Regioselective Sodium Cation-Assisted Synthesis of the First Bis-Transannular Cyclotriphosphazatriene Derivatives of a Chiral Ligand Type
Krystyna Brandt; Iwona Porwolik; Anna Olejnik; Robert A. Shaw; David B. Davies; Michael B. Hursthouse; Georgia D. Sykara; Journal of the American Chemical Society 118 (1996) 4496–4497; doi:10.1021/ja960201w

data_4117146
_publ_section_title
;
 Regioselective Sodium Cation-Assisted Synthesis of the First
 Bis-Transannular Cyclotriphosphazatriene Derivatives of a Chiral Ligand
 Type
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4496
_journal_page_last               4497
_journal_paper_doi               10.1021/ja960201w
_journal_volume                  118
_journal_year                    1996
_chemical_formula_sum            'C28 H28 Cl2 N3 O7 P3'
_chemical_formula_weight         682.34
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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_method           SHELXL
_cell_angle_alpha                84.64(2)
_cell_angle_beta                 79.90(2)
_cell_angle_gamma                77.981(11)
_cell_formula_units_Z            2
_cell_length_a                   11.110(4)
_cell_length_b                   11.740(2)
_cell_length_c                   11.823(2)
_cell_measurement_temperature    293(2)
_cell_volume                     1482.3(7)
_computing_cell_refinement       'REFINE (incorporated in MADNES)'
_computing_data_collection       'MADNES (Pflugrath & Messerchmidt, 1989)'
_computing_data_reduction        'ABSMAD (Karaulov, 1992)'
_computing_molecular_graphics    'SNOOPI (Davies, 1983)'
_computing_publication_material  SHELXL-93
_computing_structure_refinement  'SHELXL-92 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Delft Instruments FAST area detector'
_diffrn_measurement_method       '(Darr, Drake, Hursthouse & Malik, 1993)'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0836
_diffrn_reflns_av_sigmaI/netI    0.0842
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            6224
_diffrn_reflns_theta_max         25.10
_diffrn_reflns_theta_min         1.75
_exptl_absorpt_coefficient_mu    0.433
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.529
_exptl_crystal_description       needle-like
_exptl_crystal_F_000             704
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.756
_refine_diff_density_min         -0.476
_refine_diff_density_rms         0.124
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.056
_refine_ls_goodness_of_fit_obs   1.174
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         4102
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_restrained_S_obs      1.174
_refine_ls_R_factor_all          0.0680
_refine_ls_R_factor_obs          0.0591
_refine_ls_shift/esd_max         0.132
_refine_ls_shift/esd_mean        0.022
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0933P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1567
_refine_ls_wR_factor_obs         0.1545
_reflns_number_observed          3293
_reflns_number_total             4102
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja960201w_2.cif
_cod_data_source_block           s92-Compound5
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0933P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0933P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1482.3(6)
_cod_database_code               4117146