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_4088520
_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 Sb Si6'
_chemical_formula_sum            'C27 H63 Sb Si6'
_chemical_formula_weight         678.06
_chemical_name_common            hannr02
_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                81.289(7)
_cell_angle_beta                 89.569(7)
_cell_angle_gamma                61.724(6)
_cell_formula_units_Z            2
_cell_length_a                   10.643(4)
_cell_length_b                   10.792(4)
_cell_length_c                   20.226(7)
_cell_measurement_reflns_used    4096
_cell_measurement_temperature    100.0(5)
_cell_measurement_theta_max      31.54
_cell_measurement_theta_min      2.22
_cell_volume                     2016.8(13)
_computing_cell_refinement       'SAINT (Bruker, 2013)'
_computing_data_collection       'APEX2 (Bruker, 2013)'
_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 0.994
_diffrn_measured_fraction_theta_max 0.992
_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  0.0432
_diffrn_reflns_av_unetI/netI     0.0462
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            55659
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        33.729
_diffrn_reflns_theta_max         33.805
_diffrn_reflns_theta_min         1.021
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.876
_exptl_absorpt_correction_T_max  0.4359
_exptl_absorpt_correction_T_min  0.3741
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2012)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.116
_exptl_crystal_description       block
_exptl_crystal_F_000             720
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.205
_refine_diff_density_min         -1.089
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     463
_refine_ls_number_reflns         16088
_refine_ls_number_restraints     177
_refine_ls_restrained_S_all      1.126
_refine_ls_R_factor_all          0.0864
_refine_ls_R_factor_gt           0.0675
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0443P)^2^+5.1392P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1557
_refine_ls_wR_factor_ref         0.1657
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12868
_reflns_number_total             16088
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00151_si_002.cif
_cod_data_source_block           hannr02
_cod_original_cell_volume        2017.0(12)
_cod_database_code               4088520
_shelx_estimated_absorpt_t_min   0.804
_shelx_estimated_absorpt_t_max   0.902
_shelxl_version_number           2014-3
_shelx_res_checksum              85993
_shelx_hkl_checksum              56802