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_4347963
_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         'C45 H102 N3 O Si4 Sm'
_chemical_formula_sum            'C45 H102 N3 O Si4 Sm'
_chemical_formula_weight         964.00
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-02-09
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                90
_cell_angle_beta                 99.319(3)
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   19.5621(6)
_cell_length_b                   19.8625(5)
_cell_length_c                   41.3879(14)
_cell_measurement_reflns_used    14526
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.3100
_cell_measurement_theta_min      3.6220
_cell_volume                     15869.1(8)
_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    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1636
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega    4.00   88.00   0.8000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       11.5361   37.0000  -60.0000 105

  2 omega  -12.00   84.00   0.8000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       11.5361   37.0000   60.0000 120

  3 omega    6.00   40.40   0.8000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       11.5361  -57.0000  150.0000 43

  4 omega  -45.00   35.00   0.8000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       11.5361  -57.0000  120.0000 100

  5 omega  -82.00  -54.80   0.8000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -12.0049 -178.0000  -90.0000 34

  6 omega  -77.00  -37.80   0.8000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       11.5361  178.0000 -120.0000 49
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0223291000
_diffrn_orient_matrix_UB_12      -0.0230104000
_diffrn_orient_matrix_UB_13      -0.0062509000
_diffrn_orient_matrix_UB_21      0.0021505000
_diffrn_orient_matrix_UB_22      -0.0195118000
_diffrn_orient_matrix_UB_23      0.0144836000
_diffrn_orient_matrix_UB_31      -0.0290892000
_diffrn_orient_matrix_UB_32      -0.0191111000
_diffrn_orient_matrix_UB_33      -0.0072653000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0717
_diffrn_reflns_av_unetI/netI     0.0704
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            68720
_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         3.359
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.234
_exptl_absorpt_correction_T_max  0.882
_exptl_absorpt_correction_T_min  0.759
_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 red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.210
_exptl_crystal_description       cube
_exptl_crystal_F_000             6228
_exptl_crystal_size_max          0.2104
_exptl_crystal_size_mid          0.1998
_exptl_crystal_size_min          0.104
_refine_diff_density_max         0.637
_refine_diff_density_min         -0.494
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     816
_refine_ls_number_reflns         14492
_refine_ls_number_restraints     133
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0648
_refine_ls_R_factor_gt           0.0417
_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^)+(0.0187P)^2^+17.0450P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0674
_refine_ls_wR_factor_ref         0.0740
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11234
_reflns_number_total             14492
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00808_si_002.cif
_cod_data_source_block           5
_cod_original_cell_volume        15869.0(8)
_cod_database_code               4347963
_manchester_internal_coll_name   adpm46/odpm46
_manchester_internal_coll_client CAPG
_manchester_internal_coll_type   custom
_manchester_internal_coll_frame_time 4.0
_manchester_internal_coll_frame_width 0.8
_manchester_internal_coll_frame_method '\w scans'
_manchester_internal_coll_user   CAPG
_manchester_internal_coll_date   03/02/16
_manchester_internal_process_user CAPG
_manchester_internal_process_date 03/02/16
_manchester_internal_solution_user CAPG
_manchester_internal_solution_date 04/02/16
_manchester_internal_refinement_user CAPG
_manchester_internal_refinement_date 09/02/16
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         Sm(N(SiC9H21)2)2NC9H18O
_reflns_odcompleteness_completeness 99.75
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C61-C55 \\sim C60-C55 \\sim C69_$2-C68_$2 \\sim C70_$2-C68_$2 \\sim
C71_$2-C64_$2 \\sim C72_$2-
 C64_$2 \\sim C62-C59 \\sim C59-C63
 with sigma of 0.02
 N5-C68 \\sim N5-C64 \\sim N4_$3-C55_$3 \\sim N4_$3-C59_$3
 with sigma of 0.02
 C67-C68 \\sim C65-C64 \\sim C56_$3-C55_$3 \\sim C58_$3-C59_$3
 with sigma of 0.02
 C56-C57 \\sim C58-C57 \\sim C67_$2-C66_$2 \\sim C65_$2-C66_$2
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 O2, N5, N5, C64, C64, C65, C65, C66, C66, C67, C67, C68, C68, C69, C69, C70,
 C70, C71, C71, C72, C72
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: N5(0.5) C64(0.5) C65(0.5) H65A(0.5) H65B(0.5) C66(0.5) H66A(0.5)
 H66B(0.5) C67(0.5) H67A(0.5) H67B(0.5) C68(0.5) C69(0.5) H69A(0.5) H69B(0.5)
 H69C(0.5) C70(0.5) H70A(0.5) H70B(0.5) H70C(0.5) C71(0.5) H71A(0.5) H71B(0.5)
 H71C(0.5) C72(0.5) H72A(0.5) H72B(0.5) H72C(0.5)
5.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), C37(H37), C40(H40), C43(H43), C46(H46),
  C49(H49), C52(H52)
5.b Secondary CH2 refined with riding coordinates:
 C56(H56A,H56B), C57(H57A,H57B), C58(H58A,H58B), C65(H65A,H65B), C66(H66A,
 H66B), C67(H67A,H67B)
5.c Me refined with riding coordinates:
 C69(H69A,H69B,H69C), C70(H70A,H70B,H70C), C71(H71A,H71B,H71C), C72(H72A,H72B,
 H72C)
5.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), C60(H60A,H60B,H60C), C61(H61A,H61B,H61C), C62(H62A,H62B,
 H62C), C63(H63A,H63B,H63C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C41(H41A,
 H41B,H41C), C42(H42A,H42B,H42C), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C),
 C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C50(H50A,H50B,H50C), C51(H51A,H51B,
 H51C), C53(H53A,H53B,H53C), C54(H54A,H54B,H54C)
;
_shelx_res_checksum              2660
_shelx_hkl_checksum              77025
_olex2_date_sample_data_collection 2016-02-03
_olex2_exptl_crystal_mounting_method 'From fomblin on a microscope slide.'
_olex2_submission_special_instructions 'No special instructions were received'