New tertiary phosphines from cinnamaldehydes and diphenylphosphine.
Moiseev, Dmitry V.; Patrick, Brian O.; James, Brian R.; Inorganic chemistry 46 (2007) 11467–11474; doi:10.1021/ic701597g

data_4339146
_publ_section_title
;
 New tertiary phosphines from cinnamaldehydes and diphenylphosphine.
;
_journal_issue                   26
_journal_name_full               'Inorganic chemistry'
_journal_page_first              11467
_journal_page_last               11474
_journal_paper_doi               10.1021/ic701597g
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C36 H42 Cl2 O4 P2 Pd'
_chemical_formula_weight         777.94
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   14.7439(6)
_cell_length_b                   21.8538(9)
_cell_length_c                   21.9153(9)
_cell_measurement_reflns_used    6810
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.71
_cell_measurement_theta_min      2.50
_cell_volume                     7061.3(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker X8 APEX II'
_diffrn_measurement_method       'area detector'
_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  0.0664
_diffrn_reflns_av_sigmaI/netI    0.0599
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            44287
_diffrn_reflns_theta_full        27.91
_diffrn_reflns_theta_max         27.91
_diffrn_reflns_theta_min         1.86
_exptl_absorpt_coefficient_mu    0.805
_exptl_absorpt_correction_T_max  0.961
_exptl_absorpt_correction_T_min  0.703
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.464
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blade
_exptl_crystal_F_000             3200
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.006
_refine_diff_density_min         -0.947
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     450
_refine_ls_number_reflns         8420
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.118
_refine_ls_R_factor_all          0.0889
_refine_ls_R_factor_gt           0.0546
_refine_ls_shift/su_max          0.029
_refine_ls_shift/su_mean         0.020
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+36.2136P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1023
_refine_ls_wR_factor_ref         0.1129
_reflns_number_gt                5943
_reflns_number_total             8420
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic701597g-file005.cif
_cod_data_source_block           bj459
_cod_original_sg_symbol_H-M      'P bca'
_cod_database_code               4339146