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_7043171
_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         'C30 H80 K2 N10 Si4'
_chemical_formula_sum            'C30 H80 K2 N10 Si4'
_chemical_formula_weight         771.60
_chemical_properties_physical
', Air-sensitive,Moisture-sensitive,Heat-sensitive,Oxygen-sensitive'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_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                90
_cell_angle_beta                 90.829(15)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.338(6)
_cell_length_b                   16.547(11)
_cell_length_c                   14.617(9)
_cell_measurement_reflns_used    503
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      16.92
_cell_measurement_theta_min      2.46
_cell_volume                     2258(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SIR-92 (Altomare 1992)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.970
_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  0.2175
_diffrn_reflns_av_unetI/netI     0.2441
_diffrn_reflns_Laue_measured_fraction_full 0.973
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            12450
_diffrn_reflns_point_group_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.309
_diffrn_reflns_theta_min         1.859
_exptl_absorpt_coefficient_mu    0.348
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.2907
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'sadabs Bruker'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.135
_exptl_crystal_description       block
_exptl_crystal_F_000             848
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: n-pentane'
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.405
_refine_diff_density_min         -0.447
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.887
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     214
_refine_ls_number_reflns         3985
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.887
_refine_ls_R_factor_all          0.1809
_refine_ls_R_factor_gt           0.0717
_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^)+(0.0546P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1415
_refine_ls_wR_factor_ref         0.1783
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1736
_reflns_number_total             3985
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01671a2.cif
_cod_data_source_block           3
_cod_database_code               7043171
_shelx_estimated_absorpt_t_min   0.918
_shelx_estimated_absorpt_t_max   0.973
_shelxl_version_number           2013-4
_shelx_res_checksum              15448