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_4089421
_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         'C17 H28 O3 P2 Pd'
_chemical_formula_sum            'C17 H28 O3 P2 Pd'
_chemical_formula_weight         448.73
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                93.48
_cell_angle_beta                 110.08
_cell_angle_gamma                116.45
_cell_formula_units_Z            2
_cell_length_a                   9.3042(4)
_cell_length_b                   10.4077(4)
_cell_length_c                   12.3897(5)
_cell_measurement_reflns_used    9525
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      28.37
_cell_measurement_theta_min      2.26
_cell_volume                     975.78(7)
_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 0.970
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'ritating unit'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0103
_diffrn_reflns_av_sigmaI/netI    0.0175
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10911
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.81
_diffrn_standards_number         0.0
_exptl_absorpt_coefficient_mu    1.125
_exptl_absorpt_correction_T_max  0.8062
_exptl_absorpt_correction_T_min  0.7289
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_density_diffrn    1.527
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rectangle
_exptl_crystal_F_000             460
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.291
_refine_diff_density_min         -0.414
_refine_diff_density_rms         0.042
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.49(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.965
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     430
_refine_ls_number_reflns         8328
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      0.967
_refine_ls_R_factor_all          0.0149
_refine_ls_R_factor_gt           0.0139
_refine_ls_shift/su_max          0.034
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0136P)^2^+0.4732P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0340
_refine_ls_wR_factor_ref         0.0347
_reflns_number_gt                8003
_reflns_number_total             8328
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400089n_si_002.cif
_cod_data_source_block           4b
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Triclinic' was changed to
'triclinic' 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        975.80(7)
_cod_original_sg_symbol_H-M      P1
_cod_database_code               4089421