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_7128128
_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         'C37 H28 Cl N O P2 Pd'
_chemical_formula_sum            'C37 H28 Cl N O P2 Pd'
_chemical_formula_weight         706.39
_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             2019-03-31
_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                91.809(2)
_cell_angle_beta                 95.505(2)
_cell_angle_gamma                115.634(2)
_cell_formula_units_Z            2
_cell_length_a                   9.6861(2)
_cell_length_b                   10.1225(2)
_cell_length_c                   17.8430(4)
_cell_measurement_reflns_used    20869
_cell_measurement_temperature    150
_cell_measurement_theta_max      30.4430
_cell_measurement_theta_min      2.2800
_cell_volume                     1564.79(6)
_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                 CCD
_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   10.00    --  -20.00   0.00-108.00  360
  2  \w    -78.00  19.00   0.50   10.00    --  -20.00 -72.00  36.00  194
  3  \w    -75.50  19.00   0.50   10.00    --  -20.00 -72.00-108.00  189
  4  \w    -73.00 -10.00   0.50   10.00    --  -20.00 -72.00-180.00  126
  5  \w    -30.00   0.00   0.50   10.00    --  -20.00  72.00 -36.00   60
  6  \w   -110.00  25.00   0.50   10.00    --  -20.00   0.00 -36.00  270
  7  \w   -110.00  19.00   0.50   10.00    --  -20.00 -72.00 -36.00  258
  8  \w    -71.00   2.00   0.50   10.00    --  -20.00 -72.00 108.00  146
  9  \w    -59.00  -0.50   0.50   10.00    --  -20.00  72.00-108.00  117
 10  \w     -9.00  21.50   0.50   10.00    --  -20.00  72.00  36.00   61
 11  \w   -110.00  70.00   0.50   10.00    --  -20.00   0.00  36.00  360
 12  \w    -59.00  70.00   0.50   10.00    --  -20.00  72.00-180.00  258
 13  \w    -59.00  70.00   0.50   10.00    --  -20.00  72.00 108.00  258
;
_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_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0368212000
_diffrn_orient_matrix_UB_12      0.0167774000
_diffrn_orient_matrix_UB_13      -0.0320819000
_diffrn_orient_matrix_UB_21      0.0468154000
_diffrn_orient_matrix_UB_22      -0.0162850000
_diffrn_orient_matrix_UB_23      -0.0233583000
_diffrn_orient_matrix_UB_31      -0.0561132000
_diffrn_orient_matrix_UB_32      -0.0743925000
_diffrn_orient_matrix_UB_33      -0.0055420000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0812
_diffrn_reflns_av_unetI/netI     0.0412
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            37541
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.435
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Rotating Anode'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.812
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74310
_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    1.499
_exptl_crystal_description       block
_exptl_crystal_F_000             716
_exptl_crystal_size_max          0.125
_exptl_crystal_size_mid          0.085
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.628
_refine_diff_density_min         -0.593
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         5497
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0408
_refine_ls_R_factor_gt           0.0346
_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^)+(0.0337P)^2^+1.1987P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0765
_refine_ls_wR_factor_ref         0.0799
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4933
_reflns_number_total             5497
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc01591e2.cif
_cod_data_source_block           compound-3
_cod_depositor_comments
'Adding full bibliography for 7128125--7128128.cif.'
_cod_database_code               7128128
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.953
_shelx_estimated_absorpt_t_min   0.905
_reflns_odcompleteness_completeness 93.40
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     31.07
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C24(H24), C10(H10), C9(H9), C29(H29), C5(H5), C34(H34), C33(H33), C35(H35),
 C27(H27), C37(H37), C6(H6), C30(H30), C31(H31), C21(H21), C11(H11), C12(H12),
 C4(H4), C15(H15), C36(H36), C13(H13), C28(H28), C16(H16), C3(H3), C22(H22),
 C23(H23), C18(H18), C17(H17), C19(H19)
;
_shelx_res_checksum              16243
_shelx_hkl_checksum              48902
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 4.966
_oxdiff_exptl_absorpt_empirical_full_min 0.448