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_7705054
_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         'C84 H90 N3 P4 Pd Yb'
_chemical_formula_sum            'C84 H90 N3 P4 Pd Yb'
_chemical_formula_weight         1544.90
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-04-15
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.7393(19)
_cell_length_b                   16.2623(16)
_cell_length_c                   22.283(2)
_cell_measurement_reflns_used    9969
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.97
_cell_measurement_theta_min      2.26
_cell_volume                     7153.0(12)
_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 (Sheldrick, 2015)'
_diffrn_ambient_temperature      293.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0447
_diffrn_reflns_av_unetI/netI     0.0551
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            60753
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.487
_diffrn_reflns_theta_min         1.622
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.688
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4550
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.435
_exptl_crystal_description       block
_exptl_crystal_F_000             3164
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.938
_refine_diff_density_min         -0.422
_refine_diff_density_rms         0.075
_refine_ls_abs_structure_details
;
 Flack x determined using 5564 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.008(4)
_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     826
_refine_ls_number_reflns         16189
_refine_ls_number_restraints     2035
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0491
_refine_ls_R_factor_gt           0.0331
_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^)+(0.0253P)^2^+1.5459P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0693
_refine_ls_wR_factor_ref         0.0751
_reflns_Friedel_coverage         0.923
_reflns_Friedel_fraction_full    0.984
_reflns_Friedel_fraction_max     0.973
_reflns_number_gt                13244
_reflns_number_total             16189
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02708a3.cif
_cod_data_source_block           7
_cod_depositor_comments
'Adding full bibliography for 7705051--7705061.cif.'
_cod_original_cell_volume        7153.1(12)
_cod_database_code               7705054
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.729
_shelx_estimated_absorpt_t_min   0.708
_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
C51 \\sim C16 \\sim C84 \\sim C67 \\sim C11 \\sim C1 \\sim C33 \\sim C62 \\sim
C63 \\sim C79 \\sim C47 \\sim C45 \\sim C38 \\sim C41 \\sim C12 \\sim C44 \\sim
C46 \\sim C52 \\sim C83 \\sim C61 \\sim C72 \\sim C4 \\sim C56 \\sim C7 \\sim
C57 \\sim C55 \\sim C35 \\sim C34 \\sim C13 \\sim C66 \\sim C15 \\sim C29 \\sim
C60 \\sim C36 \\sim C9 \\sim C40 \\sim C14 \\sim C20 \\sim C24 \\sim C50 \\sim
C5 \\sim C43 \\sim C19 \\sim C37 \\sim C39 \\sim C23 \\sim C68 \\sim C54 \\sim
C64 \\sim C30 \\sim C26 \\sim C18 \\sim C69 \\sim C31 \\sim C73 \\sim C28 \\sim
C58 \\sim C25 \\sim C2 \\sim C10 \\sim C42 \\sim C65 \\sim C49 \\sim C27 \\sim
C22 \\sim C17 \\sim C80 \\sim C3 \\sim C32 \\sim C21 \\sim C8 \\sim C53 \\sim
C6 \\sim C48 \\sim C70 \\sim C71 \\sim C59 \\sim C78 \\sim C81 \\sim C82 \\sim
C77 \\sim C76 \\sim C74 \\sim C75: within 3.8A with sigma of 0.01 and sigma for
terminal atoms of 0.02
3.a Ternary CH refined with riding coordinates:
 C47(H47), C52(H52), C5(H5), C30(H30), C25(H25), C49(H49), C27(H27), C3(H3),
 C8(H8)
3.b Secondary CH2 refined with riding coordinates:
 C51(H51A,H51B), C46(H46A,H46B), C4(H4A,H4B), C7(H7A,H7B), C29(H29A,H29B),
 C9(H9A,H9B), C24(H24A,H24B), C50(H50A,H50B), C54(H54A,H54B), C26(H26A,H26B),
 C31(H31A,H31B), C28(H28A,H28B), C2(H2A,H2B), C10(H10A,H10B), C32(H32A,H32B),
 C53(H53A,H53B), C6(H6A,H6B), C48(H48A,H48B)
3.c Aromatic/amide H refined with riding coordinates:
 C16(H16), C84(H84), C62(H62), C63(H63), C38(H38), C41(H41), C12(H12),
 C44(H44), C83(H83), C72(H72), C56(H56), C57(H57), C35(H35), C34(H34), C13(H13),
  C66(H66), C15(H15), C60(H60), C36(H36), C40(H40), C14(H14), C20(H20),
 C43(H43), C19(H19), C37(H37), C68(H68), C64(H64), C18(H18), C69(H69), C78(H78),
  C77(H77), C76(H76), C75(H75), C74(H74), C58(H58), C42(H42), C65(H65),
 C22(H22), C80(H80), C21(H21), C70(H70), C71(H71), C59(H59), C81(H81), C82(H82)
3.d Fitted hexagon refined as free rotating group:
 C73(C78,C77,C76,C75,C74)
;
_shelx_res_checksum              6068
_olex2_submission_special_instructions 'No special instructions were received'