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_4126946
_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_moiety         'C20 H31 Cl3 Ge N P'
_chemical_formula_sum            'C20 H31 Cl3 Ge N P'
_chemical_formula_weight         495.37
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 93.664(19)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.688(2)
_cell_length_b                   14.520(4)
_cell_length_c                   15.294(5)
_cell_measurement_reflns_used    45035
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.1
_cell_measurement_theta_min      4.818
_cell_volume                     2368.6(11)
_computing_cell_refinement       'XDS (Kabsch, 2010)'
_computing_data_collection       'XDS (Kabsch, 2010)'
_computing_molecular_graphics    'SHELXLE (Huebschle, 2011)'
_computing_publication_material  'enCIFer 1.5.1, CCDC, 2015'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Microdiffractometer at PetraIII'
_diffrn_measurement_method       '\f scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6199
_diffrn_reflns_av_R_equivalents  0.1397
_diffrn_reflns_av_unetI/netI     0.0970
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            47409
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        21.835
_diffrn_reflns_theta_max         27.113
_diffrn_reflns_theta_min         4.818
_diffrn_source                   'monochromated X-rays beamline PX11@PetraIII'
_exptl_absorpt_coefficient_mu    1.169
_exptl_absorpt_correction_T_max  0.9656
_exptl_absorpt_correction_T_min  0.8164
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS version 2016/1, multi-scan. (G. M. Sheldrick, 2016)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.389
_exptl_crystal_description       needle
_exptl_crystal_F_000             1024
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.057
_refine_diff_density_min         -0.783
_refine_diff_density_rms         0.157
_refine_ls_extinction_coef       0.066(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         7827
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0490
_refine_ls_R_factor_gt           0.0486
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0561P)^2^+0.2874P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1196
_refine_ls_wR_factor_ref         0.1203
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7622
_reflns_number_total             7827
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b11977_si_003.cif
_cod_data_source_block           skr100
_cod_original_cell_volume        2368.5(11)
_cod_database_code               4126946
_shelxl_version_number           2014/6
_shelx_res_checksum              24807
_shelx_hkl_checksum              89834