Bi- and trimetallic rare-earth-palladium complexes ligated by phosphinoamides
Franziska Volcker; Felix M. Muck; Konstantinos D. Vogiatzis; Karin Fink; Peter W. Roesky; Chem.Commun. 51 (2015) 11761–; doi:10.1039/C5cc03944d

data_7117478
_publ_section_title
;
 Bi- and trimetallic rare-earth-palladium complexes ligated by
 phosphinoamides
;
_journal_name_full               Chem.Commun.
_journal_page_first              11761
_journal_paper_doi               10.1039/C5cc03944d
_journal_volume                  51
_journal_year                    2015
_chemical_formula_moiety         'C108 H92 Lu N6 P6 Pd2, C16 H32 Li O4'
_chemical_formula_sum            'C124 H124 Li Lu N6 O4 P6 Pd2'
_chemical_formula_weight         2342.81
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2015-03-20
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-05-12 deposited with the CCDC.
2015-06-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.9840(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   28.3174(4)
_cell_length_b                   14.5610(2)
_cell_length_c                   29.0288(5)
_cell_measurement_reflns_used    100833
_cell_measurement_temperature    200
_cell_measurement_theta_max      27.19
_cell_measurement_theta_min      1.40
_cell_volume                     11506.7(3)
_computing_cell_refinement       'STOE X-AREA, PLATON (A.L.Spek, 2009)'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED & LANA, PLATON (A.L.Spek, 2009)'
_computing_molecular_graphics    'Diamond 2/3, Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'MS Word, Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200
_diffrn_detector                 'image plate (34cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            'STOE image plate'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'two-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_collimation    '0.5mm monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0841
_diffrn_reflns_av_unetI/netI     0.0463
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            144868
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.771
_diffrn_reflns_theta_min         1.445
_diffrn_source                   'sealed tube, 12x0.4mm long-fine focus'
_exptl_absorpt_coefficient_mu    1.298
_exptl_absorpt_correction_T_max  0.8359
_exptl_absorpt_correction_T_min  0.4874
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE X-RED & X-SHAPE'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.352
_exptl_crystal_density_meas      .
_exptl_crystal_description       prism
_exptl_crystal_F_000             4792
_exptl_crystal_size_max          0.77
_exptl_crystal_size_mid          0.378
_exptl_crystal_size_min          0.158
_refine_diff_density_max         1.221
_refine_diff_density_min         -0.875
_refine_diff_density_rms         0.102
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1464
_refine_ls_number_reflns         24417
_refine_ls_number_restraints     205
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0682
_refine_ls_R_factor_gt           0.0520
_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^)+(0.1020P)^2^+3.8587P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1509
_refine_ls_wR_factor_ref         0.1606
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                19305
_reflns_number_total             24417
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5cc03944d2.cif
_cod_data_source_block           fv09bm
_cod_database_code               7117478
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups, All N(H,H) groups
2. Restrained distances
 Li1B-O4B
 2 with sigma of 0.02
 O4A-Li1A
 2 with sigma of 0.02
 Li1B-Li1A
 2 with sigma of 0.02
 Li1B-O2B
 2 with sigma of 0.02
 O1B-Li1B
 2 with sigma of 0.02
 O3B-Li1B
 2 with sigma of 0.02
 O2A-Li1A
 1.9 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C41A) \\sim Ueq, Uanis(C40A) \\sim Ueq, Uanis(C39A) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C207) \\sim Ueq, Uanis(C206) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C67B) \\sim Ueq, Uanis(C72B) \\sim Ueq, Uanis(C71B) \\sim Ueq,
Uanis(C70B) \\sim Ueq, Uanis(C69B) \\sim Ueq, Uanis(C68B) \\sim Ueq,
Uanis(C61B) \\sim Ueq, Uanis(C66B) \\sim Ueq, Uanis(C65B) \\sim Ueq,
Uanis(C64B) \\sim Ueq, Uanis(C63B) \\sim Ueq, Uanis(C62B) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(N6) \\sim Ueq, Uanis(C96B) \\sim Ueq, Uanis(C96A) \\sim Ueq, Uanis(C92B)
\\sim Ueq, Uanis(C92A) \\sim Ueq, Uanis(C93A) \\sim Ueq, Uanis(C93B) \\sim Ueq,
Uanis(C94A) \\sim Ueq, Uanis(C95B) \\sim Ueq, Uanis(C94B) \\sim Ueq,
Uanis(C95A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C80) \\sim Ueq, Uanis(C81) \\sim Ueq, Uanis(C82) \\sim Ueq, Uanis(C83)
\\sim Ueq, Uanis(C84) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uiso(Li1B) = Uiso(Li1A)
Uiso(O4A) = Uiso(O4B)
Uiso(C124) = Uiso(C223)
Uiso(C122) = Uiso(C222)
Uiso(C121) = Uiso(C221)
4. Others
 Fixed Sof: C19B(0.5) C20B(0.5) H20B(0.5) C21B(0.5) H21B(0.5) C22B(0.5)
 H22B(0.5) C23B(0.5) H23B(0.5) C24B(0.5) H24B(0.5) C37B(0.5) C38B(0.5)
 H38B(0.5) C39B(0.5) H39B(0.5) C40B(0.5) H40B(0.5) C41B(0.5) H41B(0.5)
 C42B(0.5) H42B(0.5) C55B(0.5) C60B(0.5) H60B(0.5) C59B(0.5) H59B(0.5)
 C58B(0.5) H58B(0.5) C57B(0.5) H57B(0.5) C56B(0.5) H56B(0.5) C67B(0.5)
 C72B(0.5) H72B(0.5) C71B(0.5) H71B(0.5) C70B(0.5) H70B(0.5) C69B(0.5)
 H69B(0.5) C68B(0.5) H68B(0.5) C61B(0.5) C66B(0.5) H66B(0.5) C65B(0.5)
 H65B(0.5) C64B(0.5) H64B(0.5) C63B(0.5) H63B(0.5) C62B(0.5) H62B(0.5)
 C91A(0.5) C92A(0.5) H92A(0.5) C93A(0.5) H93A(0.5) C94A(0.5) H94A(0.5)
 C95A(0.5) H95A(0.5) C96A(0.5) H96A(0.5) C203(0.5) C204(0.5) H204(0.5)
 C205(0.5) H205(0.5) C206(0.5) H206(0.5) C207(0.5) H207(0.5) C208(0.5)
 H208(0.5) C37A(0.5) C42A(0.5) H42A(0.5) C41A(0.5) H41A(0.5) C40A(0.5)
 H40A(0.5) C39A(0.5) H39A(0.5) C38A(0.5) H38A(0.5) C67A(0.5) C72A(0.5)
 H72A(0.5) C71A(0.5) H71A(0.5) C70A(0.5) H70A(0.5) C69A(0.5) H69A(0.5)
 C68A(0.5) H68A(0.5) C19A(0.5) C24A(0.5) H24A(0.5) C23A(0.5) H23A(0.5)
 C22A(0.5) H22A(0.5) C21A(0.5) H21A(0.5) C20A(0.5) H20A(0.5) C61A(0.5)
 C66A(0.5) H66A(0.5) C65A(0.5) H65A(0.5) C64A(0.5) H64A(0.5) C63A(0.5)
 H63A(0.5) C62A(0.5) H62A(0.5) C55A(0.5) C60A(0.5) H60A(0.5) C59A(0.5)
 H59A(0.5) C58A(0.5) H58A(0.5) C57A(0.5) H57A(0.5) C56A(0.5) H56A(0.5)
 C103(0.5) C108(0.5) H108(0.5) C107(0.5) H107(0.5) C106(0.5) H106(0.5)
 C105(0.5) H105(0.5) C104(0.5) H104(0.5) Li1A(0.5) H6a(0.5) H6b(0.5) C91B(0.5)
 C92B(0.5) H92B(0.5) C93B(0.5) H93B(0.5) C94B(0.5) H94B(0.5) C95B(0.5)
 H95B(0.5) C96B(0.5) H96B(0.5) O1A(0.5) C109(0.5) H10a(0.5) H10b(0.5) C110(0.5)
 H11a(0.5) H11b(0.5) C111(0.5) H11c(0.5) H11d(0.5) C112(0.5) H11e(0.5)
 H11f(0.5) O2A(0.5) C113(0.5) H11g(0.5) H11h(0.5) C114(0.5) H11i(0.5) H11j(0.5)
 C115(0.5) H11k(0.5) H11l(0.5) C116(0.5) H11m(0.5) H11n(0.5) O3A(0.5) C117(0.5)
 H11o(0.5) H11p(0.5) C118(0.5) H11q(0.5) H11r(0.5) C119(0.5) H11s(0.5)
 H11t(0.5) C120(0.5) H12a(0.5) H12b(0.5) Li1B(0.5) O4A(0.5) C123(0.5) H12c(0.5)
 H12d(0.5) C124(0.5) H12e(0.5) H12f(0.5) C122(0.5) H12g(0.5) H12h(0.5)
 C121(0.5) H12i(0.5) H12j(0.5) O1B(0.5) C209(0.5) H20c(0.5) H20d(0.5) C210(0.5)
 H21c(0.5) H21d(0.5) C211(0.5) H21e(0.5) H21f(0.5) C212(0.5) H21g(0.5)
 H21h(0.5) O2B(0.5) C213(0.5) H21i(0.5) H21j(0.5) C214(0.5) H21k(0.5) H21l(0.5)
 C215(0.5) H21m(0.5) H21n(0.5) C216(0.5) H21o(0.5) H21p(0.5) O3B(0.5) C217(0.5)
 H21q(0.5) H21r(0.5) C218(0.5) H21s(0.5) H21t(0.5) C219(0.5) H21u(0.5)
 H21v(0.5) C220(0.5) H22c(0.5) H22d(0.5) O4B(0.5) C221(0.5) H22e(0.5) H22f(0.5)
 C222(0.5) H22g(0.5) H22h(0.5) C223(0.5) H22i(0.5) H22j(0.5) C224(0.5)
 H22k(0.5) H22l(0.5)
 Fixed Uiso: C123(0.25) C224(0.25)
5.a Riding coordinates:
 N5(H5), N6(H6b)
5.b Free rotating group:
 O1A(C109,C110,C111,C112), O2A(C113,C114,C115,C116), O3A(C117,C118,C119,C120,
 Li1B), O4A(C123,C124,C122,C121), O1B(C209,C210,C211,C212), O2B(C213,C214,C215,
 C216), O3B(C217,C218,C219,C220), O4B(C221,C222,C223,C224)
5.c Secondary CH2 refined with riding coordinates:
 C109(H10a,H10b), C110(H11a,H11b), C111(H11c,H11d), C112(H11e,H11f), C113(H11g,
 H11h), C114(H11i,H11j), C115(H11k,H11l), C116(H11m,H11n), C117(H11o,H11p),
 C118(H11q,H11r), C119(H11s,H11t), C120(H12a,H12b), C123(H12c,H12d), C124(H12e,
 H12f), C122(H12g,H12h), C121(H12i,H12j), C209(H20c,H20d), C210(H21c,H21d),
 C211(H21e,H21f), C212(H21g,H21h), C213(H21i,H21j), C214(H21k,H21l), C215(H21m,
 H21n), C216(H21o,H21p), C217(H21q,H21r), C218(H21s,H21t), C219(H21u,H21v),
 C220(H22c,H22d), C221(H22e,H22f), C222(H22g,H22h), C223(H22i,H22j), C224(H22k,
 H22l)
5.d Aromatic/amide H refined with riding coordinates:
 C50(H50), C51(H51), C52(H52), C53(H53), C54(H54), C2(H2), C3(H3), C4(H4),
 C5(H5a), C6(H6), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30), C8(H8),
 C9(H9), C10(H10), C11(H11), C12(H12), C14(H14), C15(H15), C16(H16), C17(H17),
 C18(H18), C20B(H20B), C21B(H21B), C22B(H22B), C23B(H23B), C24B(H24B), C32(H32),
  C33(H33), C34(H34), C35(H35), C36(H36), C38B(H38B), C39B(H39B), C40B(H40B),
 C41B(H41B), C42B(H42B), C44(H44), C45(H45), C46(H46), C47(H47), C48(H48),
 C60B(H60B), C59B(H59B), C58B(H58B), C57B(H57B), C56B(H56B), C72B(H72B),
 C71B(H71B), C70B(H70B), C69B(H69B), C68B(H68B), C66B(H66B), C65B(H65B),
 C64B(H64B), C63B(H63B), C62B(H62B), C74(H74), C75(H75), C76(H76), C77(H77),
 C78(H78), C86(H86), C87(H87), C88(H88), C89(H89), C90(H90), C92A(H92A),
 C93A(H93A), C94A(H94A), C95A(H95A), C96A(H96A), C98(H98), C99(H99), C100(H100),
  C101(H101), C102(H102), C204(H204), C205(H205), C206(H206), C207(H207),
 C208(H208), C42A(H42A), C41A(H41A), C40A(H40A), C39A(H39A), C38A(H38A),
 C72A(H72A), C71A(H71A), C70A(H70A), C69A(H69A), C68A(H68A), C24A(H24A),
 C23A(H23A), C22A(H22A), C21A(H21A), C20A(H20A), C66A(H66A), C65A(H65A),
 C64A(H64A), C63A(H63A), C62A(H62A), C60A(H60A), C59A(H59A), C58A(H58A),
 C57A(H57A), C56A(H56A), C108(H108), C107(H107), C106(H106), C105(H105),
 C104(H104), N6(H6a), C92B(H92B), C93B(H93B), C94B(H94B), C95B(H95B),
 C96B(H96B), C80(H80), C81(H81), C82(H82), C83(H83), C84(H84)
5.e Fitted hexagon refined as free rotating group:
 C19B(C20B,C21B,C22B,C23B,C24B), C55B(C60B,C59B,C58B,C57B,C56B), C67B(C72B,
 C71B,C70B,C69B,C68B), C61B(C66B,C65B,C64B,C63B,C62B), C91A(C92A,C93A,C94A,C95A,
 C96A), C203(C204,C205,C206,C207,C208), C103(C108,C107,C106,C105,C104),
 C91B(C92B,C93B,C94B,C95B,C96B), C79(C80,C81,C82,C83,C84)
;
_shelx_res_checksum              1358
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'