Isocyanide insertion across the Pd-C bond of allenyl and propargyl palladium complexes bearing phosphoquinoline as a spectator ligand. Synthesis of a palladium complex bearing a coordinated cyclobutenyl fragment.
Scattolin, Thomas; Visentin, Fabiano; Santo, Claudio; Bertolasi, Valerio; Canovese, Luciano; Dalton transactions (Cambridge, England : 2003) 46 (2017) 5210–5217; doi:10.1039/c7dt00454k

data_7042536
_publ_section_title
;
 Isocyanide insertion across the Pd-C bond of allenyl and propargyl
 palladium complexes bearing phosphoquinoline as a spectator ligand.
 Synthesis of a palladium complex bearing a coordinated cyclobutenyl
 fragment.
;
_journal_issue                   16
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5210
_journal_page_last               5217
_journal_paper_doi               10.1039/c7dt00454k
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety         'C39 H32 Cl N2 O2 P Pd S, 1.5(C H2 Cl2)'
_chemical_formula_sum            'C40.5 H35 Cl4 N2 O2 P Pd S'
_chemical_formula_weight         892.93
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/6
_audit_update_record
;
2016-10-11 deposited with the CCDC.
2017-03-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.9140(18)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.6709(4)
_cell_length_b                   9.3853(3)
_cell_length_c                   23.9410(8)
_cell_measurement_reflns_used    19027
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.00
_cell_measurement_theta_min      2.28
_cell_volume                     4013.8(2)
_computing_cell_refinement       'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction        'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'ORTEPIII (Burnett & Johnson, 1996)'
_computing_publication_material
'SHELXL-2014/6 (Sheldrick, 2014), PARST (Nardelli, 1995), PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0389
_diffrn_reflns_av_unetI/netI     0.0474
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            19027
_diffrn_reflns_point_group_measured_fraction_full 0.901
_diffrn_reflns_point_group_measured_fraction_max 0.858
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.016
_diffrn_reflns_theta_min         2.280
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.858
_exptl_absorpt_correction_T_max  0.936
_exptl_absorpt_correction_T_min  0.842
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SORTAV (Blessing, 1995)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.478
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1812
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.407
_refine_diff_density_min         -0.703
_refine_diff_density_rms         0.067
_refine_ls_abs_structure_details
;
 Flack x determined using 2920 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.014(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     466
_refine_ls_number_reflns         10073
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0551
_refine_ls_R_factor_gt           0.0394
_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^)+(0.0226P)^2^+5.2029P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0789
_refine_ls_wR_factor_ref         0.0865
_reflns_Friedel_coverage         0.645
_reflns_Friedel_fraction_full    0.797
_reflns_Friedel_fraction_max     0.714
_reflns_number_gt                8370
_reflns_number_total             10073
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00454k2.cif
_cod_data_source_block           Pd_C2
_cod_depositor_comments          'Adding full bibliography for 7042536.cif.'
_cod_original_formula_sum        'C40.50 H35 Cl4 N2 O2 P Pd S'
_cod_database_code               7042536
_shelxl_version_number           2014/6
_shelx_res_checksum              58570