Synthesis and Reactivity of Five-Membered Palladalactones from Arylallenes and Carbon Dioxide: Relevance to Catalytic Lactone Synthesis
Choi, Jun-Chul; Shiraishi, Kouichi; Takenaka, Yasumasa; Yasuda, Hiroyuki; Sakakura, Toshiyasu; Organometallics 32 (2013) 3411–; doi:10.1021/om400089n

data_4089420
_publ_section_title
;
 Synthesis and Reactivity of Five-Membered Palladalactones from
 Arylallenes and Carbon Dioxide: Relevance to Catalytic Lactone Synthesis
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              3411
_journal_paper_doi               10.1021/om400089n
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'C16 H26 O2 P2 Pd'
_chemical_formula_sum            'C16 H26 O2 P2 Pd'
_chemical_formula_weight         418.71
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 99.79
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.2573(4)
_cell_length_b                   15.9973(6)
_cell_length_c                   10.1755(4)
_cell_measurement_reflns_used    9971
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      28.42
_cell_measurement_theta_min      2.23
_cell_volume                     1805.78(12)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating unit'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0140
_diffrn_reflns_av_sigmaI/netI    0.0103
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            19786
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         1.84
_diffrn_standards_number         0.0
_exptl_absorpt_coefficient_mu    1.206
_exptl_absorpt_correction_T_max  0.7136
_exptl_absorpt_correction_T_min  0.6440
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadads
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.544
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rectangular
_exptl_crystal_F_000             860
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.456
_refine_diff_density_min         -0.470
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     196
_refine_ls_number_reflns         4115
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0171
_refine_ls_R_factor_gt           0.0155
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0214P)^2^+0.9109P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0402
_refine_ls_wR_factor_ref         0.0413
_reflns_number_gt                3879
_reflns_number_total             4115
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400089n_si_002.cif
_cod_data_source_block           4a
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Monoclinic' was changed to
'monoclinic' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        1805.81(12)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4089420