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_4347964
_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         'C48 H94 N4 Si4 Sm'
_chemical_formula_sum            'C48 H94 N4 Si4 Sm'
_chemical_formula_weight         989.98
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-06-04
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 106.927(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.9505(5)
_cell_length_b                   19.0546(6)
_cell_length_c                   21.3221(7)
_cell_measurement_reflns_used    5880
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      26.7470
_cell_measurement_theta_min      3.5650
_cell_volume                     5422.3(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      150.01(10)
_diffrn_detector_area_resol_mean 8.0714
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega   20.00   89.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8601   19.0000  -30.0000 69

  2 omega   18.00   61.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8601  -99.0000  -30.0000 43

  3 omega  -43.00  -16.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.7663   37.0000 -150.0000 27

  4 omega   -8.00   89.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8601   77.0000 -150.0000 97
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0352463000
_diffrn_orient_matrix_UB_12      0.0267034000
_diffrn_orient_matrix_UB_13      0.0004824000
_diffrn_orient_matrix_UB_21      0.0372384000
_diffrn_orient_matrix_UB_22      0.0258703000
_diffrn_orient_matrix_UB_23      0.0017801000
_diffrn_orient_matrix_UB_31      -0.0140771000
_diffrn_orient_matrix_UB_32      0.0016690000
_diffrn_orient_matrix_UB_33      -0.0347131000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0550
_diffrn_reflns_av_unetI/netI     0.0967
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            23874
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.302
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.205
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.790
_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 violet'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.213
_exptl_crystal_description       prism
_exptl_crystal_F_000             2112
_exptl_crystal_recrystallization_method 'Dichroic blue/purple hexagonal prisms.'
_exptl_crystal_size_max          0.1916
_exptl_crystal_size_mid          0.1672
_exptl_crystal_size_min          0.0522
_refine_diff_density_max         0.938
_refine_diff_density_min         -0.853
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     514
_refine_ls_number_reflns         11081
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0814
_refine_ls_R_factor_gt           0.0483
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0166P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0727
_refine_ls_wR_factor_ref         0.0839
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7904
_reflns_number_total             11081
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00808_si_002.cif
_cod_data_source_block           6
_cod_database_code               4347964
_manchester_internal_coll_name   adpm121
_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   28/01/15
_manchester_internal_process_user CAPG
_manchester_internal_process_date 28/01/15
_manchester_internal_solution_user CAPG
_manchester_internal_solution_date 28/01/15
_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         '(Sm(N(SiC9H21)2)2) C12H10N2'
_reflns_odcompleteness_completeness 99.72
_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.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)
2.b Aromatic/amide H refined with riding coordinates:
 C39(H39), C38(H38), C42(H42), C41(H41), C40(H40), C44(H44), C45(H45),
 C46(H46), C47(H47), C48(H48)
2.c Fitted hexagon refined as free rotating group:
 C39(C38,C37,C42,C41,C40), C43(C44,C45,C46,C47,C48)
2.d 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              63345
_shelx_hkl_checksum              45882
_olex2_exptl_crystal_mounting_method 'From fomblin on microscope slide.'
_olex2_submission_special_instructions 'No special instructions were received'