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_7705055
_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         'C66 H78 N3 P3 Pd'
_chemical_formula_sum            'C66 H78 N3 P3 Pd'
_chemical_formula_weight         1112.62
_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   mixed
_audit_creation_date             2019-11-26
_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                105.848(2)
_cell_angle_beta                 95.818(2)
_cell_angle_gamma                104.347(2)
_cell_formula_units_Z            2
_cell_length_a                   11.3117(5)
_cell_length_b                   13.1850(6)
_cell_length_c                   23.7630(12)
_cell_measurement_reflns_used    9835
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      27.239
_cell_measurement_theta_min      2.846
_cell_volume                     3248.3(3)
_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  'XL (Sheldrick, 2008)'
_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 0.993
_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  0.0586
_diffrn_reflns_av_unetI/netI     0.0570
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            64218
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.555
_diffrn_reflns_theta_min         2.824
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.398
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5274
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0932 before and 0.0604 after correction. The Ratio of minimum to maximum transmission is 0.7073. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colorless
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.138
_exptl_crystal_description       block
_exptl_crystal_F_000             1172
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.887
_refine_diff_density_min         -1.237
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     740
_refine_ls_number_reflns         14923
_refine_ls_number_restraints     233
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0951
_refine_ls_R_factor_gt           0.0583
_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^)+(0.0619P)^2^+4.8356P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1325
_refine_ls_wR_factor_ref         0.1539
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10284
_reflns_number_total             14923
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02708a3.cif
_cod_data_source_block           9
_cod_depositor_comments
'Adding full bibliography for 7705051--7705061.cif.'
_cod_database_code               7705055
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
2. Restrained distances
 C7AA-C5AA
 1.54 with sigma of 0.001
 C9AA-C7AA
 1.54 with sigma of 0.001
 C2AA-C1AA = C5AA-C3AA = C9AA-C4AA
 1.54 with sigma of 0.005
 C2AA-C0BA = C9AA-C0BA = C6AA-C2AA
 1.54 with sigma of 0.001
 C9AA-C0BA = C2AA-C0BA
 1.54 with sigma of 0.0005
 C6AA-C5AA
 1.54 with sigma of 0.001
 C1AA-C0AA = C3AA-C0AA
 1.54 with sigma of 0.01
 C5AB-C3AB = C6AB-C5AB = C6AB-C2AB = C2AB-C1AB = C9AB-C4AB
 1.54 with sigma of 0.001
 C2AB-C0BB = C9AB-C0BB = C9AB-C7AB = C7AB-C5AB = C6AB-C5AB = C6AB-C2AB
 1.54 with sigma of 0.001
 C0AA-C5AB
 2.52 with sigma of 0.01
 C0AA-C9AB
 2.52 with sigma of 0.01
 C0AA-C2AB
 2.52 with sigma of 0.01
 C4AB-C7AB
 2.52 with sigma of 0.01
 C2AB-C5AB
 2.52 with sigma of 0.01
 C4AB-C0AA \\sim C4AA-C0AA \\sim C3AB-C0AA \\sim C3AA-C0AA \\sim C1AB-C0AA
\\sim C1AA-C0AA
 with sigma of 0.02
 C5AB-C3AB \\sim C5AA-C3AA \\sim C2AB-C1AB \\sim C2AA-C1AA \\sim C9AB-C4AB
\\sim C9AA-C4AA
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C4AA) \\sim Ueq, Uanis(C2AA) \\sim Ueq, Uanis(C3AA) \\sim Ueq,
Uanis(C9AA) \\sim Ueq, Uanis(C0BA) \\sim Ueq, Uanis(C5AA) \\sim Ueq,
Uanis(C6AA) \\sim Ueq, Uanis(C7AA) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(C0AA) \\sim Ueq, Uanis(C1AA) \\sim Ueq, Uanis(C4AA) \\sim Ueq,
Uanis(C2AA) \\sim Ueq, Uanis(C3AA) \\sim Ueq, Uanis(C9AA) \\sim Ueq,
Uanis(C0BA) \\sim Ueq, Uanis(C5AA) \\sim Ueq, Uanis(C6AA) \\sim Ueq,
Uanis(C7AA) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C23) \\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C20)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 C0AA, C1AB, C4AB, C2AB, C3AB, C9AB, C0BB, C5AB, C6AB, C7AB
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
5. Others
 Sof(C1AB)=Sof(H1AC)=Sof(H1AD)=Sof(C4AB)=Sof(H4AC)=Sof(H4AD)=Sof(C2AB)=
 Sof(H2AB)=Sof(C3AB)=Sof(H3AC)=Sof(H3AD)=Sof(C9AB)=Sof(H9AB)=Sof(C0BB)=
 Sof(H0BC)=Sof(H0BD)=Sof(C5AB)=Sof(H5AB)=Sof(C6AB)=Sof(H6AC)=Sof(H6AD)=
 Sof(C7AB)=Sof(H7AC)=Sof(H7AD)=1-FVAR(1)
 Sof(C1AA)=Sof(H1AA)=Sof(H1AB)=Sof(C4AA)=Sof(H4AA)=Sof(H4AB)=Sof(C2AA)=
 Sof(H2AA)=Sof(C3AA)=Sof(H3AA)=Sof(H3AB)=Sof(C9AA)=Sof(H9AA)=Sof(C0BA)=
 Sof(H0BA)=Sof(H0BB)=Sof(C5AA)=Sof(H5AA)=Sof(C6AA)=Sof(H6AA)=Sof(H6AB)=
 Sof(C7AA)=Sof(H7AA)=Sof(H7AB)=FVAR(1)
6.a Riding coordinates:
 N005(H005), N006(H006), N007(H007)
6.b Ternary CH refined with riding coordinates:
 C39(H39), C42(H42), C44(H44), C48(H48), C50(H50), C55(H55), C2AA(H2AA),
 C9AA(H9AA), C5AA(H5AA), C2AB(H2AB), C9AB(H9AB), C5AB(H5AB)
6.c Secondary CH2 refined with riding coordinates:
 C38(H38A,H38B), C40(H40A,H40B), C41(H41A,H41B), C43(H43A,H43B), C45(H45A,
 H45B), C46(H46A,H46B), C47(H47A,H47B), C49(H49A,H49B), C51(H51A,H51B),
 C52(H52A,H52B), C54(H54A,H54B), C56(H56A,H56B), C1AA(H1AA,H1AB), C4AA(H4AA,
 H4AB), C3AA(H3AA,H3AB), C0BA(H0BA,H0BB), C6AA(H6AA,H6AB), C7AA(H7AA,H7AB),
 C1AB(H1AC,H1AD), C4AB(H4AC,H4AD), C3AB(H3AC,H3AD), C0BB(H0BC,H0BD), C6AB(H6AC,
 H6AD), C7AB(H7AC,H7AD)
6.d Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C20(H20), C21(H21),
  C22(H22), C23(H23), C24(H24), C26(H26), C27(H27), C28(H28), C29(H29),
 C30(H30), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36)
;
_shelx_res_checksum              47615
_shelx_fab_checksum              46453
_olex2_submission_special_instructions 'No special instructions were received'