Synthesis and Characterization of the Non-Kekulé, Singlet Biradicaloid Ar'Ge(μ-NSiMe3)2GeAr' (Ar' = 2,6-Dipp2C6H3, Dipp = 2,6-i-Pr2C6H3)
Chunming Cui; Marcin Brynda; Marilyn M. Olmstead; Philip P. Power; Journal of the American Chemical Society 126 (2004) 6510–6511; doi:10.1021/ja0492182

data_4112615
_publ_section_title
;
 Synthesis and Characterization of the Non-Kekul\'e, Singlet Biradicaloid
 Ar'Ge(\m-NSiMe3)2GeAr' (Ar' = 2,6-Dipp2C6H3, Dipp = 2,6-i-Pr2C6H3)
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6510
_journal_page_last               6511
_journal_paper_doi               10.1021/ja0492182
_journal_volume                  126
_journal_year                    2004
_chemical_formula_sum            'C72 H106 Ge2 N2 Si2'
_chemical_formula_weight         1200.95
_chemical_name_common            '[Dipp*Ge(NSiMe3)]2.n-hexane'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 107.243(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.9746(16)
_cell_length_b                   11.6981(7)
_cell_length_c                   25.186(2)
_cell_measurement_reflns_used    998
_cell_measurement_temperature    91(2)
_cell_measurement_theta_max      20.0
_cell_measurement_theta_min      3.3
_cell_volume                     6746.1(8)
_computing_cell_refinement       'SMART 5.054 (Bruker, 2002)'
_computing_data_collection       'SMART 5.054 (Bruker, 2002)'
_computing_data_reduction        'SAINT 6.36A (Bruker, 2003)'
_computing_molecular_graphics    'SHELXTL 5.1, XP (Sheldrick, 1994)'
_computing_publication_material  'SHELXL-97 '
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      91(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker SMART 1000'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0346
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            10241
_diffrn_reflns_theta_full        30.51
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_min         1.69
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.967
_exptl_absorpt_correction_T_max  0.944
_exptl_absorpt_correction_T_min  0.760
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2.10 (Sheldrick, 2003)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.182
_exptl_crystal_description       block
_exptl_crystal_F_000             2576
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.128
_refine_diff_density_min         -0.623
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     360
_refine_ls_number_reflns         10241
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0619
_refine_ls_R_factor_gt           0.0385
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0423P)^2^+15.1391P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0920
_refine_ls_wR_factor_ref         0.1056
_reflns_number_gt                7873
_reflns_number_total             10241
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja0492182si20040212_061637.cif
_cod_data_source_block           ar102
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4112615