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_4117107
_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            'C38 H74 Li4 N2 O4 Si2'
_chemical_formula_weight         706.93
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 102.95(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.108(5)
_cell_length_b                   15.575(4)
_cell_length_c                   17.236(4)
_cell_measurement_reflns_used    62
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      10
_cell_volume                     4476(2)
_computing_cell_refinement       DIF4
_computing_data_collection       DIF4
_computing_data_reduction        REDU4
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_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 on 2theta/omega'
_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  0.0219
_diffrn_reflns_av_sigmaI/netI    0.0235
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6482
_diffrn_reflns_theta_max         22.51
_diffrn_reflns_theta_min         3.02
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  90
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.115
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.049
_exptl_crystal_description       blocks
_exptl_crystal_F_000             1552
_exptl_crystal_size_max          1.2
_exptl_crystal_size_mid          1.1
_exptl_crystal_size_min          0.9
_refine_diff_density_max         .356
_refine_diff_density_min         -.232
_refine_diff_density_rms         .044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.037
_refine_ls_goodness_of_fit_obs   1.063
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     494
_refine_ls_number_reflns         5829
_refine_ls_number_restraints     547
_refine_ls_restrained_S_all      1.082
_refine_ls_restrained_S_obs      1.074
_refine_ls_R_factor_all          0.0590
_refine_ls_R_factor_obs          0.0476
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
'calc w=1/[\s^2^(fo^2^)+(0.0664p)^2^+3.0143p] where p=(fo^2^+2fc^2^)/3'
_refine_ls_wR_factor_all         0.1339
_refine_ls_wR_factor_obs         0.1207
_reflns_number_observed          4900
_reflns_number_total             5832
_reflns_observed_criterion       >2sigma(i)
_cod_data_source_file            ja9521280_1.cif
_cod_data_source_block           ibiza
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_structure_factor_coef' value 'fsqd' changed to 'Fsqd'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from
2010-06-29.

'_atom_site_thermal_displace_type' value 'uani' changed
to 'Uani' according to the built-in table from CIF Core dictionary
named 'cif_core.dic' version 2.4.1 from 2010-06-29 (53
times).

'_atom_site_thermal_displace_type' value 'uiso' changed to
'Uiso' according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (80
times).

'_atom_site_refinement_flags' value 'u' changed to 'U'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (18
times).

'_atom_site_refinement_flags' value 'r' changed to 'R'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (68
times).

'_atom_site_refinement_flags' value 'd' changed to 'D'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (4 times).

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_atom_site_refinement_flags' value 'du' changed to 'DU' according to
the built-in table from CIF Core dictionary named 'cif_core.dic'
version 2.4.1 from 2010-06-29 (13 times).

'_atom_site_refinement_flags' value 'pdu' changed to 'PDU' according
to the built-in table from CIF Core dictionary named 'cif_core.dic'
version 2.4.1 from 2010-06-29 (6 times).

'_atom_site_refinement_flags' value 'pr' changed to 'PR' according to
the built-in table from CIF Core dictionary named 'cif_core.dic'
version 2.4.1 from 2010-06-29 (12 times).

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        4475.8(20)
_cod_database_code               4117107