Dimeric [3,3-Dimethyl-2-(trimethylsilyl)cyclopropenyl]- lithium-Tetramethylethylenediamine: Distortion of the Cyclopropenyl Geometry Due to Strong Rehybridization at the Lithiated Carbon
Klas Sorger; Paul von Ragué Schleyer; Dietmar Stalke; Journal of the American Chemical Society 118 (1996) 1086–1091; doi:10.1021/ja9521280

data_4117108
_publ_section_title
;
 Dimeric [3,3-Dimethyl-2-(trimethylsilyl)cyclopropenyl]-
 lithium-Tetramethylethylenediamine: Distortion of the Cyclopropenyl
 Geometry Due to Strong Rehybridization at the Lithiated Carbon
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1086
_journal_page_last               1091
_journal_paper_doi               10.1021/ja9521280
_journal_volume                  118
_journal_year                    1996
_chemical_formula_sum            'C22 H40 Li2 O3'
_chemical_formula_weight         366.42
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.272(7)
_cell_length_b                   21.323(4)
_cell_length_c                   13.051(4)
_cell_measurement_reflns_used    64
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      10
_cell_volume                     4528(3)
_computing_cell_refinement       DIF4
_computing_data_collection       DIF4
_computing_data_reduction        REDU4
_computing_molecular_graphics    'SHELXL-93 (Sheldrick, 1993)'
_computing_publication_material  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_measurement_device       STOE-AED
_diffrn_measurement_method       'profile fitted 2thetha/omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0491
_diffrn_reflns_av_sigmaI/netI    0.0291
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            4918
_diffrn_reflns_theta_max         22.51
_diffrn_reflns_theta_min         4.00
_diffrn_standards_decay_%        0.0
_diffrn_standards_interval_count 90
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.067
_exptl_absorpt_correction_T_max  0.7909
_exptl_absorpt_correction_T_min  0.4544
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.075
_exptl_crystal_description       blocks
_exptl_crystal_F_000             1616
_exptl_crystal_size_max          1.4
_exptl_crystal_size_mid          0.8
_exptl_crystal_size_min          0.8
_refine_diff_density_max         .315
_refine_diff_density_min         -.222
_refine_diff_density_rms         .048
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.10(189)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.054
_refine_ls_goodness_of_fit_obs   1.055
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     577
_refine_ls_number_reflns         4339
_refine_ls_number_restraints     531
_refine_ls_restrained_S_all      1.058
_refine_ls_restrained_S_obs      1.060
_refine_ls_R_factor_all          0.0771
_refine_ls_R_factor_obs          0.0682
_refine_ls_shift/esd_max         -0.015
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1204P)^2^+2.9289P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1909
_refine_ls_wR_factor_obs         0.1781
_reflns_number_observed          3830
_reflns_number_total             4339
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja9521280_2.cif
_cod_data_source_block           rotz
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' tag value 'orthorombic' was replaced with
'orthorhombic' value as specified in the replacement file
'/home/robertas/cod-tools/perl-scripts/inputs/replacement_values.lst'.

'_exptl_absorpt_correction_type' tag value 'psi-scans' was replaced
with 'psi-scan' value as specified in the replacement file
'/home/robertas/cod-tools/perl-scripts/inputs/replacement_values.lst'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1204P)^2^+2.9289P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1204P)^2^+2.9289P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        4528.3(25)
_cod_database_code               4117108