Serendipitous Discovery of a Phosphirene–Phosphindole Rearrangement
Panichakul, Duanghathai; Mathey, François; Organometallics 30 (2011) 348–351; doi:10.1021/om100990r

data_4063420
_publ_section_title
;
 Serendipitous Discovery of a Phosphirene--Phosphindole Rearrangement
;
_journal_issue                   2
_journal_name_full               Organometallics
_journal_page_first              348
_journal_page_last               351
_journal_paper_doi               10.1021/om100990r
_journal_volume                  30
_journal_year                    2011
_chemical_formula_moiety         'C37 H20 B F15 N O6 P W, 0.5(C H Cl3)'
_chemical_formula_sum            'C37.5 H20.5 B Cl1.5 F15 N O6 P W'
_chemical_formula_weight         1144.85
_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                77.600(2)
_cell_angle_beta                 78.274(2)
_cell_angle_gamma                72.811(2)
_cell_formula_units_Z            2
_cell_length_a                   11.2518(5)
_cell_length_b                   11.4277(5)
_cell_length_c                   16.4537(8)
_cell_measurement_reflns_used    9087
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      37.46
_cell_measurement_theta_min      2.31
_cell_volume                     1951.73(16)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      103(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \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  0.0412
_diffrn_reflns_av_sigmaI/netI    0.0552
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            55516
_diffrn_reflns_theta_full        37.69
_diffrn_reflns_theta_max         37.69
_diffrn_reflns_theta_min         1.89
_exptl_absorpt_coefficient_mu    3.224
_exptl_absorpt_correction_T_max  0.8819
_exptl_absorpt_correction_T_min  0.4655
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.948
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1110
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.912
_refine_diff_density_min         -1.736
_refine_diff_density_rms         0.215
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     599
_refine_ls_number_reflns         20390
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0488
_refine_ls_R_factor_gt           0.0357
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0460P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0799
_refine_ls_wR_factor_ref         0.0935
_reflns_number_gt                17126
_reflns_number_total             20390
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100990r_si_001.cif
_cod_data_source_block           mat57
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1673 2011-04-08 12:14:43Z adriana 
;
_cod_original_cell_volume        1951.73(15)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C37.50 H20.50 B Cl1.50 F15 N O6 P W'
_cod_database_code               4063420