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_1568479
_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         'C74 H90 N10 Pd2 Yb2, 3(C7 H8)'
_chemical_formula_sum            'C95 H114 N10 Pd2 Yb2'
_chemical_formula_weight         1954.84
_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   geom
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc2dc2yt
_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                 111.427(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.7945(4)
_cell_length_b                   34.6792(12)
_cell_length_c                   17.8510(5)
_cell_measurement_reflns_used    8637
_cell_measurement_temperature    149.99
_cell_measurement_theta_max      24.109
_cell_measurement_theta_min      2.349
_cell_volume                     8525.6(5)
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      149.99
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.993
_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  0.0964
_diffrn_reflns_av_unetI/netI     0.0795
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       46
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            100236
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.700
_diffrn_reflns_theta_min         2.315
_exptl_absorpt_coefficient_mu    2.640
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5921
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0913 before and 0.0675 after correction.
The Ratio of minimum to maximum transmission is 0.7936.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.523
_exptl_crystal_description       plate
_exptl_crystal_F_000             3944
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.653
_refine_diff_density_min         -1.642
_refine_diff_density_rms         0.172
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1290
_refine_ls_number_reflns         21851
_refine_ls_number_restraints     1848
_refine_ls_restrained_S_all      0.994
_refine_ls_R_factor_all          0.0902
_refine_ls_R_factor_gt           0.0515
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0522P)^2^+30.4974P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1148
_refine_ls_wR_factor_ref         0.1371
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14866
_reflns_number_total             21851
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc06933d2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 1568477--1568482.cif.'
_cod_database_code               1568479
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.858
_shelx_estimated_absorpt_t_min   0.467
_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. Uiso/Uaniso restraints and constraints
C74 \\sim C75 \\sim C76 \\sim C77 \\sim C79 \\sim C83 \\sim C82 \\sim C81 \\sim
C78 \\sim C80 \\sim C79A \\sim C74A \\sim C75A \\sim C76A \\sim C77A \\sim C80A
\\sim C83A \\sim C82A \\sim C81A \\sim C78A: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
C35 \\sim C37 \\sim C30 \\sim C32 \\sim C33 \\sim C36 \\sim C38 \\sim C31 \\sim
C39 \\sim C34 \\sim C32A \\sim C33A \\sim C35A \\sim C37A \\sim C30A \\sim C39A
\\sim C34A \\sim C36A \\sim C38A \\sim C31A: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
C70 \\sim C69 \\sim C68 \\sim C67 \\sim C66 \\sim C71 \\sim C1 \\sim C72 \\sim
C2 \\sim C73 \\sim C66A \\sim C70A \\sim C69A \\sim C68A \\sim C67A \\sim C73A
\\sim C71A \\sim C1A \\sim C72A \\sim C2A: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
C84 \\sim C85 \\sim C86 \\sim C87 \\sim C88 \\sim C89 \\sim C90 \\sim C84A
\\sim C85A \\sim C86A \\sim C87A \\sim C88A \\sim C89A \\sim C90A: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C25 \\sim C27 \\sim C20 \\sim C21 \\sim C23 \\sim C26 \\sim C28 \\sim C29 \\sim
C22 \\sim C24 \\sim C25A \\sim C27A \\sim C20A \\sim C21A \\sim C23A \\sim C26A
\\sim C28A \\sim C29A \\sim C22A \\sim C24A: within 2A with sigma of 0.004 and
sigma for terminal atoms of 0.008 within 2A
C74 \\sim C75 \\sim C79 \\sim C83 \\sim C82 \\sim C80 \\sim C79A \\sim C74A
\\sim C75A \\sim C80A \\sim C83A \\sim C82A \\sim C76 \\sim C77 \\sim C81 \\sim
C78 \\sim C76A \\sim C77A \\sim C81A \\sim C78A: within 2A with sigma of 0.004
and sigma for terminal atoms of 0.008 within 2A
3. Rigid body (RIGU) restrains
 C84, C85, C86, C87, C88, C89, C90, C84A, C85A, C86A, C87A, C88A, C89A, C90A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C3, C4, C91, C92, C93, C94, C95, C3A, C4A, C91A, C92A, C93A, C94A, C95A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C74, C75, C76, C77, C79, C83, C82, C81, C78, C80, C79A, C74A, C75A, C76A,
 C77A, C80A, C83A, C82A, C81A, C78A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Others
 Sof(C32A)=Sof(C33A)=Sof(C35A)=Sof(C37A)=Sof(C30A)=Sof(C39A)=Sof(H39D)=
 Sof(H39E)=Sof(H39F)=Sof(C34A)=Sof(H34D)=Sof(H34E)=Sof(H34F)=Sof(C36A)=
 Sof(H36D)=Sof(H36E)=Sof(H36F)=Sof(C38A)=Sof(H38D)=Sof(H38E)=Sof(H38F)=
 Sof(C31A)=Sof(H31D)=Sof(H31E)=Sof(H31F)=1-FVAR(1)
 Sof(C35)=Sof(C37)=Sof(C30)=Sof(C32)=Sof(C33)=Sof(C36)=Sof(H36A)=Sof(H36B)=
 Sof(H36C)=Sof(C38)=Sof(H38A)=Sof(H38B)=Sof(H38C)=Sof(C31)=Sof(H31A)=Sof(H31B)=
 Sof(H31C)=Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(H39C)=Sof(C34)=Sof(H34A)=Sof(H34B)=
 Sof(H34C)=FVAR(1)
 Sof(C25A)=Sof(C27A)=Sof(C20A)=Sof(C21A)=Sof(C23A)=Sof(C26A)=Sof(H26D)=
 Sof(H26E)=Sof(H26F)=Sof(C28A)=Sof(H28D)=Sof(H28E)=Sof(H28F)=Sof(C29A)=
 Sof(H29D)=Sof(H29E)=Sof(H29F)=Sof(C22A)=Sof(H22D)=Sof(H22E)=Sof(H22F)=
 Sof(C24A)=Sof(H24D)=Sof(H24E)=Sof(H24F)=1-FVAR(2)
 Sof(C25)=Sof(C27)=Sof(C20)=Sof(C21)=Sof(C23)=Sof(C26)=Sof(H26A)=Sof(H26B)=
 Sof(H26C)=Sof(C28)=Sof(H28A)=Sof(H28B)=Sof(H28C)=Sof(C29)=Sof(H29A)=Sof(H29B)=
 Sof(H29C)=Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(H22C)=Sof(C24)=Sof(H24A)=Sof(H24B)=
 Sof(H24C)=FVAR(2)
 Sof(C79A)=Sof(C74A)=Sof(C75A)=Sof(C76A)=Sof(C77A)=Sof(C80A)=Sof(H80D)=
 Sof(H80E)=Sof(H80F)=Sof(C83A)=Sof(H83D)=Sof(H83E)=Sof(H83F)=Sof(C82A)=
 Sof(H82D)=Sof(H82E)=Sof(H82F)=Sof(C81A)=Sof(H81D)=Sof(H81E)=Sof(H81F)=
 Sof(C78A)=Sof(H78D)=Sof(H78E)=Sof(H78F)=1-FVAR(3)
 Sof(C74)=Sof(C75)=Sof(C76)=Sof(C77)=Sof(C79)=Sof(C83)=Sof(H83A)=Sof(H83B)=
 Sof(H83C)=Sof(C82)=Sof(H82A)=Sof(H82B)=Sof(H82C)=Sof(C81)=Sof(H81A)=Sof(H81B)=
 Sof(H81C)=Sof(C78)=Sof(H78A)=Sof(H78B)=Sof(H78C)=Sof(C80)=Sof(H80A)=Sof(H80B)=
 Sof(H80C)=FVAR(3)
 Sof(C66A)=Sof(C70A)=Sof(C69A)=Sof(C68A)=Sof(C67A)=Sof(C73A)=Sof(H73D)=
 Sof(H73E)=Sof(H73F)=Sof(C71A)=Sof(H71D)=Sof(H71E)=Sof(H71F)=Sof(C1A)=Sof(H1AA)=
 Sof(H1AB)=Sof(H1AC)=Sof(C72A)=Sof(H72D)=Sof(H72E)=Sof(H72F)=Sof(C2A)=Sof(H2AA)=
 Sof(H2AB)=Sof(H2AC)=1-FVAR(4)
 Sof(C70)=Sof(C69)=Sof(C68)=Sof(C67)=Sof(C66)=Sof(C71)=Sof(H71A)=Sof(H71B)=
 Sof(H71C)=Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(H1C)=Sof(C72)=Sof(H72A)=Sof(H72B)=
 Sof(H72C)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(H2C)=Sof(C73)=Sof(H73A)=Sof(H73B)=
 Sof(H73C)=FVAR(4)
 Sof(C92A)=Sof(C91A)=Sof(H91A)=Sof(C4A)=Sof(H4A)=Sof(C3A)=Sof(H3A)=Sof(C94A)=
 Sof(H94A)=Sof(C93A)=Sof(H93A)=Sof(C95A)=Sof(H95D)=Sof(H95E)=Sof(H95F)=1-FVAR(5)
 Sof(C3)=Sof(H3)=Sof(C4)=Sof(H4)=Sof(C91)=Sof(H91)=Sof(C92)=Sof(C93)=Sof(H93)=
 Sof(C94)=Sof(H94)=Sof(C95)=Sof(H95A)=Sof(H95B)=Sof(H95C)=FVAR(5)
 Sof(C87A)=Sof(C89A)=Sof(H89A)=Sof(C90A)=Sof(H90A)=Sof(C84A)=Sof(H84A)=
 Sof(C85A)=Sof(H85A)=Sof(C86A)=Sof(H86A)=Sof(C88A)=Sof(H88D)=Sof(H88E)=
 Sof(H88F)=1-FVAR(6)
 Sof(C87)=Sof(C89)=Sof(H89)=Sof(C90)=Sof(H90)=Sof(C84)=Sof(H84)=Sof(C85)=
 Sof(H85)=Sof(C86)=Sof(H86)=Sof(C88)=Sof(H88A)=Sof(H88B)=Sof(H88C)=FVAR(6)
5.a :
 C25(C27,C20,C21,C23,C26,C28,C29,C22,C24), C35(C37,C30,C32,C33,C36,C38,C31,C39,
 C34), C70(C69,C68,C67,C66,C71,C1,C72,C2,C73), C74(C75,C76,C77,C79,C83,C82,C81,
 C78,C80), C32A(C33A,C35A,C37A,C30A,C39A,C34A,C36A,C38A,C31A), C25A(C27A,C20A,
 C21A,C23A,C26A,C28A,C29A,C22A,C24A), C79A(C74A,C75A,C76A,C77A,C80A,C83A,C82A,
 C81A,C78A), C66A(C70A,C69A,C68A,C67A,C73A,C71A,C1A,C72A,C2A), C3(C4,C91,C92,
 C93,C94)
5.b Ternary CH refined with riding coordinates:
 C16(H16), C17(H17)
5.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C8(H8), C11(H11), C12(H12), C15(H15), C18(H18),
 C19(H19), C43(H43), C44(H44), C45(H45), C46(H46), C48(H48), C49(H49), C50(H50),
  C51(H51), C52(H52), C54(H54), C55(H55), C56(H56), C57(H57), C58(H58),
 C61(H61), C62(H62), C63(H63), C64(H64), C89(H89), C90(H90), C84(H84), C85(H85),
  C86(H86), C3(H3), C4(H4), C91(H91), C93(H93), C94(H94), C91A(H91A), C4A(H4A),
 C3A(H3A), C94A(H94A), C93A(H93A), C89A(H89A), C90A(H90A), C84A(H84A),
 C85A(H85A), C86A(H86A)
5.d Fitted hexagon refined as free rotating group:
 C87(C89,C90,C84,C85,C86), C92A(C91A,C4A,C3A,C94A,C93A), C87A(C89A,C90A,C84A,
 C85A,C86A)
5.e Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C26(H26A,H26B,H26C), C28(H28A,H28B,H28C), C29(H29A,H29B,
 H29C), C22(H22A,H22B,H22C), C24(H24A,H24B,H24C), C36(H36A,H36B,H36C), C38(H38A,
 H38B,H38C), C31(H31A,H31B,H31C), C39(H39A,H39B,H39C), C34(H34A,H34B,H34C),
 C53(H53A,H53B,H53C), C59(H59A,H59B,H59C), C71(H71A,H71B,H71C), C1(H1A,H1B,H1C),
  C72(H72A,H72B,H72C), C2(H2A,H2B,H2C), C73(H73A,H73B,H73C), C83(H83A,H83B,
 H83C), C82(H82A,H82B,H82C), C81(H81A,H81B,H81C), C78(H78A,H78B,H78C), C80(H80A,
 H80B,H80C), C88(H88A,H88B,H88C), C39A(H39D,H39E,H39F), C34A(H34D,H34E,H34F),
 C36A(H36D,H36E,H36F), C38A(H38D,H38E,H38F), C31A(H31D,H31E,H31F), C26A(H26D,
 H26E,H26F), C28A(H28D,H28E,H28F), C29A(H29D,H29E,H29F), C22A(H22D,H22E,H22F),
 C24A(H24D,H24E,H24F), C80A(H80D,H80E,H80F), C83A(H83D,H83E,H83F), C82A(H82D,
 H82E,H82F), C81A(H81D,H81E,H81F), C78A(H78D,H78E,H78F), C73A(H73D,H73E,H73F),
 C71A(H71D,H71E,H71F), C1A(H1AA,H1AB,H1AC), C72A(H72D,H72E,H72F), C2A(H2AA,H2AB,
 H2AC), C95(H95A,H95B,H95C), C95A(H95D,H95E,H95F), C88A(H88D,H88E,H88F)
;
_shelx_res_checksum              45185
_shelx_hkl_checksum              8417
_olex2_submission_special_instructions 'No special instructions were received'