Transition Metal Complexes with Sterically Demanding Ligands. 2.1Meisenheimer Complex Formation and Deprotonation Reactions of a Sterically Demanding Aromatic Diimine†
Nückel, Stefan; Burger, Peter; Organometallics 19 (2000) 3305–; doi:10.1021/om000084k

data_4077492
_publ_section_title
;
 Transition Metal Complexes with Sterically Demanding Ligands.
 2.1Meisenheimer Complex Formation and Deprotonation Reactions of a
 Sterically Demanding Aromatic Diimine&#x2020;
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              3305
_journal_paper_doi               10.1021/om000084k
_journal_volume                  19
_journal_year                    2000
_chemical_compound_source        synthesis
_chemical_formula_analytical     'C34 H42 Li2 N2 * 2 DME'
_chemical_formula_sum            'C42 H62 Li2 N2 O4'
_chemical_formula_weight         672.82
_chemical_melting_point          ?
_space_group_IT_number           15
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 1'
_atom_sites_solution_hydrogens   'geom (a) and diference Fourier map (b)'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 99.000(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.3560(10)
_cell_length_b                   14.8880(10)
_cell_length_c                   19.760(2)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      n/a
_cell_measurement_theta_min      n/a
_cell_volume                     4171.4(6)
_computing_cell_refinement       'STOE IPDS Programm Package'
_computing_data_collection       'STOE IPDS Programm Package'
_computing_data_reduction        'STOE IPDS Programm Package'
_computing_molecular_graphics    'Schakal97 (Keller, 1997)'
_computing_publication_material  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measurement_device       'STOE IPDS'
_diffrn_measurement_method       'Image Plate'
_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  0.0231
_diffrn_reflns_av_sigmaI/netI    0.0455
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            7383
_diffrn_reflns_theta_max         25.87
_diffrn_reflns_theta_min         3.04
_diffrn_standards_decay_%        n/a
_diffrn_standards_interval_count n/a
_diffrn_standards_interval_time  n/a
_diffrn_standards_number         n/a
_exptl_absorpt_coefficient_mu    0.067
_exptl_absorpt_correction_T_max  n/a
_exptl_absorpt_correction_T_min  n/a
_exptl_absorpt_correction_type   n/a
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.071
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    n/a
_exptl_crystal_description       plate
_exptl_crystal_F_000             1464
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.204
_refine_diff_density_min         -0.160
_refine_diff_density_rms         0.031
_refine_ls_extinction_coef       n/a
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.068
_refine_ls_goodness_of_fit_obs   1.268
_refine_ls_hydrogen_treatment    'riding model (a), isotropic (b)'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     331
_refine_ls_number_reflns         3770
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.087
_refine_ls_restrained_S_obs      1.268
_refine_ls_R_factor_all          0.0895
_refine_ls_R_factor_obs          0.0631
_refine_ls_shift/esd_max         0.813
_refine_ls_shift/esd_mean        0.030
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+4.9321P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1657
_refine_ls_wR_factor_obs         0.1551
_reflns_number_observed          2528
_reflns_number_total             3771
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            om000084k.cif
_cod_data_source_block           Complex5
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'n/a' was changed to '?' - the value
is undefined or not given.

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

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'n/a' 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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+4.9321P] 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^)+(0.0500P)^2^+4.9321P] 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      I2/a
_cod_database_code               4077492