#------------------------------------------------------------------------------
#$Date: 2016-03-25 14:23:13 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179893 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/89/7018977.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_7018977
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 Sm2, 4(H2 O)'
_chemical_formula_sum            'C32 H42 N16 O20 Sm2'
_chemical_formula_weight         1271.54
_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                117.2010(10)
_cell_angle_beta                 98.160(2)
_cell_angle_gamma                99.347(2)
_cell_formula_units_Z            1
_cell_length_a                   9.128(3)
_cell_length_b                   11.9957(15)
_cell_length_c                   12.2137(15)
_cell_measurement_reflns_used    4004
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.20
_cell_measurement_theta_min      1.93
_cell_volume                     1137.5(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  0.0209
_diffrn_reflns_av_sigmaI/netI    0.0358
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5859
_diffrn_reflns_theta_full        25.20
_diffrn_reflns_theta_max         25.20
_diffrn_reflns_theta_min         1.93
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.651
_exptl_absorpt_correction_T_max  0.5572
_exptl_absorpt_correction_T_min  0.5037
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Apex2 (Bruker, 2005)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.856
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             630.0
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.816
_refine_diff_density_min         -0.937
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     356
_refine_ls_number_reflns         4004
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0270
_refine_ls_R_factor_gt           0.0251
_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)+(0.0357P)²+0.4705P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0628
_refine_ls_wR_factor_ref         0.0643
_reflns_number_gt                3756
_reflns_number_total             4004
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt30175j.txt
_cod_data_source_block           5
_cod_database_code               7018977
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 -0.0905(4) 0.4989(3) 0.8081(3) 0.0269(7) Uani 1 1 d .
C2 C -0.1518(4) 0.4857(3) 0.6803(3) 0.0256(7) Uani 1 1 d .
C3 C -0.1165(4) 0.3954(3) 0.5731(3) 0.0265(7) Uani 1 1 d .
H3 H -0.0535 0.3444 0.5807 0.032 Uiso 1 1 calc R
C4 C -0.1750(4) 0.3809(3) 0.4543(3) 0.0257(7) Uani 1 1 d .
C5 C -0.2671(5) 0.4597(4) 0.4445(3) 0.0365(8) Uani 1 1 d .
H5 H -0.3056 0.4515 0.3658 0.044 Uiso 1 1 calc R
C6 C -0.1413(4) 0.2866(3) 0.3399(3) 0.0274(7) Uani 1 1 d .
C7 C -0.3010(5) 0.5495(4) 0.5511(4) 0.0443(10) Uani 1 1 d .
H7 H -0.3617 0.6022 0.5441 0.053 Uiso 1 1 calc R
C8 C -0.2449(4) 0.5620(3) 0.6696(3) 0.0351(8) Uani 1 1 d .
H8 H -0.2700 0.6216 0.7411 0.042 Uiso 1 1 calc R
C9 C 0.2916(4) 0.1299(3) 0.8309(3) 0.0285(7) Uani 1 1 d .
C10 C 0.3958(4) 0.0427(3) 0.7876(3) 0.0268(7) Uani 1 1 d .
C11 C 0.5005(4) 0.0312(3) 0.8740(3) 0.0331(8) Uani 1 1 d .
H11 H 0.5064 0.0775 0.9605 0.040 Uiso 1 1 calc R
C12 C 0.5962(5) -0.0497(4) 0.8304(4) 0.0375(9) Uani 1 1 d .
H12 H 0.6644 -0.0593 0.8879 0.045 Uiso 1 1 calc R
C13 C 0.5913(4) -0.1160(4) 0.7031(4) 0.0366(8) Uani 1 1 d .
H13 H 0.6580 -0.1682 0.6753 0.044 Uiso 1 1 calc R
C14 C 0.4866(4) -0.1054(3) 0.6154(3) 0.0279(7) Uani 1 1 d .
C15 C 0.4778(4) -0.1755(3) 0.4789(3) 0.0277(7) Uani 1 1 d .
C16 C 0.3892(4) -0.0258(3) 0.6596(3) 0.0279(7) Uani 1 1 d .
H16 H 0.3184 -0.0186 0.6020 0.033 Uiso 1 1 calc R
H1 H -0.005(6) 0.188(5) 0.386(5) 0.064(15) Uiso 1 1 d .
H1A H 0.641(8) 0.324(6) 0.136(6) 0.096 Uiso 1 1 d .
H2A H 0.191(8) 0.185(6) 0.523(6) 0.096 Uiso 1 1 d .
H3A H -0.184(7) 0.156(6) 0.647(6) 0.096 Uiso 1 1 d .
H4A H 0.315(8) 0.466(6) 0.884(7) 0.096 Uiso 1 1 d .
H5A H -0.064(7) 0.126(6) 0.968(6) 0.096 Uiso 1 1 d .
H6A H -0.222(7) 0.312(6) 0.969(6) 0.096 Uiso 1 1 d .
H1B H 0.529(8) 0.320(7) 0.067(7) 0.096 Uiso 1 1 d .
H2B H 0.069(8) 0.148(7) 0.531(6) 0.096 Uiso 1 1 d .
H3B H -0.104(7) 0.065(6) 0.623(6) 0.096 Uiso 1 1 d .
H4B H 0.358(7) 0.370(6) 0.806(6) 0.096 Uiso 1 1 d .
H5B H -0.007(8) 0.047(6) 0.892(6) 0.096 Uiso 1 1 d .
H6B H -0.257(7) 0.291(6) 0.862(6) 0.096 Uiso 1 1 d .
N1 N -0.0536(4) 0.2058(3) 0.3328(3) 0.0308(6) Uani 1 1 d .
N2 N -0.0484(4) 0.1349(3) 0.2118(3) 0.0384(7) Uani 1 1 d .
N3 N -0.1317(4) 0.1721(3) 0.1467(3) 0.0422(8) Uani 1 1 d .
N4 N -0.1916(4) 0.2658(3) 0.2234(3) 0.0364(7) Uani 1 1 d .
N5 N 0.3613(3) -0.1910(3) 0.3898(3) 0.0325(7) Uani 1 1 d .
N6 N 0.3964(4) -0.2617(3) 0.2792(3) 0.0361(7) Uani 1 1 d .
N7 N 0.5276(4) -0.2866(3) 0.3016(3) 0.0382(7) Uani 1 1 d .
N8 N 0.5823(4) -0.2333(3) 0.4275(3) 0.0370(7) Uani 1 1 d .
O1 O -0.0051(3) 0.4285(2) 0.8133(2) 0.0368(6) Uani 1 1 d .
O2 O -0.1271(3) 0.5806(2) 0.9011(2) 0.0387(6) Uani 1 1 d .
O5 O 0.3128(3) 0.2116(2) 0.9458(2) 0.0381(6) Uani 1 1 d .
O6 O 0.1807(3) 0.1177(2) 0.7477(2) 0.0346(6) Uani 1 1 d .
O1W O 0.6161(4) 0.3529(3) 0.0924(4) 0.0568(9) Uani 1 1 d .
O2W O 0.1051(3) 0.1385(3) 0.4862(3) 0.0396(7) Uani 1 1 d .
O3W O -0.0909(3) 0.1414(3) 0.6641(2) 0.0344(6) Uani 1 1 d .
O4W O 0.2952(4) 0.4025(3) 0.8584(4) 0.0516(8) Uani 1 1 d .
O5W O -0.0228(4) 0.1108(3) 0.9180(3) 0.0492(8) Uani 1 1 d .
O6W O -0.1791(3) 0.2981(3) 0.9206(3) 0.0472(7) Uani 1 1 d .
Sm1 Sm 0.075312(18) 0.288643(15) 0.881626(13) 0.02404(7) 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'
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'
Sm Sm -0.1638 3.4418 '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 C1 O1 124.9(3) . .
O2 C1 C2 117.3(3) . .
O1 C1 C2 117.8(3) . .
C8 C2 C3 120.0(3) . .
C8 C2 C1 120.1(3) . .
C3 C2 C1 119.9(3) . .
C2 C3 C4 120.3(3) . .
C2 C3 H3 119.8 . .
C4 C3 H3 119.8 . .
C3 C4 C5 119.3(3) . .
C3 C4 C6 121.8(3) . .
C5 C4 C6 118.9(3) . .
C7 C5 C4 120.1(3) . .
C7 C5 H5 119.9 . .
C4 C5 H5 119.9 . .
N4 C6 N1 107.4(3) . .
N4 C6 C4 126.0(3) . .
N1 C6 C4 126.6(3) . .
C5 C7 C8 120.5(3) . .
C5 C7 H7 119.8 . .
C8 C7 H7 119.8 . .
C2 C8 C7 119.7(3) . .
C2 C8 H8 120.1 . .
C7 C8 H8 120.1 . .
O5 C9 O6 121.1(3) . .
O5 C9 C10 121.1(3) . .
O6 C9 C10 117.7(3) . .
C16 C10 C11 119.6(3) . .
C16 C10 C9 119.2(3) . .
C11 C10 C9 121.2(3) . .
C12 C11 C10 119.6(3) . .
C12 C11 H11 120.2 . .
C10 C11 H11 120.2 . .
C13 C12 C11 120.7(3) . .
C13 C12 H12 119.7 . .
C11 C12 H12 119.7 . .
C12 C13 C14 120.3(3) . .
C12 C13 H13 119.9 . .
C14 C13 H13 119.9 . .
C16 C14 C13 118.7(3) . .
C16 C14 C15 119.7(3) . .
C13 C14 C15 121.6(3) . .
N5 C15 N8 111.1(3) . .
N5 C15 C14 123.8(3) . .
N8 C15 C14 125.1(3) . .
C10 C16 C14 121.1(3) . .
C10 C16 H16 119.4 . .
C14 C16 H16 119.4 . .
C6 N1 N2 109.2(3) . .
C6 N1 H1 135(3) . .
N2 N1 H1 116(3) . .
N3 N2 N1 106.4(3) . .
N2 N3 N4 110.4(3) . .
C6 N4 N3 106.7(3) . .
C15 N5 N6 104.9(3) . .
N7 N6 N5 109.6(3) . .
N6 N7 N8 109.3(3) . .
C15 N8 N7 105.2(3) . .
C1 O1 Sm1 152.7(2) . .
C1 O2 Sm1 148.3(2) . 2_567
C9 O5 Sm1 88.5(2) . .
C9 O6 Sm1 99.1(2) . .
H1A O1W H1B 102(6) . .
H2A O2W H2B 104(7) . .
Sm1 O3W H3A 117(4) . .
Sm1 O3W H3B 128(5) . .
H3A O3W H3B 105(5) . .
Sm1 O4W H4A 123(6) . .
Sm1 O4W H4B 129(4) . .
H4A O4W H4B 108(7) . .
Sm1 O5W H5A 116(5) . .
Sm1 O5W H5B 128(5) . .
H5A O5W H5B 115(7) . .
Sm1 O6W H6A 144(5) . .
Sm1 O6W H6B 122(4) . .
H6A O6W H6B 94(6) . .
O2 Sm1 O1 100.32(9) 2_567 .
O2 Sm1 O4W 94.92(12) 2_567 .
O1 Sm1 O4W 73.15(10) . .
O2 Sm1 O6 132.78(9) 2_567 .
O1 Sm1 O6 120.32(8) . .
O4W Sm1 O6 76.74(10) . .
O2 Sm1 O5W 86.14(10) 2_567 .
O1 Sm1 O5W 142.02(11) . .
O4W Sm1 O5W 144.11(11) . .
O6 Sm1 O5W 76.47(9) . .
O2 Sm1 O6W 76.80(10) 2_567 .
O1 Sm1 O6W 73.92(10) . .
O4W Sm1 O6W 143.88(11) . .
O6 Sm1 O6W 134.10(10) . .
O5W Sm1 O6W 71.26(11) . .
O2 Sm1 O3W 155.53(10) 2_567 .
O1 Sm1 O3W 75.38(9) . .
O4W Sm1 O3W 106.45(11) . .
O6 Sm1 O3W 65.61(9) . .
O5W Sm1 O3W 83.45(11) . .
O6W Sm1 O3W 78.89(10) . .
O2 Sm1 O5 81.87(8) 2_567 .
O1 Sm1 O5 145.07(9) . .
O4W Sm1 O5 71.94(10) . .
O6 Sm1 O5 51.16(8) . .
O5W Sm1 O5 72.72(10) . .
O6W Sm1 O5 138.98(10) . .
O3W Sm1 O5 115.69(8) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 O2 1.249(4) .
C1 O1 1.254(4) .
C1 C2 1.507(4) .
C2 C8 1.381(5) .
C2 C3 1.389(4) .
C3 C4 1.393(4) .
C3 H3 0.9300 .
C4 C5 1.396(5) .
C4 C6 1.455(4) .
C5 C7 1.375(5) .
C5 H5 0.9300 .
C6 N4 1.323(4) .
C6 N1 1.335(5) .
C7 C8 1.394(5) .
C7 H7 0.9300 .
C8 H8 0.9300 .
C9 O5 1.253(4) .
C9 O6 1.266(4) .
C9 C10 1.496(5) .
C10 C16 1.380(5) .
C10 C11 1.392(5) .
C11 C12 1.387(5) .
C11 H11 0.9300 .
C12 C13 1.375(5) .
C12 H12 0.9300 .
C13 C14 1.397(5) .
C13 H13 0.9300 .
C14 C16 1.391(5) .
C14 C15 1.466(5) .
C15 N5 1.331(4) .
C15 N8 1.332(4) .
C16 H16 0.9300 .
N1 N2 1.340(4) .
N1 H1 0.86(5) .
N2 N3 1.293(4) .
N3 N4 1.350(4) .
N5 N6 1.345(4) .
N6 N7 1.302(4) .
N7 N8 1.343(4) .
O1 Sm1 2.357(2) .
O2 Sm1 2.307(2) 2_567
O5 Sm1 2.645(3) .
O6 Sm1 2.414(2) .
O1W H1A 0.78(6) .
O1W H1B 0.77(7) .
O2W H2A 0.81(7) .
O2W H2B 0.65(6) .
O3W Sm1 2.485(2) .
O3W H3A 0.91(6) .
O3W H3B 0.80(6) .
O4W Sm1 2.367(3) .
O4W H4A 0.66(6) .
O4W H4B 0.91(6) .
O5W Sm1 2.431(3) .
O5W H5A 0.73(6) .
O5W H5B 0.73(6) .
O6W Sm1 2.446(3) .
O6W H6A 0.73(6) .
O6W H6B 0.89(6) .
Sm1 O2 2.307(2) 2_567
