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_4089700
_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         'C48 H109 O16 Sc Si4, C H2 Cl2'
_chemical_formula_sum            'C49 H111 Cl2 O16 Sc Si4'
_chemical_formula_weight         1184.59
_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   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2014-05-20
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_cell_angle_alpha                97.5573(13)
_cell_angle_beta                 91.3154(13)
_cell_angle_gamma                99.3144(13)
_cell_formula_units_Z            2
_cell_length_a                   13.7383(13)
_cell_length_b                   14.4897(14)
_cell_length_c                   17.4579(17)
_cell_measurement_reflns_used    9824
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.845
_cell_measurement_theta_min      2.303
_cell_volume                     3396.1(6)
_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 0.999
_diffrn_measured_fraction_theta_max 0.916
_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  0.0186
_diffrn_reflns_av_unetI/netI     0.0236
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.916
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            51589
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.916
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.093
_diffrn_reflns_theta_min         1.438
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    0.313
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.6628
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0878 before and 0.0363 after correction.
The Ratio of minimum to maximum transmission is 0.8882.
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    1.158
_exptl_crystal_description       block
_exptl_crystal_F_000             1288
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.782
_refine_diff_density_min         -0.474
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     707
_refine_ls_number_reflns         19981
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0439
_refine_ls_R_factor_gt           0.0362
_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^)+(0.0580P)^2^+1.1690P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0993
_refine_ls_wR_factor_ref         0.1047
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17120
_reflns_number_total             19981
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om501047g_si_001.cif
_cod_data_source_block           gl2161sc4_0m
_cod_database_code               4089700
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O1-H1
 0.87 with sigma of 0.01
 Si3-H1
 2.094423 with sigma of 0.02
 Sc1-H1
 2.950321 with sigma of 0.02
3. Others
 Sof(H1SC)=Sof(H1SD)=Sof(Cl1S)=Sof(Cl3S)=1-FVAR(1)
 Sof(Cl2S)=Sof(Cl4S)=Sof(H1SA)=Sof(H1SB)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C1S(H1SA,H1SB), C1S(H1SC,H1SD)
4.b Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C47(H47A,H47B,H47C), C15(H15A,H15B,H15C), C14(H14A,H14B,
 H14C), C42(H42A,H42B,H42C), C24(H24A,H24B,H24C), C6(H6A,H6B,H6C), C46(H46A,
 H46B,H46C), C44(H44A,H44B,H44C), C20(H20A,H20B,H20C), C34(H34A,H34B,H34C),
 C22(H22A,H22B,H22C), C48(H48A,H48B,H48C), C43(H43A,H43B,H43C), C11(H11A,H11B,
 H11C), C26(H26A,H26B,H26C), C23(H23A,H23B,H23C), C18(H18A,H18B,H18C), C39(H39A,
 H39B,H39C), C32(H32A,H32B,H32C), C19(H19A,H19B,H19C), C10(H10A,H10B,H10C),
 C36(H36A,H36B,H36C), C35(H35A,H35B,H35C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C),
 C8(H8A,H8B,H8C), C31(H31A,H31B,H31C), C12(H12A,H12B,H12C), C7(H7A,H7B,H7C),
 C2(H2A,H2B,H2C), C30(H30A,H30B,H30C), C28(H28A,H28B,H28C), C38(H38A,H38B,H38C),
  C40(H40A,H40B,H40C), C27(H27A,H27B,H27C)
;