Potential Protecting Group Strategy for Disila Analogues of Vinyllithiums: Synthesis and Reactivity of a 2,4,6-Trimethoxyphenyl-Substituted Disilene
Meltzer, Antje; Majumdar, Moumita; White, Andrew J. P.; Huch, Volker; Scheschkewitz, David; Organometallics 32 (2013) 6844–; doi:10.1021/om400545w

data_4081797
_publ_section_title
;
 Potential Protecting Group Strategy for Disila Analogues of
 Vinyllithiums: Synthesis and Reactivity of a
 2,4,6-Trimethoxyphenyl-Substituted Disilene
;
_journal_issue                   22
_journal_name_full               Organometallics
_journal_page_first              6844
_journal_paper_doi               10.1021/om400545w
_journal_volume                  32
_journal_year                    2013
_chemical_formula_sum            'C59 H89 N O3 Si2'
_chemical_formula_weight         916.49
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                77.539(12)
_cell_angle_beta                 73.902(11)
_cell_angle_gamma                82.448(19)
_cell_formula_units_Z            2
_cell_length_a                   11.388(5)
_cell_length_b                   13.624(6)
_cell_length_c                   19.613(10)
_cell_measurement_reflns_used    1045
_cell_measurement_temperature    132(2)
_cell_measurement_theta_max      20.40
_cell_measurement_theta_min      2.66
_cell_volume                     2846(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      132(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0566
_diffrn_reflns_av_sigmaI/netI    0.0747
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            42965
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.10
_exptl_absorpt_coefficient_mu    0.103
_exptl_absorpt_correction_T_max  0.9796
_exptl_absorpt_correction_T_min  0.9472
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, BrukerAXS 2008'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.069
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1004
_exptl_crystal_size_max          0.53
_exptl_crystal_size_mid          0.53
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.532
_refine_diff_density_min         -0.349
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     679
_refine_ls_number_reflns         11609
_refine_ls_number_restraints     266
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.1158
_refine_ls_R_factor_gt           0.0624
_refine_ls_shift/su_max          0.112
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0699P)^2^+1.5124P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1430
_refine_ls_wR_factor_ref         0.1718
_reflns_number_gt                7002
_reflns_number_total             11609
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400545w_si_010.cif
_cod_data_source_block           9
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        2847(2)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4081797