3-Aza pi-allyl palladium derived from imino migration in palladium-carbene: MCRs toward multiple substituted indole skeleton
Qiang Dai; Yan Jiang; Songjin Guo; Jin-Tao Yu; Jiang Cheng; Chem.Commun. 51 (2015) 14781–; doi:10.1039/C5cc05984D

data_7117834
_publ_section_title
;
 3-Aza pi-allyl palladium derived from imino migration in
 palladium-carbene: MCRs toward multiple substituted indole skeleton
;
_journal_name_full               Chem.Commun.
_journal_page_first              14781
_journal_paper_doi               10.1039/C5cc05984D
_journal_volume                  51
_journal_year                    2015
_chemical_formula_moiety         'C29 H32 N2 O'
_chemical_formula_sum            'C29 H32 N2 O'
_chemical_formula_weight         424.56
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-06-19 deposited with the CCDC.
2015-08-10 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 95.287(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.225(2)
_cell_length_b                   12.718(3)
_cell_length_c                   24.068(6)
_cell_measurement_reflns_used    2378
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      22.05
_cell_measurement_theta_min      2.34
_cell_volume                     2506.9(11)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Bruker, 2000)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'Bruker SMART CCD area detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0583
_diffrn_reflns_av_sigmaI/netI    0.0738
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            15586
_diffrn_reflns_theta_full        27.75
_diffrn_reflns_theta_max         27.75
_diffrn_reflns_theta_min         1.70
_exptl_absorpt_coefficient_mu    0.068
_exptl_absorpt_correction_T_max  0.9926
_exptl_absorpt_correction_T_min  0.9826
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.125
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.284
_refine_diff_density_min         -0.236
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     294
_refine_ls_number_reflns         5744
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.1475
_refine_ls_R_factor_gt           0.0686
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0975P)^2^+0.2648P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1761
_refine_ls_wR_factor_ref         0.2165
_reflns_number_gt                2762
_reflns_number_total             5744
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c5cc05984d2.cif.txt
_cod_data_source_block           6a
_cod_depositor_comments
;

2018-03-15
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_sg_symbol_Hall     '-P 2ybc '
_cod_original_sg_symbol_H-M      'p 21/c'
_cod_original_formula_moiety     'C116 H128 N8 O4'
_cod_original_formula_sum        'C116 H128 N8 O4'
_cod_original_formula_units_Z    1
_cod_original_formula_weight     1698.26
_cod_database_code               7117834