Bimetallic rare-earth/platinum complexes ligated by phosphinoamides.
Völcker, Franziska; Roesky, Peter W.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 9429–9435; doi:10.1039/c6dt00417b

data_7038795
_publ_section_title
;
 Bimetallic rare-earth/platinum complexes ligated by phosphinoamides.
;
_journal_issue                   23
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9429
_journal_page_last               9435
_journal_paper_doi               10.1039/c6dt00417b
_journal_volume                  45
_journal_year                    2016
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C90 H76 N5 P5 Pt Y, C16 H32 Li O4'
_chemical_formula_sum            'C106 H108 Li N5 O4 P5 Pt Y'
_chemical_formula_weight         1961.76
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2015-04-20
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2016-01-27 deposited with the CCDC.
2016-03-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.47(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.628(5)
_cell_length_b                   14.886(3)
_cell_length_c                   28.196(6)
_cell_measurement_reflns_used    15779
_cell_measurement_temperature    209
_cell_measurement_theta_max      27.06
_cell_measurement_theta_min      1.51
_cell_volume                     9460(4)
_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-2013 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2008)'
_diffrn_ambient_temperature      209
_diffrn_detector                 'image plate (34cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            'STOE image plate'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_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  0.1126
_diffrn_reflns_av_unetI/netI     0.1871
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            36018
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.015
_diffrn_reflns_theta_min         1.514
_diffrn_source                   'sealed tube, 12x0.4mm long-fine focus'
_exptl_absorpt_coefficient_mu    2.22
_exptl_absorpt_correction_T_max  0.8987
_exptl_absorpt_correction_T_min  0.6400
_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    1.377
_exptl_crystal_description       plate
_exptl_crystal_F_000             4024
_exptl_crystal_size_max          0.282
_exptl_crystal_size_mid          0.153
_exptl_crystal_size_min          0.055
_refine_diff_density_max         1.745
_refine_diff_density_min         -0.752
_refine_diff_density_rms         0.099
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   -0.015(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.864
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1098
_refine_ls_number_reflns         18329
_refine_ls_number_restraints     50
_refine_ls_restrained_S_all      0.863
_refine_ls_R_factor_all          0.1064
_refine_ls_R_factor_gt           0.0639
_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^)+(0.0227P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1085
_refine_ls_wR_factor_ref         0.1212
_reflns_Friedel_coverage         0.972
_reflns_Friedel_fraction_full    0.975
_reflns_Friedel_fraction_max     0.970
_reflns_number_gt                11648
_reflns_number_total             18329
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt00417b2.cif
_cod_data_source_block           2a
_cod_depositor_comments
'Adding full bibliography for 7038793--7038795.cif.'
_cod_original_cell_volume        9459(4)
_cod_database_code               7038795
_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
 C31, C36, C35, C34, C33, C32
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C31 \\sim C36 \\sim C35 \\sim C34 \\sim C33 \\sim C32: within 1.7A with sigma
of 0.04 and sigma for terminal atoms of 0.08
4. Others
 Fixed Sof: C1A(0.5) H1AA(0.5) H1AB(0.5) C96B(0.5) H96A(0.5) H96B(0.5)
 C95B(0.5) H95A(0.5) H95B(0.5) H10I(0.5) H10J(0.5) H10G(0.5) H10H(0.5)
 H10M(0.5) H10N(0.5) H10K(0.5) H10L(0.5) C97A(0.5) H97A(0.5) H97B(0.5)
 C93B(0.5) H93A(0.5) H93B(0.5) C98B(0.5) H98A(0.5) H98B(0.5) O1A(0.5) C94A(0.5)
 H94A(0.5) H94B(0.5) C91A(0.5) H91A(0.5) H91B(0.5) C92A(0.5) H92A(0.5)
 H92B(0.5) O1B(0.5) C91B(0.5) H91C(0.5) H91D(0.5) C92B(0.5) H92C(0.5) H92D(0.5)
 C94B(0.5) H94C(0.5) H94D(0.5) C98A(0.5) H98C(0.5) H98D(0.5) C97B(0.5)
 H97C(0.5) H97D(0.5) C96A(0.5) H96C(0.5) H96D(0.5) C95A(0.5) H95C(0.5)
 H95D(0.5) C93A(0.5) H93C(0.5) H93D(0.5) C1B(0.5) H1BA(0.5) H1BB(0.5)
5.a Riding coordinates:
 N5(H5)
5.b Secondary CH2 refined with riding coordinates:
 C106(H10A,H10B), C1A(H1AA,H1AB), C96B(H96A,H96B), C99(H99A,H99B), C95B(H95A,
 H95B), C102(H10C,H10D), C100(H10E,H10F), C103(H10I,H10J), C103(H10G,H10H),
 C105(H10M,H10N), C105(H10K,H10L), C97A(H97A,H97B), C101(H10O,H10P), C93B(H93A,
 H93B), C98B(H98A,H98B), C94A(H94A,H94B), C91A(H91A,H91B), C92A(H92A,H92B),
 C91B(H91C,H91D), C92B(H92C,H92D), C94B(H94C,H94D), C98A(H98C,H98D), C97B(H97C,
 H97D), C96A(H96C,H96D), C95A(H95C,H95D), C93A(H93C,H93D), C1B(H1BA,H1BB)
5.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5A), 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), C74(H74), C75(H75),
  C76(H76), C77(H77), C78(H78), C80(H80), C81(H81), C82(H82), C83(H83),
 C84(H84), C86(H86), C87(H87), C88(H88), C89(H89), C90(H90)
;
_shelx_res_checksum              32284
_olex2_submission_special_instructions 'No special instructions were received'