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_4085253
_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 Ce1 N3 Si6'
_chemical_formula_sum            'C27 H72 Ce N3 Si6'
_chemical_formula_weight         747.53
_space_group_crystal_system      trigonal
_space_group_IT_number           161
_space_group_name_Hall           'R 3 -2"c'
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Olex2 1.2
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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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_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)
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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  -47.00   45.00   1.0000  180.0000
omega____ theta____ kappa____ phi______ frames
    -       21.3360  -57.0000 -150.0000 92

  2 omega   58.00   92.00   1.0000  180.0000
omega____ theta____ kappa____ phi______ frames
    -       21.3360   57.0000    0.0000 34

  3 omega  -96.00  -56.00   1.0000  180.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.7110  -19.0000  120.0000 40
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_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
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_diffrn_orient_matrix_UB_11      -0.0043513000
_diffrn_orient_matrix_UB_12      -0.0368542000
_diffrn_orient_matrix_UB_13      0.0033794000
_diffrn_orient_matrix_UB_21      -0.0377201000
_diffrn_orient_matrix_UB_22      -0.0143654000
_diffrn_orient_matrix_UB_23      0.0141742000
_diffrn_orient_matrix_UB_31      -0.0138000000
_diffrn_orient_matrix_UB_32      -0.0082723000
_diffrn_orient_matrix_UB_33      -0.0398324000
_diffrn_radiation_monochromator  mirror
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_diffrn_reflns_point_group_measured_fraction_full 0.701
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_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         25.346
_diffrn_reflns_theta_min         3.303
_diffrn_source                   'SuperNova (Mo) X-ray Source'
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_exptl_absorpt_process_details
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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    1.252
_exptl_crystal_description       needle
_exptl_crystal_F_000             2382
_exptl_crystal_size_max          0.1219
_exptl_crystal_size_mid          0.0385
_exptl_crystal_size_min          0.0305
_refine_diff_density_max         0.849
_refine_diff_density_min         -0.448
_refine_diff_density_rms         0.096
_refine_ls_abs_structure_details
;
 Flack x determined using 377 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.02(2)
_refine_ls_extinction_method     none
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_refine_ls_number_parameters     120
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_refine_ls_structure_factor_coef Fsqd
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'w=1/[\s^2^(Fo^2^)+(0.0264P)^2^] where P=(Fo^2^+2Fc^2^)/3'
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_reflns_Friedel_fraction_full    0.465
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_reflns_number_gt                1294
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_cod_data_source_file            om501123e_si_002.cif
_cod_data_source_block           11
_cod_depositor_comments
'Adding full bibliography for 4085243--4085254.cif.'
_cod_original_cell_volume        5950.9(15)
_cod_database_code               4085253
_manchester_internal_coll_name   adpm34
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_manchester_internal_coll_type   custom
_manchester_internal_coll_frame_time 180s
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_manchester_internal_coll_user   CAPG
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_manchester_internal_process_date 25/03/2014
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_manchester_internal_solution_date 18/07/2014
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_manchester_internal_refinement_date 18/07/2014
_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         'C27 H72 N3 Ce Si6'
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_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:
 C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C2(H2A,H2B,H2C), C6(H6A,H6B,H6C), C5(H5A,
 H5B,H5C), C9(H9A,H9B,H9C), C8(H8A,H8B,H8C), C7(H7A,H7B,H7C)
;
_shelx_res_checksum              77397
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_olex2_submission_special_instructions 'No special instructions were received'