The First Isolable Pentacoordinate 1,2lambda5-Azaphosphetine: Synthesis, X-ray crystallographic Analysis, and Dynamic Behaviour
Naokazu Kano; Azusa Kikuchi; Takayuki Kawashima; Chemical Communications 20 (2001) 2096–2097; doi:10.1039/B106501G

data_7123812
_publ_section_title
;
 The First Isolable Pentacoordinate 1,2lambda5-Azaphosphetine: Synthesis,
 X-ray crystallographic Analysis, and Dynamic Behaviour
;
_journal_name_full               'Chemical Communications'
_journal_page_first              2096
_journal_page_last               2097
_journal_paper_doi               10.1039/B106501G
_journal_volume                  20
_journal_year                    2001
_chemical_formula_moiety         'C39 H37 F9 N O3 P S, 0.75(C6 H6)'
_chemical_formula_sum            'C43.5 H41.5 F9 N O3 P S'
_chemical_formula_weight         860.33
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                79.555(3)
_cell_angle_beta                 85.597(3)
_cell_angle_gamma                86.0042(10)
_cell_formula_units_Z            4
_cell_length_a                   12.246(2)
_cell_length_b                   16.830(2)
_cell_length_c                   20.7758(11)
_cell_measurement_reflns_used    8635
_cell_measurement_temperature    150.1
_cell_measurement_theta_max      13.6
_cell_measurement_theta_min      1.1
_cell_volume                     4191.7(9)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalStructure
_computing_molecular_graphics    ORTEP3
_computing_publication_material  'CrystalStructure Ver. 2.00'
_computing_structure_refinement  CRYSTALS
_computing_structure_solution    SIR92
_diffrn_detector_area_resol_mean 7.32
_diffrn_measured_fraction_theta_full 0.9637
_diffrn_measured_fraction_theta_max 0.9637
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.039
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            37809
_diffrn_reflns_theta_full        27.10
_diffrn_reflns_theta_max         27.10
_exptl_absorpt_coefficient_mu    0.195
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.363
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.36
_refine_diff_density_min         -0.30
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.477
_refine_ls_hydrogen_treatment    riding
_refine_ls_number_parameters     1137
_refine_ls_number_reflns         9247
_refine_ls_R_factor_gt           0.0410
_refine_ls_shift/su_max          0.0000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/\s^2^(Fo)'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_ref         0.0430
_reflns_number_gt                9247
_reflns_number_total             17839
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            Chem-Comm-2001-20-2096.cif
_cod_data_source_block           '_PCCN1'
_cod_depositor_comments
;
          last page corrected

2024-10-18
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_cell_volume        4191.6(7)
_cod_original_sg_symbol_H-M      'P -1       '
_cod_original_formula_moiety     'C87 H83 F18 N2 O6 P2 S2 '
_cod_original_formula_sum        'C87 H83 F18 N2 O6 P2 S2 '
_cod_original_formula_units_Z    2
_cod_original_formula_weight     1720.66
_cod_database_code               7123812