Synthesis and characterization of a pair of O-fac/O-mer 12-P-6 alkyloxaphosphates with a P-O-C-C four-membered ring
Jiang, Xin-Dong; Toya, Yuya; Matsukawa, Shiro; Kojima, Satoshi; Jimenez-Halla, Jose Oscar Carlos; Shang, Rong; Nakamoto, Masaaki; Yamamoto, Yohsuke; Chemical Science  (2019) –; doi:10.1039/C8SC05158E

data_1550623
_publ_section_title
;
 Synthesis and characterization of a pair of O-fac/O-mer 12-P-6
 alkyloxaphosphates with a P-O-C-C four-membered ring
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C8SC05158E
_journal_year                    2019
_chemical_formula_sum            'C37 H23 Cl2 F20 O3 P'
_chemical_formula_weight         997.42
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2018-07-19 deposited with the CCDC.    2019-02-18 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 127.505(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   39.2730(6)
_cell_length_b                   9.55300(10)
_cell_length_c                   26.3550(7)
_cell_measurement_reflns_used    8765
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      24.36
_cell_measurement_theta_min      2.21
_cell_volume                     7843.9(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.912
_diffrn_measured_fraction_theta_max 0.912
_diffrn_measurement_device_type  BRUKER
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    4.3140
_diffrn_reflns_limit_h_max       51
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            8582
_diffrn_reflns_theta_full        27.93
_diffrn_reflns_theta_max         27.93
_diffrn_reflns_theta_min         1.31
_exptl_absorpt_coefficient_mu    0.340
_exptl_absorpt_correction_T_max  0.9668
_exptl_absorpt_correction_T_min  0.8484
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.689
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3984
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.859
_refine_diff_density_min         -0.931
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     569
_refine_ls_number_reflns         8582
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.1034
_refine_ls_R_factor_gt           0.0678
_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^)+(0.1312P)^2^+11.1201P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2003
_refine_ls_wR_factor_ref         0.2239
_reflns_number_gt                6104
_reflns_number_total             8582
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c8sc05158e2.cif
_cod_data_source_block           ex624p
_cod_original_cell_volume        7843.9(3)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               1550623