Synthesis, Photochemical Properties, and Cytotoxicities of 2H-Naphtho[1,2-b]pyran and Its Photodimers.
Ota, Motohiro; Sasamori, Takahiro; Tokitoh, Norihiro; Onodera, Takefumi; Mizushina, Yoshiyuki; Kuramochi, Kouji; Tsubaki, Kazunori; The Journal of organic chemistry 80 (2015) 5687–5695; doi:10.1021/acs.joc.5b00645

data_4030959
_publ_section_title
;
 Synthesis, Photochemical Properties, and Cytotoxicities of
 2H-Naphtho[1,2-b]pyran and Its Photodimers.
;
_journal_issue                   11
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              5687
_journal_page_last               5695
_journal_paper_doi               10.1021/acs.joc.5b00645
_journal_volume                  80
_journal_year                    2015
_chemical_formula_moiety         'C48 H32 Br2 Cl6 O8'
_chemical_formula_sum            'C48 H32 Br2 Cl6 O8'
_chemical_formula_weight         1109.26
_chemical_melting_point          241
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                74.6642(6)
_cell_angle_beta                 74.5511(6)
_cell_angle_gamma                87.2285(8)
_cell_formula_units_Z            3
_cell_length_a                   11.78910(10)
_cell_length_b                   17.3916(2)
_cell_length_c                   17.8781(3)
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      25.5
_cell_measurement_theta_min      1.48
_cell_volume                     3406.36(8)
_computing_cell_refinement       HKL2000
_computing_data_collection       CrystalClear
_computing_data_reduction        HKL2000
_computing_molecular_graphics    'Yadokari-XG 2011 (Wakita Nemoto et al., 2011)'
_computing_publication_material  'Yadokari-XG 2011 (Wakita,Nemoto et al., 2011)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR2004
_diffrn_ambient_temperature      103(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku VariMax Saturn'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_source         'rotating-anode X-ray tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71000
_diffrn_reflns_av_R_equivalents  0.0699
_diffrn_reflns_av_sigmaI/netI    0.0676
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            47438
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         1.48
_exptl_absorpt_coefficient_mu    2.193
_exptl_absorpt_correction_T_max  0.9371
_exptl_absorpt_correction_T_min  0.8797
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 MULABS - Empirical Correction for Absorption Anisotropy.
 Blessing, R. H., Acta Cryst., A51, 33-38 (1995).
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.622
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1668
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         9.814
_refine_diff_density_min         -2.117
_refine_diff_density_rms         0.196
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     902
_refine_ls_number_reflns         12685
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.1322
_refine_ls_R_factor_gt           0.0991
_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^)+(0.1298P)^2^+51.1760P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2467
_refine_ls_wR_factor_ref         0.2734
_reflns_number_gt                9181
_reflns_number_total             12685
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo5b00645_si_003.cif
_cod_data_source_block           mo307
_cod_depositor_comments
'Adding full bibliography for 4030959--4030960.cif.'
_cod_original_sg_symbol_Hall     ' -P 1 '
_cod_database_code               4030959