Stereocontrolled C(sp3)‒P bond formation with non-activated alkyl halides and tosylates
Yang, Chu-Ting; Han, Jun; Liu, Jun; Li, Yi; Zhang, Fan; Gu, Mei; Hu, Sheng; Wang, Xiaolin; RSC Adv. 7 (2017) 24652–; doi:10.1039/C7RA02766D

data_7228249
_publ_section_title
;
 Stereocontrolled C(sp3)--P bond formation with non-activated alkyl
 halides and tosylates
;
_journal_issue                   40
_journal_name_full               'RSC Adv.'
_journal_page_first              24652
_journal_paper_doi               10.1039/C7RA02766D
_journal_volume                  7
_journal_year                    2017
_chemical_formula_sum            'C21 H27 N O3 P'
_chemical_formula_weight         372.40
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-02-11 deposited with the CCDC.
2017-04-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.437(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.7343(12)
_cell_length_b                   8.4099(12)
_cell_length_c                   14.2737(19)
_cell_measurement_reflns_used    21110
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      27.542
_cell_measurement_theta_min      2.843
_cell_volume                     1005.6(2)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  Bruker
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0291
_diffrn_reflns_av_unetI/netI     0.0246
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            21110
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.542
_diffrn_reflns_theta_min         2.843
_exptl_absorpt_coefficient_mu    0.156
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs,bruker
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.230
_exptl_crystal_description       block
_exptl_crystal_F_000             398
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   0.995
_exptl_transmission_factor_min   0.991
_refine_diff_density_max         0.635
_refine_diff_density_min         -0.814
_refine_diff_density_rms         0.206
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   -0.03(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.983
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     236
_refine_ls_number_reflns         4604
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.983
_refine_ls_R_factor_all          0.0402
_refine_ls_R_factor_gt           0.0312
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0940P)^2^+0.1579P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0943
_refine_ls_wR_factor_ref         0.1159
_reflns_Friedel_coverage         0.875
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                4398
_reflns_number_total             4604
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ra02766d2.cif
_cod_data_source_block           Yct_1
_cod_database_code               7228249
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              43874