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_7705053
_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 H75 Lu N3 P3'
_chemical_formula_sum            'C66 H75 Lu N3 P3'
_chemical_formula_weight         1178.17
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-04-08
_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                 96.253(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.6419(17)
_cell_length_b                   13.4745(10)
_cell_length_c                   20.3693(19)
_cell_measurement_reflns_used    9607
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      27.56
_cell_measurement_theta_min      3.08
_cell_volume                     6450.3(9)
_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      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  0.1135
_diffrn_reflns_av_unetI/netI     0.0425
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            137498
_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         27.609
_diffrn_reflns_theta_min         3.008
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.643
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.213
_exptl_crystal_description       block
_exptl_crystal_F_000             2432
_refine_diff_density_max         2.572
_refine_diff_density_min         -3.271
_refine_diff_density_rms         0.128
_refine_ls_abs_structure_details
;
 Flack x determined using 6367 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.021(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     586
_refine_ls_number_reflns         14902
_refine_ls_number_restraints     1636
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0670
_refine_ls_R_factor_gt           0.0647
_refine_ls_shift/su_max          0.029
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0499P)^2^+89.7918P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1458
_refine_ls_wR_factor_ref         0.1476
_reflns_Friedel_coverage         0.994
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.990
_reflns_number_gt                14404
_reflns_number_total             14902
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02708a3.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7705051--7705061.cif.'
_cod_database_code               7705053
_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
2. Restrained distances
 N1-C2
 2.5 with sigma of 0.02
 C24-C23 = C25-C24 = C32-C25 = C28-C27 = C32-C30 = C30-C29 = C49-C48 = C54-C49
 = C54-C52 = C52-C51 = C51-C45 = C53-C47 = C53-C52 = C50-C47 = C50-C49 = C3-C2 =
  C2-C1 = C3-C10 = C8-C10 = C9-C8 = C9-C5 = C6-C5 = C6-C3 = C4-C1 = C5-C4 = C8-
 C7 = C7-C1
 1.54 with sigma of 0.02
 C50-C49 = C50-C47 = C54-C49 = C53-C47 = C53-C52 = C54-C52
 1.54 with sigma of 0.01
 C53-C47 = C50-C47 = C54-C49 = C54-C52 = C53-C52 = C50-C49 = C52-C51 = C47-C46
 = C49-C48 = C51-C45
 1.54 with sigma of 0.0005
3. Uiso/Uaniso restraints and constraints
C17 \\sim C22 \\sim C19 \\sim C18 \\sim C20 \\sim C21 \\sim C45 \\sim C1 \\sim
C38 \\sim C7 \\sim C8 \\sim C6 \\sim C10 \\sim C2 \\sim C5 \\sim C37 \\sim C3
\\sim C33 \\sim C9 \\sim C4 \\sim C49 \\sim C48 \\sim C23 \\sim C25 \\sim C24
\\sim C28 \\sim C32 \\sim C29 \\sim C26 \\sim C31 \\sim C27 \\sim C40 \\sim C39
\\sim C43 \\sim C44 \\sim C34 \\sim C35 \\sim C36 \\sim C30 \\sim C42 \\sim C41
\\sim C55 \\sim C56 \\sim C60 \\sim C46 \\sim C58 \\sim C59 \\sim C57 \\sim C51
\\sim C47 \\sim C54 \\sim C11 \\sim C61 \\sim C62 \\sim C12 \\sim C66 \\sim C13
\\sim C16 \\sim C50 \\sim C52 \\sim C53 \\sim C63 \\sim C14 \\sim C15 \\sim C64
\\sim C65: within 3.8A with sigma of 0.01 and sigma for terminal atoms of 0.02
4.a Ternary CH refined with riding coordinates:
 C8(H8), C5(H5), C3(H3), C49(H49), C25(H25), C27(H27), C30(H30), C47(H47),
 C52(H52)
4.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C6(H6A,H6B), C10(H10A,H10B), C2(H2A,H2B), C9(H9A,H9B), C4(H4A,
 H4B), C48(H48A,H48B), C24(H24A,H24B), C28(H28A,H28B), C32(H32A,H32B), C29(H29A,
 H29B), C26(H26A,H26B), C31(H31A,H31B), C46(H46A,H46B), C51(H51A,H51B),
 C54(H54A,H54B), C50(H50A,H50B), C53(H53A,H53B)
4.c Aromatic/amide H refined with riding coordinates:
 C22(H22), C21(H21), C20(H20), C19(H19), C18(H18), C34(H34), C35(H35),
 C36(H36), C37(H37), C38(H38), C40(H40), C44(H44), C43(H43), C42(H42), C41(H41),
  C60(H60), C59(H59), C58(H58), C57(H57), C56(H56), C62(H62), C63(H63),
 C64(H64), C65(H65), C66(H66), C12(H12), C16(H16), C15(H15), C14(H14), C13(H13)
4.d Fitted hexagon refined as free rotating group:
 C17(C22,C21,C20,C19,C18), C33(C34,C35,C36,C37,C38), C40(C39,C44,C43,C42,C41),
 C55(C60,C59,C58,C57,C56), C61(C62,C63,C64,C65,C66), C12(C11,C16,C15,C14,C13)
;
_shelx_res_checksum              60398
_shelx_fab_checksum              41011
_olex2_submission_special_instructions 'No special instructions were received'