Synthesis and Structural Characterization of (1,4-Dihydropyrid-1-yl)aluminum Complexes
Karl Hensen; Alexander Lemke; Thorsten Stumpf; Michael Bolte; Holger Fleischer; Colin R. Pulham; Robert O. Gould; Steven Harris; Inorganic Chemistry 38 (1999) 4700–4704; doi:10.1021/ic9905695

data_4322322
_publ_contact_author
;
      Dr. Michael Bolte
      Institut f\"ur Organische Chemie
      J. W. Goethe-Universit\"at
      Marie-Curie-Str. 11
      60439 Frankfurt/Main
      Germany
;
_publ_contact_author_email       bolte@chemie.uni-frankfurt.de
_publ_contact_author_fax         '49 69 798 29128'
_publ_contact_author_phone       '49 69 798 29136'
_publ_section_title
;
 Synthesis and Structural Characterization of
 (1,4-Dihydropyrid-1-yl)aluminum Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4700
_journal_page_last               4704
_journal_paper_doi               10.1021/ic9905695
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C48 H60 Al Li N8'
_chemical_formula_weight         782.96
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           1
_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-97
_cell_angle_alpha                89.817(1)
_cell_angle_beta                 107.533(1)
_cell_angle_gamma                90.358(1)
_cell_formula_units_Z            1
_cell_length_a                   9.8484(1)
_cell_length_b                   10.4148(1)
_cell_length_c                   11.8007(1)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    173
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      1.00
_cell_volume                     1154.13(2)
_computing_cell_refinement       'Siemens SMART'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT'
_computing_molecular_graphics    'XP (Siemens XTL-Plus)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device       'Siemens CCD three circle diffractometer'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  'highly oriented graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0357
_diffrn_reflns_av_sigmaI/netI    0.0492
_diffrn_reflns_limit_h_max       12
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_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            20404
_diffrn_reflns_theta_full        26.43
_diffrn_reflns_theta_max         26.43
_diffrn_reflns_theta_min         1.96
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  840
_diffrn_standards_number         192
_exptl_absorpt_coefficient_mu    0.085
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7800
_exptl_absorpt_correction_type   'empirical, SADABS (Sheldrick,1996)'
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.127
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             420
_exptl_crystal_size_max          1.00
_exptl_crystal_size_mid          0.70
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.403
_refine_diff_density_min         -0.284
_refine_diff_density_rms         0.046
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.1(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.955
_refine_ls_goodness_of_fit_ref   0.955
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     527
_refine_ls_number_reflns         8894
_refine_ls_number_restraints     23
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.1071
_refine_ls_R_factor_gt           0.0773
_refine_ls_R_factor_obs          0.0773
_refine_ls_shift/su_max          0.481
_refine_ls_shift/su_mean         0.018
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1337P)^2^+0.4246P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2280
_refine_ls_wR_factor_gt          0.2020
_refine_ls_wR_factor_obs         0.2020
_refine_ls_wR_factor_ref         0.2280
_reflns_number_gt                6121
_reflns_number_total             8894
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic9905695_3.cif
_cod_data_source_block           II
_cod_depositor_comments
;
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^)+(0.1337P)^2^+0.4246P] 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^)+(0.1337P)^2^+0.4246P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1154.133(19)
_cod_database_code               4322322