Stereoselective synthesis, structural aspects, and NMR properties of stable C-fluorinated phosphaalkenes
Shigekazu Ito; Takeshi Nakagawa; Koichi Mikami; Chem.Commun. 49 (2013) 9221–; doi:10.1039/c3cc45237a

data_7109818
_publ_section_title
;
 Stereoselective synthesis, structural aspects, and NMR properties of
 stable C-fluorinated phosphaalkenes
;
_journal_name_full               Chem.Commun.
_journal_page_first              9221
_journal_paper_doi               10.1039/c3cc45237a
_journal_volume                  49
_journal_year                    2013
_chemical_formula_sum            'C19 H29 Br F P'
_chemical_formula_weight         387.30
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 95.877(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   5.9989(4)
_cell_length_b                   12.7211(9)
_cell_length_c                   25.6766(13)
_cell_measurement_temperature    123(2)
_cell_volume                     1949.1(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0881
_diffrn_reflns_av_sigmaI/netI    0.0903
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            15220
_diffrn_reflns_theta_full        25.34
_diffrn_reflns_theta_max         25.34
_diffrn_reflns_theta_min         2.88
_exptl_absorpt_coefficient_mu    2.195
_exptl_absorpt_correction_T_max  0.7942
_exptl_absorpt_correction_T_min  0.5685
_exptl_absorpt_correction_type   numerical
_exptl_crystal_density_diffrn    1.320
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             808
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.404
_refine_diff_density_min         -0.298
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.757
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     315
_refine_ls_number_reflns         3557
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.757
_refine_ls_R_factor_all          0.0542
_refine_ls_R_factor_gt           0.0365
_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/[?^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0983
_refine_ls_wR_factor_ref         0.1124
_reflns_number_gt                2748
_reflns_number_total             3557
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cc45237a.txt
_cod_data_source_block           nakabrf
_cod_original_cell_volume        1949.2(2)
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7109818