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_4085247
_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, C7 H8'
_chemical_formula_sum            'C31 H68 K2 N2 Si4'
_chemical_formula_weight         659.43
_chemical_name_systematic        bis(tertbutyldimethylsilyl)amidopotassium
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2014-04-02
_audit_creation_method
;
Olex2 1.2
(compiled 2014.02.17 svn.r2891 for OlexSys, GUI svn.r4773)
;
_cell_angle_alpha                65.835(8)
_cell_angle_beta                 78.506(6)
_cell_angle_gamma                66.789(7)
_cell_formula_units_Z            1
_cell_length_a                   9.6065(6)
_cell_length_b                   10.3964(9)
_cell_length_c                   11.8240(10)
_cell_measurement_reflns_used    2381
_cell_measurement_temperature    150.02(10)
_cell_measurement_theta_max      28.2270
_cell_measurement_theta_min      3.4660
_cell_volume                     989.20(16)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.02(10)
_diffrn_detector_area_resol_mean 16.1428
_diffrn_measured_fraction_theta_full 0.9980
_diffrn_measured_fraction_theta_max 0.8492
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0199259000
_diffrn_orient_matrix_UB_12      -0.0767053000
_diffrn_orient_matrix_UB_13      0.0087966000
_diffrn_orient_matrix_UB_21      0.0442840000
_diffrn_orient_matrix_UB_22      -0.0217192000
_diffrn_orient_matrix_UB_23      0.0504621000
_diffrn_orient_matrix_UB_31      -0.0641036000
_diffrn_orient_matrix_UB_32      -0.0038450000
_diffrn_orient_matrix_UB_33      0.0413291000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0337
_diffrn_reflns_av_unetI/netI     0.0695
_diffrn_reflns_Laue_measured_fraction_full 0.931
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6340
_diffrn_reflns_point_group_measured_fraction_full 0.931
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         25.346
_diffrn_reflns_theta_min         3.050
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.382
_exptl_absorpt_correction_T_max  0.953
_exptl_absorpt_correction_T_min  0.922
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.107
_exptl_crystal_description
;
;
_exptl_crystal_F_000             362
_exptl_crystal_recrystallization_method 'From toluene'
_exptl_crystal_size_max          0.2988
_exptl_crystal_size_mid          0.2137
_exptl_crystal_size_min          0.1487
_refine_diff_density_max         0.316
_refine_diff_density_min         -0.263
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     196
_refine_ls_number_reflns         3622
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0633
_refine_ls_R_factor_gt           0.0454
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0361P)^2^+0.1296P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0946
_refine_ls_wR_factor_ref         0.1083
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2821
_reflns_number_total             3622
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om501123e_si_002.cif
_cod_data_source_block           5
_cod_depositor_comments
'Adding full bibliography for 4085243--4085254.cif.'
_cod_original_cell_volume        989.20(15)
_cod_database_code               4085247
_manchester_internal_coll_name   adpm20
_manchester_internal_coll_client CAPG/DPM
_manchester_internal_coll_type   custom
_manchester_internal_coll_frame_time 1.22
_manchester_internal_coll_frame_width 1
_manchester_internal_coll_frame_method '\w scans'
_manchester_internal_coll_user   CAPG
_manchester_internal_coll_date   29/01/2014
_manchester_internal_process_user CAPG
_manchester_internal_process_date 29/01/2014
_manchester_internal_solution_user CAPG/FO
_manchester_internal_solution_date 02/04/2014
_manchester_internal_refinement_user CAPG/FO
_manchester_internal_refinement_date 02/04/2014
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'K Si2 C12 H36 N C14 H16'
_reflns_odcompleteness_completeness 99.80
_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. Restrained distances
 H15-C15
 0.96 with sigma of 0.001
3. Others
 Fixed Sof: C16(0.5) H16A(0.5) H16B(0.5) H16C(0.5) H15(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C14(H14), C13(H13)
4.b Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C6(H6A,
 H6B,H6C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,
 H11C), C12(H12A,H12B,H12C), C16(H16A,H16B,H16C)
;
_shelx_res_checksum              80075
_shelx_hkl_checksum              59087
_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'
_olex2_computing_structure_solution_long 'ShelXS (Sheldrick, 2008)'