Synthesis, Crystal Structure and Hydrolysis of Novel Isomeric Cage (P–C/P–O)-Phosphoranes on the basis of 4,4,5,5-Tetramethyl-2-(2-oxo-1,2-diphenylethoxy)-1,3,2-dioxaphospholane and Hexafluoroacetone
Khasiyatullina, Nadezhda; Mironov, Vladimir Fedorovich; Krivolapov, Dmitry; Mironova, Ekaterina V.; Gnezdilov, Oleg I.; RSC Adv.  (2016) –; doi:10.1039/C6RA17983E

data_7226367
_publ_section_title
;
 Synthesis, Crystal Structure and Hydrolysis of Novel Isomeric Cage
 (P--C/P--O)-Phosphoranes on the basis of
 4,4,5,5-Tetramethyl-2-(2-oxo-1,2-diphenylethoxy)-1,3,2-dioxaphospholane
 and Hexafluoroacetone
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C6RA17983E
_journal_year                    2016
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C23 H23 F6 O5 P'
_chemical_formula_sum            'C23 H23 F6 O5 P'
_chemical_formula_weight         524.38
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2016-04-18 deposited with the CCDC.
2016-08-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.517(8)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.485(6)
_cell_length_b                   11.002(7)
_cell_length_c                   12.115(8)
_cell_measurement_reflns_used    3685
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      21.80
_cell_measurement_theta_min      2.50
_cell_volume                     1238.8(14)
_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      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0709
_diffrn_reflns_av_unetI/netI     0.0825
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_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            12827
_diffrn_reflns_point_group_measured_fraction_full 0.939
_diffrn_reflns_point_group_measured_fraction_max 0.933
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         1.715
_exptl_absorpt_coefficient_mu    0.187
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.4139
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.406
_exptl_crystal_description       prism
_exptl_crystal_F_000             540
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.336
_refine_diff_density_min         -0.479
_refine_diff_density_rms         0.111
_refine_ls_abs_structure_details
;
 Flack x determined using 1038 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.0(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     320
_refine_ls_number_reflns         4529
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.1100
_refine_ls_R_factor_gt           0.0667
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.1250P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1629
_refine_ls_wR_factor_ref         0.2021
_reflns_Friedel_coverage         0.770
_reflns_Friedel_fraction_full    0.872
_reflns_Friedel_fraction_max     0.859
_reflns_number_gt                2921
_reflns_number_total             4529
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ra17983e2.cif
_cod_data_source_block           k51_fin
_cod_database_code               7226367
_shelx_estimated_absorpt_t_min   0.946
_shelx_estimated_absorpt_t_max   0.963
_shelxl_version_number           2013-2
_shelx_res_checksum              81536