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_1568478
_publ_section_title
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 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         'C74 H90 N10 Pd2 Yb2, 2(C4 H8 O), 4[O1C4H8]'
_chemical_formula_sum            'C98 H138 N10 O6 Pd2 Yb2'
_chemical_formula_weight         2111.06
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc2dc2zv
_audit_creation_date             2022-10-19
_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                101.902(7)
_cell_angle_beta                 102.431(7)
_cell_angle_gamma                113.691(7)
_cell_formula_units_Z            2
_cell_length_a                   14.758(4)
_cell_length_b                   17.469(5)
_cell_length_c                   20.212(6)
_cell_measurement_reflns_used    5572
_cell_measurement_temperature    149.99
_cell_measurement_theta_max      21.836
_cell_measurement_theta_min      2.184
_cell_volume                     4403(2)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_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      149.99
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_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  0.1951
_diffrn_reflns_av_unetI/netI     0.1656
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            96195
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.069
_diffrn_reflns_theta_max         25.069
_diffrn_reflns_theta_min         1.347
_exptl_absorpt_coefficient_mu    2.568
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5772
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1252 before and 0.0841 after correction.
The Ratio of minimum to maximum transmission is 0.7746.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.592
_exptl_crystal_description       needle
_exptl_crystal_F_000             2152
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.937
_refine_diff_density_min         -1.172
_refine_diff_density_rms         0.178
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     905
_refine_ls_number_reflns         15419
_refine_ls_number_restraints     61
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.1530
_refine_ls_R_factor_gt           0.0674
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0898P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1502
_refine_ls_wR_factor_ref         0.1898
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7861
_reflns_number_total             15419
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc06933d2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 1568477--1568482.cif.'
_cod_database_code               1568478
_shelx_shelxl_version_number     2019/2
_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. Restrained distances
 C76-C75 \\sim C77-C78
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C82 \\sim O2 \\sim C79 \\sim C80 \\sim C81: within 2A with sigma of 0.004 and
sigma for terminal atoms of 0.008 within 2A
O1 \\sim C75 \\sim C76 \\sim C77 \\sim C78: within 2A with sigma of 0.004 and
sigma for terminal atoms of 0.008 within 2A
4.a Ternary CH refined with riding coordinates:
 C4(H4), C19(H19)
4.b Secondary CH2 refined with riding coordinates:
 C75(H75A,H75B), C76(H76A,H76B), C77(H77A,H77B), C78(H78A,H78B), C79(H79A,
 H79B), C80(H80A,H80B), C81(H81A,H81B), C82(H82A,H82B)
4.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12), C13(H13),
 C14(H14), C15(H15), C16(H16), C20(H20), C21(H21), C25(H25), C26(H26), C27(H27),
  C28(H28), C29(H29), C30(H30), C31(H31), C32(H32), C33(H33)
4.d Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C34(H34A,H34B,H34C), C40(H40A,H40B,H40C), C41(H41A,H41B,
 H41C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C44(H44A,H44B,H44C), C50(H50A,
 H50B,H50C), C51(H51A,H51B,H51C), C52(H52A,H52B,H52C), C53(H53A,H53B,H53C),
 C54(H54A,H54B,H54C), C60(H60A,H60B,H60C), C61(H61A,H61B,H61C), C62(H62A,H62B,
 H62C), C63(H63A,H63B,H63C), C64(H64A,H64B,H64C), C70(H70A,H70B,H70C), C71(H71A,
 H71B,H71C), C72(H72A,H72B,H72C), C73(H73A,H73B,H73C), C74(H74A,H74B,H74C)
;
_smtbx_masks_special_details
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A solvent mask was calculated and 340 electrons were 
found in a volume of 864\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
4[O1C4H8] per Asymmetric Unit 
which account for 320 electrons 
per unit cell.
;
_shelx_res_checksum              25730
_shelx_hkl_checksum              12445
_shelx_fab_checksum              94133
_olex2_submission_special_instructions 'No special instructions were received'