Synthesis of meso-5-azaindolyl-appended Zn(II) porphyrins via Pd-catalyzed annulation.
Maeda, Chihiro; Shinokubo, Hiroshi; Osuka, Atsuhiro; Organic letters 9 (2007) 2493–2496; doi:10.1021/ol070885k

data_1505424
_publ_section_title
;
 Synthesis of meso-5-azaindolyl-appended Zn(II) porphyrins via
 Pd-catalyzed annulation.
;
_journal_issue                   13
_journal_name_full               'Organic letters'
_journal_page_first              2493
_journal_page_last               2496
_journal_paper_doi               10.1021/ol070885k
_journal_volume                  9
_journal_year                    2007
_chemical_formula_sum            'C77 H94 Cl3 N6 O Zn'
_chemical_formula_weight         1291.30
_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                98.296(3)
_cell_angle_beta                 94.448(3)
_cell_angle_gamma                96.059(3)
_cell_formula_units_Z            4
_cell_length_a                   11.7096(19)
_cell_length_b                   20.183(3)
_cell_length_c                   31.905(5)
_cell_measurement_reflns_used    6519
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      28.01
_cell_measurement_theta_min      2.32
_cell_volume                     7387(2)
_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 0.974
_diffrn_measured_fraction_theta_max 0.974
_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  0.0542
_diffrn_reflns_av_sigmaI/netI    0.1427
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            35370
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.03
_exptl_absorpt_coefficient_mu    0.487
_exptl_absorpt_correction_T_max  0.9089
_exptl_absorpt_correction_T_min  0.7589
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.161
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2748
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.594
_refine_diff_density_min         -0.792
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1675
_refine_ls_number_reflns         25307
_refine_ls_number_restraints     1372
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.1702
_refine_ls_R_factor_gt           0.0932
_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^)+(0.1052P)^2^+36.3875P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2266
_refine_ls_wR_factor_ref         0.2783
_reflns_number_gt                13956
_reflns_number_total             25307
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol070885ksi20070417_030722.cif
_cod_data_source_block           cmaeda70225
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_database_code               1505424