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 131 (2009) 14123–14123; doi:10.1021/ja907161j

data_4105091
_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              14123
_journal_page_last               14123
_journal_paper_doi               10.1021/ja907161j
_journal_volume                  131
_journal_year                    2009
_chemical_formula_moiety         'C46 H39 Cl N2 O P Rh S '
_chemical_formula_sum            'C46 H39 Cl N2 O P Rh S'
_chemical_formula_weight         837.18
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.964(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.669(6)
_cell_length_b                   14.829(7)
_cell_length_c                   18.824(8)
_cell_measurement_reflns_used    10161
_cell_measurement_temperature    143(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     3813(3)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        'CrystalStructure 3.8.2'
_computing_publication_material  'CrystalStructure 3.8.2'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      143(2)
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_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  0.0700
_diffrn_reflns_av_sigmaI/netI    0.0793
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            28617
_diffrn_reflns_theta_full        27.44
_diffrn_reflns_theta_max         27.44
_diffrn_reflns_theta_min         3.13
_exptl_absorpt_coefficient_mu    0.654
_exptl_absorpt_correction_T_max  0.9680
_exptl_absorpt_correction_T_min  0.7799
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.458
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1720
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.829
_refine_diff_density_min         -1.730
_refine_diff_density_rms         0.162
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.264
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     479
_refine_ls_number_reflns         8467
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.264
_refine_ls_R_factor_all          0.1435
_refine_ls_R_factor_gt           0.1127
_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^)+(0.0500P)^2^+25.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2041
_refine_ls_wR_factor_ref         0.2285
_reflns_number_gt                6542
_reflns_number_total             8467
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja907161j_si_001.cif
_cod_data_source_block           shelxl
_cod_original_cell_volume        3814(3)
_cod_database_code               4105091