Isolation and characterization of the tetralithium salt of [5]radialene tetraanion stabilized by silyl groups
Matsuo, Tsukasa; Fure, Hidetoshi; Sekiguchi, Akira; Chemical Communications  (1999) 1981–; doi:10.1039/a906253j

data_7110676
_publ_section_title
;
 Isolation and characterization of the tetralithium salt of [5]radialene
 tetraanion stabilized by silyl groups
;
_journal_issue                   19
_journal_name_full               'Chemical Communications'
_journal_page_first              1981
_journal_paper_doi               10.1039/a906253j
_journal_year                    1999
_chemical_formula_sum            'C45 H86 Li4 O4 Si8'
_chemical_formula_weight         943.63
_chemical_melting_point          ?
_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                 115.003(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   48.328(3)
_cell_length_b                   13.470(1)
_cell_length_c                   21.676(1)
_cell_measurement_reflns_used    all
_cell_measurement_temperature    180
_cell_measurement_theta_max      27.00
_cell_measurement_theta_min      1
_cell_volume                     12788.2(14)
_computing_cell_refinement       Scalepack
_computing_data_collection       'MacScience Xpress'
_computing_data_reduction        Denzo
_computing_molecular_graphics    ORTEP
_computing_publication_material  maXus
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR92
_diffrn_ambient_temperature      295
_diffrn_measured_fraction_theta_full 0.589
_diffrn_measured_fraction_theta_max 0.589
_diffrn_measurement_device       'MacScience DIP2030 Image plate'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_limit_h_max       55
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            10585
_diffrn_reflns_theta_full        24.31
_diffrn_reflns_theta_max         24.31
_diffrn_reflns_theta_min         4.07
_exptl_absorpt_coefficient_mu    0.204
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    0.981
_exptl_crystal_density_meas      ?
_exptl_crystal_description       Prism
_exptl_crystal_F_000             4496
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.875
_refine_diff_density_min         -0.528
_refine_diff_density_rms         0.091
_refine_ls_extinction_coef       0.0008(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.947
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     554
_refine_ls_number_reflns         6138
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.947
_refine_ls_R_factor_all          0.0775
_refine_ls_R_factor_gt           0.0775
_refine_ls_shift/su_max          5.752
_refine_ls_shift/su_mean         0.208
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2358
_refine_ls_wR_factor_ref         0.2358
_reflns_number_gt                6138
_reflns_number_total             10115
_reflns_threshold_expression     >3sigma(I)
_cod_data_source_file            906253jsup1.cif
_cod_data_source_block           shelxl
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

'_symmetry_cell_setting' value
'Monoclinic' changed to 'monoclinic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

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_cell_volume        12788(1)
_cod_original_sg_symbol_H-M      'C 2/c         '
_cod_database_code               7110676