Structure and bonding patterns in heterometallic organometallics with linear Ln–Pd–Ln motifs
Cemortan, Valeriu; Simler, Thomas; Moutet, Jules; Jaoul, Arnaud; Clavaguéra, Carine; Nocton, Grégory; Chemical Science 14 (2023) 2676–2685; doi:10.1039/D2SC06933D

data_1568480
_publ_section_title
;
 Structure and bonding patterns in heterometallic organometallics with
 linear Ln--Pd--Ln motifs
;
_journal_issue                   10
_journal_name_full               'Chemical Science'
_journal_page_first              2676
_journal_page_last               2685
_journal_paper_doi               10.1039/D2SC06933D
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         'C32 H51 Pd Yb'
_chemical_formula_sum            'C32 H51 Pd Yb'
_chemical_formula_weight         715.16
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc2dc32z
_audit_creation_date             2022-10-18
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-10-25 deposited with the CCDC.	2023-01-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.493(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.5080(9)
_cell_length_b                   16.1094(16)
_cell_length_c                   21.445(2)
_cell_measurement_reflns_used    9985
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      33.96
_cell_measurement_theta_min      2.28
_cell_volume                     2938.2(5)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150.00
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0586
_diffrn_reflns_av_unetI/netI     0.0286
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            117934
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         34.337
_diffrn_reflns_theta_min         2.553
_exptl_absorpt_coefficient_mu    3.793
_exptl_absorpt_correction_T_max  0.7481
_exptl_absorpt_correction_T_min  0.4937
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1271 before and 0.0623 after correction.
The Ratio of minimum to maximum transmission is 0.6599.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.617
_exptl_crystal_description       plate
_exptl_crystal_F_000             1436
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.28
_refine_diff_density_max         1.500
_refine_diff_density_min         -1.958
_refine_diff_density_rms         0.143
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     340
_refine_ls_number_reflns         12295
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.0386
_refine_ls_R_factor_gt           0.0275
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0195P)^2^+3.7830P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0588
_refine_ls_wR_factor_ref         0.0645
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10281
_reflns_number_total             12295
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc06933d2.cif
_cod_data_source_block           6
_cod_depositor_comments
'Adding full bibliography for 1568477--1568482.cif.'
_cod_database_code               1568480
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.416
_shelx_estimated_absorpt_t_min   0.209
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H) groups, All C(H,H,H) groups, All Yb(H,H) groups
2.a Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C),
 C12(H12A,H12B,H12C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,
 H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C28(H28A,H28B,H28C), C29(H29A,
 H29B,H29C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C)
;
_shelx_res_checksum              62668
_shelx_hkl_checksum              21426
_olex2_submission_special_instructions 'No special instructions were received'