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_4121391
_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            'C51 H20 F20 N6 O2'
_chemical_formula_weight         1128.73
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.476(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.064(3)
_cell_length_b                   9.7487(18)
_cell_length_c                   30.825(6)
_cell_measurement_temperature    296(2)
_cell_volume                     4522.6(15)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0514
_diffrn_reflns_av_sigmaI/netI    0.0571
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            29096
_diffrn_reflns_theta_full        26.25
_diffrn_reflns_theta_max         26.25
_diffrn_reflns_theta_min         1.85
_exptl_absorpt_coefficient_mu    0.160
_exptl_absorpt_correction_T_max  0.9873
_exptl_absorpt_correction_T_min  0.9100
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_density_diffrn    1.658
_exptl_crystal_F_000             2256
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.303
_refine_diff_density_min         -0.310
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     714
_refine_ls_number_reflns         9085
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0929
_refine_ls_R_factor_gt           0.0533
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0867P)^2^+1.6648P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1398
_refine_ls_wR_factor_ref         0.1631
_reflns_number_gt                5917
_reflns_number_total             9085
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja4112644_si_003.cif
_cod_data_source_block           mo_20704a
_cod_original_cell_volume        4522.5(14)
_cod_database_code               4121391