Synthesis of Directly and Doubly Linked Dioxoisobacteriochlorin Dimers
Satoru Hiroto; Ichiro Hisaki; Hiroshi Shinokubo; Atsuhiro Osuka; Journal of the American Chemical Society 130 (2008) 16172–16173; doi:10.1021/ja807659h

data_4108778
_publ_section_title
;
 Synthesis of Directly and Doubly Linked Dioxoisobacteriochlorin Dimers
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16172
_journal_page_last               16173
_journal_paper_doi               10.1021/ja807659h
_journal_volume                  130
_journal_year                    2008
_chemical_formula_sum            'C127 H147 Cl9 N8 O4'
_chemical_formula_weight         2168.58
_chemical_name_systematic
; 
 ? 
;
_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                93.212(3)
_cell_angle_beta                 103.856(3)
_cell_angle_gamma                110.975(3)
_cell_formula_units_Z            2
_cell_length_a                   14.333(2)
_cell_length_b                   16.550(3)
_cell_length_c                   27.977(5)
_cell_measurement_reflns_used    8810
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      27.94
_cell_measurement_theta_min      2.28
_cell_volume                     5942.4(17)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0277
_diffrn_reflns_av_sigmaI/netI    0.0652
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            30949
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         0.76
_exptl_absorpt_coefficient_mu    0.267
_exptl_absorpt_correction_T_max  0.9738
_exptl_absorpt_correction_T_min  0.8146
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.212
_exptl_crystal_description       prism
_exptl_crystal_F_000             2300
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.052
_refine_diff_density_min         -1.423
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1524
_refine_ls_number_reflns         20563
_refine_ls_number_restraints     291
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.1343
_refine_ls_R_factor_gt           0.0937
_refine_ls_shift/su_max          0.033
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1771P)^2^+9.7591P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2646
_refine_ls_wR_factor_ref         0.3056
_reflns_number_gt                13251
_reflns_number_total             20563
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja807659h_si_002.cif
_cod_data_source_block           80701hi
_cod_original_cell_volume        5942.3(17)
_cod_database_code               4108778