#------------------------------------------------------------------------------
#$Date: 2016-03-25 14:23:13 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179893 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/89/7018974.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_7018974
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 Dy2 N16 O16, 4(H2 O)'
_chemical_formula_sum            'C32 H42 Dy2 N16 O20'
_chemical_formula_weight         1295.82
_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                117.3780(10)
_cell_angle_beta                 98.139(2)
_cell_angle_gamma                99.356(2)
_cell_formula_units_Z            1
_cell_length_a                   9.164(3)
_cell_length_b                   11.9340(17)
_cell_length_c                   12.1166(17)
_cell_measurement_reflns_used    3965
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.20
_cell_measurement_theta_min      1.95
_cell_volume                     1125.1(4)
_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 0.981
_diffrn_measured_fraction_theta_max 0.981
_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  0.0177
_diffrn_reflns_av_sigmaI/netI    0.0326
_diffrn_reflns_limit_h_max       10
_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       -10
_diffrn_reflns_number            5769
_diffrn_reflns_theta_full        25.20
_diffrn_reflns_theta_max         25.20
_diffrn_reflns_theta_min         1.95
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.392
_exptl_absorpt_correction_T_max  0.4504
_exptl_absorpt_correction_T_min  0.4296
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Apex2 (Bruker, 2005)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.913
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             638.0
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.671
_refine_diff_density_min         -0.668
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         3965
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0249
_refine_ls_R_factor_gt           0.0235
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0231P)²+1.3115P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0584
_refine_ls_wR_factor_ref         0.0591
_reflns_number_gt                3786
_reflns_number_total             3965
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt30175j.txt
_cod_data_source_block           2
_cod_database_code               7018974
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 0.4098(4) 0.4987(3) 0.3134(3) 0.0247(8) Uani 1 1 d .
C2 C 0.3478(4) 0.4857(3) 0.1856(3) 0.0254(8) Uani 1 1 d .
C3 C 0.2539(5) 0.5626(4) 0.1751(4) 0.0337(9) Uani 1 1 d .
H8 H 0.2289 0.6223 0.2475 0.040 Uiso 1 1 calc R
C4 C 0.1980(5) 0.5501(4) 0.0574(4) 0.0407(10) Uani 1 1 d .
H7 H 0.1359 0.6024 0.0512 0.049 Uiso 1 1 calc R
C5 C 0.2325(5) 0.4613(4) -0.0519(4) 0.0374(10) Uani 1 1 d .
H6 H 0.1941 0.4539 -0.1309 0.045 Uiso 1 1 calc R
C6 C 0.3259(4) 0.3827(3) -0.0423(3) 0.0249(8) Uani 1 1 d .
C7 C 0.3833(4) 0.3962(3) 0.0764(3) 0.0239(7) Uani 1 1 d .
H4 H 0.4464 0.3448 0.0832 0.029 Uiso 1 1 calc R
C8 C 0.3600(4) 0.2880(4) -0.1584(3) 0.0266(8) Uani 1 1 d .
C9 C 0.2125(4) 0.8702(4) 0.6692(4) 0.0275(8) Uani 1 1 d .
C10 C 0.1067(4) 0.9568(3) 0.7125(3) 0.0262(8) Uani 1 1 d .
C11 C 0.0006(2) 0.96650(19) 0.62540(18) 0.0311(8) Uani 1 1 d .
H21 H -0.0053 0.9192 0.5381 0.037 Uiso 1 1 calc R
O1W O 0.3925(2) 0.86184(19) 1.01346(18) 0.0373(7) Uani 1 1 d R
H1B H 0.4326 0.8602 0.9545 0.056 Uiso 1 1 d R
H1A H 0.3095 0.8024 0.9768 0.056 Uiso 1 1 d R
O2W O 0.1116(2) 0.35945(19) 0.59801(18) 0.0652(10) Uani 1 1 d R
H2B H 0.0221 0.3588 0.6095 0.098 Uiso 1 1 d R
H2A H 0.1438 0.3118 0.6247 0.098 Uiso 1 1 d R
C12 C -0.0961(5) 1.0463(4) 0.6683(4) 0.0362(9) Uani 1 1 d .
H14 H -0.1652 1.0546 0.6101 0.043 Uiso 1 1 calc R
C13 C -0.0897(4) 1.1139(4) 0.7979(4) 0.0337(9) Uani 1 1 d .
H13 H -0.1566 1.1657 0.8264 0.040 Uiso 1 1 calc R
C14 C 0.0155(4) 1.1050(3) 0.8859(3) 0.0256(8) Uani 1 1 d .
C15 C 0.1145(4) 1.0268(3) 0.8419(3) 0.0260(8) Uani 1 1 d .
H11 H 0.1869 1.0216 0.9003 0.031 Uiso 1 1 calc R
C16 C 0.0242(4) 1.1759(4) 1.0237(4) 0.0273(8) Uani 1 1 d .
Dy1 Dy 0.426767(18) 0.714686(15) 0.621247(14) 0.02224(7) Uani 1 1 d .
N1 N 0.4479(4) 0.2075(3) -0.1663(3) 0.0301(7) Uani 1 1 d .
H1 H 0.4943 0.2018 -0.1030 0.036 Uiso 1 1 calc R
N2 N 0.4522(4) 0.1368(3) -0.2889(3) 0.0362(8) Uani 1 1 d .
N3 N 0.3685(4) 0.1745(3) -0.3535(3) 0.0401(8) Uani 1 1 d .
N4 N 0.3089(4) 0.2680(3) -0.2763(3) 0.0352(8) Uani 1 1 d .
N5 N 0.1394(3) 1.1915(3) 1.1138(3) 0.0307(7) Uani 1 1 d .
N6 N 0.1034(4) 1.2613(3) 1.2257(3) 0.0355(8) Uani 1 1 d .
N7 N -0.0269(4) 1.2860(3) 1.2029(3) 0.0370(8) Uani 1 1 d .
N8 N -0.0811(4) 1.2332(3) 1.0755(3) 0.0346(8) Uani 1 1 d .
O7 O 0.4966(3) 0.4295(3) 0.3189(2) 0.0340(6) Uani 1 1 d .
O8 O 0.3719(3) 0.5791(3) 0.4081(2) 0.0358(7) Uani 1 1 d .
O9 O 0.1914(3) 0.7875(3) 0.5532(3) 0.0381(7) Uani 1 1 d .
O10 O 0.32304(14) 0.88286(12) 0.75307(12) 0.0320(6) Uani 1 1 d .
O3W O 0.21127(14) 0.60021(12) 0.64260(12) 0.0476(8) Uani 1 1 d R
H3B H 0.1518 0.6312 0.6849 0.071 Uiso 1 1 d R
H3A H 0.2935 0.6124 0.6887 0.071 Uiso 1 1 d R
O5W O 0.52065(14) 0.88761(12) 0.58351(12) 0.0455(8) Uani 1 1 d R
H5B H 0.5726 0.8744 0.5311 0.068 Uiso 1 1 d R
H5A H 0.5069 0.9609 0.6119 0.068 Uiso 1 1 d R
O6W O 0.67337(14) 0.70339(12) 0.57631(12) 0.0404(7) Uani 1 1 d R
H6B H 0.7467 0.7174 0.6329 0.061 Uiso 1 1 d R
H6A H 0.6932 0.6675 0.5061 0.061 Uiso 1 1 d R
O4W O 0.59050(14) 0.85670(12) 0.83349(12) 0.0332(6) Uani 1 1 d R
H4A H 0.6002 0.9356 0.8644 0.050 Uiso 1 1 d R
H4B H 0.6725 0.8428 0.8537 0.050 Uiso 1 1 d 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'
Dy Dy -0.1892 4.4098 '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
O7 C1 O8 124.3(3) . .
O7 C1 C2 118.2(3) . .
O8 C1 C2 117.5(3) . .
C7 C2 C3 119.4(3) . .
C7 C2 C1 120.2(3) . .
C3 C2 C1 120.3(3) . .
C4 C3 C2 119.8(3) . .
C4 C3 H8 120.1 . .
C2 C3 H8 120.1 . .
C3 C4 C5 121.2(4) . .
C3 C4 H7 119.4 . .
C5 C4 H7 119.4 . .
C4 C5 C6 119.3(4) . .
C4 C5 H6 120.4 . .
C6 C5 H6 120.4 . .
C7 C6 C5 119.5(3) . .
C7 C6 C8 121.6(3) . .
C5 C6 C8 118.9(3) . .
C6 C7 C2 120.8(3) . .
C6 C7 H4 119.6 . .
C2 C7 H4 119.6 . .
N4 C8 N1 107.6(3) . .
N4 C8 C6 125.6(3) . .
N1 C8 C6 126.8(3) . .
O9 C9 O10 121.0(3) . .
O9 C9 C10 120.8(3) . .
O10 C9 C10 118.1(3) . .
C15 C10 C11 119.6(3) . .
C15 C10 C9 118.8(3) . .
C11 C10 C9 121.6(3) . .
C12 C11 C10 120.1(3) . .
C12 C11 H21 119.9 . .
C10 C11 H21 119.9 . .
H1B O1W H1A 106.2 . .
H2B O2W H2A 106.1 . .
C11 C12 C13 119.8(3) . .
C11 C12 H14 120.1 . .
C13 C12 H14 120.1 . .
C12 C13 C14 120.6(3) . .
C12 C13 H13 119.7 . .
C14 C13 H13 119.7 . .
C13 C14 C15 119.0(3) . .
C13 C14 C16 121.5(3) . .
C15 C14 C16 119.5(3) . .
C10 C15 C14 120.7(3) . .
C10 C15 H11 119.6 . .
C14 C15 H11 119.6 . .
N5 C16 N8 111.0(3) . .
N5 C16 C14 123.9(3) . .
N8 C16 C14 125.0(3) . .
O8 Dy1 O7 96.52(10) . 2_666
O8 Dy1 O3W 92.51(8) . .
O7 Dy1 O3W 72.85(8) 2_666 .
O8 Dy1 O10 133.23(7) . .
O7 Dy1 O10 122.26(7) 2_666 .
O3W Dy1 O10 77.11(4) . .
O8 Dy1 O5W 87.89(8) . .
O7 Dy1 O5W 142.66(8) 2_666 .
O3W Dy1 O5W 144.21(6) . .
O10 Dy1 O5W 76.76(4) . .
O8 Dy1 O4W 155.78(8) . .
O7 Dy1 O4W 76.67(8) 2_666 .
O3W Dy1 O4W 107.2 . .
O10 Dy1 O4W 66.80(4) . .
O5W Dy1 O4W 84.3 . .
O8 Dy1 O6W 76.19(8) . .
O7 Dy1 O6W 74.34(8) 2_666 .
O3W Dy1 O6W 143.70(6) . .
O10 Dy1 O6W 135.06(6) . .
O5W Dy1 O6W 70.8 . .
O4W Dy1 O6W 79.6 . .
O8 Dy1 O9 81.40(9) . .
O7 Dy1 O9 144.64(10) 2_666 .
O3W Dy1 O9 71.99(8) . .
O10 Dy1 O9 51.92(7) . .
O5W Dy1 O9 72.70(8) . .
O4W Dy1 O9 117.62(7) . .
O6W Dy1 O9 137.45(7) . .
O8 Dy1 H3A 104.4 . .
O7 Dy1 H3A 55.7 2_666 .
O3W Dy1 H3A 20.4 . .
O10 Dy1 H3A 81.2 . .
O5W Dy1 H3A 157.6 . .
O4W Dy1 H3A 91.0 . .
O6W Dy1 H3A 129.9 . .
O9 Dy1 H3A 90.4 . .
C8 N1 N2 109.0(3) . .
C8 N1 H1 125.5 . .
N2 N1 H1 125.5 . .
N3 N2 N1 106.5(3) . .
N2 N3 N4 110.9(3) . .
C8 N4 N3 106.1(3) . .
C16 N5 N6 105.1(3) . .
N7 N6 N5 109.4(3) . .
N6 N7 N8 109.5(3) . .
C16 N8 N7 105.0(3) . .
C1 O7 Dy1 152.9(3) . 2_666
C1 O8 Dy1 148.7(2) . .
C9 O9 Dy1 87.7(2) . .
C9 O10 Dy1 99.34(17) . .
Dy1 O3W H3B 126.9 . .
Dy1 O3W H3A 63.0 . .
H3B O3W H3A 111.4 . .
Dy1 O5W H5B 118.1 . .
Dy1 O5W H5A 130.7 . .
H5B O5W H5A 111.1 . .
Dy1 O6W H6B 120.0 . .
Dy1 O6W H6A 128.1 . .
H6B O6W H6A 109.7 . .
Dy1 O4W H4A 117.8 . .
Dy1 O4W H4B 119.9 . .
H4A O4W H4B 109.9 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 O7 1.252(4) .
C1 O8 1.251(4) .
C1 C2 1.499(5) .
C2 C7 1.390(5) .
C2 C3 1.391(5) .
C3 C4 1.376(6) .
C3 H8 0.9300 .
C4 C5 1.383(6) .
C4 H7 0.9300 .
C5 C6 1.400(5) .
C5 H6 0.9300 .
C6 C7 1.385(5) .
C6 C8 1.460(5) .
C7 H4 0.9300 .
C8 N4 1.333(5) .
C8 N1 1.330(5) .
C9 O9 1.254(4) .
C9 O10 1.265(4) .
C9 C10 1.501(5) .
C10 C15 1.381(5) .
C10 C11 1.389(4) .
C11 C12 1.383(4) .
C11 H21 0.9300 .
O1W H1B 0.8426 .
O1W H1A 0.8469 .
O2W H2B 0.8506 .
O2W H2A 0.8443 .
C12 C13 1.384(6) .
C12 H14 0.9300 .
C13 C14 1.387(5) .
C13 H13 0.9300 .
C14 C15 1.391(5) .
C14 C16 1.467(5) .
C15 H11 0.9300 .
C16 N5 1.328(5) .
C16 N8 1.335(5) .
Dy1 O8 2.251(2) .
Dy1 O7 2.318(3) 2_666
Dy1 O3W 2.3294(14) .
Dy1 O10 2.3632(12) .
Dy1 O5W 2.3685(13) .
Dy1 O4W 2.4102(13) .
Dy1 O6W 2.4086(14) .
Dy1 O9 2.617(3) .
Dy1 H3A 2.0891 .
N1 N2 1.339(4) .
N1 H1 0.8600 .
N2 N3 1.292(5) .
N3 N4 1.342(5) .
N5 N6 1.348(4) .
N6 N7 1.299(5) .
N7 N8 1.346(5) .
O7 Dy1 2.318(3) 2_666
O3W H3B 0.8161 .
O3W H3A 0.8192 .
O5W H5B 0.8200 .
O5W H5A 0.8189 .
O6W H6B 0.8228 .
O6W H6A 0.8215 .
O4W H4A 0.8204 .
O4W H4B 0.8236 .
