Lithium Aluminate Complexes and Alumoles from 1,4-Dilithio-1,3-Butadienes and AlEt2Cl.
Zhang, Yongliang; Wei, Junnian; Zhang, Wen-Xiong; Xi, Zhenfeng; Inorganic chemistry 54 (2015) 10695–10700; doi:10.1021/acs.inorgchem.5b01551

data_4346461
_publ_section_title
;
 Lithium Aluminate Complexes and Alumoles from 1,4-Dilithio-1,3-Butadienes
 and AlEt2Cl.
;
_journal_issue                   22
_journal_name_full               'Inorganic chemistry'
_journal_page_first              10695
_journal_page_last               10700
_journal_paper_doi               10.1021/acs.inorgchem.5b01551
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C28 H58 Al2 Si4'
_chemical_formula_sum            'C28 H58 Al2 Si4'
_chemical_formula_weight         561.06
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-06-23
_audit_creation_method
;
Olex2 1.2
(compiled 2014.08.28 svn.r2986 for OlexSys, GUI svn.r4874)
;
_cell_angle_alpha                90
_cell_angle_beta                 91.278(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.2887(5)
_cell_length_b                   14.9352(6)
_cell_length_c                   11.8613(5)
_cell_measurement_temperature    180.01(10)
_cell_volume                     1822.20(14)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      180.01(10)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Altas'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0299
_diffrn_reflns_av_unetI/netI     0.0443
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8475
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.021
_diffrn_reflns_theta_min         2.929
_exptl_absorpt_coefficient_mu    0.226
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.77308
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'metallic light yellow'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.023
_exptl_crystal_description       block
_exptl_crystal_F_000             616
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.270
_refine_diff_density_min         -0.243
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         3734
_refine_ls_number_restraints     198
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0661
_refine_ls_R_factor_gt           0.0425
_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^)+(0.0496P)^2^+0.5601P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0982
_refine_ls_wR_factor_ref         0.1100
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2794
_reflns_number_total             3734
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b01551_si_002.cif
_cod_data_source_block           1_a_dis
_cod_database_code               4346461
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.978
_shelx_estimated_absorpt_t_min   0.978
_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
2. Restrained distances
 Si2-C13 = Si2-C16 = Si2-C17
 1.87 with sigma of 0.02
 H12e-H18c
 2.1 with sigma of 0.02
 H12f-H19a
 2.1 with sigma of 0.02
 H12e-H19a
 2.1 with sigma of 0.02
 H14d-H21c
 2.2 with sigma of 0.02
 C13-C16 \\sim C16-C17 \\sim C17-C13
 with sigma of 0.02
 C1-C2 \\sim C3-C4 \\sim C9-C10
 with sigma of 0.01
 Al1-C1 \\sim Al1-C4 \\sim Al2-C9
 with sigma of 0.01
 C9-Si3 \\sim C9'-Si3
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1.7A with sigma of 0.01 and sigma
for terminal atoms of 0.02
Uanis(C4) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(Al2') \\sim Ueq, Uanis(C9')
\\sim Ueq, Uanis(C10') \\sim Ueq, Uanis(C12') \\sim Ueq, Uanis(C14') \\sim Ueq,
Uanis(C15') \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Same fragment restrains
{Al2, C9, C10, C12, C14, C15}
as
{Al2', C9', C10', C12', C14', C15'}
5. Others
 Sof(C9')=Sof(C10')=Sof(C12')=Sof(H12d)=Sof(H12e)=Sof(H12f)=1-FVAR(1)
 Sof(Al2')=Sof(C14')=Sof(H14c)=Sof(H14d)=Sof(C15')=Sof(H15d)=Sof(H15e)=
 Sof(H15f)=0.5*(1-FVAR(2))
 Sof(Al2)=Sof(C14)=Sof(H14a)=Sof(H14b)=Sof(C15)=Sof(H15a)=Sof(H15b)=Sof(H15c)=
 0.5*FVAR(2)
 Sof(C9)=Sof(C10)=Sof(C12)=Sof(H12a)=Sof(H12b)=Sof(H12c)=FVAR(1)
 Fixed Sof: Si2(0.5) Al1(0.5) C1(0.5) C2(0.5) C3(0.5) C4(0.5) C5(0.5) H5a(0.5)
 H5b(0.5) H5c(0.5) C6(0.5) H6a(0.5) H6b(0.5) H6c(0.5) C7(0.5) H7a(0.5) H7b(0.5)
 C8(0.5) H8a(0.5) H8b(0.5) H8c(0.5) C13(0.5) H13a(0.5) H13b(0.5) H13c(0.5)
 C16(0.5) H16a(0.5) H16b(0.5) H16c(0.5) C17(0.5) H17a(0.5) H17b(0.5) H17c(0.5)
 H22a(0.5) H22b(0.5) H22c(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C14(H14a,H14b), C14'(H14c,H14d), C7(H7a,H7b)
6.b Me refined with riding coordinates:
 C15'(H15d,H15e,H15f)
6.c Idealised Me refined as rotating group:
 C12(H12a,H12b,H12c), C15(H15a,H15b,H15c), C12'(H12d,H12e,H12f), C5(H5a,H5b,
 H5c), C6(H6a,H6b,H6c), C8(H8a,H8b,H8c), C13(H13a,H13b,H13c), C16(H16a,H16b,
 H16c), C17(H17a,H17b,H17c), C18(H18a,H18b,H18c), C19(H19a,H19b,H19c), C20(H20a,
 H20b,H20c), C21(H21a,H21b,H21c), C22(H22a,H22b,H22c)
;
_olex2_submission_special_instructions 'No special instructions were received'