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_1550622
_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            'C36 H21 F20 O3 P'
_chemical_formula_weight         912.50
_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
_audit_update_record
;
2018-07-19 deposited with the CCDC.    2019-02-18 downloaded from the CCDC.
;
_cell_angle_alpha                88.6960(10)
_cell_angle_beta                 79.3540(10)
_cell_angle_gamma                62.5700(10)
_cell_formula_units_Z            2
_cell_length_a                   9.9730(2)
_cell_length_b                   10.4830(2)
_cell_length_c                   19.3940(5)
_cell_measurement_reflns_used    8569
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      22.63
_cell_measurement_theta_min      2.35
_cell_volume                     1764.13(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.907
_diffrn_measured_fraction_theta_max 0.907
_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    0.0224
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            7683
_diffrn_reflns_theta_full        27.95
_diffrn_reflns_theta_max         27.95
_diffrn_reflns_theta_min         1.07
_exptl_absorpt_coefficient_mu    0.223
_exptl_absorpt_correction_T_max  0.9568
_exptl_absorpt_correction_T_min  0.9362
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.718
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         2.415
_refine_diff_density_min         -1.198
_refine_diff_density_rms         0.311
_refine_ls_extinction_coef       0.108(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     543
_refine_ls_number_reflns         7683
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.1066
_refine_ls_R_factor_gt           0.0935
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1641P)^2^+5.3163P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2444
_refine_ls_wR_factor_ref         0.2661
_reflns_number_gt                6884
_reflns_number_total             7683
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c8sc05158e2.cif
_cod_data_source_block           ex641
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1550622