Synthesis, Structures, and Coordinating Properties of Phosphole-Containing Hybrid Calixpyrroles
Nakabuchi, Takashi; Matano, Yoshihiro; Imahori, Hiroshi; Organometallics 27 (2008) 3142–; doi:10.1021/om800099h

data_4071313
_publ_section_title
;
 Synthesis, Structures, and Coordinating Properties of
 Phosphole-Containing Hybrid Calixpyrroles
;
_journal_issue                   13
_journal_name_full               Organometallics
_journal_page_first              3142
_journal_paper_doi               10.1021/om800099h
_journal_volume                  27
_journal_year                    2008
_chemical_formula_moiety         'C74 H86 Cl2 N4 P2 Pd S2, C H2 Cl2'
_chemical_formula_sum            'C75 H88 Cl4 N4 P2 Pd S2'
_chemical_formula_weight         1419.75
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_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                83.596(3)
_cell_angle_beta                 82.667(3)
_cell_angle_gamma                70.280(2)
_cell_formula_units_Z            2
_cell_length_a                   13.0181(10)
_cell_length_b                   16.1257(13)
_cell_length_c                   19.4032(17)
_cell_measurement_reflns_used    11849
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.7
_cell_measurement_theta_min      3.2
_cell_volume                     3792.8(5)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.8.0'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR97
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.947
_diffrn_measured_fraction_theta_max 0.947
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0152
_diffrn_reflns_av_sigmaI/netI    0.0247
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            30108
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.17
_exptl_absorpt_coefficient_mu    0.525
_exptl_absorpt_correction_T_max  0.9023
_exptl_absorpt_correction_T_min  0.7793
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.243
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1484
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.795
_refine_diff_density_min         -1.990
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     794
_refine_ls_number_reflns         16453
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0539
_refine_ls_R_factor_gt           0.0503
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0806P)^2^+10.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1439
_refine_ls_wR_factor_ref         0.1471
_reflns_number_gt                14915
_reflns_number_total             16453
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800099h-file001.cif
_cod_data_source_block           14ii
_cod_database_code               4071313