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#$Date: 2025-08-21 13:21:36 +0200 (Thu 21 de Aug de 2025) $
#$Revision: 301847 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/39/7013963.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_7013963
loop_
_publ_author_name
'Avent, Anthony G.'
'Caro, Catherine F.'
'Hitchcock, Peter B.'
'Lappert, Michael F.'
'Li, Zhengning'
'Wei, Xue-Hong'
_publ_section_title
;
 Synthetic and structural experiments on yttrium, cerium and magnesium
 trimethylsilylmethyls and their reaction products with nitriles; with
 a note on two cerium beta-diketiminates.
;
_journal_issue                   10
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1567
_journal_page_last               1577
_journal_paper_doi               10.1039/b316695n
_journal_year                    2004
_chemical_formula_sum            'C18 H48 Mg O Si4'
_chemical_formula_weight         417.23
_space_group_IT_number           20
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'C 2c 2'
_symmetry_space_group_name_H-M   'C 2 2 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.676(4)
_cell_length_b                   16.620(8)
_cell_length_c                   17.173(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      10
_cell_measurement_theta_min      7
_cell_volume                     2761.7(18)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Nonius CAD4'
_diffrn_measurement_method       'omega-2theta scans'
_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  0.0555
_diffrn_reflns_av_sigmaI/netI    0.0582
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            4864
_diffrn_reflns_theta_full        24.97
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         2.37
_exptl_absorpt_coefficient_mu    0.243
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.003
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             928
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.274
_refine_diff_density_min         -0.468
_refine_diff_density_rms         0.078
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     110
_refine_ls_number_reflns         2447
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0383
_refine_ls_R_factor_gt           0.0347
_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)+(0.0587P)²+0.2368P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0889
_refine_ls_wR_factor_ref         0.0904
_reflns_number_gt                2354
_reflns_number_total             2447
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b316695n.txt
_cod_data_source_block           (15)-apr2297
_cod_original_sg_symbol_H-M      C222(1)
_cod_database_code               7013963
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x, -y, -z'
'-x, -y, z+1/2'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'x+1/2, -y+1/2, -z'
'-x+1/2, -y+1/2, z+1/2'
'-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
Mg Mg 0.41150(8) 0.0000 0.0000 0.0203(2) Uani 1 2 d S . .
Si1 Si 0.27648(6) -0.12451(3) 0.14200(3) 0.02643(15) Uani 1 1 d . . .
Si2 Si 0.26685(6) 0.06554(3) 0.15510(3) 0.02579(15) Uani 1 1 d . . .
O O 0.62273(18) 0.0000 0.0000 0.0276(4) Uani 1 2 d S . .
C1 C 0.35135(18) -0.02572(10) 0.11735(10) 0.0218(4) Uani 1 1 d . . .
H1 H 0.4416 -0.0263 0.1457 0.026 Uiso 1 1 calc R . .
C2 C 0.4063(2) -0.20628(12) 0.12556(14) 0.0402(5) Uani 1 1 d . . .
H2C H 0.3652 -0.2584 0.1389 0.060 Uiso 1 1 calc R . .
H2B H 0.4875 -0.1968 0.1585 0.060 Uiso 1 1 calc R . .
H2A H 0.4344 -0.2065 0.0707 0.060 Uiso 1 1 calc R . .
C3 C 0.1174(3) -0.14934(14) 0.08432(14) 0.0425(5) Uani 1 1 d . . .
H3C H 0.0827 -0.2023 0.1000 0.064 Uiso 1 1 calc R . .
H3B H 0.1401 -0.1501 0.0287 0.064 Uiso 1 1 calc R . .
H3A H 0.0463 -0.1086 0.0941 0.064 Uiso 1 1 calc R . .
C4 C 0.2230(3) -0.13473(14) 0.24719(13) 0.0479(6) Uani 1 1 d . . .
H4C H 0.1843 -0.1885 0.2559 0.072 Uiso 1 1 calc R . .
H4B H 0.1530 -0.0940 0.2595 0.072 Uiso 1 1 calc R . .
H4A H 0.3037 -0.1270 0.2808 0.072 Uiso 1 1 calc R . .
C5 C 0.0773(2) 0.06591(15) 0.13304(15) 0.0440(5) Uani 1 1 d . . .
H5C H 0.0355 0.1151 0.1538 0.066 Uiso 1 1 calc R . .
H5B H 0.0337 0.0189 0.1572 0.066 Uiso 1 1 calc R . .
H5A H 0.0636 0.0639 0.0765 0.066 Uiso 1 1 calc R . .
C6 C 0.3479(3) 0.15745(12) 0.10977(13) 0.0423(5) Uani 1 1 d . . .
H6C H 0.3027 0.2059 0.1300 0.063 Uiso 1 1 calc R . .
H6B H 0.3366 0.1552 0.0531 0.063 Uiso 1 1 calc R . .
H6A H 0.4465 0.1590 0.1226 0.063 Uiso 1 1 calc R . .
C7 C 0.2874(3) 0.08119(14) 0.26311(12) 0.0409(5) Uani 1 1 d . . .
H7C H 0.2398 0.1307 0.2786 0.061 Uiso 1 1 calc R . .
H7B H 0.3858 0.0856 0.2759 0.061 Uiso 1 1 calc R . .
H7A H 0.2472 0.0354 0.2911 0.061 Uiso 1 1 calc R . .
C8 C 0.7048(2) 0.05678(13) -0.04452(12) 0.0339(5) Uani 1 1 d . . .
H8B H 0.6517 0.0741 -0.0909 0.041 Uiso 1 1 calc R . .
H8A H 0.7899 0.0297 -0.0629 0.041 Uiso 1 1 calc R . .
C9 C 0.7436(2) 0.12929(13) 0.00244(16) 0.0454(5) Uani 1 1 d . . .
H9C H 0.7988 0.1659 -0.0297 0.068 Uiso 1 1 calc R . .
H9B H 0.7978 0.1125 0.0478 0.068 Uiso 1 1 calc R . .
H9A H 0.6597 0.1569 0.0199 0.068 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'
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'
Mg Mg 0.0486 0.0363 '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
O Mg C1 105.78(5) . 2 ?
O Mg C1 105.78(5) . . ?
C1 Mg C1 148.45(10) 2 . ?
C1 Si1 C2 110.36(10) . . ?
C1 Si1 C3 113.39(9) . . ?
C2 Si1 C3 108.14(11) . . ?
C1 Si1 C4 114.06(9) . . ?
C2 Si1 C4 105.26(11) . . ?
C3 Si1 C4 105.10(12) . . ?
C1 Si2 C5 111.49(10) . . ?
C1 Si2 C7 114.43(9) . . ?
C5 Si2 C7 107.59(12) . . ?
C1 Si2 C6 109.72(10) . . ?
C5 Si2 C6 108.74(11) . . ?
C7 Si2 C6 104.53(11) . . ?
C8 O C8 113.6(2) . 2 ?
C8 O Mg 123.19(11) . . ?
C8 O Mg 123.19(11) 2 . ?
Si2 C1 Si1 118.58(10) . . ?
Si2 C1 Mg 106.72(8) . . ?
Si1 C1 Mg 120.05(9) . . ?
O C8 C9 112.13(16) . . ?
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
Mg O 2.044(2) . ?
Mg C1 2.1408(17) 2 ?
Mg C1 2.1408(17) . ?
Si1 C1 1.8438(19) . ?
Si1 C2 1.872(2) . ?
Si1 C3 1.876(2) . ?
Si1 C4 1.887(2) . ?
Si2 C1 1.8411(19) . ?
Si2 C5 1.872(2) . ?
Si2 C7 1.883(2) . ?
Si2 C6 1.885(2) . ?
O C8 1.451(2) . ?
O C8 1.451(2) 2 ?
C8 C9 1.498(3) . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139155582
