Neo-N-confused Phlorins and Phlorinone: Rational Synthesis and Tunable Properties.
Kong, Jiahui; Shao, Jiewei; Li, Chengjie; Qi, Dongdong; Li, Minzhi; Liang, Xu; Zhu, Weihua; Jiang, Jianzhuang; Xie, Yongshu; Organic letters 19 (2017) 650–653; doi:10.1021/acs.orglett.6b03816

data_1545139
_publ_section_title
;
 Neo-N-confused Phlorins and Phlorinone: Rational Synthesis and Tunable
 Properties.
;
_journal_issue                   3
_journal_name_full               'Organic letters'
_journal_page_first              650
_journal_page_last               653
_journal_paper_doi               10.1021/acs.orglett.6b03816
_journal_volume                  19
_journal_year                    2017
_chemical_formula_sum            'C52 H24.5 Cl0.5 F15 N4 O'
_chemical_formula_weight         1023.98
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_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                111.361(3)
_cell_angle_beta                 106.737(2)
_cell_angle_gamma                99.7020(10)
_cell_formula_units_Z            2
_cell_length_a                   12.5205(12)
_cell_length_b                   14.7808(13)
_cell_length_c                   15.1296(14)
_cell_measurement_temperature    298(2)
_cell_volume                     2376.9(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0248
_diffrn_reflns_av_sigmaI/netI    0.0667
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            11436
_diffrn_reflns_theta_full        24.52
_diffrn_reflns_theta_max         24.52
_diffrn_reflns_theta_min         2.34
_exptl_absorpt_coefficient_mu    0.154
_exptl_absorpt_correction_T_max  0.9465
_exptl_absorpt_correction_T_min  0.9337
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.431
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1032
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.36
_refine_diff_density_max         1.112
_refine_diff_density_min         -0.330
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     719
_refine_ls_number_reflns         7766
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.1591
_refine_ls_R_factor_gt           0.0925
_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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2659
_refine_ls_wR_factor_ref         0.3166
_reflns_number_gt                4054
_reflns_number_total             7766
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol6b03816_si_004.cif
_cod_data_source_block           160424f
_cod_depositor_comments
'Adding full bibliography for 1545137--1545139.cif.'
_cod_original_formula_sum        'C52 H24.50 Cl0.50 F15 N4 O'
_cod_database_code               1545139