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_7117474
_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 Lu N4 O4 P4 Pd, 2(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      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                90
_cell_angle_beta                 90.84(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.559(3)
_cell_length_b                   28.870(6)
_cell_length_c                   22.627(5)
_cell_measurement_reflns_used    10535
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      23.27
_cell_measurement_theta_min      1.41
_cell_volume                     8856(3)
_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 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details
;
 147 frames, detector distance = 120 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  0.1217
_diffrn_reflns_av_unetI/netI     0.4563
_diffrn_reflns_laue_measured_fraction_full 0.999
_diffrn_reflns_laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            51954
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.017
_diffrn_reflns_theta_min         1.411
_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    1.47
_exptl_absorpt_correction_T_max  0.9162
_exptl_absorpt_correction_T_min  0.8049
_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    1.397
_exptl_crystal_description       fragment
_exptl_crystal_F_000             3832
_exptl_crystal_size_max          0.193
_exptl_crystal_size_mid          0.142
_exptl_crystal_size_min          0.067
_refine_diff_density_max         1.170
_refine_diff_density_min         -0.585
_refine_diff_density_rms         0.092
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.807
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1041
_refine_ls_number_reflns         17364
_refine_ls_number_restraints     130
_refine_ls_restrained_S_all      0.806
_refine_ls_R_factor_all          0.1967
_refine_ls_R_factor_gt           0.0579
_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^)+(0.0166P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0859
_refine_ls_wR_factor_ref         0.1194
_reflns_Friedel_coverage         0.000
_reflns_friedel_fraction_full    .
_reflns_friedel_fraction_max     .
_reflns_number_gt                6499
_reflns_number_total             17364
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5cc03944d2.cif
_cod_data_source_block           1b
_cod_database_code               7117474
_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
 C86B, C87B, C85A, C88A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O2, C77, C78, C79, C80
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C85B, C88B, C86A, C87A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O3B, C81B, C82B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O3A, C81A, C82A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
O2 \\sim C77 \\sim C78 \\sim C79 \\sim C80: within 1.7A with sigma of 0.04 and
sigma for terminal atoms of 0.08
Uanis(C82B) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C81A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C86B) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C87B) \\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(C87A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C86A) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C86A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C80) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C74) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O4) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C85A) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C85B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O3A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Same fragment restrains
{O6, C93, C94, C95, C96} sigma for 1-2: 0.02, 1-3: 0.02
as
{O5, C89, C90, C91, C92}
5. Others
 Sof(H83C)=Sof(H83D)=Sof(C82B)=Sof(H82C)=Sof(H82D)=1-FVAR(1)
 Sof(H83A)=Sof(H83B)=Sof(C82A)=Sof(H82A)=Sof(H82B)=FVAR(1)
 Fixed Sof: H84C(0.5) H84D(0.5) H84A(0.5) H84B(0.5) C81A(0.5) H81A(0.5)
 H81B(0.5) C85B(0.5) H85A(0.5) H85B(0.5) C86B(0.5) H86A(0.5) H86B(0.5)
 C87B(0.5) H87A(0.5) H87B(0.5) C88B(0.5) H88A(0.5) H88B(0.5) C81B(0.5)
 H81C(0.5) H81D(0.5) C85A(0.5) H85C(0.5) H85D(0.5) C86A(0.5) H86C(0.5)
 H86D(0.5) C87A(0.5) H87C(0.5) H87D(0.5) C88A(0.5) H88C(0.5) H88D(0.5) O3B(0.5)
 O3A(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), C77(H77A,
 H77B), C78(H78A,H78B), C79(H79A,H79B), C80(H80A,H80B), C83(H83C,H83D),
 C83(H83A,H83B), C84(H84C,H84D), C84(H84A,H84B), C81A(H81A,H81B), C82A(H82A,
 H82B), C85B(H85A,H85B), C86B(H86A,H86B), C87B(H87A,H87B), C88B(H88A,H88B),
 C81B(H81C,H81D), C82B(H82C,H82D), C85A(H85C,H85D), C86A(H86C,H86D), C87A(H87C,
 H87D), C88A(H88C,H88D), C89(H89A,H89B), C90(H90A,H90B), C91(H91A,H91B),
 C92(H92A,H92B), C93(H93A,H93B), C94(H94A,H94B), C95(H95A,H95B), C96(H96A,H96B)
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), C62(H62), C63(H63), C64(H64), C65(H65),
 C66(H66), C68(H68), C69(H69), C70(H70), C71(H71), C72(H72)
;
_shelx_res_checksum              87206
_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'
_olex2_computing_structure_solution_long 'SHELXS-97 (Sheldrick, 1997)'
_olex2_submission_special_instructions 'No special instructions were received'