Macrocycle Contraction and Expansion of a Dihydrosapphyrin Isomer
Yongshu Xie; Pingchun Wei; Xin Li; Tao Hong; Kai Zhang; Hiroyuki Furuta; Journal of the American Chemical Society 135 (2013) 19119–19122; doi:10.1021/ja4112644

data_4121390
_publ_section_title
;
 Macrocycle Contraction and Expansion of a Dihydrosapphyrin Isomer
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              19119
_journal_page_last               19122
_journal_paper_doi               10.1021/ja4112644
_journal_volume                  135
_journal_year                    2013
_chemical_formula_sum            'C52.5 H28.5 F20 N5 O2.5 S2.5'
_chemical_formula_weight         1229.45
_chemical_name_systematic
; 
 ? 
;
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_symmetry_cell_setting           monoclinic
_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                82.796(2)
_cell_angle_beta                 80.9420(10)
_cell_angle_gamma                68.5830(10)
_cell_formula_units_Z            2
_cell_length_a                   12.6242(11)
_cell_length_b                   13.2594(12)
_cell_length_c                   17.3455(15)
_cell_measurement_temperature    298(2)
_cell_volume                     2662.0(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 0.986
_diffrn_measured_fraction_theta_max 0.986
_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  0.0623
_diffrn_reflns_av_sigmaI/netI    0.1525
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            13250
_diffrn_reflns_theta_full        24.30
_diffrn_reflns_theta_max         24.30
_diffrn_reflns_theta_min         2.38
_exptl_absorpt_coefficient_mu    0.237
_exptl_absorpt_correction_T_max  0.9836
_exptl_absorpt_correction_T_min  0.9518
_exptl_crystal_density_diffrn    1.534
_exptl_crystal_F_000             1237
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.461
_refine_diff_density_min         -0.406
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.923
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     810
_refine_ls_number_reflns         8539
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.923
_refine_ls_R_factor_all          0.2072
_refine_ls_R_factor_gt           0.0857
_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^)+(0.0992P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1829
_refine_ls_wR_factor_ref         0.2372
_reflns_number_gt                3149
_reflns_number_total             8539
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja4112644_si_002.cif
_cod_data_source_block           110611a
_cod_original_formula_sum        'C52.50 H28.50 F20 N5 O2.50 S2.50'
_cod_database_code               4121390