Asymmetric synthesis and photophysical properties of benzopyrano- or naphthopyrano-fused helical phosphafluorenes.
Fukawa, Naohiro; Osaka, Takuya; Noguchi, Keiichi; Tanaka, Ken; Organic letters 12 (2010) 1324–1327; doi:10.1021/ol100227k

data_1502891
_publ_section_title
;
 Asymmetric synthesis and photophysical properties of benzopyrano- or
 naphthopyrano-fused helical phosphafluorenes.
;
_journal_issue                   6
_journal_name_full               'Organic letters'
_journal_page_first              1324
_journal_page_last               1327
_journal_paper_doi               10.1021/ol100227k
_journal_volume                  12
_journal_year                    2010
_chemical_formula_moiety         'C39 H27 O3 P, C3 H6 O'
_chemical_formula_sum            'C42 H33 O4 P'
_chemical_formula_weight         632.65
_chemical_name_common            phosphafluorene
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 114.023(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.8985(6)
_cell_length_b                   14.4684(6)
_cell_length_c                   17.6975(7)
_cell_measurement_reflns_used    20342
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      67.8
_cell_measurement_theta_min      3.1
_cell_volume                     3250.5(2)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        CrystalStructure
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR2004
_diffrn_ambient_temperature      193(2)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0773
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            5938
_diffrn_reflns_theta_full        68.17
_diffrn_reflns_theta_max         68.17
_diffrn_reflns_theta_min         3.48
_exptl_absorpt_coefficient_mu    1.096
_exptl_absorpt_correction_T_max  0.989
_exptl_absorpt_correction_T_min  0.903
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
    Higashi, T. (1999). Program for Absorption Correction.
    Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.293
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1328
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.633
_refine_diff_density_min         -0.379
_refine_diff_density_rms         0.065
_refine_ls_extinction_coef       0.0012(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.442
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     405
_refine_ls_number_reflns         5938
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.509
_refine_ls_R_factor_all          0.1610
_refine_ls_R_factor_gt           0.0900
_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^)+(0.0700P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2136
_refine_ls_wR_factor_ref         0.2399
_reflns_number_gt                2655
_reflns_number_total             5938
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol100227k_si_001.cif
_cod_data_source_block           I
_cod_database_code               1502891