Synthesis of azadiphosphiridine complexes. Theoretical studies on ring formation, the P-to-P' metal shift and the resulting nitrogen geometry.
Schmer, Alexander; García Alcaraz, Antonio; Kyri, Andreas Wolfgang; Schnakenburg, Gregor; Espinosa Ferao, Arturo; Streubel, Rainer; Dalton transactions (Cambridge, England : 2003) 51 (2022) 3275–3279; doi:10.1039/d1dt04252a

data_7709415
_publ_section_title
;
 Synthesis of azadiphosphiridine complexes. Theoretical studies on ring
 formation, the P-to-P' metal shift and the resulting nitrogen geometry.
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3275
_journal_page_last               3279
_journal_paper_doi               10.1039/d1dt04252a
_journal_volume                  51
_journal_year                    2022
_chemical_formula_moiety         'C33 H36 N2 O5 P2 W'
_chemical_formula_sum            'C33 H36 N2 O5 P2 W'
_chemical_formula_weight         786.43
_chemical_name_systematic        AS-241
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-03-20
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_audit_update_record
;
2021-06-23 deposited with the CCDC.	2022-02-03 downloaded from the CCDC.
;
_cell_angle_alpha                100.746(4)
_cell_angle_beta                 90.409(3)
_cell_angle_gamma                97.893(4)
_cell_formula_units_Z            4
_cell_length_a                   10.5675(6)
_cell_length_b                   16.9702(11)
_cell_length_c                   18.6599(10)
_cell_measurement_reflns_used    9895
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.94
_cell_measurement_theta_min      2.27
_cell_volume                     3254.7(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker X8-KappaApexII'
_diffrn_measurement_method       'fine slicing \w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0979
_diffrn_reflns_av_unetI/netI     0.0590
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            139084
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.999
_diffrn_reflns_theta_min         1.810
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.690
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6152
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1036 before and 0.0743 after correction. The Ratio of minimum to maximum transmission is 0.8246. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.605
_exptl_crystal_description       plate
_exptl_crystal_F_000             1568
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.312
_refine_diff_density_min         -1.521
_refine_diff_density_rms         0.140
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     787
_refine_ls_number_reflns         15651
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0584
_refine_ls_R_factor_gt           0.0352
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0207P)^2^+4.7752P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0668
_refine_ls_wR_factor_ref         0.0749
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11791
_reflns_number_total             15651
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt04252a2.cif
_cod_data_source_block           5575f
_cod_depositor_comments
'Adding full bibliography for 7709415--7709416.cif.'
_cod_database_code               7709415
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.866
_shelx_estimated_absorpt_t_min   0.732
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C20(H20), C23(H23), C26(H26), C20'(H20'), C23'(H23'), C26'(H26')
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C9(H9), C10(H10), C11(H11), C12(H12),
 C13(H13), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C3'(H3'), C4'(H4'),
  C5'(H5'), C6'(H6'), C7'(H7'), C9'(H9'), C10'(H10'), C11'(H11'), C12'(H12'),
 C13'(H13'), C15'(H15'), C16'(H16'), C17'(H17'), C18'(H18'), C19'(H19')
2.c Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C24(H24A,H24B,H24C), C25(H25A,H25B,
 H25C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C21'(H21D,H21E,H21F),
 C22'(H22D,H22E,H22F), C24'(H24D,H24E,H24F), C25'(H25D,H25E,H25F), C27'(H27D,
 H27E,H27F), C28'(H28D,H28E,H28F)
;
_shelx_res_checksum              98050
_shelx_hkl_checksum              53001
_olex2_submission_special_instructions 'No special instructions were received'