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_7038793
_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_formula_moiety         'C88 H93 Cl Li N4 O4 P4 Pt Y, C4 H8 O'
_chemical_formula_sum            'C92 H101 Cl Li N4 O5 P4 Pt Y'
_chemical_formula_weight         1793.03
_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   geom
_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                99.59(3)
_cell_angle_beta                 98.88(3)
_cell_angle_gamma                99.85(3)
_cell_formula_units_Z            2
_cell_length_a                   13.302(3)
_cell_length_b                   15.181(3)
_cell_length_c                   22.663(5)
_cell_measurement_reflns_used    44690
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.61
_cell_measurement_theta_min      1.58
_cell_volume                     4366.6(18)
_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      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 0.982
_diffrn_measured_fraction_theta_max 0.978
_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  0.0478
_diffrn_reflns_av_unetI/netI     0.0472
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            31469
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.515
_diffrn_reflns_theta_min         1.582
_diffrn_source                   'sealed tube, 12x0.4mm long-fine focus'
_exptl_absorpt_coefficient_mu    2.418
_exptl_absorpt_correction_T_max  0.6757
_exptl_absorpt_correction_T_min  0.5077
_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       fragment
_exptl_crystal_F_000             1836
_exptl_crystal_size_max          0.353
_exptl_crystal_size_mid          0.244
_exptl_crystal_size_min          0.19
_refine_diff_density_max         1.255
_refine_diff_density_min         -1.449
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.988
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1092
_refine_ls_number_reflns         15963
_refine_ls_number_restraints     141
_refine_ls_restrained_S_all      0.993
_refine_ls_R_factor_all          0.0451
_refine_ls_R_factor_gt           0.0368
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0648P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0918
_refine_ls_wR_factor_ref         0.0947
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13680
_reflns_number_total             15963
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt00417b2.cif
_cod_data_source_block           1a
_cod_depositor_comments
'Adding full bibliography for 7038793--7038795.cif.'
_cod_original_cell_volume        4366.3(16)
_cod_database_code               7038793
_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 N(H) groups
2. Restrained distances
 O3A-Li1
 2 with sigma of 0.02
3. Rigid bond restraints
 O2A, C77A, C78A, C79A, C80A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C77B \\sim C78B \\sim C79B \\sim C80B: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08
Uanis(C87A) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C87A) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C87A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C88A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C88B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O4A) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C86B) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(O4A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C77A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C78A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Li1) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C82A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C82A) \\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(C83B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C84B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C84A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C83A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C84A) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O3A) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C80B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Same fragment restrains
{O2B, C77B, C78B, C79A, C80B} sigma for 1-2: 0.02, 1-3: 0.02
as
{O1, C73, C74, C75, C76}
{O3A, C84B, C83B, C82B, C81B} sigma for 1-2: 0.02, 1-3: 0.02
as
{O3B, C81A, C82A, C83A, C84A}
6. Others
 Fixed Sof: O2A(0.33333) O3B(0.66667) C81A(0.66667) H81A(0.66667)
 H81B(0.66667) C82A(0.66667) H82A(0.66667) H82B(0.66667) C83A(0.66667)
 H83A(0.66667) H83B(0.66667) C84A(0.66667) H84A(0.66667) H84B(0.66667) O4B(0.5)
 C77A(0.33333) H77A(0.33333) H77B(0.33333) C78A(0.33333) H78A(0.33333)
 H78B(0.33333) O2B(0.66667) C77B(0.66667) H77C(0.66667) H77D(0.66667)
 C78B(0.66667) H78C(0.66667) H78D(0.66667) C79A(0.33333) H79A(0.33333)
 H79B(0.33333) C80B(0.66667) H80A(0.66667) H80B(0.66667) C80A(0.33333)
 H80C(0.33333) H80D(0.33333) C85A(0.5) H85A(0.5) H85B(0.5) C86A(0.5) H86A(0.5)
 H86B(0.5) C87A(0.5) H87A(0.5) H87B(0.5) C88A(0.5) H88A(0.5) H88B(0.5)
 O3A(0.33333) C84B(0.33333) H84C(0.33333) H84D(0.33333) C83B(0.33333)
 H83C(0.33333) H83D(0.33333) C82B(0.33333) H82C(0.33333) H82D(0.33333)
 C81B(0.33333) H81C(0.33333) H81D(0.33333) O4A(0.5) C79B(0.66667) H79C(0.66667)
 H79D(0.66667) C85B(0.5) H85C(0.5) H85D(0.5) C86B(0.5) H86C(0.5) H86D(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:
 C73(H73A,H73B), C74(H74A,H74B), C75(H75A,H75B), C76(H76A,H76B), C81A(H81A,
 H81B), C82A(H82A,H82B), C83A(H83A,H83B), C84A(H84A,H84B), C77A(H77A,H77B),
 C78A(H78A,H78B), C77B(H77C,H77D), C78B(H78C,H78D), C79A(H79A,H79B), C80B(H80A,
 H80B), C80A(H80C,H80D), C85A(H85A,H85B), C86A(H86A,H86B), C87A(H87A,H87B),
 C88A(H88A,H88B), C84B(H84C,H84D), C83B(H83C,H83D), C82B(H82C,H82D), C81B(H81C,
 H81D), C79B(H79C,H79D), C85B(H85C,H85D), C86B(H86C,H86D), C87B(H87C,H87D),
 C88B(H88C,H88D), C89(H89A,H89B), C90(H90A,H90B), C91(H91A,H91B), C92(H92A,H92B)
7.b Aromatic/amide H refined with riding coordinates:
 N4(H4), C3(H3), C2(H2), C6(H6), C5(H5), C9(H9), C4(H4A), C12(H12), C11(H11),
 C10(H10), C8(H8), 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              20953
_olex2_submission_special_instructions 'No special instructions were received'