#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:24:52 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179109 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/71/4307183.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_4307183
loop_
_publ_author_name
'Jie Zhang'
'Ruifang Cai'
'Zhenxia Chen'
'Xigeng Zhou'
_publ_section_title
;
Facile Construction of Lanthanide Metallomacrocycles with the Bridging
Imidazolate and Triazolate Ligands and Their Ring Expansions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              321
_journal_page_last               327
_journal_paper_doi               10.1021/ic061722f
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C60 H54 Dy3 N9 O3'
_chemical_formula_weight         1436.62
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           148
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   30.575(6)
_cell_length_b                   30.575(6)
_cell_length_c                   13.945(4)
_cell_measurement_reflns_used    966
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20.633
_cell_measurement_theta_min      2.307
_cell_volume                     11290(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0457
_diffrn_reflns_av_sigmaI/netI    0.0450
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            15913
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.65
_diffrn_standards_decay_%        5.50
_exptl_absorpt_coefficient_mu    2.987
_exptl_absorpt_correction_T_max  0.7544
_exptl_absorpt_correction_T_min  0.5865
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_density_diffrn    1.268
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4194
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.523
_refine_diff_density_min         -0.625
_refine_diff_density_rms         0.257
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     185
_refine_ls_number_reflns         4430
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.118
_refine_ls_R_factor_all          0.1266
_refine_ls_R_factor_gt           0.0769
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1669P)²+37.5750P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2403
_refine_ls_wR_factor_ref         0.2903
_reflns_number_gt                2618
_reflns_number_total             4430
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic061722fsi20060911_110728.cif
_cod_data_source_block           f41206a
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Rhombohedral' changed to 'rhombohedral'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        11290(4)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4307183
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
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 0.07447(3) 0.89203(2) 0.24646(6) 0.0855(4) Uani 1 1 d . . .
N1 N 0.1199(5) 0.9839(5) 0.2338(11) 0.102(4) Uani 1 1 d . . .
N2 N -0.0762(4) 0.8600(4) 0.2361(11) 0.100(4) Uani 1 1 d . . .
C1 C 0.0634(4) 0.8622(5) 0.4166(6) 0.25(3) Uani 1 1 d G . .
H1A H 0.0307 0.8397 0.4469 0.305 Uiso 1 1 calc R . .
C2 C 0.0894(5) 0.9102(5) 0.4302(7) 0.31(4) Uani 1 1 d G . .
H2A H 0.0785 0.9301 0.4678 0.377 Uiso 1 1 calc R . .
C3 C 0.1347(5) 0.9255(6) 0.4016(7) 0.32(5) Uani 1 1 d G . .
H3A H 0.1637 0.9595 0.4101 0.382 Uiso 1 1 calc R . .
C4 C 0.1367(4) 0.8869(6) 0.3702(9) 0.26(3) Uani 1 1 d G . .
H4A H 0.1676 0.8864 0.3540 0.307 Uiso 1 1 calc R . .
C5 C 0.0926(4) 0.8479(5) 0.3795(8) 0.31(4) Uani 1 1 d G . .
H5A H 0.0853 0.8128 0.3771 0.375 Uiso 1 1 calc R . .
C6 C 0.0538(4) 0.8530(5) 0.0700(6) 0.192(15) Uani 1 1 d G . .
H6A H 0.0219 0.8413 0.0356 0.231 Uiso 1 1 calc R . .
C7 C 0.0962(5) 0.9030(6) 0.0676(6) 0.28(3) Uani 1 1 d G . .
H7A H 0.0990 0.9306 0.0274 0.333 Uiso 1 1 calc R . .
C8 C 0.1373(4) 0.9024(6) 0.1149(8) 0.24(2) Uani 1 1 d G . .
H8A H 0.1727 0.9295 0.1121 0.288 Uiso 1 1 calc R . .
C9 C 0.1203(4) 0.8520(6) 0.1465(10) 0.27(2) Uani 1 1 d G . .
H9A H 0.1417 0.8396 0.1734 0.327 Uiso 1 1 calc R . .
C10 C 0.0687(4) 0.8215(5) 0.1188(8) 0.198(15) Uani 1 1 d G . .
H10A H 0.0482 0.7847 0.1263 0.238 Uiso 1 1 calc R . .
C11 C -0.0513(3) 0.7789(3) 0.2544(5) 0.080(4) Uani 1 1 d G . .
C12 C -0.0658(3) 0.7479(3) 0.1769(6) 0.122(6) Uani 1 1 d G . .
H12A H -0.0524 0.7608 0.1168 0.146 Uiso 1 1 calc R . .
C13 C -0.0999(3) 0.6979(3) 0.1873(9) 0.184(13) Uani 1 1 d G . .
H13A H -0.1098 0.6767 0.1342 0.220 Uiso 1 1 calc R . .
C14 C -0.1195(4) 0.6791(4) 0.2751(9) 0.163(11) Uani 1 1 d G . .
H14A H -0.1428 0.6449 0.2822 0.196 Uiso 1 1 calc R . .
C15 C -0.1050(4) 0.7102(4) 0.3526(8) 0.223(17) Uani 1 1 d G . .
H15A H -0.1184 0.6973 0.4127 0.267 Uiso 1 1 calc R . .
C16 C -0.0709(3) 0.7601(3) 0.3422(6) 0.154(10) Uani 1 1 d G . .
H16A H -0.0609 0.7814 0.3953 0.184 Uiso 1 1 calc R . .
N3 N -0.0161(4) 0.8314(4) 0.2479(10) 0.089(3) Uani 1 1 d . . .
C17 C -0.0255(5) 0.8679(5) 0.2423(11) 0.084(4) Uani 1 1 d . . .
O1 O 0.0089(3) 0.9134(3) 0.2395(8) 0.089(3) Uani 1 1 d . . .
C18 C -0.1231(9) 0.8172(7) 0.215(3) 0.195(14) Uani 1 1 d . . .
H18A H -0.1278 0.7860 0.1959 0.234 Uiso 1 1 calc R . .
C19 C 0.1043(5) 1.0164(5) 0.2397(9) 0.072(3) Uani 1 1 d . . .
H19A H 0.0704 1.0067 0.2460 0.086 Uiso 1 1 calc R . .
C20 C 0.1723(8) 1.0142(8) 0.225(3) 0.202(15) Uani 1 1 d . . .
H20A H 0.1954 1.0029 0.2267 0.242 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'
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'
Dy Dy -0.1892 4.4098 '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
O1 Dy1 N1 75.9(4) . . ?
O1 Dy1 N3 54.7(3) . . ?
N1 Dy1 N3 130.6(4) . . ?
O1 Dy1 C1 99.1(4) . . ?
N1 Dy1 C1 112.6(5) . . ?
N3 Dy1 C1 79.6(4) . . ?
O1 Dy1 C5 127.9(4) . . ?
N1 Dy1 C5 121.4(4) . . ?
N3 Dy1 C5 93.3(4) . . ?
C1 Dy1 C5 29.69(9) . . ?
O1 Dy1 C8 128.0(5) . . ?
N1 Dy1 C8 81.1(5) . . ?
N3 Dy1 C8 126.6(4) . . ?
C1 Dy1 C8 132.9(4) . . ?
C5 Dy1 C8 104.0(4) . . ?
O1 Dy1 C7 97.0(5) . . ?
N1 Dy1 C7 79.5(5) . . ?
N3 Dy1 C7 103.3(4) . . ?
C1 Dy1 C7 161.9(5) . . ?
C5 Dy1 C7 132.6(5) . . ?
C8 Dy1 C7 32.39(9) . . ?
O1 Dy1 C2 93.6(4) . . ?
N1 Dy1 C2 83.6(5) . . ?
N3 Dy1 C2 99.4(4) . . ?
C1 Dy1 C2 29.01(7) . . ?
C5 Dy1 C2 47.82(12) . . ?
C8 Dy1 C2 129.5(3) . . ?
C7 Dy1 C2 157.1(4) . . ?
O1 Dy1 C4 140.3(4) . . ?
N1 Dy1 C4 95.9(4) . . ?
N3 Dy1 C4 121.9(4) . . ?
C1 Dy1 C4 47.72(14) . . ?
C5 Dy1 C4 28.82(10) . . ?
C8 Dy1 C4 87.5(3) . . ?
C7 Dy1 C4 119.9(4) . . ?
C2 Dy1 C4 46.74(12) . . ?
O1 Dy1 C6 92.4(4) . . ?
N1 Dy1 C6 108.6(5) . . ?
N3 Dy1 C6 75.1(4) . . ?
C1 Dy1 C6 138.8(5) . . ?
C5 Dy1 C6 120.4(5) . . ?
C8 Dy1 C6 52.39(15) . . ?
C7 Dy1 C6 31.61(9) . . ?
C2 Dy1 C6 167.4(5) . . ?
C4 Dy1 C6 126.5(4) . . ?
O1 Dy1 C9 143.6(4) . . ?
N1 Dy1 C9 111.3(5) . . ?
N3 Dy1 C9 108.2(4) . . ?
C1 Dy1 C9 109.6(4) . . ?
C5 Dy1 C9 80.3(3) . . ?
C8 Dy1 C9 31.61(11) . . ?
C7 Dy1 C9 52.39(16) . . ?
C2 Dy1 C9 122.2(4) . . ?
C4 Dy1 C9 75.7(3) . . ?
C6 Dy1 C9 51.29(17) . . ?
O1 Dy1 C3 115.8(4) . . ?
N1 Dy1 C3 74.5(5) . . ?
N3 Dy1 C3 125.6(4) . . ?
C1 Dy1 C3 47.05(12) . . ?
C5 Dy1 C3 46.97(13) . . ?
C8 Dy1 C3 101.5(3) . . ?
C7 Dy1 C3 130.5(3) . . ?
C2 Dy1 C3 28.01(7) . . ?
C4 Dy1 C3 27.94(8) . . ?
C6 Dy1 C3 151.1(4) . . ?
C9 Dy1 C3 100.2(3) . . ?
C19 N1 C20 103.5(13) . . ?
C19 N1 Dy1 131.3(10) . . ?
C20 N1 Dy1 125.0(11) . . ?
C19 N2 C18 101.8(14) 3_465 . ?
C19 N2 C17 125.2(12) 3_465 . ?
C18 N2 C17 132.6(15) . . ?
C5 C1 C2 108.0 . . ?
C5 C1 Dy1 75.6(3) . . ?
C2 C1 Dy1 80.3(3) . . ?
C3 C2 C1 108.0 . . ?
C3 C2 Dy1 79.31(19) . . ?
C1 C2 Dy1 70.7(2) . . ?
C2 C3 C4 108.0 . . ?
C2 C3 Dy1 72.69(17) . . ?
C4 C3 Dy1 73.5(3) . . ?
C5 C4 C3 108.0 . . ?
C5 C4 Dy1 70.5(2) . . ?
C3 C4 Dy1 78.6(2) . . ?
C1 C5 C4 108.0 . . ?
C1 C5 Dy1 74.7(2) . . ?
C4 C5 Dy1 80.6(2) . . ?
C10 C6 C7 108.0 . . ?
C10 C6 Dy1 77.2(3) . . ?
C7 C6 Dy1 70.0(2) . . ?
C8 C7 C6 108.0 . . ?
C8 C7 Dy1 73.8(2) . . ?
C6 C7 Dy1 78.4(2) . . ?
C7 C8 C9 108.0 . . ?
C7 C8 Dy1 73.80(19) . . ?
C9 C8 Dy1 78.4(3) . . ?
C10 C9 C8 108.0 . . ?
C10 C9 Dy1 77.23(18) . . ?
C8 C9 Dy1 70.0(2) . . ?
C9 C10 C6 108.0 . . ?
C9 C10 Dy1 72.16(18) . . ?
C6 C10 Dy1 72.15(19) . . ?
C12 C11 C16 120.0 . . ?
C12 C11 N3 122.6(6) . . ?
C16 C11 N3 117.4(6) . . ?
C11 C12 C13 120.0 . . ?
C14 C13 C12 120.0 . . ?
C15 C14 C13 120.0 . . ?
C16 C15 C14 120.0 . . ?
C15 C16 C11 120.0 . . ?
C17 N3 C11 127.7(11) . . ?
C17 N3 Dy1 90.1(9) . . ?
C11 N3 Dy1 142.1(7) . . ?
O1 C17 N3 122.3(13) . . ?
O1 C17 N2 114.7(12) . . ?
N3 C17 N2 123.0(13) . . ?
O1 C17 Dy1 60.2(7) . . ?
N3 C17 Dy1 62.1(7) . . ?
N2 C17 Dy1 174.5(10) . . ?
C17 O1 Dy1 92.8(8) . . ?
C20 C18 N2 109.6(19) 3_465 . ?
N1 C19 N2 115.1(12) . 2_675 ?
C18 C20 N1 108.4(18) 2_675 . ?
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 O1 2.402(9) . ?
Dy1 N1 2.438(12) . ?
Dy1 N3 2.444(12) . ?
Dy1 C1 2.503(7) . ?
Dy1 C5 2.514(8) . ?
Dy1 C8 2.559(9) . ?
Dy1 C7 2.559(9) . ?
Dy1 C2 2.613(10) . ?
Dy1 C4 2.631(9) . ?
Dy1 C6 2.669(7) . ?
Dy1 C9 2.669(10) . ?
Dy1 C3 2.690(11) . ?
N1 C19 1.302(16) . ?
N1 C20 1.40(2) . ?
N2 C19 1.308(16) 3_465 ?
N2 C18 1.41(2) . ?
N2 C17 1.445(17) . ?
C1 C5 1.285(3) . ?
C1 C2 1.286(3) . ?
C2 C3 1.285(3) . ?
C3 C4 1.286(3) . ?
C4 C5 1.286(3) . ?
C6 C10 1.428(3) . ?
C6 C7 1.428(3) . ?
C7 C8 1.428(3) . ?
C8 C9 1.428(3) . ?
C9 C10 1.428(3) . ?
C11 C12 1.359(3) . ?
C11 C16 1.359(3) . ?
C11 N3 1.419(13) . ?
C12 C13 1.359(3) . ?
C13 C14 1.359(3) . ?
C14 C15 1.358(3) . ?
C15 C16 1.358(3) . ?
N3 C17 1.288(17) . ?
C17 O1 1.256(15) . ?
C18 C20 1.27(3) 3_465 ?
C19 N2 1.308(16) 2_675 ?
C20 C18 1.27(3) 2_675 ?
