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_4121392
_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            'C49 H15 F20 N5 O2 Zn'
_chemical_formula_weight         1151.03
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 116.539(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.774(5)
_cell_length_b                   34.488(12)
_cell_length_c                   17.962(6)
_cell_measurement_temperature    293(2)
_cell_volume                     9296(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0876
_diffrn_reflns_av_sigmaI/netI    0.1124
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            54188
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         1.38
_exptl_absorpt_coefficient_mu    0.656
_exptl_absorpt_correction_T_max  0.929
_exptl_absorpt_correction_T_min  0.878
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_density_diffrn    1.645
_exptl_crystal_F_000             4560
_exptl_crystal_size_max          0.254
_exptl_crystal_size_mid          0.165
_exptl_crystal_size_min          0.113
_refine_diff_density_max         0.542
_refine_diff_density_min         -0.424
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.983
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1405
_refine_ls_number_reflns         17303
_refine_ls_number_restraints     244
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.1632
_refine_ls_R_factor_gt           0.0683
_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^)+(0.0848P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1569
_refine_ls_wR_factor_ref         0.1952
_reflns_number_gt                7817
_reflns_number_total             17303
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja4112644_si_004.cif
_cod_data_source_block           cd212357
_cod_database_code               4121392