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_4347959
_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 Eu N2 Si4'
_chemical_formula_sum            'C36 H84 Eu N2 Si4'
_chemical_formula_weight         809.37
_chemical_name_systematic        bis(bis(triisopropylamido)europium(II)
_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             2016-01-06
_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                   20.5188(7)
_cell_length_b                   16.0971(10)
_cell_length_c                   26.4535(10)
_cell_measurement_reflns_used    7205
_cell_measurement_temperature    150.01(11)
_cell_measurement_theta_max      27.8260
_cell_measurement_theta_min      3.5480
_cell_volume                     8737.4(7)
_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)'
_diffrn_ambient_temperature      150.01(11)
_diffrn_detector_area_resol_mean 8.0714
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega   58.00   86.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       19.4509 -178.0000   90.0000 28

  2 omega   14.00   56.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       19.4509   57.0000  -60.0000 42

  3 omega  -28.00   92.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       19.4509    0.0000   90.0000 120
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0280283000
_diffrn_orient_matrix_UB_12      0.0209248000
_diffrn_orient_matrix_UB_13      0.0091549000
_diffrn_orient_matrix_UB_21      0.0062397000
_diffrn_orient_matrix_UB_22      -0.0154593000
_diffrn_orient_matrix_UB_23      0.0246293000
_diffrn_orient_matrix_UB_31      0.0192361000
_diffrn_orient_matrix_UB_32      0.0355839000
_diffrn_orient_matrix_UB_33      0.0053149000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0817
_diffrn_reflns_av_unetI/netI     0.0689
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            27090
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         3.353
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.570
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.507
_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 green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.231
_exptl_crystal_description       plank
_exptl_crystal_F_000             3464
_exptl_crystal_size_max          0.9088
_exptl_crystal_size_mid          0.6064
_exptl_crystal_size_min          0.1649
_refine_diff_density_max         1.098
_refine_diff_density_min         -0.817
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     416
_refine_ls_number_reflns         7976
_refine_ls_number_restraints     576
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0700
_refine_ls_R_factor_gt           0.0487
_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^)+(0.0555P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1135
_refine_ls_wR_factor_ref         0.1264
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5939
_reflns_number_total             7976
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00808_si_002.cif
_cod_data_source_block           2-150K
_cod_database_code               4347959
_manchester_internal_coll_name   adpm107
_manchester_internal_coll_client CAPG/CAPG
_manchester_internal_coll_type   custom
_manchester_internal_coll_frame_time 5.00
_manchester_internal_coll_frame_width 1
_manchester_internal_coll_frame_method '\w scans'
_manchester_internal_coll_user   CAPG
_manchester_internal_coll_date   28/11/14
_manchester_internal_process_user CAPG
_manchester_internal_process_date 29/11/14
_manchester_internal_solution_user CAPG
_manchester_internal_solution_date 29/11/14
_manchester_internal_refinement_user CAPG
_manchester_internal_refinement_date 04/06/15
_manchester_internal_validation_user CAPG
_manchester_internal_validation_date 04/06/15
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         C60S1O4N4H60
_reflns_odcompleteness_completeness 99.42
_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(Eu1B) = Uanis(Eu1A)
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(Eu1B)=1-FVAR(1)
 Sof(Eu1A)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C25(H25), C34(H34), C7(H7), C13(H13), C4(H4), C16(H16), C22(H22), C31(H31),
 C28(H28), C10(H10), C19(H19), C1(H1)
5.b Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C8(H8A,H8B,H8C), C15(H15A,H15B,H15C), C23(H23C,H23A,H23B),
 C26(H26B,H26A,H26C), C17(H17A,H17B,H17C), C24(H24B,H24A,H24C), C6(H6A,H6B,H6C),
  C3(H3A,H3B,H3C), C27(H27A,H27C,H27B), C11(H11A,H11B,H11C), C14(H14A,H14B,
 H14C), C2(H2A,H2B,H2C), C21(H21B,H21A,H21C), C18(H18C,H18A,H18B), C20(H20A,
 H20C,H20B), C12(H12A,H12B,H12C), C33(H33C,H33A,H33B), C32(H32B,H32A,H32C),
 C35(H35C,H35A,H35B), C29(H29A,H29C,H29B), C36(H36B,H36A,H36C), C5(H5A,H5B,H5C),
  C30(H30B,H30A,H30C)
;
_shelx_res_checksum              41290
_shelx_hkl_checksum              11373
_ins_header
;
TITL adpm107 in Pbca 
REM Pbca (#61, found as Pcab in ba-c setting)
CELL 0.71073  20.518795  16.097071  26.453547  90.0000  90.0000  90.0000
ZERR    7.00   0.000732   0.000966   0.000986   0.0000   0.0000   0.0000
LATT  1
SYMM -x+1/2,-y, z+1/2 
SYMM -x, y+1/2,-z+1/2 
SYMM  x+1/2,-y+1/2,-z 
SFAC C H N O S
UNIT 420.00 420.00 28.00 28.00 7.00
TREF
HKLF 4
END
;
_olex2_exptl_crystal_mounting_method 'From fomblin on microscope slide.'
_olex2_submission_special_instructions 'No special instructions were received'