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_4085248
_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         'C15 H36 K N Si2'
_chemical_formula_sum            'C15 H36 K N Si2'
_chemical_formula_weight         325.73
_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   geom
_audit_creation_date             2014-08-07
_audit_creation_method
;
Olex2 1.2
(compiled 2014.05.21 svn.r2940 for OlexSys, GUI svn.r4846)
;
_cell_angle_alpha                90
_cell_angle_beta                 109.225(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.8947(12)
_cell_length_b                   12.0009(14)
_cell_length_c                   15.3957(16)
_cell_measurement_reflns_used    1740
_cell_measurement_temperature    139(15)
_cell_measurement_theta_max      24.7380
_cell_measurement_theta_min      3.6810
_cell_volume                     2075.1(4)
_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      139(15)
_diffrn_detector_area_resol_mean 5.1852
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_details
;
  1 omega   15.00   75.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -        9.6159   57.0000 -150.0000 60

  2 omega  -39.00   55.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       -9.7722   77.0000  -60.0000 94
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0404158000
_diffrn_orient_matrix_UB_12      -0.0195155000
_diffrn_orient_matrix_UB_13      0.0216832000
_diffrn_orient_matrix_UB_21      0.0004462000
_diffrn_orient_matrix_UB_22      0.0532084000
_diffrn_orient_matrix_UB_23      0.0201814000
_diffrn_orient_matrix_UB_31      -0.0485455000
_diffrn_orient_matrix_UB_32      0.0167092000
_diffrn_orient_matrix_UB_33      -0.0387758000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0738
_diffrn_reflns_av_unetI/netI     0.1646
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7612
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.349
_diffrn_reflns_theta_min         3.132
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.363
_exptl_absorpt_correction_T_max  0.998
_exptl_absorpt_correction_T_min  0.994
_exptl_absorpt_correction_type   analytical
_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)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.043
_exptl_crystal_description
;
;
_exptl_crystal_F_000             720
_exptl_crystal_size_max          0.2667
_exptl_crystal_size_mid          0.2006
_exptl_crystal_size_min          0.0658
_refine_diff_density_max         0.343
_refine_diff_density_min         -0.321
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     183
_refine_ls_number_reflns         3744
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.1598
_refine_ls_R_factor_gt           0.0847
_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^)+1.6032P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1097
_refine_ls_wR_factor_ref         0.1460
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2085
_reflns_number_total             3744
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om501123e_si_002.cif
_cod_data_source_block           6
_cod_depositor_comments
'Adding full bibliography for 4085243--4085254.cif.'
_cod_database_code               4085248
_manchester_internal_coll_name   adpm8
_manchester_internal_coll_client CAPG/DPM
_manchester_internal_coll_type   custom
_manchester_internal_coll_frame_time 10
_manchester_internal_coll_frame_width 1
_manchester_internal_coll_frame_method '\w scans'
_manchester_internal_coll_user   CAPG
_manchester_internal_coll_date   13/11/2013
_manchester_internal_process_user CAPG
_manchester_internal_process_date 17/11/2013
_manchester_internal_solution_user CAPG
_manchester_internal_solution_date 15/01/2014
_manchester_internal_refinement_user CAPG
_manchester_internal_refinement_date 15/01/2014
_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         C15Si2N1Li1H36
_reflns_odcompleteness_completeness 98.08
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.30
_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.a Ternary CH refined with riding coordinates:
 C1(H1), C4(H4), C7(H7)
2.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), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C13(H13A,
 H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C)
;
_shelx_res_checksum              4691
_shelx_hkl_checksum              12630
_ins_header
;
TITL adpm8 in P2(1)/c 
REM P2(1)/c (#14 in standard setting)
CELL 0.71073  11.894692  12.000912  15.395659  90.0000 109.2246  90.0000
ZERR    6.00   0.001222   0.001416   0.001556   0.0000   0.0112   0.0000
LATT  1
SYMM -x, y+1/2,-z+1/2 
SFAC C H Li N Si
UNIT 90.00 216.00 6.00 6.00 12.00
TREF
HKLF 4
END
;
_olex2_submission_special_instructions 'No special instructions were received'