Synthesis and characterisation of neutral and cationic alkyl aluminium complexes bearing N,O-Schiff base chelates with pendant donor arms
Paul A. Cameron; Vernon C. Gibson; Carl Redshaw; John A. Segal; Andrew J. P. White; David J. Williams; J. Chem. Soc., Dalton Trans.  (2002) 415–422; doi:10.1039/b106131n

data_7010982
_publ_section_title
;
 Synthesis and characterisation of neutral and cationic alkyl aluminium
 complexes bearing N,O-Schiff base chelates with pendant donor arms
;
_journal_issue                   3
_journal_name_full               'J. Chem. Soc., Dalton Trans.'
_journal_page_first              415
_journal_page_last               422
_journal_paper_doi               10.1039/b106131n
_journal_year                    2002
_chemical_formula_sum            'C52 H66 Al2 N4 O2'
_chemical_formula_weight         833.05
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                113.608(5)
_cell_angle_beta                 96.623(6)
_cell_angle_gamma                95.982(7)
_cell_formula_units_Z            4
_cell_length_a                   13.6167(10)
_cell_length_b                   18.114(2)
_cell_length_c                   22.0652(14)
_cell_measurement_reflns_used    27
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.71
_cell_measurement_theta_min      10.66
_cell_volume                     4885.6(8)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0304
_diffrn_reflns_av_sigmaI/netI    0.0536
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -3
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            14666
_diffrn_reflns_theta_max         59.99
_diffrn_reflns_theta_min         2.22
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.856
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.133
_exptl_crystal_description       'blocky needles'
_exptl_crystal_F_000             1792
_exptl_crystal_size_max          0.77
_exptl_crystal_size_mid          0.43
_exptl_crystal_size_min          0.27
_refine_diff_density_max         0.495
_refine_diff_density_min         -0.534
_refine_diff_density_rms         0.056
_refine_ls_extinction_coef       0.00057(14)
_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   1.025
_refine_ls_goodness_of_fit_obs   1.100
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1170
_refine_ls_number_reflns         12611
_refine_ls_number_restraints     2064
_refine_ls_restrained_S_all      1.228
_refine_ls_restrained_S_obs      1.316
_refine_ls_R_factor_all          0.1076
_refine_ls_R_factor_obs          0.0713
_refine_ls_shift/esd_max         -0.012
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1343P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2160
_refine_ls_wR_factor_obs         0.1809
_reflns_number_observed          9453
_reflns_number_total             13981
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b106131n.txt
_cod_data_source_block           VG9834
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1343P)^2^+0.0000P] 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^)+(0.1343P)^2^+0.0000P] 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        4885.5(7)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C52 H66 N4 O2 Al2'
_cod_database_code               7010982