Reversible Skeletal Transmetalations of Inorganic Rings: Isolation of Aluminatophosphazenes, a Zwitterionic Phosphazene, and a Donor-Stabilized Alumazine-Phosphazene Hybrid Cation
Eric Rivard; Paul J. Ragogna; Andrew R. McWilliams; Alan J. Lough; Ian Manners; Inorganic Chemistry 44 (2005) 6789–6798; doi:10.1021/ic0509938

data_4309616
_publ_contact_author_address
;Department of Chemistry
Lash Miller Chemical Laboratories
Universtiy of Toronto
Toronto, ON
M5S 3H6, CANADA
;
_publ_contact_author_email       imanners@chem.utoronto.ca
_publ_contact_author_fax         416-978-2450
_publ_contact_author_name        'Ian Manners'
_publ_contact_author_phone       416-978-6157
_publ_section_title
;
Reversible Skeletal Transmetalations of Inorganic Rings: Isolation of
Aluminatophosphazenes, a Zwitterionic Phosphazene, and a Donor-Stabilized
Alumazine-Phosphazene Hybrid Cation
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6789
_journal_page_last               6798
_journal_paper_doi               10.1021/ic0509938
_journal_volume                  44
_journal_year                    2005
_chemical_formula_moiety         'C2 H6 Cl4 F4 N3 P3'
_chemical_formula_sum            'C2 H6 Cl4 F4 N3 P3'
_chemical_formula_weight         382.81
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 96.0266(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.3252(1)
_cell_length_b                   12.2722(3)
_cell_length_c                   15.9610(4)
_cell_measurement_reflns_used    11084
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.6
_cell_volume                     1232.11(5)
_computing_cell_refinement       'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2003)'
_computing_data_reduction        Denzo-SMN
_computing_molecular_graphics    'SHELXTL V6.12'
_computing_publication_material  'SHELXTL V6.12'
_computing_structure_refinement  'SHELXTL V6.12(Sheldrick, 2001)'
_computing_structure_solution    'SIR-92 (Altomare et al., 1993)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker-Nonius KappaCCD'
_diffrn_measurement_method       '\f scans and \w scans with \k offsets'
_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  0.0447
_diffrn_reflns_av_sigmaI/netI    0.0509
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            9415
_diffrn_reflns_theta_full        27.44
_diffrn_reflns_theta_max         27.44
_diffrn_reflns_theta_min         2.57
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.374
_exptl_absorpt_correction_T_max  0.764
_exptl_absorpt_correction_T_min  0.703
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995)
;
_exptl_crystal_density_diffrn    2.064
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             752
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.425
_refine_diff_density_min         -0.498
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     147
_refine_ls_number_reflns         2788
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0622
_refine_ls_R_factor_gt           0.0353
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0348P)^2^+0.5058P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0765
_refine_ls_wR_factor_ref         0.0866
_reflns_number_gt                2038
_reflns_number_total             2788
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic0509938rom20050617_094215_2.cif
_cod_data_source_block           k02183
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 
;
_cod_original_cell_volume        1232.05(5)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4309616