The arched four-rung ladder structure of the unsolvated dilithium salt of N,N′-bis(trimethylsilyl)-2-aminobenzylamine, and its structural deformation on THF complexation
Gauvin, Régis M.; Kress, Jacky; Kyritsakas, Nathalie; Fischer, Jean; Chemical Communications  (2000) 965–; doi:10.1039/b002004o

data_7110925
_publ_section_title
;
 The arched four-rung ladder structure of the unsolvated dilithium salt of
 N,N&#x2032;-bis(trimethylsilyl)-2-aminobenzylamine, and its structural
 deformation on THF complexation
;
_journal_issue                   11
_journal_name_full               'Chemical Communications'
_journal_page_first              965
_journal_paper_doi               10.1039/b002004o
_journal_year                    2000
_chemical_formula_moiety         'C34 H64 Li4 N4 O2 Si4'
_chemical_formula_sum            'C34 H64 Li4 N4 O2 Si4'
_chemical_formula_weight         701.02
_chemical_name_systematic        ' ?'
_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'
_cell_angle_alpha                90
_cell_angle_beta                 99.750(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.9167(9)
_cell_length_b                   9.8818(2)
_cell_length_c                   22.1151(9)
_cell_measurement_reflns_used    29787
_cell_measurement_temperature    173
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1.4
_cell_volume                     4289.7(3)
_computing_publication_material  CIFGEN_IN_OpenMoleN_(_1997)
_computing_structure_refinement  LSFM_OpenMoleN_(_1997)
_computing_structure_solution    Direct_methods_(SIR,_Burla_et_al.,_1989)
_diffrn_ambient_temperature      173
_diffrn_measurement_details
;
  29787 reflections were collected using program Collect
 ("Collect" Data collection software, Nonius B.V., 1998)
 The conditions were as follow : crystal to detector distance =  35. mm.
 Scan angle =  2.1 deg 1 scans of  100 sec per frame.
 Data collection was divided into  2 sets
 with the following starting angles and number of frames :

 Set 1 Theta =    8.09 Omega =  180.00 Kappa =    0.00   87 frames
 Set 2 Theta =   -8.08 Kappa =  173.50 Phi   =    0.00   32 frames
 Friedel pairs were not averaged. Internal R = 0.04
;
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       '\p scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           Mo-K\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.045
_diffrn_reflns_av_sigmaI/netI    0.333
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            29787
_diffrn_reflns_theta_max         27.53
_diffrn_reflns_theta_min         2.5
_diffrn_source                   xray_tube
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.170
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.09
_exptl_crystal_density_method    none
_exptl_crystal_description       prism
_exptl_crystal_F_000             1520
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.483
_refine_diff_density_min         -0.173
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.580
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     442
_refine_ls_number_reflns         4972
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.102
_refine_ls_R_factor_gt           0.043
_refine_ls_shift/esd_mean        0.001
_refine_ls_shift/su_max          0.004
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 4Fo^2^/(\s^2^(Fo^2^) + 0.0064 Fo^4^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.097
_refine_ls_wR_factor_ref         0.064
_reflns_number_gt                4972
_reflns_number_total             10292
_reflns_threshold_expression     3.0\s(I)
_cod_data_source_file            b002004osup1.cif
_cod_data_source_block           st416
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value '4Fo^2^/(\s^2^(Fo^2^) + 0.0064
Fo^4^)' was changed to 'calc'. New tag '_refine_ls_weighting_details'
was created. The value of the new tag was set to 'w =
4Fo^2^/(\s^2^(Fo^2^) + 0.0064 Fo^4^)'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_original_cell_volume        4289.7(5)
_cod_database_code               7110925