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_7709416
_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         '2(C33 H27 N O5 P2 W), C4 H10 O'
_chemical_formula_sum            'C70 H64 N2 O11 P4 W2'
_chemical_formula_weight         1600.81
_chemical_name_systematic        AS-226
_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                86.110(4)
_cell_angle_beta                 76.077(3)
_cell_angle_gamma                72.024(4)
_cell_formula_units_Z            1
_cell_length_a                   9.2415(5)
_cell_length_b                   13.4649(8)
_cell_length_c                   14.4358(8)
_cell_measurement_reflns_used    9879
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.13
_cell_measurement_theta_min      2.38
_cell_volume                     1658.40(17)
_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  0.0574
_diffrn_reflns_av_unetI/netI     0.0402
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            50896
_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         3.181
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.623
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.4717
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1162 before and 0.0603 after correction. The Ratio of minimum to maximum transmission is 0.6322. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.603
_exptl_crystal_description       plate
_exptl_crystal_F_000             794
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.546
_refine_diff_density_min         -1.300
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     415
_refine_ls_number_reflns         7983
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0357
_refine_ls_R_factor_gt           0.0260
_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^)+(0.0203P)^2^+2.3593P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0528
_refine_ls_wR_factor_ref         0.0569
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7005
_reflns_number_total             7983
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt04252a2.cif
_cod_data_source_block           5550f
_cod_depositor_comments
'Adding full bibliography for 7709415--7709416.cif.'
_cod_original_cell_volume        1658.41(17)
_cod_database_code               7709416
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.840
_shelx_estimated_absorpt_t_min   0.503
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
2. Restrained distances
 C35-C34S = C35-C34
 1.5 with sigma of 0.02
 C35-C34S
 1.5 with sigma of 0.001
3. Others
 Sof(C34S)=Sof(H34C)=Sof(H34D)=Sof(H35D)=Sof(H35E)=Sof(H35F)=1-FVAR(1)
 Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(H35A)=Sof(H35B)=Sof(H35C)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C7(H7)
4.b Secondary CH2 refined with riding coordinates:
 C34(H34A,H34B), C34S(H34C,H34D)
4.c Me refined with riding coordinates:
 C35(H35A,H35B,H35C), C35(H35D,H35E,H35F)
4.d Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C12(H12), C13(H13), C14(H14),
 C15(H15), C16(H16), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C24(H24),
  C25(H25), C26(H26), C27(H27), C28(H28)
4.e Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C)
;
_shelx_res_checksum              46165
_shelx_hkl_checksum              61205
_olex2_submission_special_instructions 'No special instructions were received'