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_7117473
_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         'C88 H93 Cl Li N4 O4 P4 Pd Y, 2(C4 H8 O)'
_chemical_formula_sum            'C96 H109 Cl Li N4 O6 P4 Pd Y'
_chemical_formula_weight         1776.45
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2015-03-11
_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                99.348(6)
_cell_angle_beta                 98.546(6)
_cell_angle_gamma                99.455(5)
_cell_formula_units_Z            2
_cell_length_a                   13.4049(9)
_cell_length_b                   15.2317(9)
_cell_length_c                   22.790(2)
_cell_measurement_reflns_used    18069
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      28.58
_cell_measurement_theta_min      1.51
_cell_volume                     4455.0(6)
_computing_cell_refinement       'STOE X-AREA, PLATON (A.L.Spek, 2005)'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED, PLATON (A.L.Spek, 2005)'
_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, 2014)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_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 0.983
_diffrn_measured_fraction_theta_max 0.994
_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  0.0719
_diffrn_reflns_av_unetI/netI     0.1155
_diffrn_reflns_laue_measured_fraction_full 0.983
_diffrn_reflns_laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            38213
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.148
_diffrn_reflns_theta_min         1.506
_diffrn_source                   'sealed tube, 12x0.4mm long-fine focus'
_exptl_absorpt_coefficient_mu    1.007
_exptl_absorpt_correction_T_max  0.9173
_exptl_absorpt_correction_T_min  0.8527
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE X-RED & X-SHAPE'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.324
_exptl_crystal_description       prism
_exptl_crystal_F_000             1852
_exptl_crystal_size_max          0.172
_exptl_crystal_size_mid          0.124
_exptl_crystal_size_min          0.089
_refine_diff_density_max         0.955
_refine_diff_density_min         -0.383
_refine_diff_density_rms         0.073
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.892
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1067
_refine_ls_number_reflns         15855
_refine_ls_number_restraints     110
_refine_ls_restrained_S_all      0.892
_refine_ls_R_factor_all          0.1024
_refine_ls_R_factor_gt           0.0536
_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^)+(0.0448P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0996
_refine_ls_wR_factor_ref         0.1122
_reflns_Friedel_coverage         0.000
_reflns_friedel_fraction_full    .
_reflns_friedel_fraction_max     .
_reflns_number_gt                9720
_reflns_number_total             15855
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5cc03944d2.cif
_cod_data_source_block           1a
_cod_database_code               7117473
_shelxl_version_number           2013-2
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All N(H) groups
2. Rigid bond restraints
 C79, C80B, C77B, C78B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C79 \\sim C80B \\sim C77B \\sim C78B: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08
Uanis(C81B) \\sim Ueq, Uanis(C84B) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(C88B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C78A) \\sim Ueq, Uanis(C77A) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(C80B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O3B) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C86A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C88A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C85A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C86B) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C82) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C87A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Same fragment restrains
{O6, C1J, C1I, C1H, C1K} sigma for 1-2: 0.02, 1-3: 0.02
as
{O5, C89, C90, C91, C92}
5. Others
 Fixed Sof: H79C(0.5) H79D(0.5) H79A(0.5) H79B(0.5) H83A(0.5) H83B(0.5)
 H83C(0.5) H83D(0.5) O3A(0.5) C77A(0.5) H77A(0.5) H77B(0.5) C78A(0.5) H78A(0.5)
 H78B(0.5) C80B(0.5) H80A(0.5) H80B(0.5) C81A(0.5) H81A(0.5) H81B(0.5)
 H82A(0.5) H82B(0.5) H82C(0.5) H82D(0.5) C84A(0.5) H84A(0.5) H84B(0.5)
 C85A(0.5) H85A(0.5) H85B(0.5) C86A(0.5) H86A(0.5) H86B(0.5) C87A(0.5)
 H87A(0.5) H87B(0.5) C88A(0.5) H88A(0.5) H88B(0.5) O3B(0.5) C77B(0.5) H77C(0.5)
 H77D(0.5) C78B(0.5) H78C(0.5) H78D(0.5) C80A(0.5) H80C(0.5) H80D(0.5)
 C81B(0.5) H81C(0.5) H81D(0.5) C84B(0.5) H84C(0.5) H84D(0.5) C85B(0.5)
 H85C(0.5) H85D(0.5) C86B(0.5) H86C(0.5) H86D(0.5) C87B(0.5) H87C(0.5)
 H87D(0.5) C88B(0.5) H88C(0.5) H88D(0.5)
6.a Riding coordinates:
 N4(H4)
6.b Secondary CH2 refined with riding coordinates:
 C73(H73A,H73B), C74(H74A,H74B), C75(H75A,H75B), C76(H76A,H76B), C79(H79C,
 H79D), C79(H79A,H79B), C83(H83A,H83B), C83(H83C,H83D), C77A(H77A,H77B),
 C78A(H78A,H78B), C80B(H80A,H80B), C81A(H81A,H81B), C82(H82A,H82B), C82(H82C,
 H82D), C84A(H84A,H84B), C85A(H85A,H85B), C86A(H86A,H86B), C87A(H87A,H87B),
 C88A(H88A,H88B), C77B(H77C,H77D), C78B(H78C,H78D), C80A(H80C,H80D), C81B(H81C,
 H81D), C84B(H84C,H84D), C85B(H85C,H85D), C86B(H86C,H86D), C87B(H87C,H87D),
 C88B(H88C,H88D), C89(H89A,H89B), C90(H90A,H90B), C91(H91A,H91B), C92(H92A,
 H92B), C1J(H1JA,H1JB), C1I(H1IA,H1IB), C1H(H1HA,H1HB), C1K(H1KA,H1KB)
6.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4A), 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), C38(H38), C39(H39),
  C40(H40), C41(H41), C42(H42), C44(H44), C45(H45), C46(H46), C47(H47),
 C48(H48), C50(H50), C51(H51), C52(H52), C53(H53), C54(H54), C56(H56), C57(H57),
  C58(H58), C59(H59), C60(H60), C62A(H62A), C63A(H63A), C64B(H64B), C65A(H65A),
 C66A(H66A), C68(H68), C69(H69), C70(H70), C71(H71), C72(H72)
;
_shelx_res_checksum              66906
_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'
_olex2_submission_special_instructions 'No special instructions were received'