Trapping of Brønsted acids with a phosphorus-centered biradicaloid - synthesis of hydrogen pseudohalide addition products.
Beer, Henrik; Bläsing, Kevin; Bresien, Jonas; Chojetzki, Lukas; Schulz, Axel; Stoer, Philip; Villinger, Alexander; Dalton transactions (Cambridge, England : 2003) 49 (2020) 13655–13662; doi:10.1039/d0dt03251d

data_7705741
_publ_section_title
;
 Trapping of Br\/onsted acids with a phosphorus-centered biradicaloid -
 synthesis of hydrogen pseudohalide addition products.
;
_journal_issue                   39
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13655
_journal_page_last               13662
_journal_paper_doi               10.1039/d0dt03251d
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C49 H51 N2 O P3'
_chemical_formula_sum            'C49 H51 N2 O P3'
_chemical_formula_weight         776.82
_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'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2020-07-06 deposited with the CCDC.	2020-09-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.781(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.6722(11)
_cell_length_b                   20.9488(19)
_cell_length_c                   16.0188(15)
_cell_measurement_reflns_used    6346
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      23.72
_cell_measurement_theta_min      2.35
_cell_volume                     4092.2(6)
_computing_cell_refinement       'Bruker Apex V7.51A'
_computing_data_collection       'Bruker Apex V7.51A'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP-3v2.01 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Apex Kappa-II-CCD-diffractometer'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0944
_diffrn_reflns_av_unetI/netI     0.0627
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            69830
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.498
_diffrn_reflns_theta_min         2.668
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.185
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.6875
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.261
_exptl_crystal_description       block
_exptl_crystal_F_000             1648
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.070
_refine_diff_density_max         0.323
_refine_diff_density_min         -0.417
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     595
_refine_ls_number_reflns         10351
_refine_ls_number_restraints     229
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0960
_refine_ls_R_factor_gt           0.0529
_refine_ls_shift/su_max          0.050
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0519P)^2^+2.1520P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1134
_refine_ls_wR_factor_ref         0.1347
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6777
_reflns_number_total             10351
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03251d2.cif
_cod_data_source_block           is_kbhm22b
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7705741
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.952
_shelx_estimated_absorpt_t_max   0.987
_shelx_res_checksum              45188