Phosphorus complexes of a triply-fused [24]pentaphyrin
Higashino, Tomohiro; Osuka, Atsuhiro; Chemical Science 3 (2012) 103–; doi:10.1039/c1sc00653c

data_1515271
_publ_section_title
;
 Phosphorus complexes of a triply-fused [24]pentaphyrin
;
_journal_issue                   1
_journal_name_full               'Chemical Science'
_journal_page_first              103
_journal_paper_doi               10.1039/c1sc00653c
_journal_volume                  3
_journal_year                    2012
_chemical_formula_moiety         'C55 H11 B F24 N5 P, 1.5(C6 H14), 0.5(C7 H8)'
_chemical_formula_sum            'C67.5 H36 B F24 N5 P'
_chemical_formula_weight         1414.79
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 106.2569(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   30.1073(6)
_cell_length_b                   18.0820(3)
_cell_length_c                   22.4608(4)
_cell_measurement_reflns_used    43042
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      68.385
_cell_measurement_theta_min      3.06
_cell_volume                     11738.8(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      93(2)
_diffrn_detector_area_resol_mean 10.0
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.1381
_diffrn_reflns_av_sigmaI/netI    0.1279
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            55183
_diffrn_reflns_theta_full        68.24
_diffrn_reflns_theta_max         68.24
_diffrn_reflns_theta_min         3.06
_exptl_absorpt_coefficient_mu    1.556
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.4554
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_density_diffrn    1.601
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             5696
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.638
_refine_diff_density_min         -0.432
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     912
_refine_ls_number_reflns         10540
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.1220
_refine_ls_R_factor_gt           0.0759
_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^)+(0.0400P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1433
_refine_ls_wR_factor_ref         0.1619
_reflns_number_gt                5634
_reflns_number_total             10540
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1sc00653c.txt
_cod_data_source_block           0412hi
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C67.50 H36 B F24 N5 P'
_cod_database_code               1515271