meso-Aryl-Substituted Subporphyrins: Synthesis, Structures, and Large Substituent Effects on Their Electronic Properties
Yasuhide Inokuma; Zin Seok Yoon; Dongho Kim; Atsuhiro Osuka; Journal of the American Chemical Society 129 (2007) 4747–4761; doi:10.1021/ja069324z

data_4109309
_publ_section_title
;
 meso-Aryl-Substituted Subporphyrins: Synthesis, Structures, and Large
 Substituent Effects on Their Electronic Properties
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4747
_journal_page_last               4761
_journal_paper_doi               10.1021/ja069324z
_journal_volume                  129
_journal_year                    2007
_chemical_formula_moiety
'C43 H42 B N3 O10, C1.56 H4.93 Cl1.31 O1.12, C0.56 H2.22 O1.44'
_chemical_formula_sum            'C45.63 H51.21 B Cl1.31 N3 O13.57'
_chemical_formula_weight         916.17
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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                111.674(2)
_cell_angle_beta                 103.125(2)
_cell_angle_gamma                101.496(2)
_cell_formula_units_Z            2
_cell_length_a                   12.6630(11)
_cell_length_b                   14.0703(13)
_cell_length_c                   14.9534(13)
_cell_measurement_reflns_used    6144
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      28.23
_cell_measurement_theta_min      2.43
_cell_volume                     2290.2(4)
_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 0.875
_diffrn_measured_fraction_theta_max 0.875
_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  0.0163
_diffrn_reflns_av_sigmaI/netI    0.0412
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            14188
_diffrn_reflns_theta_full        28.32
_diffrn_reflns_theta_max         28.32
_diffrn_reflns_theta_min         1.55
_exptl_absorpt_coefficient_mu    0.168
_exptl_absorpt_correction_T_max  0.9513
_exptl_absorpt_correction_T_min  0.8985
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.329
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             857
_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.729
_refine_diff_density_min         -0.782
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     658
_refine_ls_number_reflns         9959
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0934
_refine_ls_R_factor_gt           0.0724
_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^)+(0.0890P)^2^+2.7986P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1831
_refine_ls_wR_factor_ref         0.1978
_reflns_number_gt                7571
_reflns_number_total             9959
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja069324zsi20061228_021924.cif
_cod_data_source_block           s246ome
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_formula_sum        'C45.63 H51.21 B Cl1.31 N3 O13.57 '
_cod_database_code               4109309