#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:24:52 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179109 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/71/4307182.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_4307182
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 N9 O3 Yb3'
_chemical_formula_weight         1468.24
_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                   30.451(5)
_cell_length_b                   30.451(5)
_cell_length_c                   13.919(3)
_cell_measurement_reflns_used    992
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      19.247
_cell_measurement_theta_min      2.513
_cell_volume                     11177(4)
_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      298(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0711
_diffrn_reflns_av_sigmaI/netI    0.0874
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            15667
_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    3.774
_exptl_absorpt_correction_T_max  0.7041
_exptl_absorpt_correction_T_min  0.4522
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.309
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4266
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.402
_refine_diff_density_min         -0.636
_refine_diff_density_rms         0.241
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.970
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     192
_refine_ls_number_reflns         4378
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.970
_refine_ls_R_factor_all          0.1419
_refine_ls_R_factor_gt           0.0633
_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)+(0.1142P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1778
_refine_ls_wR_factor_ref         0.2148
_reflns_number_gt                2035
_reflns_number_total             4378
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic061722fsi20060911_110532.cif
_cod_data_source_block           f40330b
_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        11178(4)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4307182
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
Yb1 Yb 0.18160(2) 0.07367(2) 0.25408(5) 0.0811(3) Uani 1 1 d . . .
O1 O 0.0960(3) 0.0094(3) 0.2604(7) 0.084(3) Uani 1 1 d . . .
N1 N 0.1519(4) -0.0154(4) 0.2508(8) 0.079(3) Uani 1 1 d . . .
N2 N 0.0634(4) -0.0759(4) 0.2641(10) 0.089(4) Uani 1 1 d . . .
C1 C 0.2034(6) 0.0568(5) 0.4256(7) 0.154(10) Uani 1 1 d G . .
H1A H 0.1844 0.0251 0.4618 0.185 Uiso 1 1 calc R . .
C2 C 0.1970(7) 0.0986(6) 0.4324(10) 0.29(3) Uani 1 1 d G . .
H2A H 0.1731 0.1017 0.4752 0.349 Uiso 1 1 calc R . .
C3 C 0.2358(7) 0.1381(6) 0.3816(10) 0.35(4) Uani 1 1 d G . .
H3A H 0.2442 0.1736 0.3836 0.417 Uiso 1 1 calc R . .
C4 C 0.2664(6) 0.1206(5) 0.3434(11) 0.29(3) Uani 1 1 d G . .
H4A H 0.2996 0.1418 0.3134 0.351 Uiso 1 1 calc R . .
C5 C 0.2463(5) 0.0704(4) 0.3706(9) 0.166(10) Uani 1 1 d G . .
H5A H 0.2627 0.0500 0.3617 0.199 Uiso 1 1 calc R . .
C17 C 0.1692(3) -0.0501(3) 0.2417(6) 0.084(4) Uani 1 1 d G . .
C12 C 0.1661(5) -0.0721(4) 0.1513(7) 0.160(10) Uani 1 1 d G . .
H12 H 0.1534 -0.0632 0.0988 0.192 Uiso 1 1 calc R . .
C13 C 0.1823(5) -0.1078(4) 0.1403(9) 0.231(17) Uani 1 1 d G . .
H13 H 0.1803 -0.1223 0.0806 0.277 Uiso 1 1 calc R . .
C14 C 0.2016(4) -0.1213(4) 0.2197(10) 0.160(9) Uani 1 1 d G . .
H14 H 0.2124 -0.1449 0.2125 0.192 Uiso 1 1 calc R . .
C15 C 0.2047(4) -0.0993(4) 0.3101(9) 0.156(10) Uani 1 1 d G . .
H15 H 0.2174 -0.1083 0.3626 0.187 Uiso 1 1 calc R . .
C16 C 0.1885(4) -0.0637(3) 0.3212(6) 0.127(7) Uani 1 1 d G . .
H16 H 0.1905 -0.0491 0.3809 0.152 Uiso 1 1 calc R . .
C11 C 0.1049(5) -0.0261(5) 0.2582(11) 0.076(4) Uani 1 1 d . . .
C18 C 0.0571(9) -0.1259(9) 0.285(2) 0.181(11) Uani 1 1 d . . .
H18 H 0.0834 -0.1318 0.3001 0.217 Uiso 1 1 calc R . .
C6 C 0.2040(14) 0.0581(8) 0.0881(16) 0.26(3) Uani 1 1 d G . .
H6A H 0.2008 0.0261 0.0658 0.312 Uiso 1 1 calc R . .
C7 C 0.1708(8) 0.0720(16) 0.0754(16) 0.38(5) Uani 1 1 d G . .
H7A H 0.1386 0.0523 0.0412 0.450 Uiso 1 1 calc R . .
C8 C 0.1919(17) 0.1197(15) 0.095(2) 0.46(6) Uani 1 1 d G . .
H8A H 0.1777 0.1415 0.0798 0.557 Uiso 1 1 calc R . .
C9 C 0.2382(14) 0.1353(9) 0.119(2) 0.24(2) Uani 1 1 d G . .
H9A H 0.2645 0.1708 0.1285 0.286 Uiso 1 1 calc R . .
C10 C 0.2457(11) 0.0972(15) 0.115(2) 0.34(3) Uani 1 1 d G . .
H10A H 0.2787 0.0992 0.1197 0.410 Uiso 1 1 calc R . .
N3 N -0.0181(4) -0.1376(5) 0.2673(9) 0.092(4) Uani 1 1 d . . .
C20 C 0.0154(5) -0.0866(5) 0.2612(9) 0.068(3) Uani 1 1 d . . .
H20 H 0.0056 -0.0623 0.2557 0.082 Uiso 1 1 calc R . .
C19 C 0.0102(7) -0.1605(7) 0.278(2) 0.170(11) Uani 1 1 d . . .
H19 H -0.0022 -0.1952 0.2804 0.205 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'
Yb Yb -0.3850 5.5486 '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 Yb1 N3 76.7(4) . 2 ?
O1 Yb1 N1 54.9(3) . . ?
N3 Yb1 N1 131.6(4) 2 . ?
O1 Yb1 C7 86.6(7) . . ?
N3 Yb1 C7 89.0(10) 2 . ?
N1 Yb1 C7 89.2(11) . . ?
O1 Yb1 C6 99.8(8) . . ?
N3 Yb1 C6 117.8(9) 2 . ?
N1 Yb1 C6 75.7(6) . . ?
C7 Yb1 C6 29.7(4) . . ?
O1 Yb1 C3 129.6(5) . . ?
N3 Yb1 C3 80.3(5) 2 . ?
N1 Yb1 C3 128.2(4) . . ?
C7 Yb1 C3 137.3(10) . . ?
C6 Yb1 C3 130.6(9) . . ?
O1 Yb1 C8 105.6(12) . . ?
N3 Yb1 C8 72.3(5) 2 . ?
N1 Yb1 C8 118.5(9) . . ?
C7 Yb1 C8 29.4(4) . . ?
C6 Yb1 C8 48.5(6) . . ?
C3 Yb1 C8 109.1(11) . . ?
O1 Yb1 C4 146.6(4) . . ?
N3 Yb1 C4 109.9(5) 2 . ?
N1 Yb1 C4 110.3(4) . . ?
C7 Yb1 C4 125.3(7) . . ?
C6 Yb1 C4 104.9(10) . . ?
C3 Yb1 C4 31.49(12) . . ?
C8 Yb1 C4 107.6(12) . . ?
O1 Yb1 C2 99.9(5) . . ?
N3 Yb1 C2 79.9(5) 2 . ?
N1 Yb1 C2 105.3(4) . . ?
C7 Yb1 C2 165.3(11) . . ?
C6 Yb1 C2 156.2(10) . . ?
C3 Yb1 C2 31.45(10) . . ?
C8 Yb1 C2 136.2(9) . . ?
C4 Yb1 C2 51.86(17) . . ?
O1 Yb1 C10 129.0(9) . . ?
N3 Yb1 C10 117.7(8) 2 . ?
N1 Yb1 C10 96.0(9) . . ?
C7 Yb1 C10 48.4(6) . . ?
C6 Yb1 C10 29.2(4) . . ?
C3 Yb1 C10 101.4(10) . . ?
C8 Yb1 C10 47.9(6) . . ?
C4 Yb1 C10 78.3(9) . . ?
C2 Yb1 C10 129.8(10) . . ?
O1 Yb1 C5 119.5(4) . . ?
N3 Yb1 C5 129.6(4) 2 . ?
N1 Yb1 C5 80.3(3) . . ?
C7 Yb1 C5 135.6(7) . . ?
C6 Yb1 C5 106.5(10) . . ?
C3 Yb1 C5 51.76(19) . . ?
C8 Yb1 C5 132.5(11) . . ?
C4 Yb1 C5 31.20(14) . . ?
C2 Yb1 C5 51.52(19) . . ?
C10 Yb1 C5 89.7(8) . . ?
O1 Yb1 C1 95.1(4) . . ?
N3 Yb1 C1 108.7(4) 2 . ?
N1 Yb1 C1 77.4(4) . . ?
C7 Yb1 C1 162.2(10) . . ?
C6 Yb1 C1 133.3(9) . . ?
C3 Yb1 C1 51.70(18) . . ?
C8 Yb1 C1 158.7(12) . . ?
C4 Yb1 C1 51.54(19) . . ?
C2 Yb1 C1 31.12(13) . . ?
C10 Yb1 C1 120.7(8) . . ?
C5 Yb1 C1 30.99(13) . . ?
C11 O1 Yb1 95.1(8) . . ?
C11 N1 C17 126.6(11) . . ?
C11 N1 Yb1 91.6(8) . . ?
C17 N1 Yb1 141.7(7) . . ?
C20 N2 C11 123.3(12) . . ?
C20 N2 C18 101.2(13) . . ?
C11 N2 C18 135.2(14) . . ?
C2 C1 C5 108.0 . . ?
C2 C1 Yb1 73.3(2) . . ?
C5 C1 Yb1 74.3(4) . . ?
C1 C2 C3 108.0 . . ?
C1 C2 Yb1 75.6(3) . . ?
C3 C2 Yb1 73.4(4) . . ?
C4 C3 C2 108.0 . . ?
C4 C3 Yb1 74.8(4) . . ?
C2 C3 Yb1 75.2(4) . . ?
C3 C4 C5 108.0 . . ?
C3 C4 Yb1 73.7(3) . . ?
C5 C4 Yb1 75.7(3) . . ?
C1 C5 C4 108.0 . . ?
C1 C5 Yb1 74.7(4) . . ?
C4 C5 Yb1 73.1(3) . . ?
N1 C17 C12 118.7(6) . . ?
N1 C17 C16 121.3(6) . . ?
C12 C17 C16 120.0 . . ?
C13 C12 C17 120.0 . . ?
C12 C13 C14 120.0 . . ?
C15 C14 C13 120.0 . . ?
C14 C15 C16 120.0 . . ?
C17 C16 C15 120.0 . . ?
O1 C11 N1 118.4(12) . . ?
O1 C11 N2 117.7(12) . . ?
N1 C11 N2 123.9(13) . . ?
O1 C11 Yb1 58.2(7) . . ?
N1 C11 Yb1 60.2(7) . . ?
N2 C11 Yb1 175.5(10) . . ?
C19 C18 N2 110.7(16) . . ?
C7 C6 C10 108.0 . . ?
C7 C6 Yb1 74.6(9) . . ?
C10 C6 Yb1 78.0(9) . . ?
C8 C7 C6 108.0 . . ?
C8 C7 Yb1 77.5(8) . . ?
C6 C7 Yb1 75.7(9) . . ?
C7 C8 C9 108.0 . . ?
C7 C8 Yb1 73.0(8) . . ?
C9 C8 Yb1 77.5(9) . . ?
C10 C9 C8 108.0 . . ?
C10 C9 Yb1 74.6(8) . . ?
C8 C9 Yb1 73.6(8) . . ?
C9 C10 C6 108.0 . . ?
C9 C10 Yb1 76.6(8) . . ?
C6 C10 Yb1 72.8(8) . . ?
C19 N3 C20 106.6(13) . . ?
C19 N3 Yb1 124.5(12) . 3 ?
C20 N3 Yb1 128.9(10) . 3 ?
N2 C20 N3 112.3(12) . . ?
C18 C19 N3 108.4(17) . . ?
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
Yb1 O1 2.352(8) . ?
Yb1 N3 2.377(12) 2 ?
Yb1 N1 2.393(11) . ?
Yb1 C7 2.51(2) . ?
Yb1 C6 2.519(18) . ?
Yb1 C3 2.547(10) . ?
Yb1 C8 2.56(2) . ?
Yb1 C4 2.562(11) . ?
Yb1 C2 2.569(12) . ?
Yb1 C10 2.579(18) . ?
Yb1 C5 2.593(9) . ?
Yb1 C1 2.598(10) . ?
O1 C11 1.243(14) . ?
N1 C11 1.303(15) . ?
N1 C17 1.400(13) . ?
N2 C20 1.329(15) . ?
N2 C11 1.409(16) . ?
N2 C18 1.46(2) . ?
C1 C2 1.387(3) . ?
C1 C5 1.387(3) . ?
C2 C3 1.387(3) . ?
C3 C4 1.386(3) . ?
C4 C5 1.387(3) . ?
C17 C12 1.407(3) . ?
C17 C16 1.408(3) . ?
C12 C13 1.407(3) . ?
C13 C14 1.407(3) . ?
C14 C15 1.407(3) . ?
C15 C16 1.408(3) . ?
C18 C19 1.28(3) . ?
C6 C7 1.288(17) . ?
C6 C10 1.288(17) . ?
C7 C8 1.288(17) . ?
C8 C9 1.288(17) . ?
C9 C10 1.288(17) . ?
N3 C19 1.36(2) . ?
N3 C20 1.369(16) . ?
N3 Yb1 2.377(11) 3 ?
