#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:18:24 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179240 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/60/4316043.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_4316043
loop_
_publ_author_name
'George S. Goff'
'Michael R. Cisneros'
'Chandra Kluk'
'Kevin Williamson'
'Brian Scott'
'Sean Reilly'
'Wolfgang Runde'
_publ_section_title
;
 Synthesis and Structural Characterization of Molecular Dy(III) and
 Er(III) Tetra-Carbonates
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6558
_journal_page_last               6564
_journal_paper_doi               10.1021/ic1004598
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'C9 H52 Er N15 O23'
_chemical_formula_weight         905.92
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 94.3980(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.8160(6)
_cell_length_b                   21.0121(14)
_cell_length_c                   19.6496(14)
_cell_measurement_temperature    293(2)
_cell_volume                     3629.2(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.993
_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  0.0665
_diffrn_reflns_av_sigmaI/netI    0.0547
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            39384
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.13
_diffrn_reflns_theta_min         1.94
_exptl_absorpt_coefficient_mu    2.411
_exptl_crystal_density_diffrn    1.658
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1852
_refine_diff_density_max         1.745
_refine_diff_density_min         -0.974
_refine_diff_density_rms         0.157
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.950
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         7979
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.950
_refine_ls_R_factor_all          0.0784
_refine_ls_R_factor_gt           0.0605
_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)+(0.0218P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1176
_refine_ls_wR_factor_ref         0.1203
_reflns_number_gt                6513
_reflns_number_total             7979
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic1004598_si_001_2.cif
_cod_data_source_block           apx502
_cod_database_code               4316043
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -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
Er1 Er 0.24703(3) 0.237777(14) 0.672717(14) 0.01405(9) Uani 1 1 d . . .
O1 O 0.1184(5) 0.1685(2) 0.5941(2) 0.0149(10) Uani 1 1 d . . .
O2 O 0.2334(5) 0.1301(2) 0.5042(2) 0.0178(10) Uani 1 1 d . . .
O3 O 0.3660(5) 0.1820(2) 0.5892(2) 0.0184(10) Uani 1 1 d . . .
O4 O 0.3629(5) 0.1626(2) 0.7479(2) 0.0179(10) Uani 1 1 d . . .
O5 O 0.2374(5) 0.1210(2) 0.8330(2) 0.0214(11) Uani 1 1 d . . .
O6 O 0.1229(5) 0.1867(2) 0.7561(2) 0.0180(10) Uani 1 1 d . . .
O7 O 0.4900(5) 0.2833(2) 0.6835(2) 0.0184(10) Uani 1 1 d . . .
O8 O 0.5641(5) 0.3487(2) 0.7697(2) 0.0235(11) Uani 1 1 d . . .
O9 O 0.3230(5) 0.3142(2) 0.7543(2) 0.0181(10) Uani 1 1 d . . .
O10 O 0.1773(5) 0.3168(2) 0.5937(2) 0.0153(10) Uani 1 1 d . . .
O11 O -0.0632(5) 0.3529(2) 0.5768(2) 0.0194(10) Uani 1 1 d . . .
O12 O 0.0070(5) 0.2876(2) 0.6641(2) 0.0170(10) Uani 1 1 d . . .
N1 N 0.7335(6) 0.1972(3) 0.9514(3) 0.0195(13) Uani 1 1 d . . .
H1A H 0.7264 0.1943 0.9947 0.023 Uiso 1 1 calc R . .
H1B H 0.8151 0.2119 0.9360 0.023 Uiso 1 1 calc R . .
N2 N 0.4921(6) 0.1560(2) 0.9315(3) 0.0176(13) Uani 1 1 d . . .
H2A H 0.4182 0.1439 0.9034 0.021 Uiso 1 1 calc R . .
H2B H 0.4841 0.1533 0.9748 0.021 Uiso 1 1 calc R . .
N3 N 0.6290(6) 0.1827(3) 0.8416(3) 0.0206(13) Uani 1 1 d . . .
H3A H 0.5546 0.1706 0.8138 0.025 Uiso 1 1 calc R . .
H3B H 0.7106 0.1975 0.8261 0.025 Uiso 1 1 calc R . .
N4 N 0.9115(7) 0.0524(3) 0.8468(3) 0.0302(15) Uani 1 1 d . . .
H4A H 0.8366 0.0297 0.8299 0.036 Uiso 1 1 calc R . .
H4B H 0.9732 0.0695 0.8203 0.036 Uiso 1 1 calc R . .
N5 N 0.8386(6) 0.0349(3) 0.9543(3) 0.0246(14) Uani 1 1 d . . .
H5A H 0.7634 0.0123 0.9377 0.029 Uiso 1 1 calc R . .
H5B H 0.8525 0.0406 0.9977 0.029 Uiso 1 1 calc R . .
N6 N 1.0485(6) 0.0952(3) 0.9381(3) 0.0231(14) Uani 1 1 d . . .
H6A H 1.1094 0.1116 0.9108 0.028 Uiso 1 1 calc R . .
H6B H 1.0637 0.1012 0.9813 0.028 Uiso 1 1 calc R . .
N7 N 0.7455(7) 0.1986(2) 0.6691(3) 0.0211(12) Uani 1 1 d . . .
H7A H 0.8268 0.2198 0.6630 0.025 Uiso 1 1 calc R . .
H7B H 0.6597 0.2180 0.6699 0.025 Uiso 1 1 calc R . .
N8 N 0.8802(6) 0.1053(3) 0.6761(3) 0.0294(15) Uani 1 1 d . . .
H8A H 0.9629 0.1257 0.6701 0.035 Uiso 1 1 calc R . .
H8B H 0.8822 0.0647 0.6814 0.035 Uiso 1 1 calc R . .
N9 N 0.6241(6) 0.1036(3) 0.6853(3) 0.0216(13) Uani 1 1 d . . .
H9A H 0.6269 0.0629 0.6898 0.026 Uiso 1 1 calc R . .
H9B H 0.5389 0.1235 0.6860 0.026 Uiso 1 1 calc R . .
N10 N -0.0109(6) 0.1721(3) 0.4114(3) 0.0215(14) Uani 1 1 d . . .
H10A H -0.0041 0.1709 0.3680 0.026 Uiso 1 1 calc R . .
H10B H 0.0643 0.1598 0.4387 0.026 Uiso 1 1 calc R . .
N11 N -0.2522(6) 0.2118(3) 0.3945(3) 0.0193(13) Uani 1 1 d . . .
H11A H -0.3343 0.2253 0.4106 0.023 Uiso 1 1 calc R . .
H11B H -0.2453 0.2106 0.3511 0.023 Uiso 1 1 calc R . .
N12 N -0.1487(7) 0.1950(3) 0.5024(3) 0.0255(14) Uani 1 1 d . . .
H12A H -0.2310 0.2086 0.5183 0.031 Uiso 1 1 calc R . .
H12B H -0.0738 0.1828 0.5299 0.031 Uiso 1 1 calc R . .
N13 N 0.3158(7) -0.0486(3) 0.5777(3) 0.0304(15) Uani 1 1 d . . .
H13A H 0.3139 -0.0487 0.6214 0.036 Uiso 1 1 calc R . .
H13B H 0.2445 -0.0300 0.5528 0.036 Uiso 1 1 calc R . .
N14 N 0.4309(6) -0.0758(3) 0.4811(3) 0.0242(14) Uani 1 1 d . . .
H14A H 0.5048 -0.0938 0.4624 0.029 Uiso 1 1 calc R . .
H14B H 0.3598 -0.0572 0.4561 0.029 Uiso 1 1 calc R . .
N15 N 0.5362(7) -0.1053(3) 0.5866(3) 0.0302(15) Uani 1 1 d . . .
H15A H 0.5354 -0.1057 0.6303 0.036 Uiso 1 1 calc R . .
H15B H 0.6088 -0.1236 0.5673 0.036 Uiso 1 1 calc R . .
C1 C 0.2382(7) 0.1592(3) 0.5611(3) 0.0170(15) Uani 1 1 d . . .
C2 C 0.2398(8) 0.1560(3) 0.7804(3) 0.0162(15) Uani 1 1 d . . .
C3 C 0.4625(8) 0.3167(3) 0.7364(3) 0.0199(16) Uani 1 1 d . . .
C4 C 0.0352(8) 0.3198(3) 0.6107(3) 0.0172(15) Uani 1 1 d . . .
C5 C 0.6180(7) 0.1788(3) 0.9083(3) 0.0151(14) Uani 1 1 d . . .
C6 C 0.9319(7) 0.0608(3) 0.9136(3) 0.0169(15) Uani 1 1 d . . .
C7 C 0.7523(8) 0.1361(3) 0.6771(3) 0.0156(14) Uani 1 1 d . . .
C8 C -0.1374(8) 0.1930(3) 0.4362(3) 0.0175(15) Uani 1 1 d . . .
C9 C 0.4265(9) -0.0766(3) 0.5492(4) 0.0244(17) Uani 1 1 d . . .
O1W O -0.0775(5) 0.2401(2) 0.8372(2) 0.0224(10) Uani 1 1 d . . .
O2W O 0.5511(5) 0.2483(2) 0.5079(2) 0.0248(12) Uani 1 1 d . . .
O3W O 0.8623(5) 0.3569(2) 0.7630(2) 0.0238(11) Uani 1 1 d . . .
O4W O -0.3670(6) 0.3586(2) 0.5829(3) 0.0372(14) Uani 1 1 d . . .
O5W O 0.3568(5) 0.4252(2) 0.5974(2) 0.0242(11) Uani 1 1 d . . .
O6W O -0.0435(5) 0.4790(2) 0.5609(3) 0.0279(12) Uani 1 1 d . . .
O7W O 0.2182(7) 0.4321(3) 0.7840(3) 0.0523(18) Uani 1 1 d . . .
O8W O 0.6484(6) -0.0105(2) 0.7695(3) 0.0415(15) Uani 1 1 d . . .
O9W O 0.3485(7) 0.0041(2) 0.8293(3) 0.0448(16) Uani 1 1 d . . .
O10W O 0.1304(7) 0.0151(3) 0.4668(3) 0.0552(18) Uani 1 1 d . . .
O11W O 0.5600(9) 0.4717(3) 0.8256(3) 0.074(2) Uani 1 1 d . . .
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'
Er Er -0.2586 4.9576 '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
O6 Er1 O10 133.82(15) . . ?
O6 Er1 O3 122.01(15) . . ?
O10 Er1 O3 89.97(15) . . ?
O6 Er1 O7 127.39(15) . . ?
O10 Er1 O7 87.82(15) . . ?
O3 Er1 O7 79.10(15) . . ?
O6 Er1 O9 87.67(15) . . ?
O10 Er1 O9 90.81(15) . . ?
O3 Er1 O9 135.22(15) . . ?
O7 Er1 O9 56.20(15) . . ?
O6 Er1 O1 86.96(15) . . ?
O10 Er1 O1 85.07(15) . . ?
O3 Er1 O1 56.38(15) . . ?
O7 Er1 O1 134.81(14) . . ?
O9 Er1 O1 167.84(15) . . ?
O6 Er1 O4 56.30(15) . . ?
O10 Er1 O4 169.52(15) . . ?
O3 Er1 O4 84.66(15) . . ?
O7 Er1 O4 82.34(15) . . ?
O9 Er1 O4 86.71(15) . . ?
O1 Er1 O4 99.32(15) . . ?
O6 Er1 O12 77.59(15) . . ?
O10 Er1 O12 56.24(14) . . ?
O3 Er1 O12 128.58(15) . . ?
O7 Er1 O12 129.49(15) . . ?
O9 Er1 O12 87.25(15) . . ?
O1 Er1 O12 80.94(15) . . ?
O4 Er1 O12 133.68(15) . . ?
O6 Er1 C1 107.57(18) . . ?
O10 Er1 C1 84.64(17) . . ?
O3 Er1 C1 28.42(17) . . ?
O7 Er1 C1 106.75(17) . . ?
O9 Er1 C1 162.60(18) . . ?
O1 Er1 C1 28.17(16) . . ?
O4 Er1 C1 94.72(17) . . ?
O12 Er1 C1 103.90(17) . . ?
O6 Er1 C2 27.77(17) . . ?
O10 Er1 C2 161.23(18) . . ?
O3 Er1 C2 105.53(18) . . ?
O7 Er1 C2 105.20(17) . . ?
O9 Er1 C2 85.58(17) . . ?
O1 Er1 C2 94.65(17) . . ?
O4 Er1 C2 28.59(17) . . ?
O12 Er1 C2 105.13(17) . . ?
C1 Er1 C2 103.88(18) . . ?
O6 Er1 C3 107.86(17) . . ?
O10 Er1 C3 90.64(17) . . ?
O3 Er1 C3 106.94(18) . . ?
O7 Er1 C3 27.98(16) . . ?
O9 Er1 C3 28.28(17) . . ?
O1 Er1 C3 162.66(18) . . ?
O4 Er1 C3 82.36(18) . . ?
O12 Er1 C3 110.50(18) . . ?
C1 Er1 C3 134.7(2) . . ?
C2 Er1 C3 94.75(19) . . ?
O6 Er1 C4 105.25(18) . . ?
O10 Er1 C4 28.61(17) . . ?
O3 Er1 C4 109.24(17) . . ?
O7 Er1 C4 111.68(17) . . ?
O9 Er1 C4 91.29(17) . . ?
O1 Er1 C4 79.62(17) . . ?
O4 Er1 C4 161.49(18) . . ?
O12 Er1 C4 27.82(16) . . ?
C1 Er1 C4 92.65(19) . . ?
C2 Er1 C4 132.9(2) . . ?
C3 Er1 C4 104.22(18) . . ?
C1 O1 Er1 93.0(4) . . ?
C1 O3 Er1 93.6(4) . . ?
C2 O4 Er1 92.3(4) . . ?
C2 O6 Er1 95.0(4) . . ?
C3 O7 Er1 93.9(4) . . ?
C3 O9 Er1 93.9(4) . . ?
C4 O10 Er1 94.1(4) . . ?
C4 O12 Er1 93.6(4) . . ?
O2 C1 O1 122.6(6) . . ?
O2 C1 O3 121.1(6) . . ?
O1 C1 O3 116.2(6) . . ?
O2 C1 Er1 171.7(5) . . ?
O1 C1 Er1 58.8(3) . . ?
O3 C1 Er1 58.0(3) . . ?
O5 C2 O6 122.2(6) . . ?
O5 C2 O4 121.6(6) . . ?
O6 C2 O4 116.2(6) . . ?
O5 C2 Er1 176.4(5) . . ?
O6 C2 Er1 57.2(3) . . ?
O4 C2 Er1 59.1(3) . . ?
O8 C3 O7 122.4(6) . . ?
O8 C3 O9 121.8(6) . . ?
O7 C3 O9 115.8(6) . . ?
O8 C3 Er1 174.6(5) . . ?
O7 C3 Er1 58.2(3) . . ?
O9 C3 Er1 57.8(3) . . ?
O11 C4 O12 123.5(6) . . ?
O11 C4 O10 121.2(6) . . ?
O12 C4 O10 115.3(6) . . ?
O11 C4 Er1 173.5(5) . . ?
O12 C4 Er1 58.6(3) . . ?
O10 C4 Er1 57.3(3) . . ?
N2 C5 N3 119.5(6) . . ?
N2 C5 N1 120.4(6) . . ?
N3 C5 N1 120.1(6) . . ?
N4 C6 N5 120.5(6) . . ?
N4 C6 N6 118.6(6) . . ?
N5 C6 N6 121.0(6) . . ?
N8 C7 N7 121.5(6) . . ?
N8 C7 N9 119.3(6) . . ?
N7 C7 N9 119.2(6) . . ?
N11 C8 N12 119.7(6) . . ?
N11 C8 N10 120.0(6) . . ?
N12 C8 N10 120.3(6) . . ?
N15 C9 N13 120.7(7) . . ?
N15 C9 N14 119.1(7) . . ?
N13 C9 N14 120.2(7) . . ?
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
Er1 O6 2.304(4) . ?
Er1 O10 2.324(4) . ?
Er1 O3 2.330(4) . ?
Er1 O7 2.341(4) . ?
Er1 O9 2.332(4) . ?
Er1 O1 2.349(4) . ?
Er1 O4 2.344(4) . ?
Er1 O12 2.355(4) . ?
Er1 C1 2.742(7) . ?
Er1 C2 2.729(7) . ?
Er1 C3 2.749(7) . ?
Er1 C4 2.755(7) . ?
O1 C1 1.296(8) . ?
O2 C1 1.272(8) . ?
O3 C1 1.307(7) . ?
O4 C2 1.307(7) . ?
O5 C2 1.270(7) . ?
O6 C2 1.276(8) . ?
O7 C3 1.293(7) . ?
O8 C3 1.262(8) . ?
O9 C3 1.306(8) . ?
O10 C4 1.323(8) . ?
O11 C4 1.262(8) . ?
O12 C4 1.288(7) . ?
N1 C5 1.331(8) . ?
N2 C5 1.322(8) . ?
N3 C5 1.323(8) . ?
N4 C6 1.323(8) . ?
N5 C6 1.309(8) . ?
N6 C6 1.317(8) . ?
N7 C7 1.324(8) . ?
N8 C7 1.301(8) . ?
N9 C7 1.341(8) . ?
N10 C8 1.326(8) . ?
N11 C8 1.313(8) . ?
N12 C8 1.312(8) . ?
N13 C9 1.303(9) . ?
N14 C9 1.343(8) . ?
N15 C9 1.314(9) . ?
