Stereospecific Preparations of P-Stereogenic Phosphonothioates and Phosphonoselenoates.
Wang, Wei-Min; Liu, Li-Juan; Yao, Lan; Meng, Fan-Jie; Sun, Yong-Ming; Zhao, Chang-Qiu; Xu, Qing; Han, Li-Biao; The Journal of organic chemistry 81 (2016) 6843–6847; doi:10.1021/acs.joc.6b01192

data_4036996
_publ_section_title
;
 Stereospecific Preparations of P-Stereogenic Phosphonothioates and
 Phosphonoselenoates.
;
_journal_issue                   15
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              6843
_journal_page_last               6847
_journal_paper_doi               10.1021/acs.joc.6b01192
_journal_volume                  81
_journal_year                    2016
_chemical_absolute_configuration r
_chemical_formula_sum            'C17 H27 O2 P S'
_chemical_formula_weight         326.42
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21 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                 102.457(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.517(5)
_cell_length_b                   6.258(3)
_cell_length_c                   18.063(9)
_cell_measurement_reflns_used    1594
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      21.984
_cell_measurement_theta_min      2.982
_cell_volume                     940.1(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0248
_diffrn_reflns_av_sigmaI/netI    0.0550
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            4760
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.31
_exptl_absorpt_coefficient_mu    0.259
_exptl_absorpt_correction_T_max  0.9286
_exptl_absorpt_correction_T_min  0.9033
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.153
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             352
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.29
_refine_diff_density_max         0.314
_refine_diff_density_min         -0.220
_refine_diff_density_rms         0.046
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.11(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     194
_refine_ls_number_reflns         3157
_refine_ls_number_restraints     457
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0774
_refine_ls_R_factor_gt           0.0536
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0443P)^2^+0.4292P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1095
_refine_ls_wR_factor_ref         0.1229
_reflns_number_gt                2329
_reflns_number_total             3157
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo6b01192_si_002.cif
_cod_data_source_block           090705f
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Monoclinic' was changed to
'monoclinic' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        940.0(9)
_cod_original_sg_symbol_H-M      'P2(1)   '
_cod_database_code               4036996