Bis[N,N′-diisopropylbenzamidinato(−)]silicon(II): Cycloaddition Reactions with Organic 1,3-Dienes and 1,2-Diketones
Laskowski, Nadine; Junold, Konstantin; Kupper, Claudia; Baus, Johannes A.; Burschka, Christian; Tacke, Reinhold; Organometallics 33 (2014) 6141–; doi:10.1021/om500787k

data_4084473
_publ_section_title
;
 Bis[N,N&#x2032;-diisopropylbenzamidinato(&#x2212;)]silicon(II):
 Cycloaddition Reactions with Organic 1,3-Dienes and 1,2-Diketones
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              6141
_journal_paper_doi               10.1021/om500787k
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C40 H48 N4 O2 Si'
_chemical_formula_sum            'C40 H48 N4 O2 Si'
_chemical_formula_weight         644.91
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 95.724(12)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.256(2)
_cell_length_b                   9.9817(19)
_cell_length_c                   13.766(2)
_cell_measurement_reflns_used    8334
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.99
_cell_measurement_theta_min      2.56
_cell_volume                     1812.4(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP & POV-Ray'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_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-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0364
_diffrn_reflns_av_unetI/netI     0.0421
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            25475
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.020
_diffrn_reflns_theta_min         3.560
_diffrn_source                   'rotating anode'
_exptl_absorpt_coefficient_mu    0.104
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.7079
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs 2008/1 (Bruker 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.182
_exptl_crystal_description       block
_exptl_crystal_F_000             692
_exptl_crystal_size_max          0.501
_exptl_crystal_size_mid          0.431
_exptl_crystal_size_min          0.302
_refine_diff_density_max         0.165
_refine_diff_density_min         -0.188
_refine_diff_density_rms         0.034
_refine_ls_abs_structure_details
;
 Flack x determined using 2787 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.04(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     432
_refine_ls_number_reflns         7119
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0400
_refine_ls_R_factor_gt           0.0337
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0319P)^2^+0.2236P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0693
_refine_ls_wR_factor_ref         0.0724
_reflns_Friedel_coverage         0.887
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                6470
_reflns_number_total             7119
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om500787k_si_002.cif
_cod_data_source_block           LAS32B
_cod_depositor_comments
'Adding full bibliography for 4084466--4084473.cif.'
_cod_original_cell_volume        1812.3(6)
_cod_database_code               4084473
_shelx_estimated_absorpt_t_min   0.950
_shelx_estimated_absorpt_t_max   0.969
_shelxl_version_number           2013-4
_shelx_res_checksum              19460
_shelx_hkl_checksum              80213