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#$Date: 2025-08-20 22:19:29 +0300 (Wed, 20 Aug 2025) $
#$Revision: 301836 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/30/51/4305137.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_4305137
loop_
_publ_author_name
'Yunjun Wu'
'Shaowu Wang'
'Xiancui Zhu'
'Gaosheng Yang'
'Yun Wei'
'Lijun Zhang'
'Hai-bin Song'
_publ_section_title
;
Synthesis, Characterization, and Catalytic Activity of Rare Earth Metal
Amides Supported by a Diamido Ligand with a CH2SiMe2 Link
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5503
_journal_page_last               5511
_journal_paper_doi               10.1021/ic800496d
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C25 H23 N3 O4'
_chemical_formula_weight         429.46
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                91.117(2)
_cell_angle_beta                 115.099(2)
_cell_angle_gamma                119.092(2)
_cell_formula_units_Z            2
_cell_length_a                   11.2432(17)
_cell_length_b                   11.3103(17)
_cell_length_c                   11.493(3)
_cell_measurement_temperature    293(2)
_cell_volume                     1108.5(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 0.944
_diffrn_measured_fraction_theta_max 0.944
_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  0.0399
_diffrn_reflns_av_sigmaI/netI    0.0778
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8412
_diffrn_reflns_theta_full        27.61
_diffrn_reflns_theta_max         27.61
_diffrn_reflns_theta_min         2.04
_exptl_absorpt_coefficient_mu    0.089
_exptl_crystal_density_diffrn    1.287
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             452
_refine_diff_density_max         0.438
_refine_diff_density_min         -0.486
_refine_diff_density_rms         0.086
_refine_ls_extinction_coef       0.006(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         4852
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.1914
_refine_ls_R_factor_gt           0.0690
_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)+(0.2000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2273
_refine_ls_wR_factor_ref         0.3311
_reflns_number_gt                2487
_reflns_number_total             4852
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic800496d-file002_6.cif
_cod_data_source_block           1
_cod_database_code               4305137
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
N3 N 0.9038(3) 0.8528(3) 0.2908(2) 0.0486(7) Uani 1 1 d . . .
N1 N 0.7309(3) 0.9228(3) 0.2647(2) 0.0484(7) Uani 1 1 d . . .
N2 N 0.9687(3) 1.0795(3) 0.2727(2) 0.0520(7) Uani 1 1 d . . .
O1 O 0.7920(3) 1.1388(3) 0.2353(2) 0.0649(7) Uani 1 1 d . . .
O3 O 0.6681(3) 0.7010(3) 0.2754(2) 0.0616(7) Uani 1 1 d . . .
O2 O 1.1323(3) 1.0074(3) 0.2971(3) 0.0735(8) Uani 1 1 d . . .
C1 C 0.8257(3) 1.0519(3) 0.2544(3) 0.0471(7) Uani 1 1 d . . .
C3 C 0.7593(3) 0.8148(3) 0.2760(2) 0.0482(8) Uani 1 1 d . . .
C2 C 1.0105(4) 0.9805(4) 0.2873(3) 0.0510(8) Uani 1 1 d . . .
C15 C 1.0795(3) 1.2177(3) 0.2744(3) 0.0486(8) Uani 1 1 d . . .
C4 C 0.5806(3) 0.8870(3) 0.2482(3) 0.0503(8) Uani 1 1 d . . .
C16 C 0.9371(3) 0.7428(3) 0.2973(3) 0.0459(7) Uani 1 1 d . . .
C10 C 1.0689(4) 1.2488(4) 0.1587(3) 0.0663(10) Uani 1 1 d . . .
H10 H 0.9899 1.1805 0.0769 0.080 Uiso 1 1 calc R . .
C14 C 1.1966(4) 1.3194(4) 0.3964(3) 0.0636(10) Uani 1 1 d . . .
H14 H 1.2036 1.2987 0.4761 0.076 Uiso 1 1 calc R . .
C21 C 0.8667(4) 0.6422(4) 0.1816(3) 0.0614(9) Uani 1 1 d . . .
H21 H 0.7991 0.6442 0.1004 0.074 Uiso 1 1 calc R . .
C5 C 0.4571(4) 0.8453(4) 0.1210(3) 0.0662(11) Uani 1 1 d . . .
H5 H 0.4705 0.8417 0.0468 0.079 Uiso 1 1 calc R . .
C17 C 1.0390(4) 0.7436(4) 0.4162(3) 0.0626(10) Uani 1 1 d . . .
H17 H 1.0879 0.8135 0.4943 0.075 Uiso 1 1 calc R . .
C9 C 0.5648(4) 0.8950(4) 0.3593(3) 0.0617(9) Uani 1 1 d . . .
H9 H 0.6490 0.9239 0.4447 0.074 Uiso 1 1 calc R . .
C18 C 1.0688(5) 0.6370(6) 0.4188(4) 0.0799(12) Uani 1 1 d . . .
H18 H 1.1381 0.6358 0.4994 0.096 Uiso 1 1 calc R . .
C19 C 0.9973(5) 0.5356(5) 0.3046(5) 0.0804(12) Uani 1 1 d . . .
H19 H 1.0171 0.4645 0.3074 0.096 Uiso 1 1 calc R . .
C6 C 0.3151(5) 0.8092(5) 0.1050(5) 0.0845(14) Uani 1 1 d . . .
H6 H 0.2310 0.7797 0.0194 0.101 Uiso 1 1 calc R . .
C20 C 0.8971(5) 0.5370(5) 0.1865(5) 0.0802(13) Uani 1 1 d . . .
H20 H 0.8486 0.4672 0.1084 0.096 Uiso 1 1 calc R . .
C13 C 1.3018(4) 1.4507(4) 0.3982(4) 0.0783(13) Uani 1 1 d . . .
H13 H 1.3806 1.5191 0.4800 0.094 Uiso 1 1 calc R . .
C7 C 0.2956(5) 0.8161(5) 0.2142(5) 0.0833(14) Uani 1 1 d . . .
H7 H 0.1987 0.7919 0.2024 0.100 Uiso 1 1 calc R . .
C8 C 0.4193(5) 0.8589(5) 0.3413(5) 0.0808(13) Uani 1 1 d . . .
H8 H 0.4057 0.8636 0.4152 0.097 Uiso 1 1 calc R . .
C12 C 1.2934(5) 1.4830(4) 0.2830(5) 0.0811(13) Uani 1 1 d . . .
H12 H 1.3664 1.5722 0.2857 0.097 Uiso 1 1 calc R . .
C11 C 1.1753(6) 1.3820(6) 0.1619(4) 0.0839(12) Uani 1 1 d . . .
H11 H 1.1673 1.4035 0.0823 0.101 Uiso 1 1 calc R . .
C24 C 0.4788(5) 0.3507(5) 0.0999(4) 0.0793(12) Uani 1 1 d . . .
H24A H 0.4597 0.4235 0.1131 0.095 Uiso 1 1 calc R . .
H24B H 0.5402 0.3781 0.0549 0.095 Uiso 1 1 calc R . .
C22 C 0.4466(7) 0.2141(7) 0.2431(5) 0.120(2) Uani 1 1 d . . .
H22A H 0.4138 0.2442 0.2969 0.144 Uiso 1 1 calc R . .
H22B H 0.4860 0.1579 0.2855 0.144 Uiso 1 1 calc R . .
C25 C 0.3132(6) 0.1310(5) 0.1048(5) 0.0922(15) Uani 1 1 d . . .
H25A H 0.3110 0.0489 0.0745 0.111 Uiso 1 1 calc R . .
H25B H 0.2146 0.0992 0.1020 0.111 Uiso 1 1 calc R . .
C23 C 0.5636(7) 0.3326(7) 0.2303(4) 0.115(2) Uani 1 1 d . . .
H23A H 0.6406 0.3155 0.2312 0.138 Uiso 1 1 calc R . .
H23B H 0.6166 0.4159 0.3028 0.138 Uiso 1 1 calc R . .
O4 O 0.3361(4) 0.2205(3) 0.0228(2) 0.0864(10) 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'
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
C2 N3 C3 125.4(3) . . ?
C2 N3 C16 117.4(3) . . ?
C3 N3 C16 116.9(3) . . ?
C1 N1 C3 125.0(3) . . ?
C1 N1 C4 118.5(3) . . ?
C3 N1 C4 116.1(3) . . ?
C1 N2 C2 124.1(3) . . ?
C1 N2 C15 118.2(3) . . ?
C2 N2 C15 117.7(3) . . ?
O1 C1 N1 123.2(3) . . ?
O1 C1 N2 121.4(3) . . ?
N1 C1 N2 115.4(3) . . ?
O3 C3 N3 123.1(3) . . ?
O3 C3 N1 122.5(3) . . ?
N3 C3 N1 114.4(3) . . ?
O2 C2 N3 123.2(3) . . ?
O2 C2 N2 121.6(3) . . ?
N3 C2 N2 115.3(3) . . ?
C10 C15 C14 120.1(4) . . ?
C10 C15 N2 120.7(3) . . ?
C14 C15 N2 119.1(3) . . ?
C9 C4 C5 121.5(3) . . ?
C9 C4 N1 119.3(3) . . ?
C5 C4 N1 119.3(3) . . ?
C17 C16 C21 121.3(3) . . ?
C17 C16 N3 120.0(2) . . ?
C21 C16 N3 118.7(3) . . ?
C15 C10 C11 120.0(3) . . ?
C13 C14 C15 119.2(4) . . ?
C16 C21 C20 119.2(3) . . ?
C6 C5 C4 119.4(4) . . ?
C16 C17 C18 118.6(3) . . ?
C4 C9 C8 118.4(3) . . ?
C19 C18 C17 120.4(4) . . ?
C18 C19 C20 120.3(4) . . ?
C5 C6 C7 120.5(4) . . ?
C19 C20 C21 120.2(3) . . ?
C12 C13 C14 121.2(3) . . ?
C6 C7 C8 120.1(4) . . ?
C7 C8 C9 120.1(4) . . ?
C13 C12 C11 119.2(4) . . ?
C12 C11 C10 120.1(4) . . ?
O4 C24 C23 107.2(4) . . ?
C23 C22 C25 106.2(5) . . ?
O4 C25 C22 106.9(4) . . ?
C22 C23 C24 105.2(4) . . ?
C25 O4 C24 109.2(3) . . ?
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
N3 C2 1.373(5) . ?
N3 C3 1.392(4) . ?
N3 C16 1.458(4) . ?
N1 C1 1.372(4) . ?
N1 C3 1.399(4) . ?
N1 C4 1.454(4) . ?
N2 C1 1.396(4) . ?
N2 C2 1.399(4) . ?
N2 C15 1.443(4) . ?
O1 C1 1.207(4) . ?
O3 C3 1.191(4) . ?
O2 C2 1.201(4) . ?
C15 C10 1.353(5) . ?
C15 C14 1.386(4) . ?
C4 C9 1.369(5) . ?
C4 C5 1.379(4) . ?
C16 C17 1.357(4) . ?
C16 C21 1.364(4) . ?
C10 C11 1.382(7) . ?
C14 C13 1.369(6) . ?
C21 C20 1.384(5) . ?
C5 C6 1.366(6) . ?
C17 C18 1.396(6) . ?
C9 C8 1.395(5) . ?
C18 C19 1.354(7) . ?
C19 C20 1.355(6) . ?
C6 C7 1.368(8) . ?
C13 C12 1.357(7) . ?
C7 C8 1.377(7) . ?
C12 C11 1.379(7) . ?
C24 O4 1.405(5) . ?
C24 C23 1.479(6) . ?
C22 C23 1.416(8) . ?
C22 C25 1.486(6) . ?
C25 O4 1.404(7) . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 30660799
2 PubChem 139127989
