Pd(II) Complexes Ligated by 1,3-Bis(diphenylphosphino)calix[4]arene: Preparation, X-ray Structures, and Catalyses
Hirasawa, Kengo; Tanaka, Shinya; Horiuchi, Takeru; Kobayashi, Takahiro; Sato, Takumi; Morohashi, Naoya; Hattori, Tetsutaro; Organometallics 35 (2016) 420–; doi:10.1021/acs.organomet.5b00999

data_4088317
_publ_section_title
;
 Pd(II) Complexes Ligated by 1,3-Bis(diphenylphosphino)calix[4]arene:
 Preparation, X-ray Structures, and Catalyses
;
_journal_issue                   3
_journal_name_full               Organometallics
_journal_page_first              420
_journal_paper_doi               10.1021/acs.organomet.5b00999
_journal_volume                  35
_journal_year                    2016
_chemical_formula_sum            'C80 H97 Cl10 N O2 P2 Pd'
_chemical_formula_weight         1627.43
_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                111.7260(10)
_cell_angle_beta                 90.3860(10)
_cell_angle_gamma                105.8190(10)
_cell_formula_units_Z            2
_cell_length_a                   14.0745(17)
_cell_length_b                   15.3088(19)
_cell_length_c                   20.273(3)
_cell_measurement_reflns_used    9926
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.82
_cell_measurement_theta_min      2.17
_cell_volume                     3875.7(9)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker APEXII'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics
'Yadokari-XG 2009 (Wakita Nemoto et al., 2009)'
_computing_publication_material
'Yadokari-XG 2009 (Wakita,Nemoto et al., 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'Bruker Helios multilayered confocal mirror'
_diffrn_radiation_source         'Bruker TXS fine-focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0330
_diffrn_reflns_av_sigmaI/netI    0.0427
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            44085
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.47
_exptl_absorpt_coefficient_mu    0.672
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6848
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.395
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1692
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.959
_refine_diff_density_min         -0.730
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     916
_refine_ls_number_reflns         17402
_refine_ls_number_restraints     107
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0469
_refine_ls_R_factor_gt           0.0343
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0299P)^2^+3.9067P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0764
_refine_ls_wR_factor_ref         0.0829
_reflns_number_gt                14381
_reflns_number_total             17402
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om5b00999_si_003.cif
_cod_data_source_block           complex9
_cod_original_cell_volume        3875.8(8)
_cod_database_code               4088317