Stereospecific isomerisation of P-heterocycles triggered by coordination: synthesis of the first P,N-chelates featuring a 2-phospholene moiety
Leca, François; Sauthier, Mathieu; Le Guennic, Boris; Lescop, Christophe; Toupet, Loic; Halet, Jean-François; Réau, Régis; Chemical Communications (Cambridge, United Kingdom)  (2003) 1774–1775; doi:10.1039/b304308h

data_7103771
_publ_section_title
;
 Stereospecific isomerisation of P-heterocycles triggered by coordination:
 synthesis of the first P,N-chelates featuring a 2-phospholene moiety
;
_journal_coden_ASTM              CHCOFS
_journal_name_full
;
 Chemical Communications (Cambridge, United Kingdom)
;
_journal_page_first              1774
_journal_page_last               1775
_journal_paper_doi               10.1039/b304308h
_journal_year                    2003
_chemical_formula_sum            'C25 H22 Cl2 N P Pd'
_chemical_formula_weight         544.70
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 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                 104.844(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   21.587(5)
_cell_length_b                   8.979(5)
_cell_length_c                   26.183(5)
_cell_measurement_temperature    293(2)
_cell_volume                     4906(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.864
_diffrn_measured_fraction_theta_max 0.864
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       none
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0864
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            4831
_diffrn_reflns_theta_full        27.41
_diffrn_reflns_theta_max         27.41
_diffrn_reflns_theta_min         1.95
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.051
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.475
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2192
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         5.063
_refine_diff_density_min         -1.242
_refine_diff_density_rms         0.368
_refine_ls_extinction_coef       0.0034(9)
_refine_ls_extinction_expression Fc^*^==kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.697
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         4831
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.697
_refine_ls_R_factor_all          0.1919
_refine_ls_R_factor_gt           0.1582
_refine_ls_shift/su_max          0.052
_refine_ls_shift/su_mean         0.010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w==1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P==(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4315
_refine_ls_wR_factor_ref         0.4475
_reflns_number_gt                3352
_reflns_number_total             4831
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b304308h.txt
_cod_data_source_block           compound_2b
_cod_depositor_comments
;

2018-03-14
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_sg_symbol_H-M      'I 2/a'
_cod_original_formula_sum        'C50 H44 Cl4 N2 P2 Pd2'
_cod_original_formula_units_Z    4
_cod_original_formula_weight     1089.41
_cod_database_code               7103771