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_4063193
_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            'C26 H42 Li2 N2 O'
_chemical_formula_weight         412.515
_chemical_melting_point          'impossible to measure'
_chemical_name_common            2
_chemical_name_systematic
; 
 (4,6 dimethyl-2-(dimethylaminomethyl)phenyl lithium)2 . et2O 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                76.21(3)
_cell_angle_beta                 73.58(2)
_cell_angle_gamma                70.06(2)
_cell_formula_units_Z            2
_cell_length_a                   10.642(5)
_cell_length_b                   11.231(7)
_cell_length_c                   12.641(6)
_cell_measurement_reflns_used    30
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      12
_cell_measurement_theta_min      10
_cell_volume                     1345.4(12)
_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  0.0922
_diffrn_reflns_av_sigmaI/netI    0.0462
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            5109
_diffrn_reflns_theta_max         24.94
_diffrn_reflns_theta_min         3.58
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  90
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.060
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.018
_exptl_crystal_description       blocks
_exptl_crystal_F_000             452
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.80
_exptl_crystal_size_min          0.50
_refine_diff_density_max         0.240
_refine_diff_density_min         -0.257
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.021
_refine_ls_goodness_of_fit_obs   1.041
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         4686
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_restrained_S_obs      1.041
_refine_ls_R_factor_all          0.0979
_refine_ls_R_factor_obs          0.0646
_refine_ls_shift/esd_max         -0.416
_refine_ls_shift/esd_mean        0.009
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0968P)^2^+0.6997P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1981
_refine_ls_wR_factor_obs         0.1627
_reflns_number_observed          3203
_reflns_number_total             4690
_reflns_observed_criterion       >2sigma(I)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0968P)^2^+0.6997P] 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^)+(0.0968P)^2^+0.6997P] 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      P-1
_cod_database_code               4063193