An unprecedented coordination mode for hemilabile pendant-arm 1,4,7-triazacyclononanes and the synthesis of cationic organoaluminium complexes
Robson, David A.; Rees, Leigh H.; Mountford, Philip; Schröder, Martin; Chemical Communications  (2000) 1269–; doi:10.1039/b003019h

data_7110973
_publ_section_title
;
 An unprecedented coordination mode for hemilabile pendant-arm
 1,4,7-triazacyclononanes and the synthesis of cationic organoaluminium
 complexes
;
_journal_issue                   14
_journal_name_full               'Chemical Communications'
_journal_page_first              1269
_journal_paper_doi               10.1039/b003019h
_journal_year                    2000
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C34 H76 Al2  N6 O2'
_chemical_formula_structural     'C34 H76 AL2 N6 O2'
_chemical_formula_sum            'C34 H76 Al2 N6 O2'
_chemical_formula_weight         654.97
_chemical_name_systematic
;
 [Al2(L-2)Me4]
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 95.998(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.2690(5)
_cell_length_b                   13.4100(6)
_cell_length_c                   12.4290(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     2033.71(14)
_computing_cell_refinement       DENZO
_computing_data_collection       'Enraf-Nonius DIP2000 Software - XPRESS'
_computing_data_reduction        'DENZO & SCALEPACK'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1998)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    SIR-92
_diffrn_ambient_temperature      150(2)
_diffrn_measurement_device
'Enraf-Nonius DIP2000 Image Plate Diffractometer'
_diffrn_measurement_method       'Omega scans'
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0452
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            4232
_diffrn_reflns_theta_max         26.49
_diffrn_reflns_theta_min         1.67
_exptl_absorpt_coefficient_mu    0.106
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.070
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       prism
_exptl_crystal_F_000             728
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.462
_refine_diff_density_min         -0.261
_refine_diff_density_rms         0.068
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.09(28)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.298
_refine_ls_goodness_of_fit_obs   1.311
_refine_ls_matrix_type           full
_refine_ls_number_parameters     411
_refine_ls_number_reflns         4231
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.342
_refine_ls_restrained_S_obs      1.310
_refine_ls_R_factor_all          0.0726
_refine_ls_R_factor_obs          0.0691
_refine_ls_shift/esd_max         0.011
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0703P)^2^+1.6410P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1740
_refine_ls_wR_factor_obs         0.1677
_reflns_number_observed          4128
_reflns_number_total             4232
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b003019hsup1.cif
_cod_data_source_block           compound2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' 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^)+(0.0703P)^2^+1.6410P] 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^)+(0.0703P)^2^+1.6410P] 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      'P 21'
_cod_database_code               7110973