Novel approach to benzo-fused 1,2-azaphospholene involving a Pd(II)-assisted tandem P-C bond cleavage and P-N bond formation reaction.
Kunchur, Harish S.; Radhakrishna, Latchupatula; Pandey, Madhusudan K.; Balakrishna, Maravanji S.; Chemical communications (Cambridge, England) 57 (2021) 4835–4838; doi:10.1039/d1cc01591e

data_7128126
_publ_section_title
;
 Novel approach to benzo-fused 1,2-azaphospholene involving a
 Pd(II)-assisted tandem P-C bond cleavage and P-N bond formation reaction.
;
_journal_issue                   39
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              4835
_journal_page_last               4838
_journal_paper_doi               10.1039/d1cc01591e
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety
'C62 H46 Cl2 N2 O2 P4 Pd2, 2(F6 Sb), 4(C6 H6)'
_chemical_formula_sum            'C86 H70 Cl2 F12 N2 O2 P4 Pd2 Sb2'
_chemical_formula_weight         2042.52
_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
_audit_creation_date             2020-10-22
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-02-15 deposited with the CCDC.	2021-04-05 downloaded from the CCDC.
;
_cell_angle_alpha                63.884(2)
_cell_angle_beta                 64.063(3)
_cell_angle_gamma                63.623(3)
_cell_formula_units_Z            1
_cell_length_a                   12.7967(4)
_cell_length_b                   14.2667(4)
_cell_length_c                   14.5382(4)
_cell_measurement_reflns_used    22352
_cell_measurement_temperature    150
_cell_measurement_theta_max      30.9040
_cell_measurement_theta_min      2.0730
_cell_volume                     2036.34(12)
_computing_cell_refinement
'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_computing_data_reduction
'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.0
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -110.00  70.00   0.50   10.00    --  -20.00   0.00 108.00  360
  2  \w    -74.50  19.00   0.50   10.00    --  -20.00 -72.00 -36.00  187
  3  \w    -60.00 -30.00   0.50   10.00    --  -20.00 -72.00 108.00   60
  4  \w    -70.00  70.00   0.50   10.00    --  -20.00   0.00  36.00  280
  5  \w    -59.00  15.50   0.50   10.00    --  -20.00  72.00  36.00  149
  6  \w    -59.00 -25.50   0.50   10.00    --  -20.00  72.00 -36.00   67
  7  \w    -41.00 -10.50   0.50   10.00    --  -20.00 -72.00  36.00   61
  8  \w   -110.00 -54.00   0.50   10.00    --  -20.00   0.00-180.00  112
  9  \w   -110.00  70.00   0.50   10.00    --  -20.00   0.00 108.00  360
 10  \w    -74.50  19.00   0.50   10.00    --  -20.00 -72.00 -36.00  187
 11  \w    -60.00 -30.00   0.50   10.00    --  -20.00 -72.00 108.00   60
 12  \w    -70.00 -50.00   0.50   10.00    --  -20.00   0.00  36.00   40
;
_diffrn_measurement_device       'AFC12 (Right): Kappa 3 circle'
_diffrn_measurement_device_type  'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0562
_diffrn_reflns_av_unetI/netI     0.0346
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            37404
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.951
_exptl_absorpt_coefficient_mu    1.312
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83731
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.666
_exptl_crystal_description       block
_exptl_crystal_F_000             1012
_exptl_crystal_size_max          0.165
_exptl_crystal_size_mid          0.108
_exptl_crystal_size_min          0.091
_refine_diff_density_max         1.810
_refine_diff_density_min         -1.684
_refine_diff_density_rms         0.151
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     532
_refine_ls_number_reflns         6991
_refine_ls_number_restraints     82
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0627
_refine_ls_R_factor_gt           0.0555
_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^)+(0.0717P)^2^+8.7241P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1422
_refine_ls_wR_factor_ref         0.1494
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6178
_reflns_number_total             6991
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc01591e2.cif
_cod_data_source_block           compound-6
_cod_depositor_comments
'Adding full bibliography for 7128125--7128128.cif.'
_cod_original_cell_volume        2036.34(13)
_cod_database_code               7128126
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.890
_shelx_estimated_absorpt_t_min   0.813
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C28-C29 \\sim C28-C29A
 with sigma of 0.02
 C26-C31 \\sim C26-C31A
 with sigma of 0.02
 C31-C30 \\sim C31A-C30A
 with sigma of 0.02
 C29-C30 \\sim C29A-C30A
 with sigma of 0.02
 C28-C30 \\sim C28-C30A
 with sigma of 0.04
 C26-C30 \\sim C26-C30A
 with sigma of 0.04
 C31-C29 \\sim C31A-C29A
 with sigma of 0.04
3. Restrained planarity
 C42, C41, C40, C39, C38, C43
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(C41) \\sim Ueq, Uanis(C40) \\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(C38)
\\sim Ueq, Uanis(C43) \\sim Ueq, Uanis(C42) \\sim Ueq: with sigma of 0.001 and
sigma for terminal atoms of 0.002
Uanis(C29A) \\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(C30) \\sim Ueq, Uanis(C30A)
\\sim Ueq, Uanis(C31A) \\sim Ueq, Uanis(C31) \\sim Ueq: with sigma of 0.001 and
sigma for terminal atoms of 0.002
5. Others
 Fixed Sof: H28(0.7) H28A(0.3) C31(0.7) H31(0.7) C29(0.7) H29(0.7) C30(0.7)
 H30(0.7) C31A(0.3) H31A(0.3) C30A(0.3) H30A(0.3) C29A(0.3) H29A(0.3)
6.a Aromatic/amide H refined with riding coordinates:
 C28(H28), C28(H28A), C18(H18), C21(H21), C27(H27), C4(H4), C25(H25), C22(H22),
  C17(H17), C6(H6), C15(H15), C5(H5), C13(H13), C9(H9), C3(H3), C31(H31),
 C24(H24), C12(H12), C16(H16), C23(H23), C29(H29), C11(H11), C10(H10), C37(H37),
  C30(H30), C36(H36), C33(H33), C32(H32), C34(H34), C35(H35), C42(H42),
 C38(H38), C43(H43), C41(H41), C39(H39), C40(H40), C31A(H31A), C30A(H30A),
 C29A(H29A)
;
_shelx_res_checksum              60468
_shelx_hkl_checksum              70238
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;