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_7705056
_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 Sc'
_chemical_formula_sum            'C84 H90 N3 P4 Pd Sc'
_chemical_formula_weight         1416.82
_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
_audit_creation_date             2020-05-29
_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                   19.6769(10)
_cell_length_b                   16.1787(8)
_cell_length_c                   22.2319(11)
_cell_measurement_reflns_used    9627
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      3.04
_cell_volume                     7077.5(6)
_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 0.996
_diffrn_measured_fraction_theta_max 0.986
_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  0.0877
_diffrn_reflns_av_unetI/netI     0.0395
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            233897
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.580
_diffrn_reflns_theta_min         2.873
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.488
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.330
_exptl_crystal_description       block
_exptl_crystal_F_000             2968
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.254
_refine_diff_density_min         -1.424
_refine_diff_density_rms         0.124
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.11(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.166
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     839
_refine_ls_number_reflns         15923
_refine_ls_number_restraints     2071
_refine_ls_restrained_S_all      1.148
_refine_ls_R_factor_all          0.1041
_refine_ls_R_factor_gt           0.0879
_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^)+40.7659P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1556
_refine_ls_wR_factor_ref         0.1644
_reflns_Friedel_coverage         0.921
_reflns_Friedel_fraction_full    0.990
_reflns_Friedel_fraction_max     0.957
_reflns_number_gt                13698
_reflns_number_total             15923
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02708a3.cif
_cod_data_source_block           5
_cod_depositor_comments
'Adding full bibliography for 7705051--7705061.cif.'
_cod_database_code               7705056
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.909
_shelx_estimated_absorpt_t_min   0.900
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.89(5)
 0.11(5)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
3. Uiso/Uaniso restraints and constraints
C34 \\sim C79 \\sim C17 \\sim C67 \\sim C2 \\sim C11 \\sim C23 \\sim C33 \\sim
C16 \\sim C14 \\sim C45 \\sim C55 \\sim C62 \\sim C72 \\sim C1 \\sim C24 \\sim
C43 \\sim C39 \\sim C15 \\sim C22 \\sim C48 \\sim C40 \\sim C60 \\sim C61 \\sim
C49 \\sim C29 \\sim C56 \\sim C73 \\sim C13 \\sim C35 \\sim C57 \\sim C44 \\sim
C84 \\sim C46 \\sim C12 \\sim C71 \\sim C65 \\sim C18 \\sim C58 \\sim C80 \\sim
C59 \\sim C42 \\sim C66 \\sim C25 \\sim C32 \\sim C38 \\sim C63 \\sim C70 \\sim
C27 \\sim C30 \\sim C51 \\sim C36 \\sim C26 \\sim C64 \\sim C41 \\sim C81 \\sim
C47 \\sim C82 \\sim C50 \\sim C83 \\sim C53 \\sim C21 \\sim C31 \\sim C7 \\sim
C3 \\sim C6 \\sim C10 \\sim C54 \\sim C8 \\sim C19 \\sim C68 \\sim C28 \\sim C5
\\sim C4 \\sim C52 \\sim C69 \\sim C37 \\sim C74 \\sim C75 \\sim C20 \\sim C9
\\sim C78 \\sim C76 \\sim C77: within 3.8A with sigma of 0.01 and sigma for
terminal atoms of 0.02
4.a Ternary CH refined with riding coordinates:
 C49(H49), C25(H25), C27(H27), C30(H30), C47(H47), C3(H3), C8(H8), C5(H5),
 C52(H52)
4.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C24(H24A,H24B), C48(H48A,H48B), C29(H29A,H29B), C46(H46A,H46B),
 C32(H32A,H32B), C51(H51A,H51B), C26(H26A,H26B), C50(H50A,H50B), C53(H53A,H53B),
  C31(H31A,H31B), C7(H7A,H7B), C6(H6A,H6B), C10(H10A,H10B), C54(H54A,H54B),
 C28(H28A,H28B), C4(H4A,H4B), C9(H9A,H9B)
4.c Aromatic/amide H refined with riding coordinates:
 C34(H34), C16(H16), C14(H14), C62(H62), C72(H72), C43(H43), C15(H15),
 C22(H22), C40(H40), C60(H60), C56(H56), C13(H13), C35(H35), C57(H57), C44(H44),
  C84(H84), C12(H12), C71(H71), C65(H65), C18(H18), C58(H58), C80(H80),
 C59(H59), C42(H42), C66(H66), C38(H38), C63(H63), C70(H70), C36(H36), C64(H64),
  C41(H41), C81(H81), C82(H82), C83(H83), C21(H21), C19(H19), C68(H68),
 C69(H69), C37(H37), C74(H74), C75(H75), C20(H20), C78(H78), C76(H76), C77(H77)
;
_shelx_res_checksum              47875
_olex2_submission_special_instructions 'No special instructions were received'