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_7117475
_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
'C76 H69 Cl Lu N4 O P4 Pd, C16 H32 Li O4, C4 H8 O'
_chemical_formula_sum            'C96 H109 Cl Li Lu N4 O6 P4 Pd'
_chemical_formula_weight         1862.51
_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                88.53(3)
_cell_angle_beta                 80.90(3)
_cell_angle_gamma                83.96(3)
_cell_formula_units_Z            2
_cell_length_a                   13.332(3)
_cell_length_b                   15.349(3)
_cell_length_c                   21.771(4)
_cell_measurement_reflns_used    58579
_cell_measurement_temperature    150
_cell_measurement_theta_max      29.56
_cell_measurement_theta_min      1.63
_cell_volume                     4374.4(16)
_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      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 0.996
_diffrn_measured_fraction_theta_max 0.992
_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  0.0395
_diffrn_reflns_av_unetI/netI     0.0370
_diffrn_reflns_laue_measured_fraction_full 0.996
_diffrn_reflns_laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            36650
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.517
_diffrn_reflns_theta_min         1.629
_diffrn_source                   'sealed tube, 12x0.4mm long-fine focus'
_exptl_absorpt_coefficient_mu    1.49
_exptl_absorpt_correction_T_max  0.8934
_exptl_absorpt_correction_T_min  0.6493
_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    1.414
_exptl_crystal_description       prism
_exptl_crystal_F_000             1916
_exptl_crystal_size_max          0.275
_exptl_crystal_size_mid          0.203
_exptl_crystal_size_min          0.079
_refine_diff_density_max         1.392
_refine_diff_density_min         -1.368
_refine_diff_density_rms         0.097
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1026
_refine_ls_number_reflns         16187
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0422
_refine_ls_R_factor_gt           0.0358
_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^)+(0.0672P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0933
_refine_ls_wR_factor_ref         0.0960
_reflns_Friedel_coverage         0.000
_reflns_friedel_fraction_full    .
_reflns_friedel_fraction_max     .
_reflns_number_gt                14119
_reflns_number_total             16187
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5cc03944d2.cif
_cod_data_source_block           1b`
_cod_original_cell_volume        4374.2(16)
_cod_database_code               7117475
_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. Restrained distances
 C95-C94
 1.47 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C82) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C80B) \\sim Ueq, Uanis(C78A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Others
 Fixed Sof: H95C(0.5) H95D(0.5) H95A(0.5) H95B(0.5) C96B(0.5) H96A(0.5)
 H96B(0.5) C96A(0.5) H96C(0.5) H96D(0.5)
5.a Riding coordinates:
 N4(H4)
5.b Secondary CH2 refined with riding coordinates:
 C73(H73A,H73B), C74(H74A,H74B), C75(H75A,H75B), C76(H76A,H76B), C81(H81A,
 H81B), C82(H82A,H82B), C83(H83A,H83B), C84(H84A,H84B), C85(H85A,H85B),
 C86(H86A,H86B), C87(H87A,H87B), C88(H88A,H88B), C89(H89A,H89B), C90(H90A,H90B),
  C91(H91A,H91B), C92(H92A,H92B), C77A(H77A,H77B), C78A(H78A,H78B), C79A(H79A,
 H79B), C80B(H80A,H80B), C93(H93A,H93B), C94(H94A,H94B), C95(H95C,H95D),
 C95(H95A,H95B), C96B(H96A,H96B), C96A(H96C,H96D)
5.c Aromatic/amide H refined with riding coordinates:
 C0AA(H0AA), C1AA(H1AA), C2AA(H2AA), C3AA(H3AA), C4(H4A), C4AA(H4AA), C8(H8),
 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), C62(H62), C63(H63),
 C64(H64), C65(H65), C66(H66), C68(H68), C69(H69), C70(H70), C71(H71), C72(H72)
;
_shelx_res_checksum              72269
_olex2_submission_special_instructions 'No special instructions were received'