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_7705057
_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 Lu N3 P4 Pd'
_chemical_formula_sum            'C84 H90 Lu N3 P4 Pd'
_chemical_formula_weight         1546.83
_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             2019-04-10
_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                   19.7190(13)
_cell_length_b                   16.2376(10)
_cell_length_c                   22.2512(14)
_cell_measurement_reflns_used    9764
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      27.62
_cell_measurement_theta_min      3.03
_cell_volume                     7124.6(8)
_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      273.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.994
_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  0.0933
_diffrn_reflns_av_unetI/netI     0.0350
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.994
_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            283355
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.655
_diffrn_reflns_theta_min         2.864
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.767
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.3343
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.442
_exptl_crystal_description       block
_exptl_crystal_F_000             3168
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.2
_refine_diff_density_max         3.760
_refine_diff_density_min         -1.605
_refine_diff_density_rms         0.158
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.075(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     731
_refine_ls_number_reflns         16470
_refine_ls_number_restraints     2061
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0789
_refine_ls_R_factor_gt           0.0625
_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^)+(0.0103P)^2^+77.9673P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1228
_refine_ls_wR_factor_ref         0.1351
_reflns_Friedel_coverage         0.941
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.987
_reflns_number_gt                14256
_reflns_number_total             16470
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02708a3.cif
_cod_data_source_block           8
_cod_depositor_comments
'Adding full bibliography for 7705051--7705061.cif.'
_cod_database_code               7705057
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.719
_shelx_estimated_absorpt_t_min   0.697
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.925(13)
 0.075(13)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
3. Restrained distances
 C6-C5 = C9-C8
 1.54 with sigma of 0.01
 C46-C45 = C53-C52 = C53-C47 = C54-C52 = C54-C49
 1.54 with sigma of 0.01
 C5-C10
 1.54 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
C39 \\sim C45 \\sim C11 \\sim C55 \\sim C00E \\sim C00F \\sim C7 \\sim C17
\\sim C23 \\sim C8 \\sim C18 \\sim C22 \\sim C46 \\sim C60 \\sim C00O \\sim C44
\\sim C2 \\sim C1 \\sim C00S \\sim C56 \\sim C61 \\sim C53 \\sim C51 \\sim C37
\\sim C47 \\sim C12 \\sim C010 \\sim C16 \\sim C29 \\sim C34 \\sim C26 \\sim C3
\\sim C40 \\sim C27 \\sim C24 \\sim C15 \\sim C33 \\sim C9 \\sim C21 \\sim C38
\\sim C19 \\sim C58 \\sim C62 \\sim C01H \\sim C35 \\sim C36 \\sim C41 \\sim
C50 \\sim C20 \\sim C01N \\sim C28 \\sim C66 \\sim C01Q \\sim C59 \\sim C43
\\sim C65 \\sim C57 \\sim C42 \\sim C10 \\sim C30 \\sim C52 \\sim C49 \\sim C6
\\sim C32 \\sim C022 \\sim C31 \\sim C64 \\sim C4 \\sim C5 \\sim C54 \\sim C48
\\sim C029 \\sim C13 \\sim C63 \\sim C14 \\sim C02D \\sim C25 \\sim C02G \\sim
C02H \\sim C02I \\sim C02M \\sim C02P \\sim C02Q \\sim C030: within 3.8A with
sigma of 0.01 and sigma for terminal atoms of 0.02
5.a Ternary CH refined with riding coordinates:
 C8(H8), C47(H47), C3(H3), C27(H27), C30(H30), C52(H52), C49(H49), C5(H5),
 C25(H25)
5.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C46(H46A,H46B), C2(H2A,H2B), C53(H53A,H53B), C51(H51A,H51B),
 C29(H29A,H29B), C26(H26A,H26B), C24(H24A,H24B), C9(H9A,H9B), C50(H50A,H50B),
 C28(H28A,H28B), C10(H10A,H10B), C6(H6A,H6B), C32(H32A,H32B), C31(H31A,H31B),
 C4(H4A,H4B), C54(H54A,H54B), C48(H48A,H48B)
5.c Aromatic/amide H refined with riding coordinates:
 C44(H44), C43(H43), C42(H42), C41(H41), C40(H40), C12(H12), C13(H13),
 C14(H14), C15(H15), C16(H16), C56(H56), C57(H57), C58(H58), C59(H59), C60(H60),
  C010(H010), C01H(H01H), C02G(H02G), C02I(H02I), C01Q(H01Q), C18(H18),
 C19(H19), C20(H20), C21(H21), C22(H22), C022(H022), C02Q(H02Q), C02H(H02H),
 C00O(H00O), C00E(H00E), C66(H66), C65(H65), C64(H64), C63(H63), C62(H62),
 C34(H34), C35(H35), C36(H36), C37(H37), C38(H38), C030(H030), C02P(H02P),
 C02D(H02D), C02M(H02M), C029(H029)
5.d Fitted hexagon refined as free rotating group:
 C39(C44,C43,C42,C41,C40), C11(C12,C13,C14,C15,C16), C55(C56,C57,C58,C59,C60),
 C00F(C010,C01H,C02G,C02I,C01Q), C17(C18,C19,C20,C21,C22), C00S(C022,C02Q,C02H,
 C00O,C00E), C61(C66,C65,C64,C63,C62), C33(C34,C35,C36,C37,C38), C01N(C030,C02P,
 C02D,C02M,C029)
;
_shelx_res_checksum              57830
_olex2_submission_special_instructions 'No special instructions were received'