Formation of phosphanoxy-substituted phosphaalkenes via sterically promoted cleavage of the P[double bond, length as m-dash]P diphosphene bond
Shigekazu Ito; Shunsuke Okabe; Yasuhiro Ueta; Koichi Mikami; Chem.Commun. 50 (2014) 9204–; doi:10.1039/C4cc03274H

data_7115441
_publ_section_title
;
 Formation of phosphanoxy-substituted phosphaalkenes via sterically
 promoted cleavage of the P[double bond, length as m-dash]P diphosphene
 bond
;
_journal_name_full               Chem.Commun.
_journal_page_first              9204
_journal_paper_doi               10.1039/C4cc03274H
_journal_volume                  50
_journal_year                    2014
_chemical_formula_sum            'C47 H72 O P2'
_chemical_formula_weight         714.99
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 111.4075(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.1477(6)
_cell_length_b                   18.6492(7)
_cell_length_c                   16.6712(7)
_cell_measurement_temperature    123(2)
_cell_volume                     4384.6(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0549
_diffrn_reflns_av_sigmaI/netI    0.0500
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            41578
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.09
_exptl_absorpt_coefficient_mu    0.131
_exptl_absorpt_correction_T_max  0.9793
_exptl_absorpt_correction_T_min  0.9667
_exptl_crystal_density_diffrn    1.083
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1568
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.296
_refine_diff_density_min         -0.286
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.937
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     739
_refine_ls_number_reflns         10032
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.937
_refine_ls_R_factor_all          0.0544
_refine_ls_R_factor_gt           0.0394
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1164
_refine_ls_wR_factor_ref         0.1311
_reflns_number_gt                7957
_reflns_number_total             10032
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4cc03274h2.cif
_cod_data_source_block           okabe01
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7115441