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_4089698
_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 Nd O16 Si4, 0.5(C2 H4 Cl4)'
_chemical_formula_sum            'C49 H111 Cl2 Nd O16 Si4'
_chemical_formula_weight         1283.87
_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             2014-06-30
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_cell_angle_alpha                71.842(3)
_cell_angle_beta                 89.146(3)
_cell_angle_gamma                80.549(3)
_cell_formula_units_Z            4
_cell_length_a                   13.485(3)
_cell_length_b                   22.616(4)
_cell_length_c                   24.217(5)
_cell_measurement_reflns_used    9055
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.451
_cell_measurement_theta_min      2.248
_cell_volume                     6917(2)
_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    'ShelXS (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 0.787
_diffrn_measured_fraction_theta_max 0.991
_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  0.0344
_diffrn_reflns_av_unetI/netI     0.0354
_diffrn_reflns_Laue_measured_fraction_full 0.787
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            59436
_diffrn_reflns_point_group_measured_fraction_full 0.787
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         23.256
_diffrn_reflns_theta_min         1.497
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    0.951
_exptl_absorpt_correction_T_max  0.9
_exptl_absorpt_correction_T_min  0.8
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1464 before and 0.0536 after correction.
The Ratio of minimum to maximum transmission is 0.8417.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear bluish blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   bluish
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.233
_exptl_crystal_description       block
_exptl_crystal_F_000             2732
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.23
_refine_diff_density_max         5.760
_refine_diff_density_min         -2.598
_refine_diff_density_rms         0.180
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.203
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1532
_refine_ls_number_reflns         19662
_refine_ls_number_restraints     1895
_refine_ls_restrained_S_all      1.170
_refine_ls_R_factor_all          0.1090
_refine_ls_R_factor_gt           0.1013
_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^)+(0.0001P)^2^+209.3566P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2454
_refine_ls_wR_factor_ref         0.2496
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17672
_reflns_number_total             19662
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om501047g_si_001.cif
_cod_data_source_block           nd41_0m
_cod_database_code               4089698
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 C12-Cl3
 1.8 with sigma of 0.02
 O1B-H1B
 0.85 with sigma of 0.01
 O1A-H1A
 0.85 with sigma of 0.01
 C33B-C35B
 1.6 with sigma of 0.02
 C31B-C35B
 3 with sigma of 0.02
 Si1B-H1B
 2.070564 with sigma of 0.02
 Nd1B-H1B
 3.216085 with sigma of 0.02
 Si1A-H1A
 2.058096 with sigma of 0.02
 Nd1A-H1A
 3.233611 with sigma of 0.02
3. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
Uanis(C12) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(C41A)=Sof(H41D)=Sof(H41E)=Sof(H41F)=Sof(C39A)=Sof(H39A)=Sof(H39B)=
 Sof(H39C)=Sof(C43A)=Sof(H43D)=Sof(H43E)=Sof(H43F)=Sof(C45A)=1-FVAR(1)
 Sof(C40A)=Sof(H40D)=Sof(H40E)=Sof(H40F)=Sof(C42A)=Sof(H42D)=Sof(H42E)=
 Sof(H42F)=Sof(C38A)=Sof(H38A)=Sof(H38B)=Sof(H38C)=Sof(C44A)=FVAR(1)
 Sof(C31B)=Sof(H31A)=Sof(H31B)=Sof(H31C)=Sof(C32B)=Sof(C29B)=Sof(H29A)=
 Sof(H29B)=Sof(H29C)=Sof(C30B)=Sof(H30A)=Sof(H30B)=Sof(H30C)=1-FVAR(2)
 Sof(C28B)=Sof(H28A)=Sof(H28B)=Sof(H28C)=Sof(C25B)=Sof(C26B)=Sof(H26A)=
 Sof(H26B)=Sof(H26C)=Sof(C27B)=Sof(H27A)=Sof(H27B)=Sof(H27C)=FVAR(2)
 Sof(C42B)=Sof(H42A)=Sof(H42B)=Sof(H42C)=Sof(C43B)=Sof(H43A)=Sof(H43B)=
 Sof(H43C)=Sof(C45B)=Sof(C44B)=Sof(H44A)=Sof(H44B)=Sof(H44C)=1-FVAR(3)
 Sof(C41B)=Sof(H41A)=Sof(H41B)=Sof(H41C)=Sof(C39B)=Sof(C40B)=Sof(H40A)=
 Sof(H40B)=Sof(H40C)=Sof(C37B)=Sof(H37A)=Sof(H37B)=Sof(H37C)=FVAR(3)
 Sof(O9B)=1-FVAR(4)
 Sof(O7B)=FVAR(4)
 Fixed Sof: Cl6(0.5) Cl9(0.5) C3M(0.5) H3MA(0.5) H3MB(0.5) Cl3(0.5) Cl4(0.5)
 C12(0.5) H9A(0.5) H9B(0.5)
7.a Secondary CH2 refined with riding coordinates:
 C3M(H3MA,H3MB), C12(H9A,H9B), C2G(H2GA,H2GB)
7.b Idealised Me refined as rotating group:
 C2B(H2BA,H2BB,H2BC), C20B(H20A,H20B,H20C), C24B(H24A,H24B,H24C), C18B(H18A,
 H18B,H18C), C22B(H22A,H22B,H22C), C6B(H6BA,H6BB,H6BC), C11B(H11A,H11B,H11C),
 C4B(H4BA,H4BB,H4BC), C10B(H10A,H10B,H10C), C46B(H46A,H46B,H46C), C19B(H19A,
 H19B,H19C), C15B(H15A,H15B,H15C), C3B(H3BA,H3BB,H3BC), C21B(H21A,H21B,H21C),
 C16B(H16A,H16B,H16C), C36B(H36A,H36B,H36C), C35B(H35A,H35B,H35C), C34B(H34A,
 H34B,H34C), C48B(H48A,H48B,H48C), C12B(H12A,H12B,H12C), C14B(H14A,H14B,H14C),
 C8B(H8BA,H8BB,H8BC), C14(H14D,H14E,H14F), C16(H16D,H16E,H16F), C49B(H49A,H49B,
 H49C), C53B(H53A,H53B,H53C), C52B(H52A,H52B,H52C), C32(H32A,H32B,H32C),
 C50B(H50A,H50B,H50C), C7B(H7BA,H7BB,H7BC), C28B(H28A,H28B,H28C), C41B(H41A,
 H41B,H41C), C40B(H40A,H40B,H40C), C26B(H26A,H26B,H26C), C37B(H37A,H37B,H37C),
 C27B(H27A,H27B,H27C), C42B(H42A,H42B,H42C), C43B(H43A,H43B,H43C), C31B(H31A,
 H31B,H31C), C29B(H29A,H29B,H29C), C30B(H30A,H30B,H30C), C44B(H44A,H44B,H44C),
 C8A(H8AA,H8AB,H8AC), C16A(H16G,H16H,H16I), C31A(H31D,H31E,H31F), C55A(H55A,
 H55B,H55C), C48A(H48D,H48E,H48F), C23A(H23A,H23B,H23C), C34A(H34D,H34E,H34F),
 C18A(H18D,H18E,H18F), C35A(H35D,H35E,H35F), C10A(H10D,H10E,H10F), C32A(H32D,
 H32E,H32F), C11A(H11D,H11E,H11F), C2A(H2AA,H2AB,H2AC), C22A(H22D,H22E,H22F),
 C47A(H47A,H47B,H47C), C53A(H53D,H53E,H53F), C20A(H20D,H20E,H20F), C5A(H5AA,
 H5AB,H5AC), C12A(H12D,H12E,H12F), C19A(H19D,H19E,H19F), C50A(H50D,H50E,H50F),
 C7A(H7AA,H7AB,H7AC), C36A(H36D,H36E,H36F), C3A(H3AA,H3AB,H3AC), C49A(H49D,H49E,
 H49F), C24A(H24D,H24E,H24F), C54A(H54A,H54B,H54C), C27A(H27D,H27E,H27F),
 C26A(H26D,H26E,H26F), C15A(H15D,H15E,H15F), C30A(H30D,H30E,H30F), C28A(H28D,
 H28E,H28F), C14A(H14G,H14H,H14I), C40A(H40D,H40E,H40F), C42A(H42D,H42E,H42F),
 C38A(H38A,H38B,H38C), C41A(H41D,H41E,H41F), C39A(H39A,H39B,H39C), C43A(H43D,
 H43E,H43F)
;