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_4085249
_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         'C18 H42 K N Si2'
_chemical_formula_sum            'C18 H42 K N Si2'
_chemical_formula_weight         367.80
_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_Hall           'P 2 2ab'
_space_group_name_H-M_alt        'P 21 21 2'
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2014-10-02
_audit_creation_method
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.400(2)
_cell_length_b                   9.7973(11)
_cell_length_c                   7.6315(11)
_cell_measurement_reflns_used    766
_cell_measurement_temperature    150.02(11)
_cell_measurement_theta_max      25.4000
_cell_measurement_theta_min      3.3780
_cell_volume                     1151.4(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
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 8.0714
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.788
_diffrn_measurement_details
;
  1 omega  -94.00  -52.00   1.0000  165.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.7110 -178.0000  -60.0000 42

  2 omega  -39.00   68.00   1.0000  165.0000
omega____ theta____ kappa____ phi______ frames
    -       21.3360   19.0000 -120.0000 107
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0371991000
_diffrn_orient_matrix_UB_12      -0.0370822000
_diffrn_orient_matrix_UB_13      0.0269860000
_diffrn_orient_matrix_UB_21      -0.0165668000
_diffrn_orient_matrix_UB_22      0.0024947000
_diffrn_orient_matrix_UB_23      -0.0867579000
_diffrn_orient_matrix_UB_31      0.0215939000
_diffrn_orient_matrix_UB_32      -0.0620512000
_diffrn_orient_matrix_UB_33      -0.0196526000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0403
_diffrn_reflns_av_unetI/netI     0.0925
_diffrn_reflns_Laue_measured_fraction_full 0.893
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            2665
_diffrn_reflns_point_group_measured_fraction_full 0.843
_diffrn_reflns_point_group_measured_fraction_max 0.940
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         25.008
_diffrn_reflns_theta_min         3.384
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.334
_exptl_absorpt_correction_T_max  0.994
_exptl_absorpt_correction_T_min  0.802
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.061
_exptl_crystal_description       needle
_exptl_crystal_F_000             408
_exptl_crystal_size_max          0.1817
_exptl_crystal_size_mid          0.0879
_exptl_crystal_size_min          0.0543
_refine_diff_density_max         0.576
_refine_diff_density_min         -0.252
_refine_diff_density_rms         0.064
_refine_ls_abs_structure_details
;
 Flack x determined using 422 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.32(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     107
_refine_ls_number_reflns         1912
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0917
_refine_ls_R_factor_gt           0.0688
_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^)+(0.1011P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1762
_refine_ls_wR_factor_ref         0.1951
_reflns_Friedel_coverage         0.608
_reflns_Friedel_fraction_full    0.772
_reflns_Friedel_fraction_max     0.867
_reflns_number_gt                1472
_reflns_number_total             1912
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om501123e_si_002.cif
_cod_data_source_block           7
_cod_depositor_comments
'Adding full bibliography for 4085243--4085254.cif.'
_cod_original_cell_volume        1151.5(3)
_cod_database_code               4085249
_manchester_internal_coll_name   adpm38
_manchester_internal_coll_client CAPG/DPM
_manchester_internal_coll_type   custom
_manchester_internal_coll_frame_time 165s
_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
_manchester_internal_process_user CAPG
_manchester_internal_process_date 25/03/2014
_manchester_internal_solution_user CAPG
_manchester_internal_solution_date 25/03/2014
_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         'K N Si2 C18 H42'
_reflns_odcompleteness_completeness 98.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C8-C7 \\sim C9-C7 \\sim C3-C1 \\sim C2-C1 \\sim C5-C4 \\sim C6-C4
 with sigma of 0.002
3.a Ternary CH refined with riding coordinates:
 C1(H1), C4(H4), C7(H7)
3.b 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)
;
_shelx_res_checksum              33888
_shelx_hkl_checksum              4082
_olex2_exptl_crystal_mounting_method 'From fomblin on microscope slide.'
_olex2_submission_special_instructions 'No special instructions were received'