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_4107316
_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         'C46 H41 Cl2 N3 P Rh, C4 H10 O'
_chemical_formula_sum            'C50 H51 Cl2 N3 O P Rh'
_chemical_formula_weight         914.76
_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'
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.5195(7)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   9.57301(17)
_cell_length_b                   10.8775(2)
_cell_length_c                   40.2774(7)
_cell_measurement_reflns_used    34025
_cell_measurement_temperature    100.1
_cell_measurement_theta_max      68.3
_cell_measurement_theta_min      3.3
_cell_volume                     4193.93(13)
_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    'PATTY (Beurskens, 1994)'
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.087
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            45872
_diffrn_reflns_theta_full        68.25
_diffrn_reflns_theta_max         68.25
_exptl_absorpt_coefficient_mu    5.151
_exptl_absorpt_correction_T_max  0.662
_exptl_absorpt_correction_T_min  0.530
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
    Higashi, T. (1995). Program for Absorption Correction.
    Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.449
_exptl_crystal_description       block
_exptl_crystal_F_000             1896.00
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.18
_refine_diff_density_min         -0.83
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     530
_refine_ls_number_reflns         7682
_refine_ls_R_factor_gt           0.0539
_refine_ls_shift/su_max          0.0010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0374P)^2^+12.0247P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1334
_reflns_number_gt                6001
_reflns_number_total             7682
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ja076709o-file005.cif
_cod_data_source_block           '_RGK1350raplt'
_cod_original_cell_volume        4193.95(13)
_cod_original_formula_sum        'C50 H51 Cl2 N3 O P Rh '
_cod_database_code               4107316