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_7117477
_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 N6 P6 Pd2 Y, C16 H32 Li O4'
_chemical_formula_sum            'C124 H124 Li N6 O4 P6 Pd2 Y'
_chemical_formula_weight         2256.75
_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             2015-05-05
_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                 106.14(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   28.427(6)
_cell_length_b                   14.576(3)
_cell_length_c                   29.040(6)
_cell_measurement_reflns_used    32017
_cell_measurement_temperature    150
_cell_measurement_theta_max      25.13
_cell_measurement_theta_min      1.44
_cell_volume                     11559(5)
_computing_cell_refinement       'STOE X-AREA, PLATON (A.L.Spek, 2009)'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED & X-SHAPE, 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      150
_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 IPDS2'
_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  0.1160
_diffrn_reflns_av_unetI/netI     0.1144
_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       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            93327
_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         26.768
_diffrn_reflns_theta_min         1.443
_diffrn_source                   'sealed tube, 12x0.4mm long-fine focus'
_exptl_absorpt_coefficient_mu    0.942
_exptl_absorpt_correction_T_max  0.9489
_exptl_absorpt_correction_T_min  0.7768
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE X-RED & X-SHAPE'
_exptl_crystal_colour            'yellowish green'
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.297
_exptl_crystal_density_meas      .
_exptl_crystal_description       prism
_exptl_crystal_F_000             4664
_exptl_crystal_size_max          0.307
_exptl_crystal_size_mid          0.223
_exptl_crystal_size_min          0.063
_refine_diff_density_max         1.123
_refine_diff_density_min         -0.682
_refine_diff_density_rms         0.093
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.957
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1399
_refine_ls_number_reflns         24548
_refine_ls_number_restraints     357
_refine_ls_restrained_S_all      0.955
_refine_ls_R_factor_all          0.1540
_refine_ls_R_factor_gt           0.0752
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0886P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1614
_refine_ls_wR_factor_ref         0.1939
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                12407
_reflns_number_total             24548
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5cc03944d2.cif
_cod_data_source_block           2a
_cod_original_cell_volume        11559(4)
_cod_database_code               7117477
_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
 Li1B-O4B
 2 with sigma of 0.02
 O4A-Li1A
 2 with sigma of 0.02
 Li1B-Li1A
 2 with sigma of 0.02
3. Rigid bond restraints
 C37B, C38B, C39B, C40B, C41B, C42B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Uiso/Uaniso restraints and constraints
C80B \\sim C81B \\sim C82B \\sim C83B \\sim C84B: within 1.7A with sigma of
0.01 and sigma for terminal atoms of 0.02
C79A \\sim C79B: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
C80A \\sim C80B: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
C81A \\sim C81B: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
C82A \\sim C82B: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
C83A \\sim C83B: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
C84A \\sim C84B: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
C19A \\sim C19B: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
C20A \\sim C20B: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
C21A \\sim C21B: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
C22A \\sim C22B: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
C23A \\sim C23B: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
C24A \\sim C24B: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
C2 \\sim C3 \\sim C4 \\sim C5: within 1.7A with sigma of 0.01 and sigma for
terminal atoms of 0.02
C32 \\sim C33 \\sim C34: within 1.7A with sigma of 0.02 and sigma for terminal
atoms of 0.04
C55A \\sim C55B: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
C56A \\sim C56B: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
C57B \\sim C57A: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
C58B \\sim C58A: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
C59B \\sim C59A: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
C60B \\sim C60A: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
C61A \\sim C61B: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
C62A \\sim C62B: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
C63A \\sim C63B: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
C64A \\sim C64B: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
C65A \\sim C65B: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
C66A \\sim C66B: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
C67A \\sim C67B: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.04
C68A \\sim C68B: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.04
C69A \\sim C69B: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.04
C70A \\sim C70B: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C71A \\sim C71B: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C72A \\sim C72B: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C103 \\sim C104 \\sim C105 \\sim C106 \\sim C107 \\sim C108: within 1.7A with
sigma of 0.01 and sigma for terminal atoms of 0.02
C37B \\sim C37A: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.04
C42B \\sim C42A: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.04
C41B \\sim C41A: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.04
C40B \\sim C40A: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.04
C39B \\sim C39A: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.04
C38B \\sim C38A: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.04
C67B \\sim C68B \\sim C69B \\sim C70B \\sim C71B \\sim C72B: within 1.7A with
sigma of 0.04 and sigma for terminal atoms of 0.08
Uiso(C221) = Uiso(C121)
Uiso(C122) = Uiso(C222)
Uiso(C224) = Uiso(C123)
Uiso(C223) = Uiso(C124)
Uiso(O4A) = Uiso(O4B)
Uiso(Li1B) = Uiso(Li1A)
5. Others
 Fixed Sof: 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) 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) C55A(0.5) C56A(0.5) H56A(0.5) C57B(0.5) H57B(0.5)
 C58B(0.5) H58B(0.5) C59B(0.5) H59B(0.5) C60B(0.5) H60B(0.5) C61A(0.5)
 C62A(0.5) H62A(0.5) C63A(0.5) H63A(0.5) C64A(0.5) H64A(0.5) C65A(0.5)
 H65A(0.5) C66A(0.5) H66A(0.5) C67A(0.5) C68A(0.5) H68A(0.5) C69A(0.5)
 H69A(0.5) C70A(0.5) H70A(0.5) C71A(0.5) H71A(0.5) C72A(0.5) H72A(0.5)
 C79A(0.5) C80A(0.5) H80A(0.5) C81A(0.5) H81A(0.5) C82A(0.5) H82A(0.5)
 C83A(0.5) H83A(0.5) C84A(0.5) H84A(0.5) C19B(0.5) C24B(0.5) H24B(0.5)
 C23B(0.5) H23B(0.5) C22B(0.5) H22B(0.5) C21B(0.5) H21B(0.5) C20B(0.5)
 H20B(0.5) C37A(0.5) C38A(0.5) H38A(0.5) C39A(0.5) H39A(0.5) C40A(0.5)
 H40A(0.5) C41A(0.5) H41A(0.5) C42A(0.5) H42A(0.5) C55B(0.5) C56B(0.5)
 H56B(0.5) C57A(0.5) H57A(0.5) C58A(0.5) H58A(0.5) C59A(0.5) H59A(0.5)
 C60A(0.5) H60A(0.5) C61B(0.5) C62B(0.5) H62B(0.5) C63B(0.5) H63B(0.5)
 C64B(0.5) H64B(0.5) C65B(0.5) H65B(0.5) C66B(0.5) H66B(0.5) C67B(0.5)
 C68B(0.5) H68B(0.5) C69B(0.5) H69B(0.5) C70B(0.5) H70B(0.5) C71B(0.5)
 H71B(0.5) C72B(0.5) H72B(0.5) C79B(0.5) C80B(0.5) H80B(0.5) C81B(0.5)
 H81B(0.5) C82B(0.5) H82B(0.5) C83B(0.5) H83B(0.5) C84B(0.5) H84B(0.5)
 Li1A(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) 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)
 Li1B(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)
6.a Riding coordinates:
 N5(H5), N6(H6)
6.b Free rotating group:
 O1A(C109,C110,C111,C112), O2A(C113,C114,C115,C116), O3A(C117,C118,C119,C120),
 O4A(C123,C124,C122,C121,Li1B), O1B(C209,C210,C211,C212), O2B(C213,C214,C215,
 C216), O3B(C217,C218,C219,C220), O4B(C221,C222,C223,C224)
6.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)
6.d Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5A), C6(H6A), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C26(H26), C27(H27),
  C28(H28), C29(H29), C30(H30), C32(H32), C33(H33), C34(H34), C35(H35),
 C36(H36), C44(H44), C45(H45), C46(H46), C47(H47), C48(H48), C50(H50), C51(H51),
  C52(H52), C53(H53), C54(H54), C74(H74), C75(H75), C76(H76), C77(H77),
 C78(H78), C86(H86), C87(H87), C88(H88), C89(H89), C90(H90), C92(H92), C93(H93),
  C94(H94), C95(H95), C96(H96), C98(H98), C99(H99), C100(H100), C101(H101),
 C102(H102), C104(H104), C105(H105), C106(H106), C107(H107), C108(H108),
 C24A(H24A), C23A(H23A), C22A(H22A), C21A(H21A), C20A(H20A), C38B(H38B),
 C39B(H39B), C40B(H40B), C41B(H41B), C42B(H42B), C56A(H56A), C57B(H57B),
 C58B(H58B), C59B(H59B), C60B(H60B), C62A(H62A), C63A(H63A), C64A(H64A),
 C65A(H65A), C66A(H66A), C68A(H68A), C69A(H69A), C70A(H70A), C71A(H71A),
 C72A(H72A), C80A(H80A), C81A(H81A), C82A(H82A), C83A(H83A), C84A(H84A),
 C24B(H24B), C23B(H23B), C22B(H22B), C21B(H21B), C20B(H20B), C38A(H38A),
 C39A(H39A), C40A(H40A), C41A(H41A), C42A(H42A), C56B(H56B), C57A(H57A),
 C58A(H58A), C59A(H59A), C60A(H60A), C62B(H62B), C63B(H63B), C64B(H64B),
 C65B(H65B), C66B(H66B), C68B(H68B), C69B(H69B), C70B(H70B), C71B(H71B),
 C72B(H72B), C80B(H80B), C81B(H81B), C82B(H82B), C83B(H83B), C84B(H84B)
6.e Fitted hexagon refined as free rotating group:
 C19A(C24A,C23A,C22A,C21A,C20A), C55A(C56A,C57B,C58B,C59B,C60B), C61A(C62A,
 C63A,C64A,C65A,C66A), C67A(C68A,C69A,C70A,C71A,C72A), C79A(C80A,C81A,C82A,C83A,
 C84A), C19B(C24B,C23B,C22B,C21B,C20B), C55B(C56B,C57A,C58A,C59A,C60A),
 C61B(C62B,C63B,C64B,C65B,C66B), C67B(C68B,C69B,C70B,C71B,C72B), C79B(C80B,C81B,
 C82B,C83B,C84B)
;
_shelx_res_checksum              67950
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'