P-Cl bond-induced lactamization of 2(2'-hydroxyl)phenyloxazoline to form a cyclic phosphinite, 3-(2-chloroethyl)-2-phenyl-2H-benzo[e][1,3,2]oxaza-phosphinin-4(3H)-one: synthesis, structural studies and transition metal complexes.
Chaubey, Bimba; Mobin, Shaikh M.; Balakrishna, Maravanji S.; Dalton transactions (Cambridge, England : 2003) 43 (2014) 584–591; doi:10.1039/c3dt52223g

data_7028264
_publ_section_title
;
 P-Cl bond-induced lactamization of 2(2'-hydroxyl)phenyloxazoline to form
 a cyclic phosphinite,
 3-(2-chloroethyl)-2-phenyl-2H-benzo[e][1,3,2]oxaza-phosphinin-4(3H)-one:
 synthesis, structural studies and transition metal complexes.
;
_journal_issue                   2
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              584
_journal_page_last               591
_journal_paper_doi               10.1039/c3dt52223g
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety         'C30 H26 Cl4 N2 O4 P2 Pd'
_chemical_formula_sum            'C30 H26 Cl4 N2 O4 P2 Pd'
_chemical_formula_weight         788.67
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 114.2900(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.875(8)
_cell_length_b                   12.995(6)
_cell_length_c                   17.358(8)
_cell_measurement_reflns_used    2453
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.30
_cell_measurement_theta_min      3.00
_cell_volume                     3058(3)
_computing_cell_refinement       'CrystalClear-SM Expert 2.1 b23'
_computing_data_collection
'CrystalClear-SM Expert 2.1 b23 (Rigaku, 2012)'
_computing_data_reduction        'CrystalClear-SM Expert 2.1 b23'
_computing_molecular_graphics    'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_publication_material  'CrystalStructure 4.0'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 7.111
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Rigaku Saturn724'
_diffrn_measurement_method       \w
_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  0.1396
_diffrn_reflns_av_sigmaI/netI    0.0802
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            11351
_diffrn_reflns_theta_full        25.34
_diffrn_reflns_theta_max         25.34
_diffrn_reflns_theta_min         3.05
_diffrn_standards_interval_count -
_exptl_absorpt_coefficient_mu    1.102
_exptl_absorpt_correction_T_max  0.811
_exptl_absorpt_correction_T_min  0.660
_exptl_absorpt_process_details   'NUMABS (Rigaku, 1999)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.713
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1584
_exptl_crystal_size_max          0.420
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.190
_refine_diff_density_max         1.062
_refine_diff_density_min         -1.256
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     195
_refine_ls_number_reflns         2765
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0429
_refine_ls_R_factor_gt           0.0397
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0423P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0905
_refine_ls_wR_factor_ref         0.0927
_reflns_number_gt                2343
_reflns_number_total             2765
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt52223g.txt
_cod_data_source_block           bc02b
_cod_database_code               7028264