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_4108779
_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            'C126.66 H143.32 Cl4.02 N8.66 Ni2 O4'
_chemical_formula_weight         2110.96
_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                66.993(12)
_cell_angle_beta                 86.554(14)
_cell_angle_gamma                78.472(12)
_cell_formula_units_Z            1
_cell_length_a                   13.188(5)
_cell_length_b                   14.388(5)
_cell_length_c                   16.656(7)
_cell_measurement_reflns_used    15186
_cell_measurement_temperature    123.1
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     2849.8(19)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.8'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123.1
_diffrn_detector_area_resol_mean 5.00
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0807
_diffrn_reflns_av_sigmaI/netI    0.1135
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            21582
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.01
_exptl_absorpt_coefficient_mu    0.481
_exptl_absorpt_correction_T_max  0.9535
_exptl_absorpt_correction_T_min  0.7949
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
    Higashi, T. (1995). Program for Absorption Correction.
    Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.230
_exptl_crystal_description       prism
_exptl_crystal_F_000             1120
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.708
_refine_diff_density_min         -0.445
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     773
_refine_ls_number_reflns         9836
_refine_ls_number_restraints     105
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.1517
_refine_ls_R_factor_gt           0.0860
_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^)+(0.1364P)^2^+2.3887P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2190
_refine_ls_wR_factor_ref         0.2661
_reflns_number_gt                5552
_reflns_number_total             9836
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja807659h_si_003.cif
_cod_data_source_block           shelxl
_cod_original_cell_volume        2849.9(19)
_cod_database_code               4108779