Facile ring-opening of THF at lithium induced by a pendant Si-H bond and BPh3
Okuda, Jun; Mukherjee, Debabrata; Osseili, Hassan; Spaniol, Thomas Paul; Dalton Trans.  (2017) –; doi:10.1039/C7DT01671A

data_7043170
_publ_section_title
;
 Facile ring-opening of THF at lithium induced by a pendant Si-H bond and
 BPh3
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT01671A
_journal_year                    2017
_chemical_formula_moiety         'C37 H61 B Li N5 O1 Si2, 2(C4 H8 O)'
_chemical_formula_sum            'C45 H77 B Li N5 O3 Si2'
_chemical_formula_weight         810.04
_chemical_name_systematic
;
 ?
;
_chemical_properties_physical
', Air-sensitive,Moisture-sensitive,Oxygen-sensitive'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2017-04-19 deposited with the CCDC.
2017-05-31 downloaded from the CCDC.
;
_cell_angle_alpha                87.199(12)
_cell_angle_beta                 77.299(12)
_cell_angle_gamma                65.471(11)
_cell_formula_units_Z            2
_cell_length_a                   11.063(4)
_cell_length_b                   11.919(7)
_cell_length_c                   19.901(11)
_cell_measurement_reflns_used    590
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      17.02
_cell_measurement_theta_min      2.22
_cell_volume                     2326(2)
_computing_cell_refinement       'Bruker SMART (2001)'
_computing_data_collection       'Bruker SMART (2001)'
_computing_data_reduction        'Bruker SAINT+ (1999)'
_computing_molecular_graphics    'ORTEP-III (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SIR-92 (Altomare 1992)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.947
_diffrn_measurement_device_type  'Bruker APEX-I CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  'multilayer optics'
_diffrn_radiation_source         microsource
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1852
_diffrn_reflns_av_unetI/netI     0.4176
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.947
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            22016
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.947
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.343
_diffrn_reflns_theta_min         1.050
_exptl_absorpt_coefficient_mu    0.120
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.4027
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs Bruker'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.156
_exptl_crystal_description       plate
_exptl_crystal_F_000             884
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: n-pentane and thf'
_exptl_crystal_size_max          0.310
_exptl_crystal_size_mid          0.270
_exptl_crystal_size_min          0.110
_refine_diff_density_max         0.467
_refine_diff_density_min         -0.423
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     536
_refine_ls_number_reflns         9958
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      0.837
_refine_ls_R_factor_all          0.2292
_refine_ls_R_factor_gt           0.0841
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0592P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1721
_refine_ls_wR_factor_ref         0.2000
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3277
_reflns_number_total             9958
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01671a2.cif
_cod_data_source_block           7
_cod_database_code               7043170
_shelx_estimated_absorpt_t_min   0.964
_shelx_estimated_absorpt_t_max   0.987
_shelxl_version_number           2013-4
_shelx_res_checksum              94678