Hydrosilylation catalysis by an earth alkaline metal silyl: synthesis, characterization, and reactivity of bis(triphenylsilyl)calcium
Valeri Leich; Thomas P. Spaniol; Laurent Maron; Jun Okuda; Chem.Commun. 50 (2014) 2311–; doi:10.1039/c3cc49308c

data_7112010
_publ_section_title
;
 Hydrosilylation catalysis by an earth alkaline metal silyl: synthesis,
 characterization, and reactivity of bis(triphenylsilyl)calcium
;
_journal_name_full               Chem.Commun.
_journal_page_first              2311
_journal_paper_doi               10.1039/c3cc49308c
_journal_volume                  50
_journal_year                    2014
_chemical_formula_moiety         'C52 H62 Ca O4 Si2'
_chemical_formula_sum            'C52 H62 Ca O4 Si2'
_chemical_formula_weight         847.28
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 105.746(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.1370(10)
_cell_length_b                   11.833(2)
_cell_length_c                   20.015(2)
_cell_measurement_reflns_used    1076
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      18.42
_cell_measurement_theta_min      2.54
_cell_volume                     2310.7(5)
_computing_cell_refinement       'Bruker SMART (2001)'
_computing_data_collection       'Bruker SMART (2001)'
_computing_data_reduction        'Bruker SAINT+ (1999)'
_computing_molecular_graphics    'ORTEP-III (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-92 (Altomare 1992)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-I CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  multilayer
_diffrn_radiation_source         microsource
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1203
_diffrn_reflns_av_sigmaI/netI    0.0834
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            27383
_diffrn_reflns_theta_full        26.43
_diffrn_reflns_theta_max         26.43
_diffrn_reflns_theta_min         2.02
_exptl_absorpt_coefficient_mu    0.232
_exptl_absorpt_correction_T_max  0.9750
_exptl_absorpt_correction_T_min  0.9595
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker Sadabs'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.218
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             908
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.426
_refine_diff_density_min         -0.289
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     268
_refine_ls_number_reflns         4740
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0932
_refine_ls_R_factor_gt           0.0545
_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^)+(0.0335P)^2^+0.7854P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1020
_refine_ls_wR_factor_ref         0.1183
_reflns_number_gt                3205
_reflns_number_total             4740
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cc49308c.txt
_cod_data_source_block           2a
_cod_database_code               7112010