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_7717634
_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 La O Si2)'
_chemical_formula_sum            'C38 H66 La2 O2 Si4'
_chemical_formula_weight         945.08
_chemical_name_systematic        '[La(Cp')2(OiPr)]2'
_chemical_properties_physical    Moisture-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                 101.345(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.0071(7)
_cell_length_b                   13.8430(6)
_cell_length_c                   18.6821(7)
_cell_measurement_reflns_used    9426
_cell_measurement_temperature    173.0
_cell_measurement_theta_max      27.672
_cell_measurement_theta_min      2.668
_cell_volume                     4565.9(3)
_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 0.992
_diffrn_measured_fraction_theta_max 0.939
_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  0.0562
_diffrn_reflns_av_unetI/netI     0.0263
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.939
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            208523
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.939
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.181
_diffrn_reflns_theta_min         2.056
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.978
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6469
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1154 before and 0.0806 after correction.
The Ratio of minimum to maximum transmission is 0.8676.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.375
_exptl_crystal_description       block
_exptl_crystal_F_000             1920
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.467
_refine_diff_density_min         -0.395
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     474
_refine_ls_number_reflns         10533
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0259
_refine_ls_R_factor_gt           0.0226
_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^)+(0.0221P)^2^+2.2662P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0529
_refine_ls_wR_factor_ref         0.0550
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9342
_reflns_number_total             10533
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02137a2.cif
_cod_data_source_block           mo_dh20240319_b_0m
_cod_database_code               7717634
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.827
_shelx_estimated_absorpt_t_min   0.743
_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, All C(H,H,H,H,H,H) groups
2. Restrained distances
 O1-C17A \\sim O1-C17B
 with sigma of 0.02
 C17A-C19 \\sim C17B-C19
 with sigma of 0.02
 C17A-C18 \\sim C17B-C18
 with sigma of 0.02
 Si4-C33 \\sim Si4-C33A
 with sigma of 0.02
 Si4-C34 \\sim Si4-C34A
 with sigma of 0.02
 Si4-C35 \\sim Si4-C35A
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 Si4, C33, C34, C35, C33A, C34A, C35A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(H18D)=Sof(H18E)=Sof(H18F)=Sof(H19D)=Sof(H19E)=Sof(H19F)=Sof(C17B)=
 Sof(H17B)=1-FVAR(1)
 Sof(H18A)=Sof(H18B)=Sof(H18C)=Sof(H19A)=Sof(H19B)=Sof(H19C)=Sof(C17A)=
 Sof(H17A)=FVAR(1)
 Sof(C33A)=Sof(H33D)=Sof(H33E)=Sof(H33F)=Sof(C34A)=Sof(H34D)=Sof(H34E)=
 Sof(H34F)=Sof(C35A)=Sof(H35D)=Sof(H35E)=Sof(H35F)=1-FVAR(2)
 Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(H33C)=Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(H34C)=
 Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(H35C)=FVAR(2)
5.a Ternary CH refined with riding coordinates:
 C17A(H17A), C17B(H17B), C36(H36)
5.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), C28(H28), C29(H29), C30(H30), C31(H31)
5.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), C18(H18D,H18E,
 H18F), C19(H19A,H19B,H19C), C19(H19D,H19E,H19F), C25(H25A,H25B,H25C), C26(H26A,
 H26B,H26C), C27(H27A,H27B,H27C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C),
 C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C33A(H33D,H33E,
 H33F), C34A(H34D,H34E,H34F), C35A(H35D,H35E,H35F)
;
_shelx_res_checksum              27202
_olex2_submission_special_instructions 'No special instructions were received'