Donor-rich and acceptor-rich pyridine-phosphadiazonium adducts: Diversifying the Lewis acceptor chemistry of phosphorus(iii)
Burford, Neil; Spinney, Heather A.; Ferguson, Michael J.; McDonald, Robert; Chemical Communications  (2004) 2696–2697; doi:10.1039/b412267d

data_7111479
_publ_section_title
;
 Donor-rich and acceptor-rich pyridine-phosphadiazonium adducts:
 Diversifying the Lewis acceptor chemistry of phosphorus(iii)
;
_journal_issue                   23
_journal_name_full               'Chemical Communications'
_journal_page_first              2696
_journal_page_last               2697
_journal_paper_doi               10.1039/b412267d
_journal_year                    2004
_chemical_formula_moiety         'C46 H66 N4 P2, 2(C F3 O3 S), 1.5(C H2 Cl2)'
_chemical_formula_sum            'C49.5 H69 Cl3 F6 N4 O6 P2 S2'
_chemical_formula_weight         1162.50
_chemical_name_systematic
;
?
;
_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-97
_cell_angle_alpha                110.8114(7)
_cell_angle_beta                 91.4223(7)
_cell_angle_gamma                90.1012(7)
_cell_formula_units_Z            2
_cell_length_a                   10.1616(4)
_cell_length_b                   16.9451(6)
_cell_length_c                   18.9324(7)
_cell_measurement_reflns_used    6137
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      26.369
_cell_measurement_theta_min      2.339
_cell_volume                     3046.1(2)
_computing_cell_refinement       'Bruker SAINT (Bruker, 1997)'
_computing_data_collection       'Bruker SMART (Bruker, 1997)'
_computing_data_reduction        'Bruker SAINT (Bruker, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL (Bruker, 1997)'
_computing_publication_material  'Bruker SHELXTL (Bruker, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'DIRDIF-96 (Beurskens et al., 1996)'
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type
'Bruker PLATFORM diffractometer/SMART 1000 CCD area detector'
_diffrn_measurement_method       '\w scans'
_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  0.0123
_diffrn_reflns_av_sigmaI/netI    0.0226
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            14079
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.00
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.336
_exptl_absorpt_correction_T_max  0.8830
_exptl_absorpt_correction_T_min  0.8343
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'Bruker SHELXTL (Bruker, 1997)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.267
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1218
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.46
_exptl_crystal_size_min          0.38
_refine_diff_density_max         1.338
_refine_diff_density_min         -0.846
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     635
_refine_ls_number_reflns         10613
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0544
_refine_ls_R_factor_gt           0.0489
_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^)+(0.0779P)^2^+2.2060P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1364
_refine_ls_wR_factor_ref         0.1406
_reflns_number_gt                9229
_reflns_number_total             10613
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b412267dsup1.cif
_cod_data_source_block           '[(Mes*NP)2(4,4'-BIPY)][OTf]2'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_formula_sum        'C49.50 H69 Cl3 F6 N4 O6 P2 S2'
_cod_database_code               7111479