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_7717633
_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         '2(C19 H33 Ce O Si2)'
_chemical_formula_sum            'C38 H66 Ce2 O2 Si4'
_chemical_formula_weight         947.50
_chemical_name_systematic        '[Ce(Cp')2(OiPr)]2'
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yac'
_space_group_name_H-M_alt        'P 1 2/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-07-12
_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                 100.767(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.043(2)
_cell_length_b                   13.8611(19)
_cell_length_c                   18.671(3)
_cell_measurement_reflns_used    9823
_cell_measurement_temperature    173.0
_cell_measurement_theta_max      27.451
_cell_measurement_theta_min      2.663
_cell_volume                     4587.3(11)
_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      173.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1295
_diffrn_reflns_av_unetI/netI     0.0702
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            125523
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.732
_diffrn_reflns_theta_min         2.058
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    2.091
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.5456
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1222 before and 0.1003 after correction.
The Ratio of minimum to maximum transmission is 0.7319.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.372
_exptl_crystal_description       plate
_exptl_crystal_F_000             1928
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.113
_refine_diff_density_min         -0.708
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     493
_refine_ls_number_reflns         10704
_refine_ls_number_restraints     123
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0948
_refine_ls_R_factor_gt           0.0527
_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/[\s^2^(Fo^2^)+(0.0595P)^2^+8.8239P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1335
_refine_ls_wR_factor_ref         0.1583
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6186
_reflns_number_total             10704
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02137a2.cif
_cod_data_source_block           mo_dh20240216_c_0m
_cod_database_code               7717633
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.940
_shelx_estimated_absorpt_t_min   0.851
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Si4-C33 \\sim Si4-C33A
 with sigma of 0.02
 Si4-C32 \\sim Si4-C32A
 with sigma of 0.02
 Si4-C34 \\sim Si4-C34A
 with sigma of 0.02
 C17-C19 \\sim C17A-C19A
 with sigma of 0.02
 O1-C17 \\sim O1-C17A
 with sigma of 0.02
 C18-C19 \\sim C18A-C19A
 with sigma of 0.04
 C17-C18 \\sim C17A-C18A
 with sigma of 0.02
 O1-C18 \\sim O1-C18A
 with sigma of 0.04
 O1-C19 \\sim O1-C19A
 with sigma of 0.04
3. Rigid bond restraints
 Si4, C32, C33, C34
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O1, C17, C18, C19
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Si4, C32, C33, C34, C32A, C33A, C34A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Si4 \\sim C32 \\sim C33 \\sim C34: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 1.7A
O1 \\sim C17 \\sim C18 \\sim C19: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 1.7A
Si4 \\sim C32 \\sim C33 \\sim C34 \\sim C32A \\sim C33A \\sim C34A: within 1.7A
with sigma of 0.04 and sigma for terminal atoms of 0.08 within 1.7A
5. Rigid body (RIGU) restrains
 Si4, C32, C33, C34
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O1, C17, C18, C19
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Si4, C32, C33, C34, C32A, C33A, C34A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C35, C36, C37
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C17, C18, C19, C17A, C18A, C19A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(C32A)=Sof(H32D)=Sof(H32E)=Sof(H32F)=Sof(C33A)=Sof(H33D)=Sof(H33E)=
 Sof(H33F)=Sof(C34A)=Sof(H34D)=Sof(H34E)=Sof(H34F)=1-FVAR(1)
 Sof(C32)=Sof(H32A)=Sof(H32B)=Sof(H32C)=Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(H33C)=
 Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(H34C)=FVAR(1)
 Fixed Sof: C17(0.5) H17(0.5) C18(0.5) H18A(0.5) H18B(0.5) H18C(0.5) C19(0.5)
 H19A(0.5) H19B(0.5) H19C(0.5) C17A(0.5) H17A(0.5) C18A(0.5) H18D(0.5)
 H18E(0.5) H18F(0.5) C19A(0.5) H19D(0.5) H19E(0.5) H19F(0.5)
7.a Ternary CH refined with riding coordinates:
 C17(H17), C17A(H17A), C35(H35)
7.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C9(H9), C10(H10), C11(H11), C12(H12),
 C20(H20), C21(H21), C22(H22), C23(H23), C27(H27), C28(H28), C29(H29), C30(H30)
7.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), C19(H19A,H19B,
 H19C), C18A(H18D,H18E,H18F), C19A(H19D,H19E,H19F), C24(H24A,H24B,H24C),
 C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C36(H36A,H36B,H36C), C37(H37A,H37B,
 H37C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C),
 C32A(H32D,H32E,H32F), C33A(H33D,H33E,H33F), C34A(H34D,H34E,H34F)
;
_shelx_res_checksum              90469
_olex2_submission_special_instructions 'No special instructions were received'