Mn(OAc)3-mediated phosphonation-lactonization of alkenoic acids: synthesis of phosphono-gamma-butyrolactones
Yuzhen Gao; Xueqin Li; Jian Xu; Yile Wu; Weizhu Chen; Guo Tang; Yufen Zhao; Chem.Commun. 51 (2015) 1605–; doi:10.1039/C4cc07978G

data_7116415
_publ_section_title
;
 Mn(OAc)3-mediated phosphonation-lactonization of alkenoic acids:
 synthesis of phosphono-gamma-butyrolactones
;
_journal_name_full               Chem.Commun.
_journal_page_first              1605
_journal_paper_doi               10.1039/C4cc07978G
_journal_volume                  51
_journal_year                    2015
_chemical_formula_sum            'C26 H27 O3 P'
_chemical_formula_weight         418.45
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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
;
2014-10-06 deposited with the CCDC.
2014-12-08 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 107.621(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.332(4)
_cell_length_b                   6.1364(12)
_cell_length_c                   20.639(4)
_cell_measurement_reflns_used    5245
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      28.18
_cell_measurement_theta_min      2.33
_cell_volume                     2212.8(8)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0414
_diffrn_reflns_av_sigmaI/netI    0.0430
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            15575
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.17
_exptl_absorpt_coefficient_mu    0.149
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.256
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       stick
_exptl_crystal_F_000             888
_refine_diff_density_max         0.437
_refine_diff_density_min         -0.222
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     274
_refine_ls_number_reflns         4318
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0643
_refine_ls_R_factor_gt           0.0542
_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^)+(0.0945P)^2^+0.3118P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1459
_refine_ls_wR_factor_ref         0.1530
_reflns_number_gt                3598
_reflns_number_total             4318
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4cc07978g2.cif
_cod_data_source_block           3
_cod_original_cell_volume        2212.7(8)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7116415