Synthesis and Structure of Aryllithium Compounds Containing ortho-Directing (Dimethylamino)methyl and Trimethylhydrazino Substituents
Johannes Belzner; Dirk Schär; Uwe Dehnert; Mathias Noltemeyer; Organometallics 16 (1997) 285–288; doi:10.1021/om960858q

data_4063194
_publ_section_title
;
 Synthesis and Structure of Aryllithium Compounds Containing
 ortho-Directing (Dimethylamino)methyl and Trimethylhydrazino
 Substituents
;
_journal_issue                   2
_journal_name_full               Organometallics
_journal_page_first              285
_journal_page_last               288
_journal_paper_doi               10.1021/om960858q
_journal_volume                  16
_journal_year                    1997
_chemical_formula_sum            'C24 H42 Li2 N6'
_chemical_formula_weight         428.52
_chemical_name_common            6
_chemical_name_systematic
; 
 (2-(trimethylhydrazino)phenyl lithium)2 TMEDA 
;
_chemical_temperature_decomposition 438.15
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 110.22(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.106(2)
_cell_length_b                   13.654(3)
_cell_length_c                   17.189(3)
_cell_measurement_reflns_used    30
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      12
_cell_measurement_theta_min      10
_cell_volume                     2666.2(9)
_computing_cell_refinement       'Stoe Dif4'
_computing_data_collection       'Stoe Dif4'
_computing_data_reduction        'Stoe Redu4'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_measurement_device       'Stoe AED2'
_diffrn_measurement_method       'profile fitting'
_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  0.0388
_diffrn_reflns_av_sigmaI/netI    0.0445
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            3052
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         3.59
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  90
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.064
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            none
_exptl_crystal_density_diffrn    1.068
_exptl_crystal_description       plates
_exptl_crystal_F_000             936
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.70
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.221
_refine_diff_density_min         -0.238
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.034
_refine_ls_goodness_of_fit_obs   1.059
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     151
_refine_ls_number_reflns         1728
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_restrained_S_obs      1.059
_refine_ls_R_factor_all          0.0792
_refine_ls_R_factor_obs          0.0619
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0800P)^2^+4.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1794
_refine_ls_wR_factor_obs         0.1556
_reflns_number_observed          1352
_reflns_number_total             1732
_reflns_observed_criterion       >2sigma(I)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' tag was changed to
'_chemical_temperature_decomposition' since the value had been given
as 'dec. 165 \%C'. The value 'dec. 165 \%C' was changed to '438.15' -
it was converted from degrees Celsius(C) to Kelvins(K).

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0800P)^2^+4.0000P] 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^)+(0.0800P)^2^+4.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4063194