eu1 O10 82.00(10) 2_667 .
O7 Eu1 O10 145.07(11) . .
O4W Eu1 O10 71.98(12) . .
O9 Eu1 O10 51.29(9) . .
O6W Eu1 O10 72.50(12) . .
O5W Eu1 O10 138.53(11) . .
O3W Eu1 O10 116.26(10) . .
O8 Eu1 H4B 90.2(16) 2_667 .
O7 Eu1 H4B 64.0(15) . .
O4W Eu1 H4B 10.5(15) . .
O9 Eu1 H4B 86.7(16) . .
O6W Eu1 H4B 153.6(15) . .
O5W Eu1 H4B 133.2(15) . .
O3W Eu1 H4B 108.0(16) . .
O10 Eu1 H4B 81.1(15) . .
C5 N1 N2 106.5(3) . .
N3 N2 N1 110.5(3) . .
N2 N3 N4 106.7(3) . .
N3 N4 C5 108.8(4) . .
N3 N4 H9 116(4) . .
C5 N4 H9 136(4) . .
N6 N5 C15 104.8(3) . .
N7 N6 N5 110.2(3) . .
N6 N7 N8 109.0(3) . .
C15 N8 N7 104.7(3) . .
C1 O7 Eu1 153.4(3) . .
C1 O8 Eu1 148.6(3) . 2_667
C9 O9 Eu1 99.2(2) . .
C9 O10 Eu1 88.7(2) . .
H1A O1W H1B 118(7) . .
H2A O2W H2B 100(8) . .
Eu1 O3W H3A 121(4) . .
Eu1 O3W H3B 116(4) . .
H3A O3W H3B 109(5) . .
Eu1 O4W H4B 126(7) . .
Eu1 O4W H4A 124(4) . .
H4B O4W H4A 107(8) . .
Eu1 O5W H5A 119(4) . .
Eu1 O5W H5B 129(6) . .
H5A O5W H5B 109(7) . .
Eu1 O6W H6B 126(5) . .
Eu1 O6W H6A 118(5) . .
H6B O6W H6A 116(7) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 O8 1.249(5) .
C1 O7 1.258(5) .
C1 C2 1.503(5) .
C2 C3 1.383(5) .
C2 C8 1.389(6) .
C3 C4 1.383(5) .
C3 H7 0.93(4) .
C4 C6 1.393(6) .
C4 C5 1.464(5) .
C5 N1 1.320(5) .
C5 N4 1.335(5) .
C6 C7 1.378(6) .
C6 H8 0.98(5) .
C7 C8 1.385(6) .
C7 H6 0.83(6) .
C8 H5 0.97(4) .
C9 O10 1.250(5) .
C9 O9 1.269(5) .
C9 C10 1.502(5) .
C10 C16 1.383(5) .
C10 C11 1.396(6) .
C11 C12 1.368(6) .
C11 H1 0.89(4) .
C12 C13 1.384(6) .
C12 H2 0.94(5) .
C13 C14 1.401(6) .
C13 H3 0.88(5) .
C14 C16 1.381(5) .
C14 C15 1.469(6) .
C15 N5 1.333(5) .
C15 N8 1.335(5) .
C16 H4 0.95(5) .
Eu1 O8 2.289(3) 2_667
Eu1 O7 2.351(3) .
Eu1 O4W 2.358(4) .
Eu1 O9 2.403(3) .
Eu1 O6W 2.415(3) .
Eu1 O5W 2.448(3) .
Eu1 O3W 2.459(3) .
Eu1 O10 2.635(3) .
Eu1 H4B 2.77(7) .
N1 N2 1.342(5) .
N2 N3 1.287(5) .
N3 N4 1.333(5) .
N4 H9 0.79(5) .
N5 N6 1.331(5) .
N6 N7 1.304(5) .
N7 N8 1.348(5) .
O8 Eu1 2.289(3) 2_667
O1W H1A 0.66(6) .
O1W H1B 0.76(6) .
O2W H2A 0.72(7) .
O2W H2B 0.81(8) .
O3W H3A 0.83(5) .
O3W H3B 0.84(6) .
O4W H4B 0.63(7) .
O4W H4A 0.94(7) .
O5W H5A 0.86(6) .
O5W H5B 0.67(6) .
O6W H6B 0.79(6) .
O6W H6A 0.77(7) .
