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_4322320
_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_moiety         '[Al(Hpyr)3(pyr)].0.5PhMe'
_chemical_formula_sum            'C23.5 H27 Al N4'
_chemical_formula_weight         392.47
_chemical_name_systematic
; 
 ? 
;
_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   difmap
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL
_cell_angle_alpha                109.74(3)
_cell_angle_beta                 98.28(3)
_cell_angle_gamma                96.43(3)
_cell_formula_units_Z            2
_cell_length_a                   9.202(5)
_cell_length_b                   10.888(5)
_cell_length_c                   11.756(5)
_cell_measurement_reflns_used    32
_cell_measurement_temperature    220(2)
_cell_measurement_theta_max      16
_cell_measurement_theta_min      15
_cell_volume                     1080.6(9)
_computing_cell_refinement       'Stoe DIF4'
_computing_data_collection       'Stoe DIF4'
_computing_data_reduction        'Stoe REDU4'
_computing_molecular_graphics    SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    SHELXTL
_diffrn_ambient_temperature      220(2)
_diffrn_measurement_device
; 
Stoe Stadi-4 diffractometer with 
Oxford Cryosystems variable temperature device. 
;
_diffrn_measurement_method       'Omega-theta with learnt profile (Clegg)'
_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  0.1072
_diffrn_reflns_av_sigmaI/netI    0.0364
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7090
_diffrn_reflns_theta_max         27.54
_diffrn_reflns_theta_min         2.65
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.110
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.206
_exptl_crystal_description       block
_exptl_crystal_F_000             418
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.47
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.358
_refine_diff_density_min         -0.196
_refine_diff_density_rms         0.042
_refine_ls_extinction_coef       0.0014(23)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.021
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     383
_refine_ls_number_reflns         4919
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.046
_refine_ls_restrained_S_obs      1.029
_refine_ls_R_factor_all          0.0736
_refine_ls_R_factor_gt           0.0498
_refine_ls_shift/esd_mean        0.000
_refine_ls_shift/su_max          -0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0512P)^2^+0.5330P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1354
_refine_ls_wR_factor_ref         0.1163
_reflns_number_gt                3656
_reflns_number_total             4950
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9905695_1.cif
_cod_data_source_block           IV
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0512P)^2^+0.5330P] 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^)+(0.0512P)^2^+0.5330P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 

The following automatic conversions were performed:

'_atom_sites_solution_hydrogens' value 'difference Fourier map' was
changed to 'difmap'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_formula_sum        'C23.50 H27 Al N4'
_cod_database_code               4322320