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_7128125
_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         'C31 H23 Cl2 N O P2 Pd'
_chemical_formula_sum            'C31 H23 Cl2 N O P2 Pd'
_chemical_formula_weight         664.74
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.0176(5)
_cell_length_b                   11.6607(3)
_cell_length_c                   11.4688(2)
_cell_measurement_reflns_used    16934
_cell_measurement_temperature    150
_cell_measurement_theta_max      30.9130
_cell_measurement_theta_min      1.9830
_cell_volume                     2810.77(11)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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    8.00    --  -20.00   0.00-108.00  360
  2  \w    -62.00 -32.00   0.50    8.00    --  -20.00 -72.00 -36.00   60
  3  \w   -110.00 -37.50   0.50    8.00    --  -20.00   0.00 -36.00  145
  4  \w   -110.00  70.00   0.50    8.00    --  -20.00   0.00 -36.00  360
  5  \w    -28.50   2.00   0.50    8.00    --  -20.00  72.00 -36.00   61
  6  \w   -110.00-103.50   0.50    8.00    --  -20.00   0.00  36.00   13
;
_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  0.0505
_diffrn_reflns_av_unetI/netI     0.0342
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            25416
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.997
_exptl_absorpt_coefficient_mu    0.990
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71881
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (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    1.571
_exptl_crystal_description       block
_exptl_crystal_F_000             1336
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.524
_refine_diff_density_min         -0.359
_refine_diff_density_rms         0.088
_refine_ls_abs_structure_details
;
 Flack x determined using 2009 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.051(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         4891
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0312
_refine_ls_R_factor_gt           0.0292
_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^)+(0.0316P)^2^+1.3166P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0640
_refine_ls_wR_factor_ref         0.0657
_reflns_Friedel_coverage         0.874
_reflns_Friedel_fraction_full    0.972
_reflns_Friedel_fraction_max     0.972
_reflns_number_gt                4680
_reflns_number_total             4891
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc01591e2.cif
_cod_data_source_block           compound-2
_cod_depositor_comments
'Adding full bibliography for 7128125--7128128.cif.'
_cod_original_cell_volume        2810.78(11)
_cod_database_code               7128125
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.882
_shelx_estimated_absorpt_t_min   0.834
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C17(H17), C21(H21), C16(H16), C15(H15), C4(H4), C18(H18), C5(H5),
 C22(H22), C28(H28), C13(H13), C25(H25), C24(H24), C6(H6), C23(H23), C31(H31),
 C12(H12), C30(H30), C9(H9), C10(H10), C29(H29), C27(H27), C11(H11)
;
_shelx_res_checksum              87608
_shelx_hkl_checksum              39149
_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
;