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_4085251
_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         '2(C18 H48 I La N2 Si4)'
_chemical_formula_sum            'C36 H96 I2 La2 N4 Si8'
_chemical_formula_weight         1341.50
_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             2014-09-30
_audit_creation_method
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_cell_angle_alpha                94.293(5)
_cell_angle_beta                 96.373(5)
_cell_angle_gamma                99.075(5)
_cell_formula_units_Z            2
_cell_length_a                   9.1458(6)
_cell_length_b                   14.9960(9)
_cell_length_c                   22.8837(15)
_cell_measurement_reflns_used    3842
_cell_measurement_temperature    150.01(16)
_cell_measurement_theta_max      27.2480
_cell_measurement_theta_min      3.3830
_cell_volume                     3066.4(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.01(16)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0714
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.928
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -88.00   37.00   1.0000   63.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.7110  -19.0000  -60.0000 125

  2 omega   20.00   66.00   1.0000   63.0000
omega____ theta____ kappa____ phi______ frames
    -       21.3360  -99.0000   30.0000 46

  3 omega  -12.00   94.00   1.0000   63.0000
omega____ theta____ kappa____ phi______ frames
    -       21.3360   77.0000  -90.0000 106

  4 omega   34.00  103.00   1.0000   63.0000
omega____ theta____ kappa____ phi______ frames
    -       21.3360 -178.0000 -120.0000 69

  5 omega -100.00  -75.00   1.0000   63.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.7110 -178.0000 -120.0000 25

  6 omega  -11.00   95.00   1.0000   63.0000
omega____ theta____ kappa____ phi______ frames
    -       21.3360   37.0000 -180.0000 106
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0171893000
_diffrn_orient_matrix_UB_12      0.0028644000
_diffrn_orient_matrix_UB_13      0.0294834000
_diffrn_orient_matrix_UB_21      -0.0185916000
_diffrn_orient_matrix_UB_22      -0.0479497000
_diffrn_orient_matrix_UB_23      -0.0017896000
_diffrn_orient_matrix_UB_31      0.0749970000
_diffrn_orient_matrix_UB_32      -0.0027221000
_diffrn_orient_matrix_UB_33      0.0104377000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1574
_diffrn_reflns_av_unetI/netI     0.2233
_diffrn_reflns_Laue_measured_fraction_full 0.928
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            23282
_diffrn_reflns_point_group_measured_fraction_full 0.928
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         25.349
_diffrn_reflns_theta_min         2.986
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.563
_exptl_absorpt_correction_T_max  0.952
_exptl_absorpt_correction_T_min  0.554
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.453
_exptl_crystal_description
;
;
_exptl_crystal_F_000             1344
_exptl_crystal_size_max          0.5148
_exptl_crystal_size_mid          0.0413
_exptl_crystal_size_min          0.0263
_refine_diff_density_max         1.522
_refine_diff_density_min         -0.984
_refine_diff_density_rms         0.198
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.839
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     469
_refine_ls_number_reflns         11184
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      0.839
_refine_ls_R_factor_all          0.1308
_refine_ls_R_factor_gt           0.0591
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w=1/[\s^2^(Fo^2^)] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1005
_refine_ls_wR_factor_ref         0.1343
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5943
_reflns_number_total             11184
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om501123e_si_002.cif
_cod_data_source_block           9
_cod_depositor_comments
'Adding full bibliography for 4085243--4085254.cif.'
_cod_database_code               4085251
_manchester_internal_coll_name   adpm29
_manchester_internal_coll_client CAPG/DPM
_manchester_internal_coll_type   custom
_manchester_internal_coll_frame_time 63s
_manchester_internal_coll_frame_width 1
_manchester_internal_coll_frame_method '\w scans'
_manchester_internal_coll_user   CAPG
_manchester_internal_coll_date   24/02/2014
_manchester_internal_process_user CAPG/FO
_manchester_internal_process_date 30/07/2014
_manchester_internal_solution_user CAPG/FO
_manchester_internal_solution_date 30/07/2014
_manchester_internal_refinement_user CAPG/FO
_manchester_internal_refinement_date 30/07/2014
_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         'La I Si4 N2 C18 H48'
_reflns_odcompleteness_completeness 99.76
_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. Rigid body (RIGU) restrains
 C26, C25, C27, Si6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3.a Me refined with riding coordinates:
 C5(H5A,H5B,H5C), C15(H15A,H15B,H15C), C7(H7A,H7B,H7C), C14(H14A,H14B,H14C),
 C4(H4A,H4B,H4C), C2(H2A,H2B,H2C), C9(H9A,H9B,H9C), C8(H8A,H8B,H8C), C3(H3A,H3B,
 H3C), C32(H32A,H32B,H32C), C6(H6A,H6B,H6C), C35(H35A,H35B,H35C), C23(H23A,H23B,
 H23C), C24(H24A,H24B,H24C), C16(H16A,H16B,H16C), C18(H18A,H18B,H18C), C27(H27A,
 H27B,H27C), C25(H25A,H25B,H25C), C34(H34A,H34B,H34C), C17(H17A,H17B,H17C),
 C33(H33A,H33B,H33C), C11(H11A,H11B,H11C), C26(H26A,H26B,H26C), C36(H36A,H36B,
 H36C), C30(H30A,H30B,H30C), C29(H29A,H29B,H29C), C12(H12A,H12B,H12C), C20(H20A,
 H20B,H20C), C13(H13A,H13B,H13C), C31(H31A,H31B,H31C), C21(H21A,H21B,H21C),
 C22(H22A,H22B,H22C)
;
_shelx_res_checksum              93214
_shelx_hkl_checksum              69987
_olex2_submission_special_instructions 'No special instructions were received'