Iminophosphine Cycloaddition Reactions of a Diazaphosphoniaaluminatacyclobutane and a Novel Intramolecular Phosphiridine P\ρightarrowP Coordination
Neil Burford; Daren J. LeBlanc; Inorganic Chemistry 38 (1999) 2248–2249; doi:10.1021/ic9813718

data_4322021
_publ_contact_author_address
;  Department of Chemistry
   Dalhousie University
   Halifax, NS B3H 4J3
   CANADA
;
_publ_contact_author_email       burford@chem1.chem.dal.ca
_publ_contact_author_fax         '(902) 494-1310'
_publ_contact_author_name        'Neil Burford'
_publ_contact_author_phone       '(902) 494-3681'
_publ_section_title
;
 Iminophosphine Cycloaddition Reactions of a
 Diazaphosphoniaaluminatacyclobutane and a Novel Intramolecular
 Phosphiridine P\\rightarrowP Coordination
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2248
_journal_page_last               2249
_journal_paper_doi               10.1021/ic9813718
_journal_volume                  38
_journal_year                    1999
_chemical_formula_moiety         'C15 H45 Al Cl2 N4 P2 Si5'
_chemical_formula_sum            'C15 H45 Al Cl2 N4 P2 Si5'
_chemical_formula_weight         581.82
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 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                 119.5280(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.2416(14)
_cell_length_b                   8.9070(7)
_cell_length_c                   18.5029(13)
_cell_measurement_reflns_used    11799
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.35
_cell_measurement_theta_min      4.10
_cell_volume                     3189.4(4)
_computing_cell_refinement       'DENZO-SMN (Nonius, 1997)'
_computing_data_collection       'KappaCCD Server software (Nonius, 1997)'
_computing_data_reduction        'DENZO-SMN (Nonius, 1997)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1994)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 9.2
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '1\% rotations on \f'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube (50 kV, 23 mA)'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.071
_diffrn_reflns_av_sigmaI/netI    0.0896
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            11799
_diffrn_reflns_theta_full        26.35
_diffrn_reflns_theta_max         26.35
_diffrn_reflns_theta_min         4.10
_diffrn_standards_decay_%        negligible
_exptl_absorpt_coefficient_mu    0.531
_exptl_absorpt_correction_T_max  0.9246
_exptl_absorpt_correction_T_min  0.8787
_exptl_absorpt_correction_type   'multi-scan (Nonius, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.212
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1240
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.237
_refine_diff_density_min         -0.318
_refine_diff_density_rms         0.057
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0..45(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.979
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     295
_refine_ls_number_reflns         6229
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      0.978
_refine_ls_R_factor_all          0.0656
_refine_ls_R_factor_gt           0.0414
_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^)+(0.0321P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0836
_refine_ls_wR_factor_ref         0.0910
_reflns_number_gt                4795
_reflns_number_total             6229
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            ic9813718_1.cif
_cod_data_source_block           djl52_3
_cod_database_code               4322021