Palladacycles with a Metal-Bonded sp3-Hybridized Carbon as Intermediates in the Synthesis of 2,2,3,4-Tetrasubstituted 2H-1-Benzopyrans and 1,2-Dihydroquinolines. Effects of Auxiliary Ligands and Substitution at a Palladium-Bonded Tertiary Carbon
Lu, Genliang; Portscheller, Janelle L.; Malinakova, Helena C.; Organometallics 24 (2005) 945–; doi:10.1021/om0491544

data_4089331
_publ_section_title
;
 Palladacycles with a Metal-Bonded sp3-Hybridized Carbon as Intermediates
 in the Synthesis of 2,2,3,4-Tetrasubstituted 2H-1-Benzopyrans and
 1,2-Dihydroquinolines. Effects of Auxiliary Ligands and Substitution at a
 Palladium-Bonded Tertiary Carbon
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              945
_journal_paper_doi               10.1021/om0491544
_journal_volume                  24
_journal_year                    2005
_chemical_formula_moiety         'C48 H45 I O3 P2 Pd'
_chemical_formula_sum            'C48 H45 I O3 P2 Pd'
_chemical_formula_weight         965.08
_space_group_IT_number           2
_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                75.415(3)
_cell_angle_beta                 88.903(3)
_cell_angle_gamma                77.105(3)
_cell_formula_units_Z            2
_cell_length_a                   9.734(2)
_cell_length_b                   14.126(3)
_cell_length_c                   15.694(4)
_cell_measurement_reflns_used    9378
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.00
_cell_measurement_theta_min      2.27
_cell_volume                     2034.2(8)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2000)'
_computing_publication_material  'SHELXTL (Sheldrick, 2000)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2000)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2000)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX'
_diffrn_measurement_method       '\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  0.0224
_diffrn_reflns_av_sigmaI/netI    0.0329
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            17803
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.15
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.336
_exptl_absorpt_correction_T_max  0.9362
_exptl_absorpt_correction_T_min  0.7487
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2002)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.576
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             972
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.350
_refine_diff_density_min         -0.515
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     515
_refine_ls_number_reflns         7974
_refine_ls_number_restraints     57
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0359
_refine_ls_R_factor_gt           0.0307
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+1.3000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0795
_refine_ls_wR_factor_ref         0.0826
_reflns_number_gt                7062
_reflns_number_total             7974
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om0491544si20041030_111302.cif
_cod_data_source_block           compound_6a
_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_database_code               4089331