Dilithium 1,4-Disilacyclohexa-2,5-diene-1,4-diide by the Reduction of 1,4-Disilabicyclo[2.2.0]hexa-2,5-diene: Synthesis and Characterization
Nakata, Norio; Oikawa, Toru; Matsumoto, Takeshi; Kabe, Yoshio; Sekiguchi, Akira; Organometallics 25 (2006) 5850–; doi:10.1021/om0609261

data_4074592
_publ_section_title
;
 Dilithium 1,4-Disilacyclohexa-2,5-diene-1,4-diide by the Reduction of
 1,4-Disilabicyclo[2.2.0]hexa-2,5-diene:&#x00A0; Synthesis and
 Characterization
;
_journal_issue                   25
_journal_name_full               Organometallics
_journal_page_first              5850
_journal_paper_doi               10.1021/om0609261
_journal_volume                  25
_journal_year                    2006
_chemical_formula_sum            'C38 H78 Li2 O2 Si4'
_chemical_formula_weight         693.24
_chemical_name_systematic
; 
 1,4-disilabenzene dianion
;
_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                 97.8140(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.8090(2)
_cell_length_b                   18.5430(7)
_cell_length_c                   22.7350(8)
_cell_measurement_reflns_used    8056
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      25.75
_cell_measurement_theta_min      2.12
_cell_volume                     4514.5(2)
_computing_cell_refinement       'HKL scalepack'
_computing_data_collection       'MacScience Xpress'
_computing_data_reduction        Denzo
_computing_molecular_graphics    ORTEP
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR92
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.932
_diffrn_measured_fraction_theta_max 0.932
_diffrn_measurement_device_type  'MacScience DIP2030 Image plate'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0217
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            8056
_diffrn_reflns_theta_full        25.75
_diffrn_reflns_theta_max         25.75
_diffrn_reflns_theta_min         2.12
_exptl_absorpt_coefficient_mu    0.159
_exptl_absorpt_correction_T_max  0.969
_exptl_absorpt_correction_T_min  0.963
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.020
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1536
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.717
_refine_diff_density_min         -0.417
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         8056
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0539
_refine_ls_R_factor_gt           0.0499
_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^)+(0.0788P)^2^+2.5454P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1343
_refine_ls_wR_factor_ref         0.1382
_reflns_number_gt                7370
_reflns_number_total             8056
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0609261si20061009_094656.cif
_cod_data_source_block           dianion
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21/c          '
_cod_database_code               4074592