#------------------------------------------------------------------------------
#$Date: 2016-03-25 14:23:13 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179893 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/89/7018975.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_7018975
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 Er2 N16 O16, 4(H2 O)'
_chemical_formula_sum            'C32 H42 Er2 N16 O20'
_chemical_formula_weight         1305.34
_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                117.455(2)
_cell_angle_beta                 98.129(3)
_cell_angle_gamma                99.353(3)
_cell_formula_units_Z            1
_cell_length_a                   9.169(4)
_cell_length_b                   11.884(2)
_cell_length_c                   12.081(2)
_cell_measurement_reflns_used    4011
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      0.384
_cell_measurement_theta_min      0.33
_cell_volume                     1116.9(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 0.979
_diffrn_measured_fraction_theta_max 0.979
_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  0.0193
_diffrn_reflns_av_sigmaI/netI    0.0366
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5726
_diffrn_reflns_theta_full        25.19
_diffrn_reflns_theta_max         25.19
_diffrn_reflns_theta_min         1.96
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.828
_exptl_absorpt_correction_T_max  0.384
_exptl_absorpt_correction_T_min  0.330
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Apex2 (Bruker, 2005)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.941
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             642.0
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.922
_refine_diff_density_min         -0.995
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     330
_refine_ls_number_reflns         3929
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0277
_refine_ls_R_factor_gt           0.0247
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0306P)²+0.7034P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0594
_refine_ls_wR_factor_ref         0.0607
_reflns_number_gt                3638
_reflns_number_total             4011
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt30175j.txt
_cod_data_source_block           6
_cod_database_code               7018975
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 0.5903(4) 0.0014(4) 0.1850(4) 0.0237(8) Uani 1 1 d .
C2 C 0.6516(4) 0.0134(4) 0.3130(3) 0.0241(8) Uani 1 1 d .
C3 C 0.6159(5) 0.1022(4) 0.4222(4) 0.0247(8) Uani 1 1 d .
C4 C 0.6742(4) 0.1166(4) 0.5415(4) 0.0252(8) Uani 1 1 d .
C5 C 0.7670(5) 0.0380(4) 0.5505(4) 0.0354(10) Uani 1 1 d .
C6 C 0.8021(6) -0.0512(5) 0.4410(4) 0.0429(12) Uani 1 1 d .
C7 C 0.7476(5) -0.0617(4) 0.3232(4) 0.0349(10) Uani 1 1 d .
C8 C 0.6404(5) 0.2113(4) 0.6586(4) 0.0268(9) Uani 1 1 d .
C9 C 0.2134(5) 0.3693(4) 0.1687(4) 0.0282(9) Uani 1 1 d .
C10 C 0.1088(4) 0.4567(4) 0.2123(4) 0.0252(8) Uani 1 1 d .
C11 C 0.0023(5) 0.4659(4) 0.1249(4) 0.0310(9) Uani 1 1 d .
C12 C -0.0953(5) 0.5451(4) 0.1681(4) 0.0369(10) Uani 1 1 d .
C13 C -0.0905(5) 0.6123(4) 0.2978(4) 0.0350(10) Uani 1 1 d .
C14 C 0.0167(5) 0.6047(4) 0.3868(4) 0.0264(9) Uani 1 1 d .
C15 C 0.1166(5) 0.5279(4) 0.3422(4) 0.0271(9) Uani 1 1 d .
C16 C 0.0250(4) 0.6760(4) 0.5250(4) 0.0280(9) Uani 1 1 d .
Er1 Er 0.42761(2) 0.215334(17) 0.122349(15) 0.02326(7) Uani 1 1 d .
H1 H -0.006(5) 0.413(5) 0.039(5) 0.043(13) Uiso 1 1 d .
H2 H -0.171(5) 0.553(4) 0.103(4) 0.030(11) Uiso 1 1 d .
H3 H -0.165(5) 0.649(5) 0.330(4) 0.042(13) Uiso 1 1 d .
H4 H 0.175(5) 0.515(4) 0.395(4) 0.024(11) Uiso 1 1 d .
H5 H 0.558(5) 0.139(4) 0.412(4) 0.020(11) Uiso 1 1 d .
H6 H 0.779(5) -0.112(4) 0.253(4) 0.033(12) Uiso 1 1 d .
H7 H 0.862(6) -0.097(5) 0.448(5) 0.053(15) Uiso 1 1 d .
H8 H 0.802(6) 0.045(5) 0.628(5) 0.052(15) Uiso 1 1 d .
N1 N 0.5521(4) 0.2923(3) 0.6670(3) 0.0305(8) Uani 1 1 d .
H9 H 0.5056 0.2978 0.6033 0.037 Uiso 1 1 calc R
N2 N 0.5469(4) 0.3639(4) 0.7897(3) 0.0363(9) Uani 1 1 d .
N3 N 0.6316(5) 0.3256(4) 0.8547(3) 0.0398(9) Uani 1 1 d .
N4 N 0.6906(4) 0.2309(4) 0.7762(3) 0.0365(9) Uani 1 1 d .
N5 N -0.0808(4) 0.7324(4) 0.5763(3) 0.0351(8) Uani 1 1 d .
N6 N -0.0274(4) 0.7860(4) 0.7044(3) 0.0375(9) Uani 1 1 d .
N7 N 0.1040(4) 0.7612(4) 0.7269(3) 0.0361(8) Uani 1 1 d .
N8 N 0.1389(4) 0.6919(3) 0.6157(3) 0.0314(8) Uani 1 1 d .
O7 O 0.1937(4) 0.2868(3) 0.0525(3) 0.0386(7) Uani 1 1 d .
O8 O 0.3245(3) 0.3827(3) 0.2530(3) 0.0330(7) Uani 1 1 d .
O9 O 0.5018(3) 0.0698(3) 0.1794(3) 0.0337(7) Uani 1 1 d .
O10 O 0.62904(13) -0.07900(12) 0.08945(11) 0.0355(7) Uani 1 1 d .
O1W O 0.10848(13) 0.86239(12) 0.10205(11) 0.0687(12) Uani 1 1 d R
H1A H 0.1488 0.8195 0.1314 0.103 Uiso 1 1 d R
H1B H 0.0141 0.8234 0.0732 0.103 Uiso 1 1 d R
O2W O 0.39242(13) 0.36258(12) 0.51419(11) 0.0386(7) Uani 1 1 d R
H2A H 0.4381 0.3546 0.4565 0.058 Uiso 1 1 d R
H2B H 0.3034 0.3134 0.4779 0.058 Uiso 1 1 d R
O3W O 0.21569(13) 0.10343(12) 0.14409(11) 0.0483(9) Uani 1 1 d R
H3A H 0.2039 0.0256 0.1222 0.072 Uiso 1 1 d R
H3B H 0.1474 0.1305 0.1781 0.072 Uiso 1 1 d R
O4W O 0.58898(13) 0.35453(12) 0.33227(11) 0.0329(7) Uani 1 1 d R
H4A H 0.6710 0.3404 0.3498 0.049 Uiso 1 1 d R
H4B H 0.5944 0.4330 0.3682 0.049 Uiso 1 1 d R
O5W O 0.52143(13) 0.38684(12) 0.08520(11) 0.0433(8) Uani 1 1 d R
H5A H 0.4951 0.4550 0.1113 0.065 Uiso 1 1 d R
H5B H 0.5749 0.3787 0.0354 0.065 Uiso 1 1 d R
O6W O 0.67114(13) 0.20341(12) 0.07517(11) 0.0403(8) Uani 1 1 d R
H6A H 0.7434 0.2081 0.1273 0.060 Uiso 1 1 d R
H6B H 0.6874 0.1725 0.0033 0.060 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'
Er Er -0.2586 4.9576 '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
O9 C1 O10 124.2(3) . .
O9 C1 C2 118.3(3) . .
O10 C1 C2 117.5(3) . .
C3 C2 C7 119.5(4) . .
C3 C2 C1 120.3(3) . .
C7 C2 C1 120.2(3) . .
C2 C3 C4 121.0(4) . .
C2 C3 H5 117(3) . .
C4 C3 H5 122(3) . .
C3 C4 C5 119.2(4) . .
C3 C4 C8 122.0(4) . .
C5 C4 C8 118.7(4) . .
C6 C5 C4 119.7(4) . .
C6 C5 H8 121(3) . .
C4 C5 H8 119(3) . .
C7 C6 C5 120.7(4) . .
C7 C6 H7 120(4) . .
C5 C6 H7 119(4) . .
C6 C7 C2 119.9(4) . .
C6 C7 H6 121(3) . .
C2 C7 H6 119(3) . .
N4 C8 N1 107.5(3) . .
N4 C8 C4 125.9(4) . .
N1 C8 C4 126.5(3) . .
O7 C9 O8 120.8(4) . .
O7 C9 C10 121.3(4) . .
O8 C9 C10 117.9(3) . .
C15 C10 C11 119.4(4) . .
C15 C10 C9 119.1(3) . .
C11 C10 C9 121.5(4) . .
C12 C11 C10 120.0(4) . .
C12 C11 H1 122(3) . .
C10 C11 H1 118(3) . .
C13 C12 C11 120.2(4) . .
C13 C12 H2 120(2) . .
C11 C12 H2 119(2) . .
C12 C13 C14 120.3(4) . .
C12 C13 H3 124(3) . .
C14 C13 H3 114(3) . .
C15 C14 C13 118.6(4) . .
C15 C14 C16 120.0(4) . .
C13 C14 C16 121.3(4) . .
C10 C15 C14 121.3(4) . .
C10 C15 H4 119(3) . .
C14 C15 H4 119(3) . .
N8 C16 N5 110.8(4) . .
N8 C16 C14 124.2(3) . .
N5 C16 C14 125.0(4) . .
O10 Er1 O3W 92.12(4) 2_655 .
O10 Er1 O9 95.72(8) 2_655 .
O3W Er1 O9 72.77(8) . .
O10 Er1 O5W 88.40(4) 2_655 .
O3W Er1 O5W 144.24(5) . .
O9 Er1 O5W 142.74(8) . .
O10 Er1 O8 132.88(7) 2_655 .
O3W Er1 O8 76.78(8) . .
O9 Er1 O8 122.83(10) . .
O5W Er1 O8 76.86(8) . .
O10 Er1 O4W 156.209(17) 2_655 .
O3W Er1 O4W 106.8 . .
O9 Er1 O4W 76.92(8) . .
O5W Er1 O4W 84.5 . .
O8 Er1 O4W 67.24(8) . .
O10 Er1 O6W 76.14(5) 2_655 .
O3W Er1 O6W 144.10(6) . .
O9 Er1 O6W 74.79(8) . .
O5W Er1 O6W 70.3 . .
O8 Er1 O6W 135.38(8) . .
O4W Er1 O6W 80.1 . .
O10 Er1 O7 80.71(7) 2_655 .
O3W Er1 O7 71.93(8) . .
O9 Er1 O7 144.34(11) . .
O5W Er1 O7 72.89(8) . .
O8 Er1 O7 52.23(9) . .
O4W Er1 O7 118.41(7) . .
O6W Er1 O7 136.63(8) . .
C8 N1 N2 109.6(3) . .
C8 N1 H9 125.2 . .
N2 N1 H9 125.2 . .
N3 N2 N1 105.8(3) . .
N2 N3 N4 110.7(3) . .
C8 N4 N3 106.4(3) . .
C16 N5 N6 105.1(3) . .
N7 N6 N5 108.9(3) . .
N6 N7 N8 109.3(3) . .
C16 N8 N7 105.9(3) . .
C9 O7 Er1 87.5(2) . .
C9 O8 Er1 99.4(2) . .
C1 O9 Er1 152.2(3) . .
C1 O10 Er1 148.29(19) . 2_655
H1A O1W H1B 105.9 . .
H2A O2W H2B 107.7 . .
Er1 O3W H3A 119.9 . .
Er1 O3W H3B 129.9 . .
H3A O3W H3B 109.9 . .
Er1 O4W H4A 118.7 . .
Er1 O4W H4B 119.3 . .
H4A O4W H4B 111.6 . .
Er1 O5W H5A 124.7 . .
Er1 O5W H5B 121.7 . .
H5A O5W H5B 113.0 . .
Er1 O6W H6A 121.2 . .
Er1 O6W H6B 125.9 . .
H6A O6W H6B 110.2 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 O9 1.254(5) .
C1 O10 1.257(4) .
C1 C2 1.500(5) .
C2 C3 1.382(5) .
C2 C7 1.383(6) .
C3 C4 1.385(5) .
C3 H5 0.77(4) .
C4 C5 1.391(6) .
C4 C8 1.461(5) .
C5 C6 1.383(6) .
C5 H8 0.90(5) .
C6 C7 1.381(6) .
C6 H7 0.85(5) .
C7 H6 0.91(4) .
C8 N4 1.326(5) .
C8 N1 1.334(5) .
C9 O7 1.251(5) .
C9 O8 1.266(5) .
C9 C10 1.497(5) .
C10 C15 1.382(5) .
C10 C11 1.388(6) .
C11 C12 1.384(6) .
C11 H1 0.92(5) .
C12 C13 1.382(6) .
C12 H2 1.02(4) .
C13 C14 1.397(6) .
C13 H3 0.90(5) .
C14 C15 1.385(5) .
C14 C16 1.466(6) .
C15 H4 0.86(4) .
C16 N8 1.322(5) .
C16 N5 1.332(5) .
Er1 O10 2.2293(12) 2_655
Er1 O3W 2.2891(14) .
Er1 O9 2.298(3) .
Er1 O5W 2.3406(13) .
Er1 O8 2.341(3) .
Er1 O4W 2.3732(12) .
Er1 O6W 2.3914(15) .
Er1 O7 2.603(3) .
N1 N2 1.339(5) .
N1 H9 0.8600 .
N2 N3 1.303(5) .
N3 N4 1.348(5) .
N5 N6 1.348(5) .
N6 N7 1.307(5) .
N7 N8 1.332(5) .
O10 Er1 2.2293(12) 2_655
O1W H1A 0.8442 .
O1W H1B 0.8489 .
O2W H2A 0.8398 .
O2W H2B 0.8414 .
O3W H3A 0.8193 .
O3W H3B 0.8251 .
O4W H4A 0.8169 .
O4W H4B 0.8161 .
O5W H5A 0.8146 .
O5W H5B 0.8111 .
O6W H6A 0.8220 .
O6W H6B 0.8188 .
