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_4085250
_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         'C30 H66 K N O3 Si2'
_chemical_formula_sum            'C30 H66 K N O3 Si2'
_chemical_formula_weight         584.11
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2014-08-07
_audit_creation_method
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Olex2 1.2
(compiled 2014.05.21 svn.r2940 for OlexSys, GUI svn.r4846)
;
_cell_angle_alpha                90
_cell_angle_beta                 95.585(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.9958(5)
_cell_length_b                   22.5304(15)
_cell_length_c                   17.8861(11)
_cell_measurement_reflns_used    2130
_cell_measurement_temperature    150.02(11)
_cell_measurement_theta_max      21.3860
_cell_measurement_theta_min      3.4950
_cell_volume                     3607.9(4)
_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
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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)'
_diffrn_ambient_temperature      150.02(11)
_diffrn_detector_area_resol_mean 16.1428
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.867
_diffrn_measurement_details
;
  1 omega  -20.00   25.00   1.0000   85.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.8628  -99.0000    0.0000 45

  2 omega  -40.00   50.00   1.0000   85.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.8628   57.0000    0.0000 90

  3 omega  -12.00   91.00   1.0000   85.0000
omega____ theta____ kappa____ phi______ frames
    -       19.6440   77.0000 -120.0000 103

  4 omega  -12.00   91.00   1.0000   85.0000
omega____ theta____ kappa____ phi______ frames
    -       19.6440   77.0000  120.0000 103
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0417381000
_diffrn_orient_matrix_UB_12      -0.0009335000
_diffrn_orient_matrix_UB_13      0.0316147000
_diffrn_orient_matrix_UB_21      0.0022634000
_diffrn_orient_matrix_UB_22      -0.0314633000
_diffrn_orient_matrix_UB_23      -0.0004770000
_diffrn_orient_matrix_UB_31      0.0672785000
_diffrn_orient_matrix_UB_32      0.0005261000
_diffrn_orient_matrix_UB_33      0.0242741000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1142
_diffrn_reflns_av_unetI/netI     0.1598
_diffrn_reflns_Laue_measured_fraction_full 0.930
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            20543
_diffrn_reflns_point_group_measured_fraction_full 0.930
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         2.944
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.241
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.677
_exptl_absorpt_correction_type   gaussian
_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)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
;
_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    1.075
_exptl_crystal_description
;
;
_exptl_crystal_F_000             1296
_exptl_crystal_size_max          0.554
_exptl_crystal_size_mid          0.2594
_exptl_crystal_size_min          0.0743
_refine_diff_density_max         0.633
_refine_diff_density_min         -0.297
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.977
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     429
_refine_ls_number_reflns         6589
_refine_ls_number_restraints     283
_refine_ls_restrained_S_all      0.972
_refine_ls_R_factor_all          0.1787
_refine_ls_R_factor_gt           0.0753
_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^)+(0.0700P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1550
_refine_ls_wR_factor_ref         0.2056
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3021
_reflns_number_total             6589
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om501123e_si_002.cif
_cod_data_source_block           8
_cod_depositor_comments
'Adding full bibliography for 4085243--4085254.cif.'
_cod_database_code               4085250
_manchester_internal_archive_date 07/08/14
_manchester_internal_coll_client CAPG/DPM
_manchester_internal_coll_date   30/01/2014
_manchester_internal_coll_frame_method '\w scans'
_manchester_internal_coll_frame_time 85s
_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 17/03/2014
_manchester_internal_process_user CAPG
_manchester_internal_refinement_date 29/06/2014
_manchester_internal_refinement_user CAPG
_manchester_internal_solution_date 29/06/2014
_manchester_internal_solution_user CAPG
_manchester_internal_validation_date 07/08/14
_manchester_internal_validation_user 'Inigo J. Vitorica-Yrezabal'
_olex2_submission_special_instructions 'No special instructions were received'
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         'K Si2 N C30 H60'
_reflns_odcompleteness_completeness 99.70
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C28A-C27A
 1.47 with sigma of 0.02
 C26B-C23C
 2.33 with sigma of 0.02
 C25B-C23C
 2.33 with sigma of 0.02
 C24B-C26B
 2.33 with sigma of 0.02
 C23B-C25A
 2.33 with sigma of 0.02
 C26A-C23B
 2.33 with sigma of 0.02
 C26A-C24A
 2.33 with sigma of 0.02
 C21-C22 \\sim C24A-C25A \\sim C24B-C25B
 with sigma of 0.02
 C20-C19 \\sim C24A-C23B \\sim C26A-C25A
 with sigma of 0.02
 O2B-C23B \\sim O2B-C26A
 with sigma of 0.02
 O2A-C23C \\sim O2A-C26B
 with sigma of 0.02
 K1-O2A \\sim K1-O2B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C23B \\sim C26A \\sim C25A \\sim C24A \\sim C26B \\sim C25B \\sim C24B \\sim
C23C: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
O2B \\sim O2A: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C27 \\sim C27A \\sim C28A \\sim C28 \\sim C29 \\sim C29A \\sim C30 \\sim C30A:
within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
4. Rigid body (RIGU) restrains
 C23B, C26A, C25A, C24A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O3, C30, C29, C28, C27
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O3, C27A, C28A, C29A, C30A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C27A)=Sof(H27C)=Sof(H27D)=Sof(C28A)=Sof(H28C)=Sof(H28D)=Sof(C29A)=
 Sof(H29C)=Sof(H29D)=Sof(C30A)=Sof(H30C)=Sof(H30D)=1-FVAR(1)
 Sof(C27)=Sof(H27A)=Sof(H27B)=Sof(C28)=Sof(H28A)=Sof(H28B)=Sof(C29)=Sof(H29A)=
 Sof(H29B)=Sof(C30)=Sof(H30A)=Sof(H30B)=FVAR(1)
 Sof(O2A)=Sof(C26B)=Sof(H26C)=Sof(H26D)=Sof(C25B)=Sof(H25C)=Sof(H25D)=
 Sof(C24B)=Sof(H24C)=Sof(H24D)=Sof(C23C)=Sof(H23C)=Sof(H23D)=1-FVAR(2)
 Sof(C23B)=Sof(H23A)=Sof(H23B)=Sof(C26A)=Sof(H26A)=Sof(H26B)=Sof(C25A)=
 Sof(H25A)=Sof(H25B)=Sof(C24A)=Sof(H24A)=Sof(H24B)=Sof(O2B)=FVAR(2)
6.a Ternary CH refined with riding coordinates:
 C1(H1), C4(H4), C7(H7), C10(H10), C13(H13), C16(H16)
6.b Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B), C22(H22A,H22B), C23B(H23A,
 H23B), C26A(H26A,H26B), C27(H27A,H27B), C27A(H27C,H27D), C28(H28A,H28B),
 C28A(H28C,H28D), C29(H29A,H29B), C29A(H29C,H29D), C30(H30A,H30B), C30A(H30C,
 H30D), C25A(H25A,H25B), C24A(H24A,H24B), C26B(H26C,H26D), C25B(H25C,H25D),
 C24B(H24C,H24D), C23C(H23C,H23D)
6.c Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C8(H8A,
 H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C14(H14A,
 H14B,H14C), C15(H15A,H15B,H15C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C)
;
_shelx_res_checksum              73367
_shelx_hkl_checksum              87034