Synthesis and reduction of [(C<sub>5</sub>H<sub>4</sub>SiMe<sub>3</sub>)<sub>2</sub>Ln(μ-OR)]<sub>2</sub> (Ln = La, Ce) complexes: structural effects of bridging alkoxides.
Brown, Adrian N.; Kelleher, Jack N.; Brown, Alexander M.; Saghy, Peter; Bohl, Joshua J.; Robinson, Jerome R.; Huh, Daniel N.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 18856–18864; doi:10.1039/d4dt02137a

data_7717632
_publ_section_title
;
 Synthesis and reduction of
 [(C<sub>5</sub>H<sub>4</sub>SiMe<sub>3</sub>)<sub>2</sub>Ln(&#x3bc;-OR)]<sub>2</sub>
 (Ln = La, Ce) complexes: structural effects of bridging alkoxides.
;
_journal_issue                   47
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              18856
_journal_page_last               18864
_journal_paper_doi               10.1039/d4dt02137a
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C18 H31 Ce O Si2'
_chemical_formula_sum            'C18 H31 Ce O Si2'
_chemical_formula_weight         459.73
_chemical_name_systematic        '[Ce(Cp')2(OEt)]2'
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-02-23
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-07-22 deposited with the CCDC.	2024-08-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.647(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.433(2)
_cell_length_b                   11.0399(16)
_cell_length_c                   14.619(2)
_cell_measurement_reflns_used    9376
_cell_measurement_temperature    177
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      2.684
_cell_volume                     2153.4(5)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      177
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0555
_diffrn_reflns_av_unetI/netI     0.0270
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            57458
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.501
_diffrn_reflns_theta_min         2.684
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.225
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6920
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0676 before and 0.0573 after correction.
The Ratio of minimum to maximum transmission is 0.9288.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.418
_exptl_crystal_description       block
_exptl_crystal_F_000             932
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.329
_refine_diff_density_min         -0.755
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     206
_refine_ls_number_reflns         4948
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0191
_refine_ls_R_factor_gt           0.0184
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0216P)^2^+0.7069P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0463
_refine_ls_wR_factor_ref         0.0466
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4763
_reflns_number_total             4948
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02137a2.cif
_cod_data_source_block           mo_dh20240216_0m
_cod_original_cell_volume        2153.4(6)
_cod_database_code               7717632
_shelx_shelxl_version_number     2019/1
_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. Rigid body (RIGU) restrains
 O1, C17, C18
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3.a Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B)
3.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C9(H9), C10(H10), C11(H11), C12(H12)
3.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C14(H14A,H14B,H14C),
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C18(H18A,H18B,H18C)
;
_shelx_res_checksum              12811
_olex2_submission_special_instructions 'No special instructions were received'