#------------------------------------------------------------------------------
#$Date: 2024-12-06 22:19:14 +0200 (Fri, 06 Dec 2024) $
#$Revision: 296636 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/06/34/7063466.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_7063466
loop_
_publ_author_name
'Liu, Kang'
'Chi, Xiaowang'
'Guo, Yan'
'Hu, Kongqiu'
'Mei, Lei'
'Yu, Jipan'
'Shi, Weiqun'
_publ_section_title
;
 Advancing the understanding of M--O covalency in isostructural M--OSiMe3
 (M = Ce, Th, U) complexes
;
_journal_issue                   42
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              18241
_journal_page_last               18248
_journal_paper_doi               10.1039/D4NJ03128H
_journal_volume                  48
_journal_year                    2024
_chemical_formula_moiety         'C33 H54 Ce1 N4 O1 Si4'
_chemical_formula_sum            'C33 H54 Ce N4 O Si4'
_chemical_formula_weight         775.28
_space_group_crystal_system      trigonal
_space_group_IT_number           161
_space_group_name_Hall           'R 3 -2"c'
_space_group_name_H-M_alt        'R 3 c :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2024-02-25
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-05-30 deposited with the CCDC.	2024-10-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   16.9979(6)
_cell_length_b                   16.9979(6)
_cell_length_c                   23.6994(10)
_cell_measurement_reflns_used    3350
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      28.6350
_cell_measurement_theta_min      3.2050
_cell_volume                     5930.1(4)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.15
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.828
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -42.87 158.63   0.50   10.00    --   -6.25  73.75  71.28  403
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0637
_diffrn_reflns_av_unetI/netI     0.0416
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.828
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            9847
_diffrn_reflns_point_group_measured_fraction_full 0.877
_diffrn_reflns_point_group_measured_fraction_max 0.684
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.310
_diffrn_reflns_theta_min         3.258
_exptl_absorpt_coefficient_mu    1.302
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54220
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic dark blue'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.303
_exptl_crystal_description       block
_exptl_crystal_F_000             2412
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.434
_refine_diff_density_min         -0.468
_refine_diff_density_rms         0.079
_refine_ls_abs_structure_details
;
 Flack x determined using 828 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.02(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     134
_refine_ls_number_reflns         2472
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0368
_refine_ls_R_factor_gt           0.0327
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0534P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0830
_refine_ls_wR_factor_ref         0.0874
_reflns_Friedel_coverage         0.646
_reflns_Friedel_fraction_full    0.776
_reflns_Friedel_fraction_max     0.538
_reflns_number_gt                2226
_reflns_number_total             2472
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4nj03128h2.cif
_cod_data_source_block           mo_ce_i_autored
_cod_depositor_comments
'Adding full bibliography for 7063465--7063469.cif.'
_cod_original_cell_volume        5930.1(5)
_cod_original_sg_symbol_H-M      'R 3 c'
_cod_database_code               7063466
_shelx_shelxl_version_number     2018/3
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.870
_shelx_estimated_absorpt_t_min   0.839
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6)
2.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C8(H8A,H8B,H8C)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x+y, y, z+1/2'
'x, x-y, z+1/2'
'-y, -x, z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'-x+y+2/3, y+1/3, z+5/6'
'x+2/3, x-y+1/3, z+5/6'
'-y+2/3, -x+1/3, z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x+y+1/3, y+2/3, z+7/6'
'x+1/3, x-y+2/3, z+7/6'
'-y+1/3, -x+2/3, z+7/6'
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ce1 Ce 0.666667 0.333333 0.47329(6) 0.02474(16) Uani 1 3 d S T P . .
Si4 Si 0.666667 0.333333 0.63014(19) 0.0357(7) Uani 1 3 d S T P . .
Si1 Si 0.60408(8) 0.50383(8) 0.47868(8) 0.0363(3) Uani 1 1 d . . . . .
O1 O 0.666667 0.333333 0.5616(5) 0.034(3) Uani 1 3 d S T P . .
N4 N 0.666667 0.333333 0.3604(6) 0.030(3) Uani 1 3 d S T P . .
N1 N 0.5827(3) 0.3987(3) 0.4551(2) 0.0312(10) Uani 1 1 d . . . . .
C11 C 0.6337(6) 0.2183(5) 0.6564(4) 0.0674(16) Uani 1 1 d . . . . .
H11A H 0.668555 0.195331 0.636342 0.101 Uiso 1 1 calc R U . . .
H11B H 0.568663 0.177433 0.649822 0.101 Uiso 1 1 calc R U . . .
H11C H 0.646377 0.221166 0.696912 0.101 Uiso 1 1 calc R U . . .
C1 C 0.6128(4) 0.3742(4) 0.3385(3) 0.0421(16) Uani 1 1 d . . . . .
H1A H 0.608101 0.367666 0.296903 0.050 Uiso 1 1 calc R U . . .
H1B H 0.644946 0.439865 0.347404 0.050 Uiso 1 1 calc R U . . .
C2 C 0.5188(3) 0.3301(3) 0.3633(2) 0.0401(11) Uani 1 1 d . . . . .
C9 C 0.5060(4) 0.4988(4) 0.5175(4) 0.057(2) Uani 1 1 d . . . . .
H9A H 0.486401 0.452882 0.547354 0.085 Uiso 1 1 calc R U . . .
H9B H 0.455698 0.482540 0.491194 0.085 Uiso 1 1 calc R U . . .
H9C H 0.524545 0.558210 0.534274 0.085 Uiso 1 1 calc R U . . .
C10 C 0.7027(4) 0.5488(3) 0.5273(2) 0.0455(13) Uani 1 1 d . . . . .
H10A H 0.749589 0.538010 0.511181 0.068 Uiso 1 1 calc R U . . .
H10B H 0.683179 0.517990 0.563801 0.068 Uiso 1 1 calc R U . . .
H10C H 0.727482 0.614216 0.532497 0.068 Uiso 1 1 calc R U . . .
C3 C 0.4442(4) 0.2761(4) 0.3297(3) 0.0516(14) Uani 1 1 d . . . . .
H3 H 0.452735 0.266124 0.291296 0.062 Uiso 1 1 calc R U . . .
C4 C 0.3567(4) 0.2366(4) 0.3519(3) 0.0614(17) Uani 1 1 d . . . . .
H4 H 0.305775 0.199331 0.328777 0.074 Uiso 1 1 calc R U . . .
C8 C 0.6303(5) 0.5810(4) 0.4174(3) 0.0598(15) Uani 1 1 d . . . . .
H8A H 0.578726 0.555298 0.391305 0.090 Uiso 1 1 calc R U . . .
H8B H 0.684395 0.588063 0.397990 0.090 Uiso 1 1 calc R U . . .
H8C H 0.641795 0.640490 0.430600 0.090 Uiso 1 1 calc R U . . .
C7 C 0.5064(3) 0.3458(3) 0.4201(2) 0.0367(10) Uani 1 1 d . . . . .
C5 C 0.3442(3) 0.2514(4) 0.4067(3) 0.0574(16) Uani 1 1 d . . . . .
H5 H 0.284510 0.224604 0.421854 0.069 Uiso 1 1 calc R U . . .
C6 C 0.4185(3) 0.3055(3) 0.4406(2) 0.0432(12) Uani 1 1 d . . . . .
H6 H 0.408797 0.315136 0.478878 0.052 Uiso 1 1 calc R U . . .
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'
Ce Ce -0.2486 2.6331 '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'
Si Si 0.0817 0.0704 '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
O1 Ce1 N4 180.0 . . ?
O1 Ce1 N1 101.06(14) . 2_655 ?
O1 Ce1 N1 101.06(14) . 3_665 ?
O1 Ce1 N1 101.06(14) . . ?
N1 Ce1 N4 78.94(14) 2_655 . ?
N1 Ce1 N4 78.94(14) 3_665 . ?
N1 Ce1 N4 78.94(14) . . ?
N1 Ce1 N1 116.41(9) 2_655 . ?
N1 Ce1 N1 116.41(9) 2_655 3_665 ?
N1 Ce1 N1 116.41(9) 3_665 . ?
Si4 O1 Ce1 180.0 . . ?
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
Ce1 O1 2.092(12) . ?
Ce1 N4 2.675(13) . ?
Ce1 N1 2.246(5) . ?
Ce1 N1 2.246(5) 2_655 ?
Ce1 N1 2.246(5) 3_665 ?
Si4 O1 1.625(12) . ?
Si4 C11 1.852(7) . ?
Si4 C11 1.852(7) 2_655 ?
Si4 C11 1.852(7) 3_665 ?
Si1 N1 1.728(5) . ?
Si1 C9 1.867(8) . ?
Si1 C10 1.855(5) . ?
Si1 C8 1.856(6) . ?
N4 C1 1.493(9) . ?
N4 C1 1.493(9) 2_655 ?
N4 C1 1.493(9) 3_665 ?
N1 C7 1.419(7) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C2 1.505(8) . ?
C2 C3 1.387(7) . ?
C2 C7 1.408(7) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C3 H3 0.9500 . ?
C3 C4 1.393(10) . ?
C4 H4 0.9500 . ?
C4 C5 1.360(10) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C7 C6 1.383(7) . ?
C5 H5 0.9500 . ?
C5 C6 1.387(8) . ?
C6 H6 0.9500 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ce1 N4 C1 C2 -52.9(5) . . . . ?
Ce1 N1 C7 C2 -67.2(5) . . . . ?
Ce1 N1 C7 C6 110.4(4) . . . . ?
Si1 N1 C7 C2 112.0(5) . . . . ?
Si1 N1 C7 C6 -70.4(6) . . . . ?
N4 C1 C2 C3 -110.2(7) . . . . ?
N4 C1 C2 C7 71.8(8) . . . . ?
N1 C7 C6 C5 -177.9(5) . . . . ?
C1 N4 C1 C2 -174.0(5) 3_665 . . . ?
C1 N4 C1 C2 68.2(11) 2_655 . . . ?
C1 C2 C3 C4 -178.6(5) . . . . ?
C1 C2 C7 N1 -3.9(7) . . . . ?
C1 C2 C7 C6 178.4(5) . . . . ?
C2 C3 C4 C5 0.5(9) . . . . ?
C2 C7 C6 C5 -0.2(7) . . . . ?
C9 Si1 N1 Ce1 -124.9(4) . . . . ?
C9 Si1 N1 C7 55.9(6) . . . . ?
C10 Si1 N1 Ce1 -5.2(4) . . . . ?
C10 Si1 N1 C7 175.7(4) . . . . ?
C3 C2 C7 N1 178.2(5) . . . . ?
C3 C2 C7 C6 0.5(6) . . . . ?
C3 C4 C5 C6 -0.3(9) . . . . ?
C4 C5 C6 C7 0.1(9) . . . . ?
C8 Si1 N1 Ce1 114.6(4) . . . . ?
C8 Si1 N1 C7 -64.5(5) . . . . ?
C7 C2 C3 C4 -0.6(7) . . . . ?
