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_1550625
_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            'C44 H36 F20 K O5 P'
_chemical_formula_weight         1094.80
_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
_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                 111.443(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.972(4)
_cell_length_b                   13.493(3)
_cell_length_c                   19.631(4)
_cell_measurement_reflns_used    9981
_cell_measurement_temperature    173
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      2.23
_cell_volume                     4677.5(17)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Yadokari-XG 2009 (Wakita Nemoto et al., 2009)'
_computing_publication_material  'Yadokari-XG 2009 (Wakita,Nemoto et al., 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR-2004
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'Bruker Helios multilayered confocal mirror'
_diffrn_radiation_source         'Bruker TXS fine-focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0342
_diffrn_reflns_av_sigmaI/netI    0.0429
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            23825
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.28
_exptl_absorpt_coefficient_mu    0.272
_exptl_absorpt_correction_T_max  0.969
_exptl_absorpt_correction_T_min  0.680
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
 SADABS (Sheldrick, 1997)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.555
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2216
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.154
_refine_diff_density_min         -0.827
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     600
_refine_ls_number_reflns         10406
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.1152
_refine_ls_R_factor_gt           0.0927
_refine_ls_shift/su_max          0.056
_refine_ls_shift/su_mean         0.012
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1311P)^2^+15.5326P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2534
_refine_ls_wR_factor_ref         0.2786
_reflns_number_gt                7898
_reflns_number_total             10406
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c8sc05158e2.cif
_cod_data_source_block           ydkr
_cod_original_cell_volume        4677.6(17)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1550625