#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/57/7015752.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_7015752
loop_
_publ_author_name
'Chen, Gong-Jun'
'Gao, Chun-Yan'
'Tian, Jin-Lei'
'Tang, Jinkui'
'Gu, Wen'
'Liu, Xin'
'Yan, Shi-Ping'
'Liao, Dai-Zheng'
'Cheng, Peng'
_publ_section_title
;
 Coordination-perturbed single-molecule magnet behaviour of mononuclear
 dysprosium complexes.
;
_journal_issue                   20
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5579
_journal_page_last               5583
_journal_paper_doi               10.1039/c1dt10050e
_journal_volume                  40
_journal_year                    2011
_chemical_formula_sum            'C27 H29 Dy N2 O6'
_chemical_formula_weight         640.02
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 116.52(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.5010(19)
_cell_length_b                   21.015(4)
_cell_length_c                   16.246(5)
_cell_measurement_temperature    293(2)
_cell_volume                     2902.4(13)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker P4'
_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  0.0504
_diffrn_reflns_av_sigmaI/netI    0.0534
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            20794
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.08
_exptl_absorpt_coefficient_mu    2.613
_exptl_absorpt_correction_T_max  0.609
_exptl_absorpt_correction_T_min  0.461
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   crystalclear
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.465
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1276
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.710
_refine_diff_density_min         -0.788
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     331
_refine_ls_number_reflns         6609
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0656
_refine_ls_R_factor_gt           0.0396
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0344P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0763
_refine_ls_wR_factor_ref         0.0820
_reflns_number_gt                4853
_reflns_number_total             6647
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1dt10050e.txt
_cod_data_source_block           a
_cod_original_cell_volume        2902.4(12)
_cod_original_sg_symbol_H-M      P21/c
_cod_original_formula_sum        'C27 H29 Dy N2 O6 '
_cod_database_code               7015752
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy1 Dy 0.76142(2) 0.846645(8) 0.340635(12) 0.03888(8) Uani 1 1 d . . .
O1 O 0.8264(4) 0.95364(13) 0.3477(2) 0.0562(8) Uani 1 1 d . . .
O2 O 0.7142(3) 0.89093(13) 0.45597(19) 0.0517(7) Uani 1 1 d . . .
O3 O 0.7568(4) 0.86539(14) 0.1988(2) 0.0615(9) Uani 1 1 d . . .
O4 O 0.5135(4) 0.88845(14) 0.2459(2) 0.0619(8) Uani 1 1 d . . .
O5 O 0.8349(4) 0.75033(13) 0.2999(2) 0.0583(8) Uani 1 1 d . . .
O6 O 0.5931(3) 0.76897(13) 0.3477(2) 0.0563(8) Uani 1 1 d . . .
N1 N 1.0572(4) 0.85097(14) 0.3895(2) 0.0428(8) Uani 1 1 d . . .
N2 N 0.9421(4) 0.79234(14) 0.4952(2) 0.0419(8) Uani 1 1 d . . .
C1 C 1.1149(6) 0.8809(2) 0.3400(3) 0.0559(12) Uani 1 1 d . . .
H1 H 1.0474 0.9061 0.2914 0.067 Uiso 1 1 calc R . .
C2 C 1.2724(6) 0.8767(3) 0.3568(4) 0.0652(15) Uani 1 1 d . . .
H2 H 1.3079 0.8984 0.3197 0.078 Uiso 1 1 calc R . .
C3 C 1.3711(6) 0.8408(2) 0.4269(4) 0.0712(16) Uani 1 1 d . . .
H3 H 1.4757 0.8370 0.4381 0.085 Uiso 1 1 calc R . .
C4 C 1.3181(5) 0.8094(2) 0.4832(3) 0.0591(12) Uani 1 1 d . . .
C5 C 1.4171(6) 0.7722(3) 0.5618(4) 0.0880(18) Uani 1 1 d . . .
H5 H 1.5226 0.7671 0.5756 0.106 Uiso 1 1 calc R . .
C6 C 1.3623(7) 0.7446(3) 0.6157(4) 0.0879(18) Uani 1 1 d . . .
H6 H 1.4305 0.7215 0.6669 0.106 Uiso 1 1 calc R . .
C7 C 1.1994(7) 0.7499(2) 0.5958(3) 0.0650(13) Uani 1 1 d . . .
C8 C 1.1363(8) 0.7244(3) 0.6518(4) 0.0825(17) Uani 1 1 d . . .
H8 H 1.2005 0.7012 0.7038 0.099 Uiso 1 1 calc R . .
C9 C 0.9848(8) 0.7332(2) 0.6312(4) 0.0792(17) Uani 1 1 d . . .
H9 H 0.9437 0.7172 0.6693 0.095 Uiso 1 1 calc R . .
C10 C 0.8891(6) 0.7670(2) 0.5513(3) 0.0567(12) Uani 1 1 d . . .
H10 H 0.7833 0.7720 0.5367 0.068 Uiso 1 1 calc R . .
C11 C 1.0961(5) 0.78480(18) 0.5182(3) 0.0438(10) Uani 1 1 d . . .
C12 C 1.1579(5) 0.81549(19) 0.4616(3) 0.0430(10) Uani 1 1 d . . .
C13 C 0.8418(8) 1.0652(2) 0.3554(4) 0.0901(19) Uani 1 1 d . . .
H13A H 0.9440 1.0792 0.3995 0.135 Uiso 1 1 calc R . .
H13B H 0.7644 1.0960 0.3513 0.135 Uiso 1 1 calc R . .
H13C H 0.8407 1.0605 0.2963 0.135 Uiso 1 1 calc R . .
C14 C 0.8046(6) 1.0021(2) 0.3854(3) 0.0580(12) Uani 1 1 d . . .
C15 C 0.7535(6) 1.0008(2) 0.4530(4) 0.0692(14) Uani 1 1 d . . .
H15 H 0.7430 1.0396 0.4773 0.083 Uiso 1 1 calc R . .
C16 C 0.7172(5) 0.9467(2) 0.4869(3) 0.0571(12) Uani 1 1 d . . .
C17 C 0.6810(6) 0.9499(3) 0.5690(3) 0.0811(16) Uani 1 1 d . . .
H17A H 0.5889 0.9251 0.5566 0.122 Uiso 1 1 calc R . .
H17B H 0.6626 0.9934 0.5798 0.122 Uiso 1 1 calc R . .
H17C H 0.7686 0.9334 0.6225 0.122 Uiso 1 1 calc R . .
C18 C 0.7600(9) 0.9233(3) 0.0748(4) 0.117(3) Uani 1 1 d . . .
H18A H 0.8258 0.9600 0.0992 0.175 Uiso 1 1 calc R . .
H18B H 0.6798 0.9325 0.0141 0.175 Uiso 1 1 calc R . .
H18C H 0.8226 0.8882 0.0723 0.175 Uiso 1 1 calc R . .
C19 C 0.6836(7) 0.9061(3) 0.1366(3) 0.0717(15) Uani 1 1 d . . .
C20 C 0.5444(7) 0.9349(3) 0.1233(4) 0.0919(19) Uani 1 1 d . . .
H20 H 0.4995 0.9636 0.0750 0.110 Uiso 1 1 calc R . .
C21 C 0.4669(7) 0.9241(3) 0.1765(4) 0.0836(17) Uani 1 1 d . . .
C22 C 0.3082(8) 0.9581(4) 0.1517(5) 0.154(4) Uani 1 1 d . . .
H22A H 0.2245 0.9275 0.1294 0.231 Uiso 1 1 calc R . .
H22B H 0.2898 0.9894 0.1049 0.231 Uiso 1 1 calc R . .
H22C H 0.3119 0.9786 0.2055 0.231 Uiso 1 1 calc R . .
C23 C 0.9305(10) 0.6463(2) 0.3061(6) 0.121(3) Uani 1 1 d . . .
H23A H 0.9058 0.6406 0.2424 0.181 Uiso 1 1 calc R . .
H23B H 0.9233 0.6061 0.3321 0.181 Uiso 1 1 calc R . .
H23C H 1.0354 0.6627 0.3387 0.181 Uiso 1 1 calc R . .
C24 C 0.8166(7) 0.6923(2) 0.3138(3) 0.0670(14) Uani 1 1 d . . .
C25 C 0.6972(8) 0.6709(2) 0.3350(4) 0.0763(16) Uani 1 1 d . . .
H25 H 0.6896 0.6272 0.3413 0.092 Uiso 1 1 calc R . .
C26 C 0.5909(6) 0.7085(2) 0.3472(3) 0.0653(13) Uani 1 1 d . . .
C27 C 0.4592(7) 0.6778(3) 0.3606(5) 0.102(2) Uani 1 1 d . . .
H27A H 0.4796 0.6818 0.4238 0.152 Uiso 1 1 calc R . .
H27B H 0.4525 0.6336 0.3445 0.152 Uiso 1 1 calc R . .
H27C H 0.3617 0.6985 0.3221 0.152 Uiso 1 1 calc 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
_geom_angle_publ_flag
O2 Dy1 O3 144.47(10) . . ?
O2 Dy1 O1 73.33(9) . . ?
O3 Dy1 O1 76.77(10) . . ?
O2 Dy1 O6 81.69(10) . . ?
O3 Dy1 O6 117.43(11) . . ?
O1 Dy1 O6 148.42(10) . . ?
O2 Dy1 O5 140.52(10) . . ?
O3 Dy1 O5 74.96(10) . . ?
O1 Dy1 O5 138.44(10) . . ?
O6 Dy1 O5 72.80(10) . . ?
O2 Dy1 O4 83.03(11) . . ?
O3 Dy1 O4 73.46(11) . . ?
O1 Dy1 O4 80.56(11) . . ?
O6 Dy1 O4 77.46(10) . . ?
O5 Dy1 O4 118.78(11) . . ?
O2 Dy1 N1 108.59(10) . . ?
O3 Dy1 N1 80.38(11) . . ?
O1 Dy1 N1 73.68(10) . . ?
O6 Dy1 N1 134.00(10) . . ?
O5 Dy1 N1 72.06(10) . . ?
O4 Dy1 N1 146.76(10) . . ?
O2 Dy1 N2 71.08(10) . . ?
O3 Dy1 N2 138.47(11) . . ?
O1 Dy1 N2 109.41(10) . . ?
O6 Dy1 N2 79.36(10) . . ?
O5 Dy1 N2 74.91(10) . . ?
O4 Dy1 N2 147.35(10) . . ?
N1 Dy1 N2 63.50(10) . . ?
C14 O1 Dy1 135.5(3) . . ?
C16 O2 Dy1 135.6(3) . . ?
C19 O3 Dy1 131.8(3) . . ?
C21 O4 Dy1 131.5(3) . . ?
C24 O5 Dy1 134.6(3) . . ?
C26 O6 Dy1 135.4(3) . . ?
C1 N1 C12 117.6(4) . . ?
C1 N1 Dy1 121.8(3) . . ?
C12 N1 Dy1 120.1(2) . . ?
C10 N2 C11 117.2(4) . . ?
C10 N2 Dy1 123.3(3) . . ?
C11 N2 Dy1 119.2(2) . . ?
N1 C1 C2 123.5(5) . . ?
N1 C1 H1 118.2 . . ?
C2 C1 H1 118.2 . . ?
C3 C2 C1 118.9(5) . . ?
C3 C2 H2 120.6 . . ?
C1 C2 H2 120.6 . . ?
C2 C3 C4 120.3(5) . . ?
C2 C3 H3 119.8 . . ?
C4 C3 H3 119.8 . . ?
C3 C4 C12 117.5(5) . . ?
C3 C4 C5 123.9(5) . . ?
C12 C4 C5 118.6(5) . . ?
C6 C5 C4 121.9(5) . . ?
C6 C5 H5 119.1 . . ?
C4 C5 H5 119.1 . . ?
C5 C6 C7 121.0(5) . . ?
C5 C6 H6 119.5 . . ?
C7 C6 H6 119.5 . . ?
C8 C7 C11 116.9(5) . . ?
C8 C7 C6 123.6(5) . . ?
C11 C7 C6 119.5(5) . . ?
C9 C8 C7 120.7(5) . . ?
C9 C8 H8 119.7 . . ?
C7 C8 H8 119.7 . . ?
C8 C9 C10 118.8(5) . . ?
C8 C9 H9 120.6 . . ?
C10 C9 H9 120.6 . . ?
N2 C10 C9 123.3(5) . . ?
N2 C10 H10 118.3 . . ?
C9 C10 H10 118.3 . . ?
N2 C11 C7 123.0(4) . . ?
N2 C11 C12 118.0(4) . . ?
C7 C11 C12 118.9(4) . . ?
N1 C12 C4 122.2(4) . . ?
N1 C12 C11 117.6(4) . . ?
C4 C12 C11 120.2(4) . . ?
C14 C13 H13A 109.5 . . ?
C14 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C14 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
O1 C14 C15 124.4(4) . . ?
O1 C14 C13 116.3(4) . . ?
C15 C14 C13 119.2(4) . . ?
C16 C15 C14 125.0(4) . . ?
C16 C15 H15 117.5 . . ?
C14 C15 H15 117.5 . . ?
O2 C16 C15 124.8(4) . . ?
O2 C16 C17 114.4(4) . . ?
C15 C16 C17 120.7(4) . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C19 C18 H18A 109.5 . . ?
C19 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C19 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
O3 C19 C20 124.5(5) . . ?
O3 C19 C18 115.6(5) . . ?
C20 C19 C18 119.9(5) . . ?
C21 C20 C19 124.8(5) . . ?
C21 C20 H20 117.6 . . ?
C19 C20 H20 117.6 . . ?
O4 C21 C20 125.9(5) . . ?
O4 C21 C22 114.8(5) . . ?
C20 C21 C22 119.3(5) . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C24 C23 H23A 109.5 . . ?
C24 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C24 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
O5 C24 C25 123.0(5) . . ?
O5 C24 C23 116.4(5) . . ?
C25 C24 C23 120.6(5) . . ?
C26 C25 C24 125.7(4) . . ?
C26 C25 H25 117.1 . . ?
C24 C25 H25 117.1 . . ?
O6 C26 C25 124.7(5) . . ?
O6 C26 C27 116.0(5) . . ?
C25 C26 C27 119.3(5) . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Dy1 O2 2.309(3) . ?
Dy1 O3 2.318(3) . ?
Dy1 O1 2.321(3) . ?
Dy1 O6 2.324(3) . ?
Dy1 O5 2.331(3) . ?
Dy1 O4 2.335(3) . ?
Dy1 N1 2.558(3) . ?
Dy1 N2 2.589(3) . ?
O1 C14 1.252(5) . ?
O2 C16 1.271(5) . ?
O3 C19 1.268(5) . ?
O4 C21 1.257(6) . ?
O5 C24 1.267(5) . ?
O6 C26 1.271(5) . ?
N1 C1 1.317(5) . ?
N1 C12 1.358(5) . ?
N2 C10 1.334(5) . ?
N2 C11 1.348(5) . ?
C1 C2 1.399(6) . ?
C1 H1 0.9300 . ?
C2 C3 1.338(7) . ?
C2 H2 0.9300 . ?
C3 C4 1.393(6) . ?
C3 H3 0.9300 . ?
C4 C12 1.407(6) . ?
C4 C5 1.433(7) . ?
C5 C6 1.336(7) . ?
C5 H5 0.9300 . ?
C6 C7 1.437(8) . ?
C6 H6 0.9300 . ?
C7 C8 1.400(7) . ?
C7 C11 1.409(6) . ?
C8 C9 1.338(8) . ?
C8 H8 0.9300 . ?
C9 C10 1.401(7) . ?
C9 H9 0.9300 . ?
C10 H10 0.9300 . ?
C11 C12 1.445(5) . ?
C13 C14 1.507(6) . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 C15 1.386(6) . ?
C15 C16 1.373(6) . ?
C15 H15 0.9300 . ?
C16 C17 1.521(6) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 C19 1.522(7) . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 C20 1.380(7) . ?
C20 C21 1.382(7) . ?
C20 H20 0.9300 . ?
C21 C22 1.551(8) . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C23 C24 1.498(7) . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C24 C25 1.398(8) . ?
C25 C26 1.365(7) . ?
C25 H25 0.9300 . ?
C26 C27 1.508(7) . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
