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_4085243
_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         'C36 H96 Li6 N6 Si6'
_chemical_formula_sum            'C36 H96 Li6 N6 Si6'
_chemical_formula_weight         823.36
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2014-08-06
_audit_creation_method
;
Olex2 1.2
(compiled 2014.05.21 svn.r2940 for OlexSys, GUI svn.r4846)
;
_cell_angle_alpha                90
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_cell_formula_units_Z            2
_cell_length_a                   12.3694(11)
_cell_length_b                   19.5146(10)
_cell_length_c                   13.2445(11)
_cell_measurement_reflns_used    4694
_cell_measurement_temperature    100.3(5)
_cell_measurement_theta_max      27.0720
_cell_measurement_theta_min      3.3430
_cell_volume                     2835.3(5)
_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28a (release 18-03-2013 CrysAlis171 .NET)
(compiled Mar 18 2013,11:47:30)
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_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28a (release 18-03-2013 CrysAlis171 .NET)
(compiled Mar 18 2013,11:47:30)
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_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28a (release 18-03-2013 CrysAlis171 .NET)
(compiled Mar 18 2013,11:47:30)
;
_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      100.3(5)
_diffrn_detector_area_resol_mean 8.3367
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega -117.00   -6.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.0746  -77.0000  -60.0000 111

  2 omega   34.00   69.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.0746  179.0000  -60.0000 35

  3 omega -113.00  -32.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.0746  179.0000  -60.0000 81

  4 omega  -57.00   51.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       22.4027  -37.0000  150.0000 108
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0124905000
_diffrn_orient_matrix_UB_12      0.0017487000
_diffrn_orient_matrix_UB_13      0.0578384000
_diffrn_orient_matrix_UB_21      0.0579296000
_diffrn_orient_matrix_UB_22      0.0145043000
_diffrn_orient_matrix_UB_23      0.0144796000
_diffrn_orient_matrix_UB_31      -0.0259822000
_diffrn_orient_matrix_UB_32      0.0332973000
_diffrn_orient_matrix_UB_33      -0.0095578000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0488
_diffrn_reflns_av_unetI/netI     0.0534
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            14690
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         3.087
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.174
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80335
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28a (release 18-03-2013 CrysAlis171 .NET)
(compiled Mar 18 2013,11:47:30)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    0.964
_exptl_crystal_description
;
;
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.4778
_exptl_crystal_size_mid          0.3961
_exptl_crystal_size_min          0.3079
_refine_diff_density_max         0.462
_refine_diff_density_min         -0.274
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         5174
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0649
_refine_ls_R_factor_gt           0.0479
_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^)+(0.0618P)^2^+1.1543P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1172
_refine_ls_wR_factor_ref         0.1308
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4052
_reflns_number_total             5174
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om501123e_si_002.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 4085243--4085254.cif.'
_cod_database_code               4085243
_manchester_internal_coll_name   odpm1
_manchester_internal_coll_client SL/DPM
_manchester_internal_coll_type   custom
_manchester_internal_coll_frame_time 60s
_manchester_internal_coll_frame_width 1
_manchester_internal_coll_frame_method '\w scans'
_manchester_internal_coll_user   DPM
_manchester_internal_coll_date   31/07/2013
_manchester_internal_process_user DPM
_manchester_internal_process_date 01/08/2013
_manchester_internal_solution_user DPM
_manchester_internal_solution_date 09/08/2013
_manchester_internal_refinement_user DPM/FO
_manchester_internal_refinement_date 31/07/2014
_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         'C12 H31 N Si2'
_reflns_odcompleteness_completeness 99.77
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N1-H1
 0.88 with sigma of 0.02
 N2-H2
 0.88 with sigma of 0.02
 N3-H3
 0.88 with sigma of 0.02
3.a Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C6(H6A,
 H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C10(H10A,H10B,H10C), C11(H11A,H11B,
 H11C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C16(H16A,
 H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C)
;
_shelx_res_checksum              22341
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_olex2_submission_special_instructions 'No special instructions were received'