Homoleptic Trigonal Planar Lanthanide Complexes Stabilized by Superbulky Silylamide Ligands
Goodwin, Conrad A. P.; Joslin, Kristian C.; Lockyer, Selena J.; Formanuik, Alasdair; Morris, Gareth A.; Ortu, Fabrizio; Vitorica-Yrezabal, Iñigo. J.; Mills, David P.; Organometallics 34 (2015) 2314–; doi:10.1021/om501123e

data_4085246
_publ_section_title
;
 Homoleptic Trigonal Planar Lanthanide Complexes Stabilized by Superbulky
 Silylamide Ligands
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              2314
_journal_paper_doi               10.1021/om501123e
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C24 H60 K2 N2 Si4'
_chemical_formula_sum            'C24 H60 K2 N2 Si4'
_chemical_formula_weight         567.30
_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             2014-09-30
_audit_creation_method
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_cell_angle_alpha                89.235(14)
_cell_angle_beta                 89.606(14)
_cell_angle_gamma                69.549(16)
_cell_formula_units_Z            2
_cell_length_a                   10.3328(18)
_cell_length_b                   11.995(2)
_cell_length_c                   15.134(3)
_cell_measurement_reflns_used    809
_cell_measurement_temperature    150.01(13)
_cell_measurement_theta_max      22.0290
_cell_measurement_theta_min      3.4880
_cell_volume                     1757.4(6)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.01(13)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0714
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.883
_diffrn_measurement_details
;
  1 omega  -82.00   31.00   1.0000  210.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.7892  -19.0000   90.0000 113

  2 omega  -12.00   94.00   1.0000  210.0000
omega____ theta____ kappa____ phi______ frames
    -       21.3360   77.0000   60.0000 106

  3 omega  -20.00   60.00   1.0000  210.0000
omega____ theta____ kappa____ phi______ frames
    -       21.3360  -99.0000  -60.0000 80

  4 omega   17.00   65.00   1.0000  210.0000
omega____ theta____ kappa____ phi______ frames
    -       21.3360  -99.0000 -180.0000 48
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0725014000
_diffrn_orient_matrix_UB_12      0.0226419000
_diffrn_orient_matrix_UB_13      -0.0065901000
_diffrn_orient_matrix_UB_21      -0.0059190000
_diffrn_orient_matrix_UB_22      -0.0500280000
_diffrn_orient_matrix_UB_23      0.0228350000
_diffrn_orient_matrix_UB_31      -0.0086771000
_diffrn_orient_matrix_UB_32      0.0311171000
_diffrn_orient_matrix_UB_33      0.0403981000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0979
_diffrn_reflns_av_unetI/netI     0.2576
_diffrn_reflns_Laue_measured_fraction_full 0.915
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            9612
_diffrn_reflns_point_group_measured_fraction_full 0.915
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         25.404
_diffrn_reflns_theta_min         3.222
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.420
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73084
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.072
_exptl_crystal_description
;
;
_exptl_crystal_F_000             624
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.444
_refine_diff_density_min         -0.490
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         6334
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.2429
_refine_ls_R_factor_gt           0.1135
_refine_ls_shift/su_max          0.030
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0668P)^2^+4.3415P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2235
_refine_ls_wR_factor_ref         0.2831
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2554
_reflns_number_total             6334
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om501123e_si_002.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 4085243--4085254.cif.'
_cod_database_code               4085246
_manchester_internal_archive_date 07/08/14
_manchester_internal_coll_client CAPG/DPM
_manchester_internal_coll_date   10/02/2014
_manchester_internal_coll_frame_method '\w scans'
_manchester_internal_coll_frame_time 210s
_manchester_internal_coll_frame_width 1
_manchester_internal_coll_name   adpm22
_manchester_internal_coll_type   custom
_manchester_internal_coll_user   CAPG
_manchester_internal_process_date 30/07/2014
_manchester_internal_process_user CAPG/FO
_manchester_internal_refinement_date 30/07/2014
_manchester_internal_refinement_user CAPG/FO
_manchester_internal_solution_date 30/07/2014
_manchester_internal_solution_user CAPG/FO
_manchester_internal_validation_date 07/08/14
_manchester_internal_validation_user 'Inigo J. Vitorica-Yrezabal'
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         'K2 N2 Si4 C12 H30'
_reflns_odcompleteness_completeness 88.70
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C7(H7), C1(H1), C16(H16), C19(H19), C4(H4), C13(H13)
2.b Me refined with riding coordinates:
 C18(H18A,H18B,H18C), C24(H24A,H24B,H24C), C15(H15A,H15B,H15C), C17(H17A,H17B,
 H17C), C20(H20A,H20B,H20C), C10(H10A,H10B,H10C), C6(H6A,H6B,H6C), C8(H8A,H8B,
 H8C), C21(H21A,H21B,H21C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C22(H22A,
 H22B,H22C), C3(H3A,H3B,H3C), C5(H5A,H5B,H5C), C9(H9A,H9B,H9C), C23(H23A,H23B,
 H23C), C11(H11A,H11B,H11C), C2(H2A,H2B,H2C)
;
_shelx_res_checksum              86429
_shelx_hkl_checksum              67821
_olex2_submission_special_instructions 'No special instructions were received'