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_4089702
_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         'C36 H81 O12 Si3 Yb'
_chemical_formula_sum            'C36 H81 O12 Si3 Yb'
_chemical_formula_weight         963.31
_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             2014-06-19
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_cell_angle_alpha                100.3664(14)
_cell_angle_beta                 90.0573(14)
_cell_angle_gamma                119.6623(12)
_cell_formula_units_Z            4
_cell_length_a                   13.5871(13)
_cell_length_b                   13.7326(13)
_cell_length_c                   31.236(3)
_cell_measurement_reflns_used    9722
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.363
_cell_measurement_theta_min      2.405
_cell_volume                     4954.1(8)
_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 0.999
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_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  0.0315
_diffrn_reflns_av_unetI/netI     0.0252
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            133679
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.433
_diffrn_reflns_theta_min         0.666
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    2.009
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6174
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1036 before and 0.0462 after correction.
The Ratio of minimum to maximum transmission is 0.8275.
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    1.292
_exptl_crystal_description       block
_exptl_crystal_F_000             2020
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.19
_refine_diff_density_max         1.908
_refine_diff_density_min         -1.339
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.197
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1011
_refine_ls_number_reflns         29617
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.197
_refine_ls_R_factor_all          0.0474
_refine_ls_R_factor_gt           0.0413
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0222P)^2^+11.6154P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0878
_refine_ls_wR_factor_ref         0.0900
_reflns_Friedel_coverage         0.000
_reflns_number_gt                26720
_reflns_number_total             29617
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om501047g_si_001.cif
_cod_data_source_block           gl2102_0m
_cod_database_code               4089702
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C12A-O6A
 2.4 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O26G) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.05
Uanis(O26G) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.05
4. Others
 Sof(O9B)=1-FVAR(1)
 Sof(O7B)=FVAR(1)
 Sof(O26G)=1-FVAR(2)
 Sof(O8A)=FVAR(2)
5.a Idealised Me refined as rotating group:
 C16B(H16D,H16E,H16F), C24A(H24A,H24B,H24C), C25B(H25A,H25B,H25C), C30A(H30A,
 H30B,H30C), C22A(H22A,H22B,H22C), C15B(H15D,H15E,H15F), C14A(H14A,H14B,H14C),
 C2A(H2AA,H2AB,H2AC), C31A(H31A,H31B,H31C), C3B(H3BA,H3BB,H3BC), C12B(H12D,H12E,
 H12F), C26B(H26D,H26E,H26F), C18B(H18D,H18E,H18F), C36A(H36A,H36B,H36C),
 C20A(H20A,H20B,H20C), C34B(H34D,H34E,H34F), C8B(H8BA,H8BB,H8BC), C17B(H17A,
 H17B,H17C), C19A(H19A,H19B,H19C), C8A(H8AA,H8AB,H8AC), C6A(H6AA,H6AB,H6AC),
 C6B(H6BA,H6BB,H6BC), C10B(H10D,H10E,H10F), C35A(H35A,H35B,H35C), C4B(H4BA,H4BB,
 H4BC), C31B(H31D,H31E,H31F), C27A(H27A,H27B,H27C), C30B(H30D,H30E,H30F),
 C16A(H16A,H16B,H16C), C28A(H28A,H28B,H28C), C3A(H3AA,H3AB,H3AC), C11B(H11D,
 H11E,H11F), C15A(H15A,H15B,H15C), C33B(H33A,H33B,H33C), C23A(H23A,H23B,H23C),
 C13B(H13A,H13B,H13C), C10A(H10A,H10B,H10C), C27B(H27D,H27E,H27F), C23B(H23D,
 H23E,H23F), C26A(H26A,H26B,H26C), C32B(H32D,H32E,H32F), C2B(H2BA,H2BB,H2BC),
 C4A(H4AA,H4AB,H4AC), C32A(H32A,H32B,H32C), C24B(H24D,H24E,H24F), C34A(H34A,
 H34B,H34C), C11A(H11A,H11B,H11C), C35B(H35D,H35E,H35F), C22B(H22D,H22E,H22F),
 C12A(H12A,H12B,H12C), C7A(H7AA,H7AB,H7AC), C7B(H7BA,H7BB,H7BC), C20B(H20D,H20E,
 H20F), C18A(H18A,H18B,H18C)
;