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_4347965
_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         'C88 H124 N2 O4 Si4 Sm2'
_chemical_formula_sum            'C88 H124 N2 O4 Si4 Sm2'
_chemical_formula_weight         1686.94
_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             2014-11-12
_audit_creation_method
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_cell_angle_alpha                90
_cell_angle_beta                 106.146(16)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.605(2)
_cell_length_b                   18.611(2)
_cell_length_c                   15.900(2)
_cell_measurement_reflns_used    2118
_cell_measurement_temperature    150.02(10)
_cell_measurement_theta_max      24.0820
_cell_measurement_theta_min      3.5780
_cell_volume                     4151.4(10)
_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
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
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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      150.02(10)
_diffrn_detector_area_resol_mean 8.0714
_diffrn_measured_fraction_theta_full 0.9966
_diffrn_measured_fraction_theta_max 0.8145
_diffrn_measurement_details
;
  1 omega  -91.00   26.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.3571  -19.0000    0.0000 117

  2 omega  -78.00   42.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.3571    0.0000   90.0000 120

  3 omega  -49.00   39.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       19.4509  -57.0000 -180.0000 88
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0232611000
_diffrn_orient_matrix_UB_12      0.0301316000
_diffrn_orient_matrix_UB_13      -0.0120818000
_diffrn_orient_matrix_UB_21      -0.0372159000
_diffrn_orient_matrix_UB_22      0.0032234000
_diffrn_orient_matrix_UB_23      -0.0394376000
_diffrn_orient_matrix_UB_31      -0.0250699000
_diffrn_orient_matrix_UB_32      0.0231255000
_diffrn_orient_matrix_UB_33      0.0213452000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1348
_diffrn_reflns_av_unetI/netI     0.1677
_diffrn_reflns_Laue_measured_fraction_full 0.896
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            22976
_diffrn_reflns_point_group_measured_fraction_full 0.896
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         3.353
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.508
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.938
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
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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            yellow
_exptl_crystal_density_diffrn    1.350
_exptl_crystal_description       cube
_exptl_crystal_F_000             1756
_exptl_crystal_size_max          0.1001
_exptl_crystal_size_mid          0.0805
_exptl_crystal_size_min          0.0416
_refine_diff_density_max         1.124
_refine_diff_density_min         -0.925
_refine_diff_density_rms         0.140
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.943
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     439
_refine_ls_number_reflns         7305
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.943
_refine_ls_R_factor_all          0.1240
_refine_ls_R_factor_gt           0.0607
_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^)] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0762
_refine_ls_wR_factor_ref         0.0923
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4353
_reflns_number_total             7305
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00808_si_002.cif
_cod_data_source_block           7
_cod_original_cell_volume        4151.2(10)
_cod_database_code               4347965
_manchester_internal_coll_name   adpm98
_manchester_internal_coll_client CAPG/FO
_manchester_internal_coll_type   custom
_manchester_internal_coll_frame_time 60.00
_manchester_internal_coll_frame_width 1
_manchester_internal_coll_frame_method '\w scans'
_manchester_internal_coll_user   CAPG/FO
_manchester_internal_coll_date   11/11/14
_manchester_internal_process_user CAPG
_manchester_internal_process_date 11/11/14
_manchester_internal_solution_user CAPG
_manchester_internal_solution_date 11/11/14
_manchester_internal_refinement_user CAPG
_manchester_internal_refinement_date 11/11/14
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         Sm(N(SiC9H21)2)2OC13
_reflns_odcompleteness_completeness 99.66
_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), C32(H32)
2.b Aromatic/amide H refined with riding coordinates:
 C25(H25), C24(H24), C23(H23), C22(H22), C21(H21), C27(H27), C28(H28),
 C29(H29), C30(H30), C31(H31), C33(H33), C34(H34), C36(H36), C37(H37), C40(H40),
  C41(H41), C42(H42), C43(H43), C44(H44)
2.c Fitted hexagon refined as free rotating group:
 C20(C25,C24,C23,C22,C21), C26(C27,C28,C29,C30,C31)
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)
;
_shelx_res_checksum              81256
_shelx_hkl_checksum              60910
_olex2_submission_special_instructions 'No special instructions were received'