Formation of a 1,4-Diamino-2,3-disila-1,3-butadiene Derivative
Kartik Chandra Mondal; Herbert W. Roesky; Birger Dittrich; Nicole Holzmann; Markus Hermann; Gernot Frenking; Alke Meents; Journal of the American Chemical Society 135 (2013) 15990–15993; doi:10.1021/ja4072139

data_4121011
_publ_section_title
;
 Formation of a 1,4-Diamino-2,3-disila-1,3-butadiene Derivative
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15990
_journal_page_last               15993
_journal_paper_doi               10.1021/ja4072139
_journal_volume                  135
_journal_year                    2013
_chemical_formula_moiety         'C20 H31 Cl4 N Si'
_chemical_formula_sum            'C20 H31 Cl4 N Si'
_chemical_formula_weight         455.35
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2012
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.177(4)
_cell_length_b                   14.588(5)
_cell_length_c                   15.114(6)
_cell_measurement_reflns_used    34748
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22.40
_cell_measurement_theta_min      1.62
_cell_volume                     2243.9(15)
_computing_cell_refinement       'XDS (Kabsch, 2010)'
_computing_data_collection       'XDS (Kabsch, 2010)'
_computing_publication_material  'enCIFer 1.4, CCDC, 2011'
_computing_structure_refinement  'SHELXL-2012 (Sheldrick, 2012)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Microdiffractometer at the SLS'
_diffrn_measurement_method       '\f scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6358
_diffrn_reflns_av_R_equivalents  0.0752
_diffrn_reflns_av_unetI/netI     0.0461
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            40936
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        22.425
_diffrn_reflns_theta_max         27.023
_diffrn_reflns_theta_min         1.736
_diffrn_source                   'monochromated x-rays beamline X10SA@SLS'
_exptl_absorpt_coefficient_mu    0.424
_exptl_absorpt_correction_T_max  0.7426
_exptl_absorpt_correction_T_min  0.6832
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS version 2008/2, multi-scan. (G. M. Sheldrick, 2008)
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.3479
_exptl_crystal_description       plate
_exptl_crystal_F_000             960
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.582
_refine_diff_density_min         -0.597
_refine_diff_density_rms         0.069
_refine_ls_abs_structure_details
;
 Flack x determined using 2950 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.04(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     282
_refine_ls_number_reflns         6778
_refine_ls_number_restraints     91
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0348
_refine_ls_R_factor_gt           0.0346
_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^)+(0.0380P)^2^+0.9153P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0917
_refine_ls_wR_factor_ref         0.0919
_reflns_Friedel_coverage         0.786
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.985
_reflns_number_gt                6744
_reflns_number_total             6778
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja4072139_si_003.cif
_cod_data_source_block           km117
_cod_original_cell_volume        2243.9(14)
_cod_database_code               4121011
_shelxl_version_number           2012-9
_shelx_res_checksum              76604