Heterobimetallic Pd(0) complexes with Pd→ Ln (Ln = Sc, Y, Yb, Lu) dative bonds: rare-earth metal-dominated frustrated Lewis pair-like reactivity.
Du, Jun; Zhang, Yanan; Huang, Zeming; Zhou, Shuangliu; Fang, Huayi; Cui, Peng; Dalton transactions (Cambridge, England : 2003) 49 (2020) 12311–12318; doi:10.1039/d0dt02708a

data_7705061
_publ_section_title
;
 Heterobimetallic Pd(0) complexes with Pd\\rightarrow Ln (Ln = Sc, Y, Yb,
 Lu) dative bonds: rare-earth metal-dominated frustrated Lewis pair-like
 reactivity.
;
_journal_issue                   35
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12311
_journal_page_last               12318
_journal_paper_doi               10.1039/d0dt02708a
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C80 H85 N3 O P3 Pd Sc'
_chemical_formula_sum            'C80 H85 N3 O P3 Pd Sc'
_chemical_formula_weight         1348.78
_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
_audit_creation_date             2019-12-25
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-05-29 deposited with the CCDC.	2020-08-06 downloaded from the CCDC.
;
_cell_angle_alpha                101.234(2)
_cell_angle_beta                 95.789(2)
_cell_angle_gamma                105.159(2)
_cell_formula_units_Z            2
_cell_length_a                   13.7460(7)
_cell_length_b                   14.8611(8)
_cell_length_c                   20.7806(12)
_cell_measurement_reflns_used    9803
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      27.445
_cell_measurement_theta_min      2.861
_cell_volume                     3966.9(4)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_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  0.0606
_diffrn_reflns_av_unetI/netI     0.0530
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            80922
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.538
_diffrn_reflns_theta_min         2.860
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.414
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5393
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0933 before and 0.0609 after correction. The Ratio of minimum to maximum transmission is 0.7233. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.129
_exptl_crystal_description       block
_exptl_crystal_F_000             1412
_exptl_crystal_size_max          0.023
_exptl_crystal_size_mid          0.022
_exptl_crystal_size_min          0.021
_refine_diff_density_max         0.906
_refine_diff_density_min         -0.844
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     802
_refine_ls_number_reflns         18192
_refine_ls_number_restraints     2088
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0893
_refine_ls_R_factor_gt           0.0556
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0743P)^2^+4.3842P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1380
_refine_ls_wR_factor_ref         0.1594
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12411
_reflns_number_total             18192
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02708a3.cif
_cod_data_source_block           14
_cod_depositor_comments
'Adding full bibliography for 7705051--7705061.cif.'
_cod_original_cell_volume        3966.8(4)
_cod_database_code               7705061
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.991
_shelx_estimated_absorpt_t_min   0.991
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Uiso/Uaniso restraints and constraints
C0AA \\sim C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8
\\sim C9 \\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16
\\sim C17 \\sim C18 \\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim C24
\\sim C25 \\sim C26 \\sim C27 \\sim C28 \\sim C29 \\sim C30 \\sim C31 \\sim C32
\\sim C33 \\sim C34 \\sim C35 \\sim C36 \\sim C37 \\sim C38 \\sim C39 \\sim C40
\\sim C41 \\sim C42 \\sim C43 \\sim C44 \\sim C45 \\sim C46 \\sim C47 \\sim C48
\\sim C49 \\sim C50 \\sim C51 \\sim C52 \\sim C53 \\sim C54 \\sim C55 \\sim C56
\\sim C57 \\sim C58 \\sim C59 \\sim C60 \\sim C61 \\sim C62 \\sim C63 \\sim C64
\\sim C65 \\sim C66 \\sim C67 \\sim C68 \\sim C69 \\sim C70 \\sim C71 \\sim C72
\\sim C73 \\sim C74 \\sim C75 \\sim C76 \\sim C77 \\sim C78 \\sim C79: within
3.8A with sigma of 0.01 and sigma for terminal atoms of 0.02
3.a Ternary CH refined with riding coordinates:
 C14(H14), C19(H19), C22(H22), C38(H38), C40(H40), C42(H42), C69(H69),
 C72(H72), C74(H74)
3.b Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C15(H15A,H15B), C16(H16A,H16B), C18(H18A,H18B), C20(H20A,
 H20B), C21(H21A,H21B), C35(H35A,H35B), C37(H37A,H37B), C39(H39A,H39B),
 C41(H41A,H41B), C43(H43A,H43B), C44(H44A,H44B), C70(H70A,H70B), C71(H71A,H71B),
  C73(H73A,H73B), C75(H75A,H75B), C76(H76A,H76B), C78(H78A,H78B)
3.c Aromatic/amide H refined with riding coordinates:
 C0AA(H0AA), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C11(H11),
 C12(H12), C23(H23), C25(H25), C26(H26), C27(H27), C28(H28), C30(H30), C31(H31),
  C32(H32), C33(H33), C34(H34), C45(H45), C46(H46), C47(H47), C48(H48),
 C49(H49), C52(H52), C53(H53), C54(H54), C55(H55), C56(H56), C57(H57), C58(H58),
  C59(H59), C60(H60), C61(H61), C64(H64), C65(H65), C66(H66), C67(H67), C68(H68)
;
_shelx_res_checksum              37261
_shelx_fab_checksum              37204
_olex2_submission_special_instructions 'No special instructions were received'