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_1568482
_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         'C50 H68 N2 Pd Sm2, 2(C7 H8)'
_chemical_formula_sum            'C64 H84 N2 Pd Sm2'
_chemical_formula_weight         1288.43
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc2dc30x
_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                 91.602(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.7006(11)
_cell_length_b                   13.8198(8)
_cell_length_c                   26.6978(17)
_cell_measurement_reflns_used    4862
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      22.161
_cell_measurement_theta_min      2.595
_cell_volume                     5790.6(6)
_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      150.00
_diffrn_measured_fraction_theta_full 0.999
_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     0.71069
_diffrn_reflns_av_R_equivalents  0.1212
_diffrn_reflns_av_unetI/netI     0.0864
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            46629
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         26.369
_diffrn_reflns_theta_min         2.465
_exptl_absorpt_coefficient_mu    2.348
_exptl_absorpt_correction_T_max  0.7416
_exptl_absorpt_correction_T_min  0.6781
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0774 before and 0.0700 after correction.
The Ratio of minimum to maximum transmission is 0.9144.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.478
_exptl_crystal_description       block
_exptl_crystal_F_000             2608
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.131
_refine_diff_density_min         -1.282
_refine_diff_density_rms         0.171
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.891
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     323
_refine_ls_number_reflns         5915
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.891
_refine_ls_R_factor_all          0.0594
_refine_ls_R_factor_gt           0.0378
_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^)+(0.0205P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0685
_refine_ls_wR_factor_ref         0.0739
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4113
_reflns_number_total             5915
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc06933d2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 1568477--1568482.cif.'
_cod_database_code               1568482
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.912
_shelx_estimated_absorpt_t_min   0.766
_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.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C28(H28), C29(H29), C30(H30), C31(H31),
 C32(H32)
2.b Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C14(H14A,H14B,
 H14C), C15(H15A,H15B,H15C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,
 H23B,H23C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C)
;
_shelx_res_checksum              53816
_shelx_hkl_checksum              36914
_olex2_submission_special_instructions 'No special instructions were received'