Reagent for Introducing Base-Stabilized Phosphorus Atoms into Organic and Inorganic Compounds.
Kundu, Subrata; Sinhababu, Soumen; Luebben, Anna V.; Mondal, Totan; Koley, Debasis; Dittrich, Birger; Roesky, Herbert W.; Journal of the American Chemical Society  (2017) –; doi:10.1021/jacs.7b11977

data_4126947
_publ_section_title
;
 Reagent for Introducing Base-Stabilized Phosphorus Atoms into Organic and
 Inorganic Compounds.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b11977
_journal_year                    2017
_chemical_formula_sum            'C56 H94 Li2 N2 O4 P2'
_chemical_formula_weight         935.15
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2017/1
_cell_angle_alpha                77.4360(10)
_cell_angle_beta                 80.4960(10)
_cell_angle_gamma                88.6590(10)
_cell_formula_units_Z            2
_cell_length_a                   9.4012(3)
_cell_length_b                   11.6829(4)
_cell_length_c                   26.3727(8)
_cell_measurement_reflns_used    141064
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.131
_cell_measurement_theta_min      0.802
_cell_volume                     2788.19(16)
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Smart APEX II Quazar'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0364
_diffrn_reflns_av_unetI/netI     0.0230
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            141064
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.131
_diffrn_reflns_theta_min         0.802
_diffrn_source                   'Rotating Anode'
_exptl_absorpt_coefficient_mu    0.122
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.6901
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2015/1
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.114
_exptl_crystal_description       bar
_exptl_crystal_F_000             1024
_exptl_crystal_size_max          .3
_exptl_crystal_size_mid          .24
_exptl_crystal_size_min          .15
_refine_diff_density_max         0.585
_refine_diff_density_min         -0.278
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     843
_refine_ls_number_reflns         14992
_refine_ls_number_restraints     1379
_refine_ls_restrained_S_all      0.993
_refine_ls_R_factor_all          0.0554
_refine_ls_R_factor_gt           0.0413
_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^)+(0.0562P)^2^+1.0419P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1054
_refine_ls_wR_factor_ref         0.1147
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12068
_reflns_number_total             14992
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b11977_si_002.cif
_cod_data_source_block           subrata_251
_cod_original_cell_volume        2788.20(16)
_cod_database_code               4126947
_shelx_shelxl_version_number     2017/1
_shelx_res_checksum              8888
_shelx_hkl_checksum              42363