Physicochemical Properties of Near-Linear Lanthanide(II) Bis(silylamide) Complexes (Ln = Sm, Eu, Tm, Yb).
Goodwin, Conrad A. P.; Chilton, Nicholas F.; Vettese, Gianni F.; Moreno Pineda, Eufemio; Crowe, Iain F.; Ziller, Joseph W.; Winpenny, Richard E. P.; Evans, William J.; Mills, David P.; Inorganic chemistry 55 (2016) 10057–10067; doi:10.1021/acs.inorgchem.6b00808

data_4347962
_publ_section_title
;
 Physicochemical Properties of Near-Linear Lanthanide(II) Bis(silylamide)
 Complexes (Ln = Sm, Eu, Tm, Yb).
;
_journal_issue                   20
_journal_name_full               'Inorganic chemistry'
_journal_page_first              10057
_journal_page_last               10067
_journal_paper_doi               10.1021/acs.inorgchem.6b00808
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C36 H84 N2 Si4 Yb'
_chemical_formula_sum            'C36 H84 N2 Si4 Yb'
_chemical_formula_weight         830.45
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-02-08
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   20.4979(7)
_cell_length_b                   16.1891(6)
_cell_length_c                   26.1295(8)
_cell_measurement_reflns_used    6851
_cell_measurement_temperature    150.02(10)
_cell_measurement_theta_max      26.8150
_cell_measurement_theta_min      3.7030
_cell_volume                     8670.9(5)
_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, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.02(10)
_diffrn_detector_area_resol_mean 8.0714
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
  1 omega  -20.00   61.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       18.7038  -99.0000   90.0000 81

  2 omega  -24.00   91.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       18.7038   19.0000    0.0000 115
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0105106000
_diffrn_orient_matrix_UB_12      0.0025152000
_diffrn_orient_matrix_UB_13      0.0258302000
_diffrn_orient_matrix_UB_21      0.0296376000
_diffrn_orient_matrix_UB_22      0.0183724000
_diffrn_orient_matrix_UB_23      -0.0081089000
_diffrn_orient_matrix_UB_31      -0.0143906000
_diffrn_orient_matrix_UB_32      0.0397070000
_diffrn_orient_matrix_UB_33      0.0021174000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0629
_diffrn_reflns_av_unetI/netI     0.0707
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            29531
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         3.207
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.292
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.801
_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            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.272
_exptl_crystal_description
;
;
_exptl_crystal_F_000             3520
_exptl_crystal_size_max          0.2294
_exptl_crystal_size_mid          0.2221
_exptl_crystal_size_min          0.0785
_refine_diff_density_max         0.711
_refine_diff_density_min         -0.605
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     422
_refine_ls_number_reflns         7918
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0649
_refine_ls_R_factor_gt           0.0403
_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^)+(0.0199P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0700
_refine_ls_wR_factor_ref         0.0826
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5698
_reflns_number_total             7918
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00808_si_002.cif
_cod_data_source_block           4
_cod_original_cell_volume        8670.8(5)
_cod_database_code               4347962
_manchester_internal_coll_name   adpm263
_manchester_internal_coll_client CAPG
_manchester_internal_coll_type   custom
_manchester_internal_coll_frame_time 4s
_manchester_internal_coll_frame_width 1
_manchester_internal_coll_frame_method '\w scans'
_manchester_internal_coll_user   CAPG
_manchester_internal_coll_date   22/10/2015
_manchester_internal_process_user CAPG
_manchester_internal_process_date 22/10/2015
_manchester_internal_solution_user CAPG
_manchester_internal_solution_date 23/10/2015
_manchester_internal_refinement_user CAPG
_manchester_internal_refinement_date 26/10/2015
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         Yb(N(SiC9H21)2)2
_reflns_odcompleteness_completeness 99.26
_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. Uiso/Uaniso restraints and constraints
Uanis(Yb1B) \\sim Ueq: with sigma of 0.006 and sigma for terminal atoms of 0.008
3. Others
 Sof(Yb1A)=1-FVAR(1)
 Sof(Yb1B)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C1(H1), C4(H4), C7(H7), C10(H10), C13(H13), C16(H16), C19(H19), C22(H22),
 C25(H25), C28(H28), C31(H31), C34(H34)
4.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), C14(H14A,
 H14B,H14C), C15(H15A,H15B,H15C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C),
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C29(H29A,H29B,H29C), C30(H30A,
 H30B,H30C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C35(H35A,H35B,H35C),
 C36(H36A,H36B,H36C)
;
_shelx_res_checksum              1584
_shelx_hkl_checksum              29111
_olex2_exptl_crystal_mounting_method 'From fomblin on microscope slide.'
_olex2_submission_special_instructions 'No special instructions were received'