Synthesis and Structures of Complexes Demonstrating the Coordinative Versatility of the 2,4-Diimino-3-phosphinopentene Anion (γ-Phosphino-β-diketiminate)
Neil Burford; Mark D'eon; Paul J. Ragogna; Robert McDonald; Michael J. Ferguson; Inorganic Chemistry 43 (2004) 734–738; doi:10.1021/ic0351444

data_4310467
_publ_contact_author_address
;Department of Chemistry
Dalhousie University
Halifax, NS
B3H 4J3, CANADA
;
_publ_contact_author_email       Neil.Burford@dal.ca
_publ_contact_author_fax         902-494-1310
_publ_contact_author_name        'Neil Burford'
_publ_contact_author_phone       902-494-1390
_publ_section_title
;
 Synthesis and Structures of Complexes Demonstrating the Coordinative
 Versatility of the 2,4-Diimino-3-phosphinopentene Anion
 (\g-Phosphino-\b-diketiminate)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              734
_journal_page_last               738
_journal_paper_doi               10.1021/ic0351444
_journal_volume                  43
_journal_year                    2004
_chemical_formula_moiety         'C41 H50 Al Cl2 N2 P'
_chemical_formula_sum            'C41 H50 Al Cl2 N2 P'
_chemical_formula_weight         699.68
_chemical_melting_point          450
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      61
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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            8
_cell_length_a                   18.3867(11)
_cell_length_b                   20.2465(12)
_cell_length_c                   21.2320(13)
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      25.914
_cell_measurement_theta_min      2.215
_cell_volume                     7904.0(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1194
_diffrn_reflns_av_sigmaI/netI    0.0739
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            48531
_diffrn_reflns_theta_full        26.49
_diffrn_reflns_theta_max         26.49
_diffrn_reflns_theta_min         1.78
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.257
_exptl_absorpt_correction_T_max  0.9674
_exptl_absorpt_correction_T_min  0.9223
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.176
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             2976
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.476
_refine_diff_density_min         -0.474
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     424
_refine_ls_number_reflns         8131
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.1092
_refine_ls_R_factor_gt           0.0564
_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^)+(0.0531P)^2^+4.2710P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1175
_refine_ls_wR_factor_ref         0.1380
_reflns_number_gt                5024
_reflns_number_total             8131
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0351444si20031001_094042.cif
_cod_data_source_block           dal0386
_cod_database_code               4310467