Influence of Mixed Substituents on the Macrocyclic Ring Distortions of Free Base Porphyrins and Their Metal Complexes
P. Bhyrappa; C. Arunkumar; B. Varghese; Inorganic Chemistry 48 (2009) 3954–3965; doi:10.1021/ic801618m

data_4302045
_publ_contact_author_address
'Dept. of Chem., Indian Institute of Technology Madras, Chennai 600 036, India'
_publ_contact_author_email       pbhyrappa@hotmail.com
_publ_contact_author_fax         091-44-2257-0509
_publ_contact_author_name        'P. Bhyrappa'
_publ_contact_author_phone       091-44-2257-4222
_publ_section_title
;
Influence of Mixed Substituents on the Macrocyclic Ring Distortions of Free
Base Porphyrins and Their Metal Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3954
_journal_page_last               3965
_journal_paper_doi               10.1021/ic801618m
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         '2(C68 H42 Br4 N4), 4(C4 H8 O), 3(CH4 O)'
_chemical_formula_sum            'C155 H128 Br8 N8 O7'
_chemical_formula_weight         2853.93
_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                113.3310(10)
_cell_angle_beta                 94.8680(10)
_cell_angle_gamma                107.2520(10)
_cell_formula_units_Z            1
_cell_length_a                   13.1059(3)
_cell_length_b                   16.1824(3)
_cell_length_c                   17.7714(4)
_cell_measurement_reflns_used    7608
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.7
_cell_measurement_theta_min      2.2
_cell_volume                     3215.99(13)
_computing_cell_refinement       'APEX2/SAINT (Bruker, 2004)'
_computing_data_reduction        'SAINT (Bruker, 2003)'
_computing_molecular_graphics
'ORTEP32 (Farrugia, 1997) & Mercury (Bruno et al., 2002)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       '\w and \f scan'
_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  0.0352
_diffrn_reflns_av_sigmaI/netI    0.0448
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            36959
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.28
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    2.557
_exptl_absorpt_correction_T_max  0.5701
_exptl_absorpt_correction_T_min  0.479
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, 2004'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.474
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1450
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.445
_refine_diff_density_min         -1.335
_refine_diff_density_rms         0.163
_refine_ls_extinction_coef       0.0043(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     771
_refine_ls_number_reflns         11177
_refine_ls_number_restraints     29
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0926
_refine_ls_R_factor_gt           0.0644
_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^)+(0.1008P)^2^+11.1332P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1776
_refine_ls_wR_factor_ref         0.1970
_reflns_number_gt                8160
_reflns_number_total             11177
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic801618m_si_003_4.cif
_cod_data_source_block           H2TPP(Ph)4Br4.2THF.1.5CH3OH
_cod_original_cell_volume        3215.98(12)
_cod_database_code               4302045