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_7038794
_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 Lu N4 O4 P4 Pt, C4 H8 O, C7 H8'
_chemical_formula_sum            'C99 H109 Cl Li Lu N4 O5 P4 Pt'
_chemical_formula_weight         1971.23
_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   mixed
_audit_creation_date             2015-12-16
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2016-01-27 deposited with the CCDC.
2016-03-09 downloaded from the CCDC.
;
_cell_angle_alpha                99.85(3)
_cell_angle_beta                 98.77(3)
_cell_angle_gamma                97.53(3)
_cell_formula_units_Z            2
_cell_length_a                   13.388(3)
_cell_length_b                   15.201(3)
_cell_length_c                   22.573(5)
_cell_measurement_reflns_used    11874
_cell_measurement_temperature    210(2)
_cell_measurement_theta_max      28.15
_cell_measurement_theta_min      1.67
_cell_volume                     4414.6(18)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      210
_diffrn_detector                 'image plate (34cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            'STOE image plate'
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_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  0.0947
_diffrn_reflns_av_unetI/netI     0.2475
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       15
_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       -27
_diffrn_reflns_number            34017
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         1.807
_diffrn_source                   'sealed tube, 12x0.4mm long-fine focus'
_exptl_absorpt_coefficient_mu    2.853
_exptl_absorpt_correction_T_max  0.8397
_exptl_absorpt_correction_T_min  0.7371
_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    1.483
_exptl_crystal_description       prism
_exptl_crystal_F_000             2000
_exptl_crystal_size_max          0.159
_exptl_crystal_size_mid          0.119
_exptl_crystal_size_min          0.084
_refine_diff_density_max         1.102
_refine_diff_density_min         -0.604
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.649
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     959
_refine_ls_number_reflns         17155
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.649
_refine_ls_R_factor_all          0.1300
_refine_ls_R_factor_gt           0.0469
_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^)+(0.0004P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0629
_refine_ls_wR_factor_ref         0.0763
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7750
_reflns_number_total             17155
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt00417b2.cif
_cod_data_source_block           1b
_cod_depositor_comments
'Adding full bibliography for 7038793--7038795.cif.'
_cod_original_cell_volume        4414.6(16)
_cod_database_code               7038794
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: H73C(0.5) H73D(0.5) H73A(0.5) H73B(0.5) C74B(0.66666)
 H74A(0.66666) H74B(0.66666) C75B(0.66666) H75A(0.66666) H75B(0.66666)
 H76C(0.66666) H76D(0.66666) H76A(0.33333) H76B(0.33333) C80B(0.5) H80A(0.5)
 H80B(0.5) C78A(0.5) H78A(0.5) H78B(0.5) O3B(0.5) C81B(0.5) H81A(0.5) H81B(0.5)
 C88B(0.5) H88A(0.5) H88B(0.5) C83B(0.5) H83A(0.5) H83B(0.5) C85B(0.5)
 H85A(0.5) H85B(0.5) C84B(0.5) H84A(0.5) H84B(0.5) C82B(0.5) H82A(0.5)
 H82B(0.5) C87B(0.5) H87A(0.5) H87B(0.5) C86B(0.5) H86A(0.5) H86B(0.5)
 C84A(0.5) H84C(0.5) H84D(0.5) C82A(0.5) H82C(0.5) H82D(0.5) C83A(0.5)
 H83C(0.5) H83D(0.5) C79B(0.5) H79A(0.5) H79B(0.5) C77A(0.5) H77A(0.5)
 H77B(0.5) C81A(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) C78B(0.5) H78C(0.5) H78D(0.5) C77B(0.5) H77C(0.5)
 H77D(0.5) C74A(0.33333) H74C(0.33333) H74D(0.33333) C75A(0.33333)
 H75C(0.33333) H75D(0.33333) C80A(0.5) H80C(0.5) H80D(0.5) C79A(0.5) H79C(0.5)
 H79D(0.5) O3A(0.5)
3.a Riding coordinates:
 N4(H4)
3.b Secondary CH2 refined with riding coordinates:
 C73(H73C,H73D), C73(H73A,H73B), C74B(H74A,H74B), C75B(H75A,H75B), C76(H76C,
 H76D), C76(H76A,H76B), C80B(H80A,H80B), C78A(H78A,H78B), C81B(H81A,H81B),
 C88B(H88A,H88B), C83B(H83A,H83B), C85B(H85A,H85B), C84B(H84A,H84B), C82B(H82A,
 H82B), C87B(H87A,H87B), C86B(H86A,H86B), C92(H92A,H92B), C90(H90A,H90B),
 C89(H89A,H89B), C91(H91A,H91B), C84A(H84C,H84D), C82A(H82C,H82D), C83A(H83C,
 H83D), C79B(H79A,H79B), C77A(H77A,H77B), C81A(H81C,H81D), C85A(H85C,H85D),
 C86A(H86C,H86D), C87A(H87C,H87D), C88A(H88C,H88D), C78B(H78C,H78D), C77B(H77C,
 H77D), C74A(H74C,H74D), C75A(H75C,H75D), C80A(H80C,H80D), C79A(H79C,H79D)
3.c Aromatic/amide H refined with riding coordinates:
 C53(H53), C8(H8), C30(H30), C42(H42), C12(H12), C66(H66), C38(H38), C54(H54),
 C26(H26), C62(H62), C29(H29), C39(H39), C41(H41), C9(H9), C27(H27), C40(H40),
 C28(H28), C52(H52), C48(H48), C47(H47), C14(H14), C5(H5), C44(H44), C32(H32),
 C2(H2), C6(H6), C60(H60), C51(H51), C34(H34), C36(H36), C15(H15), C46(H46),
 C56(H56), C18(H18), C45(H45), C20(H20), C22(H22), C68(H68), C24(H24), C58(H58),
  C4(H4A), C50(H50), C10(H10), C63(H63), C21(H21), C11(H11), C57(H57), C65(H65),
  C69(H69), C35(H35), C59(H59), C64(H64), C33(H33), C3(H3), C16(H16), C70(H70),
 C72(H72), C17(H17), C23(H23), C71(H71), C94(H94), C95(H95), C96(H96), C97(H97),
  C98(H98)
3.d Fitted hexagon refined as free rotating group:
 C93(C94,C95,C96,C97,C98)
3.e Idealised Me refined as rotating group:
 C99(H99A,H99B,H99C)
;
_shelx_res_checksum              72633
_olex2_submission_special_instructions 'No special instructions were received'