Masked Imidazolyl-Dipyrromethanes in the Synthesis of Imidazole-Substituted Porphyrins
Jayeeta Bhaumik; Zhen Yao; K. Eszter Borbas; Masahiko Taniguchi; Jonathan S. Lindsey; Journal of Organic Chemistry 71 (2006) 8807–8817; doi:10.1021/jo061461r

data_4022067
_publ_contact_author_address
;
 Department of Chemistry
 North Carolina State University
 Raleigh, NC 27695-8204, USA
;
_publ_contact_author_email       jlindsey@ncsu.edu
_publ_contact_author_name        'Jonathan S. Lindsey'
_publ_section_title
;
 Masked Imidazolyl-Dipyrromethanes in the Synthesis of
 Imidazole-Substituted Porphyrins
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              8807
_journal_page_last               8817
_journal_paper_doi               10.1021/jo061461r
_journal_volume                  71
_journal_year                    2006
_chemical_formula_moiety         'C46 H68 B2 N4 O3 Si '
_chemical_formula_sum            'C46 H68 B2 N4 O3 Si'
_chemical_formula_weight         774.76
_chemical_name_systematic        (9-BBN)25
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                78.820(3)
_cell_angle_beta                 71.278(3)
_cell_angle_gamma                85.826(3)
_cell_formula_units_Z            2
_cell_length_a                   11.1750(9)
_cell_length_b                   13.0823(10)
_cell_length_c                   16.1471(12)
_cell_measurement_reflns_used    5934
_cell_measurement_temperature    110
_cell_measurement_theta_max      24.22
_cell_measurement_theta_min      2.26
_cell_volume                     2193.1(3)
_computing_cell_refinement       'Bruker-Nonius Apex2'
_computing_data_collection       'Bruker-Nonius Apex2'
_computing_data_reduction        SAINT+
_computing_molecular_graphics    NRCVAX
_computing_publication_material  'NRCVAX TABLES Jan 94 Version'
_computing_structure_refinement  'NRCVAX LSTSQ'
_computing_structure_solution    SIR92
_diffrn_ambient_temperature      110
_diffrn_measured_fraction_theta_full 1.00
_diffrn_measurement_device       'Bruker-Nonius X8 Apex2'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'xray tube'
_diffrn_radiation_type           'Molybdenum K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.062
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            28845
_diffrn_reflns_theta_full        24.77
_diffrn_reflns_theta_max         24.77
_diffrn_reflns_theta_min         1.91
_exptl_absorpt_coefficient_mu    0.10
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7763
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'pale greenish-yellow'
_exptl_crystal_density_diffrn    1.173
_exptl_crystal_description       prism
_exptl_crystal_F_000             840.58
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.41
_refine_diff_density_min         -0.78
_refine_ls_extinction_coef       3.6(7)
_refine_ls_extinction_method     Larson
_refine_ls_goodness_of_fit_ref   2.01
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     515
_refine_ls_number_reflns         5953
_refine_ls_R_factor_all          0.102
_refine_ls_R_factor_gt           0.082
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     '1/(\s^2^(F)+0.0005F^2^) '
_refine_ls_wR_factor_all         0.096
_refine_ls_wR_factor_ref         0.091
_reflns_number_gt                5977
_reflns_number_total             7502
_reflns_threshold_expression     'Inet > 1.0\s(Inet)'
_cod_data_source_file            jo061461rsi20060908_054816.cif
_cod_depositor_comments
;
 Changing the _atom_site_occupancy data item value from '.' to '1'
 for all fully occupied atom sites.

 Antanas Vaitkus,
 2017-02-19
;
_cod_original_formula_sum        'C46 H68 B2 N4 O3 Si '
_cod_database_code               4022067