Intramolecular arene epoxidation by phosphadioxiranes.
Zhang, Dong; Gao, Ruomei; Afzal, Shabana; Vargas, Mario; Sharma, Shantanu; McCurdy, Alison; Yousufuddin, Muhammed; Stewart, Timothy; Bau, Robert; Selke, Matthias; Organic letters 8 (2006) 5125–5128; doi:10.1021/ol0622007

data_1506272
_publ_section_title
;
 Intramolecular arene epoxidation by phosphadioxiranes.
;
_journal_issue                   22
_journal_name_full               'Organic letters'
_journal_page_first              5125
_journal_page_last               5128
_journal_paper_doi               10.1021/ol0622007
_journal_volume                  8
_journal_year                    2006
_chemical_formula_sum            'C30 H37 O3 P'
_chemical_formula_weight         476.57
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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                94.968(4)
_cell_angle_beta                 95.671(4)
_cell_angle_gamma                117.303(4)
_cell_formula_units_Z            2
_cell_length_a                   10.675(2)
_cell_length_b                   11.455(3)
_cell_length_c                   12.152(3)
_cell_measurement_temperature    153(2)
_cell_volume                     1299.3(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0485
_diffrn_reflns_av_sigmaI/netI    0.0953
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7074
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         1.70
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.135
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.218
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             512
_exptl_crystal_recrystallization_method 'ethanol solvent'
_refine_diff_density_max         0.366
_refine_diff_density_min         -0.382
_refine_diff_density_rms         0.061
_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     316
_refine_ls_number_reflns         4822
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0937
_refine_ls_R_factor_gt           0.0645
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0544P)^2^+0.7210P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1579
_refine_ls_wR_factor_ref         0.1661
_reflns_number_gt                3129
_reflns_number_total             4822
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol0622007si20060905_094925.cif
_cod_data_source_block           shphm
_cod_database_code               1506272