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_7117479
_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         'C72 H60 N4 P4 Y, C16 H32 Li O4, 3(C4 H8 O)'
_chemical_formula_sum            'C100 H116 Li N4 O7 P4 Y'
_chemical_formula_weight         1705.69
_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   geom
_audit_creation_date             2015-03-05
_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                 104.10(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.911(3)
_cell_length_b                   24.635(5)
_cell_length_c                   26.155(5)
_cell_measurement_reflns_used    47228
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      26.60
_cell_measurement_theta_min      1.41
_cell_volume                     9318(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 1.000
_diffrn_measured_fraction_theta_max 0.993
_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  0.1534
_diffrn_reflns_av_unetI/netI     0.1017
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            141956
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.816
_diffrn_reflns_theta_min         1.408
_diffrn_source                   'sealed tube, 12x0.4mm long-fine focus'
_exptl_absorpt_coefficient_mu    0.750
_exptl_absorpt_correction_T_max  0.8698
_exptl_absorpt_correction_T_min  0.6879
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE X-RED & X-SHAPE'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.216
_exptl_crystal_description       fragment
_exptl_crystal_F_000             3608
_exptl_crystal_size_max          0.391
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.141
_refine_diff_density_max         0.859
_refine_diff_density_min         -0.561
_refine_diff_density_rms         0.061
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1150
_refine_ls_number_reflns         19814
_refine_ls_number_restraints     76
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.1522
_refine_ls_R_factor_gt           0.0831
_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^)+(0.0941P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1728
_refine_ls_wR_factor_ref         0.2011
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                11193
_reflns_number_total             19814
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5cc03944d2.cif
_cod_data_source_block           Y(PN)4
_cod_database_code               7117479
_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
2. Restrained distances
 C98-C99
 1.45 with sigma of 0.02
 C93-C94
 1.45 with sigma of 0.02
3. Rigid bond restraints
 C81A, C82A, C83A, C84A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C74A, C73A, C75A, C76A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C81B \\sim C82B \\sim C83B \\sim C84B: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08
C77B \\sim C78B \\sim C79B \\sim C80B: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08
C74A \\sim C73A \\sim C75A \\sim C76A: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08
5. Same fragment restrains
{O1A, C76A, C75A, C74A, C73A} sigma for 1-2: 0.02, 1-3: 0.02
as
{O3A, C81A, C82A, C83A, C84A}
6. Others
 Fixed Sof: O1A(0.5) C76A(0.5) H76A(0.5) H76B(0.5) C75A(0.5) H75A(0.5)
 H75B(0.5) H74A(0.5) H74B(0.5) H74C(0.5) H74D(0.5) C73A(0.5) H73A(0.5)
 H73B(0.5) O2A(0.5) O3A(0.5) C81A(0.5) H81A(0.5) H81B(0.5) C82A(0.5) H82A(0.5)
 H82B(0.5) C83A(0.5) H83A(0.5) H83B(0.5) C84A(0.5) H84A(0.5) H84B(0.5) O4A(0.5)
 C6GA(0.5) H6GA(0.5) H6GB(0.5) C77A(0.5) H77A(0.5) H77B(0.5) C78A(0.5)
 H78A(0.5) H78B(0.5) C79A(0.5) H79A(0.5) H79B(0.5) C80A(0.5) H80A(0.5)
 H80B(0.5) C85A(0.5) H85A(0.5) H85B(0.5) C87A(0.5) H87A(0.5) H87B(0.5)
 C88A(0.5) H88A(0.5) H88B(0.5) O1B(0.5) O2B(0.5) O3B(0.5) O4B(0.5) C73B(0.5)
 H73C(0.5) H73D(0.5) C75B(0.5) H75C(0.5) H75D(0.5) C76B(0.5) H76C(0.5)
 H76D(0.5) C77B(0.5) H77C(0.5) H77D(0.5) C78B(0.5) H78C(0.5) H78D(0.5)
 C79B(0.5) H79C(0.5) H79D(0.5) C80B(0.5) H80C(0.5) H80D(0.5) C81B(0.5)
 H81C(0.5) H81D(0.5) C82B(0.5) H82C(0.5) H82D(0.5) C83B(0.5) H83C(0.5)
 H83D(0.5) C84B(0.5) H84C(0.5) H84D(0.5) C85B(0.5) H85C(0.5) H85D(0.5)
 C86B(0.5) H86A(0.5) H86B(0.5) C87B(0.5) H87C(0.5) H87D(0.5) C88B(0.5)
 H88C(0.5) H88D(0.5)
7.a Secondary CH2 refined with riding coordinates:
 C76A(H76A,H76B), C75A(H75A,H75B), C74A(H74A,H74B), C74A(H74C,H74D), C73A(H73A,
 H73B), C81A(H81A,H81B), C82A(H82A,H82B), C83A(H83A,H83B), C84A(H84A,H84B),
 C6GA(H6GA,H6GB), C77A(H77A,H77B), C78A(H78A,H78B), C79A(H79A,H79B), C80A(H80A,
 H80B), C85A(H85A,H85B), C87A(H87A,H87B), C88A(H88A,H88B), C73B(H73C,H73D),
 C75B(H75C,H75D), C76B(H76C,H76D), C77B(H77C,H77D), C78B(H78C,H78D), C79B(H79C,
 H79D), C80B(H80C,H80D), C81B(H81C,H81D), C82B(H82C,H82D), C83B(H83C,H83D),
 C84B(H84C,H84D), C85B(H85C,H85D), C86B(H86A,H86B), C87B(H87C,H87D), C88B(H88C,
 H88D), C93(H93A,H93B), C94(H94A,H94B), C95(H95A,H95B), C96(H96A,H96B),
 C89(H89A,H89B), C90(H90A,H90B), C91(H91A,H91B), C92(H92A,H92B), C97(H97A,H97B),
  C98(H98A,H98B), C99(H99A,H99B), C100(H10A,H10B)
7.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C38(H38), C39(H39),
  C40(H40), C41(H41), C42(H42), C44(H44), C45(H45), C46(H46), C47(H47),
 C48(H48), C54(H54), C53(H53), C52(H52), C51(H51), C50(H50), C24(H24), C23(H23),
  C22(H22), C21(H21), C20(H20), C30(H30), C29(H29), C28(H28), C27(H27),
 C26(H26), C36(H36), C35(H35), C34(H34), C33(H33), C32(H32), 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              72357
_olex2_submission_special_instructions 'No special instructions were received'