The contrasting behaviour of bridged amido-cyclopentadienyl (constrained geometry) group 15 chlorides and cations derived therefrom
Wiacek, Robert J.; Macdonald, Charles L. B.; Jones, Jamie N.; Pietryga, Jeffrey M.; Cowley, Alan H.; Chemical Communications (Cambridge, United Kingdom)  (2003) 430–431; doi:10.1039/b211591c

data_7113695
_publ_section_title
;
 The contrasting behaviour of bridged amido-cyclopentadienyl (constrained
 geometry) group 15 chlorides and cations derived therefrom
;
_journal_coden_ASTM              CHCOFS
_journal_issue                   3
_journal_name_full
;
 Chemical Communications (Cambridge, United Kingdom)
;
_journal_page_first              430
_journal_page_last               431
_journal_paper_doi               10.1039/b211591c
_journal_year                    2003
_chemical_formula_moiety         '[C15 H27 N P Si][Al Cl4]'
_chemical_formula_sum            'C13.33 H24 Al0.89 Cl3.56 N0.89 P0.89 Si0.89'
_chemical_formula_weight         399.30
_chemical_name_common            '(CGC)phosphium aluminum tetrachloride'
_chemical_name_systematic
;
t-butyl(dimetyl(tetra-methylcyclopentadienyl)silyl)amido phosphium 
aluminum tetrachloride
;
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            9
_cell_length_a                   18.064(4)
_cell_length_b                   8.3447(17)
_cell_length_c                   30.103(6)
_cell_measurement_reflns_used    all
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      27.45
_cell_measurement_theta_min      3.01
_cell_volume                     4537.7(16)
_computing_cell_refinement       Denzo-SMN
_computing_data_collection       'Collect software, Nonius B.V. 1998'
_computing_data_reduction        Scalepack
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_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    0.0389
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            9381
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         3.01
_exptl_absorpt_coefficient_mu    0.682
_exptl_absorpt_correction_T_max  0.8756
_exptl_absorpt_correction_T_min  0.8756
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange-red
_exptl_crystal_density_diffrn    1.315
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1872
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         2.448
_refine_diff_density_min         -0.678
_refine_diff_density_rms         0.121
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.52(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     479
_refine_ls_number_reflns         9381
_refine_ls_number_restraints     91
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0862
_refine_ls_R_factor_gt           0.0767
_refine_ls_shift/su_max          0.611
_refine_ls_shift/su_mean         0.108
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1150P)^2^+9.5945P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1960
_refine_ls_wR_factor_ref         0.2060
_reflns_number_gt                8336
_reflns_number_total             9381
_reflns_threshold_expression     >2sigma(I)
_cod_duplicate_entry             7103964
_cod_data_source_file            b211591c.txt
_cod_data_source_block           pca21
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_cell_volume        4537.6(16)
_cod_original_sg_symbol_H-M      Pca2(1)
_cod_database_code               7113695