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_4107319
_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 H40 N3 P, C H2 Cl2 '
_chemical_formula_sum            'C46 H42 Cl2 N3 P'
_chemical_formula_weight         738.74
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_audit_creation_date             2007-03-07
_audit_creation_method           'by CrystalStructure 3.8'
_cell_angle_alpha                90.0000
_cell_angle_beta                 113.4033(7)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            8
_cell_length_a                   25.9707(5)
_cell_length_b                   10.16657(18)
_cell_length_c                   31.7731(6)
_cell_measurement_reflns_used    52761
_cell_measurement_temperature    93.1
_cell_measurement_theta_max      68.2
_cell_measurement_theta_min      4.2
_cell_volume                     7699.0(3)
_computing_cell_refinement       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_collection       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_reduction        'CrystalStructure (R/MSC, Rigaku, 2005)'
_computing_molecular_graphics    'ORTEP (Johnson, 1976)'
_computing_publication_material  'CrystalStructure (R/MSC, Rigaku, 2005)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.091
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            92356
_diffrn_reflns_theta_full        68.24
_diffrn_reflns_theta_max         68.24
_exptl_absorpt_coefficient_mu    2.187
_exptl_absorpt_correction_T_max  0.957
_exptl_absorpt_correction_T_min  0.779
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
    Higashi, T. (1995). Program for Absorption Correction.
    Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.275
_exptl_crystal_description       needle
_exptl_crystal_F_000             3104.00
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.75
_refine_diff_density_min         -1.02
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.237
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     940
_refine_ls_number_reflns         13776
_refine_ls_R_factor_gt           0.1414
_refine_ls_shift/su_max          0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.4181
_reflns_number_gt                6099
_reflns_number_total             13776
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ja076709o-file008.cif
_cod_data_source_block           '_RGK1410'
_cod_original_formula_sum        'C46 H42 Cl2 N3 P '
_cod_database_code               4107319