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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/4/30/51/4305138.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_4305138
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            'C24 H21 N3 O3'
_chemical_formula_weight         399.44
_space_group_IT_number           7
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P -2yac'
_symmetry_space_group_name_H-M   'P 1 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                 90.0100(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.4057(9)
_cell_length_b                   4.5668(4)
_cell_length_c                   18.9688(14)
_cell_measurement_temperature    293(2)
_cell_volume                     988.04(14)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0199
_diffrn_reflns_av_sigmaI/netI    0.0229
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            8049
_diffrn_reflns_theta_full        27.55
_diffrn_reflns_theta_max         27.55
_diffrn_reflns_theta_min         2.08
_exptl_absorpt_coefficient_mu    0.090
_exptl_crystal_density_diffrn    1.343
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             420
_refine_diff_density_max         0.121
_refine_diff_density_min         -0.101
_refine_diff_density_rms         0.023
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   1.2(8)
_refine_ls_extinction_coef       0.032(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         4114
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0310
_refine_ls_R_factor_gt           0.0287
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0425P)²+0.0688P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0778
_refine_ls_wR_factor_ref         0.0797
_reflns_number_gt                3861
_reflns_number_total             4114
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic800496d-file002_7.cif
_cod_data_source_block           070830a_0m
_cod_database_code               4305138
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x+1/2, -y, 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
N1 N 0.16918(9) 0.2849(2) 0.32383(6) 0.0408(2) Uani 1 1 d . . .
N3 N 0.03520(8) 0.5758(2) 0.26210(5) 0.0396(2) Uani 1 1 d . . .
N2 N 0.03512(8) 0.5759(2) 0.38558(5) 0.0395(2) Uani 1 1 d . . .
O3 O 0.16597(9) 0.2910(3) 0.20430(5) 0.0605(3) Uani 1 1 d . . .
O1 O 0.16596(9) 0.2908(3) 0.44333(5) 0.0604(3) Uani 1 1 d . . .
O2 O -0.09101(10) 0.8621(2) 0.32391(7) 0.0644(3) Uani 1 1 d . . .
C2 C -0.01285(11) 0.6843(3) 0.32390(7) 0.0408(3) Uani 1 1 d . . .
C18 C -0.00996(12) 0.6834(3) 0.45401(7) 0.0460(3) Uani 1 1 d . . .
H18A H -0.0521 0.8652 0.4464 0.055 Uiso 1 1 calc R . .
H18B H 0.0558 0.7251 0.4849 0.055 Uiso 1 1 calc R . .
C11 C -0.01022(12) 0.6833(3) 0.19376(7) 0.0460(3) Uani 1 1 d . . .
H11A H 0.0554 0.7258 0.1629 0.055 Uiso 1 1 calc R . .
H11B H -0.0525 0.8646 0.2015 0.055 Uiso 1 1 calc R . .
C3 C 0.12597(10) 0.3768(3) 0.25945(7) 0.0411(3) Uani 1 1 d . . .
C1 C 0.12592(10) 0.3769(3) 0.38832(7) 0.0410(3) Uani 1 1 d . . .
C5 C 0.38433(10) 0.3078(3) 0.32385(8) 0.0438(3) Uani 1 1 d . . .
C6 C 0.43275(12) 0.4035(4) 0.38686(9) 0.0546(3) Uani 1 1 d . . .
H6 H 0.4013 0.3408 0.4295 0.066 Uiso 1 1 calc R . .
C8 C 0.57564(13) 0.6843(4) 0.32381(11) 0.0648(4) Uani 1 1 d . . .
H8 H 0.6402 0.8087 0.3238 0.078 Uiso 1 1 calc R . .
C9 C 0.52776(13) 0.5918(4) 0.26136(10) 0.0629(4) Uani 1 1 d . . .
H9 H 0.5595 0.6562 0.2189 0.075 Uiso 1 1 calc R . .
C4 C 0.27904(12) 0.1100(3) 0.32375(9) 0.0486(3) Uani 1 1 d . . .
H4A H 0.2810 -0.0143 0.2823 0.058 Uiso 1 1 calc R . .
H4B H 0.2810 -0.0149 0.3651 0.058 Uiso 1 1 calc R . .
C7 C 0.52765(13) 0.5918(4) 0.38637(10) 0.0632(4) Uani 1 1 d . . .
H7 H 0.5593 0.6565 0.4288 0.076 Uiso 1 1 calc R . .
C12 C -0.09002(11) 0.4688(3) 0.15778(7) 0.0431(3) Uani 1 1 d . . .
C19 C -0.09017(11) 0.4681(3) 0.48991(7) 0.0432(3) Uani 1 1 d . . .
C17 C -0.19165(13) 0.3715(3) 0.18997(8) 0.0546(3) Uani 1 1 d . . .
H17 H -0.2099 0.4346 0.2353 0.066 Uiso 1 1 calc R . .
C24 C -0.19146(13) 0.3713(3) 0.45778(8) 0.0543(3) Uani 1 1 d . . .
H24 H -0.2096 0.4342 0.4124 0.065 Uiso 1 1 calc R . .
C15 C -0.24074(19) 0.0861(4) 0.08878(11) 0.0727(5) Uani 1 1 d . . .
H15 H -0.2913 -0.0417 0.0657 0.087 Uiso 1 1 calc R . .
C22 C -0.24094(18) 0.0862(4) 0.55902(10) 0.0721(5) Uani 1 1 d . . .
H22 H -0.2915 -0.0415 0.5821 0.087 Uiso 1 1 calc R . .
C23 C -0.26637(15) 0.1817(4) 0.49241(11) 0.0678(4) Uani 1 1 d . . .
H23 H -0.3346 0.1185 0.4702 0.081 Uiso 1 1 calc R . .
C16 C -0.26628(16) 0.1814(4) 0.15542(11) 0.0678(4) Uani 1 1 d . . .
H16 H -0.3344 0.1178 0.1776 0.081 Uiso 1 1 calc R . .
C13 C -0.06513(17) 0.3706(4) 0.09070(8) 0.0606(4) Uani 1 1 d . . .
H13 H 0.0029 0.4330 0.0683 0.073 Uiso 1 1 calc R . .
C20 C -0.06525(16) 0.3706(3) 0.55718(8) 0.0602(4) Uani 1 1 d . . .
H20 H 0.0027 0.4335 0.5797 0.072 Uiso 1 1 calc R . .
C14 C -0.1404(2) 0.1801(4) 0.05637(10) 0.0774(5) Uani 1 1 d . . .
H14 H -0.1227 0.1157 0.0111 0.093 Uiso 1 1 calc R . .
C21 C -0.1405(2) 0.1802(4) 0.59139(10) 0.0776(5) Uani 1 1 d . . .
H21 H -0.1227 0.1157 0.6366 0.093 Uiso 1 1 calc R . .
C10 C 0.43271(12) 0.4037(3) 0.26081(8) 0.0539(3) Uani 1 1 d . . .
H10 H 0.4012 0.3414 0.2182 0.065 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'
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
C3 N1 C1 124.16(10) . . ?
C3 N1 C4 117.57(11) . . ?
C1 N1 C4 117.69(11) . . ?
C3 N3 C2 124.32(11) . . ?
C3 N3 C11 116.71(10) . . ?
C2 N3 C11 118.95(11) . . ?
C1 N2 C2 124.39(10) . . ?
C1 N2 C18 116.54(10) . . ?
C2 N2 C18 119.05(11) . . ?
O2 C2 N2 122.23(13) . . ?
O2 C2 N3 122.24(13) . . ?
N2 C2 N3 115.54(11) . . ?
N2 C18 C19 113.01(10) . . ?
N3 C11 C12 113.20(10) . . ?
O3 C3 N3 121.99(12) . . ?
O3 C3 N1 122.18(12) . . ?
N3 C3 N1 115.82(10) . . ?
O1 C1 N2 122.16(12) . . ?
O1 C1 N1 122.07(12) . . ?
N2 C1 N1 115.76(11) . . ?
C6 C5 C10 119.00(13) . . ?
C6 C5 C4 120.55(13) . . ?
C10 C5 C4 120.42(14) . . ?
C7 C6 C5 120.11(15) . . ?
C9 C8 C7 119.55(15) . . ?
C8 C9 C10 120.65(16) . . ?
N1 C4 C5 110.54(9) . . ?
C8 C7 C6 120.61(17) . . ?
C13 C12 C17 118.39(14) . . ?
C13 C12 C11 120.46(13) . . ?
C17 C12 C11 121.13(12) . . ?
C24 C19 C20 118.51(13) . . ?
C24 C19 C18 121.23(12) . . ?
C20 C19 C18 120.23(13) . . ?
C16 C17 C12 120.59(15) . . ?
C19 C24 C23 120.57(15) . . ?
C14 C15 C16 119.57(17) . . ?
C23 C22 C21 119.45(16) . . ?
C22 C23 C24 120.50(17) . . ?
C15 C16 C17 120.46(17) . . ?
C12 C13 C14 120.70(16) . . ?
C19 C20 C21 120.57(17) . . ?
C15 C14 C13 120.28(17) . . ?
C22 C21 C20 120.39(17) . . ?
C9 C10 C5 120.08(15) . . ?
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
N1 C3 1.3821(17) . ?
N1 C1 1.3844(17) . ?
N1 C4 1.4859(16) . ?
N3 C3 1.3785(16) . ?
N3 C2 1.3858(17) . ?
N3 C11 1.4797(17) . ?
N2 C1 1.3786(16) . ?
N2 C2 1.3832(17) . ?
N2 C18 1.4802(16) . ?
O3 C3 1.2067(16) . ?
O1 C1 1.2051(16) . ?
O2 C2 1.2058(16) . ?
C18 C19 1.5060(19) . ?
C11 C12 1.5011(19) . ?
C5 C6 1.387(2) . ?
C5 C10 1.388(2) . ?
C5 C4 1.5028(18) . ?
C6 C7 1.383(2) . ?
C8 C9 1.371(3) . ?
C8 C7 1.374(3) . ?
C9 C10 1.383(2) . ?
C12 C13 1.379(2) . ?
C12 C17 1.384(2) . ?
C19 C24 1.379(2) . ?
C19 C20 1.381(2) . ?
C17 C16 1.381(2) . ?
C24 C23 1.383(2) . ?
C15 C14 1.368(3) . ?
C15 C16 1.368(3) . ?
C22 C23 1.368(3) . ?
C22 C21 1.369(3) . ?
C13 C14 1.385(3) . ?
C20 C21 1.383(3) . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 11312
2 PubChem 11805
