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_4085252
_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         'C27 H72 La1 N3 Si6'
_chemical_formula_sum            'C27 H72 La N3 Si6'
_chemical_formula_weight         746.32
_space_group_crystal_system      trigonal
_space_group_IT_number           161
_space_group_name_Hall           'R 3 -2"c'
_space_group_name_H-M_alt        'R 3 c :H'
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Olex2 1.2
(compiled 2014.05.21 svn.r2940 for OlexSys, GUI svn.r4846)
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_cell_length_c                   16.7604(7)
_cell_measurement_reflns_used    2009
_cell_measurement_temperature    149.99(10)
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_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)
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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)
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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)
;
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_diffrn_measurement_details
;
  1 omega  -49.00   45.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       21.3360  -57.0000 -150.0000 94

  2 omega   65.00   92.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       21.3360   57.0000    0.0000 27
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_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
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_diffrn_orient_matrix_UB_12      0.0015953000
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_diffrn_orient_matrix_UB_22      -0.0392230000
_diffrn_orient_matrix_UB_23      0.0094117000
_diffrn_orient_matrix_UB_31      -0.0001672000
_diffrn_orient_matrix_UB_32      -0.0088306000
_diffrn_orient_matrix_UB_33      -0.0409615000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
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_diffrn_reflns_point_group_measured_fraction_full 0.636
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_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         25.348
_diffrn_reflns_theta_min         3.290
_diffrn_source                   'SuperNova (Mo) X-ray Source'
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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)
Numerical absorption correction based on gaussian integration over
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;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
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_exptl_crystal_density_diffrn    1.237
_exptl_crystal_description       needle
_exptl_crystal_F_000             2376
_exptl_crystal_size_max          0.3181
_exptl_crystal_size_mid          0.1105
_exptl_crystal_size_min          0.0937
_refine_diff_density_max         0.536
_refine_diff_density_min         -0.560
_refine_diff_density_rms         0.068
_refine_ls_abs_structure_details
;
 Flack x determined using 357 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.015(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
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_refine_ls_matrix_type           full
_refine_ls_number_parameters     120
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_refine_ls_R_factor_all          0.0328
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_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0226P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
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_cod_data_source_file            om501123e_si_002.cif
_cod_data_source_block           10
_cod_depositor_comments
'Adding full bibliography for 4085243--4085254.cif.'
_cod_original_cell_volume        6013.4(5)
_cod_database_code               4085252
_manchester_internal_coll_name   adpm33
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_manchester_internal_coll_type   custom
_manchester_internal_coll_frame_time 8s
_manchester_internal_coll_frame_width 1
_manchester_internal_coll_frame_method '\w scans'
_manchester_internal_coll_user   CAPG
_manchester_internal_coll_date   24/03/2014
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_manchester_internal_process_date 25/03/2014
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_manchester_internal_solution_date 03/04/2014
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_manchester_internal_refinement_date 03/04/2014
_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         'C27 H72 N3 La Si6'
_reflns_odcompleteness_completeness 99.73
_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.a 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), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C)
;
_shelx_res_checksum              37770
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_olex2_submission_special_instructions 'No special instructions were received'