Synthesis and X-ray Structure of the Novel Aluminum Complex [{η3-HB(3-Phpz)2(5-Phpz)}2Al][AlCl4]. Catalysis of CO2/Propylene Oxide to Propylene Carbonate by the AlCl4-Anion
Donald J. Darensbourg; Ernest L. Maynard; Matthew W. Holtcamp; Kevin K. Klausmeyer; Joseph H. Reibenspies; Inorganic Chemistry 35 (1996) 2682–2684; doi:10.1021/ic951018r

data_4323807
_publ_section_title
;
 Synthesis and X-ray Structure of the Novel Aluminum Complex
 [{\h3-HB(3-Phpz)2(5-Phpz)}2Al][AlCl4]. Catalysis of CO2/Propylene Oxide
 to Propylene Carbonate by the AlCl4-Anion
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2682
_journal_page_last               2684
_journal_paper_doi               10.1021/ic951018r
_journal_volume                  35
_journal_year                    1996
_chemical_formula_sum            'C62 H60 Al2 B2 Cl4 N12 O2'
_chemical_formula_weight         1222.64
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.924(2)
_cell_length_b                   17.483(6)
_cell_length_c                   20.572(3)
_cell_measurement_temperature    293(2)
_cell_volume                     6087(2)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_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    0.1297
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5923
_diffrn_reflns_theta_max         25.06
_diffrn_reflns_theta_min         2.53
_exptl_absorpt_coefficient_mu    0.278
_exptl_crystal_density_diffrn    1.334
_exptl_crystal_F_000             2544
_refine_diff_density_max         1.340
_refine_diff_density_min         -0.460
_refine_diff_density_rms         0.093
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.15(23)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.042
_refine_ls_goodness_of_fit_obs   1.135
_refine_ls_matrix_type           full
_refine_ls_number_parameters     691
_refine_ls_number_reflns         5922
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_restrained_S_obs      1.135
_refine_ls_R_factor_all          0.1664
_refine_ls_R_factor_obs          0.0840
_refine_ls_shift/esd_max         0.140
_refine_ls_shift/esd_mean        0.010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1129P)^2^+16.2544P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2585
_refine_ls_wR_factor_obs         0.2093
_reflns_number_observed          3581
_reflns_number_total             5923
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic951018r.cif
_cod_data_source_block           complex1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1129P)^2^+16.2544P] 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^)+(0.1129P)^2^+16.2544P] where P=(Fo^2^+2Fc^2^)/3'.

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

2020-09-02
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C31 H30 Al B Cl2 N6 O'
_cod_original_formula_weight         611.32
_cod_original_formula_units_Z            8
_cod_original_cell_volume        6086.9(24)
_cod_database_code               4323807