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_4121010
_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         'C40 H62 Cl2 N2 Si2'
_chemical_formula_sum            'C40 H62 Cl2 N2 Si2'
_chemical_formula_weight         698.00
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2012
_cell_angle_alpha                106.28(3)
_cell_angle_beta                 99.73(2)
_cell_angle_gamma                92.60(2)
_cell_formula_units_Z            4
_cell_length_a                   9.079(7)
_cell_length_b                   19.085(7)
_cell_length_c                   24.21(3)
_cell_measurement_reflns_used    45971
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.5
_cell_measurement_theta_min      0.98
_cell_volume                     3950(6)
_computing_cell_refinement       'SAINT V8.27B (Bruker AXS, 2012)'
_computing_data_collection       'APEX2 v2009.11-0'
_computing_data_reduction        'SAINT V8.27B (Bruker AXS, 2012)'
_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 0.952
_diffrn_measured_fraction_theta_max 0.939
_diffrn_measurement_device_type  'Microdiffractometer at the P11 beamline'
_diffrn_measurement_method       '\f scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6199
_diffrn_reflns_av_R_equivalents  0.0469
_diffrn_reflns_av_unetI/netI     0.0510
_diffrn_reflns_Laue_measured_fraction_full 0.952
_diffrn_reflns_Laue_measured_fraction_max 0.939
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            64661
_diffrn_reflns_point_group_measured_fraction_full 0.952
_diffrn_reflns_point_group_measured_fraction_max 0.939
_diffrn_reflns_theta_full        21.835
_diffrn_reflns_theta_max         24.410
_diffrn_reflns_theta_min         0.974
_diffrn_source                   'monochromated x-rays beamline P11@PetraIII'
_exptl_absorpt_coefficient_mu    0.175
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6787
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS version 2012/1, multi-scan. (G. M. Sheldrick, 2012)
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.174
_exptl_crystal_description       rectangle
_exptl_crystal_F_000             1512
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.24
_refine_diff_density_max         1.072
_refine_diff_density_min         -0.588
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     881
_refine_ls_number_reflns         18420
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0591
_refine_ls_R_factor_gt           0.0525
_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^)+(0.0797P)^2^+2.1731P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1486
_refine_ls_wR_factor_ref         0.1538
_reflns_number_gt                15871
_reflns_number_total             18420
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja4072139_si_002.cif
_cod_data_source_block           km132
_cod_database_code               4121010
_shelxl_version_number           2012-9
_shelx_res_checksum              9912