#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:23:56 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179375 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/72/4327236.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_4327236
loop_
_publ_author_name
'Jeff Vipond'
'Mark Woods'
'Piyu Zhao'
'Gyula Tircsó'
'Jimin Ren'
'Simon G. Bott'
'Doug Ogrin'
'Garry E. Kiefer'
'Zoltan Kovacs'
'A. Dean Sherry'
_publ_section_title
;
 A Bridge to Coordination Isomer Selection in Lanthanide(III)
 DOTA-tetraamide Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2584
_journal_page_last               2595
_journal_paper_doi               10.1021/ic062184+
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C22 H46 N11 O17 Yb'
_chemical_formula_weight         909.74
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           152
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'P 31 2"'
_symmetry_space_group_name_H-M   'P 31 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   10.7750(15)
_cell_length_b                   10.7750(15)
_cell_length_c                   27.882(6)
_cell_measurement_temperature    293(2)
_cell_volume                     2803.4(8)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_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  0.0376
_diffrn_reflns_av_sigmaI/netI    0.0276
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            26222
_diffrn_reflns_theta_max         27.97
_diffrn_reflns_theta_min         2.18
_exptl_absorpt_coefficient_mu    2.584
_exptl_crystal_density_diffrn    1.617
_exptl_crystal_F_000             1383
_refine_diff_density_max         0.726
_refine_diff_density_min         -0.379
_refine_diff_density_rms         0.091
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.033(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.125
_refine_ls_goodness_of_fit_obs   1.101
_refine_ls_matrix_type           full
_refine_ls_number_parameters     232
_refine_ls_number_reflns         4092
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.125
_refine_ls_restrained_S_obs      1.101
_refine_ls_R_factor_all          0.0263
_refine_ls_R_factor_obs          0.0235
_refine_ls_shift/esd_max         -0.016
_refine_ls_shift/esd_mean        0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0273P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0519
_refine_ls_wR_factor_obs         0.0496
_reflns_number_observed          3915
_reflns_number_total             4092
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic0621842Bsi20070202_110554.cif
_cod_data_source_block           sgb
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0273P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0273P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4327236
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z+1/3'
'-x+y, -x, z+2/3'
'y, x, -z'
'x-y, -y, -z+2/3'
'-x, -x+y, -z+1/3'
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
Yb Yb -0.23382(2) 0.0000 -0.1667 0.02966(5) Uani 1 d S
N1 N -0.0271(3) 0.1557(3) -0.11217(11) 0.0406(7) Uani 1 d .
C2 C -0.0208(5) 0.0638(4) -0.07224(13) 0.0474(9) Uani 1 d .
H2A H -0.0951(5) 0.0442(4) -0.04943(13) 0.057 Uiso 1 d R
H2B H 0.0696(5) 0.1150(4) -0.05592(13) 0.057 Uiso 1 d R
C3 C -0.0406(4) -0.0775(5) -0.0909(2) 0.0509(10) Uani 1 d .
H3A H -0.0364(4) -0.1330(5) -0.0647(2) 0.061 Uiso 1 d R
H3B H 0.0361(4) -0.0586(5) -0.1126(2) 0.061 Uiso 1 d R
N4 N -0.1818(3) -0.1633(3) -0.11596(10) 0.0402(6) Uani 1 d .
C5 C -0.1854(5) -0.2818(4) -0.14594(13) 0.0509(9) Uani 1 d .
H5A H -0.2836(5) -0.3547(4) -0.15033(13) 0.061 Uiso 1 d R
H5B H -0.1376(5) -0.3237(4) -0.12912(13) 0.061 Uiso 1 d R
C6 C -0.1176(5) -0.2302(5) -0.19481(13) 0.0503(9) Uani 1 d .
H6A H -0.1284(5) -0.3099(5) -0.21343(13) 0.060 Uiso 1 d R
H6B H -0.0170(5) -0.1647(5) -0.19062(13) 0.060 Uiso 1 d R
C8 C -0.0656(4) 0.2611(4) -0.09115(13) 0.0471(9) Uani 1 d .
H8A H -0.0360(4) 0.3411(4) -0.11239(13) 0.057 Uiso 1 d R
H8B H -0.0173(4) 0.2962(4) -0.06104(13) 0.057 Uiso 1 d R
O9 O -0.3060(3) 0.0581(3) -0.09840(8) 0.0421(5) Uani 1 d .
C9 C -0.2286(5) 0.1853(4) -0.08342(12) 0.0434(8) Uani 1 d .
N10 N -0.2847(4) 0.2545(4) -0.06116(11) 0.0570(9) Uani 1 d .
H10A H -0.2275(4) 0.3471(4) -0.05326(11) 0.068 Uiso 1 d R
C11 C -0.4373(6) 0.1857(6) -0.04976(12) 0.0665(11) Uani 1 d .
H11A H -0.4478(6) 0.2152(6) -0.01826(12) 0.080 Uiso 1 d R
H11B H -0.4752(6) 0.0840(6) -0.04891(12) 0.080 Uiso 1 d R
C12 C -0.5268(6) 0.2180(7) -0.08515(15) 0.0703(14) Uani 1 d .
H12A H -0.4873(6) 0.3200(7) -0.08650(15) 0.084 Uiso 1 d R
H12B H -0.6225(6) 0.1770(7) -0.07284(15) 0.084 Uiso 1 d R
O13 O -0.5315(4) 0.1669(4) -0.13352(10) 0.0665(9) Uani 1 d .
C14 C -0.6154(5) 0.0147(6) -0.13992(14) 0.0600(11) Uani 1 d .
H14A H -0.7087(5) -0.0231(6) -0.12579(14) 0.072 Uiso 1 d R
H14B H -0.5683(5) -0.0314(6) -0.12536(14) 0.072 Uiso 1 d R
C41 C -0.3014(5) -0.2298(5) -0.08028(12) 0.0477(9) Uani 1 d .
H41A H -0.2863(5) -0.1638(5) -0.05481(12) 0.057 Uiso 1 d R
H41B H -0.3043(5) -0.3130(5) -0.06663(12) 0.057 Uiso 1 d R
O42 O -0.4379(3) -0.2088(3) -0.14537(8) 0.0435(6) Uani 1 d .
N42 N -0.5626(5) -0.3721(4) -0.08717(11) 0.0657(9) Uani 1 d .
H42A H -0.6565(5) -0.4108(4) -0.10859(11) 0.079 Uiso 1 d R
H42B H -0.5777(5) -0.3881(4) -0.05576(11) 0.079 Uiso 1 d R
C42 C -0.4417(4) -0.2728(4) -0.10627(13) 0.0443(8) Uani 1 d .
N100 N -0.3392(5) 0.0400(7) -0.3650(2) 0.090(2) Uani 1 d .
O101 O -0.3052(7) -0.0395(10) -0.3507(2) 0.174(4) Uani 1 d .
O102 O -0.4147(6) 0.0250(6) -0.3992(2) 0.120(2) Uani 1 d .
O103 O -0.2911(10) 0.1569(9) -0.3441(2) 0.213(4) Uani 1 d .
N200 N 0.0000 -0.3661(5) -0.3333 0.0440(10) Uani 1 d S
O201 O 0.0000 -0.4818(4) -0.3333 0.080(2) Uani 1 d S
O202 O -0.0903(4) -0.3554(4) -0.30793(12) 0.0694(9) Uani 1 d .
O1S O -0.5832(4) -0.1825(4) -0.46736(13) 0.0835(10) Uani 1 d .
H1S H -0.5234(4) -0.1219(4) -0.44656(13) 0.100 Uiso 1 d R
H2S H -0.5701(4) -0.2623(4) -0.47986(13) 0.100 Uiso 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'
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
O9 Yb O9 122.27(13) 5_554 .
O9 Yb O42 76.14(10) 5_554 5_554
O9 Yb O42 77.83(9) . 5_554
O9 Yb O42 77.83(9) 5_554 .
O9 Yb O42 76.14(10) . .
O42 Yb O42 124.41(13) 5_554 .
O9 Yb N1 67.65(9) 5_554 5_554
O9 Yb N1 155.82(10) . 5_554
O42 Yb N1 126.12(9) 5_554 5_554
O42 Yb N1 85.67(9) . 5_554
O9 Yb N1 155.82(10) 5_554 .
O9 Yb N1 67.65(9) . .
O42 Yb N1 85.67(9) 5_554 .
O42 Yb N1 126.12(9) . .
N1 Yb N1 113.13(14) 5_554 .
O9 Yb N4 87.04(9) 5_554 5_554
O9 Yb N4 126.97(10) . 5_554
O42 Yb N4 67.14(9) 5_554 5_554
O42 Yb N4 156.87(9) . 5_554
N1 Yb N4 72.33(10) 5_554 5_554
N1 Yb N4 71.09(9) . 5_554
O9 Yb N4 126.97(10) 5_554 .
O9 Yb N4 87.04(9) . .
O42 Yb N4 156.87(9) 5_554 .
O42 Yb N4 67.14(9) . .
N1 Yb N4 71.09(10) 5_554 .
N1 Yb N4 72.33(10) . .
N4 Yb N4 110.57(14) 5_554 .
O9 Yb C9 21.89(11) 5_554 5_554
O9 Yb C9 128.98(11) . 5_554
O42 Yb C9 98.03(10) 5_554 5_554
O42 Yb C9 64.63(9) . 5_554
N1 Yb C9 51.90(11) 5_554 5_554
N1 Yb C9 163.36(10) . 5_554
N4 Yb C9 95.29(10) 5_554 5_554
N4 Yb C9 105.09(10) . 5_554
O9 Yb C9 128.98(11) 5_554 .
O9 Yb C9 21.89(11) . .
O42 Yb C9 64.63(9) 5_554 .
O42 Yb C9 98.03(10) . .
N1 Yb C9 163.36(10) 5_554 .
N1 Yb C9 51.90(11) . .
N4 Yb C9 105.09(10) 5_554 .
N4 Yb C9 95.29(10) . .
C9 Yb C9 143.9(2) 5_554 .
O9 Yb C42 67.99(10) 5_554 5_554
O9 Yb C42 97.97(10) . 5_554
O42 Yb C42 20.55(9) 5_554 5_554
O42 Yb C42 135.09(10) . 5_554
N1 Yb C42 106.18(10) 5_554 5_554
N1 Yb C42 89.48(10) . 5_554
N4 Yb C42 49.68(10) 5_554 5_554
N4 Yb C42 157.77(10) . 5_554
C9 Yb C42 88.61(10) 5_554 5_554
C9 Yb C42 82.69(10) . 5_554
O9 Yb C42 97.97(10) 5_554 .
O9 Yb C42 67.99(10) . .
O42 Yb C42 135.09(10) 5_554 .
O42 Yb C42 20.55(9) . .
N1 Yb C42 89.48(10) 5_554 .
N1 Yb C42 106.18(10) . .
N4 Yb C42 157.77(10) 5_554 .
N4 Yb C42 49.68(10) . .
C9 Yb C42 82.69(9) 5_554 .
C9 Yb C42 88.61(10) . .
C42 Yb C42 151.68(15) 5_554 .
C6 N1 C8 111.6(3) 5_554 .
C6 N1 C2 110.4(3) 5_554 .
C8 N1 C2 109.0(3) . .
C6 N1 Yb 112.2(2) 5_554 .
C8 N1 Yb 104.6(2) . .
C2 N1 Yb 108.8(2) . .
N1 C2 C3 111.9(3) . .
N4 C3 C2 111.6(3) . .
C41 N4 C3 110.6(3) . .
C41 N4 C5 108.1(3) . .
C3 N4 C5 111.5(3) . .
C41 N4 Yb 105.5(2) . .
C3 N4 Yb 109.9(2) . .
C5 N4 Yb 111.0(2) . .
N4 C5 C6 112.6(3) . .
N1 C6 C5 111.7(3) 5_554 .
N1 C8 C9 109.0(3) . .
C9 O9 Yb 116.5(2) . .
O9 C9 N10 121.6(4) . .
O9 C9 C8 119.2(3) . .
N10 C9 C8 119.2(3) . .
O9 C9 Yb 41.7(2) . .
N10 C9 Yb 149.6(3) . .
C8 C9 Yb 83.3(2) . .
C9 N10 C11 122.1(4) . .
N10 C11 C12 114.8(4) . .
O13 C12 C11 114.7(4) . .
C14 O13 C12 115.7(4) . .
O13 C14 C14 107.5(5) . 5_554
N4 C41 C42 108.4(3) . .
C42 O42 Yb 120.3(2) . .
O42 C42 N42 122.3(4) . .
O42 C42 C41 118.8(3) . .
N42 C42 C41 118.9(4) . .
O42 C42 Yb 39.2(2) . .
N42 C42 Yb 158.2(3) . .
C41 C42 Yb 80.6(2) . .
O101 N100 O102 127.8(8) . .
O101 N100 O103 117.6(7) . .
O102 N100 O103 114.6(6) . .
O201 N200 O202 118.7(3) . .
O201 N200 O202 118.7(3) . 6_554
O202 N200 O202 122.6(5) . 6_554
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Yb O9 2.260(2) 5_554
Yb O9 2.260(2) .
Yb O42 2.303(2) 5_554
Yb O42 2.303(2) .
Yb N1 2.519(3) 5_554
Yb N1 2.519(3) .
Yb N4 2.529(3) 5_554
Yb N4 2.529(3) .
Yb C9 3.044(4) 5_554
Yb C9 3.044(4) .
Yb C42 3.148(4) 5_554
Yb C42 3.148(4) .
N1 C6 1.497(5) 5_554
N1 C8 1.508(5) .
N1 C2 1.515(5) .
C2 C3 1.520(5) .
C3 N4 1.500(5) .
N4 C41 1.497(5) .
N4 C5 1.510(5) .
C5 C6 1.514(5) .
C6 N1 1.497(5) 5_554
C8 C9 1.538(6) .
O9 C9 1.267(5) .
C9 N10 1.325(5) .
N10 C11 1.461(7) .
C11 C12 1.536(6) .
C12 O13 1.448(5) .
O13 C14 1.434(6) .
C14 C14 1.517(8) 5_554
C41 C42 1.525(6) .
O42 C42 1.279(4) .
N42 C42 1.316(5) .
N100 O101 1.158(7) .
N100 O102 1.211(6) .
N100 O103 1.242(9) .
N200 O201 1.246(7) .
N200 O202 1.255(4) .
N200 O202 1.255(4) 6_554
