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_7117476
_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         'C90.4 H97.8 Cl Li Lu N4 O4.6 P4 Pd, C4 H8 O'
_chemical_formula_sum            'C94.4 H105.8 Cl Li Lu N4 O5.6 P4 Pd'
_chemical_formula_weight         1833.66
_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   geom
_atom_sites_solution_primary     heavy
_audit_creation_date             2015-02-25
_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                88.38(3)
_cell_angle_beta                 80.40(3)
_cell_angle_gamma                84.17(3)
_cell_formula_units_Z            2
_cell_length_a                   13.414(3)
_cell_length_b                   15.386(3)
_cell_length_c                   22.048(4)
_cell_measurement_reflns_used    9426
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.20
_cell_measurement_theta_min      1.62
_cell_volume                     4463.2(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      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 0.971
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measurement_details
;
 185 frames, detector distance = 100 mm
;
_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_polarisn_norm  0
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1767
_diffrn_reflns_av_unetI/netI     0.3488
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 0.952
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            43644
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.952
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.185
_diffrn_reflns_theta_min         1.618
_diffrn_source                   'sealed tube, 12x0.4mm long-fine focus'
_diffrn_source_current           40
_diffrn_source_power             2.00
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    1.456
_exptl_absorpt_correction_T_max  0.9235
_exptl_absorpt_correction_T_min  0.7764
_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    1.364
_exptl_crystal_description       prism
_exptl_crystal_F_000             1884
_exptl_crystal_size_max          0.242
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.052
_refine_diff_density_max         0.895
_refine_diff_density_min         -0.985
_refine_diff_density_rms         0.138
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.831
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1078
_refine_ls_number_reflns         23041
_refine_ls_number_restraints     280
_refine_ls_restrained_S_all      0.829
_refine_ls_R_factor_all          0.2260
_refine_ls_R_factor_gt           0.0855
_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^)]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1100
_refine_ls_wR_factor_ref         0.1476
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8384
_reflns_number_total             23041
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5cc03944d2.cif
_cod_data_source_block           1b1b`
_cod_original_formula_sum        'C94.40 H105.80 Cl Li Lu N4 O5.60 P4 Pd'
_cod_database_code               7117476
_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
 1.25 with sigma of 0.02
 C83A-C82A
 1.45 with sigma of 0.02
 C94-C95
 1.3 with sigma of 0.02
 O2-C77
 1.4 with sigma of 0.02
 O2-C80
 1.4 with sigma of 0.02
 O3-C84A
 1.4 with sigma of 0.02
 O3-C81A
 1.4 with sigma of 0.02
 C77-C80
 2.2 with sigma of 0.04
3. Rigid bond restraints
 O4A, C85A, C87A, C88A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C86, O4B, C87B, C88B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C89B, C90B, C91B, C92B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O3, C81A, C84A, C83A, C82A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O2, C80, C77, C78, C79
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C81B, C82B, C83B, C84B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C91B \\sim C92B: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
Uanis(Li1B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Li4) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C85A) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C88A) \\sim Ueq: with sigma of 0.0001 and sigma for terminal atoms of
0.0002
Uanis(C87A) \\sim Ueq: with sigma of 0.00001 and sigma for terminal atoms of
0.00002
Uanis(O2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C85B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O4B) \\sim Ueq, Uanis(C88B) \\sim Ueq, Uanis(C87B) \\sim Ueq, Uanis(C86)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C58) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C90B) \\sim Ueq, Uanis(C89B) \\sim Ueq, Uanis(C91B) \\sim Ueq: with sigma
of 0.001 and sigma for terminal atoms of 0.002
Uanis(C92B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O5B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O3) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C84A) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C83A) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C82A) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C81A) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C84B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C83B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C82B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C81B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C77) \\sim Ueq, Uanis(C78) \\sim Ueq, Uanis(C79) \\sim Ueq, Uanis(C80)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
5. Same fragment restrains
{O4B, C88B, C87B, C86, C85B} sigma for 1-2: 0.02, 1-3: 0.02
as
{O1, C76, C75, C74, C73}
{O3, C84B, C83B, C82B, C81B, C81A, C84A, C83A, C82A} sigma for 1-2: 0.02, 1-3:
0.02
as
{O6, C93, C94, C95, C96, C80, C77, C78, C79}
6. Others
 Fixed Sof: C84B(0.6) H84A(0.6) H84B(0.6) C83B(0.6) H83A(0.6) H83B(0.6)
 C82B(0.6) H82A(0.6) H82B(0.6) C81B(0.6) H81A(0.6) H81B(0.6) C81A(0.4)
 H81C(0.4) H81D(0.4) C84A(0.4) H84C(0.4) H84D(0.4) C83A(0.4) H83C(0.4)
 H83D(0.4) C82A(0.4) H82C(0.4) H82D(0.4) O5B(0.6) C89B(0.6) H89A(0.6) H89B(0.6)
 C90B(0.6) H90A(0.6) H90B(0.6) C91B(0.6) H91A(0.6) H91B(0.6) C92B(0.6)
 H92A(0.6) H92B(0.6) O4A(0.4) C85A(0.4) H85A(0.4) H85B(0.4) O4B(0.6) C88B(0.6)
 H88A(0.6) H88B(0.6) C87B(0.6) H87A(0.6) H87B(0.6) H86A(0.4) H86B(0.4)
 H86C(0.6) H86D(0.6) C85B(0.6) H85C(0.6) H85D(0.6) C87A(0.4) H87C(0.4)
 H87D(0.4) C88A(0.4) H88C(0.4) H88D(0.4) Li4(0.4) Li1B(0.6)
7.a Secondary CH2 refined with riding coordinates:
 C76(H76A,H76B), C75(H75A,H75B), C74(H74A,H74B), C73(H73A,H73B), C84B(H84A,
 H84B), C83B(H83A,H83B), C82B(H82A,H82B), C81B(H81A,H81B), C81A(H81C,H81D),
 C84A(H84C,H84D), C83A(H83C,H83D), C82A(H82C,H82D), C89B(H89A,H89B), C90B(H90A,
 H90B), C91B(H91A,H91B), C92B(H92A,H92B), C85A(H85A,H85B), C88B(H88A,H88B),
 C87B(H87A,H87B), C86(H86A,H86B), C86(H86C,H86D), C85B(H85C,H85D), C87A(H87C,
 H87D), C88A(H88C,H88D), C93(H93A,H93B), C94(H94A,H94B), C95(H95A,H95B),
 C96(H96A,H96B), C80(H80A,H80B), C77(H77A,H77B), C78(H78A,H78B), C79(H79A,H79B)
7.b Aromatic/amide H refined with riding coordinates:
 N4(H4), C6(H6), C5(H5), C4(H4A), C3(H3), C2(H2), 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), C62(H62), C63(H63), C64(H64),
 C65(H65), C66(H66), C68(H68), C69(H69), C70(H70), C71(H71), C72(H72)
;
_shelx_res_checksum              31482
_olex2_submission_special_instructions 'No special instructions were received'