#------------------------------------------------------------------------------
#$Date: 2020-10-06 09:10:49 +0300 (Tue, 06 Oct 2020) $
#$Revision: 257243 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/12/71/7127170.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_7127170
loop_
_publ_author_name
'Prodius, Denis'
'Klocke, Matthew'
'Smetana, Volodymyr'
'Alammar, Tarek'
'Perez Garcia, Marilu'
'Windus, Theresa L.'
'Nlebedim, Ikenna C.'
'Mudring, Anja-Verena'
_publ_section_title
;
 Rationally designed rare earth separation by selective oxalate
 solubilization.
;
_journal_issue                   77
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              11386
_journal_page_last               11389
_journal_paper_doi               10.1039/d0cc02270e
_journal_volume                  56
_journal_year                    2020
_chemical_formula_sum            'C24 H28 Lu N8 O18'
_chemical_formula_weight         891.51
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2019-02-19 deposited with the CCDC.	2020-08-18 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 98.384(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.038(5)
_cell_length_b                   17.562(5)
_cell_length_c                   18.345(7)
_cell_measurement_reflns_used    62090
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      32.02
_cell_measurement_theta_min      4.41
_cell_volume                     3837(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.98
_diffrn_measured_fraction_theta_max 0.98
_diffrn_measurement_device_type  'Bruker CCD'
_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  0.0315
_diffrn_reflns_av_sigmaI/netI    0.0258
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            62090
_diffrn_reflns_theta_full        32.02
_diffrn_reflns_theta_max         32.02
_diffrn_reflns_theta_min         4.41
_exptl_absorpt_coefficient_mu    2.652
_exptl_absorpt_correction_T_max  0.18
_exptl_absorpt_correction_T_min  0.11
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_density_diffrn    1.543
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular fragment'
_exptl_crystal_F_000             1772
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.280
_refine_diff_density_min         -0.603
_refine_diff_density_rms         0.151
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     460
_refine_ls_number_reflns         12745
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0520
_refine_ls_R_factor_gt           0.0415
_refine_ls_shift/su_max          0.017
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0786P)²+5.1309P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1176
_refine_ls_wR_factor_ref         0.1255
_reflns_number_gt                10730
_reflns_number_total             12745
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d0cc02270e2.cif
_cod_data_source_block           22_in_cc
_cod_depositor_comments
'Adding full bibliography for 7127165--7127177.cif.'
_cod_original_cell_volume        3837(3)
_cod_original_sg_symbol_H-M      Cc
_cod_database_code               7127170
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x, -y, z+1/2'
'x+1/2, y+1/2, 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
Lu1 Lu 0.16457(10) 0.124668(8) 0.37264(7) 0.03479(6) Uani 1 1 d . . .
O1 O 0.2338(7) 0.2325(4) 0.3236(5) 0.059(2) Uani 1 1 d . . .
O2 O 0.2420(6) 0.0195(4) 0.4384(4) 0.0564(17) Uani 1 1 d . . .
O3 O 0.0870(5) 0.0191(3) 0.3097(3) 0.0426(13) Uani 1 1 d . . .
O4 O 0.0911(5) 0.2297(3) 0.4256(4) 0.0415(13) Uani 1 1 d . . .
O5 O 0.0202(5) 0.0968(3) 0.4466(3) 0.0459(14) Uani 1 1 d . . .
O6 O 0.4448(12) 0.1266(5) 0.2412(7) 0.062(3) Uani 1 1 d . . .
O7 O 0.2984(5) 0.0868(3) 0.3067(3) 0.0448(14) Uani 1 1 d . . .
O8 O -0.1141(12) 0.1381(6) 0.4949(8) 0.072(3) Uani 1 1 d . . .
O9 O 0.3104(7) 0.1590(4) 0.4584(5) 0.0604(19) Uani 1 1 d . . .
O10 O 0.0194(7) 0.1589(3) 0.2813(4) 0.0543(16) Uani 1 1 d . . .
O11 O -0.0471(6) 0.2803(4) 0.4796(4) 0.0598(18) Uani 1 1 d . . .
C1 C 0.3595(7) 0.1467(5) 0.2772(4) 0.0323(15) Uani 1 1 d . . .
C2 C 0.3320(10) 0.0275(6) 0.4734(7) 0.066(3) Uani 1 1 d . . .
O12 O 0.3668(9) 0.2803(4) 0.2703(6) 0.082(3) Uani 1 1 d . . .
C3 C -0.0387(13) 0.1399(9) 0.4672(9) 0.065(4) Uani 1 1 d . . .
O13 O 0.4020(7) -0.0284(5) 0.5053(6) 0.078(2) Uani 1 1 d . . .
C4 C -0.0005(9) 0.2295(6) 0.4581(6) 0.053(2) Uani 1 1 d . . .
C5 C 0.3187(8) 0.2240(4) 0.2902(4) 0.0355(16) Uani 1 1 d . . .
C6 C -0.0327(9) 0.1116(7) 0.2438(6) 0.052(2) Uani 1 1 d . . .
C7 C -0.0062(8) 0.0249(4) 0.2637(5) 0.0458(19) Uani 1 1 d . . .
O14 O -0.0514(7) -0.0251(4) 0.2309(5) 0.079(3) Uani 1 1 d . . .
C8 C 0.3880(8) 0.1079(6) 0.4824(6) 0.0471(19) Uani 1 1 d . . .
O15 O 0.4859(7) 0.1178(4) 0.5086(6) 0.083(3) Uani 1 1 d . . .
O16 O -0.1031(13) 0.1247(4) 0.1912(8) 0.131(6) Uani 1 1 d . . .
N1 N 0.2860(10) 0.2388(6) 0.0617(6) 0.065(2) Uani 1 1 d . . .
H1 H 0.3320 0.2643 0.0395 0.200 Uiso 1 1 calc . . .
C9 C 0.1652(8) 0.1950(7) 0.1300(5) 0.066(2) Uani 1 1 d D . .
H9 H 0.1130 0.1923 0.1626 0.200 Uiso 1 1 calc . . .
C10 C 0.2745(9) 0.1620(6) 0.0612(4) 0.066(2) Uani 1 1 d . . .
H10 H 0.3123 0.1290 0.0337 0.200 Uiso 1 1 calc . . .
C11 C 0.2082(13) 0.2696(7) 0.1055(8) 0.093(4) Uani 1 1 d D . .
H11 H 0.1900 0.3196 0.1155 0.200 Uiso 1 1 calc . . .
C12 C 0.1736(12) 0.0584(8) 0.1189(7) 0.094(3) Uani 1 1 d . . .
H12A H 0.2202 0.0255 0.0945 0.200 Uiso 1 1 calc . . .
H12B H 0.0961 0.0492 0.1001 0.200 Uiso 1 1 calc . . .
H12C H 0.1864 0.0484 0.1709 0.200 Uiso 1 1 calc . . .
N2 N 0.2021(9) 0.1401(8) 0.1052(7) 0.109(5) Uani 1 1 d D . .
N3 N 0.3416(6) 0.0625(3) 0.7950(4) 0.0648(19) Uani 1 1 d . . .
H3 H 0.3445 0.0136 0.7934 0.200 Uiso 1 1 calc . . .
C13 C 0.2779(10) 0.1098(5) 0.8307(5) 0.069(2) Uani 1 1 d . . .
H13 H 0.2260 0.0931 0.8600 0.200 Uiso 1 1 calc . . .
C14 C 0.2417(11) 0.2499(6) 0.8472(6) 0.081(3) Uani 1 1 d . . .
H14A H 0.2730 0.2955 0.8296 0.200 Uiso 1 1 calc . . .
H14B H 0.2537 0.2498 0.9001 0.200 Uiso 1 1 calc . . .
H14C H 0.1626 0.2482 0.8298 0.200 Uiso 1 1 calc . . .
N4 N 0.2982(6) 0.1808(3) 0.8190(3) 0.0560(14) Uani 1 1 d . . .
C15 C 0.3812(9) 0.1778(7) 0.7774(7) 0.095(4) Uani 1 1 d D . .
H15 H 0.4200 0.2190 0.7618 0.200 Uiso 1 1 calc . . .
C16 C 0.3956(6) 0.1130(4) 0.7644(4) 0.0540(16) Uani 1 1 d D . .
H16 H 0.4454 0.0990 0.7325 0.200 Uiso 1 1 calc . . .
N5 N 0.1477(16) 0.3803(4) 0.3728(15) 0.129(8) Uani 1 1 d . . .
H5 H 0.1414 0.3317 0.3677 0.200 Uiso 1 1 calc . . .
N6 N 0.1892(6) 0.4906(4) 0.3482(4) 0.0497(14) Uani 1 1 d . . .
C17 C 0.0895(14) 0.4201(10) 0.4233(16) 0.152(10) Uani 1 1 d . . .
H17 H 0.0495 0.4034 0.4600 0.200 Uiso 1 1 calc . . .
C18 C 0.1153(13) 0.4987(9) 0.3968(10) 0.099(5) Uani 1 1 d . . .
H18 H 0.0859 0.5444 0.4112 0.200 Uiso 1 1 calc . . .
C19 C 0.2215(11) 0.5697(6) 0.3170(8) 0.095(3) Uani 1 1 d . . .
H19A H 0.1871 0.6098 0.3413 0.200 Uiso 1 1 calc . . .
H19B H 0.1956 0.5718 0.2650 0.200 Uiso 1 1 calc . . .
H19C H 0.3016 0.5758 0.3256 0.200 Uiso 1 1 calc . . .
C20 C 0.2145(10) 0.4218(8) 0.3322(5) 0.080(4) Uani 1 1 d . . .
H20 H 0.2644 0.4048 0.3016 0.200 Uiso 1 1 calc . . .
C21 C 0.0413(8) 0.2234(7) 0.6815(5) 0.055(2) Uani 1 1 d . . .
H21 H -0.0141 0.2256 0.7118 0.200 Uiso 1 1 calc . . .
C22 C 0.0882(12) 0.2788(9) 0.6567(6) 0.096(5) Uani 1 1 d . . .
H22 H 0.0738 0.3298 0.6651 0.200 Uiso 1 1 calc . . .
N7 N 0.0867(11) 0.1576(6) 0.6556(5) 0.092(4) Uani 1 1 d . . .
H7 H 0.0581 0.1129 0.6579 0.200 Uiso 1 1 calc . . .
C23 C 0.1763(19) 0.1717(12) 0.6279(15) 0.257(19) Uani 1 1 d D . .
H23 H 0.2334 0.1390 0.6186 0.400 Uiso 1 1 calc . . .
N8 N 0.1639(6) 0.2519(4) 0.6151(4) 0.0553(15) Uani 1 1 d D . .
C24 C 0.2371(9) 0.3031(9) 0.5722(6) 0.092(3) Uani 1 1 d . . .
H24A H 0.2836 0.2717 0.5462 0.200 Uiso 1 1 calc . . .
H24B H 0.2838 0.3353 0.6062 0.200 Uiso 1 1 calc . . .
H24C H 0.1894 0.3340 0.5376 0.200 Uiso 1 1 calc . . .
O1W O 0.5798(6) 0.0340(4) 0.1095(5) 0.0849(19) Uani 1 1 d . . .
O2W O 0.3000(7) 0.5181(6) 0.5918(5) 0.110(3) 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'
Lu Lu -0.4720 5.8584 '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
O9 Lu1 O7 84.7(3) . . ?
O9 Lu1 O3 141.1(2) . . ?
O7 Lu1 O3 76.3(2) . . ?
O9 Lu1 O1 76.4(3) . . ?
O7 Lu1 O1 72.8(2) . . ?
O3 Lu1 O1 127.4(3) . . ?
O9 Lu1 O4 78.6(2) . . ?
O7 Lu1 O4 143.72(19) . . ?
O3 Lu1 O4 134.2(2) . . ?
O1 Lu1 O4 72.04(14) . . ?
O9 Lu1 O10 149.44(14) . . ?
O7 Lu1 O10 102.2(3) . . ?
O3 Lu1 O10 68.8(2) . . ?
O1 Lu1 O10 77.4(3) . . ?
O4 Lu1 O10 78.6(2) . . ?
O9 Lu1 O2 68.8(2) . . ?
O7 Lu1 O2 77.3(2) . . ?
O3 Lu1 O2 73.98(12) . . ?
O1 Lu1 O2 135.6(3) . . ?
O4 Lu1 O2 124.3(3) . . ?
O10 Lu1 O2 141.6(2) . . ?
O9 Lu1 O5 102.3(3) . . ?
O7 Lu1 O5 151.08(15) . . ?
O3 Lu1 O5 81.1(2) . . ?
O1 Lu1 O5 136.0(2) . . ?
O4 Lu1 O5 64.84(19) . . ?
O10 Lu1 O5 86.0(3) . . ?
O2 Lu1 O5 79.3(2) . . ?
C5 O1 Lu1 116.9(5) . . ?
C2 O2 Lu1 116.9(7) . . ?
C7 O3 Lu1 120.5(5) . . ?
C4 O4 Lu1 125.3(5) . . ?
C3 O5 Lu1 126.0(8) . . ?
C1 O7 Lu1 115.7(5) . . ?
C8 O9 Lu1 119.3(6) . . ?
C6 O10 Lu1 120.8(6) . . ?
O6 C1 O7 117.6(8) . . ?
O6 C1 C5 128.0(6) . . ?
O7 C1 C5 114.4(6) . . ?
O2 C2 O13 127.2(10) . . ?
O2 C2 C8 120.7(9) . . ?
O13 C2 C8 112.0(10) . . ?
O8 C3 O5 136.7(15) . . ?
O8 C3 C4 109.5(14) . . ?
O5 C3 C4 113.7(12) . . ?
O11 C4 O4 128.9(10) . . ?
O11 C4 C3 123.0(10) . . ?
O4 C4 C3 108.1(9) . . ?
O12 C5 O1 119.6(8) . . ?
O12 C5 C1 120.7(7) . . ?
O1 C5 C1 119.7(6) . . ?
O10 C6 O16 125.0(11) . . ?
O10 C6 C7 117.6(9) . . ?
O16 C6 C7 117.4(10) . . ?
O14 C7 O3 124.9(7) . . ?
O14 C7 C6 123.1(8) . . ?
O3 C7 C6 110.3(7) . . ?
O15 C8 O9 129.1(10) . . ?
O15 C8 C2 123.2(9) . . ?
O9 C8 C2 107.7(9) . . ?
C10 N1 C11 107.8(9) . . ?
N2 C9 C11 115.5(8) . . ?
N2 C10 N1 111.1(11) . . ?
N1 C11 C9 97.0(8) . . ?
C9 N2 C10 108.4(11) . . ?
C9 N2 C12 127.3(9) . . ?
C10 N2 C12 124.3(13) . . ?
C16 N3 C13 98.4(7) . . ?
N4 C13 N3 112.0(9) . . ?
N4 C13 C16 72.8(6) . . ?
N3 C13 C16 39.2(4) . . ?
C13 N4 C15 103.2(8) . . ?
C13 N4 C14 127.5(8) . . ?
C15 N4 C14 129.3(8) . . ?
C16 C15 N4 107.3(8) . . ?
C15 C16 N3 118.7(9) . . ?
C15 C16 C13 76.4(6) . . ?
N3 C16 C13 42.4(5) . . ?
C20 N5 C17 118.1(9) . . ?
C20 N6 C18 116.5(11) . . ?
C20 N6 C19 131.8(10) . . ?
C18 N6 C19 111.5(11) . . ?
N5 C17 C18 95.5(16) . . ?
N6 C18 C17 107.5(14) . . ?
N6 C20 N5 101.4(12) . . ?
C22 C21 N7 107.7(11) . . ?
C21 C22 N8 108.1(14) . . ?
C23 N7 C21 111.7(12) . . ?
N7 C23 N8 100.4(11) . . ?
C22 N8 C23 108.3(11) . . ?
C22 N8 C24 124.2(9) . . ?
C23 N8 C24 126.8(11) . . ?
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
Lu1 O9 2.262(8) . ?
Lu1 O7 2.251(5) . ?
Lu1 O3 2.308(6) . ?
Lu1 O1 2.305(6) . ?
Lu1 O4 2.319(6) . ?
Lu1 O10 2.317(8) . ?
Lu1 O2 2.325(6) . ?
Lu1 O5 2.407(6) . ?
O1 C5 1.274(10) . ?
O2 C2 1.185(14) . ?
O3 C7 1.306(10) . ?
O4 C4 1.327(11) . ?
O5 C3 1.139(18) . ?
O6 C1 1.347(14) . ?
O7 C1 1.433(8) . ?
O8 C3 1.10(2) . ?
O9 C8 1.322(14) . ?
O10 C6 1.196(15) . ?
O11 C4 1.153(11) . ?
C1 C5 1.474(12) . ?
C2 O13 1.369(12) . ?
C2 C8 1.564(15) . ?
O12 C5 1.228(10) . ?
C3 C4 1.655(17) . ?
C6 O16 1.210(14) . ?
C6 C7 1.587(13) . ?
C7 O14 1.155(10) . ?
C8 O15 1.219(12) . ?
N1 C10 1.354(13) . ?
N1 C11 1.427(14) . ?
C9 N2 1.180(14) . ?
C9 C11 1.501(14) . ?
C10 N2 1.329(13) . ?
C12 N2 1.506(18) . ?
N3 C16 1.277(9) . ?
N3 C13 1.361(14) . ?
C13 N4 1.295(9) . ?
C13 C16 1.998(14) . ?
C14 N4 1.519(12) . ?
N4 C15 1.343(12) . ?
C15 C16 1.181(12) . ?
N5 C20 1.38(3) . ?
N5 C17 1.42(4) . ?
N6 C20 1.290(13) . ?
N6 C18 1.357(14) . ?
N6 C19 1.572(12) . ?
C17 C18 1.51(2) . ?
C21 C22 1.244(15) . ?
C21 N7 1.391(16) . ?
C22 N8 1.355(16) . ?
N7 C23 1.28(2) . ?
C23 N8 1.432(19) . ?
N8 C24 1.552(14) . ?
