Synthesis and Characterization of Rare Earth Siloxide Complexes, M[OSi(OtBu)3]3(L)x where L is HOSi(OtBu)3 and x = 0 or 1
Lapadula, Giuseppe; Conley, Matthew P.; Copéret, Christophe; Andersen, Richard A.; Organometallics 34 (2014) 2271–; doi:10.1021/om501047g

data_4089699
_publ_section_title
;
 Synthesis and Characterization of Rare Earth Siloxide Complexes,
 M[OSi(OtBu)3]3(L)x where L is HOSi(OtBu)3 and x = 0 or 1
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              2271
_journal_paper_doi               10.1021/om501047g
_journal_volume                  34
_journal_year                    2014
_chemical_formula_moiety         '4(C36 H81 O12 Sc Si3)'
_chemical_formula_sum            'C144 H324 O48 Sc4 Si12'
_chemical_formula_weight         3340.93
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2014-05-13
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_cell_angle_alpha                88.3820(18)
_cell_angle_beta                 86.6834(18)
_cell_angle_gamma                60.0286(15)
_cell_formula_units_Z            1
_cell_length_a                   13.5964(16)
_cell_length_b                   13.6207(16)
_cell_length_c                   30.778(4)
_cell_measurement_reflns_used    9269
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.613
_cell_measurement_theta_min      2.232
_cell_volume                     4929.4(10)
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0339
_diffrn_reflns_av_unetI/netI     0.0422
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            66308
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.281
_diffrn_reflns_theta_min         1.325
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    0.271
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6655
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0981 before and 0.0504 after correction.
The Ratio of minimum to maximum transmission is 0.8920.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.125
_exptl_crystal_description       block
_exptl_crystal_F_000             1824
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.411
_refine_diff_density_min         -0.372
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.226
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1062
_refine_ls_number_reflns         24332
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.226
_refine_ls_R_factor_all          0.0794
_refine_ls_R_factor_gt           0.0668
_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^)+(0.0003P)^2^+10.5868P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1404
_refine_ls_wR_factor_ref         0.1446
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20580
_reflns_number_total             24332
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om501047g_si_001.cif
_cod_data_source_block           gl2159_0m
_cod_original_cell_volume        4929.3(10)
_cod_database_code               4089699
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(C39A)=Sof(H39D)=Sof(H39E)=Sof(H39F)=Sof(C22A)=Sof(H22D)=Sof(H22E)=
 Sof(H22F)=Sof(C25A)=Sof(H25A)=Sof(H25B)=Sof(H25C)=1-FVAR(1)
 Sof(C26A)=Sof(H26D)=Sof(H26E)=Sof(H26F)=Sof(C23A)=Sof(H23D)=Sof(H23E)=
 Sof(H23F)=Sof(C24A)=Sof(H24D)=Sof(H24E)=Sof(H24F)=FVAR(1)
 Sof(C5B)=Sof(H5BA)=Sof(H5BB)=Sof(H5BC)=Sof(C3B)=Sof(H3BA)=Sof(H3BB)=Sof(H3BC)=
 Sof(C7B)=Sof(H7BA)=Sof(H7BB)=Sof(H7BC)=Sof(C1B)=1-FVAR(2)
 Sof(C2B)=Sof(C4B)=Sof(H4BA)=Sof(H4BB)=Sof(H4BC)=Sof(C6B)=Sof(H6BA)=Sof(H6BB)=
 Sof(H6BC)=Sof(C8B)=Sof(H8BA)=Sof(H8BB)=Sof(H8BC)=FVAR(2)
3.a Idealised Me refined as rotating group:
 C15A(H15D,H15E,H15F), C39B(H39A,H39B,H39C), C36A(H36D,H36E,H36F), C33A(H33D,
 H33E,H33F), C35A(H35D,H35E,H35F), C26B(H26A,H26B,H26C), C20B(H20A,H20B,H20C),
 C10A(H10D,H10E,H10F), C28B(H28A,H28B,H28C), C33B(H33A,H33B,H33C), C11B(H11A,
 H11B,H11C), C11A(H11D,H11E,H11F), C35B(H35A,H35B,H35C), C15B(H15A,H15B,H15C),
 C28A(H28D,H28E,H28F), C4A(H4AA,H4AB,H4AC), C6A(H6AA,H6AB,H6AC), C31B(H31A,H31B,
 H31C), C40B(H40A,H40B,H40C), C14A(H14D,H14E,H14F), C14B(H14A,H14B,H14C),
 C17A(H17A,H17B,H17C), C23B(H23A,H23B,H23C), C29A(H29A,H29B,H29C), C16B(H16A,
 H16B,H16C), C27A(H27D,H27E,H27F), C9A(H9AA,H9AB,H9AC), C36B(H36A,H36B,H36C),
 C16A(H16D,H16E,H16F), C32A(H32D,H32E,H32F), C18B(H18A,H18B,H18C), C38B(H38A,
 H38B,H38C), C10B(H10A,H10B,H10C), C3A(H3AA,H3AB,H3AC), C31A(H31D,H31E,H31F),
 C19B(H19A,H19B,H19C), C30B(H30A,H30B,H30C), C22B(H22A,H22B,H22C), C8A(H8AA,
 H8AB,H8AC), C37A(H37A,H37B,H37C), C18A(H18D,H18E,H18F), C7A(H7AA,H7AB,H7AC),
 C12B(H12A,H12B,H12C), C2A(H2AA,H2AB,H2AC), C4B(H4BA,H4BB,H4BC), C26A(H26D,H26E,
 H26F), C27B(H27A,H27B,H27C), C32B(H32A,H32B,H32C), C19A(H19D,H19E,H19F),
 C24B(H24A,H24B,H24C), C6B(H6BA,H6BB,H6BC), C23A(H23D,H23E,H23F), C8B(H8BA,H8BB,
 H8BC), C24A(H24D,H24E,H24F), C39A(H39D,H39E,H39F), C22A(H22D,H22E,H22F),
 C25A(H25A,H25B,H25C), C5B(H5BA,H5BB,H5BC), C3B(H3BA,H3BB,H3BC), C7B(H7BA,H7BB,
 H7BC)
;