A new bulky iminophosphonamide as an N,N'-chelating ligand: synthesis and structural characterization of heteroleptic group 13 element complexes.
Prashanth, Billa; Singh, Sanjay; Dalton transactions (Cambridge, England : 2003) 43 (2014) 16880–16888; doi:10.1039/c4dt02637c

data_7032556
_publ_section_title
;
 A new bulky iminophosphonamide as an N,N'-chelating ligand: synthesis and
 structural characterization of heteroleptic group 13 element complexes.
;
_journal_issue                   44
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16880
_journal_page_last               16888
_journal_paper_doi               10.1039/c4dt02637c
_journal_volume                  43
_journal_year                    2014
_chemical_formula_sum            'C42 H47 Al F5 N2 P'
_chemical_formula_weight         732.77
_chemical_name_systematic
;
 ?
;
_chemical_properties_physical
'Air-sensitive, Moisture-sensitive, Hygroscopic'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-09-09T18:08:35-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                70.9320(10)
_cell_angle_beta                 73.0260(10)
_cell_angle_gamma                67.0570(10)
_cell_formula_units_Z            2
_cell_length_a                   11.95580(10)
_cell_length_b                   11.98410(10)
_cell_length_c                   16.9461(2)
_cell_measurement_reflns_used    7924
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.48
_cell_measurement_theta_min      2.479
_cell_volume                     2075.14(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0212
_diffrn_reflns_av_unetI/netI     0.0282
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            17938
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         1.29
_exptl_absorpt_coefficient_mu    0.14
_exptl_absorpt_correction_T_max  0.7473
_exptl_absorpt_correction_T_min  0.671
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
R(int) was 0.0512 before and 0.0346 after correction.
The Ratio of minimum to maximum transmission is 0.8979.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_density_diffrn    1.173
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             772
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: '
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_platon_squeeze_details
;
;
_refine_diff_density_max         1.478
_refine_diff_density_min         -0.819
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.226
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     439
_refine_ls_number_reflns         7546
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.226
_refine_ls_R_factor_all          0.0741
_refine_ls_R_factor_gt           0.0642
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0854P)^2^+2.2914P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1781
_refine_ls_wR_factor_ref         0.1855
_reflns_number_gt                6293
_reflns_number_total             7546
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt02637c2.cif
_cod_data_source_block           Compound_8_100k_0m
_cod_depositor_comments
'Adding full bibliography for 7032550--7032556.cif.'
_cod_original_cell_volume        2075.14(3)
_cod_database_code               7032556