Syntheses, Structures, and Coordination Chemistry of Phosphole-Containing Hybrid Calixphyrins: Promising Macrocyclic P,N2,X-Mixed Donor Ligands for Designing Reactive Transition-Metal Complexes
Yoshihiro Matano; Tooru Miyajima; Noriaki Ochi; Takashi Nakabuchi; Motoo Shiro; Yoshihide Nakao; Shigeyoshi Sakaki; Hiroshi Imahori; Journal of the American Chemical Society 130 (2008) 990–1002; doi:10.1021/ja076709o

data_4107315
_publ_contact_author_email       matano@scl.kyoto-u.ac.jp
_publ_contact_author_fax         +81-75-383-2571
_publ_contact_author_name        'Yoshihiro Matano'
_publ_contact_author_phone       +81-75-383-2567
_publ_section_title
;
 Syntheses, Structures, and Coordination Chemistry of Phosphole-Containing
 Hybrid Calixphyrins: Promising Macrocyclic P,N2,X-Mixed Donor Ligands for
 Designing Reactive Transition-Metal Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              990
_journal_page_last               1002
_journal_paper_doi               10.1021/ja076709o
_journal_volume                  130
_journal_year                    2008
_chemical_formula_moiety         'C45 H41 N2 O P, C H2 Cl2'
_chemical_formula_sum            'C46 H43 Cl2 N2 O P'
_chemical_formula_weight         741.69
_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                80.666(6)
_cell_angle_beta                 86.396(6)
_cell_angle_gamma                66.557(5)
_cell_formula_units_Z            2
_cell_length_a                   11.4831(18)
_cell_length_b                   13.406(2)
_cell_length_c                   13.519(2)
_cell_measurement_reflns_used    4939
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     1884.1(5)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.7.0'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR92
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.951
_diffrn_measured_fraction_theta_max 0.951
_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  0.0199
_diffrn_reflns_av_sigmaI/netI    0.0375
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            15138
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.02
_exptl_absorpt_coefficient_mu    0.254
_exptl_absorpt_correction_T_max  0.9509
_exptl_absorpt_correction_T_min  0.8729
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
    Higashi, T. (1999). Program for Absorption Correction.
    Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.307
_exptl_crystal_description       block
_exptl_crystal_F_000             780
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.061
_refine_diff_density_min         -0.953
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     470
_refine_ls_number_reflns         8219
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0747
_refine_ls_R_factor_gt           0.0579
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0350P)^2^+3.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1214
_refine_ls_wR_factor_ref         0.1306
_reflns_number_gt                6673
_reflns_number_total             8219
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja076709o-file004.cif
_cod_data_source_block           shelxl
_cod_database_code               4107315