Synthesis and structures of lithium alkoxytris(dimethylphenylsilyl)borates
Tsurusaki, Akihiro; Yoshida, Keisuke; Kyushin, Soichiro; Dalton Trans.  (2017) –; doi:10.1039/C7DT00395A

data_7042611
_publ_section_title
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 Synthesis and structures of lithium
 alkoxytris(dimethylphenylsilyl)borates
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT00395A
_journal_year                    2017
_chemical_formula_moiety         'C33 H52 B Li O3 Si3'
_chemical_formula_sum            'C33 H52 B Li O3 Si3'
_chemical_formula_weight         598.77
_chemical_melting_point          381.6(5)
_chemical_name_common            compound1a
_chemical_name_systematic
; 
 Lithium Methoxytris(dimethylphenylsilyl)borate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2017-01-30 deposited with the CCDC.
2017-03-28 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 95.103(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   11.216(2)
_cell_length_b                   20.479(4)
_cell_length_c                   30.789(5)
_cell_measurement_reflns_used    13671
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      29.9
_cell_measurement_theta_min      2.0
_cell_volume                     7044(2)
_computing_cell_refinement
'CrystalClear-SM Expert 2.1 b29 (Rigaku, 2013)'
_computing_data_collection
'CrystalClear-SM Expert 2.1 b29 (Rigaku, 2013)'
_computing_data_reduction
'CrystalClear-SM Expert 2.1 b29 (Rigaku, 2013)'
_computing_molecular_graphics    '<i>ORTEP-3</i> (Farrugia, 1997)'
_computing_publication_material
'<i>SHELXL97</i> and <i>Yadokari-XG 2009</i> (Kabuto <i>et al.</i>, 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR2004 (Giacovazzo <i>et al.</i>, 2005)'
_diffrn_ambient_temperature      123
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'Rigaku Pilatus 200K'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0525
_diffrn_reflns_av_sigmaI/netI    0.0482
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            92373
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.23
_exptl_absorpt_coefficient_mu    0.164
_exptl_absorpt_correction_T_max  0.9386
_exptl_absorpt_correction_T_min  0.9252
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(R. Jacobson, private communication, 1998)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.129
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             2592
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.39
_refine_diff_density_max         0.928
_refine_diff_density_min         -0.435
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.133
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     823
_refine_ls_number_reflns         15760
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.132
_refine_ls_R_factor_all          0.1074
_refine_ls_R_factor_gt           0.0985
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0673P)^2^+34.6840P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2627
_refine_ls_wR_factor_ref         0.2678
_reflns_number_gt                13724
_reflns_number_total             15760
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7dt00395a2.cif
_cod_data_source_block           compound_1a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '108--109 \%C.' was changed to
'381.6(5)' - it was converted from degrees Celsius(C) to Kelvins(K),
the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7042611