Transmetallation reactions of a lithium disilenide
Michael J. Cowley; Kai Abersfelder; Andrew J. P. White; Moumita Majumdar; David Scheschkewitz; Chem.Commun. 48 (2012) 6595–; doi:10.1039/c2cc33047d

data_7107893
_publ_section_title
;
 Transmetallation reactions of a lithium disilenide
;
_journal_name_full               Chem.Commun.
_journal_page_first              6595
_journal_paper_doi               10.1039/c2cc33047d
_journal_volume                  48
_journal_year                    2012
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C90 H138 Cu Si4, C12 H30 Li O6'
_chemical_formula_sum            'C102 H168 Cu Li O6 Si4'
_chemical_formula_weight         1673.20
_space_group_IT_number           7
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P -2yac'
_symmetry_space_group_name_H-M   'P 1 n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 110.058(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   14.8462(2)
_cell_length_b                   19.6370(3)
_cell_length_c                   19.5727(4)
_cell_measurement_reflns_used    24364
_cell_measurement_temperature    173
_cell_measurement_theta_max      32.9695
_cell_measurement_theta_min      3.0152
_cell_volume                     5360.02(17)
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd'
_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173
_diffrn_detector_area_resol_mean 15.9825
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.903
_diffrn_measurement_device_type  'OD Xcalibur 3'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0275
_diffrn_reflns_av_sigmaI/netI    0.0463
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            61261
_diffrn_reflns_theta_full        31.50
_diffrn_reflns_theta_max         33.04
_diffrn_reflns_theta_min         3.02
_exptl_absorpt_coefficient_mu    0.295
_exptl_absorpt_correction_T_max  0.947
_exptl_absorpt_correction_T_min  0.897
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.037
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             1832
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.43
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.828
_refine_diff_density_min         -0.313
_refine_diff_density_rms         0.062
_refine_ls_abs_structure_details
'Flack H D (1983), Acta Cryst. A39, 876-881, 10479 Friedel pairs'
_refine_ls_abs_structure_Flack   0.059(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1086
_refine_ls_number_reflns         28790
_refine_ls_number_restraints     276
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0942
_refine_ls_R_factor_gt           0.0610
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0876P)^2^+0.7279P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1496
_refine_ls_wR_factor_ref         0.1684
_reflns_number_gt                20672
_reflns_number_total             28790
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc33047d.txt
_cod_data_source_block           4
_cod_original_sg_symbol_H-M      Pn
_cod_database_code               7107893