Air and water stable secondary phosphine oxides as diazaphospholene precatalysts.
Lundrigan, Travis; Tien, Chieh-Hung; Robertson, Katherine N.; Speed, Alexander W. H.; Chemical communications (Cambridge, England) 56 (2020) 8027–8030; doi:10.1039/d0cc01072c

data_7126146
_publ_section_title
;
 Air and water stable secondary phosphine oxides as diazaphospholene
 precatalysts.
;
_journal_issue                   58
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              8027
_journal_page_last               8030
_journal_paper_doi               10.1039/d0cc01072c
_journal_volume                  56
_journal_year                    2020
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C26 H25 N2 O P, 0.5(C4 H8 O2)'
_chemical_formula_sum            'C28 H29 N2 O2 P'
_chemical_formula_weight         456.50
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     'dual space'
_audit_creation_method           SHELXL-2018/1
_audit_update_record
;
2020-02-05 deposited with the CCDC.	2020-03-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.1724(2)
_cell_length_b                   11.6412(3)
_cell_length_c                   22.2670(6)
_cell_measurement_reflns_used    9518
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      79.3355
_cell_measurement_theta_min      3.7971
_cell_volume                     2377.62(10)
_computing_cell_refinement       'SAINT V8.40A (Bruker Nano, Inc., 2019)'
_computing_data_collection       'Bruker Instrument Service vV6.2.12'
_computing_data_reduction        'SAINT V8.40A (Bruker Nano, Inc., 2019)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT-2014 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 '100 \\times 140 mm^2^ CMOS sensor'
_diffrn_detector_area_resol_mean 7.41
_diffrn_detector_type            'Bruker PHOTON III'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       '\k--geometry diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_radiation_monochromator  'multilayer mirror'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0294
_diffrn_reflns_av_unetI/netI     0.0186
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            50273
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         79.580
_diffrn_reflns_theta_min         3.970
_diffrn_source_type              'Incoatec I\mS 3.0'
_exptl_absorpt_coefficient_mu    1.240
_exptl_absorpt_correction_T_max  0.7543
_exptl_absorpt_correction_T_min  0.6726
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.275
_exptl_crystal_description       pyramidal
_exptl_crystal_F_000             968
_exptl_crystal_size_max          0.219
_exptl_crystal_size_mid          0.207
_exptl_crystal_size_min          0.104
_refine_diff_density_max         0.209
_refine_diff_density_min         -0.268
_refine_diff_density_rms         0.051
_refine_ls_abs_structure_details
;
 Flack x determined using 2136 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.060(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.158
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     333
_refine_ls_number_reflns         5094
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.158
_refine_ls_R_factor_all          0.0367
_refine_ls_R_factor_gt           0.0365
_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^)+(0.0249P)^2^+1.8200P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0955
_refine_ls_wR_factor_ref         0.0955
_reflns_Friedel_coverage         0.749
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.977
_reflns_number_gt                5069
_reflns_number_total             5094
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc01072c2.cif
_cod_data_source_block           AS021B_Cu
_cod_depositor_comments          'Adding full bibliography for 7126146.cif.'
_cod_database_code               7126146
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_min   0.773
_shelx_estimated_absorpt_t_max   0.882
_diffrn_source_source            'microfocus sealed tube'
_shelx_res_checksum              57128