Mechanochemical Influence on the Stereoselectivity of Halide Metathesis: Synthesis of Group 15 Tris(allyl) Complexes
Rightmire, Nicholas R.; Bruns, David L.; Hanusa, Timothy P.; Brennessel, William W.; Organometallics 35 (2016) 1698–; doi:10.1021/acs.organomet.6b00151

data_4088521
_publ_section_title
;
 Mechanochemical Influence on the Stereoselectivity of Halide Metathesis:
 Synthesis of Group 15 Tris(allyl) Complexes
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              1698
_journal_paper_doi               10.1021/acs.organomet.6b00151
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C27 H63 As Si6'
_chemical_formula_sum            'C27 H63 As Si6'
_chemical_formula_weight         631.23
_chemical_name_common            hannr04
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                99.233(4)
_cell_angle_beta                 90.021(4)
_cell_angle_gamma                118.479(4)
_cell_formula_units_Z            2
_cell_length_a                   10.539(2)
_cell_length_b                   10.791(2)
_cell_length_c                   19.921(4)
_cell_measurement_reflns_used    4079
_cell_measurement_temperature    100.0(5)
_cell_measurement_theta_max      28.21
_cell_measurement_theta_min      2.21
_cell_volume                     1957.9(7)
_computing_cell_refinement       'SAINT (Bruker, 2013)'
_computing_data_collection       'APEX2 (Bruker, 2014)'
_computing_data_reduction        'SAINT (Bruker, 2013)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SIR2011 (Burla et al., 2012)'
_diffrn_ambient_temperature      100.0(5)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD platform'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0925
_diffrn_reflns_av_unetI/netI     0.0839
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            44064
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        29.575
_diffrn_reflns_theta_max         29.674
_diffrn_reflns_theta_min         2.080
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.065
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.6653
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2012)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.071
_exptl_crystal_description       block
_exptl_crystal_F_000             684
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.596
_refine_diff_density_min         -0.589
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         11007
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0915
_refine_ls_R_factor_gt           0.0493
_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^)+(0.0421P)^2^+0.3043P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0933
_refine_ls_wR_factor_ref         0.1067
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7413
_reflns_number_total             11007
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00151_si_001.cif
_cod_data_source_block           hannr04
_cod_database_code               4088521
_shelx_estimated_absorpt_t_min   0.784
_shelx_estimated_absorpt_t_max   0.920
_shelxl_version_number           2014-3
_shelx_res_checksum              59185
_shelx_hkl_checksum              96340