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_4085244
_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         'C26 H60 Li2 N2 O2 Si2'
_chemical_formula_sum            'C26 H60 Li2 N2 O2 Si2'
_chemical_formula_weight         502.82
_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             2014-08-07
_audit_creation_method
;
Olex2 1.2
(compiled 2014.05.21 svn.r2940 for OlexSys, GUI svn.r4846)
;
_cell_angle_alpha                101.206(11)
_cell_angle_beta                 105.344(10)
_cell_angle_gamma                91.823(10)
_cell_formula_units_Z            1
_cell_length_a                   8.4756(9)
_cell_length_b                   9.3105(13)
_cell_length_c                   11.1845(14)
_cell_measurement_reflns_used    2129
_cell_measurement_temperature    150.05(13)
_cell_measurement_theta_max      25.6200
_cell_measurement_theta_min      3.5510
_cell_volume                     831.67(19)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.05(13)
_diffrn_detector_area_resol_mean 10.3705
_diffrn_measured_fraction_theta_full 0.9826
_diffrn_measured_fraction_theta_max 0.8143
_diffrn_measurement_details
;
  1 omega  -36.00   52.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.6555   57.0000  150.0000 88

  2 omega  -85.00   11.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.6555  -57.0000    0.0000 96

  3 omega   35.00  102.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       11.6555  178.0000    0.0000 67
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0388084000
_diffrn_orient_matrix_UB_12      -0.0661261000
_diffrn_orient_matrix_UB_13      0.0027713000
_diffrn_orient_matrix_UB_21      0.0059255000
_diffrn_orient_matrix_UB_22      -0.0046747000
_diffrn_orient_matrix_UB_23      -0.0627001000
_diffrn_orient_matrix_UB_31      0.0777709000
_diffrn_orient_matrix_UB_32      0.0410380000
_diffrn_orient_matrix_UB_33      0.0242057000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0271
_diffrn_reflns_av_unetI/netI     0.0669
_diffrn_reflns_Laue_measured_fraction_full 0.888
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5043
_diffrn_reflns_point_group_measured_fraction_full 0.888
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         25.026
_diffrn_reflns_theta_min         3.251
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.128
_exptl_absorpt_correction_T_max  0.992
_exptl_absorpt_correction_T_min  0.990
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
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    1.004
_exptl_crystal_description       Block
_exptl_crystal_F_000             280
_exptl_crystal_size_max          0.2761
_exptl_crystal_size_mid          0.2099
_exptl_crystal_size_min          0.1876
_refine_diff_density_max         0.264
_refine_diff_density_min         -0.372
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     200
_refine_ls_number_reflns         2902
_refine_ls_number_restraints     178
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0806
_refine_ls_R_factor_gt           0.0593
_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^)+(0.0362P)^2^+0.5405P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1178
_refine_ls_wR_factor_ref         0.1379
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2312
_reflns_number_total             2902
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om501123e_si_002.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 4085243--4085254.cif.'
_cod_database_code               4085244
_manchester_internal_coll_name   adpm5
_manchester_internal_coll_client CAPG/SL/DPM
_manchester_internal_coll_type   custom
_manchester_internal_coll_frame_time 5.00
_manchester_internal_coll_frame_width 1
_manchester_internal_coll_frame_method '\w scans'
_manchester_internal_coll_user   CAPG
_manchester_internal_coll_date   30/10/2013
_manchester_internal_process_user CAPG
_manchester_internal_process_date 09/11/2013
_manchester_internal_solution_user CAPG
_manchester_internal_solution_date 09/11/2013
_manchester_internal_refinement_user CAPG
_manchester_internal_refinement_date 09/11/2013
_manchester_internal_validation_user 'Inigo J. Vitorica-Yrezabal'
_manchester_internal_validation_date 07/08/14
_manchester_internal_archive_date 07/08/14
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         H22C9SiNLi
_reflns_odcompleteness_completeness 98.26
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C13-C12 \\sim C12-C11 \\sim C11-C10
 with sigma of 0.02
 C12-C11A \\sim C12-C11
 with sigma of 0.02
 C11A-C10 \\sim C11-C10
 with sigma of 0.02
 C13-C12 \\sim C12-C11A \\sim C11A-C10
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O1 \\sim C10 \\sim C13 \\sim C12 \\sim C11A \\sim C11: within 1.7A with sigma
of 0.04 and sigma for terminal atoms of 0.08
C13 \\sim C13A \\sim C12A \\sim C12 \\sim C11A \\sim C11 \\sim C10A \\sim C10:
within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
4. Rigid body (RIGU) restrains
 C10, C11, C12, C13, O1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C10A, O1A, C13A, C12A, C11A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C11A)=Sof(H11C)=Sof(H11D)=Sof(C13A)=Sof(H13C)=Sof(H13D)=Sof(C12A)=
 Sof(H12C)=Sof(H12D)=Sof(C10A)=Sof(H10C)=Sof(H10D)=Sof(O1A)=1-FVAR(1)
 Sof(C10)=Sof(H10A)=Sof(H10B)=Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(C13)=Sof(H13A)=
 Sof(H13B)=Sof(O1)=Sof(C11)=Sof(H11A)=Sof(H11B)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C1(H1), C4(H4), C7(H7), N1(H1A)
6.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C12(H12A,H12B), C13(H13A,H13B), C11(H11A,H11B), C11A(H11C,
 H11D), C13A(H13C,H13D), C12A(H12C,H12D), C10A(H10C,H10D)
6.c Me refined with riding coordinates:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C8(H8A,
 H8B,H8C), C9(H9A,H9B,H9C)
;
_shelx_res_checksum              28490
_shelx_hkl_checksum              36360
_olex2_submission_special_instructions 'No special instructions were received'